Aa-6800 Im 01

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206-94425T

Sep. 2011

Shimadzu Atomic Absorption Spectrophotometer

AA-6800F (P/N 206-50500)


AA-6800G (P/N 206-50700)
AA-6650F (P/N 206-51200)
AA-6650G (P/N 206-51300)
INSTRUCTION MANUAL

Read the instruction manual thoroughly before you use the product.
Keep this instruction manual for future reference.
This page is intentionally left blank.
COPYRIGHT:
• © 2000-2011 Shimadzu Corporation. All rights reserved. This publication may not be
reproduced in whole or in part without written permission from Shimadzu Corporation.
• Since Shimadzu products are frequently upgraded and improved, information in this
publication is subject to change without notice.
• The contents of this manual have been thoroughly inspected. Even if errors and omissions
are found, however, we might not correct them immediately.
• MS-DOS, Windows, Windows95, Windows98, Windows NT, Windows 2000 and
Windows XP are either registered trademarks or trademarks of Microsoft Corporation in
the United States and/or other countries. Other product names described in this manual are
each manufacturer's trademarks or registered trademarks.

AA-6800/6650 Instruction i
Precautions for Safe Operation

The atomic absorption spectrophotometer is used as analytical equipment for inorganic chemical analysis.
To operate this equipment safely, strictly observe the following precautions. If not observed, the safety may be
compromised.

Do not use the equipment for any purpose other than the above-mentioned types of analysis.

Follow the procedures described in the instruction manual.

Observe all warnings and cautions.

Do not disassemble or modify the equipment without the express approval of an authorized Shimadzu
Representative.

For internal repair of the equipment, contact your Shimadzu Representative.

If the user or usage location changes, ensure that this Instruction Manual is always kept together with the
product.

To ensure safe operation, contact your Shimadzu representative if product installation, adjustment, or
re-installation (after the product is moved) is required.

The meshed descriptions about installation in this instruction manual are intended for Shimadzu service
personnel. Don't use them and install the parts by yourself because it is dangerous.

In this manual, the meaning of caution signs are provided as follows.


WARNING
Indicates a potentially hazardous situation which, if not avoided, could result in serious injury or
possibly death.
CAUTION
Indicates a potentially hazardous situation which, if not avoided, may result in minor to moderate
injury or equipment damage.
NOTE
Emphasizes additional information that is provided to ensure the proper use of this product.

ii AA-6800/6650 Instruction
Precautions on the Installation Site and Handling

In the case of atomic absorption spectrophotometer, high pressure gas is generally used. Therefore, it is
necessary to take the utmost care for the installation site and handling.
Please strictly observe each precaution described in this manual as well as the precautions listed below.

1. Ventilation
The inflammable gases used for the atomic absorption spectrophotometer are liable to cause ignition. Be
sure to ventilate the room.

2. Using fire
When measuring flammable samples, special care must be taken in handling fire.
A fire extinguisher should be placed in case of accident.

3. Exhaust duct
Be sure to prepare a ventilation duct above the atomic absorption spectrophotometer so as to exhaust the
combustion gas from the burner.

4. Condensation
Avoid using the equipment in the condition where condensation may occur. The equipment may not work
properly.

5. Power requirements
The allowable voltage range and consumption power of the atomic absorption spectrophotometer and
each attachment are shown as below. Be sure to connect them to the power sources which are suitable to
these.
AA-6800/6650 main unit
Voltage: 100, 120, 220, 230, 240 VAC
Allowable voltage range: r10 %
Power capacity: 600 VA
Source frequency: 50/60 Hz
Connections: Grounded outlet
Fuse used: 6 A TYPE M (100-120 V) 2 pieces, or 3 A TYPE T (220-240 V) 2 pieces
0.63 A TYPE T (D2), 0.25 A TYPE T (HCL)
GFA-6500
Voltage: 200, 220, 230, 240 VAC
Allowable voltage range: r10 %
Power capacity: 6 kVA
Source frequency: 50/60 Hz
Connections: Grounded M6 terminal block
Fuse used: 2 A TYPE M (CONTROL), 1 A TYPE M (PHASE)

Fuse changes must be performed by service personnel.


When a fuse change is necessary, please contact your Shimadzu Representative.

AA-6800/6650 Instruction iii


6. High temperature burner
When using a nitrous oxide-acetylene flame, be sure to use the high temperature burner.

7. Standard analytical conditions


The standard analytical conditions may be changed with the surrounding temperature and humidity,
replacement of the atomizer chamber and graphite tube, and sample solution characteristics. Before
starting the measurement, search the optimum analytical conditions for each element while varying the gas
flow rate and burner height in the case of flame method and the temperature program in the case of
furnace method.

8. Internal repair and maintenance


Since the ordinary maintenance can be performed without removing the main unit cover, do not remove
the unit cover. Also, don't exchange the fuses. If the repair which requires to remove the cover is
necessary, ask it for Shimadzu Representative.

9. Gas supply hoses


Use only the rubber hose supplied as a standard accessory with this product to supply gas to the unit.
Whenever using the equipment, check the gas supply rubber hoses for a crack or deterioration caused by
adhesive chemicals. If a crack or deterioration is found, replace it with a new hose.

10. Drain tube


The drain tube connected to the chamber is not durable with petroleums (kerosene, naphtha, gasoline,
etc). When measuring these samples, ask Shimadzu for information. Every time when using the
instrument, check the drain tube and drain tank and confirm there is no liquid leak from the drain tube.

11. When a lightning surge from the power source line is given
When a momentary large voltage change is given to the instrument from the power source during using the
instrument, the communication with PC is disconnected because some function is stopped to protect the
instrument.
In this case, once turn off the power of the main unit then turn on the power again and connect it to the PC
again. Then the preparation for restarting the measurement is ready. If the instrument doesn't work
properly when powered on, contact your Shimadzu representative.

12. Cleaning the instrument


When cleaning your instrument, wipe off the outer cover and other portions with a dry soft cloth. For details
of cleaning method for component parts, refer to the Chapter 6 "Maintenance".

iv AA-6800/6650 Instruction
Precautions on Handling High Pressure Gas

High pressure gas must be handled carefully observing the legal regulation.
Not only to the following precautions, refer to regulations and laws regarding to handle the high pressure gas.
Cautionary items in this manual should be read carefully.

1. Installation of gas cylinder


(1) Install the gas cylinders in the airy outdoors where they are not exposed to direct sunlight.
(2) Take care that gas cylinders become no hotter than 40 qC, and do not allow any flame within 2 meters
of the gas cylinders.
(3) Secure gas cylinders so that they cannot drop or fall over. Always keep liquefied gas cylinders
(acetylene, nitrous oxide, etc.) in a vertical position and do not allow them to fall to a horizontal
position.

2. Acetylene gas
(1) When using acetylene gas, please use a pressure reduction valve especially made for use with
acetylene gas. Do not allow acetylene to flow through pipes, and do not use equipment made from
copper, silver, mercury, or their alloys in order to prevent the formation of metal-acetylides.
Decomposition of such compounds could result in a "decomposition explosion" resulting from a shock.
(2) The acetylene gas cylinder contains solvents such as acetone. If the primary pressure reduced below
0.5 MPa, it should be replaced with a new cylinder in order to prevent the outflow of solvents.

3. Oxygen gas
Do not use oxygen gas.

4. Air
Supply the dry air. If air containing much moisture is used, the moisture may adhere to the inside of the gas
controller and prevent normal operation. Dehumidity with a drain separator provided on the way of piping
from the air supply source.

5. After use of gas


After the gas was used, be sure to close the main valve as well as the stop valve.

6. Pressure gauge
Periodically inspect the pressure gauge to maintain its normal function.

AA-6800/6650 Instruction v
7. Pressure regulator
(1) Use approved pressure regulators and connectors. For details, contact your Shimadzu
Representative.
(2) When installing the pressure regulator to the cylinder, be sure to wipe the dust at the outlet of the
cylinder.
(3) Damaged or cracked screws for installing the pressure regulator may cause gas leakage. Do not
install the pressure regulator forcibly, but replace with a new gas cylinder.

8. Cylinder opening/closing
(1) Before opening the cylinder, be sure to check that the stop valve is closed. Turn the secondary
pressure adjusting valve fully to the left, and open the cylinder using a special handle. Even if the main
valve is too tight to open, do not hit the handle or main valve with the hammer or spanner.
(2) After the main valve is opened, apply soapy water to the connection of the pressure regulator to check
if no gas leak is generated. Also check the connection at the main valve.
(3) Completely open the main valve of the cylinder for nitrous oxide gas, argon gas and hydrogen gas. If it
is not completely opened, the flow rate of the gas, particularly of the nitrous oxide gas, may fluctuate
during use.
(4) When opening the main valve of the cylinder for acetylene gas, rotate it by 1 rotation or 1.5 rotations
from the state of complete closing.
To prevent outflow of acetone from the inside of the cylinder, do not open the valve exceeding 1.5
rotations from the state of complete closing. On the contrary, if the main valve is not sufficiently
opened in case of nitrous oxide-acetylene flame (high temperature flame), flashback may be caused
due to insufficient acetylene when the flame is switched from an air-acetylene flame to nitrous
oxide-acetylene flame.

vi AA-6800/6650 Instruction
Action in the Case of Fuel Gas Leakage

WARNING

When executing [Start Leak Check] in the "Initialize" dialog box or [Instrument]-[Gas Leak Check] in the
menu bar, an automatic gas leak check is performed for about 11 minutes.

If the instrument does not detect any fuel gas leakage, the following message is displayed on the screen
after about 11 minutes, after which the flame can be ignited.

If the instrument detects any fuel gas leakage, the following message is displayed on the screen at that time.

In this case, please close the stop valve of the fuel gas immediately.
Once completed, disconnect the communication between PC and the instrument, and turn the power supply
off. Be sure to contact your service representative to check and repair the instrument.

AA-6800/6650 Instruction vii


Precautions on Handling Hollow Cathode Lamp

Electrodes of some hollow cathode lamps contain harmful metal elements (As, Be, Hg, Se, etc.). Some
electrode metals may ignite when touched with air or water (K, Li and Na). Read the precautions attached to the
hollow cathode lamp thoroughly and handle the lamp very carefully for safety.

1. When disposing of the lamp


If the hollow cathode lamp should be broken or its life is finished, dispose of the lamp separately from
general garbage. When disposing of the hollow cathode lamp supplied from Shimadzu Co., select a
method which will not influence the environmental pollution or human body, or ask a special disposal
dealer.
The material of hollow cathode lamp are as follows.
• Metals (including electrode element)
• Quartz glass
• Plastic
Some electrode contains harmful metal (Hg, As, etc.).

2. Specifications change
The specifications of the hollow cathode lamp are subject to change for improvement without notice. In this
case, set the lighting current referring to the precautions attached to the hollow cathode lamp.

Precautions on Handling Deuterium (D2) Lamp

When disposing of the lamp


If the deuterium (D2) lamp should be broken or its life is finished, dispose of the lamp separately from general
garbage. When disposing of the deuterium (D2) lamp supplied from Shimadzu Co., select a method which will
not influence the environmental pollution or human body, or ask a special disposal dealer.
The material of deuterium (D2) lamp are as follows.
• Metals (Tungsten)
• Quartz glass
• Ceramic
• Plastic

Handling Waste Liquid

Waste liquid discharged during measurement or pretreatment should be handled in different ways in
accordance with the solute and solvent contained in that waste liquid. The way of handling waste liquid is
different depending upon the country or region.
Be sure to dispose of waste liquid according to the location of use.
When handling waste liquids, wear protective gloves and safety goggles.

viii AA-6800/6650 Instruction


Supply Period of Replacement Parts

Replacement parts are supplied by the Shimadzu Parts Center. The supply period of these parts is determined
as below.

As a general rule, seven (7) years after the discontinuation of the product.
Note, however, that the availability of units or parts not manufactured by Shimadzu shall be determined by the
relevant manufacturers. If Shimadzu should receive a notice of the discontinuation of the units or parts, the
necessary quantity for the above period is immediately calculated and secured. However, such parts may
cease to be available within seven years after the discontinuation of the product, depending on the situation of
the relevant manufacturers or change of the necessary quantity.

Warning Marking on the Equipment

WARNING
RISK OF BURN
Do not touch the burner head and atomizer compartment before it is cooled sufficiently.

Label, WARNING

Figure 1

AA-6800/6650 Instruction ix
WARNING
HAZARDOUS VOLTAGE
Do not touch the electrodes when the power is ON.

Label, WARNING

Figure 2

WARNING
HOT SURFACE
Risk of burn.
Before replacing the lamp, set the power switch off and cool down the lamp.

Label, WARNING

Figure 3

x AA-6800/6650 Instruction
WARNING
FLAMMABLE GAS
Before ignition, be sure to read the instruction manual.

Label, WARNING

Figure 4

WARNING
RISK OF EXPLOSION
Do not use oxygen gas.

Label, WARNING

Figure 5

AA-6800/6650 Instruction xi
WARNING
FLAMMABLE GAS
Be sure to close main gas valve when gas is not in use.

Label, WARNING

Figure 6

xii AA-6800/6650 Instruction


Emergency Action

Take the following measures in case of emergency or when an abnormal condition is found in the atomic
absorption spectrophotometer.
Inspect the equipment before using it again and contact a service engineer if necessary.

Emergency Action
1. Turn OFF the power switch of the atomic absorption spectrophotometer.
Even if measurement is in progress, the burner flame can be extinguished by turning the power switch
OFF.
2. Turn OFF all the power switches of accessories.
3. Close the main valves of the gas supply pipings for acetylene, air, nitrous oxide, hydrogen and argon.
4. Close the main valve of the cooling water supply piping.
5. Shut OFF the power supply.
• Turn OFF the switchboard when the power cable is fixed to the switchboard with screws.
• Disconnect the power cable when the power cable is connected with the plug.

Power switch
Power cable

Figure 7 Power Switch and Power Cable of Atomic Absorption Spectrophotometer

Power cable Power switch

Figure 8 Power Switch and Power Cable of GFA-6500

AA-6800/6650 Instruction xiii


Inspection Procedure in Case of Flashback

Since the AA-6650/6800 is equipped with the several safety systems that prevent a flashback, there is little
possibility a flashback occurs.
In case a flashback should occur, however, a service engineer from Shimadzu will perform the following
inspection procedure. Never ignite the flame before the safety is confirmed as the result of the inspection.

<2> Cover mounting screw


<3> Chamber cover

<4'> Safety plug plate

<15> Quick-connect joint


<1> Burner head
<14> Gas tube

<16> Burner socket

<11> Impact bead


<17> O-rings

<5> O-ring <9> Retaining plate

<8> Fixing screw

<4> Safety bung

<10> Nebulizer

<12> Mixer
<6> Chamber fixing screw
<13> O-ring
<7> Drain tube

Figure 9 Burner Unit

(1) Remove the burner head <1>.


Note that the burner head is still hot just after the flame is extinguished.
(2) Loosen the chamber fixing screws <2> (4 positions) and remove the chamber cover <3>.

(3) If the safety bung <4> is released, check that the O-ring <5> of the safety valve is not cracked or
deteriorated then push the safety bung into the chamber unit <2>, and set the plate <4'> as before. Even if
the safety bung is not released, push the safety bung and check that it is properly mounted to the chamber.

(4) Remove the chamber fixing screw <6>.


Lift up the chamber upward and check that the drain tube <7> is not damaged.
Then put the chamber back to the original position and tighten the fixing screw.

xiv AA-6800/6650 Instruction


(5) Loosen the fixing screw <9> on the nebulizer retaining plate <8> and remove the nebulizer <10>.

(6) Check that the mixer <12> in the chamber is not damaged.

(7) Check that the O-ring <13> in the nebulizer is not cracked or deteriorated then mount the nebulizer back to
the chamber. At this time, be careful not to hit the Impact bead <11> to the chamber inner wall.
Also, check that the nebulizer O-ring is not pressed out from the socket.
(8) Fix the nebulizer firmly with the retaining plate.

(9) Check that the gas tube <14> connected with the chamber is not damaged.

(10) Insert the gas tube connected with the quick-connect joint <15> and check that it is not disconnected by
pulling it.

(11) Mount the chamber cover and fix it firmly with the screws.

(12) Check that burner head slot is not clogged. If clogged, clean the burner head.

(13) Check that the O-rings <17> of the burner socket <16> are not cracked or deteriorated. Then mount the
burner head on the port.

(14) When checking the drain sensor, start up the AA unit and wizAArd software beforehand. Remove the drain
tank lid <18> and take out the liquid level sensor <19> from the drain tank <20>. Check that an error
message appears on the PC screen.
Finally put the liquid level sensor back into the drain tank and close the lid.

<18> Drain tank lid

<19> Liquid level sensor

<20> Drain tank

Figure 10 Drain Tank

AA-6800/6650 Instruction xv
General Precautions

In order to use the atomic absorption spectrophotometer safely, be sure to observe the following cautions. If not
observed, the safety of this equipment may be compromised.

WARNING

(1) When pressing the ignition button (at igniting), never put your face or hands in the burner compartment
(combustion chamber). Do not look into from above the combustion chamber and do not hold your
hands over the combustion chamber.
When N2O-C2H2 flame is ignited, the flame goes up to the level of approx. 40 cm from the top of the
equipment. Care should be taken.
Before igniting a flame, be sure to close the flame shield (combustion chamber door).
(2) Do not ignite a flame unless the burner is mounted on the chamber.

(3) Do not ignite a flame unless the nebulizer is mounted on the chamber.

(4) Do not ignite a flame unless the drain tank is filled with water.

(5) Do not ignite a flame when the drain tube is removed from the chamber.

(6) Do not remove the nebulizer from the chamber during combustion.

(7) Do not remove the drain tube from the chamber during combustion.

(8) Do not remove the burner during combustion.

(9) Do not touch the burner while it is hot.

(10) Do not touch the deuterium lamp while it is hot.

(11) Do not touch the end of cleaning wire for nebulizer capillary directly by hand. Wire may stick your finger.

(12) Do not touch the flame shield during combustion. It is very hot by the heat of flame and dangerous.

(13) Do not touch the flame shield and burner directly by hand for 20 minutes after extinguishment of the
flame. It is very hot by the heat of the flame.

(14) Do not use flammable aerosol sprays (such hairsprays or spray-type insecticides) near the instrument.
The high-temperature parts of the atomizer and lamps, and sparks from the igniter, could cause
inflammation and fire.
(15) When handling highly corrosive liquids, use protective gloves and protective goggles to protect your
skin and eyes. A back fire could cause liquid to gush out.

xvi AA-6800/6650 Instruction


CAUTION

(1) Do not use the flame for any purpose other than analysis.

(2) Do not hold any substance over the flame.

(3) Do not remove the thermal shield plate when using the atomic absorption spectrophotometer in flame
method. If the thermal shield plate is removed, heat of flame is introduced to the instrument inside and
measurement may be unreliable.

(4) Check the setting of gas flow rate before igniting a flame.

(5) Do not use the standard burner (10 cm slot burner) when the recognizing key is still left in the hole of the
burner select sensor (BURNER SELECT).

(6) Do not put any foreign objects in the hole of the burner select sensor.

(7) Do not put any foreign objects in the lamp socket.

(8) Do not connect the power cable to the outlet that is not provided with grounding terminals.

(9) Do not put your fingers or hands in the hold of lamp turret, igniter and flame monitor.

Moving or Transporting the AA-6800/6650

To move or transport the installed AA-6800/6650, contact our sales office or representative.
If the AA-6800/6650 is moved or transported without the above contact, the warranty will not be applied to any
failure.

Warning on Sample to Be Measured

Do not measure any explosive sample.


Such measurement not only could cause a failure in or damage to the AA-6800/6650, but also might endanger
the user's safety.

AA-6800/6650 Instruction xvii


Safety Service Parts List

The following parts become exhausted or damaged depending on the conditions of use. Check these parts
periodically. When abnormalities are discovered in the parts, replace them immediately. There is a possibility
that an accident, i.e. gas leakage, may happen if the abnormal parts are used continuously without
replacement.
For details on the check method, see the daily check list. Even when no abnormality is found, replace these
parts at the standard replacement interval.

Periodic Check Part Replacing Part Replacing


Daily Check
(1 Time Per Year) (Chapter 1.) (Chapter 2.)

Customer (*1)

Service Engineer

(*1) Contact your Shimadzu service representative for a more assured check.

Also there is another service parts list for maintaining performance on the instruction manual. Read the
instruction manual for more details.

1. Parts which a customer can replace (replaced every 3 years)

Burner head ASSY 206-50370-92 10 cm, Titanium made

2. Parts which a service engineer replaces (replaced every 3 years)


(1) O-ring set (*2)

O-ring set 206-82037-92 Standard parts


Fluorine rubber (FKM)

(*2) The replacement cycle becomes shorter when solvents other than water are being used. Refer to
3. "Chemical resistance of the O-ring, the drain joint and the drain tube". The following O-ring sets
can be used according to the solvent.

O-ring set 206-82037-94 Refer to 3. "Chemical resistance of the O-ring, the


Silicon rubber (VMQ) drain joint and the drain tube".

O ring set 206-82037-96 Refer to 3. "Chemical resistance of the O-ring, the


Kalrez“ (FFKM) drain joint and the drain tube".

(2) Nebulizer

Elbow, 31020600 035-65268-02 Connecting Nebulizer the spray tube.

(3) High temperature burner head

Burner head ASSY 206-50300-92 5 cm, Titanium made

(4) Drain joint (*3)

Joint 206-52702-91 The joint under the chamber

(*3) The replacement cycle becomes shorter when solvents other than water are being used. Refer to
3. "Chemical resistance of the O-ring, the drain joint and the drain tube". The following O-ring sets
can be used according to the solvent.

xviii AA-6800/6650 Instruction


(5) Drain tube (*4)

Tube, Supercone 9 u 13 016-43200-08 Drain hose under the chamber.


Specify required length (standard: 30 cm).

(*4) The replacement cycle becomes shorter when solvents other than water are being used. Refer to
3. "Chemical resistance of the O-ring, the drain joint and the drain tube". The following O-ring sets
can be used according to the solvent.

(6) Drain bottle

Drain bottle ASSY 206-80771-91 Overflow system drainage trap

(7) Gas tube

Gas tube ASSY 206-65112 Gas supply nylon tube set

(8) Pressure regulator

Pressure regulator ASSY 206-61825-12 For FUEL

Pressure regulator ASSY 206-61825-13 For SUPPORT

(9) Rubber hose

Hose, 8 u 2 B-G 016-02101-01 It is attached to the high temperature burner head.


For N2O (green)
Specify required length (standard: 5 m).

Hose, 8 u 2 B-R 016-02101-03 For fuel gas (red)


Specify required length (standard: 5 m).

Hose, 8 u 2 B-BK 016-02101-04 For air (black)


Specify required length (standard: 5 m).

AA-6800/6650 Instruction xix


3. Chemical resistance of the O-ring, the drain joint and the drain tube
Verify that the material of the O-ring, the drain joint and the drain tube has tolerance for the solvent.

O-Ring Drain Tube

Fluorine Silicon Drain Joint


Kalrez“ (PP) Supercone Custom
Rubber Rubber
(FFKM) Ace Order
(FKM) (VMQ)

Water (*5)

Acetic acid

Acetone

Aqua regia

Butyl acetate

Ethanol

Gasoline

Hydrochloric acid

Hydrofluoric acid

Kerosene

Methanol

Methyl Isobutyl
Ketone (MIBK)

Nitric acid

Perchloric acid

Oil

Sodium hydroxide

Sulfuric acid

Tetrahydrofuran

Toluene

Xylene

; Good to use, replacing every three years


; Good to use, replacing every year
; Good to use, replacing every month
; Prohibit to use
(*5) 0.5% or less of acid concentration
Kalrez“ is a registered trademark of DuPont Performance Elastomers.

xx AA-6800/6650 Instruction
Daily Check List

For flame measurement of Atomic Absorption Spectrophotometer, this is the daily check list in connection with
safety. Be sure to check the points below.

Check Items Contents

Before ignition

1 There is no clogging in the burner Verify by using hard paper etc.


slot.

2 Attachment of parts is normal. Verify that the burner head and nebulizer are not loosened.

3 Checking of a pilot flame part Verify that the pilot flame is straightly suitable to the burner
head.

4 The waste fluid is not overflowing Discard the waste fluid if it has accumulated.
from the waste fluid container. The
tip of the drain hose has not sunk.

5 Funnel is correctly equipped. Four pins of Funnel have got into regular positions.

6 Each setting of the built-in pressure Press the PURGE button, verify that the fuel gas pressure is
regulators is normal. 0.05 MPa and that the support gas pressure is 0.25 MPa.

7 The gas flow rate is normal. Press the PURGE button, verify that the flow rate of the
support gas (Air) is 8 L/min.

8 Attachment of the safety plug is Verify that the safety plug plate is visible. If there is no safety
normal. plug plate, verify that the safety plug is inserted in the back
every month.

9 There is no crack etc. in the rubber Check visually every month.


hose for gas supply. The hose band
has been tightened firmly.

10 There is no gas leakage. A gas leakage check is carried out every month.
Refer to 6.3 "Checking for Gas Leaks in Tubing" in this manual.
After checking for gas leaks, check that piping is connected
securely.

11 Checking at Initialization of the Verify the following every month when initializing the
instrument instrument.
(1) When pressing the PURGE button after shutting off the
main valves of fuel gas and supporting gas, a "gas
pressure error" message should be displayed.
(2) Drain tank is filled with water or solvent.
(3) When taking out the level sensor from the Drain tank, the
message "the water level of Drain tank is low", should be
displayed.

12 There is neither a crack nor a hole Check visually every month.


in Drain hose. There is no crack in each hose between Chamber and Drain
tank, and between Drain tank and a waste fluid container.

13 When using the high temperature Verify annually that the width of the slot of the high
burner head as the optional temperature burner head is 0.55 mm or less by using a
accessory, the width of the slot has skimmer gauge (P/N 081-04202-11). Request to check for a
not spread. service engineer if needed.

AA-6800/6650 Instruction xxi


Check Items Contents

14 The check of O-rings replacing Verify the replacement intervals of the O-rings for every solvent
cycle. currently used. Request your Shimadzu service representative
to replace O-rings. The service representative will check that
no bubble is generated on applying detection liquid (P/N
670-11514) after replacement.

After using instrument

1 Water is drained from the air The scupper of the air compressor is certainly performed after
compressor. using instrument.

xxii AA-6800/6650 Instruction


Action for Environment (WEEE)

To all users of Shimadzu equipment in the European


Union:
Equipment marked with this symbol indicates that it was sold on or after 13th August 2005,
which means it should not be disposed of with general household waste. Note that our
equipment is for industrial/professional use only.

Contact Shimadzu service representative when the equipment has reached the end of
its life. They will advise you regarding the equipment take-back.

WEEE Mark

With your co-operation we are aiming to reduce contamination from waste electronic and electrical equipment
and preserve natural resource through re-use and recycling.
Do not hesitate to ask Shimadzu service representative, if you require further information.

AA-6800/6650 Instruction xxiii


xxiv AA-6800/6650 Instruction
AA-6800/6650 Instruction xxv
xxiii
This page is intentionally left blank.

xxvi
xxiv AA-6800/6650 Instruction
Contents
Precautions for Safe Operation

Precautions on the Installation Site and Handling

Precautions on Handling High Pressure Gas

Action in the Case of Fuel Gas Leakage

Precautions on Handling Hollow Cathode Lamp

Precautions on Handling Deuterium (D2) Lamp

Handling Waste Liquid

Supply Period of Replacement Parts

Warning Marking on the Equipment

Emergency Action

Inspection Procedure in Case of Flashback

General Precautions

Moving or Transporting the AA-6800/6650

Warning on Sample to Be Measured

Safety Service Parts List

Daily Check List

Action for Environment (WEEE)

Chapter 1 Overview
1.1 Overview of AA-6800/6650 .................................................................................................... 1-2
1.2 Specifications......................................................................................................................... 1-3

Chapter 2 Installation
2.1 Parts Inspection ..................................................................................................................... 2-2
2.2 Instrument Placement and Site Requirements ...................................................................... 2-6
2.3 Equipment Requirements ...................................................................................................... 2-8
2.3.1 Power Requirements ................................................................................................. 2-8
2.3.2 Water Supply Requirements ...................................................................................... 2-8
2.3.3 Gas Requirements ..................................................................................................... 2-8
2.3.4 Ventilation System ................................................................................................... 2-10
2.3.5 Use of an Air Compressor........................................................................................ 2-11
2.3.6 General Precautions for Handling Gas Cylinders .................................................... 2-12
2.3.7 Installing Pressure Regulators (Optional) and Checking for Leaks ......................... 2-13
2.3.8 Software Operation Minimum Requirements (to be provided by user) .................... 2-15
2.4 Assembling the AA-6800/6650 ............................................................................................ 2-17
2.4.1 Connecting the Drain Tube ...................................................................................... 2-17
2.4.2 Assembling the Burner............................................................................................. 2-18

AA-6800/6650 Instruction xxvii


xxv
2.4.3 Cable Connections................................................................................................... 2-19
2.4.4 Hose Connections.................................................................................................... 2-20
2.4.5 Replacing the AA-6650 Atomizer ............................................................................. 2-21
2.4.6 Installation of PC Software....................................................................................... 2-23
2.5 Mounting a Hollow Cathode Lamp....................................................................................... 2-25
2.6 Installing the ACF-6800 ....................................................................................................... 2-26

Chapter 3 Instrument Constructions


3.1 AA-6800/6650 Configurations................................................................................................ 3-2
3.1.1 Operation Switches .................................................................................................... 3-2
3.1.2 Hollow Cathode Lamp Turret ..................................................................................... 3-3
3.1.3 Deuterium Lamp......................................................................................................... 3-4
3.1.4 Burner Module............................................................................................................ 3-5
3.1.4.1 AA-6800 ...................................................................................................... 3-5
3.1.4.2 AA-6650 ...................................................................................................... 3-6
3.1.5 Burner ........................................................................................................................ 3-7
3.1.6 Gas Control Panel...................................................................................................... 3-8
3.1.7 Optical System ......................................................................................................... 3-10
3.1.8 Photometric System ................................................................................................. 3-11

Chapter 4 Basic Operation


4.1 Switching On the Power and Starting Up the Software ......................................................... 4-2
4.1.1 Switching ON the Power to Hardware........................................................................ 4-2
4.1.2 Starting Up the Software ............................................................................................ 4-3
4.2 Software Basic Operation ...................................................................................................... 4-4
4.2.1 Software Basic Operation (Flame Method) ................................................................ 4-4
4.2.1.1 Operation Flowchart (Flame Method) ......................................................... 4-4
4.2.1.2 Wizard Selection ......................................................................................... 4-5
4.2.1.3 Element Selection ....................................................................................... 4-5
4.2.1.4 Preparation Parameters .............................................................................. 4-7
4.2.1.5 Sample ID ................................................................................................. 4-10
4.2.1.6 Sample Selection ...................................................................................... 4-11
4.2.1.7 Connect to Instrument/Send Parameters.................................................. 4-12
4.2.1.8 Optics Parameters .................................................................................... 4-13
4.2.1.9 Atomizer/Gas Flow Rate Setup (AA-6800) ............................................... 4-15
4.2.1.10 Atomizer/Gas Flow Rate Setup (AA-6650) ............................................... 4-17
4.2.2 Software Basic Operation (Furnace Method)........................................................... 4-19
4.2.2.1 Operation Flowchart (Furnace Method) .................................................... 4-19
4.2.2.2 Wizard Selection ....................................................................................... 4-20
4.2.2.3 Element Selection ..................................................................................... 4-20
4.2.2.4 Preparation Parameters ............................................................................ 4-23
4.2.2.5 Sample ID ................................................................................................. 4-28
4.2.2.6 Sample Selection ...................................................................................... 4-29
4.2.2.7 Connect to Instrument/Send Parameters.................................................. 4-30
4.2.2.8 Optics Parameters .................................................................................... 4-31
4.2.2.9 Furnace Program ...................................................................................... 4-33
4.2.3 Saving the Template ................................................................................................ 4-35
4.3 Measurement Procedures.................................................................................................... 4-36
4.3.1 Measurement Operation (for Flame Method)........................................................... 4-36
4.3.2 Measurement Operation (for Furnace Method)........................................................ 4-38
4.4 Saving/Printing/Deleting the Data ........................................................................................ 4-39
4.4.1 Saving the Data........................................................................................................ 4-39

xxviii
xxvi AA-6800/6650 Instruction
4.4.2 Printing the Data ...................................................................................................... 4-39
4.4.3 Deleting the Data ..................................................................................................... 4-39
4.5 Completing the Measurement.............................................................................................. 4-40
4.6 Explanation of Main Window ............................................................................................... 4-41
4.6.1 Menu Bar ................................................................................................................. 4-42
4.6.2 Standard Tool Bar.................................................................................................... 4-42
4.6.3 Measurement Element Tool Bar .............................................................................. 4-42
4.6.4 Absorbance Digital Display ...................................................................................... 4-42
4.6.5 Real Time Graph (and Furnace Program Graph) .................................................... 4-42
4.6.6 Peak Profile (Latest Four Measurements and Overlay Display) .............................. 4-44
4.6.7 Calibration Curve Display ........................................................................................ 4-45
4.6.8 MRT Worksheet ....................................................................................................... 4-47
4.6.9 Function Buttons ...................................................................................................... 4-48
4.6.10 Status Bar ................................................................................................................ 4-49
4.7 Operating the MRT Worksheet ............................................................................................ 4-50
4.7.1 Fields of MRT Worksheet ........................................................................................ 4-50
4.7.2 Right Mouse Button Menu ....................................................................................... 4-54
4.7.3 Right Mouse Button on Summary Table .................................................................. 4-57
4.7.4 Inserting and Deleting the Measurement Row ......................................................... 4-57
4.7.5 Active Cell Movement by Shortcut Key and Cell Selection ...................................... 4-58
4.7.5.1 Moving an Active Cell ............................................................................... 4-58
4.7.5.2 Selecting Cells .......................................................................................... 4-58
4.7.6 Copy and Paste ....................................................................................................... 4-59
4.7.6.1 Copy.......................................................................................................... 4-59
4.7.6.2 Paste......................................................................................................... 4-59
4.7.7 Changing Column Width and Column Header Height of MRT Worksheet .............. 4-60
4.8 Igniting and Extinguishing the Flame ................................................................................... 4-61
4.8.1 Operation Locations ................................................................................................. 4-61
4.8.2 Safety Precautions Prior to Ignition.......................................................................... 4-61
4.8.3 Igniting and Extinguishing Air-C2H2, Air (Ar)-H2 Flames ......................................... 4-62
4.8.4 Igniting and Extinguishing N2O-C2H2 Flame ........................................................... 4-64
4.8.5 Flame Conditions When Analyzing Organic Solvent Samples ................................ 4-66
4.9 Standard Addition Method and Simple Standard Addition Method...................................... 4-67
4.9.1 Setting the [Edit Preparation Parameters] Dialog Box ............................................. 4-68
4.9.2 Measurement Procedures on MRT Worksheet........................................................ 4-70
4.10 Conditions and Operation for Flame Emission Analysis ...................................................... 4-72
4.10.1 [Optics Parameters] Page ........................................................................................ 4-72
4.10.2 [Atomizer/Gas Flow Rate Setup] Page .................................................................... 4-74
4.10.2.1 AA-6800 .................................................................................................... 4-74
4.10.2.2 AA-6650 .................................................................................................... 4-76
4.10.3 Line Search and Beam Balance .............................................................................. 4-78
4.11 Setting the Optimum Conditions for Fuel Gas Flow Rate and Burner Height (AA-6800)..... 4-79
4.11.1 Setting the Optimum Condition of Burner Height ..................................................... 4-79
4.11.2 Setting the Optimum Condition of Fuel Gas Flow Rate ........................................... 4-80

Chapter 5 Functions of Operation Menu


5.1 [Wizard Selection] Dialog Box ............................................................................................... 5-2
5.1.1 [Wizard] Page ............................................................................................................ 5-2
5.1.2 [Recent Files] Page.................................................................................................... 5-2
5.1.3 [Recent Templates] Page .......................................................................................... 5-2
5.2 [File] ....................................................................................................................................... 5-3
5.2.1 [New].......................................................................................................................... 5-3

AA-6800/6650 Instruction xxix


xxvii
5.2.2 [Open] ........................................................................................................................ 5-4
5.2.3 [Save] ......................................................................................................................... 5-4
5.2.4 [Save As...]................................................................................................................. 5-5
5.2.5 [Additional Load] ........................................................................................................ 5-5
5.2.6 [File Export...] ............................................................................................................. 5-6
5.2.7 [Export Items] ............................................................................................................. 5-6
5.2.8 [Auto Save]................................................................................................................. 5-7
5.2.9 [Print Data/Parameters...]........................................................................................... 5-9
5.2.10 [Print Table Data...] .................................................................................................. 5-10
5.2.11 [Print Style]............................................................................................................... 5-10
5.2.11.1 [Print Style Setup] Page ............................................................................ 5-10
5.2.11.2 [Table Show/Hide] Page ........................................................................... 5-11
5.2.11.3 [Font] Page................................................................................................ 5-11
5.2.12 [Print Setup] ............................................................................................................. 5-12
5.2.13 Recent Files ............................................................................................................. 5-12
5.2.14 [Exit] ......................................................................................................................... 5-12
5.3 [Edit]..................................................................................................................................... 5-13
5.3.1 [Insert Row] .............................................................................................................. 5-13
5.3.2 [Delete Rows]........................................................................................................... 5-13
5.3.3 [Import Other Schedule] ........................................................................................... 5-13
5.3.4 [Collective Edit] ........................................................................................................ 5-13
5.3.5 [Remeasure Selected Range] .................................................................................. 5-13
5.3.6 [Clear Measurement Result] .................................................................................... 5-14
5.3.7 [Copy]....................................................................................................................... 5-14
5.3.8 [Paste] ...................................................................................................................... 5-14
5.4 [Refer to Parameters]........................................................................................................... 5-15
5.5 [Parameters] ........................................................................................................................ 5-16
5.5.1 [Element Selection] Page......................................................................................... 5-17
5.5.1.1 [Cookbook] Page....................................................................................... 5-18
5.5.1.2 [Template] Page........................................................................................ 5-19
5.5.2 [Preparation Parameters] Page................................................................................ 5-20
5.5.2.1 Weight Correction Factors ........................................................................ 5-22
5.5.2.2 [Preparation Parameters]-[Standard Samples] ......................................... 5-22
5.5.2.3 [Preparation Parameters]-[Unknown Samples]......................................... 5-23
5.5.2.4 [Preparation Parameters]-[Blank Samples]............................................... 5-23
5.5.2.5 Mixing Setup and Reagent Setup ............................................................. 5-24
5.5.2.6 Coating and Boost Cycles (only for Furnace Method) .............................. 5-25
5.5.2.7 Repeat Measurement Conditions.............................................................. 5-26
5.5.3 [Sample ID] Page ..................................................................................................... 5-26
5.5.4 [Sample Selection] Page.......................................................................................... 5-28
5.5.5 [Connect to Instrument/Send Parameters] Page ..................................................... 5-28
5.5.6 [Optics Parameters] Page ........................................................................................ 5-29
5.5.6.1 [Lamp Pos. Setup] Button ......................................................................... 5-32
5.5.6.2 [Warmup Lamp] Button ............................................................................. 5-32
5.5.6.3 [Line Search] Button.................................................................................. 5-33
5.5.7 [Atomizer/Gas Flow Rate Setup] Page (for Flame Method by AA-6800) ................. 5-34
5.5.7.1 Atomizer Position ...................................................................................... 5-34
5.5.7.2 [Burner Position Auto] Button.................................................................... 5-36
5.5.7.3 Fuel Gas Flow Rate .................................................................................. 5-37
5.5.7.4 [Gas Flow Auto] Button ............................................................................. 5-38
5.5.8 [Atomizer/Gas Flow Rate Setup] Page (for Flame Method by AA-6650) ................. 5-39
5.5.8.1 Atomizer Position ...................................................................................... 5-39
5.5.8.2 Fuel Gas Flow Rate .................................................................................. 5-40

xxx
xxviii AA-6800/6650 Instruction
5.5.9 [Furnace Program] Page (for Furnace Method) ....................................................... 5-41
5.5.9.1 [Coating/Boost Cycle] Button .................................................................... 5-43
5.5.9.2 [Test Meas.] Button................................................................................... 5-44
5.5.9.3 [Cleaning] Button ...................................................................................... 5-45
5.5.9.4 [Change Graphite Tube] Button ................................................................ 5-45
5.5.9.5 [Temp. Search] Button .............................................................................. 5-46
5.6 [Edit Parameters] ................................................................................................................. 5-48
5.6.1 [Measurement Parameters] Page ............................................................................ 5-48
5.6.2 [Repeat Measurement Conditions] Page ................................................................. 5-51
5.6.3 [Weight Correction Factors] Page ............................................................................ 5-53
5.6.4 [Y-axis Print Range] Page........................................................................................ 5-54
5.6.5 [Analyst] Page.......................................................................................................... 5-54
5.6.6 [Comment] Page ...................................................................................................... 5-54
5.6.7 [Sequence] Page ..................................................................................................... 5-55
5.6.8 [ASC Parameters] Page........................................................................................... 5-56
5.6.9 [QA/QC Setup] Page................................................................................................ 5-57
5.6.10 [Calibration Curve Parameters] Page ...................................................................... 5-60
5.6.11 [Optics Parameters] Page ........................................................................................ 5-61
5.6.12 [Atomizer/Gas Flow Rate Setup] Page (Flame Method) .......................................... 5-61
5.6.13 [Furnace Program] Page (Furnace Method) ............................................................ 5-61
5.7 [Default Parameters] ............................................................................................................ 5-62
5.7.1 [Flame] ..................................................................................................................... 5-62
5.7.2 [Furnace].................................................................................................................. 5-62
5.7.3 [Graph] ..................................................................................................................... 5-62
5.7.4 [Analyst] ................................................................................................................... 5-62
5.8 [Instrument] .......................................................................................................................... 5-63
5.8.1 [Connect].................................................................................................................. 5-64
5.8.2 [Option Connect] ...................................................................................................... 5-65
5.8.3 [Configuration].......................................................................................................... 5-66
5.8.4 [Lamp Position Setup] .............................................................................................. 5-70
5.8.5 [Lamp History] .......................................................................................................... 5-71
5.8.6 [Maintenance] .......................................................................................................... 5-72
5.8.6.1 [D2 Lamp Position].................................................................................... 5-72
5.8.6.2 [Wavelength Adjustment] .......................................................................... 5-72
5.8.6.3 [Burner Origin Position Adjustment] (AA-6800) ........................................ 5-73
5.8.6.4 [Furnace Origin Position Adjustment] (AA-6800) ...................................... 5-74
5.8.6.5 [Burner Origin Position Adjustment] (AA-6650) ........................................ 5-75
5.8.6.6 [Furnace Origin Position Adjustment] (AA-6650) ...................................... 5-75
5.8.6.7 [ASC Maintenance] ................................................................................... 5-76
5.8.6.8 [Maintenance only for Service Engineer] .................................................. 5-77
5.8.7 [Lamp Status]........................................................................................................... 5-78
5.8.8 [Change Graphite Tube] .......................................................................................... 5-79
5.8.9 [Gas Controller Status]............................................................................................. 5-80
5.8.10 [Gas Leak Check] .................................................................................................... 5-80
5.8.11 [Remaining Gas Combustion] .................................................................................. 5-81
5.8.12 [Execute Line Search] .............................................................................................. 5-82
5.8.13 [Cleaning]................................................................................................................. 5-82
5.8.14 [Rinse Nozzle] .......................................................................................................... 5-82
5.8.15 [Flame Nozzle Position] ........................................................................................... 5-82
5.8.16 [Furnace Nozzle Position] ........................................................................................ 5-83
5.9 [Help] ................................................................................................................................... 5-85
5.9.1 [Search for Help on...] .............................................................................................. 5-85
5.9.2 [About WizAArd...].................................................................................................... 5-85

AA-6800/6650 Instruction xxxi


xxix
Chapter 6 Maintenance
6.1 Atomizer Position Adjustment ................................................................................................ 6-2
6.1.1 Burner Positioning Adjustment................................................................................... 6-2
6.1.1.1 AA-6800 ...................................................................................................... 6-2
6.1.1.2 AA-6650 ...................................................................................................... 6-3
6.1.2 Furnace Position Adjustment ..................................................................................... 6-4
6.1.2.1 AA-6800 ...................................................................................................... 6-4
6.1.2.2 AA-6650 ...................................................................................................... 6-4
6.2 Burner Maintenance............................................................................................................... 6-5
6.2.1 Cleaning the Burner Head.......................................................................................... 6-5
6.2.2 Nebulizer Maintenance .............................................................................................. 6-6
6.2.2.1 Cleaning the Nebulizer................................................................................ 6-6
6.2.2.2 Replacing the Polyethylene Tube ............................................................... 6-8
6.2.3 Washing the Chamber ............................................................................................... 6-8
6.3 Checking for Gas Leaks in Tubing......................................................................................... 6-9
6.4 Replacing the Deuterium Lamp ........................................................................................... 6-10
6.4.1 Specifications of Deuterium Lamp ........................................................................... 6-10
6.4.2 Replacing Procedures of Deuterium Lamp .............................................................. 6-10
6.5 Maintenance Parts ............................................................................................................... 6-12
6.6 Special Accessories............................................................................................................. 6-14
6.6.1 For Flame Analysis .................................................................................................. 6-14
6.6.2 For Furnace Analysis (for GFA-EX7) ....................................................................... 6-14
6.6.3 Autosampler ............................................................................................................. 6-14
6.6.4 Hollow Cathod Lamps (Single Element Lamps)....................................................... 6-15
6.6.5 Hollow Cathode Lamps (Single Element Lamps, Usable for SR Method) ............... 6-17
6.6.6 Hollow Cathod Lamp (Multi-element Lamps) ........................................................... 6-18
6.6.7 Other Accessories.................................................................................................... 6-18

Chapter 7 Appendix
7.1 Measurement Conditions Table for Flame Atomic Absorption Analysis ................................ 7-2
7.2 Analysis Line Wavelength Table for Flame Emission Analysis.............................................. 7-5
7.3 Graphite Tube Type Selection in Furnace Method ................................................................ 7-6
7.3.1 When Using a High Density Graphite Tube ............................................................... 7-6
7.3.2 When Using a Pyrolitic Coating Graphite Tube.......................................................... 7-7
7.3.3 When Using the Platform Type Tube ......................................................................... 7-7
7.4 Error Messages.................................................................................................................... 7-10

xxxii
xxx AA-6800/6650 Instruction
Chapter 1
Overview

CONTENTS

1.1 Overview of AA-6800/6650............................................................................................................ 1-2


1.2 Specifications................................................................................................................................. 1-3

AA-6800/6650 Instruction 1-1


Chapter 1 Overview
1.1 Overview of AA-6800/6650

The Atomic Absorption Spectrophotometer AA-6800/6650 incorporates two background correction functions,
the D2 method (Deuterium Lamp method) and the SR method (Self-Reversal method), enabling selection of the
appropriate method for the measurement sample.
The AA-6800 allows you to change the measurement mode while automatically switching the atomizer, thus
enabling quick and easy switching back and forth between flame measurement and furnace measurement. In
addition, wide ranging measurement operations are available, from manual operation to automatic continuous
measurement of multi-elements with the use of an autosampler (ASC-6100). This enables selection of the
appropriate combination to match the number of elements and samples to be analyzed as well as the skill of the
operator.
The PC software controlling the AA-6800/6650 operates on the MS-WindowsTM, and using the Wizard for
parameter setting enables an operator, even an beginner of atomic absorption spectrophotometer, to make
measurement conditions easily.

1-2 AA-6800/6650 Instruction


1.2 Specifications
1.2 Specifications

AA-6800F/6800G Common Specifications

Measurement Wavelength 190 - 900 nm


photometer

Range
Spectro-

Mounting Aberration-corrected Czerny-Turner mount

Bandwidth 0.1, 0.2, 0.5, 1.0, 2.0, 5.0 nm (6-step automatic switching)

Number of Lamp Sockets 8 lamp sockets, 2 lamps simultaneously lit (1 for warming up)
Photometric Method • High-speed self reversal method (BGC-SR)
Lamp

• High-speed 2-frequency simultanous measurement (BGC-D2)

Lamp Mode EMISSION, NON-BGC, BGC-SR, BGC-D2, D2

Software Environment WindowsTM95, WindowsTM98, WindowsTMNT4.0, Windows 2000,


Parameter Setting Windows XP
Wizard Method
Measurement Mode Flame continuous method, Furnace method

Concentration Conversion • Calibration curve (selectable among 1st, 2nd, 3rd order
Mode function)
Repeat Measurement • Standard addition method/Simple standard addition method
(1st order function)
• Max. 20 repetitions
• Indication of Average, Standard Deviation (SD) and Relative
Standard Deviation (RSD)
Data Processing

• Exclusion of deviant value based on SD value and RSD value


Baseline Correction Automatic baseline drift correction using electrical double beam
signal processing (furnace)

Sensitivity Correction Automatic calibration curve correction system by sensitivity


observation
Table Data Processing Actual concentration calculation using weight factor, dilution factor,
Functions volume factor and correction factor
Multitask Word processor software or the like can be used while executing
measurement.
Loading Parameters Template function

Procedure/Result Display MRT worksheet (MRT: Measurement Result Table)

Result Print Summary report

QA/QC Correlation factor, LCS, SPK, sample upper limit, %RSD

Power Requirements 100, 120, 220, 230, 240 VAC switching incorporated, 600 VA, 50/
60 Hz
Additional power for personal computer is necessary.
Dimensions, Weight W1080 s D550 s H460 mm, 100 kg (including gas controller, not
including PC)

Ambient Temperature Range 10 oC - 35 oC

Ambient Humidity Range 45 % - 80 % (less than 70 % if temperature is over 30 oC)

AA-6800/6650 Instruction 1-3


Chapter 1 Overview

AA-6800F Specifications

Type Air-cooled pre-mix type

Burner Head Pure titanium


Burner Unit

Nebulizer Pt-Ir capillary with PTFE orifice,


Impact bead is inseparable. Fluoric acid is usable.

Chamber Polypropylene

Positioning Burner/Furnace automatic switching by motor drive


Automatic searching for optimum burner height

Flow Rate/Pressure Control Automatic flow rate setting


Automatic searching for optimum gas flow rate

Safety Measures • Automatic gas leak check


• Air-C2H2 flame priority ignition
Gas Controller

• Air/N2O auto switching with C2H2 flow rate monitor (optical


sensor)
• Prevents raw gas discharge
• Prevents usage of wrong burner head
• Pressure monitor to prevent flashback at abnormal pressure
• Safety extinction by automatic detection of momentary power
failure
• Drain tank water level monitor to prevent flashback

* Throughout this manual, polytetrafluorethylene is abbreviated to PTFE.

AA-6800G Specifications

Heating Temperature Range Ambient to 3000 qC

Heating Control Method • Drying: Current control method


• Ashing/Atomizing: Optical temperature control method

Heating Parameter Settings • Max. 20 stages


• Heating mode: RAMP/STEP
• Inner gas type: 2-line switching
• High sensitivity setting
• Furnace concentration boost cycle: Max 20 times
• Inner gas flow rate: 0 - 1.5 L/min
• Optimum furnace program search function

1-4 AA-6800/6650 Instruction


1.2 Specifications

AA-6650F/6650G Common Specifications

Measurement Wavelength 190 - 900 nm


photometer

Range
Spectro-

Mounting Aberration-corrected Czerny-Turner mount

Bandwidth 0.1, 0.2, 0.5, 1.0, 2.0, 5.0 nm (6-step automatic switching)

Number of Lamp Sockets 8 lamp sockets, 2 lamps simultaneously lit (1 for warming up)
Photometric Method • High-speed self reversal method (BGC-SR)
Lamp

• High-speed 2-frequency simultanous measurement (BGC-D2)

Lamp Mode EMISSION, NON-BGC, BGC-SR, BGC-D2, D2

Software Environment WindowsTM95, WindowsTM98, WindowsTMNT4.0


Parameter Setting Wizard Method

Measurement Mode Flame continuous method, Furnace method

Concentration Conversion • Calibration curve (selectable among 1st, 2nd, 3rd order
Mode function)
Repeat Measurement • Standard addition method/Simple standard addition method
(1st order function)
• Max. 20 repetitions
• Indication of Average, Standard Deviation (SD) and Relative
Standard Deviation (RSD)
Data Processing

• Exclusion of deviant value based on SD value and RSD value

Baseline Correction Automatic baseline drift correction using electrical double beam
signal processing (Furnace)

Sensitivity Correction Automatic calibration curve correction system by sensitivity


observation

Table Data Processing Actual concentration calculation using weight factor, dilution factor,
Functions volume factor and correction factor
Multitask Word processor software or the like can be used while executing
measurement.

Loading Parameters Template function

Procedure/Result Display MRT worksheet (MRT: Measurement Result Table)

Result Print Summary report

QA/QC Correlation factor, LCS, SPK, sample upper limit, %RSD

Power Requirements 100, 120, 220, 230, 240 VAC switching incorporated, 600 VA, 50/
60 Hz
Additional power for personal computer is necessary.

Dimensions, Weight W1080 u D550 u H460 mm, 100 kg (including gas controller, not
including PC)

Ambient Temperature Range 10 qC - 35 qC

Ambient Humidity Range 45 % - 80 % (less than 70 % if temperature is over 30 qC)

AA-6800/6650 Instruction 1-5


Chapter 1 Overview

AA-6650F Specifications

Type Air-cooled pre-mix type

Burner Head Pure titanium


Burner Unit

Nebulizer Pt-Ir capillary with PTFE orifice,


Impact bead is inseparable. Fluoric acid is usable.

Chamber Polypropylene

Positioning Manual positioning by adjusting knob

Flow Rate/Pressure Control Automatic flow rate setting

Safety Measures • Automatic gas leak check


• Air-C2H2 flame priority ignition
• Air/N2O auto switching with C2H2 flow rate monitor (optical
Gas Controller

sensor)
• Prevents raw gas discharge
• Prevents usage of wrong burner head
• Pressure monitor to prevent flashback at abnormal pressure
• Safety extinction by automatic detection of momentary power
failure
• Drain tank water level monitor to prevent flashback

AA-6650G Specifications

Heating Temperature Range Ambient to 3000 qC


Heating Control Method • Drying: Current control method
• Ashing/Atomizing: Optical temperature control method

Heating Parameter Settings • Max. 20 stages


• Heating mode: RAMP/STEP
• Inner gas type: 2-line switching
• High sensitivity setting
• Furnace concentration boost cycle: Max 20 times
• Inner gas flow rate: 0 - 1.5 L/min
• Optimum furnace program search function

1-6 AA-6800/6650 Instruction


Chapter 2
Installation

CONTENTS

2.1 Parts Inspection ............................................................................................................................. 2-2


2.2 Instrument Placement and Site Requirements .............................................................................. 2-6
2.3 Equipment Requirements .............................................................................................................. 2-8
2.4 Assembling the AA-6800/6650 .................................................................................................... 2-17
2.5 Mounting a Hollow Cathode Lamp............................................................................................... 2-25
2.6 Installing the ACF-6800 ............................................................................................................... 2-26

AA-6800/6650 Instruction 2-1


Chapter 2 Installation
2.1 Parts Inspection

CAUTION
Since this instrument is installed and adjusted by Shimadzu service engineer, stay and check it together.
Read and strictly observe sections 2.2 and 2.3 to maintain the instrument stability, to obtain the high
reliability of analysis result and to use this instrument for a long time.

After unpacking, verify that the following parts are included in your shipment.
The standard AA-6800/6650 system configurations are as designated below.

System Standard Accessories Standard Accessories for Flame

AA-6800F (206-50500)

AA-6800G (206-50700) −

AA-6650F (206-51200)

AA-6650G (206-51300) −

Check the standard accessories referring to the above table.


If any parts are missing or damaged, please contact your Shimadzu Representative.

Table 2.1 Standard Accessories (AA-6800/6650)

Q'ty
Item No. Parts Name Part No.
6800 6650

1 Spectrophotometer Main Unit 1 1

2 Standard Accessories 1 1

-1 Vinyl Cover 1 1 206-64902

-2 Fuse, 313.250 (for HCL) 2 2 072-01664-11

-3 Fuse, 189100 (for D2) 2 2 072-01667-12

-4 AC Cable (for 100 V, 120 V) 1 1 206-13774


or
Cord Set (for 220-240 V) 071-60814-05

-5 Fuse, ULCS-61ML-6 (for 100 V, 120 V) 2 2 072-01661-24


or
Fuse 313.003 (for 220-240 V) 072-01664-30

-6 CD-ROM㧘WizAArd 1 1 206-58458-91

-7 Element Label Sheet, HCL 1 1 200-63653

-8 Instruction Manual 1 1 206-94425

-9 Drive Unit Cover 1 0 206-82031

-10 Cable RS-232C, 9.25 1 1 200-79144-01

2-2 AA-6800/6650 Instruction


2.1 Parts Inspection

NOTE
The hollow cathode lamps, high temperature burner head, pressure regulator and compressor are not
included among the standard accessories.

<2-4> <2-7>
<2-1>

<2-5> <2-3> <2-2>

<2-9>
<2-6>
<2-10>

Figure 2.1 Standard Accessories (AA)

NOTE
1. The instruction manual is not shown in the above figure.
2. In the case of AA-6650 series, the drive cover unit <2-9> in the above figure, is not provided.

AA-6800/6650 Instruction 2-3


Chapter 2 Installation

Table 2.2 Standard Accessories (for Flame)

Item No. Part Name Q'ty Part No.


1 Standard Accessories for flame 1 206-64844-91
-1 Hose Assy (for gas supply; AIR) 1 (5 m) 206-50389-91
-2 Hose Assy (for gas supply; C2H2) 1 (5 m) 206-50389-92
-3 Cleaning Wire (for cleaning capillary) 1 201-79229-01
-4 Tube (PTFE tube for sample suction) 5 204-05899-01
-5 Burner Position Adjustment Tool 1 202-38757-02
-6 Seal Joint Assy (for gas leak check) 1 206-52826-91
-7 Driver, #2 (Phillips "+") 1 086-11002
-8 Sample Stage 1 206-63686
-9 Grease in Cup 1 206-50442-91
-10 Wire Band, 16 mm (hose band) 2 037-61019
-11 Polyethylene Tube, No. 3 1 (0.3 m) 200-31328-01
-12 Gas Tube Assy (3 bundled nylon tube) 1 206-65112
-13 Silicone Rubber Tube, 9 u 12 (drain tube) 1 (2.4 m) 016-31350-22
-14 Vinyl Tube, R3603 3/8 u 1/16 (drain tube) 1 (2.4 m) 016-31409
-15 Drain Assy 1 206-80771-91
-16 Screw, SUS P3 BK M3 u 6 2 020-46534
-17 Wiring Band RF100 2 072-60315-01
-18 Sampling Tube ASSY 1 206-50772-91
-19 HEX wrench 3.0 1 086-03804

2-4 AA-6800/6650 Instruction


2.1 Parts Inspection

<1-6> <1-17>
<1-5>
<1-4> <1-7>

<1-8>
<1-9>
<1-10> <1-15>

<1-19>

<1-1>
<1-2>

<1-3>

<1-16> <1-14>
<1-11, 18> <1-12> <1-13>

Figure 2.2 Standard Accessories (For Flame)

AA-6800/6650 Instruction 2-5


Chapter 2 Installation
2.2 Instrument Placement and Site Requirements

The instrument components are positioned as shown in Figure 2.3.


In addition to this, the installation site for personal computer and printer is necessary.
(1) The installation site should be:
a. Sufficiently distant from devices that generate strong magnetic and electrical fields and high frequency
b. Sufficiently ventilated
c. Free from vibration
d. Free from excessive dust and moisture and should not be exposed to corrosive gases
e. The luminous intensity of installation site for this instrument should be below 1300 Lx in the case of
fluorescent lamp, below 800 Lx in the case of indirect outdoor daylight, and below 400 Lx in the case
of heat light source like incandescent lamp.

CAUTION
The AA-6800/6650 series are equipped with the safety system using an optical sensor. When installing the
instrument near a window, make sure that it is not exposed to strong outdoor daylight. Exposure to strong
outdoor daylight may interfere with normal operation of the extinguished flame safety system for monitoring
flame combustion (Flame Monitor). When using incandescent lamp or other heat light sources near the main
unit, select the installation site where the luminous intensity by the light source only is below 400 Lx. If not
available, don't allow the direct light from the light source to come into the combustion chamber.

f. Ambient temperature range: 10 to 35 qC


Humidity: 45 to 80 % (but less than 70 % if temperature is over 30 qC)
g. Ground is available.

NOTE
Absorbance varies 0.005Abs as the temperature changes 1 qC. When measuring many samples which
requires long time and may result in temperature change influence, execute AUTO ZERO during the
measurement if necessary. In the case of manual flame measurement (not using ASC), you can execute
AUTO ZERO at any time by clicking on the [AUTO ZERO] button on the left lower of the main window. In the
case of automatic flame measurement (using ASC), set AUTO ZERO in [Action] field on the MRT work
sheet. AUTO ZERO is executed during the nozzle rinsing. In the case of furnace measurement, setting is not
necessary because the instrument automatically execute AUTO ZERO just before measurement.

(2) The installation platform (table or counter top) must be capable of supporting the combined weights of the
components listed below and a personal computer system.

AA-6800/6650 100 kg

GFA-EX7 41 kg

ASC-6100 15 kg

(3) Since gas and water pipes and cables are connected at the back of the AA main unit, there must be a
space of about 15 to 20 cm from the back of the AA main unit to a wall.
(4) There must be a space of about 15 to 20 cm between the personal computer and the AA main unit so that
the pressure and flow rate adjusting knobs on the left side of the AA main unit can be operated.

2-6 AA-6800/6650 Instruction


2.2 Instrument Placement and Site Requirements

Front view

Duct

About 700

Plane view

(Unit: mm)

Figure 2.3 Instrument Placement

AA-6800/6650 Instruction 2-7


Chapter 2 Installation
2.3 Equipment Requirements

2.3.1 Power Requirements


The following table gives the power requirements for each of the components (The power requirement for a
personal computer system is not shown in the table).
Table 2.3 Power Requirements

AA-6800/6650

Voltage 100, 120, 220, 230, 240 V

Allowable voltage range Within r 10 % (Free from sudden voltage change)

Power capacity 600 VA

Source frequency 50/60 Hz

Connections Grounded outlet

• When the power voltage of AA-6800/6650 changes 5 %, absorbance changes approx. 0.005 Abs.

2.3.2 Water Supply Requirements


Use of the GFA (special accessory) requires piped water for cooling the graphite furnace. The following
requirements must be satisfied:
(1) A water outlet and return water drain must be located within 7 m of the instrument.
(2) Water pressure of 0.07 MPa is necessary. If the water pressure decreases below 0.05 MPa, a safety
device will activate to stop the operation. The upper limit of water pressure is about 0.1 MPa. If the water
pressure in your arrangement is too high, prepare the pressure reducing valve (special accessory,
Regulator ASSY P/N 206-86147-91) additionally.
(3) Water consumption under these conditions is approximately 1 L/min.

2.3.3 Gas Requirements


(1) Gas Specifications
Be sure that gases are supplied for flame analysis according to the specifications given in Table 2.4.
Table 2.4 Gas Specifications

Supply pressure Max. consumption Purity

Air 0.35 MPa 24 L/min Free from oil, moisture and dust

Nitrous oxide 0.35 15 Purity t 98 %, moisture d 1 %

Argon 0.35 24 Purity t 99 %

Acetylene 0.09 4.9 (Air-C2H2 flame) Purity t 98 %

9.9 (N2O-C2H2 flame)

Hydrogen 0.09 30 Purity t 99 %

WARNING
Use only gases in Table 2.4 for flame analyses.
Do not use oxygen gas.

2-8 AA-6800/6650 Instruction


2.3 Equipment Requirements

CAUTION
If the gas supply pressure changes during the analysis, resultant changes in flame combustion will adversely
affect measurement reproducibility. Ensure that gas pressure does not fluctuate.

When the GFA is used, provide gases with the specifications shown in Table 2.5.

Table 2.5 GFA Gas Specifications

Supply pressure Max. consumption Purity

Argon 0.35 MPa 3.0 L/min t 99.9 %

Oxygen/Air 0.35 MPa 1.5 L/min Free from oil, moisture and dust

Oxygen or air is effective in accelerating the ashing of organic samples. Prepare piping if necessary.
(2) Placement of gas cylinders
For safety, it is recommended that the cylinders be placed outdoors. Select a location for the cylinders
which satisfies the following conditions:
a. Not exposed to heat sources such as direct sunlight, furnaces, and heaters: Always keep the cylinders
at a temperature below 40 qC
b. Away from spark sources such as switchboards, ground wires, and high voltage power sources
c. Away from flammable materials such as oil, gasoline, and organic solvents
d. Sufficiently ventilated
e. If outdoors, not exposed to wind and rain
(3) Gas piping
If the cylinders are placed outdoors, piping must be performed separately within 5 m of the instrument. In
this case, be sure to follow the precautionary measures listed below.
a. Use stainless steel pipes for the piping. Do not use pipes that contain over 62 % copper for acetylene
piping.
b. Ensure that the pipe diameters are not too small to supply gas at the pressures indicated in Table 2.4.
A pipe diameter of at least 7 mm will be sufficient.
c. Place a drain separator in the air piping system at the location indicated in Figure 2.4. If a sufficiently
dry air supply source is used, a drain separator is unnecessary.
d. Figure 2.4 displays examples of recommended piping configurations.
e. Provide a hose nipple with an outside diameter of 8.4 to 8.9 mm so that the provided gas supply hose
(inside diameter 7.9 mm) can be connected to the end of the gas piping.

AA-6800/6650 Instruction 2-9


Chapter 2 Installation

Stop cock

Stainless steel piping


Stop cock
(inside dia. 7 mm)
Full scale 0.2 MPa
0.09 MPa

Full scale 0.2 MPa


0.09 MPa
Acetylene
gas
Hydrogen
gas
Full scale 0.5 MPa
0.35 MPa

Full scale 0.5 MPa Nitrous


0.35 MPa oxide
gas Argon gas

Full scale 0.5 MPa


0.35 MPa

Analysis room
Out- Drain
doors separator Air
compressor

Figure 2.4 Recommended Piping Setups for AA-6800/6650

2.3.4 Ventilation System


Place a ventilation duct with a hood above the atomizer.
(1) The hood, duct and ventilation fans used should be all made of metal. Those made of plastic are
inappropriate as they are softened by heat.
(2) A cooling-fan air capacity of about 600 to 1200 m3/h is appropriate. Too much suction force will cause the
flame to flicker as well as create excessive noise. Placement of a damper in the duct system is ideal for
setting the optimum air flow.

Damper
Fan

About 700

(Unit: mm)

Figure 2.5 Typical Ventilation System

2-10 AA-6800/6650 Instruction


2.3 Equipment Requirements

2.3.5 Use of an Air Compressor


The air compressor described in this section may not be available in all countries. Use of another brand of air
compressor is acceptable providing that it supplies air which is free of oil, water and dust at the pressures
indicated below. In addition, the air compressor should be equipped with the necessary safety devices and
meet the standards required by the local regulations. The following procedure is used for confirming the
operation status of the air compressor shown in Figure 2.6.
(1) Confirm that the oil level is between the red lines on the oil gauge <5>.
(2) Shut the stop cock <10> and drain cocks <6>, <7>, turn the secondary pressure control handle <1>
sufficiently counterclockwise, and then connect the compressor to the power source.
(3) When the primary pressure reaches 0.5 MPa, the motor will stop. Take out the safety valve <3> by hand
and confirm that it is working properly. (There will be a loud hissing sound at this time, but there is no
danger.)
(4) When the primary pressure reaches 0.4 MPa, the motor will start.
(5) After the primary pressure reaches 0.5 MPa again, turn the secondary pressure control handle <1>
clockwise and set the secondary pressure to 0.35 MPa. The compressor is normally used in this state.
(6) Apply soapy water or another leak detector to the connecting parts of the pressure gauges, air transformer,
etc. to check for leaks.

<4> <3>

<10> <1> <2>

<9>

<8>
<11>

<7>

<5> <6>

1 Secondary pressure control handle 7 Drain cock

2 Primary pressure gauge 8 Air transformer

3 Safety valve (not visible in photo) 9 Air output port

4 Lubrication hole 10 Stop cock

5 Oil gauge 11 Secondary pressure gauge

6 Drain cock

Figure 2.6 Air Compressor (Optional Accessory)

AA-6800/6650 Instruction 2-11


Chapter 2 Installation

CAUTION
1. If the compressor does not work using the above procedure, refer to the instruction manual provided
with the compressor.
2. In order to set the secondary pressure correctly, the secondary pressure must always be lowered to
nearly 0 Pa before turning the control handle <1>.
3. During use, make sure that the oil level always stays between the red lines on the oil gauge.
4. After use, always open the drain cocks and discharge the water and oil inside the tank and the
transformer.
5. If a hand compressor or compressed air pipe is to be used to supply air, verify the following:
a. That air is supplied at a pressure of 0.35 to 0.4 MPa
b. That the pressure does not fluctuate
c. That the air supplied does not contain water, oil, or dust

2.3.6 General Precautions for Handling Gas Cylinders


Handle the cylinders carefully, observing the following precautions.
(1) Before installing a pressure regulator on a cylinder, it is always necessary to blow away any dust in the
cylinder outlet.
(2) When opening the cylinder main valve, turn the secondary pressure control handle sufficiently
counterclockwise, and after checking that there is no one standing on the outlet side, gently open the valve
with a cylinder handle.
(3) In the case of nitrous oxide, hydrogen, argon, oxygen, etc., open the cylinder main valve sufficiently. With
acetylene, do not turn the cylinder main valve more than 1.5 turns in order to prevent the acetone or DMF
(dimethylformamide) inside from flowing out.
(4) When using a nitrous oxide-acetylene flame, always open the valve of the acetylene cylinder 1 to 1.5 turns.
If the valve is opened less than this, the acetylene flow rate may be insufficient and cause flashback when
switching from an air-acetylene flame to a nitrous oxide-acetylene flame.
(5) In the case of nitrous oxide, the flow rate may become unstable if the main valve is not opened enough.
Make sure that main valve is opened enough.
(6) Place all the cylinders upright.
(7) Always leave the cylinder handle attached to the main valve even during use.
(8) After use, not only close the stopcock but also always shut the cylinder main valve.
(9) When the source pressure of the acetylene cylinder decreases to 0.5 MPa, replace the cylinder. In the
case of acetylene gas, a porous mass inside the high-pressure container is soaked with acetone or DMF
(dimethylformamide), and the acetylene gas is dissolved in that by compression. If the internal pressure of
the cylinder decreases to less than 0.5 MPa, vapor of acetone or DMF will become mixed in the acetylene
gas, and the gas flow rate will become unstable. If the internal pressure decreases to less than 0.3 MPa,
the acetone or DMF will flow out, and control of the gas flow rate will be impossible.

2-12 AA-6800/6650 Instruction


2.3 Equipment Requirements

2.3.7 Installing Pressure Regulators (Optional) and Checking for Leaks

WARNING
1. If a mistake is made in the piping, it may cause flashback on ignition, so exercise sufficient caution.
2. Always set the gas supply pressures at the specified values.
3. Never use a broken regulator. This may result in an accident.

(1) Wipe any dust adhering to the outlet of the cylinder.


(2) Refer to Figures 2.7 to 2.9 to install these pressure regulators on the cylinders. If the screw for mounting
the regulator on the cylinder appears ready to break, replace the cylinder without attempting to mount the
regulator.
(3) Open the cylinder main valve gently after closing the stopcock and turning the secondary pressure control
handle sufficiently counterclockwise.
(4) Turn the secondary pressure control handle clockwise and set the secondary pressure to the following
values:
Acetylene 0.09 MPa
Hydrogen 0.09 MPa
Nitrous oxide 0.35 MPa
Argon 0.35 MPa
(5) Apply soapy water to each of the connecting joints to check for leaks. Due care should be taken to detect
and eliminate any leaking at the cylinder cock.

AA-6800/6650 Instruction 2-13


Chapter 2 Installation

Primary pressure gauge


Secondary pressure gauge Cylinder main valve
(Open by turning counter-clockwise;
close by turning clockwise. Use the cylinder by
making 1.5 counter-clockwise turns of the valve.)

Secondary pressure control handle (When turned clockwise, the secondary pressure rises;
when turned counter-clockwise, it decreases. The secondary
pressure is normally set to 0.09 MPa.)

Figure 2.7 Pressure Regulator for Acetylene

Secondary pressure control handle


(When turned clockwise, the secondary pressure rises;
when turned counter-clockwise, it decreases. The secondary pressure is normally set to 0.35 MPa.)

Secondary pressure gauge


Cylinder main valve
(Open by turning counter-clockwise;
close by turning clockwise. Use the cylinder
with the valve almost wide open.)
Stop cock

Connecting nut

Figure 2.8 Pressure Regulator for Nitrous Oxide

Primary pressure gauge


Secondary pressure gauge

Cylinder main valve


(Open by turning counter-clockwise; close by turning clockwise.
Use the cylinder with the valve almost wide open.)
Stop cock

Connecting nut

Flashback prevention
valve

Secondary pressure control handle (When turned clockwise, the secondary pressure rises;
when turned counter-clockwise, it decreases. The secondary
pressure is normally set to 0.09 MPa.)

Figure 2.9 Pressure Regulator for Hydrogen Gas

2-14 AA-6800/6650 Instruction


2.3 Equipment Requirements

2.3.8 Software Operation Minimum Requirements (to be provided by


user)
In order to run the AA-6800/6650 software and control the instrument, the following software and hardware
must be provided.
(1) Personal computer (PC) and peripheral accessories
(2) Operating system
(3) Connection cable
Table 2.6 PC Specifications

Specifications

CPU Pentium 75 or faster (Pentium 200 or faster CPU recommended)

RAM 32MB or larger (64MB or larger RAM recommended)

Screen resolution SVGA (800 s 600 or higher) (1024 s 768 or higher resolution recommended)

Recording device 1 CD-ROM drive (for installing the program)


Hard disk drive (with at least 10MB free disk space for AA software)

I/O port 1 serial port for AA

Peripherals Monitor

Keyboard

Mouse or other pointing device

Printer

Connection Cable
In order to connect the PC and AA-6800/6650, the RS-232C reverse cable (cross cable) is provided as
standard accessory. This cable has a male DSUB 25-pin connector for connecting to the RS-232C connector
(PC) at the rear of the AA main unit, and a female 9-pin DSUB connector for connecting to the serial port
connector on the typical IBM PC/AT and compatible computers. Figure 2.10 shows the wiring diagram of the
standard accessory cable.
If serial connector on your PC is not male 9-pin DSUB, appropriate cable for your PC must be provided by user.
In such case, use Figure 2.10 and Figure 2.11 to obtain an appropriate cable (Figure 2.11 shows the wiring
diagram of the cable which is appropriate for the PC with female 25-pin RS-232C port).

AA-6800/6650 Instruction 2-15


Chapter 2 Installation

AA side PC side
D sub 25-pin D sub 9-pin
male connector female connector

Figure 2.10 RS-232C 9,25 Cable Pin Assignments (P/N200-79144-01)

D sub 25-pin D sub 25-pin


male connector male connector

Figure 2.11 RS-232C Cable Pin Assignments (P/N208-94963-91)

Operating System
The computer must contain the WindowsTM95, WindowsTM98, WindowsTMNT4.0, WindowsTM2000 or
WindowsTMXP Professional software in order to run the AA-6800/6650 software (WindowsTM95,
WindowsTM98, WindowsTMNT4.0, WindowsTM2000 and WindowsTMXP are registered trademarks of Microsoft
Co.).

2-16 AA-6800/6650 Instruction


2.4 Assembling the AA-6800/6650
2.4 Assembling the AA-6800/6650

2.4.1 Connecting the Drain Tube


To prevent gas from leaking through the drain tube, the liquid in the drain tank placed in the drain line must be
maintained at a constant level so that the water pressure may provide proper sealing.
(1) Fasten the drain assy to the lower right on the front of the main unit using the two M3 u 6 screws.
(2) Connect the drain liquid level sensor cable to the connector for drain monitor on the gas control panel
(refer to 3.1.6).
(3) Connect the tube from the chamber to the coupling at the drain tank bottom and fix it firmly with a band.
(4) Connect the provided drain tube to the drain outlet. When analyzing water soluble samples, use vinyl tube
R3603, and for organic solvents, use the silicone rubber tube.
(5) Provide an appropriate container to receive the drained liquid.
(6) Fill water via the breather at the top of the drain tank until the water overflows from the drain tank inside the
gas flow control compartment. If the water level is not high enough, the liquid level sensor will be activated
to prevent ignition.
(7) To ensure that drainage is performed smoothly:
a. The drain tube should hang downward so that there is no crimping of the tube.
b. Leave the end of the drain tube free in the air. If drainage is not performed smoothly, excessive noise
will be produced and reproducibility may be adversely affected.

CAUTION

1. Neither vinyl tube (R3603) nor silicone rubber tube can be used for petroleum solvents.
2. Especially for organic solvent waste, prepare a suitably sized drain container (approx. 10 L) of
appropriately resistant material.
3. Frequently dispose of the drain generating hazardous gases.
4. Do not use a glass-made container since it may be broken.
5. Dispose of waste liquid according to the applicable regulation in your country or region.

Spray chamber

Liquid level sensor


Drain tank

Drain tube

Drain container

Figure 2.12 Connecting the Drain Tube

AA-6800/6650 Instruction 2-17


Chapter 2 Installation

2.4.2 Assembling the Burner

CAUTION
O-rings are placed at the mounting surfaces of the burner head and the nebulizer to prevent gas leakage.
When assembling, always verify that the O-rings are in place.

Refer to Figure 2.13 in assembling the burner.


(1) Pull out the burner head upward. If it is not pulled out easily, turn the burner head while pulling it out.
(2) After confirming that O-ring is properly fitted inside, fit the burner head onto the chamber steadily to the
end.
(3) Loosen the screw at the front of the spray chamber, remove the nebulizer retaining plate and shift the
nebulizer to the front. Confirm that the O-ring is properly fitted to the nebulizer.
(4) Exercising maximum care so as not to damage the capillary, insert the capillary of the nebulizer into the
provided PTFE tube for sample suction (cut off at a right angle).
(5) Insert the nebulizer to the chamber certainly, set the nebulizer retaining plate with the screw.
(6) Mount the sample stage in the front of the burner compartment.
(7) In the case of AA-6800 series, place the drive unit cover onto the lower part of the burner compartment. At
this time, set it so that the strut of the drive unit may fit in the notch of the drive unit cover and that the hole
on the burner compartment floor may be covered. This is to prevent foreign substances from entering
through the hole.

NOTE
1. If it is difficult to fit the PTFE tube onto the capillary, warm up the end of the tube to enlarge the opening.
Since the capillary is very thin and fragile, be careful that it does not break.
2. A polyethylene tube covers the capillary to ensure a snug fit between the PTFE tube and the capillary
(refer to Figure 6.4 in section 6.2.2).
3. Insert the nebulizer steadily. If unsteadily, sensitivity gets down.
4. As the impact bead is easily broken, be careful not to hit it.
5. When driving the atomizer unit, remove the drive unit cover.

2-18 AA-6800/6650 Instruction


2.4 Assembling the AA-6800/6650

Burner head

O-ring

Chamber
O-ring

Retaining plate

Nebulizer

Impact bead

Figure 2.13 Assembling the Burner

2.4.3 Cable Connections


Referring to Figure 2.14, connect the AC cable of standard accessory, and connect the RS-232C reverse cable
to the PC. (For details on connecting PC to monitor, keyboard, mouse and printer, refer to the appropriate
documentation.)
Connect the RS-232C reverse cable to the connector labeled "PC" on the rear of the AA, and to the serial port
on the PC. The PC serial port may be called "COM port" or "RS-232C port", depending on the PC model. Refer
to the documentation provided with the PC.
Be sure to check that the AA power switch is OFF before connecting the AC cable.

AA rear side

PC RS-232C
(PC)
RS-232C
cable

SERIAL1
SERIAL2
COM1
COM2
RS-232C
etc. AC cable AC
(called by various name.) ~

Figure 2.14 Cable Connections

CAUTION
Before connecting or disconnecting the ground wire, be sure to remove the AC cable connector from the
power socket.

CAUTION
In the case of 2-wire socket, be sure to ground the earth terminal of AC cable.

AA-6800/6650 Instruction 2-19


Chapter 2 Installation

2.4.4 Hose Connections


Refer to Figure 2.15 in connecting the hose.

Right rear of main unit

To acetylene or hydrogen gas cylinder


Red Quick-connect
To compressor, air or argon gas cylinder hose joints
Black
To nitrous oxide gas cylinder
Green

Black

Tube connectors
White

Red

Figure 2.15 Hose Connections

WARNING
DO NOT USE OXYGEN GAS.

(1) Hose connections between the compressor/gas cylinders and the connectors at right rear of main unit
a. The hose joints are connected to the rubber hoses as follows:
Black rubber hose o AIR (large) for air
Black rubber hose o SUPPORT (large) for argon
Green rubber hose o N2O (small) for nitrous oxide
Red rubber hose o C2H2 (small) for acetylene
Red rubber hose o FUEL (small) for hydrogen gas
b. Connect one end of the rubber hoses to the compressor or gas cylinders and secure firmly with the
hose bands.
c. Connect the other end (with hose joint) of the rubber hose to the specified gas inlet at the rear of main
unit. The gas inlet port is provided with cap nut and sleeve. First, pass the cap nut and sleeve through
the hose joint. Next, insert the hose joint into the gas inlet port deeply to the bottom, and tighten the
cap nut by hand. Finally, tighten the screw firmly using spanners.

2-20 AA-6800/6650 Instruction


2.4 Assembling the AA-6800/6650

(2) Connections between burner unit and connectors at right rear of main unit
a. Connect one end of the provided gas tubes (bundle of 3 nylon tubes) to the tube connectors on the
rear of the main unit as follows:
White tube o SPRAY
Black tube o AUX
Red tube o FUEL
Push each tube onto the above tube connector to the end and tighten the cap nut firmly by hand.
b. Connect the other end of the tubes to the provided seal joint, then check for gas leaks according to
section 6.3.
c. After checking for gas leaks, detach the tubes from the seal joint. Then reconnect them to the
specified gas inlet.

2.4.5 Replacing the AA-6650 Atomizer


The AA-6650F and AA-6650G are the instruments designed for flame and furnace analyses, respectively.
However, if the graphite furnace atomizer GFA and the base for furnace are prepared, the AA-6650F can be
used also for furnace analysis.

Part Name P/N

Graphite furnace atomizer GFA 206-51000-93 (220 V), -34 (230 V), -35 (240 V)

Base for furnace 206-51141

Also, if the flame conversion unit ACF-6800 and the cover for flame are prepared, the AA-6650G can be used
for the flame analysis.

Part Name P/N

Flame conversion unit ACF-6800 206-64843-92

Cover for flame 206-50554

Replacing the burner with the graphite furnace


The procedure for mounting the graphite furnace instead of the burner is described here.
(1) Remove the flame shield.
(2) Lift up the burner head and remove it from the chamber.
(3) Remove the four screws fixing the cover for flame and remove the cover for flame (refer to Figure 2.16,
upper).
(4) Using the four screws removed at the step (3), mount the base for furnace instead of the cover for flame
(refer to Figure 2.16, lower).
(5) When mounting the graphite furnace, it is necessary to adjust the furnace position so that the optical axis
and graphite furnace may have the optimum positional relation. Refer to section 6.1.2.2 for mounting the
graphite furnace and adjusting the furnace position.
(6) After mounting the graphite furnace, check that the plumbing tubes are not bent and that no excessive
force is given to the furnace heating cable.

AA-6800/6650 Instruction 2-21


Chapter 2 Installation

Replacing the graphite furnace with the burner


The procedure for mounting the burner instead of the graphite furnace is described here. Refer to section
6.1.1.2 for adjusting the burner position.
(1) Remove the four screws fixing the base for furnace, and remove the base for furnace while keeping the
graphite furnace mounted on it.
(2) Using the four screws removed in the step (1), mount the cover for flame instead of the base for furnace.
(3) Fit the burner head in the chamber firmly.
(4) Mount the flame shield.
(5) Check the gas plumbing before use.

Graphite furnace

Two screws M3 u 8 (inner)

Base for furnace


Four screws

When using the Graphite Furnace

Burner head

Cover for flame

Four screws

When using the Burner

Figure 2.16 Replacing the Atomizer Unit

2-22 AA-6800/6650 Instruction


2.4 Assembling the AA-6800/6650

2.4.6 Installation of PC Software


This procedure assumes that Windows is already installed on the PC. For its installation, refer to the
appropriate documentation.
(1) Start up Windows. In case of installing to the Windows XP, Windows 2000 or Windows NT4.0, logon to
Windows by Administrator authority.
(2) Insert CD-ROM for CD drive. Execute “\eng\setup.exe” of CD drive by using Windows explorer.
(3) First, a note for installation is displayed. Read it and click on <Next> to go ahead.
(4) Select AA-6800 or AA-6650 as main unit type that you use. Click on <Next> to go ahead.
(5) Select GFA-EX7 or GFA-6500 as GFA type that you use. Click on <Next> to go ahead.
(6) Check the installation destination folder. You may change the folder here, if desired. Click on <Next> to go
ahead.
(7) Select the program folder. Click on <Next> to start setup.
(8) Finally, when the message shows that the setup is completed, click on <Finish>.
When the [Yes, I want to read README.TXT] check box is check-marked, the README.TXT is displayed
by the Notepad. Be sure to read this, since the important information about AA software operation is
described in the README.TXT. Exit the Notepad, then installation procedure is finished.

NOTE

1. Set all the electric power-saving functions to OFF both in the BIOS setup of PC and in the control panel
of Windows. Otherwise, the electric power-saving function may cause a trouble in communication
between the AA main unit and the PC.
How to display the BIOS setup screen is different depending on the PC model. Refer to the instruction
manual provided with the PC.
2. When upgrading the WizAArd ver. 1.xx to ver. 2.xx
Don't delete "wizaa.ini" file in the Windows directory when uninstalling the WizAArd ver. 1.xx. Upgrading
to ver. 2.xx is performed more smoothly when the "wizaa.ini" file of WizAArd ver. 1.xx remains. Also, It
is highly recommended for you to back up "wizaa.ini" file before uninstalling the older version WizAArd.
3. When upgrading the WizAArd ver. 2.1x to ver. 2.20
Don't uninstall the WizAArd ver. 2.1x when it is already installed.
If the WizAArd ver. 2.1x is uninstalled, "wizaa.ini." file and lamp history data (lamphist.ref file) are
deleted and, as the result, various parameters and its lamp use time are reset. For upgrading, execute
the setup disk of ver. 2.20 and install it to overwrite "ver. 2.1x" on the folder in which the old version
software has been installed.
To keep ver. 2.1x, install ver. 2.20 in another folder. At this time, to transfer the lamp history data from
ver. 2.1x, copy the "lamphist.ref" file of ver. 2.1x to the folder in which ver. 2.20 has been installed.

AA-6800/6650 Instruction 2-23


Chapter 2 Installation

NOTE

4. When using the atomic muffle and performing the version-up of WizAArd
If your instrument type is not available for flame measurement (AA-6650G/6800G) and equipped with
the atomic muffle SARF-16C, performing the PC software version-up to WizAArd ver. 2.11 or later
may make the operation complicated, because an unnecessary checklist screen for starting a flame
measurement appears at every time of initialization.
To avoid this problem, remove the short plug inside the instrument. For details on the short plug, refer
to the instruction manual for adapter set for mounting the atomic muffle.

2-24 AA-6800/6650 Instruction


2.5 Mounting a Hollow Cathode Lamp
2.5 Mounting a Hollow Cathode Lamp

(1) Open the cover on the left side of the main unit.
(2) Remove the lamp socket from the turret peg (socket holder).
(3) Insert the hollow cathode lamp in the turret.
(4) Plug the lamp socket into the lamp.
(5) Put the provided HCL name sticker (sticker with element name) at an easy-to read location of the lamp.

AA-6800/6650 Instruction 2-25


Chapter 2 Installation
2.6 Installing the ACF-6800

Since various operations, such as removing the cover, connecting cables and plumbing gas tubes, etc., are
required when adding the ACF-6800 flame unit to the furnace-dedicated AA-6800G/6650G, be sure to have a
service representative from the nearest branch agent or office perform the installation.

2-26 AA-6800/6650 Instruction


Chapter 3
Instrument Constructions

CONTENTS

3.1 AA-6800/6650 Configurations........................................................................................................ 3-2

AA-6800/6650 Instruction 3-1


Chapter 3 Instrument Constructions
3.1 AA-6800/6650 Configurations

3.1.1 Operation Switches


<2>

<1>
<4> <3>

Figure 3.1 AA-6800/6650 Main Unit

No. (in Figure 3.1) Name Function

1 POWER switch Turns ON the instrument.

2 BURNER SELECT This key switch is for preventing mistaken use of burner heads.
switch When the high temperature burner head (optional) is to be used
with the nitrous oxide-acetylene flame, a key attached to the
burner head is used to change to the N2O-C2H2 position. If not
in this position, the nitrous oxide flame cannot be ignited. The
Air-C2H2 position would normally be used for an air-acetylene
flame or an argon (air)-hydrogen flame, but the N2O-C2H2
position can also be used.

3 EXTINGUISH Pressing this button extinguish the flame.


button

4 IGNITE buttons When these two buttons are pressed at the same time, gas is
fed to the burner and is ignited by the pilot flame.

3-2 AA-6800/6650 Instruction


3.1 AA-6800/6650 Configurations

3.1.2 Hollow Cathode Lamp Turret


Eight lamps may be installed, two of which may be on at one time. For routine analysis in which the analysis
elements are known, it is convenient if all the lamps to be used in measurement (up to eight) are installed in the
turret and the lamp current values, lamp numbers (socket numbers) along with the other measurement
parameters are stored beforehand in the instrument memory. This then allows the required lamp to be
automatically set in the optical path by just loading the stored parameters.

CAUTION
1. When installing a lamp, after inserting the lamp in the hole in the turret, insert the socket having the
same number as the turret hole onto the lamp pins. Make sure that the socket is fully seated; if it is not,
there is a danger from exposed pins carrying high voltage loads. Also, when removing the socket, make
sure that this operation is performed only after the lamp current reads 0 mA or OFF.
2. Mount unused sockets on the turret pegs near the turret holes.

Socket Boss

Figure 3.2 Hollow Cathode Lamp Turret

AA-6800/6650 Instruction 3-3


Chapter 3 Instrument Constructions

3.1.3 Deuterium Lamp


The deuterium lamp is of the hot cathode type and is used at the wavelength range of 190 nm - 430 nm in
background correction and measurement. The lamp is plugged in the instrument to allow easy replacement.
The adjusting screw is used to position the new lamp upon replacement.

Deuterium lamp

Adjusting screw

Figure 3.3 Deuterium Lamp

3-4 AA-6800/6650 Instruction


3.1 AA-6800/6650 Configurations

3.1.4 Burner Module


3.1.4.1 AA-6800
The burner drive is performed by PC operation. Therefore, there are no positioning knobs for driving the burner
module.

<4>

<3>

<1>

<2>

Figure 3.4 Burner Module (AA-6800)

No. (in Figure 3.4) Name Function

1 Burner head The types of flames which can be used with the standard
burner head are 3 types, which are air-acetylene flame and air
(argon)-hydrogen flames. Be sure to use the high temperature
burner head (optional) when using a nitrous oxide-acetylene
flame.

2 Burner head angle These allow the angle of burner slot to be adjusted relative to
adjustment lever the light path. Normally, the position at 0 on the scale (slot is
parallel with light path) is used, but when measuring high-
concentration samples, measurements of better linearity
between concentration and absorbance can be obtained by
angling the slot to decrease sensitivity.

3 Flame monitor An optical sensor is built in the instrument for monitoring the
intensity of the light emitted by the flame. If the flame goes out
and the light emission is lost, the solenoid valve in the gas
control unit is closed by a signal from the sensor and the flow of
raw gas is stopped. In addition, when switching between an air-
acetylene flame and nitrous oxide-acetylene flame, an increase
in the acetylene flow rate will be detected by an increase in the
light emission intensity, and the air and nitrous oxide will be
switched.

4 Pilot flame Pressing the IGNITE buttons on the gas controller ignites the
pilot flame.

AA-6800/6650 Instruction 3-5


Chapter 3 Instrument Constructions

3.1.4.2 AA-6650
On the front side of AA-6650 burner module, the knobs for adjusting the horizontal and vertical positions of the
burner (or graphite furnace) are prepared. The atomizer is driven with these knobs.

Vertical mark line

<1>

<2>

Front-back indicating position

<3>
Height indicating position

Enlarged view of the part marked with

Figure 3.5 Burner Module (AA-6650)

No. (in Figure 3.5) Name Function

1 Burner position The scale shows the height of the burner, indicating the height
indicator scale from the light path to the top of the burner head. In addition,
when the front-back indicating position of the burner is at the
vertical mark line, the slot of the burner head is positioned right
beneath the light path. For precise adjustment, refer to 6.1.1.2.

2 Knob for adjusting Turning this knob adjusts the front-back position of the burner.
burner vertical When the knob is turned clockwise, the burner moves forward.
position

3 Knob for adjusting Turning this knob adjusts the burner height. When the knob is
burner horizontal turned clockwise, the burner moves down.
position

3-6 AA-6800/6650 Instruction


3.1 AA-6800/6650 Configurations

3.1.5 Burner
The AA-6800/6650 has a burner head with a 10 cm length slot (standard accessory) mounted in the premixing
atomizer chamber. This burner head can be used with air-acetylene flames and air (argon)-hydrogen flames.
Please specially install a high-temperature head (optional accessory) when using a nitrous oxide-acetylene
flame.

<6>

<1>
<5>

<7>

<7>
<4>

<2>
<8> <3>

Figure 3.6 Burner

No. (in Figure 3.6) Name Function

1 Burner socket Insert the burner head into this port. The burner head is fixed
with the internal O-rings.

2 Nebulizer This uses air negative pressure to suction the sample solution
and spray it from the tip of the capillary as a mist of fine particles.

3 Impact bead This makes the fine particles of sprayed sample solution into
even finer particles, and larger particles are separated out.

4 Nebulizer retaining Fixes the nebulizer to prevent it from coming off.


plate and fixing
screw

5 Spray chamber The particles of sprayed sample solution are mixed with the
combustion gas in this chamber.

6 Mixer Mixing of the particles and combustion gas is promoted.

7 Safety bung and In case of a flashback, this bung is open to prevent the burner
safety plug plate unit from being damaged. In case a flashback should occur and
the safety bung operates, refer to "Inspection Procedure in Case
of Flashback" on the yellow pages. In case that the safety bung
operates, a safety plug plate disappears. In ignition, confirm that
a safety plug plate appears. A flashback means a combustion or
explosion that occurs in the burner when the flame combustion
rate is fast and the mixed gas flow velocity is slow.

8 Drain discharge port Large particles are discharged from this port.

AA-6800/6650 Instruction 3-7


Chapter 3 Instrument Constructions

NOTE
When measuring samples containing high-concentration coexistent material like salts or when measuring
samples with a nitrous-oxide flame, the mixer reduces the signal noises. Therefore, the mixer is usually
mounted in the chamber. When measuring samples with low-concentration coexistent material with air-
acetylene flame, however, removing the mixer may improve the sensitivity. If a high sensitivity is required for
such samples, you can remove the mixer if necessary. Remove the mixer referring to section 6.2.3.

3.1.6 Gas Control Panel

<5>

<2>

<6> <12>

<1>

<8>

<7>

<4> <3>

<10>

Figure 3.7 Gas Control Panel

3-8 AA-6800/6650 Instruction


3.1 AA-6800/6650 Configurations

No. (in Figure 3.7) Name Function

1 Support gas Displays the setting pressure for the support gas.
pressure gauge

2 Support gas flow Flow increases when turned to the left, and decreases when
adjusting knob turned to the right. Usually, use the air or argon at 8 L/min, and
nitrous oxide at 6.5 L/min.

3 Support gas Displays the flow rate for the support gas. Read the flow at the
flowmeter center of the float (ball).

4 Support gas Turning this clockwise increases the pressure, and turning this
pressure adjusting counterclockwise decreases it. This is set at 0.25 MPa before
knob shipping.

5 Fuel gas pressure Displays the setting pressure for the fuel gas.
gauge

6 Fuel gas pressure Adjust the pressure exactly to 0.05 MPa.


adjusting knob

7 BUZZER OFF A buzzer sounds when a gas leak is detected. The buzzer may
button be turned off by pressing this button.

8 PURGE button Pressing this button with the gas cylinder or compressor closed,
the gas remaining inside the tubing is purged.

9 Pilot flame This knob adjusts the flow of gas to the pilot flame. Only a
adjusting knob service engineer is allowed to operate this. Don't touch it.
(located on rear of
unit)

10 BYPASS flow The amount of acetylene increases when switching from an air-
adjusting knob acetylene to nitrous oxide-acetylene flame, and this knob is
used to adjust the amount of increase. At shipment, this is set
for an increase of 5 L/min. Only a service engineer is allowed to
operate this. Don't touch it.

11 Drain tank This prevents raw gas from leaking through the drain tube. With
(located on front of the drain tank placed midway along the tube, the liquid in the
unit) tube is maintained at a constant level to form a water pressure
seal.

12 Drain monitor This monitors the level of the water inside the drain tank. If the
(Only the water level decreases too far, the flame is automatically
connector is shown extinguished. The burner head must be removed and water
in the figure.) added via the breather at the top of the tank to bring up the
level before ignition is possible.

CAUTION
Pressing the PURGE button discharges the mixture of fuel gas and support gas. Since the gas is
inflammable, don't ignite a flame immediately after the PURGE button is pressed.

AA-6800/6650 Instruction 3-9


Chapter 3 Instrument Constructions

3.1.7 Optical System


The light from the hollow cathode lamp and the deuterium lamp is combined with a beam combiner, and while
passing through the atomizer, the atoms and concomitant substances absorb light as signal and background
absorption. The light then passes through the spectrophotometer into the photomultiplier tube. The
spectrophotometer is a high resolution Czerny-Turner type. The wavelength is selected by rotating a diffraction
grating to separate the absorption spectrum of the element being analyzed from the other spectra. The direct
drive mechanism used for wavelength selection is automated with the use of a motor. All of the optical elements
are shielded from the outside air with the quartz window plates and are protected from dust and corrosive
gases.
HCL: Hollow cathode lamp
D2: Deuterium lamp
BS: Beam splitter
W1-W4: Windows
M1-M6: Mirrors
S1, S2: Slits
G: Diffraction grating
PMT: Photomultiplier tube

Figure 3.8 Diagram of Optical System

3-10 AA-6800/6650 Instruction


3.1 AA-6800/6650 Configurations

3.1.8 Photometric System


Figure 3.9 shows the photometric system.

Lamp power
supply

Monochromator
Deuterium lamp
Hollow cathode Analog signal processor
Burner Detector
lamp

Half mirror

CPU

Gas control PC
unit

Figure 3.9 Photometric System

The following five measurement modes can be selected in the AA-6800/6650.


EMISSION mode Used for flame emission analysis.
NON-BGC mode Used for atomic absorption analysis that doesn't require background correction.
BGC-D2 mode Used for atomic absorption analysis that requires background correction.
BGC-SR mode Used for atomic absorption analysis that requires background correction and whose results
are easily affected by nearby spectral lines.
D2 mode Used for background measurement and molecular absorption measurements.

(1) EMISSION mode:


The spectrum produced by atomization of the analysis element in the flame is selected by the
monochromator, and its intensity is measured via photometric circuitry.
(2) NON-BGC mode:
The deuterium lamp is extinguished, and only the light from the hollow cathode lamp, pulsed at 400 Hz, is
passed through the atomizer. Then only the spectral line (analysis line) to be used for analysis by the
monochromator is selected. By measuring the light absorption at this time, it is possible to determine the
concentrations of the elements being analyzed. The detector outputs a signal which is the sum of a 400 Hz
pulsed signal proportional to the analysis line intensity and a direct current signal from the light emitted
from the atomizer (flame or graphite tube).

AA-6800/6650 Instruction 3-11


Chapter 3 Instrument Constructions

(3) BGC-D2 mode:


Pulsed light at 400 Hz from the hollow cathode lamp and light from a 800 Hz pulsed deuterium lamp are
passed through the atomizer simultaneously. The light from the HCL lamp is absorbed both by the atoms
of the element being analyzed and the concomitant elements as background absorption, while light from
the deuterium lamp is absorbed only as background.
In the photometric circuit, after each signal is converted to logarithms, their difference in absorption is
measured. This allows correction for the background concomitant substances and an accurate
measurement of the absorption by the element being analyzed. Characteristically, this mode offers higher
photometric sensitivity than the BGC-SR mode.
(4) BGC-SR mode:
Light from a hollow cathode lamp generated by alternating low current and high current pulses is passed
through the atomizer. The low-current-generated light is absorbed both by the element being analyzed and
the concomitant substances as background absorption, while the high-current-generated light is absorbed
only as background. After both signals are converted to logarithms in the photometric circuit, the difference
between them is calculated in order to correct for the background absorbance due to the concomitant
substances and accurately determine the absorption by the analysis element. This mode is characterized
by the elimination of the effects of nearby lines.
(5) D2 mode:
Light from the hollow cathode lamp is removed from the optical path and only the 800 Hz pulsed light from
the deuterium lamp is passed through the atomizer. This light is absorbed by molecules produced in the
atomizer, and the photometric circuit determines the degree of absorption.

Detector sensitivity adjustment


When the measurement mode is selected in the AA-6800/6650, the detector sensitivity is automatically
adjusted to the optimum condition. In the EMISSION mode, the emission signal is set to a fixed value; in the
NON-BGC mode, the selected hollow cathode lamp signal is set; and in the BGC-D2 mode and the D2 mode,
the deuterium lamp signal is set, while in the BGC-SR mode, the high current hollow cathode lamp signal is set
so that optimum detector sensitivity is obtained for each mode.

3-12 AA-6800/6650 Instruction


Chapter 4
Basic Operation

CONTENTS

4.1 Switching On the Power and Starting Up the Software ................................................................. 4-2
4.2 Software Basic Operation .............................................................................................................. 4-4
4.3 Measurement Procedures ........................................................................................................... 4-36
4.4 Saving/Printing/Deleting the Data................................................................................................ 4-39
4.5 Completing the Measurement...................................................................................................... 4-40
4.6 Explanation of Main Window ....................................................................................................... 4-41
4.7 Operating the MRT Worksheet .................................................................................................... 4-50
4.8 Igniting and Extinguishing the Flame........................................................................................... 4-61
4.9 Standard Addition Method and Simple Standard Addition Method.............................................. 4-67
4.10 Conditions and Operation for Flame Emission Analysis.............................................................. 4-72
4.11 Setting the Optimum Conditions for Fuel Gas Flow Rate and Burner Height (AA-6800) ............ 4-79

AA-6800/6650 Instruction 4-1


Chapter 4 Basic Operation
4.1 Switching On the Power and Starting Up the
Software

4.1.1 Switching ON the Power to Hardware


(1) Verify that installation has been correctly completed.
(2) When using the ASC-6100 or GFA-EX7, set the ASC-6100 power switch (Figure 4.1) or the GFA-EX7
power switch (Figure 4.2, <1>) to the ON position (" " position). At this step, leave the GFA-EX7 heating
switch (Figure 4.2 <2>) lever in the OFF position. Set this heating switch to the ON position when starting
heating.
(3) Set the power switch of AA-6800/6650 main unit (Figure 4.3) to the ON position (" " position). If the fuel
gas is not supplied, a buzzer sounds. Press the "BUZZER OFF" button on the gas controller panel or
supply the fuel gas to stop the buzzer. In addition, after 2 minutes, a buzzer sounds 3 times to indicate that
the initialization of the CPU in AA main unit has been completed.

<1>

No. (in Figure 4.1) Name

1 Power switch

Figure 4.1 Power Switch of ASC-6100

4-2 AA-6800/6650 Instruction


4.1 Switching On the Power and Starting Up the Software

<2>

<1>

No. (in Figure 4.2) Name

1 Power switch

2 Heat switch

Figure 4.2 Power Switch of GFA-EX7

<1>

No. (in Figure 4.3) Name

1 Power switch

Figure 4.3 Power Switch of AA-6800/6650

4.1.2 Starting Up the Software


Switch ON the personal computer to start up the MS-Windows. Double-click on the icon of AA Software. The
[Wizard Selection] dialog box (Figure 4.4) will appear at the center of the screen.

AA-6800/6650 Instruction 4-3


Chapter 4 Basic Operation
4.2 Software Basic Operation

With the AA software, after starting up the software, you can set the necessary settings for the measurement
just by following the instructions sequentially displayed on the screen (Wizard function). In this section, the easy
operation using this Wizard function is described for each of flame and furnace methods in regular sequence.
Refer to Chapter 5 for details of each items.

4.2.1 Software Basic Operation (Flame Method)


4.2.1.1 Operation Flowchart (Flame Method)
This Wizard has a sequence for setting as shown below. You can proceed to the next step or return to the
preceding step by using the [Next] or [Back] button, respectively.

(Starting up the AA Software)


p
(1) Wizard Selection
p
(2) Element Selection
p
(3) Preparation Parameters
p
(4) Sample ID
p
(5) Sample Selection
p
(6) Connect to Instrument/Send Parameters
p
(7) Optics Parameters
p
(8) Atomizer/Gas Flow Rate Setup
p
(Finish)
p
(Start Measurement)

NOTE
When measuring plural elements, you cannot set parameters for the elements other than the current
measurement one on the [Optics Parameters] and [Atomizer/Gas Flow Rate Setup] pages. If you use the
ASC to measure plural elements automatically and you need to modify the parameters for other elements
than the current measurement one, you can change these parameters by using the [Edit Parameters] button
in the [Element Selection] page.

4-4 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.1.2 Wizard Selection

Figure 4.4 [Wizard Selection] Dialog Box

When the [Wizard Selection] dialog box appears, if you make a new parameter set, select the [Element
Selection] icon on the [Wizard] sheet and click on [OK]. Then the [Element Selection] page will appear.

4.2.1.3 Element Selection

Figure 4.5 [Element Selection] Page

AA-6800/6650 Instruction 4-5


Chapter 4 Basic Operation

(1) First, click on [Select Elements]. Then the [Load Parameters] page will appear.

Figure 4.6 [Cookbook] Sheet in [Load Parameters] Page

(2) In this page, select the element first. You can use one of the methods below to select the element.
1. Enter the element symbol directly in the element field from the keyboard.
2. Click on the [ ] button at the right of the element field, and select the element from the element
symbol list shown in alphabetical order.
3. Click on [Periodic Table] button and select the element from the periodic table.
(3) Next, select [Flame] for the measurement method by the radio button.
(4) Select [Normal Lamp] when using a normal hollow cathode lamp ([SR Lamp] is selected only when the SR
method is used as the background correction method).
(5) When using the autosampler, click on [Using ASC] check box.
(6) After completing the settings, click on [OK]. At this time, a message about lamp setup is displayed. Press
the [No] button here. The lamp setup is also possible later. Then the [Element Selection] page is displayed
again and the selected element is shown in the table.
(7) When plural elements are to be analyzed, return to this [Element Selection] page once and then click on
the [Select Elements] button again to select the next element. Repeat the procedure below as required.
Click on the [Select Elements] button o Select an element o Click on the [OK] button.
(8) When returning to the [Element Selection] page after selecting an element, the selected element is added
to the list one by one. If you need to delete any of them, click on the row to highlight it and then click on
[Delete]. [Measurement Element] at the right lower of the page indicates the element to be analyzed first.
(9) For details on the [Edit Parameters] button, refer to section 5.6 in Chapter 5. Here, you can go ahead
without using it.
(10) Click on the [Next] button. Although another message appears, go ahead by clicking on the [Cancel]
button. Then [Preparation Parameters] page will appear.

4-6 AA-6800/6650 Instruction


4.2 Software Basic Operation

NOTE
1. When analyzing plural elements sequentially, the order on the [Element Selection] page becomes the
measurement order. If you need to change the order, click on the element to highlight it and then click
on [Up] or [Down] to move the row. If [Measurement Element] at the right lower of the page is different
from the first row element, the measurement is started from the element shown for [Measurement
Element] and the elements located above this element in the table are not to be measured.
2. When analyzing plural elements sequentially, it is necessary to set the socket numbers in alternating
odd/even. To set or change the socket number, select the [Instrument]-[Lamp Position Setup] from the
menu. For details, refer to section 5.8.4. Also, [Lamp Position Setup] can be opened if you press [Lamp
Pos. Setup] in the [Optics Parameters] page opened by clicking [Yes] in the warning message shown at
the time of element selection.

4.2.1.4 Preparation Parameters

Figure 4.7 [Preparation Parameters] Page

First, select the row of the element to be set by clicking on its row to highlight it, then click on the [Edit] button.
The [Preparation Parameters] page will appear. Set the parameters as below.

AA-6800/6650 Instruction 4-7


Chapter 4 Basic Operation

Figure 4.8 [Edit Preparation Parameters] Page

(1) Select [Calibration Curve] for [Measurement Type]. If you need to select [SMSA] (Simple Standard
Addition Method) or use standard addition method, refer to section 4.9.
(2) Select [1st] for [Order] of equation if the calibration curve is straight. You may also select [2nd] or [3rd] if it
is curved. Anyway, you can change the order after measurement. So, select [1st] here. Loading and saving
of preparation parameter files are not available.
(3) Pressing the [Repeat Conditions] button displays the [Repeat Measurement Conditions] page. The number
of measurements for the same one sample is set here. The default value of the number of measurement
repetitions is "1" in the case of flame measurement.
(4) Select [Conc. Unit] of the prepared standard samples. Click on the [ ] button to select it from the list.
(5) Input [Weight Correction Factors]. These factors are necessary for calculating the actual concentration.
[Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] are used in the following
equation.
Actual concentration = (Conc.) u [Volume Factor] u [Dilution Factor]
u [Correction Factor] / [Weight Factor]
The actual concentration is calculated with the above equation. Note that the unit is not converted
automatically. Convert the unit using [Correction Factor] if necessary (Refer to the example below).
If the above calculation for actual concentration is not necessary, leave all the factors as "1".
Each factor is expressed in MRT worksheet and data print as follows.
[Volume Factor] [VF]
[Dilution Factor] [DF]
[Correction Factor] [CF]
[Weight Factor] [WF]

4-8 AA-6800/6650 Instruction


4.2 Software Basic Operation

(Example)
2 g of sample was weighed, filled with water to 50 ml, diluted to 5 times and measured. In this case, the
actual concentration is calculated with the following equation using the factors; [Weight Factor]: 2 (g),
[Volume Factor]: 50 (mL), [Dilution Factor]: 5 (times) and [Correction Factor]: 1.
Actual conc. = (Conc.) u (50 mL) u (5 times) u 1/(2 g)
Also, if calculating the actual conc. (%) from the conc. (ppm) by converting the unit, use 0.0001 for
[Correction Factor] since 1 ppm is 0.0001 %.
Actual conc. (%) = (Conc. (ppm)) u (50 mL) u (5 times) u 0.0001/(2 g)

NOTE
Generally, "ppm" is the concentration unit of 106. In the atomic absorption analysis, "ppm" indicates both
"Pg/g" for solid samples and "Pg/mL (mg/L)" for liquid samples.

(6) Enter [Number of STD]. Then a table composed of as many rows as the sample number is created in the
[STD Samples] preparation parameters.
(7) Input the actual concentrations of the prepared standards into the table, although the default values from
the cookbook are indicated on the table. When using the ASC, also input the turntable positions (1 to 60,
R1 to R8).
(8) [Blank Samples]
Set up the periodic blank measurement here.
Periodic blank measurement is a function to create a measurement procedure on the MRT to remove the
influence of baseline drift by inserting a blank measurement at a fixed interval. Use it when the sample
number is large or the baseline drift occurs.
• When the [Periodic Blank] is not used
Leave the [Periodic Blank] field [Off].
• When the [Periodic Blank] is used
1. Click on the [Periodic Blank] field and click on the [ ] button at the right of [Off]. Then the list for
[On/Off] is displayed. Select [On].
2. Click on the [Meas. Interval] field and enter the numerical value to insert the blank measurement
in every some samples.
3. [Pos.] indicates the blank position on the ASC turntable. When using the ASC, click on the [ ]
button at the right of [Pos.] and select the position from the list.

NOTE
In the case of flame analysis, the fields for mixing parameters (sample volume, diluent, 1st reagent, etc.) are
not displayed on the dialog box. Loading and saving of preparation parameter files are not available.

(9) After setting the parameters, click on [OK] to return to the [Preparation Parameters] page. In the case of
multi-element analysis, click on the next row to highlight it, then click on [Edit] and set the parameters in the
same way.
(10) When completing all the settings, click on [Next]. Then the [Sample ID] page will appear.

AA-6800/6650 Instruction 4-9


Chapter 4 Basic Operation

4.2.1.5 Sample ID

Figure 4.9 [Sample ID] Page

(1) In this [Sample ID] page, enter the number of samples first. Then enter the sample ID (sample name) into
the cell of [Sample ID] from the keyboard one by one.
(2) When using the same name with successive No. for all the samples, click on [Collective Setup]. Then the
[Sample ID Collective Setup] dialog box will appear.

Figure 4.10 [Sample ID Collective Setup] Dialog Box

Put a check mark in the [Create Sample ID] check box, and enter a common sample name to [Name].
Then names with successive number are automatically created and shown in the table (e.g. Sample001,
Sample002,...). Entering the first sample position in [ASC Start Pos.] sets the sample positions of the
second and after in the table automatically.
Click on [OK] to return to the [Sample ID] page.
(3) You can input and change the name individually after the collective setup.
(4) [Pos.] in the table shows the sample position on ASC turntable. When not using the ASC, this is not
required.
(5) After completing the settings, click on [Next]. Then the [Sample Selection] page will appear.

4-10 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.1.6 Sample Selection

Figure 4.11 [Sample Selection] Page

In this [Sample Selection] page, the samples to be measured for each element are selected.

When all the samples are to be measured for all elements


Confirm that each field has a check mark and click on [Next] to proceed to the [Connect to Instrument/Send
Parameters] page.

When some of the samples are not to be measured for all elements
(1) Click the check box of the sample not to be measured to clear it. To clear some check boxes together, drag
the mouse cursor to select the range, and press the DEL key on the keyboard or select [Not Measure] by
clicking the right mouse button.
(2) After completing the settings, click on [Next] to proceed to the [Connect to Instrument/Send Parameters]
page.

AA-6800/6650 Instruction 4-11


Chapter 4 Basic Operation

4.2.1.7 Connect to Instrument/Send Parameters

Figure 4.12 [Connect to Instrument/Send Parameters] Page

Check that the power of the AA is already ON and click on [Connect/Send Parameters]. The [Initialize] dialog
box is opened and AA main unit is initialized.
At the step of [Start Leak Check], the following message appears.
"Gas leak check will be started. Press the EXTINGUISH button on the instrument."
According to this instruction, press the EXTINGUISH button on the right side of the combustion chamber and
click on [OK] to close the message. The instrument automatically starts the gas leak check for 10 minutes.
During this time, a flame cannot be ignited. If the fuel gas is not supplied, the following message appears.
"Gas pressure was too low to execute gas leak check. Please check that the fuel gas supply pressure and
perform the gas leak check."
Supply the fuel gas and press the EXTINGUISH button then click on [Retry]. On the other hand, when you
ignore the message and click on [Cancel], the message box is closed and the initialization is finished without
executing the gas leak check. If the gas leak check is not executed at the time of initialization, the instrument
starts the 10-minute gas leak check automatically when the fuel gas is supplied. And after the 10 minutes, if a
gas leak was not detected, you can ignite a flame.

NOTE
If the EXTINGUISH button is not pressed according to the message, the gas leak check may not be
executed correctly. It may judge that a gas leak is detected even if the instrument is working properly. When
supplying the fuel gas after the initialization, this does not occur.

After completing the initialization, click on [OK] to close the [Initialize] dialog box. Then, click on [Next] in the
[Connect to Instrument/Send Parameters] page to proceed to the [Optics Parameters] page.

4-12 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.1.8 Optics Parameters

Figure 4.13 [Optics Parameters] Page

The wavelength, slit width, socket number, lamp current and lamp mode for the element to be firstly analyzed
are set here. Note that these settings are only for the element to be firstly analyzed (the element that was
specified in [Measurement Element] at the right lower on the [Element Selection] page or [Connect to
Instrument/Send Parameters] page).

(1) For the [Wavelength] and [Slit Width], you usually need not to change the value since the appropriate set
values in the cookbook for each element are indicated. If you want to change them specially, enter the
numeric value for wavelength and select a slit width from 6 levels on the list that is displayed by clicking on
the [ ] button.
(2) Click on the [Lamp Pos. Setup] button. Then [Lamp Position Setup] dialog box will appear. Enter the
[Element] and [Lamp Type] of the lamp actually mounted for each socket number. Select the element from
the drop-down list. Select [Normal] or [SR] for [Lamp Type] from the drop-down list. Then select lamp ID in
[Lamp ID] field. You can turn lamp turret manually and change lamp while the [Lamp Position Setup] dialog
box is displayed. Click on [OK] to return to the [Optics Parameters] page.

Figure 4.14 [Lamp Position Setup] Dialog Box

AA-6800/6650 Instruction 4-13


Chapter 4 Basic Operation

(3) In the [Socket #] field, set the socket number where the lamp of the selected element is set. If the same
element lamps are set in two or more positions of the lamp turret, click on the [ ] button and select the
socket # from the drop-down list.
(4) In the [Lamp Mode] field, the appropriate mode according to the selected element and lamp is indicated, so
you need not to change it for most cases. If you want to change it specially, click on the [ ] button and
select the mode from the drop-down list.
(5) In the [Lamp ID] field, the currently used lamp ID (set at the time of lamp history data registration) is
displayed.
(6) In the [Lamp Status] field, a necessary message, for example, "Line Search is necessary" is indicated.
(7) Putting a check mark in the check box of [Lamp ON] lights on the lamp.
(8) In the [Lamp Current] field, the lamp current according to the selected element and lamp type is indicated,
so you need not to change it for most cases.
In the case of normal lamp, the numeric value is shown for [Low] and "0" is shown for [High].
The lamp current changed here is actually set on the unit at the following timings.
• when the extinguished lamp is lit.
• when [Line Search/Beam Balance] is executed in the case of main lighting lamp.
• when [Warmup Lamp] in the [Optics Parameters] page of the main lighting element is clicked
then [Apply] is clicked in the [Select Warmup Lamp] dialog box in the case of warmup lamp.
(9) [Warmup Lamp] button
This is used to warm up the lamp of the next element to be analyzed after the current element. For details,
refer to section 5.5.6.2.
(10) [Line Search] button
If the [Line Search] is clicked on, the [Line Search/Beam Balance] dialog box appears.
When [Line Search/Beam Balance] is necessary, it is automatically executed. If [Line Search/Beam
Balance] has already finished, the result is displayed.

Figure 4.15 [Line Search/Beam Balance] Dialog Box

When it is automatically executed, the line search (wavelength adjustment) is executed first, then the beam
balance (gain adjustment for detector) is performed. If only the beam balance is necessary, only the beam
balance is executed. After completed, click on [Close] to return to the [Optics Parameters] page.

4-14 AA-6800/6650 Instruction


4.2 Software Basic Operation

(11) After all the settings are completed, click on [Next] to proceed to the [Atomizer/Gas Flow Rate Setup] page.

NOTE
When measuring plural elements, you cannot set parameters for the elements other than the current
measurement one on the [Optics Parameters] and [Atomizer/Gas Flow Rate Setup] pages. If you use the
ASC to measure plural elements automatically and you need to modify the parameters for other elements
than the current measurement one, you can change these parameters by using the [Edit Parameters] button
in the [Element Selection] page.

4.2.1.9 Atomizer/Gas Flow Rate Setup (AA-6800)

Figure 4.16 [Atomizer/Gas Flow Rate Setup] Page (AA-6800)

In the [Atomizer/Gas Flow Rate Setup] page, the burner position and fuel gas flow rate are set. Select the
operation object [Atomizer Position] or [Fuel Gas Flow Rate] by clicking on the radio button to switch the page
display. You can set either of them first.

AA-6800/6650 Instruction 4-15


Chapter 4 Basic Operation

When [Fuel Gas Flow Rate] is selected


(1) You can set the flame type and the fuel gas flow rate here.
(2) In the [Flame Type] field, an suitable flame type is indicated according to the element. If you need to
change it, click on the [ ] button and select the flame type from the list. Note that you must not use N2O-
C2H2 flame with the provided standard burner head. The high temperature burner head of special
accessory is required.
(3) In the [Fuel Gas Flow Rate] field, an appropriate value is indicated according to the element. If you need to
change it specially, enter the numeric value then click on the [Flame Setup] button.
(4) You can also increase or decrease the fuel gas flow rate by using the flame set buttons [Increase] or
[Decrease] at the lower of the page. In this case, the set value in the [Fuel Gas Flow Rate] field also
changes accordingly.
(5) The [Gas Flow Auto] button is used to set the optimum fuel gas flow rate by measuring sample actually.
For the procedure of [Gas Flow Auto], refer to section 4.11.2.

When [Atomizer Position] is selected


(1) Leave [Burner Angle] as "0" for a usual use. Change it only when you want to decrease the sensitivity by
changing the angle for high concentration samples.
(2) For the [Burner Height] field, an appropriate value is indicated according to the element, so you need not to
change it for usual use. However, the optimum condition may differ depending on the gas flow rate or
sample type. In that case, change it by entering the numeric value then clicking on [Set Position].
(3) You can also move the burner position upward or downward by clicking on the position setup buttons [Up]
or [Down] at the lower of the page. In this case, the set value in the [Burner height] field also changes
accordingly.
(4) The [Burner Position Auto] button is used to set the optimum burner height condition by measuring sample
actually. For the procedure of [Burner Position Auto], refer to section 4.11.1.

After all the settings are completed, click on the [Finish] button. The Wizard ends and the main window appears.
If you want to save the set conditions as a template file, proceed to section 4.2.3. If you want to start the
measurement, proceed to section 4.3.1.

4-16 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.1.10 Atomizer/Gas Flow Rate Setup (AA-6650)

Figure 4.17 [Atomizer/Gas Flow Rate Setup] Page (AA-6650)

In the [Atomizer/Gas Flow Rate Setup] page, the burner position and fuel gas flow rate are set. Select the
operation object [Atomizer Position] or [Fuel Gas Flow Rate] by clicking on the radio button to switch the page
display. You can set either of them first.

AA-6800/6650 Instruction 4-17


Chapter 4 Basic Operation

When [Fuel Gas Flow Rate] is selected


(1) You can set the flame type and the fuel gas flow rate here.
(2) In the [Flame Type] field, an suitable flame type is indicated according to the element. If you need to
change it, click on the [ ] button and select the flame type from the list. Note that you must not use N2O-
C2H2 flame with the provided standard burner head. The high temperature burner head of special
accessory is required.
(3) In the [Fuel Gas Flow Rate] field, an appropriate value is indicated according to the element. If you need to
change it specially, enter the numeric value then click on the [Flame Setup] button.
(4) You can also increase or decrease the fuel gas flow rate by using the flame set buttons [Increase] or
[Decrease] at the lower of the page. In this case, the set value in the [Fuel Gas Flow Rate] field also
changes accordingly.

When [Atomizer Position] is selected


(1) The [Burner Height] field indicates an appropriate value according to the element. Set the burner height
using the knob for adjusting burner vertical position.
The [Burner Height] field indicates the distance from the optical axis down to the burner head using a
positive value.
The knob for adjusting burner vertical position is protruded on the lower part of the atomizer and labeled
with "VERTICAL". The burner height can be read with a scale on the atomizer base unit (Figure 3.5, <1> in
section 3.1.4.2).
The optimum condition of the burner height may be different from the standard parameter depending on
the gas flow rate and sample type. In such cases, change the burner height while spraying the sample, and
obtain the burner height with which the real time data profile shows a high and stable sensitivity.
The knob labeled with "HORIZONTAL" on the upper surface of the atomizer lower unit is used to adjust the
forward-back position of the burner. Usually, it is not necessary to change the horizontal position after
adjusting it at the time of changing the atomizer (from graphite furnace to burner). Do not touch this knob if
not necessary.
(2) Leave [Burner Angle] as "0" for a usual use. Change it only when you want to decrease the sensitivity by
changing the angle for high concentration samples.

After all the settings are completed, click on the [Finish] button. The Wizard ends and the main window appears.
If you want to save the set conditions as a template file, proceed the section 4.2.3. If you want to start the
measurement, proceed to section 4.3.1.

4-18 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.2 Software Basic Operation (Furnace Method)


4.2.2.1 Operation Flowchart (Furnace Method)
This Wizard has a sequence for setting as shown below. You can proceed to the next step or return to the
preceding step by using the [Next] or [Back] button.

(Starting up the AA Software)


p
(1) Wizard Selection
p
(2) Element Selection
p
(3) Preparation Parameters
p
(4) Sample ID
p
(5) Sample Selection
p
(6) Connect to Instrument/Send Parameters
p
(7) Optics Parameters
p
(8) Furnace Program
p
(Finish)
p
(Start Measurement)

NOTE
When measuring plural elements, you cannot set parameters for the elements other than those for the
current measurement on the [Optics Parameters] and [Furnace Program] pages. If you use the ASC to
measure plural elements automatically and you need to change the parameters for the elements other than
those for the current measurement, you can change these parameters by using the [Edit Parameters] button
in the [Element Selection] page.

AA-6800/6650 Instruction 4-19


Chapter 4 Basic Operation

4.2.2.2 Wizard Selection

Figure 4.18 [Wizard Selection] Dialog Box

When the [Wizard Selection] dialog box appears, if you make a new parameter set, select the [Element
Selection] icon on the [Wizard] sheet and click on the [OK] button. Then the [Element Selection] page will
appear.

4.2.2.3 Element Selection

Figure 4.19 [Element Selection] Page

4-20 AA-6800/6650 Instruction


4.2 Software Basic Operation

(1) First, click on the [Select Elements] button. Then the [Load Parameters] page will appear.

Figure 4.20 [Cookbook] Sheet in [Load Parameters] Page

(2) In this page, select the element first. You can use one of the methods below to select the element.
1. Enter the element symbol directly in the element field from the keyboard.
2. Click on the [ ] button at the right of the element field, and select the element from the element
symbol list shown in alphabetical order.
3. Click on [Periodic Table] and select the element from the periodic table.
(3) Next, select [Furnace] for the measurement method by clicking on the radio button.
(4) Select [Normal Lamp] when using a normal hollow cathode lamp ([SR Lamp] is selected only when the SR
method is used as the background correction method).
(5) When using the autosampler, click on the [Using ASC] check box.
(6) After completing the settings, click on the [OK] to return to the [Element Selection] page (Figure 4.19). At
this time, a message about lamp setup is displayed. Press the [No] button here. The lamp setup is also
possible later. The selected element is shown in the table on the page.
(7) When plural elements are to be analyzed, return to this [Element Selection] page once and then click on
[Select Elements] again to select the next element. Repeat the procedure below as required.
Click on [Select Elements] o Select the element o Click on the [OK] button
(8) When returning to the [Element Selection] page after selecting an element, the selected elements are
listed one by one. In the automatic measurement using the ASC, the measurement is executed in this
order. To change the order of automatic measurement, click on and highlight the row whose order is to be
changed first, then click on the button [Up] or [Down] at the right on the screen to move the row. To delete
any of the elements, click on and highlight the row then click on the [Delete] button.
(9) The [Measurement Element] field at the right lower of the page indicates the element to be analyzed first.
In the case of ASC automatic measurement, the measurement is started from the element shown for
[Measurement Element] and the elements located above this element in the table are not to be measured.

AA-6800/6650 Instruction 4-21


Chapter 4 Basic Operation

(10) When analyzing plural elements sequentially with the ASC, it is necessary to set the socket numbers in
alternating odd/even. Follow the procedure below to set or change the socket number.
1. Click on [Edit Parameters].
2. Click on the [Optics Parameters] tab.
3. Click on [Lamp Pos. Setup] to display the [Lamp Position Setup] dialog box.
4. Enter [Element], [Lamp Type] and [Lamp ID] for each socket # and click on [OK] to close the [Lamp
Position Setup] dialog box. These settings are saved, and also used when the software is started next
time.
When changing the lamp position in the lamp turret, set the parameters again in [Lamp Position
Setup] dialog box.
5. Click on the [ ] button in [Socket #] on the [Optics Parameters] page and select an appropriate
number from the list.
6. Click on [OK] to return to the [Element Selection] page.
You may also set the socket number by using the [Instrument]-[Lamp Position Setup] in the menu bar
beforehand. Then the socket numbers are automatically indicated in the table in the [Element Selection]
page. You can adjust the odd/even order by moving the row on the table or change lamp position again by
using [Lamp Pos. Setup] if necessary.
(11) When measuring plural elements continuously by using the ASC, the default values according to each
element are used as the parameters of [Optics Parameters] and [Furnace Program] for the elements other
than [Measurement Element] at the right lower of the [Element Selection] page. If you need to change
them, follow the procedure below.
1. Click on [Edit Parameters].
2. Click on the [Optics Parameters] tab or [Furnace Program] tab.
3. Set necessary items. For details on setup contents, refer to section 5.5.6 or 5.5.9.
4. Click on [OK] to return to the [Element Selection] page.
(12) After completing all the settings, click on [Next]. The [Preparation Parameters] page will appear.

4-22 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.2.4 Preparation Parameters

Figure 4.21 [Preparation Parameters] Page

First, click on the element row to highlight it, then click on [Edit]. The [Preparation Parameters] page will appear.
Set the parameters as below.

Figure 4.22 [Edit Preparation Parameters] Dialog Box

AA-6800/6650 Instruction 4-23


Chapter 4 Basic Operation

(1) Mixing Setup, Repeat Measurement Conditions, Reagent Setup, Coating and Boost Cycle
If you want to mix the sample and reagents, put a check mark in the [Mixing ON] check box. Then click on
[Mixing] to open the [Mixing Setup] dialog box.

Figure 4.23 [Mixing Setup] Dialog Box

In this step, set the [Volume] in [Injection Parameters]. The default value is 20 (PL). Leave other items in
the [Mixing Setup] dialog box as the default values. Also, leave all the items in the [Reagent Setup] dialog
box opened by clicking on [Reagent], in the [Coating and Boost Cycles] opened by clicking on [Coating],
and in the [Repeat Measurement Conditions] opened by clicking on [Repeat Conditions].

(2) Calibration Curve Parameters


1. Select [Calibration Curve] for [Measurement Type]. If you need to select [SMSA] (Simple Standard
Addition Method) or use standard addition method, refer to section 4.9.
2. Select [1st] for [Order] of equation if the calibration curve is straight. You may also select [2nd] or [3rd]
if it is curved. Anyway, you can change the order after measurement. So, select [1st] here.
3. [Zero Intercept] is used to make a calibration curve equation that forcibly intercepts the origin. This
setting can also be changed later.
4. Select [Conc. Unit] of the prepared standard samples. Click on the [ ] button to select it from the list.

(3) [STD Samples] Preparation Parameters


Input the [Number of STD]. Then a table composed of as many rows as the sample number is created in
the [STD Samples] preparation parameters table. Key in the actual concentrations of the prepared
standards in the table, although the default values from the cookbook are indicated on the table. Also, set
the preparation parameters as below.
When the standard samples are not prepared by using the ASC
Clear a check mark of [Mixing ON]. In this case, mixing is not performed and [Total Vol] becomes the
volume to be injected into the graphite tube. Enter the sample injection volume into the graphite tube for
[Standard] (You cannot input a value for [Total Vol] directly). Leave all [Diluent], [Reagent 1], [Reagent 2]
and [Reagent 3] as "0". Then [Total Vol] becomes equal to [Standard]. Don't use a value larger than 100 PL
for [Total Vol]. 20 PL is acceptable as an injection volume for usual measurements.
When only sample is injected (all of the diluent and reagent parameters are set to "0"), the instrument
automatically judges that no mixing should be performed, even if [Mixing ON] is check-marked.
When the standard samples are prepared by using the ASC
Input each field of [Diluent], [Reagent 1], [Reagent 2] and [Reagent 3]. Then [Total Vol] will be
automatically calculated.
The following example shows a case in which the standard sample is diluted to make each concentration
for calibration curve by using the ASC preparation function.

4-24 AA-6800/6650 Instruction


4.2 Software Basic Operation

NOTE
[Total Volume] must satisfy the following condition.
When the mixing is performed
(Injection Vol.) u (Max. No. of Reps.) u (No. of Boost Cycles) + 50 PL d (Total Vol.) d 600 PL
The (Injection Vol.) is the value set in the [Mixing Setup] dialog box, and the "50 PL" is the dead volume of
the mixing port. If furnace boost cycle is not performed, (No. of Boost Cycles) is "1".
When the mixing is not performed
(Injection Vol.) = (Total Vol.) d 100 PL

(EXAMPLE)
200 PL of 10 ppb, 20 ppb and 30 ppb standard samples are prepared from the 100 ppb standard sample
solution. The 100 ppb standard sample is regarded as the "Sample" here and the parameters are set as
below. The total volume is automatically calculated.

[Conc.] [Pos.] [Standard] [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] [Total Vol]


10 1 20 180 0 0 0 200
20 1 40 160 0 0 0 200
30 1 60 140 0 0 0 200

If [Sample Injection Volume] (set in the [Mixing Setup] dialog box or the [ASC Parameters] page) is "20 PL"
and the [Max. Number of Repetition] (set in the [Repeat Measurement Conditions] dialog box) is "5 times"
and furnace boost cycle is not performed (this means [Number of Boost Cycles] in [Coating and Boost
Cycles] dialog box is "1"), the calculation for total volume condition is as follows:
(20 PL) u (5 times) u (1 cycle) + 50 PL d 200 PL d 600 PL
This indicates that the settings are correct.

(4) Weight Correction Factors


Input [Weight Correction Factors]. These factors are necessary for calculating the actual concentration.
[Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factors] are used in the following
equation.
Actual concentration = (Conc.) u [Volume Factor] u [Dilution Factor]
u [Correction Factor] / [Weight Factor] ........................................................ (1)
The actual concentration is calculated with the above equation. Note that the unit is not converted
automatically. Convert the unit using the [Correction Factor] factor if necessary (Refer to the example
below).
If the above calculation for actual concentration is not necessary, leave all the factors "1".
When the auto dilution and remeasurement function was performed, the dilution ratio used for the
automatic dilution by the ASC is displayed in the [ASC DF] (ASC Dilution Factor) on the MRT worksheet,
and the actual concentration is calculated as below.
Actual concentration = (Conc.) u [Volume Factor] u [Dilution Factor] u [ASC Dilution Factor]
u [Correction Factor] / [Weight Factor] ........................................................ (2)
Each factor is expressed in MRT worksheet and data print as follows.
[Volume Factor] [VF]
[Dilution Factor] [DF]
[ASC Dilution Factor] [ASC DF]
[Correction Factor] [CF]
[Weight Factor] [WF]

AA-6800/6650 Instruction 4-25


Chapter 4 Basic Operation

(EXAMPLE)
If the reagents and diluent are added to 50 PL of the sample and filled up to 250 PL, the actual
concentration is calculated from the measured [Conc.] with the factors; [Weight Factor]: 50 PL, [Volume
Factor]: 250 PL and [Correction Factor]: 1. From the above equation (1),
Actual concentration = (Conc.) u 250 PL u 1 u 1 / 50 PL
In the same example, if calculating the actual conc. (ppm) from the conc. (ppb) by converting the unit, use
0.001 for CF since 1 ppb is 0.001 ppm.
Actual concentration ppm = (Conc. ppb) u 250 PL u 1 u 0.001 / 50 PL
If the actual concentration calculation is not necessary, set all the factors to "1".

(5) [Unknown Samples] Preparation Parameters


When the sample mixing is not performed by using the ASC
Clear a check mark from [Mixing ON]. In this case, the mixing is not performed and [Total Vol] becomes the
volume to be injected into the graphite tube. Enter the sample injection volume into the graphite tube in
[Sample] (You cannot input a value in [Total Vol] directly). Leave all [Diluent], [Reagent 1], [Reagent 2] and
[Reagent 3] as "0". [Total Vol] becomes equal to [Sample]. Don't use the value larger than 100 PL for [Total
Vol]. 20 PL is acceptable as an injection volume for usual measurements.
When only the sample is injected (all of the diluent and reagent parameters are set to "0"), the instrument
automatically judges that no mixing should be performed, even if the mixing is set to "ON".
When the sample mixing is performed by using the ASC
Input each of [Diluent], [Reagent 1], [Reagent 2] and [Reagent 3] (the unit is "PL"). Then [Total Vol] will be
automatically calculated. [Total Vol] must satisfy the following condition.
• When the mixing is performed
(Injection Volume) u (Max. No. of Reps.) u (No. of Boost Cycles) + 50 PL d (Total Volume) d 600 PL
The (Injection Volume) is the value set in the [Mixing Setup] dialog box, and the "50 PL" is the dead
volume of the mixing port. If furnace boost cycle is not performed, (No. of Boost Cycles) is "1".
• When the mixing is not performed
(Injection Volume) = (Total Volume) d 100 PL
When [Mixing ON] is check-marked, the injection volume is set in the [Mixing Setup] dialog box (Figure
4.23).

(6) [Blank Samples] Preparation Parameters


Set up the periodic blank measurement here.
The periodic blank measurement is a function to create a measurement procedure on the MRT to remove
the influence of baseline drift by inserting a blank measurement in a fixed interval.
When [Periodic Blank] is not used
Leave the [Periodic Blank] field [Off].
When the [Periodic Blank] is used
1. Click on [Periodic Blank] and click on the [ ] button at the right of [Off] to display the list for selecting
[On] or [Off]. Click on [On].
2. Click on [Meas. Interval] and enter the numerical value to insert the blank measurement in every some
samples. If "1" is entered, the sample and blank are measured alternately.
3. [Pos.] indicates the blank position on the ASC turntable. Select the position from the list.
4. Set the preparation parameters for blank sample in the same procedure as that for [Unknown
Samples] preparation parameters.

4-26 AA-6800/6650 Instruction


4.2 Software Basic Operation

(7) After setting the parameters, click on [OK] to return to the [Preparation Parameters] page. In the case of
multi-element analysis, click on the next row to highlight it, then click on [Edit] and set the parameters in the
same way.

(8) Loading/Saving the Preparation Parameters


The standard samples preparation parameters, the unknown samples preparation parameters and the
blank samples preparation parameters can be saved in a file together and used again for setting other
element parameters. Press [Save] button and specify the file name and the place to save it. In a
preparation parameter file (*.mix), the following parameters are saved together:

Parameters Screens

(A) Measurement Type [Edit Preparation Parameters] dialog box


(Calibration Curve Method or SMSA)

(B) Mixing ON/OFF [Edit Preparation Parameters] dialog box

(C) Preparation Parameters [Edit Preparation Parameters] dialog box


(STD, Unknown, Blank)

(D) Reagent Name [Reagent Setup] dialog box


Reagent Position
Intake Order

(E) Coating and Boost Cycles [Coating and Boost Cycles] dialog box

A file which was created under different conditions ((A) Measurement Type and (B) Mixing ON/OFF) from
the current setting cannot be loaded.

(9) When completing all the settings, click on [Next]. Then the [Sample ID] page will appear.

AA-6800/6650 Instruction 4-27


Chapter 4 Basic Operation

4.2.2.5 Sample ID

Figure 4.24 [Sample ID] Page

(1) In this [Sample ID] page, enter the sample number first. Then key in the sample ID (sample name) in
[Sample ID] one by one.
(2) When using the same name with successive No. for all the samples, click on [Collective Setup] button.
Then the [Sample ID Collective Setup] dialog box will appear.

Figure 4.25 [Sample ID Collective Setup] Dialog Box

Click the [Create Sample ID] check box to select it, and enter a common sample name in [Name]. Then
names with successive number are automatically created and shown in the table (e.g. Sample001,
Sample002, ...). Entering the first sample position in [ASC Start Pos.] sets the sample positions of the
second and after in the table automatically.
Click on [OK] to return the [Sample ID] page.
(3) You can input and change the name individually after the collective setup.
(4) After completing the settings, click on [Next]. Then the [Sample Selection] page will appear.

4-28 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.2.6 Sample Selection

Figure 4.26 [Sample Selection] Page

In this [Sample Selection] page, the samples to be measured for each element are selected.

When all the samples are to be measured for all elements


Confirm that each cell has a check mark and click on [Next] to proceed to [Connect to Instrument/Send
Parameters] page.

When some of the samples are not to be measured for all elements
(1) Click the check box of the sample that is not to be measured to clear it. To clear some check boxes
together, drag the mouse cursor to select the range, and press the DEL key on the keyboard or select [Not
Measure] by clicking the right mouse button.
(2) After completing the settings, click on [Next] to proceed to [Connect to Instrument/Send Parameters] page.

AA-6800/6650 Instruction 4-29


Chapter 4 Basic Operation

4.2.2.7 Connect to Instrument/Send Parameters

Figure 4.27 [Connect to Instrument/Send Parameters] Page

After checking that the power switches of the AA main unit and peripheral equipment are already turned ON,
click on [Connect/Send Parameters]. The [Initialize] dialog box is opened and the AA main unit is initialized.
After completing the initialization, click on [OK] to close the [Initialize] dialog box. Then, click on [Next] in the
[Connect to Instrument/Send Parameters] page to proceed to the [Optics Parameters] page.

4-30 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.2.8 Optics Parameters

Figure 4.28 [Optics Parameters] Page

The wavelength, slit width, socket number, lamp current and lamp mode for the element to be firstly analyzed
are set here. Note that these settings are only for the element to be firstly analyzed (the element that was
specified in [Measurement Element] at the right lower on the [Element Selection] page or [Connect to
Instrument/Send Parameters] page).

(1) For the [Wavelength] and [Slit Width], you usually need not to change the value since the default values
which are appropriate for each element are indicated. If you want to change them specially, enter the
numeric value for wavelength and select a slit width from 6 levels from the list that is displayed by clicking
on the [ ] button.
(2) Click on the [Lamp Pos. Setup] button. Then [Lamp Position Setup] dialog box will appear. Enter [Element]
and [Type] of the lamp actually mounted for each socket number. Select the element from the drop-down
list. Select [Normal Lamp] or [SR Lamp] for [Lamp Type] from the drop-down list. Then select lamp ID in
[Lamp ID] field. Click on [OK] to return to the [Optics Parameters] page. While the [Lamp Position Setup]
dialog box is displayed, you can turn the lamp turret manually and change the lamp.

Figure 4.29 [Lamp Position Setup] Dialog Box

AA-6800/6650 Instruction 4-31


Chapter 4 Basic Operation

(3) In the [Socket #] field, set the socket number where the lamp of the selected element is set. If the same
element lamps are set in two or more positions of the lamp turret, click on the [ ] button and select the
socket # from the drop-down list.
(4) In the [Lamp Mode] field, the appropriate mode according to the selected element and lamp type is
indicated, so you need not to change it for most cases. If you want to change it specially, click on the [ ]
button and select the mode from the drop-down list.
(5) In the [Lamp ID] field, the lamp ID currently used (set at the time of lamp history data registration) is
displayed.
(6) In the [Lamp Status] field, a necessary message, for example, "Line Search is necessary" is indicated.
(7) Putting a check mark in the check box of [Lamp ON] lights on the lamp.
(8) In the [Lamp Current] field, the lamp current according to the selected element and lamp type is indicated,
so you need not to change it for most cases. In the case of normal lamp, the numeric value is shown for
[Low] and "0" is shown for [High]. The lamp current changed here is actually set on the unit at the following
timings.
• when the extinguished lamp is lit.
• when [Line Search/Beam Balance] is executed in the case of main lighting lamp.
• when [Warmup Lamp] in the [Optics Parameters] page of the main lighting element is clicked
then [Apply] is clicked in the [Select Warmup Lamp] dialog box in the case of warmup lamp.
(9) [Warmup Lamp] button
This is used to warm up the lamp of the next element to be analyzed after the current element. For details,
refer to section 5.5.6.2.
(10) [Line Search] button
If the [Line Search] is clicked on, the [Line Search/Beam Balance] dialog box appears.
When line search/beam balance is necessary, it is automatically executed. If line search/beam balance
has already finished, the result is displayed.

Figure 4.30 [Line Search/Beam Balance] Dialog Box

When it is automatically executed, the line search (wavelength adjustment) is executed first, then the beam
balance (gain adjustment for detector) is performed. If only the beam balance is necessary, only the beam
balance is executed. After completed, click on [Close] to return to the [Optics Parameters] page.

4-32 AA-6800/6650 Instruction


4.2 Software Basic Operation

(11) After all the settings are completed, click on [Next] to proceed to the [Furnace Program] page.

NOTE
When measuring plural elements, you cannot set parameters for the elements other than those for the
current measurement on the [Optics Parameters] and [Furnace Program] page. If you use the ASC to
measure plural elements automatically and you need to change the parameters for the elements other than
those for the current measurement, you can change these parameters by using the [Edit Parameters] button
in the [Element Selection] page.

4.2.2.9 Furnace Program

Figure 4.31 [Furnace Program] Page

(1) Set the furnace program here. A default furnace program is automatically indicated in the table according
to the selected element, so you may use it as it is. Make any changes to this program as required.
(EXAMPLE)
The default furnace program has the following basic steps.

AA-6800/6650 Instruction 4-33


Chapter 4 Basic Operation

Table 4.1 Example of Furnace Program

Flow Rate
STAGE# Temp (qC) Time (sec) Heat Mode Sensitivity GAS Type
(L/min)

1 150 20 RAMP #1 0.1

2 250 10 RAMP #1 0.1

3 800 10 RAMP #1 1.0

4 800 10 STEP #1 1.0

5 800 3 STEP #1 0.0

6 2300 2 STEP #1 0.0

7 2500 2 STEP #1 1.0

Sampling Stage No.: 6

The above furnace program is explained as below.


• In this program, water is vaporized and the sample is "Dried" at the stage #1, and coexisting
organic substances are "Ashed" from the stage #2 to #5, then the target element is "Atomized"
at stage #6. The stage #7 is a "Cleaning" stage to eliminate the residue in the graphite tube.
• For the "Ashing" stage, change the [Temp.] and [Time] according to the contained coexisting
substances (for example, if much amount of organic compounds are contained, set the [Temp.]
higher and the [Time] longer).
• Set [Heat Mode] to "RAMP" (the temperature is increased gradually) during "Drying" stage and
at the beginning of "Ashing" stage, and set it to "STEP" (heated directly to the set temperature)
during "Ashing" and "Atomizing" stages.
• In the [Sensitivity] column, the "Atomizing" stage and its preceding stage are check-marked to
perform a high sensitivity measurement. At this time the inner gas is fixed to 0 (L/min).
• [Sampling Stage No.] indicates a stage for data sampling. Usually, the atomizing stage is
selected.
• [Gas Type] is set to #1 for all the stages when a usual measurement is performed.
(2) When changing/creating a furnace program, you can save it so that you can use the same program next
time.
[Save]
To save the furnace program, click on [Save] and enter the file name on the [Save As] dialog box. The
extension for furnace program is ".fur" (for example, "copper.fur"). Then click on [Save].
[Load]
To open the furnace program file, click on [Load]. The [Open] dialog box will appear. Then click on the file
name to be opened and click on [Open].
(3) When editing a ready-made furnace program, use the [Insert Row] or [Delete Rows] buttons to insert a row
or delete rows.
(4) The [Cleaning] button is used to heat the graphite tube to a high temperature for cleaning. Also, the [Test
Meas.] button is used to perform the test measurement actually using the set furnace program. For details,
refer to sections 5.5.9.2 and 5.5.9.3.
(5) For details of the [Coating/Boost Cycle], [Change Graphite Tube] and [Temp. Search], refer to sections
5.5.9.1, 5.5.9.4 and 5.5.9.5, respectively.
(6) After completing all the settings, click on [Finish]. The Wizard finishes and the main window will appear.

4-34 AA-6800/6650 Instruction


4.2 Software Basic Operation

4.2.3 Saving the Template


If you want to use the parameters set with the above procedures from the next time, you can save them as a
template. Then you can load it in the [Wizard Selection] dialog box.

(1) Click on [File] in the menu bar and select [Save As].

Figure 4.32 [Save As] Dialog Box

(2) Select "template (*.taa)" for [Save as type]. The extension of the file name displayed in [File name] is
changed to ".taa". The [Save As] dialog box is closed and the template file is saved.
(e.g.) If "notitle.aa" is displayed in [File name] when the [Save As] dialog box is opened, selecting "template
(*.taa)" changes the file name to "notitle.taa".
(3) Input the file name. Leave the extension as ".taa".
(e.g.) Change the part "notitle" in the "notitle.taa" to a name you like.
(4) Press the [Save] button. The [Save As] dialog box is closed and the template file is saved.

AA-6800/6650 Instruction 4-35


Chapter 4 Basic Operation
4.3 Measurement Procedures

After completing all the settings, prepare the samples. Perform the measurement following the procedure
indicated on the MRT worksheet. The current row is highlighted and its [Action] field shows the type of
measurement. When using the ASC, set the samples in proper positions.
If no setting is made on the MRT worksheet, a message appears to indicate that no schedule exists. In this
case, select [Parameters]-[Schedule Creation Wizard] from the menu and set the measurement procedures.

NOTE
If a menu or dialog box is kept open during the measurement operation, the measurement operation may be
interrupted. Be careful about it when checking the setup parameters during the operation.

4.3.1 Measurement Operation (for Flame Method)


In the case of flame method, read section 4.8 "Igniting and Extinguishing the Flame" thoroughly before starting
the measurement. Confirm that the gases are supplied at correct pressures and the burner head is mounted
properly. Note that the ignition cannot be made for 10 minutes after the automatic gas leak check is started.
If the lamp warmup time (unit: minute) is set, wait until the warmup time elapses after the light comes on, and
then start the measurement.

Manual Measurement
(1) Igniting the Flame
Press the IGNITE button on the front of the AA main unit to ignite the flame.
(2) Auto Zero
At the [AUTO ZERO] row on the MRT worksheet, put the suction nozzle into vaporized water (or solvent)
and spray it. When the signal of real time graph is stabilized, click on [START] at the bottom of the main
window (or press the F5/F6 key). Also, the auto zero can be executed by pressing [AUTO ZERO] (or F3
key), although the operation result of auto zero execution is not indicated on the MRT worksheet in this
case.
(3) Blank Measurement (if necessary)
Spray the blank sample and click on [BLANK] at the bottom of the main window (or press the F4 key). The
"BLANK" row is inserted on the MRT worksheet and the measurement result is displayed. When the
"BLANK" row is prepared on the MRT worksheet beforehand, press [START] (or F5/F6 key).
If the standard or unknown samples are measured after executing the blank measurement, their measured
values (absorbance or energy) are indicated after the measured blank value is subtracted from their actual
measured values. The difference between this measured blank value and the actual measured standard or
unknown sample value is displayed in [Abs] (or [Energy]) on the MRT until the next blank measurement is
executed.
(4) Standard Measurement
Spray the standard sample. When the signal of real time graph is stabilized, click on [START] at the bottom
of the main window (or press the F5 or F6 key) according to the set order. Measure the standard sample
while checking that it accords with the current row on the window. If the repeat measurement is selected,
clicking on [START] inserts a new row for repeat measurement according to the set repeat parameters.
Repeat the measurement following the row indication.

4-36 AA-6800/6650 Instruction


4.3 Measurement Procedures

(5) Checking the Calibration Curve


After measuring the standard samples, check the calibration curve displayed on the right upper of the
window. If the calibration curve graph display is too small, set the mouse cursor onto the border of the
calibration curve graph to indicate an arrow with two directions. Drag it to specify the range ("drag" means
moving the mouse while holding down the left mouse button).
If the calibration curve is correctly made, proceed to the measurement of unknown samples. If you want to
change the order or other parameters for calibration curve, click on [Type] above the calibration curve
graph then make a change on the [Change Calibration Curve Condition] dialog box.
(6) Unknown Sample Measurement
Spray the unknown sample. When the signal of real time graph is stabilized, click on [START] at the
bottom of the main window (or press the F5 or F6 key). If the repeat measurement is selected, clicking on
[START] inserts a new row for repeat measurement according to the set repeat parameters. Repeat the
measurement following the row indication. Then continue to measure the unknown samples according to
the specified order. Measure an unknown sample while checking that it accords with the current row on the
window.
If [START] is pressed when all the rows on the MRT worksheet have been executed, a new "UNK" row
(unknown sample row) is added and its measurement result is displayed.
When [Periodic Blank] is ON, "BLK" rows (blank measurement) are inserted in the specified interval. Spray
the blank and measure it at the rows.
If you want to make the size of MRT (Measurement Result Table) worksheet larger, set the mouse cursor
onto the upper border of the table to indicate an arrow with two directions. Press down the mouse left
button and drag it to specify the range. More number of rows can be displayed. For details on changing
sizes or using a scroll bar, refer to the WindowsTM documentation.
(7) Finishing the Measurement
After finishing the measurement, put the suction nozzle in vaporized water and spray it for a while. Then
press the EXTINGUISH button on the front of the AA main unit to extinguish the flame.

Using the ASC

NOTE
When using the ASC, put a check mark in the check box of [Using ASC] in [Sequence] sheet of [Edit
Parameters] page.

When using the ASC, verify that the position of each actual sample on the ASC turntable accords with the
setting on the MRT worksheet.
(1) Igniting the Flame
Press the IGNITE buttons on the front of the AA main unit to ignite the flame.
(2) Starting the ASC (Auto Sample Changer)
Click on [START] at the bottom of the main window (or press the F5 or F6 key) according to the set order.
The automatic measurement is started with the ASC.
(3) Extinguishing the Flame
After finishing the measurement, press the EXTINGUISH button on the front of the AA main unit to
extinguish the flame (A flame is automatically extinguished if the automatic flame extinction is selected).
(4) Checking the MRT Worksheet
Check the measured results on the MRT worksheet. If a remeasurement is necessary, refer to section
4.7.2. When printing or saving the data, proceed to section 4.4.

AA-6800/6650 Instruction 4-37


Chapter 4 Basic Operation

4.3.2 Measurement Operation (for Furnace Method)


(1) Mount the graphite tube correctly.
(2) Verify that the argon gas is supplied at the specified pressure, and flow the cooling water.
(3) Verify that the power switches on the rear of GFA-6500, both of the 100 V switch (CONTROL) and 200 V
switch (HEAT), are set to ON.
(4) Verify that the nozzle position adjustment is correctly completed. For details on the ASC nozzle position
adjustment, refer to 5.8.16.

Using the ASC


When using the ASC, verify that the position of each actual sample on the ASC turntable accords with the
setting on the MRT worksheet.
(1) Starting the ASC (Auto Sample Changer)
Click on [START] at the bottom of the main window (or press the F5 or F6 key) according to the specified
order. The automatic measurement is started with the ASC.
Before starting the measurement, the temperature calibration is executed. Note that heating is performed
when the temperature calibration is executed.
(2) When the last row of the MRT worksheet is finished, the instrument becomes in the waiting condition.
(3) Checking the MRT worksheet
Check the measured results on the MRT worksheet. If a remeasurement is necessary, refer to section
4.7.2. When printing or saving the data, proceed to section 4.4.

4-38 AA-6800/6650 Instruction


4.4 Saving/Printing/Deleting the Data
4.4 Saving/Printing/Deleting the Data

4.4.1 Saving the Data


When all measurements are completed, save the data. Select [File]-[Save As] from the menu bar, and enter the
file name in the [Save As] dialog box. File extension is limited to ".aa".

NOTE
A measurement data whose repeat measurement has not finished is not saved in the file.
If the data is necessary although the repeat measurement cannot be completed, print it out before ending the
AA software.

4.4.2 Printing the Data


Select [File]-[Print Data/Parameters] or [Print Table Data] from the menu bar. Then [Select Schedule] dialog
box will appear. Click on the elements ([Summary Report] is also available for [Print Table Data]) to highlight it.
Then click on [OK]. Printing will be executed.

[Print Data/Parameters]
The measurement parameters and measured data are printed. You can select the items to be printed in the
[File]-[Print Style]-[Print Style Setup] page.

[Print Table Data]


The current MRT worksheet is printed. You can select or change the items to be printed by selecting [File]-[Print
Style...]-[Table Show/Hide] page from menu.
In the case of [Summary Report], the columns shown in the MRT worksheet on the window are printed.

For details on printing, refer to sections 5.2.9 to 5.2.12.

4.4.3 Deleting the Data


If you want to use the same measurement conditions again, you can delete only the data with leaving the
measurement sequence. Execute [Edit]-[Clear Measurement Result] from the menu bar.
When deleting all of the measurement parameters, measured data and measurement sequence, select [File]-
[New] from the menu bar to open a new file.

AA-6800/6650 Instruction 4-39


Chapter 4 Basic Operation
4.5 Completing the Measurement

(1) When the measurement is completed, verify that the flame is extinguished and tighten the main valve of
the gas cylinder and compressor in the case of flame method. Close the main valves of the cooling water
and gas in the case of furnace method.
(2) Quit the software. For example, select [File]-[Exit] from the menu bar. The communication with the
instrument is shut off first, then the main window is closed. It takes approximately 30 seconds.
(3) Turn off the power switch of AA main unit.
(4) Turn off the power switches for peripheral equipments such as the ASC and GFA. When using the
GFA-6500, be sure to turn off the 200 V power switch.

4-40 AA-6800/6650 Instruction


4.6 Explanation of Main Window
4.6 Explanation of Main Window

When the Wizard is completed, the following main window appears.


(1) Menu bar
(2) Standard tool bar
(3) Measurement element tool bar (Display and switch the current measurement element)
(4) Absorbance digital display
(5) Real time graph (and temperature program graph)
(6) Peak profile (latest four measurements and overlay display)
(7) Calibration curve tool bar (Selection of calibration curve and type)
(8) Calibration curve display
(9) MRT worksheet
(10) Function buttons
(11) Status bar

<1> <3> <4> <6> <7>

<8>

<2>

<5>

<10> <9> <11>

Figure 4.33 Main Window

NOTE
While [Properties] is opened from the right mouse button menu on the graph or MRT worksheet, the
measurement is stopped. In this case, the measurement can be continued again when [Properties] is closed.

AA-6800/6650 Instruction 4-41


Chapter 4 Basic Operation

4.6.1 Menu Bar


Place the mouse cursor onto the menu ([File], [Edit], [Parameters], etc.) and click on it. Then a drop-down menu
appears. Select an item from the menu and click on it.
For details on each item, refer to Chapter 5.

4.6.2 Standard Tool Bar


The items frequently used are displayed in the tool bar. Quick selection is possible if you use this instead of
selecting from the menu bar. Each tool function is described below.
New: All the data and parameters are cancelled and parameters are set newly. (Same as [File]-[New] in
the menu bar)
Open: A file already created is opened. (Same as [File]-[Open] in the menu bar)
Save As: Current data and parameters are saved in the file. (Same as [File]-[Save As] in the menu bar)
Print: Data and parameters are printed. (Same as [File]-[Print Data/Parameters] in the menu bar)

4.6.3 Measurement Element Tool Bar


The element currently measured (or to be measured) is indicated. If you want to change the element, click on
the [ ] button and select one from the drop-down list. Then the page proceeds from [Optics Parameters] to
[Atomizer/Gas Flow Rate Setup] (for flame method) or [Furnace Program] (for furnace method). Set the
parameters if necessary and click on [Finish] (or [Cancel] to close the sheet without changes). The MRT
worksheet is also changed to that for selected element.

4.6.4 Absorbance Digital Display


The current absorbance value (or emission intensity in emission mode) is displayed. When the instrument is
BUSY, it is highlighted.

4.6.5 Real Time Graph (and Furnace Program Graph)


The changing absorbance value (or emission intensity in the case of emission mode) under measurement is
displayed in analog. You can check the peak shape and baseline conditions with this graph. In the case of
furnace, "Furnace Program" is also displayed.
The abscissa indicates time and the ordinate indicates absorbance (left scale) and temperature (right scale).

Right mouse button menu


If you want to change the scale or print the graph, place the cursor in the graph area and click on the right
button of the mouse. Then the pop-up menu shown in Figure 4.34 appears. Select an item and make settings.

Figure 4.34 Right Mouse Button Menu (Real Time Graph)

4-42 AA-6800/6650 Instruction


4.6 Explanation of Main Window

(1) [Properties]
[Real Time Graph Scale] (Flame)
You can change the graph ordinate and abscissa scale. Enter the maximum value and minimum value in
[Ordinate Max] and [Ordinate Min], respectively. Enter a numeric value in [Time Interval] (unit: second) for
abscissa. Clicking on [Reset] sets them to the values specified in [Parameters]-[Default Parameters]-
[Graph].
[Scale] (Furnace)
You can change the scales for [Absorbance], [Time] and [Temperature]. Enter the maximum value and
minimum value in [Max] and [Min], respectively. Clicking on [Reset] sets the absorbance scale to the
values specified in [Parameters]-[Default Parameters]-[Graph], and sets the time and temperature scales
according to the furnace program.
[Color]
You can select colors of [Data Line], [BG Line], [Background] and [Grid] (also [Furnace Program] for
furnace method). Click on the [ ] button and select the color from the list.
[Grid]
You can select grids to be displayed from [Major & Minor Grid], [Major Grid] or [None]. You can also select
the line type of [Major Grid Line] and [Minor Grid Line].
(2) [Copy]
Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor
or other application and move the cursor to the location where you want to paste the graph. Select [Paste]
command in the word processor, etc., and the graph will be displayed at the cursor position.
(3) [Cross Hair] (Furnace)
This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then
select [Cross Hair]-[Display] in the right button menu. When the mouse cursor is in the graph area, the
coordinate values at the cross hair intersection position are displayed.
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and
select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted).
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock]
condition.
(4) [Radar]
The display range is automatically set so as to display the entire graph selected by the mouse cursor.
(5) [Print]
Selecting this opens the [Print] dialog box. Check the printer name, copies, etc. and click on [OK]. The real
time waveform currently displayed will be printed.

AA-6800/6650 Instruction 4-43


Chapter 4 Basic Operation

4.6.6 Peak Profile (Latest Four Measurements and Overlay Display)


The latest four measurement signal profiles are displayed. Both standard samples and unknown samples are
displayed here. The abscissa shows time and the ordinate shows absorbance value (emission intensity in
EMISSION mode).
The signal profile is displayed during the integral time in the case of flame method, and during the pre-stage
time and sampling time in the case of furnace method.
In the rightmost area, plural number of signal profiles can be overlapped and displayed. Specify their colors in
the [Graph] on the MRT worksheet.

Right mouse button menu


If you want to change the scale or print the graph, place the cursor in the graph area and click on the right
button of the mouse. Then the pop-up menu shown in Figure 4.35 appears. Select an item and make settings.

Figure 4.35 Right Mouse Button Menu (Peak Profile)

(1) [Properties]
[Scale]
You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales.
The scale setting is used commonly for the five graph. Clicking on [Reset] sets the Y-axis to the value
specified in [Parameters]-[Default Parameters]-[Graph].
[Color]
You can select colors of [Data Line], [BG Line], [Background] and [Grid]. Click on the [ ] button and select
the color from the list.
[Grid]
You can select grids to be displayed from [Major & Minor Grid], [Major Grid] or [None]. You can also select
the line type of [Major Grid Line] and [Minor Grid Line].
(2) [Draw BG Line]
Selecting this displays a profile of background signal. The display is deleted by selecting this menu again
(The check mark of [Draw BG Line] is deleted).
(3) [Copy]
Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor
or other application and move the cursor to the location where you want to paste the graph. Select [Paste]
command in the word processor, etc., and the graph will be displayed at the cursor position.

4-44 AA-6800/6650 Instruction


4.6 Explanation of Main Window

(4) [Cross Hair]


This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then
select [Cross Hair]-[Display] from the right button menu. When the mouse cursor is in the graph area, the
coordinate values at the cross hair intersection position are displayed.
The graph area is divided into five areas, and the coordinate values can be read only in each area. If you
want to read an coordinate value in another graph, erase the cross hair cursor once by clicking the right
mouse button and selecting [Cross Hair]-[Display] (then the check mark of [Display] will be deleted), then
set the mouse cursor to another area and select [Cursor]-[Display] again.
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and
select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted).
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock]
condition.
(5) [Radar]
This automatically sets the display range so that the selected graph by the mouse cursor is displayed in an
appropriate size. At the same time, other four data scales are also changed to the same scale.
(6) [Print]
Move the mouse cursor to the graph area to be printed. Then the [Print] dialog box appears. Check the
printer name, copies, etc. and click on [OK]. Only the selected peak profile will be printed.

4.6.7 Calibration Curve Display


After the standard samples are measured, the calibration curve is created and displayed.
1. Calibration Curve Display
If you want to check a calibration curve other than the currently displayed one, set the [Latest] button to
OFF (the button is embossed) and enter the element name and calibration curve number (C#). The
settings here are limited to display and recalculation is not executed.
2. Changing the Calibration Curve Conditions
If you want to change the calibration curve parameters after viewing the created calibration curve, use the
[Type] button. Clicking on [Type] opens the [Change Calibration Curve Condition] dialog box where you
can change order of calibration curve and permission of zero intercept.

Figure 4.36 [Change Calibration Curve Condition] Dialog Box

Changing the condition and clicking on [OK] immediately recalculates the concentration of unknown
samples based on the new calibration curve and renews the quantitation result on the MRT worksheet.

AA-6800/6650 Instruction 4-45


Chapter 4 Basic Operation

The recalculation is only applied to the unknown sample using the same C# as changed calibration curve.
The result is invalid when the element is different, or when the C# is different even if the element is same.
In the case of furnace method, whether the absorbance is obtained from the peak height or from the peak
area is switched in this window.

NOTE
After the data evaluation based on the QA/QC setup is executed, the calibration curve order, zero intercept
and signal processing mode settings cannot be changed after the measurement. For details on QA/QC
setup, refer to section 5.6.9.

Symbols in Calibration Curve Equation


When a calibration curve is created, calibration curve equation is displayed above the graph.
Symbols in a calibration curve equation mean as follows;

Symbol Meaning

Abs Absorbance

E Energy (Only for EMISSION mode)

Conc Concentration

r Correlation coefficient

e When a coefficient is very small, this symbol is used to express it by using index.
"AeB" means "A u 10 B"

^ This symbol means power.


"Conc^2" means the second power of concentration.

(Example)
Calibration curve equation <1> means equation <2>.
Abs = -9.5e-005Conc^2 + 0.011636Conc + 0 ...................................... <1>
Abs = -9.5 u 10-5 u Conc2 + 0.011636 u Conc + 0............................... <2>

Right mouse button menu


If you want to change the scale or print the graph, place the cursor in the graph area and click on the right
button of the mouse. Then the pop-up menu shown in Figure 4.37 appears. Select an item and make
settings.

Figure 4.37 Right Mouse Button Menu (Calibration Curve Display)

4-46 AA-6800/6650 Instruction


4.6 Explanation of Main Window

(1) [Properties]
[Scale]
You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales.
Enter the values.
[Options]
You can set the graph color and data point shape. Clicking on each [ ] of [Data Point], [Calibration
Curve], [Background] and [Grid] displays the list from which you can select the color. The shape of [Data
Point] can be selected from the list displayed by clicking on the [ ].
[Grid]
You can select grids to be displayed from [Major & Miner Grids], [Major Grid] or [None]. You can also select
the line type of [Major Grid Line] and [Minor Grid Line].
(2) [Copy]
Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor
or other application and move the cursor to the location where you want to paste the graph. Select [Paste]
command in the word processor, etc., and the graph will be displayed at the cursor position.
(3) [Cross Hair]
This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then
select [Cross Hair]-[Display] from the right button menu. When the mouse cursor is in the graph area, the
coordinate values at the cross hair intersection position are displayed.
To erase the cross hair, select [Cross Hair]-[Display] (then the check mark of [Display] will be deleted).
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and
select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted).
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock]
condition.
(4) [Radar]
This automatically sets the display range so that the entire graph can be displayed.
(5) [Print]
Move the mouse cursor to the graph area to be printed. Then the [Print] dialog box appears. Check the
printer name, copies, etc. and click on [OK]. Then the calibration curve currently displayed is printed out.
This menu is not displayed when no calibration curve exists.

4.6.8 MRT Worksheet


It is possible to create measurement sequence, execute measurement, display the result, and calculate the
actual concentration in the MRT worksheet. If measurement of plural elements is required, the worksheet is
prepared for each element and the worksheets can be changed over with the tab. In [Summary], the
measurement result for sample can be displayed at one time. The tab title consists of the element name and
comment. As the comment, only the first line is displayed when a line feed is included in the comment, and the
first ten characters are displayed when the number of characters exceeds ten. The comment is inputted by
selecting [Parameters]-[Edit Parameters]-[Comment] page from the menu bar.
For details on each item in MRT worksheet, refer to section 4.7.

NOTE
The currently measured element (or the element about to be measured) can be changed not by the tab at
the left lower of the main window but by the measurement element tool bar.

AA-6800/6650 Instruction 4-47


Chapter 4 Basic Operation

4.6.9 Function Buttons


Functions of Wizard selection, auto zero execution, blank measurement, starting sample measurement, test
measurement, ASC rinse are assigned to the buttons at the left below the MRT worksheet. These correspond
to function keys on the keyboard as follows.
[AUTO ZERO] button: F3 key
[BLANK] button: F4 key
[START] button: F5, F6 keys This switches to [STOP] button during measurement.
[TEST MEAS.] button: F9 key
[RINSE] button: F10 key
The relations between the current measurement mode and the available buttons are shown below.
"Auto (using ASC)" means the status where the ASC is connected and the [Using ASC] check box is check-
marked in [Parameters]-[Edit Parameters]-[Sequence] page from the menu bar.

Flame Auto Furnace Auto


Flame Manual Furnace Manual
(using ASC) (using ASC)

AUTO ZERO

BLANK

START

TEST MEAS.

RINSE

= Available = Not available

Clicking on [AUTO ZERO] button executes the Auto Zero while rinsing the nozzle in the case of flame auto-
measurement (using ASC). In other cases, only the Auto Zero is executed.
When clicking on [RINSE] button, the nozzle and mixing port (mixing port is rinsed only when [Mixing] is ON)
are rinsed in the case of furnace measurement. In the case of flame measurement, nozzle rinse is executed.
The nozzle rinse time in flame measurement is set in [Configuration] dialog box opened by selecting
[Instrument]-[Configuration] from Menu. If the setting is "0", 10 seconds rinse is executed regardless the setting.
Clicking on [STOP] stops the measurement. However, while acquiring the data, the measurement is stopped
after the data acquisition is finished.

4-48 AA-6800/6650 Instruction


4.6 Explanation of Main Window

4.6.10 Status Bar

<1> <2> <3> <4> <5> <6> <7> <8>

Figure 4.38 Status Bar

The current measurement mode, operating mode, operating status of instrument, and connecting status of
peripheral equipments (ASC, GFA) are indicated here.
(1) Displays current operating status of the instrument and error messages.
(2) Displays the hollow cathode lamp which is currently lit and its socket number. While the lamp is lit, the
pane pops up.
(3) Displays the hollow cathode lamp which is under warming-up and its socket number. While the lamp is lit,
the pane pops up.
(4) Displays whether the deuterium lamp is lit or not. When the lamp is lit, the pane pops up.
The [Lamp Status] dialog box can be displayed from the [Lamp Status] menu displayed by clicking the right
mouse button in the regions of <2> to <4>.
(5) Displays whether the ASC is connected. When it is connected, "ASC" is displayed.
(6) Displays whether the GFA is connected. When it is connected, "GFA:n" is displayed. The "n" indicates the
heating number of the graphite tube.
When the current measurement mode is "furnace", the [Change Graphite Tube] dialog box can be
displayed from the [Change Graphite Tube] menu displayed by clicking the right mouse button in this
region.
(7) When a gas leak check is executed at the time of initialization or by selecting [Instrument]-[Gas Leak
Check] menu from the menu bar, the countdown before the gas leak check completion and its result are
displayed. When the current measurement mode is "furnace", however, they are not displayed.
The [Gas Controller Status] dialog box can be displayed from the [Gas Controller Status] menu displayed
by clicking the right mouse button in this region.
(8) Displays the current connecting status of the instrument.
OFF The communication between the instrument and the PC is off.
READY The instrument is ready to execute commands or conduct measurement.
BUSY The instrument is executing a command. While this is displayed, another command cannot be
executed.

AA-6800/6650 Instruction 4-49


Chapter 4 Basic Operation
4.7 Operating the MRT Worksheet

In the MRT (Measurement Result Table) worksheet, the functions of setting of measurement sequence,
execution of measurement, result display, actual concentration calculation, and setting of ASC sample position
are integrated.
For example, if you create a calibration curve by measuring three standard samples and measure eight
unknown samples, the measurement proceeds in the following procedure.
Row 1 to 3: Executes measurement of standard samples.
Row 4 to 11: Executes measurement of unknown samples (SAMPLE001 to SAMPLE008)
As the measurement procedure, prepare the sample shown in the [Action] column and click on [START]. You
can make the measurement in the order from top row to down.
When a repeat measurement is set, rows for repetition are inserted at the time of measurement.

4.7.1 Fields of MRT Worksheet


This section explains about the fields of MRT worksheet.

Figure 4.39 MRT Worksheet

(1) [Action]
Clicking on the cell in this field opens the drop-down list, showing the following indications. This [Action]
field contains the measurement operations, operation using the ASC, QA/QC operation, etc. For details on
QA/QC, refer to section 5.6.9.

NOTE
1. Executing "FILESAVE" overwrites and saves the file even if the file of the same name exists.
2. When the path name is not set at all in [FILESAVE] or [FILEEXPORT], a path name is created based on
the setting in [File]-[Auto Save]. When only the file name is set, the file is saved in the folder that was
used in the last time for [Open] or [Save as] screen.
3. To enable the QA/QC actions, it is necessary to put a check mark in the check box of each QC type in
the [QA/QC Setup] page.

4-50 AA-6800/6650 Instruction


4.7 Operating the MRT Worksheet

Figure 4.40 Drop-down List of [Action]

BLK: Specifies the blank sample measurement. The measured value of blank sample is
subtracted from the measured values of standard samples and unknown samples until a
new blank measurement is done.
STD: Specifies the standard sample measurement by calibration curve method.
UNK: Specifies the unknown sample measurement by calibration curve method.
CAL-CHK: Specifies the evaluation of calibration curve after the standard sample measurement (the
correlation coefficient is checked). This is usually inserted to the row just after the last
"STD". This setting is not necessary in the case of standard addition method or simple
standard addition method because the evaluation is done at "MSA-RES" row.
QC: Specifies the measurement and evaluation by LCS (Laboratory Control Sample/Standard
substance).
SPIKE: Specifies the measurement and evaluation by SPK (Pre-Digestion Spike/ addition and
recovery check without pretreatment). This is usually inserted to the row just after the
objective "UNK".
RESLOPE: Specifies the measurement for sensitivity correction (Usually, the standard sample of
highest concentration is used). After this, "A, B, C..." is added to C# on the MRT and a
new calibration curve number (C#) is created.
MSA: Specifies the measurement by standard addition method.
SMSA: Specifies the unknown sample measurement by simple standard addition method.
MSA-RES: Specified as the result of standard addition method. When the measurement of a set of
standard addition samples is finished, the calibration curve is created and the result is
indicated in this row at the same time.
AUTOZERO: Shifts the current displayed value to zero. In the case of flame measurement using the
ASC, the Auto Zero can be executed while suctioning the sample. The suction time in
second unit can be specified in [Sample ID] field (0 to 600 seconds).
RINSE: In the case of furnace measurement, the nozzle and mixing port are rinsed (mixing port is
rinsed only when [Mixing] is ON).
In the case of flame analysis, the nozzle is rinsed when the ASC is used. The rinse time (0
to 600 seconds) in second unit can be specified in [Sample ID] field.
CLEANING: Specifies cleaning of the graphite tube.
PAUSE: Specifies temporary stop until [OK] is selected. Input a message to be displayed on the
message box in the [Sample ID] field.
WAIT: Specifies a stop in a fixed time. Input waiting time in the unit of second in the [Sample ID]
field (0 to 7200 seconds).
COMMAND: Specifies execution of command line. Specify the command to be executed in the
[Sample ID] field.

AA-6800/6650 Instruction 4-51


Chapter 4 Basic Operation

FILESAVE: Specifies the file saving of the data collected so far. Specify the file name in the [Sample
ID] field.
FILE EXPORT: Specifies the text file saving of the data collected so far on the MRT worksheet. Specify
the file name in the [Sample ID] field.
(2) [Sample ID]
In normal operation, sample ID is entered in this field. Sample name can be entered only when [Action]
field indicates measurement of standard sample or unknown sample (STD, UNK, BLK, QC, SPIKE,
RESLOPE, MSA, SMSA and MSA-RES). When the [Action] is CAL-CHK, the sample name cannot be
entered.
When the Element Selection Wizard or Schedule Creation Wizard was executed, the sample name set in
the [Sample ID] page is entered when [Action] is unknown sample. When the [Action] is standard sample,
the name automatically given in the [Edit Preparation Parameters] dialog box (STD1, STD2,...) is entered.
In the following six cases, the [Sample ID] has a special meaning.
1. When [RINSE] is set in flame auto-measurement (using ASC), enter the suction time in second unit (0
to 600 seconds) in this [Sample ID].
2. When "PAUSE" is set, enter the message to be displayed on the message box in this [Sample ID].
3. When "WAIT" is set, enter the wait time of second unit in this [Sample ID] (0 to 7200 seconds).
4. When "COMMAND" is set, describe the command line in this [Sample ID].
5. When "FILESAVE" is set, enter the file name together with path to save the data measured so far (e.g.
C:\AA\WATER CU.aa). Use ".aa" for extension.
6. When "FILEEXPOPRT" is set, enter the file name together with path. Then the data on the MRT
worksheet data of the currently measured element is saved in a text file (e.g. C:\AA\sWATER_CU.txt).
Use ".txt" for extension.
(3) [Graph]
When overlaid the peak profiles, click on the right part of the cell and select the color of data lines from the
list. The overlaid profiles are displayed on the rightmost of peak profile area. On the other hand, the BG
lines are overlaid by the same one color.
(4) [X] (Exclusion)
Double-clicking this excludes the data in the row. Double-clicking again enables the data to be recovered.
(5) [M] (Modified)
Rewriting the absorbance data after measurement displays M mark (Modified). Once rewritten, this check
mark is always displayed and the original data cannot be recovered. Only absorbance can be written.
(6) [Q]
When the control standard which is set by selecting [Parameters] - [Edit Parameters] - [QA/QC Setup]
page from the menu bar is applied to the row, a check mark is indicated. Marked data cannot be excluded
or modified.
For details on [QA/QC setup] page, refer to section 5.6.9.
(7) [True Value (and unit)]
The set concentration (and unit) of standard samples is indicated. This can be entered only when the
[Action] is STD, SPIKE, RESLOPE, QC or MSA. In the case of "SPIKE", enter the added concentration.
(8) [Conc. (and Unit)]
Displays the result of concentration obtained with measurement. As the [True Value] column heading, the
unit specified in the [Preparation Parameters] page is automatically displayed.

4-52 AA-6800/6650 Instruction


4.7 Operating the MRT Worksheet

(9) [Abs.]
Displays the measured absorbance. Energy intensity is displayed instead in the case of EMISSION mode.
If a blank measurement is executed prior to this, the value is indicated after the measured blank value is
subtracted from the actual measured value.
(10) [BG]
For measurement in BGC-D2 or BGC-SR mode, absorbance of background signal is displayed. This is not
displayed in the lamp modes in which the background signal is not acquired.
When [Peak Height] is selected for signal processing mode in furnace measurement, this field indicates the
background value at the time of acquisition of the absorbance signal peak.
(11) [Pos.]
Indicates the sample position in the turntable of the autosampler (ASC). For details, refer to the instruction
manual provided with the ASC.
(12) [VOL] [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] [Total Volume]
These are sample and reagent volume values necessary for sample mixing using ASC in furnace
measurement. The values set in [STD Samples] or [Unknown Samples] preparation parameters table in
the [Edit Preparation Parameters] dialog box are displayed here. The header row of [Diluent] [Reagent 1]
[Reagent 2] [Reagent 3] displays the settings in [Diluent/Reagent Name & Position] which are set in
[Parameters]-[Edit Parameters]-[ASC Parameters] page from the menu bar.
(13) [WF] [VF] [DF] [ASC DF] [CF]
Each acronym means as follows.
[WF] [Weight Factor]
[VF] [Volume Factor]
[DF] [Dilution Factor]
[ASC DF] [ASC Dilution Factor]
[CF] [Correction Factor]
These are factors necessary for actual concentration calculation. The factors set in [Weight Correction
Factors] in the [Edit Preparation Parameters] dialog box are displayed.
For details on the equation of actual concentration calculation, refer to section 5.5.2.1.
The [ASC DF] is displayed only in the case of furnace auto-measurement using ASC. The dilution factor of
automatic dilution is displayed when the automatic dilution and remeasurement is performed.
(14) [Actual Conc.]
Indicates the result of actual concentration calculation. For the calculation, the factors of WF, VF, DF and
CF are used.
(15) [Actual Conc. Unit]
Enter the unit used for actual concentration of the sample. Clicking on the right part of the cell opens the
drop-down list from which the unit can be selected. Note that changing this unit does not recalculate the
actual concentration. It is necessary to change the factors used for calculation.
(16) [%RSD] [SD] [%R]
The [%RSD] and [SD] are calculated in repeat measurement.
The [%R] is calculated when "QC" or "SPIKE" is measured.
For details on these calculation equations, refer to sections 5.6.2 and 5.6.9.

AA-6800/6650 Instruction 4-53


Chapter 4 Basic Operation

(17) [C#]
Indicates calibration curve number. When plural calibration curves are created on the same sheet, number
is put in the order of creation and indicated.
If entering a changed number, in the case of standard sample, a calibration curve is created by the
standard samples of the same curve number and in the case of unknown sample, the concentration is
calculated using the calibration curve of the entered number. This can be entered when the [Action] is
STD, UNK, CAL-CHK, QC, SPIKE, RESLOPE, MSA or SMSA.
This number is also used when selecting the calibration curve to be displayed (refer to 4.6.7).
(18) [Out of Control Remark]
A note is displayed when QA/QC function judges that the acquired data is out of standard range.
(19) [Date]
Displays the date when the data was obtained by measurement.
(20) [Time]
Displays the time when the data was obtained by measurement. In the case of repeat measurement, the
time displayed in the average row is the time of the first measurement.

4.7.2 Right Mouse Button Menu


Clicking on the right mouse button on the MRT worksheet opens the pop-up menu as below (Figure 4.41).

Figure 4.41 Right Mouse Button Menu (MRT Worksheet)

(1) [Properties]
[Table Show/Hide]
You can select to show or hide each column on the MRT worksheet. Only check-marked items are
displayed. Click on the item you don't want to show, and erase the check mark. The show/hide selection for
each column has no relation to the print items in the [File]-[Print Table Data]. To select the items to be
printed in Table Print, select [File]-[Print Style] from the menu and select the items in [Table Show/Hide]
page.
When the ASC is set not to be used in the [Parameters]-[Edit Parameters]-[Sequence], the items related to
ASC such as [Pos.], [VOL], [Diluent], [Reagent 1], [Reagent 2], [Reagent 3], [Total Volume] and [ASC DF]
are not shown or printed, even if these items are set to be shown or printed in the [Table Show/Hide] page.

4-54 AA-6800/6650 Instruction


4.7 Operating the MRT Worksheet

Figure 4.42 Table Show/Hide (MRT worksheet)

[Row Style]
Font (character style, size, etc.), color and ruled line type can be set for each row group (row and column
header, basic style, current row, measurement result row and excluded row).

Figure 4.43 Row Style (MRT Worksheet)

AA-6800/6650 Instruction 4-55


Chapter 4 Basic Operation

(2) [Hide Repetition]


When this is selected in the case of repeat measurement, only the row of average value is shown and the
rows of repeating process are not shown. The repetition rows are not printed by selecting [Print Table
Data], either. While this is selected, a check mark is indicated in the drop-down menu.
(3) [Hide Excluded Row]
When this is selected, a row with a check mark in its [X] (excluded) field is not shown. The excluded rows
are not printed by selecting [Print Table Data], either.
(4) [Hide Blank]
When this is selected, a row of blank measurement is not shown. The blank rows are not printed by
selecting [Print Table Data], either.
(5) [Hide Command Row]
When this is selected, a row whose [Action] field is "Command" is not shown. The command rows are not
printed by selecting [Print Table Data], either.
(6) [Keep Meas. Row Visible]
When this is selected, the MRT worksheet is automatically scrolled as the measurement proceeds so that
the row under measurement may be always displayed.
(7) [Add Successive No. to Meas.]
Selecting this puts successive numbers to "UNK" and "SMSA" of [Action]. This setting also has an effect on
[Print Table Data].
(8) [Remeasure Selected Range]
When excluding measured rows and remeasuring the sample, the operation is as follows.
1. First, select rows to be remeasured by using the mouse (Click the first row and drag to the last row
while pressing the button). In the case of repeat measurement, the selected range must include the
average row. A row (or sample) that is already excluded cannot be remeasured. If remeasuring the
excluded row is necessary, double-click the [X] field to recover it once.
2. Click the right mouse button and select [Remeasure Selected Range] from the displayed menu.
3. The remeasurement rows are added below the last measured row on the MRT worksheet. The rows in
the selected range are marked in the [X] fields and excluded.
(9) [Collective Edit]
To change the factors and unit for actual concentration calculation together which are already set on the
MRT worksheet, follow the procedure described below.
1. Select the cell range to be changed by using the mouse (Click the first row to be changed and drag to
the last row while pressing the button).
2. Click the right mouse button and select the [Collective Edit] from the displayed menu. Then the
[Collective Edit] dialog box appears. Put a check mark to the check box of each item to be changed.
Enter a new setup value to the item with the check mark.

4-56 AA-6800/6650 Instruction


4.7 Operating the MRT Worksheet

Figure 4.44 [Collective Edit] Dialog Box


(In the case of flame measurement, [Volume] and [Coating] are not displayed.)

3. When completed, click on [OK] to close the [Collective Edit] dialog box. Settings are changed and the
actual concentration is recalculated simultaneously and the worksheet is renewed.
In rows already measured, however, [Volume] and [Coating] cannot be edited.

4.7.3 Right Mouse Button on Summary Table


Clicking on the right mouse button on the summary table displays the pop-up menu where you can select
[Show/Hide of Absorbance], [Concentration], [Actual Concentration] and [Concentration Unit]. This show/hide
selection is also used for [Print Table Data].

4.7.4 Inserting and Deleting the Measurement Row


Only the row that has not been measured can be inserted or deleted for measurement.
To insert the row:
(1) Click on the number of row position to be inserted (a new row is added above the row).
(2) Select [Edit]-[Insert Row] from the menu bar.
To delete the row:
(1) Select the number of row (or the range of plural rows) to be deleted.
(2) Select [Edit]-[Delete Rows] from the menu bar.

NOTE
Insertion and deletion of a row next to current measuring row can't be done during measurement.

AA-6800/6650 Instruction 4-57


Chapter 4 Basic Operation

4.7.5 Active Cell Movement by Shortcut Key and Cell Selection


4.7.5.1 Moving an Active Cell
Clicking a cell with the mouse pointer displays a bold frame around the cell. The cell in this status is called an
active cell. However, all the cells cannot be activated. Some cells can be activated but others cannot be.
The active cell can be moved through the following key input.
Home
This key moves the active cell to the leftmost cell that can be active in the current row.
End
This key moves the active cell to the rightmost cell that can be active in the current row.
Ctrl + Home
These keys move the active cell to the leftmost cell that can be active in the first row unexecuted.
Ctrl + End
These keys move the active cell to the rightmost cell that can be active in the last measurement row.
Tab
This key moves the active cell to the right. After moving to the rightmost cell, it moves to the leftmost cell in the
next row below. It skips a cell that cannot be activated and moves to the next cell.
Shift + Tab
These keys move the active cell to the left. After moving to the leftmost cell, it moves to the rightmost cell in the
upper row. It skips a cell that cannot be activated and moves to the next cell.

4.7.5.2 Selecting Cells


Using the mouse can select contiguous plural cells as described below.
Cell range
Click the cell in the upper left corner of the region to be selected and drag to the cell in the lower right corner.
Column
When selecting a column, click the column header of the column to be selected. When selecting contiguous
plural columns, drag along the column header.
Row
When selecting a row, click the row header of the row to be selected. When selecting contiguous plural rows,
drag along the row header.
Whole table
Click the upper left cell of the header. Then all of the rows entered on the table are selected.

4-58 AA-6800/6650 Instruction


4.7 Operating the MRT Worksheet

4.7.6 Copy and Paste


Numeric values and characters on the MRT worksheet and summary table can be copied to the clipboard. Also,
text data can be pasted from the clipboard only to the sample ID column in the MRT worksheet.

4.7.6.1 Copy
Select an area on the table to be copied using the mouse and select [Edit]-[Copy] menu or press Ctrl + C key.
Then the values in the selected area are copied to the clipboard. These copied values can be pasted as text
data to the word processor or spreadsheet software.

NOTE
1. The contents of column header and row header are not copied.
2. Graph column is never copied.
3. Hidden column is not copied.
4. Hidden row included in the selected area is always copied.

4.7.6.2 Paste
Text data can be pasted from the clipboard to the sample ID column.

Copy & Paste of Sample ID between MRT Worksheets


1. Select a cell area of sample ID as the copy source and copy it to the clipboard by [Edit]-[Copy] menu or Ctrl
+ C key.
If hidden rows are included in the selected area, the contents of the sample ID cells in the hidden rows are
also copied. Therefore, set all the rows displayed and check the contents to be copied before executing the
copy.
2. Click the top cell of the sample ID cell area in the paste destination. Note that paste is not applied to the
rows already measured or rows under repeat measurement.
3. Select [Edit]-[Paste] menu or press Ctrl + V key in this status. Then the sample ID is overwritten on the
cells from the top cell to down.
4. When the number of sample ID in the copy source is over the number of rows in the paste destination, the
excess are added as new rows.

NOTE

1. If a value other than numeric value is pasted to the items for which time should be set in the sample ID
field (WAIT, AUTO ZERO or RINSE at the use of ASC), it is reset to "0". Numeric values out of the
acceptable entry range are also ignored.
2. If the paste is applied to the items for which nothing can be entered in sample ID field (CAL-CHK, etc.),
it is ignored.
3. Also, sample IDs created using a word processor or spreadsheet software can be pasted to the MRT
worksheet. When creating sample IDs using a word processor, insert a line feed between the sample
IDs. Also, the sample ID must not contain the tab code.

AA-6800/6650 Instruction 4-59


Chapter 4 Basic Operation

4.7.7 Changing Column Width and Column Header Height of MRT


Worksheet
The column width for an arbitrary column and the column header height can be changed in the MRT worksheet.

Procedure for setting the column width


(1) Position the mouse cursor on the column border line in the column header. The mouse shape changes to a
two-direction arrow.
(2) While the mouse cursor is in the two-direction arrow status, press the left mouse button down and drag to
the right or left. The cell width of the column header is changed.
(3) Release the left mouse button at the appropriate position. The column width is set at the position.

Procedure for setting the column header height


(1) Position the mouse cursor on the bottom line of the leftmost cell in the column header. The mouse shape
changes to a two-direction arrow.
(2) While the mouse cursor is in the two-direction arrow status, press the left mouse button down and drag
upward or downward. The height of the leftmost cell is changed.
(3) Release the left mouse button at the appropriate position. The column header height is set at the position.

4-60 AA-6800/6650 Instruction


4.8 Igniting and Extinguishing the Flame
4.8 Igniting and Extinguishing the Flame

4.8.1 Operation Locations


Locations associated with igniting and extinguishing of the flame are described here.
Firstly, the IGNITE buttons, EXTINGUISH button and BURNER SELECT switch are located on the front side of
the AA main unit. In addition, operation panel of gas controller is located at the rear of the right side of AA main
unit.

4.8.2 Safety Precautions Prior to Ignition


(1) Switch ON the power for the fan of the room exhaust duct.
(2) Verify that the gas to be used is appropriate and that the gas pressure is set correctly
Gas type Air, N2O, Ar C2H2, H2
Supply pressure 0.35 MPa 0.09 MPa
Setting pressure 0.25 MPa 0.05 MPa
"Supply pressure" is a value indicated by the pressure regulator in the analysis room and "Setting
pressure" is a value indicated by the pressure gauge in the gas controller panel of the AA main unit.
(3) Confirm that the drain tank is filled with water.
(4) Verify that there are no leaks in any of the gas lines (refer to section 6.3).
(5) Verify that the flame and burner head to be used are appropriately matched.
Table 4.2 Type of Burner Heads and Usable Flames

High temperature burner head


Standard burner head
(optional)

Slot length 10 cm 5 cm

Usable flame Air-acetylene Air-acetylene


Air-hydrogen Air-hydrogen
Argon-hydrogen Argon-hydrogen
Nitrous oxide-acetylene

(6) Confirm that a safety plug plate appears normally.

CAUTION
Before igniting a flame, check that the IGNITE buttons work properly.
<Checking procedure>
1. Referring to section 4.1, turn on the power of the instrument.
2. Referring to section 4.2.1.7, initialize the instrument and wait until the 10-minute gas leak check step
after the initialization has finished.
3. Perform Element Selection Wizard of AA software or open a flame measurement file to set the
instrument to flame measurement mode.
4. Press the upper button (black) of the two buttons. When no ignition is executed, it is normal.
5. Next, press the lower button (white). When no ignition is executed, it is normal.
6. If the above step 4 or 5 should ignite a flame, the switch system is broken. Stop using the instrument
immediately.

AA-6800/6650 Instruction 4-61


Chapter 4 Basic Operation

NOTE
If the power is turned on and the fuel gas is supplied at the time of [Connect to Instrument], a gas leak check
is automatically conducted for 10 minutes. During this time, no flame can be ignited. On the [Initialize] dialog
box, press the EXTINGUISH button at the time of [Start Leak Check]. The fuel gas will be filled inside the
pipe of the gas controller by this action. If the EXTINGUISH button is not pressed, buzzer can sound within
10 minutes even if there is no gas leak.
If the buzzer sounds within 10 minutes after starting the gas leak check, stop using the instrument
immediately and perform an inspection (Pressing the BUZZER OFF button in the gas controller to turn off the
buzzer).
In case that a gas leakage is detected, a buzzer sounds immediately after the gas leakage check is started.
The time of 10 minutes is set as a sufficient value for safety, and there is no problem when a buzzer sounds
after 10 minutes or later.
Pressing the PURGE button during the gas leak check will purge the gas from the gas lines and cancel the
gas leak check. To perform the gas leak check next, execute the [Instrument]-[Gas Leak Check] from the
menu. However, if the PURGE button is pressed within 10 minutes after turning on the power and the gas
leak check is to be performed again, press the EXTINGUISH button.
When the PURGE button is pressed, an error message indicating that fuel gas pressure is too low may be
displayed. This message, however, may be ignored.

4.8.3 Igniting and Extinguishing Air-C2H2, Air (Ar)-H2 Flames


(1) Set the fuel gas flow rate in a range listed below. To set the fuel gas flow rate, click on the radio button of
[Fuel Gas Flow Rate] on the [Atomizer/Gas Flow Rate Setup] page and enter a numeric value in [Fuel Gas
Flow Rate] and click on the [Flame Setup] button. You can also use [Increase] or [Decrease] buttons.
Acetylene gas 2.0 - 3.0 (L/min)
Hydrogen gas at least 4.0 (L/min)
(2) Keep the PURGE button pressed, check the support gas (Air) flow rate and adjust it by using the support
gas flow rate control knob so that the scale may indicate "8.0".

CAUTION
The support gas flow meter indicates both the scale for air and the scale for N2O.
Read the proper scale when adjusting the support gas flow rate. Read the flow rate at the center of the ball.

(3) In the case of Ar-H2 flame, it is necessary to invalidate the flame monitor safety device. Since the flame is
colorless, the sensor cannot detect it and stops the gas supply. In the cases other than Ar-H2 flame,
however, be sure to validate the flame monitor safety device. (When the instrument is initialized, the flame
monitor safety device is always valid.)
To invalidate the flame monitor safety device, select [Instrument]-[Gas Controller Status] menu to display
the [Gas Controller Status] dialog box and clear the [Flame Monitor ON] check box.

CAUTION
When the [Flame Monitor ON] check box is cleared, the flame monitor safety device doesn't operate.
Therefore, stay near the instrument and always check that the flame doesn't go out. If the flame should go
out, press the EXTINGUISH button.

4-62 AA-6800/6650 Instruction


4.8 Igniting and Extinguishing the Flame

(4) Press two IGNITE buttons at the same time. A pilot flame is ignited first, then the burner head is flamed.
Keep pressing the IGNITE buttons until the flame is completely ignited.
If no flame is ignited even if the buttons are pressed for three seconds or more, stop igniting operation
once, and retry after ten seconds or more.
When ignition has failed, the AA software may display an error message like "Flame has been
extinguished". When such a message is displayed, the AA main unit is locked so that the igniting operation
cannot be done. To release this lock, close all the error messages displayed on the software.
(5) Set the fuel gas flow rate and support gas pressure and flow rate if necessary.
(6) To extinguish the flame, press the EXTINGUISH button.

NOTE

1. If the gas pressure decreases while the flame is burning, the flame is automatically extinguished. In that
case, check the gas supply pressure before igniting a flame again.
2. If a momentary AC supply power outage should occur, the flame is automatically extinguished.
3. In the following cases, an error message stating that the fuel gas pressure is too low will be displayed,
but this message can be ignored.
a. When the PURGE button is pressed
b. When the flame out safety device is activated because the flame is extinguished due to an obvious
reason (such as wind blowing out the flame, etc.).
c. When the automatic measurement by ASC is completed and the flame is automatically
extinguished according to the setup.
d. When there is a momentary AC power outage.
4. After the error message of too low fuel gas pressure is displayed, the pilot flame is not ignited by
pressing the IGNITE button even if the instrument condition is set ready for ignition. In this case, once
press the EXTINGUISH button then press the IGNITE button.
5. If ignition is attempted when the support gas is not being supplied, or when the support gas pressure is
low, the ignition spark is generated but the flame is not ignited (At this time, as the safety mechanism
functions, the fuel gas does not flow through the burner slot). However, in this case, a low pressure error
message will not be displayed. Therefore, if an error message will not be displayed in spite of
impossible ignition, check the support gas pressure.
6. When the following error messages are displayed on the AA software, the AA main unit is locked so that
ignition cannot be done. To release this lock, solve the problems in the instrument settings then close all
the error messages displayed on the software. While the error message is displayed, no ignition can be
done.
• Fuel gas leak is detected.
• Fuel gas pressure is too low.
• Support gas pressure is too low.
• Flame has been extinguished.
• Drain tank water level is too low.
• Momentary electric shutdown occurred in the gas controller. Forcibly support gas type is
changed to air and flame monitor is set to ON.

AA-6800/6650 Instruction 4-63


Chapter 4 Basic Operation

NOTE
7. If the flame should not be extinguished even by pressing the EXTINGUISH button, do not panic and
take action of following operation.
a. Turn off the main unit POWER switch (on the left side of the main unit). This operation
mechanically closes the solenoid valve of the gas controller, shutting off the gas supply safely.
b. Close the gas main valve.
c. Contact your service representative immediately. Do not operate the instrument until the repair by
service person completes.

4.8.4 Igniting and Extinguishing N2O-C2H2 Flame


(1) Take off the standard burner head (slot length 10 cm) and mount the high temperature burner head (slot
length 5 cm) supplied as an optional accessory.
(2) On the [Atomizer/Gas Flow Rate Setup] page, click on the [Fuel Gas Flow Rate] radio button. Select [N2O-
C2H2] for [Flame Type] and enter the flow rate (7.0 to 8.0 L/min) in the [Fuel Gas Flow Rate] field. Also, the
flow rate can be changed by the [Increase] and [Decrease] buttons.
(3) Insert the burner recognizing key connected to the high temperature burner head with a wire into the hole
of the BURNER SELECT switch.
(4) Press two IGNITE buttons at the same time to ignite the flame. First, the Air-C2H2 flame will be ignited.
Keep pressing the IGNITE buttons until the flame is completely ignited.
If the flame is not ignited even if the buttons are pressed for three seconds or more, stop igniting operation
once, and retry after ten seconds or more.
When the ignition has failed, the AA software may display an error message like "Flame has been
extinguished". When such a message is displayed, the AA main unit is locked so that the igniting operation
cannot be done. To release this lock, close all the error messages displayed on the software.
Approx. 10 seconds after the flame ignition is achieved, the C2H2 flow rate is automatically increased to
5.0 L/min and the flame emission intensity is increased. Then the support gas is automatically switched
from Air to N2O, changing the Air-C2H2 flame to N2O-C2H2 flame.

NOTE
Even if the [Flame Type] is set to N2O-C2H2, the flame will not be switched unless the BURNER SELECT
switch is set to N2O-C2H2 with a key attached to the high temperature burner head. In this case, if the
BURNER SELECT switch is changed from the Air-C2H2 to the N2O-C2H2 position while Air-C2H2 is flaming,
the support gas is automatically switched from Air to N2O, changing the Air-C2H2 flame to N2O-C2H2 flame.

(5) To extinguish the flame, press the EXTINGUISH button. The support gas is automatically switched from
N2O to Air, changing the N2O-C2H2 flame to Air-C2H2 flame. Then the flame is extinguished.

4-64 AA-6800/6650 Instruction


4.8 Igniting and Extinguishing the Flame

CAUTION
1. Always use high temperature burner head when using a nitrous oxide-acetylene flame. Using the
standard burner head with this gas causes a danger of flashback.
2. When the acetylene flow rate is high, carbon is deposited around the burner slot. When this occurs, use
the provided large screwdriver to scrap off the carbon deposit while taking care about the following
points.
• Insert the screwdriver at the center on the burner slot while keeping the top portion of the
screwdriver lengthwise. Don't close a large part of the burner slot by keeping the top portion
of screwdriver horizontally.
• While keeping the top portion of screwdriver lengthwise, slide it from the center to the
outside (right or left side) and scrap off the carbon deposit gently. To prevent the flame from
going out, don't slide the screwdriver from the outside to the center. Insert it at the center
again and scrap off to the outside.
• Be careful not to scratch the burner head and slot.
• Remove the carbon deposit inside the burner slot using a piece of hard paper, after the
flame is extinguished and the burner is completely cooled.

Carbon deposit

High temperature burner head

Figure 4.45 Removing Carbon Deposit in N2O-C2H2 Flame

3. When using a nitrous oxide-acetylene, decreasing the acetylene or increasing the nitrous oxide will
cause the pink portion of the flame (red feather) to gradually decrease. If this decreases to less than
2 mm, the flame will split, and if the acetylene flow is further reduced, a flashback may occur.

Blue

Pink (Red feather)

Dark blue

Figure 4.46 N2O-C2H2 Flame

AA-6800/6650 Instruction 4-65


Chapter 4 Basic Operation

CAUTION
In case of flashback, set the safety valve at the back of the chamber as it was if it is out of place. Also,
remove the spray unit to check it and if the disperser is separated, mount it as it was. Check the tube from
the drain outlet is firmly connected.

4.8.5 Flame Conditions When Analyzing Organic Solvent Samples


Since an organic solvent itself will burn in the flame, the flame will not be completely combusted using the
normal flame conditions, as the result, the measurement accuracy will be decreased. To perform an accurate
measurement, it is necessary to decrease the sample spray amount as well as decrease the acetylene gas flow
rate, compared with the aqueous solution. The procedure for setting the flame conditions when using organic
solvent is as follows.

(1) Replace the suction nozzle with the provided polyethylene capillary tube.
(2) While solvent is being sprayed into the flame, decrease the acetylene gas flow rate so that the color of the
flame is from blue or slightly red (in the case of air-acetylene flame). Next, while organic sample is being
sprayed, try various acetylene flow rates and burner heights until the maximum S/N ratio (signal to noise
ratio) is achieved.
(3) Overly decreasing the acetylene flow may cause the flame to go out when spraying of the organic sample
is stopped. In this situation, increase the acetylene gas flow rate in 0.1 L/min increments until the flame no
longer goes out at the end of spraying the organic solvent sample, and then adjust the flame condition by
increasing the support gas flow rate. When using a nitrous oxide-acetylene flame, be sure that the red
feather (red portion of the flame) is more than 2 - 3 mm.
If a stable flame is not achieved after performing the above procedure, continue with the steps (4) to (6)
outlined below, and then search for the optimal flame conditions using steps (2) to (3) again.
(4) Return the acetylene flow rate to its normal value.
(5) Rotate the support gas pressure adjusting knob so that the support gas pressure is in the range of 0.1 to
0.25 MPa, and decrease the amount of sample sprayed.
(6) Increase the support gas flow rate by rotating the support gas flow adjusting knob to approach the flow rate
used prior to decreasing the support gas pressure.

4-66 AA-6800/6650 Instruction


4.9 Standard Addition Method and Simple Standard Addition
4.9 Standard Addition Method and Simple Method
Standard Addition Method

The standard addition method is used when there is interference by coexistent material (matrix) in the sample
and its influence is given to the measured value. For the standard addition method, equal volumes of unknown
sample solution are prepared, and a standard solution of different but known concentration is added to each of
the unknown sample solutions. The absorbance is measured for each of these samples, and a calibration curve
is created. The unknown sample concentration is obtained from the point at which the extended calibration
curve intersects with the horizontal axis.

Absorbance

Standard addition concentration


Concentration of unknown sample

Figure 4.47 Standard Addition Method

When the coexistent material or matrix of plural unknown samples are similar, measure one of them by
standard addition method, and you can use the slope of the same calibration curve to determine the
concentrations of other unknown samples. This is called simple standard addition method.
Absorbance

Sample concentration by simple standard addition method

Figure 4.48 Simple Standard Addition Method

When using these methods, the absorbance of standard addition samples must be within the range that has
linearity of calibration curve. To check whether the result is valid or not, refer to the coefficient of correlation.

AA-6800/6650 Instruction 4-67


Chapter 4 Basic Operation

4.9.1 Setting the [Edit Preparation Parameters] Dialog Box


Note that parameters for "MSA (Method of Standard Addition)" cannot be set using the Wizard. Follow the
procedure below. First, set [Measurement Type] to "SMSA" and [Number of STD] to "1" and finish the settings.
Then set necessary items on the MRT worksheet. In the case of furnace measurement using the ASC, settings
of [Preparation Parameters] are also necessary.

In the case of flame method


When the [Preparation Parameters] page is displayed, first, click on the element row for setup to highlight it and
click on [Edit]. Then the [Edit Preparation Parameters] dialog box opens.
(1) Select "SMSA" for the [Measurement Type].
(2) Setup of [Order] and [Zero Intercept] is not possible. The order is automatically set to the 1st (linear) and
zero is not intercepted.
(3) Select [Conc. Unit]. Click on the [ ] button and select the unit from the list.
(4) Entering [Number of STD] displays the table of [Conc]. Enter the concentrations of standard samples to be
added.
(5) Enter [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] in the field of [Weight
Correction Factors].
(6) When completing the setup, click on [OK]. Then [Preparation Parameters] page is displayed again. When
measuring plural elements, make setup for other elements in the same procedure.

In the case of furnace method


When the [Preparation Parameters] page is displayed, first, click on the element row for setup to highlight it and
click on [Edit]. Then the [Edit Preparation Parameters] dialog box opens.
(1) Select "SMSA" for [Measurement Type].
(2) Setup of [Order] and [Zero Intercept] is not possible. The order is automatically set to the 1st (linear) and
zero is not intercepted.
(3) Select [Conc. Unit]. Click on the [ ] button and select the unit from the list.
(4) Entering [Number of STD] displays a table of [STD Samples] preparation parameters. Enter the
concentrations of standard samples in [Conc.] fields and the volume of unknown sample in the [Unknown
Samples]. When using the ASC to add the standard sample automatically for preparation, regard the
standard sample as [Reagent 3] for setup.
(5) In the case of "SMSA", the [Pos.] in the table indicates the ASC position of unknown sample to which the
standard is to be added.
(6) Enter [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] in the field of [Weight
Correction Factors].
(7) In the case of "SMSA", enter the [Unknown Sample] preparation parameters (sample volume, diluent,
Reagent 1, etc.). In the case of "MSA", this can be ignored.
(8) When completing the setup, click on [OK]. Then [Preparation Parameters] page is displayed again. When
measuring plural elements, make setup for other elements in the same procedure.

4-68 AA-6800/6650 Instruction


4.9 Standard Addition Method and Simple Standard Addition
Method

(Example)
In this example, the ASC is used to add the standard samples of 0 ppb, 10 ppb, 20 ppb and 30 ppb to the
unknown samples which are being diluted 5 times. Standard sample of 100 ppb is prepared for addition
and is regarded as the Reagent 3.
As other conditions, assume that [Mixing] is to be performed, [Injection Volume] is 20 PL, and [No. of
repetition] is 3 ([Max No. of repetition] is 5).
[Sample] must be constant for all the concentrations. Here, assume it is 40 (PL).

[Conc] [Sample] [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] [Total Vol]

0 40 160 0 0 0 200

10 40 140 0 0 20 200

20 40 120 0 0 40 200

30 40 100 0 0 60 200

This [Total Vol] must satisfy the following condition.


[(Injection Volume) u (Max. No. of repetition) u (No. of Boost Cycles) + 50 PL]
d [Total Volume] d 600 (PL)
In this equation, the [Injection Volume] means the [Volume] set in the [Mixing Setup] dialog box. "50 PL"
indicates the dead volume of mixing port. If furnace boost cycle is not performed, (No. of Boost Cycles) is
"1".
Based on settings made up to now, the calculation is as follows:
[(20 PL) u (5 times) u (1 cycle) + 50 PL] d [200 PL] d 600 (PL)
This indicates that the settings are correct.
Assume that unknown samples B and C which have similar matrix components to that of unknown sample
A in the above setup example. These concentrations are calculated using the calibration curve created by
unknown sample A (simple standard addition method). In this case, since the [Sample] is 40 PL and the
[Total Vol] is 200 PL, the [Unknown Sample] preparation parameters are set as below.

[Sample] [Diluent] [Reagent 1] [Reagent 2] [Reagent 3] [Total Volume]

40 160 0 0 0 200

In the [Weight Correction Factors] field, enter 40 (PL) in [Weight Factor] and 200 (PL) in [Volume Factor].
Then the actual concentration before dilution can be calculated.

AA-6800/6650 Instruction 4-69


Chapter 4 Basic Operation

4.9.2 Measurement Procedures on MRT Worksheet


The indication of [Action] on the MRT worksheet related to "SMSA (Simple Method of Standard Addition)" and
"MSA (Method of Standard Addition)" is described below.
MSA: Indicates standard addition method.
MSA-RES: Indicates the concentration of unknown sample calculated from the result of measuring a set of
standard addition samples.
SMSA: Indicates simple standard addition method. Unknown sample is measured using a calibration
curve created by another sample for standard addition method.
In the case of the "Simple standard addition method" setup example described above, the procedure is as
follows.

Table 4.3 Measurement Procedure of Simple Standard Addition Method

[Action] C#

1 MSA (Measures Sample A with standard 0 ppb addition) 01

2 MSA (Measures Sample A with standard 10 ppb addition) 01

3 MSA (Measures Sample A with standard 20 ppb addition) 01

4 MSA (Measures Sample A with standard 30 ppb addition) 01

5 MSA-RES (Indicates concentration result of Sample A) 01

6 SMSA (Measures unknown Sample B) 01

7 SMSA (Measures unknown Sample C) 01

If the samples A, B and C are measured by "MSA", the procedure is as follows.


(1) First, delete the raws No. 6 and 7 in Table 4.3 by selecting [Edit]-[Delete Rows] from menu.
(2) Next, create the raws No. 6 to 15 shown in Table 4.4 newly on the MRT worksheet.

4-70 AA-6800/6650 Instruction


4.9 Standard Addition Method and Simple Standard Addition
Method

Table 4.4 Measurement Procedure of Standard Addition Method

[Action] C#

1 MSA (Measures Sample A with standard 0 ppb addition) 01

2 MSA (Measures Sample A with standard 10 ppb addition) 01

3 MSA (Measures Sample A with standard 20 ppb addition) 01

4 MSA (Measures Sample A with standard 30 ppb addition) 01

5 MSA-RES (Indicates concentration result of Sample A) 01

6 MSA (Measures Sample B with standard 0 ppb addition) 02

7 MSA (Measures Sample B with standard 10 ppb addition) 02

8 MSA (Measures Sample B with standard 20 ppb addition) 02

9 MSA (Measures Sample B with standard 30 ppb addition) 02

10 MSA-RES (Indicates concentration result of Sample B) 02

11 MSA (Measures Sample C with standard 0 ppb addition) 03

12 MSA (Measures Sample C with standard 10 ppb addition) 03

13 MSA (Measures Sample C with standard 20 ppb addition) 03

14 MSA (Measures Sample C with standard 30 ppb addition) 03

15 MSA-RES (Indicates concentration result of Sample C) 03

In this case, three calibration curves are created. When "MSA" is added in the MRT worksheet, C# (calibration
curve number) is automatically allocated. Check that C# corresponds properly to the series of standard addition
samples.

AA-6800/6650 Instruction 4-71


Chapter 4 Basic Operation
4.10 Conditions and Operation for Flame Emission
Analysis

Flame emission quantitative analysis is described here. As the case of atomic absorption analysis, the Wizard
can be used for setup. However, the setup procedures in the [Optics Parameters] and [Atomizer/Gas Flow Rate
Setup] pages are different in some points. Other operations are the same as those of the flame method of
atomic absorption analysis.

4.10.1 [Optics Parameters] Page

Figure 4.49 [Optics Parameters] Page

(1) [Wavelength]
For wavelength used for flame emission analysis, refer to Table 4.5. Enter the numeric value if the
wavelength is different from that for atomic absorption analysis.
(2) [Slit Width]
It is recommended to set the slit width to "0.5 nm".
(3) [Socket #]
Although a lamp is not used, it is necessary to set an arbitrary socket number as a dummy.(Procedure for
dummy setup)
1. Press the [Lamp Pos. Setup] button to display the [Lamp Position Setup] dialog box.
2. For an arbitrary [Socket #], select "*" in the [Element] and "Normal" in the [Lamp Type].
3. Select "Emission" in [Lamp ID]. This lamp ID is a special ID of dummy lamp for flame emission
analysis.
4. Press [OK] to close the [Lamp Position Setup] dialog box and return to the [Optics Parameters] page.
Then select the socket # in which the dummy lamp for flame emission analysis was set.
When performing the line search using a lamp, set a proper lamp in [Lamp Position Setup] dialog box.
(4) [Lamp Mode]
Set the [Lamp Mode] to "EMISSION".
(5) [Lamp Current]
Set [Low] to "0" (zero). When the lamp mode is set to "EMISSION", [High] is automatically set to "0" (zero)
and cannot be entered.

4-72 AA-6800/6650 Instruction


4.10 Conditions and Operation for Flame Emission Analysis

(6) [Line Search]


In the case of flame emission analysis, a line search is performed when the flame has been ignited and the
standard sample is being sprayed. So, the line search is not performed in this page. Proceed to the next
[Atomizer/Gas Flow Rate Setup] page first and set the parameters so that ignition may be possible. After
that, return to this page and perform the line search.
It is also possible to perform a line search using the hollow cathode lamp. In this case, light the hollow
cathode lamp to perform the line search. If the lamp is lit in the EMISSION mode, the lamp is automatically
turned off when [START] is pressed to start the measurement. Don't forget to turn off the lamp, however,
when observing a signal in the [Atomizer/Gas Flow Rate Setup] page while aspirating the sample.
(7) Click on [Next] button to proceed to the [Atomizer/Gas Flow Rate Setup] page first.

Table 4.5 Analysis Line Wavelength Table for Flame Emission Analysis

Element Wavelength (nm) Element Wavelength (nm) Element Wavelength (nm)

Ag 328.1 Hf 531.2 Re 346.1

Al 396.2 Hg 253.7 Rh 343.5

As 193.7 In 451.1 Ru 372.8

Au 267.6 Ho 410.4 Sc 402.4

B 518.0* Ir 550.0 Si 251.6

Ba 455.4 K 766.5 Sm 476.0

Be 234.9 La 442.0 Sn 317.5

Bi 306.8 Li 670.8 Sr 460.7

Ca 422.7 Lu 451.9 Ta 474.0

Cd 326.1 Mg 285.2 Tb 534.0*

Ce 494.0* Mn 403.3 Te 486.6

Co 345.4 Mo 390.3 Ti 334.9

Cr 425.4 Na 589.0 Th 492.0

Cs 455.5 Nb 405.9 Tl 377.6

Cu 324.8 Nd 492.5 U 544.8

Dy 404.6 Ni 352.5 V 437.9

Er 400.8 Os 442.1 W 430.2

Eu 459.4 Pb 405.8 Y 597.2

Fe 372.0 Pd 363.5 Yb 398.8

Ga 417.2 Pr 495.1 Zn 636.2

Gd 622.0 Pt 265.9 Zr 360.1

Ge 265.1 Rb 794.8

*: Band spectrum

AA-6800/6650 Instruction 4-73


Chapter 4 Basic Operation

4.10.2 [Atomizer/Gas Flow Rate Setup] Page


The [Atomizer/Gas Flow Rate Setup] pages are different in AA-6800 and AA-6650.
Refer to the description for your AA type.

4.10.2.1 AA-6800
(1) Firstly, select the [Fuel Gas Flow Rate] for [Operation Object] by clicking on the radio button.

Figure 4.50 [Atomizer/Gas Flow Rate Setup] Page (in the case of [Fuel Gas Flow Rate])

[Flame Type]
Since the flame used for atomic absorption analysis is indicated, click on the [ ] button and select the
flame type used for flame emission analysis. As a flame type used for flame emission analysis, generally,
the high temperature N2O-C2H2 flame is good. However, in the cases of alkaline metals (Na, K, etc.), other
flame (Air-C2H2) is also available for measurement of sufficiently minute quantities. The Air-H2 flame with
low background can also be used effectively for flame emission analysis.

[Fuel Gas Flow Rate]


Since the flow rate for atomic absorption analysis is indicated by default, enter the flow rate value for flame
emission analysis. It is necessary to check the optimum value for each element beforehand. In general, a
low acetylene flow rate is best. When using the N2O-C2H2 flame, adjust the flow rate so that the red feather
(pink portion of flame) is approx. 2 to 3 mm in height.
To obtain the optimum gas flow rate, the function of the [Gas Flow Auto] button is convenient. Use it after
setting the ignition conditions and performing the line search.

4-74 AA-6800/6650 Instruction


4.10 Conditions and Operation for Flame Emission Analysis

(2) Select the [Atomizer Position] for [Operation Object] by clicking on the radio button.

Figure 4.51 [Atomizer/Gas Flow Rate Setup] Page (in the case of [Atomizer Position])

[Burner Height]
Since the value for atomic absorption analysis is indicated by default, enter the optimum value for flame
emission analysis. If the optimum value is not known, as a first step, set it to 7 mm for Air-C2H2, 11 mm for
N2O-C2H2 and 15 mm for Air-H2. Then, after setting the ignition conditions and performing the line search,
obtain the optimum value again.
To obtain the optimum burner position, the function of the [Burner Position Auto] button is convenient.

[Burner Lateral]
This is used to change the position intentionally from the burner origin position set in [Maintenance]. For
example, set a value here to lower the sensitivity of a particular element in full-automatic continuous
measurement of plural elements (this is a substitute for changing a burner angle in manual measurement
to lower the sensitivity).
When simply setting the optimum position of burner lateral, select [Instrument]-[Maintenance]-[Burner
Origin Position Adjustment] from the menu and set [Burner Lateral] to zero.

[Burner Angle]
Set the angle of burner head according to the purpose.
Generally, the S/N ratio is better when the angle is set at 0 degrees for optical axis (parallel) than at 90
degrees, but its linearity may become worse. When the concentration of analysis element is relatively high,
the burner head is used at 90 degrees.

AA-6800/6650 Instruction 4-75


Chapter 4 Basic Operation

4.10.2.2 AA-6650
(1) Firstly, select the [Fuel Gas Flow Rate] for [Operation Object] by clicking on the radio button.

Figure 4.52 [Atomizer/Gas Flow Rate Setup] Page (in the case of [Fuel Gas Flow Rate])

[Flame Type]
Since the flame used for atomic absorption analysis is indicated, click on the [ ] button and select the
flame type used for flame emission analysis. As a flame type used for flame emission analysis, generally,
the high temperature N2O-C2H2 flame is good. However, in the cases of alkaline metals (Na, K, etc.), other
flame (Air-C2H2) is also available for measurement of sufficiently minute quantities. The Air-H2 flame with
low background can also be used effectively for flame emission analysis.

[Fuel Gas Flow Rate]


Since the flow rate for atomic absorption analysis is indicated by default, enter the flow rate value for flame
emission analysis. It is necessary to check the optimum value for each element beforehand. In general, a
low acetylene flow rate is best. When using the N2O-C2H2 flame, adjust the flow rate so that the red feather
(pink portion of flame) is approx. 2 to 3 mm in height.

4-76 AA-6800/6650 Instruction


4.10 Conditions and Operation for Flame Emission Analysis

(2) Select the [Atomizer Position] for [Operation Object] by clicking on the radio button.

Figure 4.53 [Atomizer/Gas Flow Rate Setup] Page (in the case of [Atomizer Position])

[Burner Height]
Since the value for atomic absorption analysis is indicated, enter the optimum value for flame emission
analysis and set the burner height using the knob for adjusting burner vertical position.
The "Burner Height" indicates the distance from the optical axis down to the burner head by a positive
value.
If the optimum value is not known, as the first step, set it to 7 mm for Air-C2H2 and 11 mm for N2O-C2H2.
Then after setting the ignition conditions and performing the line search, obtain the optimum value newly.
To obtain the optimum value, change the burner height while spraying the sample, and search the burner
height so that the real time data profile shows a high and stable sensitivity.

[Burner Angle]
Set the angle of burner head according to the purpose.
Generally, the S/N ratio is better when the angle is set at 0 degrees for optical axis (parallel) than at 90
degrees, but its linearity may become worse. When the concentration of analysis element is relatively high,
the burner head is used at 90 degrees.

AA-6800/6650 Instruction 4-77


Chapter 4 Basic Operation

4.10.3 Line Search and Beam Balance


After completing the condition setup in the [Atomizer/Gas Flow Rate Setup] page, click on [Back] to return to the
[Optics Parameter] page.
Read section 4.8 thoroughly and set the conditions so that a flame can be ignited.

(1) Ignite the flame.


(2) Start spraying the standard sample of the highest concentration. If the sample position of the highest
concentration standard sample on ASC turntable is set to the [ASC Sample Pos. for EMISSION Line
Search], the automatic spray using the ASC is possible.
(3) While spraying the sample, click on the [Line Search] button. Then the line search/beam balance is
executed. Continue spraying the sample until the line search/beam balance operation is completely
finished.
When the ASC is used, the spray of the sample in the specified position on the ASC turntable is started
before starting the line search/beam balance. The line search/beam balance is started when the pre-spray
time set in [Parameters]-[Edit Parameters]-[Measurement Parameters] is finished after starting the spray.
(4) If the line search fails and the message stating insufficient energy is displayed, prepare and spray a
standard sample of even higher concentration and try it again.
(5) When the line search is completed, click on [Close] to return to the [Optics Parameters] page. Then click
on the [Next] button to proceed to the [Atomizer/Gas Flow Rate Setup] page again.
While monitoring the real time graph on the [Atomizer/Gas Flow Rate Setup] page, spray vaporized water
and check that the signal becomes almost zero.
(6) If the signal does not become small, it is possible that the analysis line was not correctly detected. In that
case, go back to the [Optics Parameters] page and perform the line search once again following the
procedures (1) to (5).

4-78 AA-6800/6650 Instruction


4.11 Setting the Optimum Conditions for Fuel Gas Flow Rate and
4.11 Setting the Optimum Conditions Burner
for Fuel
HeightGas
(AA-6800)
Flow Rate and Burner Height (AA-6800)

In the atomic absorption analysis, the [Fuel Gas Flow Rate] and [Burner Height] affect the absorption sensitivity.
Although standard values are automatically set as default values by selecting an element, the optimum
condition may differ depending on the sample characteristics and matrix components.
[Optimum Burner Height Search] and [Optimum Gas Flow Rate Search] are the functions to search the
optimum conditions by the measurement while changing the burner height or gas flow rate automatically. In this
section, the operation procedures are described. For details on each item of the dialog box, refer to section
5.5.7. In addition, read section 4.8 thoroughly and set the conditions for ignition.

NOTE
[Burner Position Auto] and [Gas Flow Auto] cannot be used in the AA-6650.

4.11.1 Setting the Optimum Condition of Burner Height


(1) Open the [Atomizer/Gas Flow Rate Setup] page in the Wizard.
(2) Click on the radio button of [Atomizer Position] for operation object, then the [Burner Position Auto] button
is available. The optimum condition of burner height is obtained in the procedure described below.
1. Click on [Burner Position Auto]. Then the [Optimum Burner Height Search] dialog box appears.

Figure 4.54 [Optimum Burner Height Search] Dialog Box

2. Set the [Start] and [End] of the burner position search range. Although the available search range is
within 0 to 25 (mm), you may set the range 5 to 10 (mm) for Air-C2H2 and 8 to 14 (mm) for N2O-C2H2.
3. Press the IGNITE button on the front side of AA main unit to ignite a flame.
4. Start spraying the blank solution and click on the [Blank Meas.] button. The measurement is
performed while the burner height is changed by 1 mm step in the selected range. Continue to spray it
until the measurement is completed.
5. Next, start spraying the standard (or sample) solution and click on the [STD Meas.] button. In the
same way as blank measurement, the measurement is performed while the burner height is changed.
Continue to spray it until the measurement is completed.
6. The dialog box displays the graph which is created by subtracting the measurement result of 4. from
the measurement result of 5. And the burner height with which the absorbance becomes the highest is
also displayed in [Current Value].

AA-6800/6650 Instruction 4-79


Chapter 4 Basic Operation

7. If the result is acceptable, extinguish the flame and click on [OK]. The [Optimum Burner Height
Search] dialog box is closed to return to the [Atomizer/Gas Flow Rate Setup] page, and the obtained
value is indicated and used as the [Burner Height]. If [Cancel] is pressed, the burner height is returned
to the original position.

4.11.2 Setting the Optimum Condition of Fuel Gas Flow Rate


(1) Open the [Atomizer/Gas Flow Rate Setup] page in the Wizard.
(2) Click on the radio button of [Fuel Gas Flow Rate] for operation object, then the [Gas Flow Auto] button is
available. The optimum condition of fuel gas flow rate is obtained in the procedure described below.
1. Click on [Gas Flow Auto]. Then the [Optimum Gas Flow Rate Search] dialog box appears.

Figure 4.55 [Optimum Gas Flow Rate Search] Dialog Box

2. Set the [Start] and [End] of the burner position search range. The range can be set within 0.6 to 4.9 L/
min in the case of Air-C2H2 and within 5.6 to 9.9 L/min in the case of N2O-C2H2. It is recommended to
set the range within the standard condition r 0.5 L/min.
3. Press the IGNITE button on the front side of AA main unit to ignite a flame.
4. Start spraying the blank solution and click on the [Blank Meas.] button. The measurement is
performed while the fuel gas flow rate is changed by 0.1 L/min step in the selected range. Continue to
spray it until the measurement is completed.
5. Next, start spraying the standard (or sample) solution and click on the [STD Meas.] button. In the
same way as blank measurement, the measurement is performed while the fuel gas flow rate is
changed. Continue to spray it until the measurement is completed.
6. The dialog box displays the graph which is created by subtracting the measurement result of 4. from
the measurement result of 5. And the fuel gas flow rate with which the absorbance becomes the
highest is also displayed in [Current Value].
7. If the result is acceptable, extinguish the flame and click on [OK]. The [Optimum Gas Flow Rate
Search] dialog box is closed to return to the [Atomizer/Gas Flow Rate Setup] dialog box, and the
obtained value is indicated as the [Fuel Gas Flow Rate]. If [Cancel] is pressed, the fuel gas flow rate is
returned to the original position.

4-80 AA-6800/6650 Instruction


4.11 Setting the Optimum Conditions for Fuel Gas Flow Rate and
Burner Height (AA-6800)

If [Fuel Gas Flow Rate] is changed, distribution of atoms in the flame changes, as the result, the optimum
[Burner Height] also changes. On the other hand, changing [Burner Height] also changes the optimum gas
flow rate. Note that the optimum condition changes if the other condition is changed.
To search the optimum condition precisely, for example, select several levels of burner height and search
the optimum gas flow rate at each level of burner height. Then select the best combination that shows
highest sensitivity. (Or you can also select several levels of gas flow rate and search the burner height at
each flow rate).
Although some elements (such as Cu) are not affected so much by these conditions, other elements (such
as Cr) are affected greatly. If these settings are not appropriate, not only the sensitivity decreases, but also
poor reproducibility of data may be caused by sensitivity fluctuation. Utilize these functions for setting the
optimum conditions when required.

AA-6800/6650 Instruction 4-81


Chapter 4 Basic Operation

This page is intentionally left blank.

4-82 AA-6800/6650 Instruction


Chapter 5
Functions of Operation
Menu

CONTENTS

5.1 [Wizard Selection] Dialog Box ....................................................................................................... 5-2


5.2 [File] ............................................................................................................................................... 5-3
5.3 [Edit]............................................................................................................................................. 5-13
5.4 [Refer to Parameters] .................................................................................................................. 5-15
5.5 [Parameters] ................................................................................................................................ 5-16
5.6 [Edit Parameters] ......................................................................................................................... 5-48
5.7 [Default Parameters].................................................................................................................... 5-62
5.8 [Instrument].................................................................................................................................. 5-63
5.9 [Help] ........................................................................................................................................... 5-85

AA-6800/6650 Instruction 5-1


Chapter 5 Functions of Operation Menu
5.1 [Wizard Selection] Dialog Box

After the software is started, the [Wizard Selection] dialog box shown in Figure 5.1 is displayed. Clicking on
[Cancel] closes this dialog box, and clicking on [Wizard] at left lower of the main window displays this dialog box
again.

Figure 5.1 [Wizard Selection] Dialog Box

5.1.1 [Wizard] Page


The following three icons are indicated on the [Wizard] page in the [Wizard Selection] dialog box. Each Wizard
can be started by selecting one of the icons and clicking on [OK]. However, when you start newly, or when no
element has been selected, [Schedule Creation] and [Measurement Preparation] are not displayed.
[Element Selection]
The element selection Wizard is started. Selection of measurement elements, setup of measurement element
order and selection of flame/furnace are performed here. You may close the Wizard in the element selection
page only. Or you may also proceed to the pages of schedule creation and measurement preparation to set the
parameters until the measurement can be performed in that conditions.
This is equivalent to selecting [Parameters]-[Element Selection Wizard] from the menu.
[Schedule Creation]
Setup of calibration curve parameters, setup of sample preparation parameters, setup of the sample
information, and input of factors for actual concentration calculation are performed here and the measurement
sequence is created on the MRT worksheet.
This is equivalent to selecting [Parameters]-[Schedule Creation Wizard] from the menu.
[Measurement Preparation]
This is applied for one element when the measurement sequence is already created. Lighting of hollow cathode
lamp, line search/beam balance, and setup of the burner position and gas flow rate or setup of furnace
temperature program are performed.
This is equivalent to selecting [Parameters]-[Measurement Preparation Wizard] from the menu.

5.1.2 [Recent Files] Page


A data file lately used can be selected from the list and opened.

5.1.3 [Recent Templates] Page


A template lately used can be selected from the list and opened.

5-2 AA-6800/6650 Instruction


5.2 [File]
5.2 [File]

This menu summarizes functions associated with WizAArd's file and print.
In the WizAArd, two file types of "*.aa" and "*.taa" are handled. The "*.aa" refers to a data file and contains the
measurement parameters, calibration curve, sample informations, measurement procedure and measured
data. These informations for plural elements can be saved in one file.
The "*.taa" refers to a template and is different from a data file in the following points.
(1) Measured data is not included.
The contents are the same as those of "*.aa" file before measurement. If a file is saved as a template file in
[File]-[Save As] after measurement, the measured data is cleared and other contents are saved.
(2) When a template file is loaded, it has no name.
When a template file is loaded, the title bar displays "notitle - WizAArd". If selecting the [File]-[Save], the
[Save As] dialog box always appear instead.
(3) It can be utilized as a cookbook (standard parameters for each element).
When using the parameters, such as wavelength, lamp current and furnace program, which are different
from the standard parameters built in the software, save them as a template file so that you can use it
easily instead of the built-in standard parameters (refer to section 5.5.1.2. "[Template] page").

Figure 5.2 Drop-down Menu of [File]

5.2.1 [New]
This command is used to create measurement parameters and measurement procedures. Execution of this
command resets the data and parameters already existing on MRT worksheet. When the data exists on MRT
worksheet, save the data with [Save] or [Save As...] command before executing [New].

AA-6800/6650 Instruction 5-3


Chapter 5 Functions of Operation Menu

5.2.2 [Open]
This command is used to read the files already saved in the disk.
Execution of this command opens the [Open] dialog box (Figure 5.3). Specify the [Look in], [Files of type] and
[File name], and click on [Open].

Figure 5.3 [Open] Dialog Box

[Comment]
If a comment has been written with the file to be opened, the comment can be read. Enter [File name] and click
on [Comment], then the comment is displayed.

5.2.3 [Save]
This command is used to save the parameters and data currently loading on the software, without changing the
file name.
When the file name does not exist (not named), same as [Save As...] is executed.

NOTE
A measurement data whose repeat measurement has not finished is not saved in the file. If the data is
necessary when the repeat measurement cannot be completed, print it before ending the AA software.

5-4 AA-6800/6650 Instruction


5.2 [File]

5.2.4 [Save As...]


This command is used to save the parameters and data currently loading on the software with a new file name.
When this command is executed, the [Save As] dialog box (Figure 5.4) opens. Specify the [Save in], [Save as
type] and [File Name], and click on [Save]. If the "*.taa" is selected for file type, data is not saved.

NOTE
A measurement data whose repeat measurement has not finished is not saved in the file. If the data is
necessary when the repeat measurement cannot be completed, print it before ending the AA software.

Figure 5.4 [Save As] Dialog Box

If a file is saved as "template.aa" in the same folder (default: C:\Program Files\WizAArd\") of the execution file
("Wizaa.exe"), the "template.aa" file is automatically loaded when starting AA software at next time or when
newly creating file with [New] command. It is convenient to save a frequently used measurement parameter file
in your routine as "template.aa".
[Comment]
This button is used to record your comment. Click on the [Comment] button, then [File Comment] dialog box
opens. Write your comment and click on [OK]. The comment is saved with the file.

5.2.5 [Additional Load]


Schedules of measurement element in a file saved in the disk are added to the end of the current schedule of
measurement element. This function can be used for the following purposes.

(1) A file for continuous measurement of plural elements can be created using several measurement files (or
measurement template files) created for single element.
(2) One summary report can be created from several files.
When a schedule of the same element is added, it is not combined in one schedule but added as another
schedule. When the total number of schedules exceeds 20, the schedules over it are not read in.

AA-6800/6650 Instruction 5-5


Chapter 5 Functions of Operation Menu

5.2.6 [File Export...]


This command is used to create a text file from data on the MRT worksheet of currently opened file.
The text file can be read in word processor software or spreadsheet software.
Executing this command opens the dialog box (Figure 5.5) to indicate the selection items. From this list, select
items to be converted to text data and click on [OK]. Then the [Save As] dialog box as shown in Figure 5.4
opens. Specify the [Save in], [Save as type] and [File name], and click on [Save].

NOTE
Only the data on the MRT worksheet can be output to text file. Measurement parameters and waveform data
cannot be output.

Figure 5.5 [Select Schedule] Dialog Box

5.2.7 [Export Items]


This specifies output items to output the data on the MRT worksheet to the text file. This setting is valid to the
following text file output functions.
• Output from [File]-[File Export...] menu.
• Output by setting the automatic output of text file in [File]-[Auto Save] menu
• Output by setting "FILEEXPORT" in [Action] field in the MRT worksheet

5-6 AA-6800/6650 Instruction


5.2 [File]

5.2.8 [Auto Save]

<1> <2>

<3> <4>

<5>
<6>

<7> <8>

<9>

<10> <13>
<11>
<12>

Figure 5.6 [File Auto Saving and Exporting] Dialog Box

Saving the backup file automatically


Automatic saving of the backup of measurement file can be set up in the style of "every X samples are
measured".
This setting is valid both for automatic measurement using the auto-sampler and for manual measurement.

1. [Auto Save]
When saving a backup file automatically, select this check box. The saving interval and file name can be
entered.
2. [every X samples]
Enter the interval for saving a backup file. The input range is 1 to 300. The number of measurement items
(BLK, STD, UNK, MSA, SMSA, RESLOPE, QC and SPIKE) on the MRT is counted as the sample number.
3. [File Name]
Set a path name (drive name + folder name + file name) of backup file. A path name can be entered easily
by using [Brows...] (<4>).
If a backup name is not entered, the default file name "autosave.aa" is automatically set.
When the automatic saving is executed, the preceding backup file of auto-saving is renamed and backed
up by adding ".sav." to the end of the file name.

Example:
When the auto saving is set with a file of the name "autosave.aa", executing another auto saving creates
"autosave.aa.sav." as a backup of the preceding file.

AA-6800/6650 Instruction 5-7


Chapter 5 Functions of Operation Menu

Exporting the MRT worksheet data automatically in text file


When performing an automatic measurement using the auto-sampler, the measurement result of the
schedule and summary report can be exported in text style at the end of schedule of each element (or
when the execution of the last row of each element on the MRT is finished).
This setup is invalid for manual measurement. Also, only the data in the MRT worksheet can be exported
in text file, but the measurement parameters and waveform data cannot be exported.

NOTE
To perform the text file auto export in manual measurement, set a "FILEEXPORT" row in the MRT
worksheet.

5. [One element text file at the end of the schedule]


Select this check box to export the measurement result of each element in text style.
6. [Summary text file at the end of the schedule]
Select this check box to export the summary report in text style.
7. [Folder Name]
This sets a destination folder of the text file automatically exported. Selecting the check box <5> or <6>
makes this entry possible. A destination folder name can be entered easily by using [Brows...] (<8>).

The AA software automatically gives a file name of the automatically exported text file. The measurement
result of each element schedule is given a file name as "element name + measurement type (Flame:1,
Furnace:2, HVG/MVU:3).txt". For example, when Pb is measured in furnace method, the text file name is
"Pb2.txt". The file name of summary report is fixed to "summary.txt".
These files are saved over the preceding one without any warning message. Therefore, "summary.txt" is
overwritten whenever a measurement of each element is finished. Also, when the same element is
measured in the same measurement method, note that firstly exported measurement result is overwritten.
This automatic export function can be used for the automatic data collection by the host computer on the
network, in a combination with the following "Executing a program by command line".

Executing a program by command line


In the automatic measurement using the auto-sampler, a command line can execute a program when the
schedule of each element is finished (when the execution of the last row on the MRT worksheet of each
element is finished, or immediately after the auto-export of text file is finished).
A command line means a method to specify an execution file name and start/execute the program, as MS-
DOS prompt or [Start]-[Run...] in Windows.
When executing a program from the command line, specify a combination of the execution file name or
batch file name and its argument. In this dialog box, a name of text file to be exported automatically can be
set up as argument.

NOTE
When executing a program by command line in manual measurement, set up "COMMAND" row in the MRT
worksheet.

9. [Execute command (after exporting text file)]


Select this check box to execute a program by command line. Then the command file name can be
entered.
10. [Command File Name]
Enter the execution file name. A file name can be entered easily by using [Brows...] (<13>).

5-8 AA-6800/6650 Instruction


5.2 [File]

11. [Add the element file name to the command]


When this check box is selected, the single element text file name is set up as argument of command.
This check box is selectable when the check boxes <5> and <9> are selected.
12. [Add the summary file name to the command]
When this check box is selected, the summary text file name is set up as argument of command.
This check box is selectable when the check boxes <6> and <9> are selected.
A file name of text file automatically exported is enclosed by " " (double quotation marks) and added to the
end of a specified command line with an intervening space between them. When both file names of
schedule measurement result and summary report are added in the setting, the file name of summary
report is added to the end of the file name of measurement result with an intervening space between them.
For example, when the command line is "C:\something.bat" and when the Pb furnace measurement result
and summary report are to be automatically exported to the "C:\My Documents\AA Export" folder, and both
file names are to be added to the command line, the actual command line to be executed is as follows.
C:\something.bat "C:\My Documents\AA Export\Pb2.txt" "C:\My Documents\AA Export\summary.txt"
If a special program is additionally prepared, this function can be utilized to give a notice of the
measurement end to another room through a computer network or to collect or handle the measurement
results outputted in text style.

5.2.9 [Print Data/Parameters...]


This command is used to print the measurement parameters and data of the currently opened file.
When this command is selected, the element symbols available for printing the data and parameters are
displayed in the dialog box that is same as Figure 5.5. From this list, select items to be printed and click on [OK].
Then the dialog box shown in Figure 5.7 opens. Set the [Copies], and click on [Print]. In the [Print] dialog box
invoked from [Print Data/Parameters] menu, only [All] can be selected at [Print range].

NOTE
When the parameters are changed in the middle of the measurement in one schedule, only the final
parameters are printed out. To print the measured data and its parameters correctly on the report, create
another schedule when measuring one element with different parameters.

Figure 5.7 [Print] Dialog Box

AA-6800/6650 Instruction 5-9


Chapter 5 Functions of Operation Menu

5.2.10 [Print Table Data...]


This command is used to print out the contents of MRT worksheet of currently opened file (for [Table Show/
Hide], refer to 5.2.11.2).
When this command is executed, items which can be printed out are displayed in the dialog box as Figure 5.5.
From this list box, select [Summary] or elements you want to print and click on [OK]. Clicking on [OK] button
opens the [Print] dialog box (Figure 5.7). Operate in the same way as section 5.2.9. The data is printed out
according to the format displayed on each MRT worksheet.

5.2.11 [Print Style]


This command is used to make settings related to printing data and parameters from the [Print Data/
Parameters] menu. You can set the print mode, items and font here.
When printing a peak profile data (waveform), set the graph scale in the [Y-axis Print Range] page by selecting
[Parameters]-[Edit Parameters] from the menu bar.

5.2.11.1 [Print Style Setup] Page

Figure 5.8 [Print Style Setup] Page

Put check marks to the items or contents you want to print. Clicking on [Details] displays more detail items.
In [Data Print Mode], you can select it from the following three.
All: All the data of repeat measurement with peak profile
Without Profile: All the data of repeat measurement without peak profile
Only Average: Only the average value calculated from repeat measurement data

5-10 AA-6800/6650 Instruction


5.2 [File]

5.2.11.2 [Table Show/Hide] Page


When printing the data of MRT worksheet, select items in this page. Put check marks in the items to be printed.

5.2.11.3 [Font] Page

Figure 5.9 [Font] Page

Set the font type, size, style and other items. A sample of the characters based on the settings are displayed in
[Preview].
These settings are valid only for [Print Data/Parameters].

AA-6800/6650 Instruction 5-11


Chapter 5 Functions of Operation Menu

5.2.12 [Print Setup]


Set the items related to the printer. Executing this command opens the [Print Setup] dialog box shown in Figure
5.10.

Figure 5.10 [Print Setup] Dialog Box

[Printer]
Select the printer to be used from the drop-down list of [Name].

[Paper]
Select [Size] and [Source].

[Orientation]
Select [Portrait] or [Landscape] by clicking on radio button.

5.2.13 Recent Files


Maximum four measurement file names recently opened are displayed. Click on the file name to be opened.

5.2.14 [Exit]
When this command is executed, the communication with the instrument is shut off first and then the software is
closed. Therefore, it takes approx. 30 seconds to exit the program. If the data has not been saved, a warning
message to ask you whether you want to save the data before exiting from the program or not is displayed.

5-12 AA-6800/6650 Instruction


5.3 [Edit]
5.3 [Edit]

Functions to be used in editing the data row on MRT worksheet are summarized.

Figure 5.11 Drop-down Menu of [Edit]

5.3.1 [Insert Row]


This command is used to insert one row just before the row selected in the table. However, a row cannot be
inserted before the row already measured.

5.3.2 [Delete Rows]


This command is used to delete the selected rows in the table. However, the row already measured cannot be
deleted.

NOTE
Insertion and deletion of a row next to the current measuring row can't be done during measurement.

5.3.3 [Import Other Schedule]


A measurement procedure created in other element's schedule is copied to the currently displayed (active)
MRT worksheet.

5.3.4 [Collective Edit]


The values of a specified item can be changed collectively in selected rows on the MRT worksheet. The
available items are [C# (Calibration Number)], [Actual Conc. Unit], [Sample Volume], [Diluent Volume],
[Reagent 1 to 3], [Weight Factor], [Volume Factor], [Dilution Factor], [Correction Factor] and [Coating Reagent].

5.3.5 [Remeasure Selected Range]


This is a function to perform a remeasurement on the data already measured.
After selecting rows to be remeasured on the MRT worksheet, execute this. The rows already measured are
excluded from the measruement result and new rows for the same measurement items are added on the MRT
worksheet. In the case of repeat measurement, select a range including average rows to perform a
remeasurement. A remeasurement cannot be executed for rows already excluded or rows with no data (RINSE,
AUTO ZERO, etc).

AA-6800/6650 Instruction 5-13


Chapter 5 Functions of Operation Menu

5.3.6 [Clear Measurement Result]


All the measurement data on the MRT worksheet currently displayed are cleared and the status before
measurement is recovered. The setting of measurement procedure remains without a change.

5.3.7 [Copy]
Numeric values and characters on the MRT worksheet and summary table can be copied to the clipboard.
Refer to section 4.7.6 for details.

5.3.8 [Paste]
Text data can be pasted from the clipboard only to the sample ID row in the MRT worksheet. Refer to section
4.7.6 for details.

5-14 AA-6800/6650 Instruction


5.4 [Refer to Parameters]
5.4 [Refer to Parameters]

Clicking on [Parameters] in the menu bar during the measurement opens a drop-down menu.

Figure 5.12 [Parameters] Drop-Down Menu

Selecting [Refer to Parameters] from this drop-down menu opens the property sheet, which is a dialog box to
show the parameters for the element under measurement. The parameters can be shown but cannot be
changed. To change the parameters, stop the measurement once and select [Parameters]-[Edit Parameters]
from menu bar (refer to section 5.6).

NOTE
If a dialog box ([Coating and Boost Cycles], etc.) is opened in the sheet for referring to the parameters, the
measurement operation is stopped temporarily. Therefore, close the dialog box immediately after referring to
the necessary parameters.

AA-6800/6650 Instruction 5-15


Chapter 5 Functions of Operation Menu
5.5 [Parameters]

Functions on parameter setup are summarized here.

Figure 5.13 Drop-down Menu of [Parameters]

The following three Wizards are available.

[Element Selection Wizard]


Selection of measurement elements, setup of measurement element order and selection of flame/furnace are
performed here. You may close the Wizard in the element selection page only. Or you may also proceed to the
pages of schedule creation and measurement preparation to set the parameters until the measurement can be
performed in that conditions.
You can proceed to the next page only after selecting an element newly. Use the [Schedule Creation Wizard] or
[Measurement Preparation Wizard] for elements already selected.

[Schedule Creation Wizard]


Setup of calibration curve parameters, setup of periodic blank measurement, setup of the sample information,
and input of factors for actual concentration calculation are performed here and the measurement sequence is
created on the MRT worksheet.
This menu is valid when the element has been selected on the MRT worksheet.

[Measurement Preparation Wizard]


This is used for an element currently selected. Lighting of hollow cathode lamp, line search/beam balance, and
setup of burner position/gas flow rate or setup of furnace temperature program are performed. This menu is
valid when an element exists on the MRT worksheet.
Each Wizard is composed of the pages shown below. Clicking on [Next] in each page opens the next page. You
can close the Wizard by clicking on [Finish] when the settings are completed on each page.

[Element Selection Wizard] [Schedule Creation Wizard]


Element Selection Element Selection
Preparation Parameters Preparation Parameters
Sample ID Sample ID
Sample Selection Sample Selection
Connect to Instrument/Send Parameters
Optics Parameters
Atomizer/Gas Flow Rate Setup (for flame method)
Furnace Program (for furnace method)

5-16 AA-6800/6650 Instruction


5.5 [Parameters]

[Measurement Preparation Wizard]


Connect to Instrument/Send Parameters
Optics Parameters
Atomizer/Gas Flow Rate Setup (for flame method)
Furnace Program (for furnace method)

In the [Element Selection Wizard], the [Next] button is valid only when a newly selected element exists. In the
[Measurement Preparation Wizard], the [Optics Parameters] page is displayed first when the connection with
instrument is already completed.
The followings are description of each page in the Wizard.

5.5.1 [Element Selection] Page


Measurement elements are selected and their parameters are edited here.

Figure 5.14 [Element Selection] Page

[Select Elements]
When adding an element to be measured, click on this button. Then [Load Parameters] dialog box opens.

[Edit Parameters]
Select an element row and click on this button. Then the measurement property sheet opens. For details, refer
to section 5.6.

NOTE
After selecting an element row, click on the right mouse button. Then a selection of [Stop/Continue] at the
end of measurement can be set up.

AA-6800/6650 Instruction 5-17


Chapter 5 Functions of Operation Menu

[Up]
Select an element row and click on this button. Then the row moves up one row upper.

[Down]
Select an element row and click on this button. Then the row moves down one row lower.

[Delete]
If you want to delete a row, click on the row to make its color reversed and then click on [Delete]. When the
lamp of selected element is lit, you can't delete it. Please turn off the lamp in the [Optics Parameters] page for
current measurement element or [Instrument]-[Lamp Status] menu and delete the element.

[Connect]
Communication between the personal computer and AA main unit is established. For details, refer to 5.8.1.

[Measurement Element]
Select the element to be measured first from the drop-down list. The measurement is started from this element
and performed to the last row in order.

5.5.1.1 [Cookbook] Page


In the [Cookbook] page, select the target element from the drop-down list. Also, select the method from flame or
furnace and select the hollow cathode lamp type from normal or SR in this page. At this time, description of
each parameter to be set is displayed on the screen. Since the contents of this cookbook has been written in
the program beforehand, you cannot make a change.

Figure 5.15 [Cookbook] Page

[Periodic Table]
Click on this button, then you can select the target element from the periodic table or element list.

[Using ASC]
When using the autosampler, put a check mark in the check box.

5-18 AA-6800/6650 Instruction


5.5 [Parameters]

[HVG] and [MVU]


Putting a check mark in the check box calls the parameters for using the hydride vaporizer unit (HVG) or the
mercury vaporizer unit (MVU).

This check box gets active when the element measured by the cold vapor mercury technique or the hydride
vapor technique is specified.

5.5.1.2 [Template] Page

Figure 5.16 [Template] Page

In the [Template] page, a template (*.taa) already created can be read. Click on [Browse] to open the [Open]
dialog box. Then specify the [Look in] and [File name] and click on [Open]. When the template is opened, Figure
5.16 is displayed.
Click on the element in [Element Selection] to highlight it, then the description of parameters for the element are
displayed in the right side of the element. When the template contains plural elements, you can specify the
element to read the parameters. Put a check mark in the check box next to the element name only for the
element you need. Clicking on [OK] returns to the [Element Selection] page. You can check that the selected
element name is added in the measurement order field.
When using a wavelength or flame type which is different from that in [Cookbook], it is convenient to create a
template (*.taa) with the parameters beforehand. In WizAArd, "Cookbook.taa" (flames for Ca, Pb and Sn) and
"HyperLamp.taa" (hyper lamps for As, Se, Sb and Pb) are already prepared.

AA-6800/6650 Instruction 5-19


Chapter 5 Functions of Operation Menu

5.5.2 [Preparation Parameters] Page


You can set the calibration curve parameters and the preparation parameters for standard / unknown / periodic
blank samples.

Figure 5.17 [Preparation Parameters] Page

Double-click on the element to be edited, or select the element row and click on [Edit] to open the [Edit
Preparation Parameters] dialog box.

Figure 5.18 [Edit Preparation Parameters] Dialog Box

5-20 AA-6800/6650 Instruction


5.5 [Parameters]

[Measurement Type]
Select either of "Calibration Curve" (calibration curve method) or "SMSA (Simple Method of Standard
Addition)". In this case, the "MSA (Method of Standard Addition)" cannot be selected. To set the calibration
curve parameters for MSA (Method of Standard Addition), refer to 4.9.

[Order] and [Zero Intercept]


Select the order of calibration curve polynomial. You can select 1st, 2nd or 3rd. Putting a check mark to [Zero
Intercept] will force the calibration curve to pass through the origin.
When the simple standard addition method is selected, 1st order without zero intercept are automatically set,
and these items are not displayed on the screen.

[Conc. Unit]
Set the concentration unit used for [True Value] and [Conc.] in MRT worksheet.

[Load]
A preparation parameter file (*.mix) already saved can be loaded. Clicking this button opens the [Open] dialog
box. Specify the [Look in] and [File name] and click on [Open]. In a preparation parameter file (*.mix), the
following parameters are saved together:

Parameters Screens

(A) Measurement Type [Edit Preparation Parameters] dialog box


(Calibration Curve Method or SMSA)

(B) Mixing ON/OFF [Edit Preparation Parameters] dialog box

(C) Preparation Parameters [Edit Preparation Parameters] dialog box


(STD, Unknown, Blank)

(D) Reagent Name [Reagent Setup] dialog box


Reagent Position
Intake Order

(E) Coating and Boost Cycles [Coating and Boost Cycles] dialog box

A file which was created under different conditions ((A) Measurement Type and (B) Mixing ON/OFF) from the
current setting cannot be loaded.

[Save]
The current preparation parameters are saved in the file. Clicking this button opens the [Save As] dialog box.
Specify the [Save in] and [File name] and click on [Save].
For contents to be saved, refer to the [Load] described above.

AA-6800/6650 Instruction 5-21


Chapter 5 Functions of Operation Menu

5.5.2.1 Weight Correction Factors


The factors used for calculating the actual concentration are set here.

NOTE
Actual concentration is calculated with the following equation.
Actual Conc. = (Measured Conc.) u [Volume Factor] u [Dilution Factor] u [ASC Dilution Factor] u [Correction
Factor] / [Weight Factor]
However, there is no particular function to set units for [Weight Factor] and [Volume Factor]. Note that the
entered values are only calculated using the above equation. Use [Correction Factor] to convert the unit.
[ASC Dilution Factor] is a value automatically set by the software to correct a change of the actual dilution
factor when the preparation parameters are changed automatically by the software in the case of "Auto
Dilution and Remeasurement" (refer to 5.6.9 (4)).

5.5.2.2 [Preparation Parameters]-[Standard Samples]


The standard sample preparation parameters are set here. (when the ASC is not used, only the [Conc.] field on
the table is set).

[Number of STD]
Enter the number of standard samples to be measured. Maximum 8 can be entered. The row number of the
[Preparation Parameters]-[STD Samples] table displayed on the screen is set by this number.

[Conc.]
Enter the concentrations of standard samples in the order of measurement.

[Pos.]
In the case of calibration curve method, enter the position (1 to 60, R1 to R8) of standard sample. In the case of
simple standard addition method ("SMSA"), enter the position (1 to 60, R1 to R8) of unknown sample to which
the standard sample is added.

[Standard (PL)]
Enter the volume of standard sample. In the case of simple standard addition method ("SMSA"), the indication
in this field becomes [Sample]. Enter the volume of unknown sample to which the standard sample is added.
When performing the sample preparation using the connected autosampler in furnace method, set the following
items in addition.

[Diluent] [Reagent 1] [Reagent 2] [Reagent 3]


Enter the volume to be used for mixing.

The titles of these fields are changed depending on the settings in the [Reagent Setup] dialog box and
[Coating and Boost Cycles] dialog box.
The upper line indicates the reagent name and the lower indicates the position on the ASC. When a reagent
is set to be used for coating, the position is enclosed by [ ] (brackets). This indication is common for
[Preparation Parameters]-[Unknown Samples] and [Preparation Parameters]-[Blank Samples].

5-22 AA-6800/6650 Instruction


5.5 [Parameters]

[Total Vol (PL)]


Total volume of solutions to be mixed is calculated and indicated. The reagent volume used for coating is not
included in this total volume.

NOTE
When using the ASC, put a check mark in the check box of [Using ASC] in [Sequence] page of [Edit
Parameters] dialog box.

5.5.2.3 [Preparation Parameters]-[Unknown Samples]


[Sample (PL)]
Enter the sample volume to be used for mixing.

[Diluent] [Reagent 1] [Reagent 2] [Reagent 3]


Enter the volume to be used for mixing.

[Total Vol (PL)]


Total volume of solutions to be mixed is calculated and indicated. The reagent volume used for coating is not
included in this total volume.

5.5.2.4 [Preparation Parameters]-[Blank Samples]


Set the timing of inserting a blank measurement in unknown sample measurements at the time of automatic
creation of measurement schedule. When using the ASC in furnace method, set the preparation parameters for
blank sample in addition.

[Periodic Blank]
Selecting [On] will insert a blank measurement periodically at the time of automatic creation of measurement
schedule.

[Meas. Interval]
For example, entering "5" will insert the blank measurement row after every five unknown sample rows.

[Pos.]
Set the position (1 to 60, R1 to R8) of blank sample when using the ASC.

In furnace method, set the following items in addition.


[Sample (PL)]
Enter the sample volume to be used for mixing.

[Diluent] [Reagent 1] [Reagent 2] [Reagent 3]


Enter the volume to be used for mixing.

[Total Vol (PL)]


Total volume of solutions to be mixed is calculated and indicated. The reagent volume used for coating is not
included in this total volume.

AA-6800/6650 Instruction 5-23


Chapter 5 Functions of Operation Menu

5.5.2.5 Mixing Setup and Reagent Setup


When the [Using ASC] is check-marked and the furnace method is selected at the [Element Selection] page,
you can use the [Mixing], [Reagent] and [Coating] buttons. First, put a check mark in the check box of [Mixing
ON] then click on the [Mixing] button. Then the [Mixing Setup] dialog box will open.

Figure 5.19 [Mixing Setup] Dialog Box

[Rinse with Sample]


This sets the type of rinsing to be conducted in this mixing port prior to mixing. Rinsing with sample refers to the
use of sample to rinse the mixing port based on the set mixing conditions, after first rinsing with rinse liquid. This
sample liquid is discarded and is not used for measurement. This method is used in high accuracy
measurement to prevent the diluting of measurement sample with the very small amount of rinse liquid
remaining after rinsing with rinse liquid. With this method, however, the rinse time is doubled and the amount of
sample required is increased.

[Volume]
When mixing is set to ON, the volume of mixed sample set here is drawn into the ASC nozzle and injected into
the graphite tube. Determine the injection volume in consideration of the total volume of mixed sample in the
mixing port and the maximum number of repeat measurement. When mixing is set to OFF, [Total Vol] in the
sample preparation parameters becomes the volume to be injected into the graphite tube.

[Speed]
This sets the speed at which the sample is injected into the furnace. The default value is 25 (PL/sec).

Clicking on [OK] after completing the setup returns to the [Edit Preparation Parameters] dialog box. Clicking on
[Reagent] opens the [Reagent Setup] dialog box.

Figure 5.20 [Reagent Setup] Dialog Box

[Reagent Name], [Reagent Position] and the intake order of sample and reagents can be set here for four kinds
of reagents.

5-24 AA-6800/6650 Instruction


5.5 [Parameters]

5.5.2.6 Coating and Boost Cycles (only for Furnace Method)


Pressing the [Coating] button opens the [Coating and Boost Cycles] dialog box.

Figure 5.21 [Coating and Boost Cycles] Dialog Box.

Coating means injecting a specified reagent into the furnace and drying it prior to the sample injection (coating
the tube surface). First, the check-marked reagent is injected in the furnace, and heating is executed up to the
furnace program stage specified in [Last Coating Cycle]. After this, the sample is injected.
Furnace boost cycle refers to the repetitive cycle of sample injection into the furnace, and drying and ashing of
the sample in order to raise the concentration of the target element in the sample. Repeating this boost cycle
enables measurement of the sample whose concentration is lower than the quantitation range by concentrating
it and raising its absorbance to the quantitative range of the calibration curve.

For details on the setting items, refer to 5.5.9.1.

NOTE
When [NONE] is selected for the reagent position, the reagent is not used in the setting and not displayed on
the MRT, and it is excluded from the calculation of total volume of the preparation. This change has an effect
on the entire one schedule. If the reagent position is changed to or from [NONE] in the middle of the
schedule measurement, the displayed/printed total volume in the sample data already measured is also
changed to be different from the actual volume. Therefore, when quitting a use of the reagent in the middle of
one schedule, do not use [NONE] but set the reagent volume to zero.

AA-6800/6650 Instruction 5-25


Chapter 5 Functions of Operation Menu

5.5.2.7 Repeat Measurement Conditions


Pressing the [Repeat Conditions] button opens the [Repeat Measurement Conditions] dialog box.

Figure 5.22 [Repeat Measurement Conditions] Dialog Box.

Repeat measurement conditions are set here. For details on the setting items, refer to 5.6.2. The maximum
number of repetition set here has a relation to the preparation parameters setup.

5.5.3 [Sample ID] Page


The number of unknown samples to be measured, sample names and sample positions for connected
autosampler are set in the screen.

Figure 5.23 [Sample ID] Page

[Number of Samples]
Enter the number of unknown samples here. Then the rows as much as the sample number are created in the
table. For each sample, the following setup are available.

[Sample ID]
Enter the name to identify the sample. In the [Summary] of MRT worksheet, concentration result of each
element is listed based on this sample ID, then the summary report of plural elements are created for each
sample.

5-26 AA-6800/6650 Instruction


5.5 [Parameters]

NOTE
In the case of simple standard addition method, the position setting for the 1st sample is ignored because the
1st unknown sample is measured by the method of standard addition. The 1st sample position is set as the
item of [STD Samples] preparation parameters in the [Edit Preparation Parameters] dialog box.

[Pos.]
When using the autosampler, set the sample position on the sampler turntable.

[Collective Setup]
Clicking on this button opens the [Sample ID Collective Setup] dialog box. In this dialog box, the sample ID
described above can be easily entered.

Figure 5.24 [Sample ID Collective Setup] Dialog Box

This dialog box is used to set sample ID with successive No. automatically and ASC start position for the
autosampler. When completing the settings, click on [OK].

[Number of Samples]
Enter the number of unknown samples.

[Create Sample ID]


Marking a check in this box allows to enter sample ID automatically.

[Name]
Enter a common sample name here.

[Start No.]
Enter the first number of successive number.

[ASC Start No.]


Enter the measurement start position on the autosampler turntable when using the ASC. Successive numbers
are set as many as the number of samples.

AA-6800/6650 Instruction 5-27


Chapter 5 Functions of Operation Menu

5.5.4 [Sample Selection] Page


Specify the elements to be measured for each sample.

Figure 5.25 [Sample Selection] Page

Place a mark in the cell of element to be measured and delete a mark from the cell of element not to be
measured. When selecting plural cells, drag them and click on the right mouse button to select [Measure/Not
Measure].

5.5.5 [Connect to Instrument/Send Parameters] Page

Figure 5.26 [Connect to Instrument/Send Parameters] Page

5-28 AA-6800/6650 Instruction


5.5 [Parameters]

[Connect/Send Parameters]
Communication between the personal computer and AA main unit is connected. If the communication
connection has been already completed, this button is invalid.
For details, refer to section 5.8.1.

[Connect Options]
If the power of ASC or GFA is not ON when connected to the instrument, these options are not recognized. At
that time, turn on the power of ASC and GFA then click on this button.

[Measurement Element]
Select an element whose parameters are to be set in the following [Optics Parameters] page and [Atomizer/Gas
Flow Rate Setup] or [Furnace Program] page.

5.5.6 [Optics Parameters] Page


Wavelength, slit width, socket number, lamp current, lamp mode, lamp ON/OFF are set for the selected
element. Since the default values in the [Element Selection] page of Wizard are automatically set, you don't
have to change wavelength, slit width or lamp current. Select lamp mode according to the sample to be
analyzed.

Figure 5.27 [Optics Parameters] Page

[Wavelength]
The analysis wavelength is selected. As the default value, the wavelength of first resonance line (analysis line
of the highest absorption sensitivity) is displayed. To use another wavelength, enter the value in the range of
190.0 to 900.0 (nm). When line search is executed, the wavelength is automatically set to this value.

AA-6800/6650 Instruction 5-29


Chapter 5 Functions of Operation Menu

[Slit Width]
The slit width of monochromator is set. A slit width used ordinarily is displayed.
If the light intensity of hollow cathode lamp is weak and if there is too much baseline noise, widen the slit width
slightly.
Note that in the BGC-D2 mode, it is necessary to consider the balance between the light intensities of the
deuterium lamp and the hollow cathode lamp. If the light intensity of the deuterium lamp is too great, narrow the
slit width slightly. Conversely, if the light intensity of the hollow cathode lamp is too great, widen the slit width
slightly.

NOTE
When a neighboring line exists, note that the neighboring line may not be separated if the slit width is
widened.

[Socket #]
Enter the socket number to which the hollow cathode lamp of the selected element is mounted.

[Lamp Current (Low, High)]


The lamp current is entered here. A recommended current has been entered already. If you want to change the
lamp current, enter the current value not exceeding the maximum lamp current value according to the
instruction manual of the hollow cathode lamp. Lamp is automatically lit with the specified current value when
executing [Line Search]. [Lamp Current (High)] is valid only when [Lamp Mode] is "BGC-SR".
When the lamp current is changed, it is actually reflected on the instrument in the following cases.
• When the line search/beam balance is executed.
• When the [Parameters] sheet or Wizard is closed with [OK/Finish] (except when a necessary line search is
cancelled).
• The lamp current of warmup lamp is changed only when [Apply] is clicked in the [Select Warmup Lamp]
dialog box after [Warmup] is clicked in the [Optics Parameters] page of the main element lamp.

[Lamp Mode]
The following five modes are available (also refer to section 3.1.8).

EMISSION mode
This mode is used in flame emission analysis or when performing lamp or burner positioning adjustment. A
value proportional to the intensity of light incident upon the detector is displayed.
In flame emission analysis, energy intensity of emission spectrum of the target element generated in flame is
measured without using the hollow cathode lamp.

NON-BGC mode
This mode is used for atomic absorption analysis that does not require background correction, or atomic
absorption analysis in the long wavelength range (430 to 900 nm) where background correction by deuterium
lamp cannot be used.
The deuterium lamp does not light, so only the light of hollow cathode lamp is used. Transmission amount of
lamp energy that passed the atomizer unit is detected and then is converted into absorbance. If molecular
absorption other than the atomic absorption exists on the same wavelength of the target element, such
absorption is simultaneously observed. In such case, use BGC-D2 mode or BGC-SR mode.

5-30 AA-6800/6650 Instruction


5.5 [Parameters]

BGC-D2 mode
This mode is used for atomic absorption with background correction by deuterium lamp. If molecular absorption
other than the atomic absorption exists on the same wavelength of the target element, true absorbance cannot
be obtained in NON-BGC mode. In such case, make the light of deuterium lamp together with the light of hollow
cathode lamp pass through the atomizer unit.
Though the light of deuterium lamp cannot detect atomic absorption of narrow band, it can detect absorption of
wide band such as the molecular absorption. Accordingly, it is possible to get true absorbance by taking
difference of absorbance at both lamps.

BGC-SR mode
Background correction is performed using the phenomenon of self-reversal of the spectrum when a hollow
cathode lamp is used at a high current value. This mode is effective for a measurement of sample causing a
spectral interference or in long-wavelength range (430 nm - 900 nm) in which the deuterium lamp cannot be
used.

CAUTION
To use the BGC-SR mode, the SR lamp (L2433 series) is necessary. If a normal lamp is lit in the BGC-SR
mode, it may be damaged.

D2 mode
The absorbance measured by using the deuterium (D2) is displayed. Generally, this lamp is used to measure
absorbance value of molecular that gives a broad absorbance spectrum.

[Lamp Status]
When line search is not finished or when wavelength or slit width is changed after execution of line search,
"Line Search is necessary" is indicated. When the lamp current or lamp mode is changed after execution of
beam balance, "Beam Balance is necessary" is indicated. If the [Line Search] button is pressed while these are
indicated, line search/beam balance is appropriately executed. When closing the [Optics Parameters] page with
[Next] or [Finish] button, a message appears to ask whether to execute [Line Search/Beam Balance] or not.
Execute it, if necessary.

[Lamp ON]
Click on the check box to put a mark in it. Then the hollow cathode lamp of specified socket number is lit on.
When a check mark is already indicated, clicking on the check box will delete the check mark and the lamp is
turned off. The lamp will be automatically lit when [Line Search] is executed even if [Lamp ON] is OFF.

[ASC Sample Pos. for EMISSION Line Search]


In flame emission analysis, [Line Search] can be performed while spraying a sample automatically using the
ASC. Set the position of the sample (ordinarily, the standard sample of the highest concentration) on the ASC
turntable. This setting is valid only when the lamp mode is EMISSION and [Lamp Current (Low)] is "0".

AA-6800/6650 Instruction 5-31


Chapter 5 Functions of Operation Menu

5.5.6.1 [Lamp Pos. Setup] Button


It is necessary to set the hollow cathode lamp to be used and its socket No. beforehand. Clicking on this button
opens the [Lamp Position Setup] dialog box in Figure 5.28. Enter the element symbol of the lamp to be set in
each socket No. The "*" mark is used as a wild card. When using a multi-element lamp, enter "*" instead of
element symbol. Also, an element can be selected from the drop-down list displayed by clicking [Element]. In
[Lamp type], select the correct type of hollow cathode lamp to be used.

Figure 5.28 [Lamp Position Setup] Dialog Box

While this dialog box is displayed, you can turn the lamp turret and change the lamp.

5.5.6.2 [Warmup Lamp] Button


Set the items to warm up the hollow cathode lamp of the element to be measured next. Clicking on this button
opens the [Select Warmup Lamp] dialog box. First, select an element in [Schedule].

Figure 5.29 [Select Warmup Lamp] Dialog Box

Next, click on [Apply], then the parameters, [Socket #] and [Lamp Current], loaded in the element selection are
automatically set and the lamp is lit ON. If you don't want to light on the lamp here, select [Schedule] then click
on [OK].

NOTE
Be sure to combine appropriately odd/even or even/odd socket numbers in [Optics Parameters] and
[Warmup Lamp Setup]. If odd/odd or even/even socket numbers are combined, the lamp warmup cannot be
executed.

5-32 AA-6800/6650 Instruction


5.5 [Parameters]

When plural elements are selected in the [Element Selection] page and autosampler is used, the instrument
automatically judge and light on the warm-up lamp if no setting is made in this [Warmup lamp Setup] dialog box.
In addition, according to the setting [Lamp Warmup Time] in the [Sequence] page, the ending time is estimated
and warming up of the hollow cathode lamp of the next measurement element is started. Therefore, when
starting a measurement, the lamp of the next measurement element may not be lit.

5.5.6.3 [Line Search] Button


Clicking on this button opens the [Line Search/Beam Balance] dialog box. When the [Line Search] button is
pressed in the [Optics Parameters] page of the currently measured element, line search/beam balance is
automatically executed, if necessary. If line search/beam balance is already finished, only the result is
displayed.
When the element is not the currently measured element, only the result of line search/beam balance execution
is displayed.

Figure 5.30 [Line Search/Beam Balance] Dialog Box

[Close]
When this button is clicked on, this dialog box is closed to return to previous screen.

[Stop]
If this button is clicked on during execution of line search, beam balance execution stops.

[Do Line Search]


Clicking on this button lights the lamp, scans wavelength near the set wavelength, and detects the highest peak
in the emission profile according to the parameters set on [Optics Parameters] page. Scanning wavelength is
performed within the range of the set wavelength r 0.5 nm. When the correct peak is detected, "Line Search:
OK" is indicated. Successively setup of lamp mode and optimization of detector sensitivity (beam balance) are
performed. When the sensitivity setup is finished, "Beam Balance: OK" is indicated.

NOTE
When beam balance is performed, in some cases, an error message indicating that hollow cathode lamp
emission is too high or too low compared with D2 lamp emission. Change [Lamp Current (Low)] to a smaller
value when it is too high, and change [Lamp Current (Low)] to a larger value when it is too low.

[Print]
The result of line search is printed out.

AA-6800/6650 Instruction 5-33


Chapter 5 Functions of Operation Menu

5.5.7 [Atomizer/Gas Flow Rate Setup] Page (for Flame Method by


AA-6800)
Parameters related to burner (burner height and fuel gas flow rate) are set in this screen. In the graph
displaying real time data, the right mouse button menu can be used as in the real time graph of the main
window (refer to section 4.6.5). (Only the [Properties], [Copy] and [Radar] are available.)

5.5.7.1 Atomizer Position

Figure 5.31 [Atomizer/Gas Flow Rate Setup] Page

When adjusting the burner position, select [Atomizer Position] by the radio button of [Operation Object]. Ignite a
flame and introduce the sample. While monitoring the [Measured Data] indication or real time data, change the
burner position upward and downward to search the optimum position. After entering [Burner Height], click on
[Set Position]. Then the burner moves to the position. The distance from the optical path down to the burner is
indicated in a positive value. Clicking on [Up] or [Down] moves the burner 1 mm upward or downward. Since the
[Burner Lateral] position has been adjusted prior to shipping, set it to zero ordinarily. If the lateral position
should move with some reason, execute [Instrument]-[Maintenance]-[Burner Origin Position Adjustment] from
the menu bar (refer to sections 5.8.6.3 and 6.1.1.1).
[Burner Lateral] is used to lower the sensitivity of a particular element intentionally in the continuous
measurement of plural elements. After clicking on [Fore]/[Back] or entering a numeric value directly, click on
[Set Position]. Then the burner is moved forward or back. Search an appropriate lateral position to lower the
sensitivity of the element while spraying the sample.
The data reproducibility is better when lowering the sensitivity by the burner angle setting instead of the burner
lateral position setting.

[Operation Object]
Select the item to be adjusted. Select [Atomizer Position] when adjusting the burner position. Select [Fuel Gas
Flow Rate] when adjusting the fuel gas flow rate.

[Measured Data]
The current measurement data is displayed. In the background correction modes, the indicated value as
[Measured Data] is the result calculated by subtracting the background data from the original measured data.

5-34 AA-6800/6650 Instruction


5.5 [Parameters]

[Background Data]
In the background correction mode, the background data is displayed.

[Burner Height]
When the burner is below the optical path, the value is positive. You can enter the value in 1 mm increments.
This is automatically set when the parameters are called.

[Burner Lateral]
This is used to shift the position intentionally from the burner origin adjusted in [Maintenance]. For example,
when lowering the sensitivity of a particular element intentionally in the full-auto continuous measurement of
plural elements, enter a numeric value here.

[Burner Angle]
The burner angle may be entered as a comment. The burner angle can be adjusted manually by using the
burner head angle adjustment lever.
Usually, the burner angle is zero for ordinary use. Change the burner angle only when decreasing the sensitivity
by changing the burner angle, for example, in the case of high-concentration sample.

[Set Position]
Enter the value to [Burner Height] or [Burner Lateral] and click on this button. Then the burner moves to the set
position.

[Auto Zero]
The current indicated value is shifted to zero.

[Up]
This moves the burner upward. Each time this button is clicked on, the burner height value is decreased by
1 mm.

[Down]
This moves the burner upward. Each time this button is clicked on, the burner height value is increased by
1 mm.

[Fore]
This moves the burner forward. Each time this button is clicked on, the burner moves by 1 pulse of the pulse
motor.

[Back]
This moves the burner backward. Each time this button is clicked on, the burner moves by 1 pulse of the pulse
motor.

AA-6800/6650 Instruction 5-35


Chapter 5 Functions of Operation Menu

5.5.7.2 [Burner Position Auto] Button


Clicking on this button opens the dialog box in Figure 5.32.

Figure 5.32 [Optimum Burner Height Search] Dialog Box

This automatically searches for and sets the burner height which provides the maximum sensitivity based on
the current gas flow rate setting.

[Search Range]
This sets the search range. Set the range within 0 to 25 mm.

[Current Value]
During the search, this displays the current burner height. After the search, the optimum position is displayed.

[OK]
After completing the search, click on this button to validate the burner height search result for use in
measurement. The value displayed for [Current Value] will be set.

[Cancel]
This ignores the burner height search result, and returns to the previous setting.

[Blank Meas.]
This executes the measurement of blank sample. Set a blank sample, then click on this button.

[STD Meas.]
This executes the measurement of standard sample. Set a standard sample, then click on this button.

[Stop]
This interrupts and stop the search.

5-36 AA-6800/6650 Instruction


5.5 [Parameters]

5.5.7.3 Fuel Gas Flow Rate

Figure 5.33 [Atomizer/Gas Flow Rate Setup] Page

When setting the flame type and the fuel gas flow rate, select [Fuel Gas Flow Rate] by the radio button of
[Operation Object]. Ignite a flame and introduce the sample. While monitoring the [Measured Data] indication or
real time waveform, change the fuel gas flow rate to search the optimum flow rate. After entering the [Fuel Gas
Flow Rate], click on [Flame Setup]. Then the gas flow rate is set to the value.

[Flame Type]
This is for selecting the type of support gas and fuel gas. Select the appropriate one from the drop-down list.

[Fuel Gas Flow Rate]


This is for entering the fuel gas flow rate. Enter the gas flow rate and click on [Flame Setup]. Then the gas flow
rate is set to the value. Note that the setting range of fuel gas flow rate differs depending on the type of support
gas.

[Flame Setup]
Click on this button after entering a value in [Fuel Gas Flow Rate], then the flow rate is set to the entered value.

[Auto Zero]
The current indicated value is shifted to zero.

[Increase]
Each time this button is clicked on, the fuel gas flow rate increases by 0.1 L/min.

[Decrease]
Each time this button is clicked on, the fuel gas flow rate decreases by 0.1 L/min.

AA-6800/6650 Instruction 5-37


Chapter 5 Functions of Operation Menu

5.5.7.4 [Gas Flow Auto] Button


Clicking on this button opens the dialog box in Figure 5.34.

Figure 5.34 [Optimum Gas Flow Rate Search] Dialog Box

This automatically searches for and sets the fuel gas flow rate which provides the maximum sensitivity based
on the current burner height setting.

[Search Range]
This sets [Start] and [End] of search range. The setting range of fuel gas flow rate differs depending on the type
of support gas. Set the range within 0.6 to 4.9 L/min for Air-C2H2, and 5.6 to 9.9 L/min for N2O-C2H2.

[Current Value]
During the search, this displays the current fuel gas flow rate. After the search, the optimum flow rate is
displayed.

[OK]
After completing the search, click on this button to validate the fuel gas flow rate result for use in measurement.
The value displayed for [Fuel Gas Flow Rate] will be set.

[Cancel]
This ignores the search result, and returns to the previous setting.

[Blank Meas.]
This executes the measurement of blank sample. Set a blank sample, then click on this button.

[STD Meas.]
This executes the measurement of standard sample. Set a standard sample, then click on this button.

[Stop]
This interrupts and stop the search.

5-38 AA-6800/6650 Instruction


5.5 [Parameters]

5.5.8 [Atomizer/Gas Flow Rate Setup] Page (for Flame Method by


AA-6650)
Parameters related to burner (burner height and fuel gas flow rate) are set in this screen. In the graph
displaying real time data, the right mouse button menu can be used as in the real time graph of the main
window (refer to section 4.6.5). (Only the [Properties], [Copy] and [Radar] are available.)

5.5.8.1 Atomizer Position

Figure 5.35 [Atomizer/Gas Flow Rate Setup] Page

When adjusting the burner position, select [Atomizer Position] by the radio button of [Operation Object]. Ignite a
flame and introduce the sample. While monitoring the [Measured Data] indication or real time data, change the
burner position upward and downward to search the optimum position. To change the burner height, use the
knob for adjusting burner vertical position.
Usually, the burner forward-back position is not changed. However, if the forward-back position is moved with
some reason, adjust the forward-back position referring to 6.1.1.2.

[Operation Object]
Select the item to be adjusted. Select [Atomizer Position] when adjusting the burner position. Select [Fuel Gas
Flow Rate] when adjusting the fuel gas flow rate.

[Measured Data]
The current measurement data is displayed. In the background correction modes, the indicated value as
[Measured Data] is the result calculated by subtracting the background data from the original measured data.

[Background Data]
In the background correction mode, the background data is displayed.

[Burner Height]
When the burner is below the optical path, the value is positive. You can enter the value in 1 mm increments.
Use the knob for adjusting burner vertical position to adjust the burner height.

AA-6800/6650 Instruction 5-39


Chapter 5 Functions of Operation Menu

[Burner Angle]
The burner angle may be entered as a comment. The burner angle can be adjusted manually by using the
burner angle adjustment lever.
Usually, the burner angle is zero for ordinary use. Change the burner angle only when decreasing the sensitivity
by changing the burner angle, for example, in the case of high-concentration sample.

[Auto Zero]
The current indicated value is shifted to zero.

5.5.8.2 Fuel Gas Flow Rate

Figure 5.36 [Atomizer/Gas Flow Rate Setup] Page

When setting the flame type and the fuel gas flow rate, select [Fuel Gas Flow Rate] by the radio button of
[Operation Object]. Ignite a flame and introduce the sample. While monitoring the [Measured Data] indication or
real time waveform, change the fuel gas flow rate to search the optimum flow rate. After entering the [Fuel Gas
Flow Rate], click on [Flame Setup]. Then the gas flow rate is set to the value.

[Flame Type]
This is for selecting the type of support gas and fuel gas. Select the appropriate one from the drop-down list.

[Fuel Gas Flow Rate]


This is for entering the fuel gas flow rate. Enter the gas flow rate and click on [Flame Setup]. Then the gas flow
rate is set to the value. Note that the setting range of fuel gas flow rate differs depending on the type of support
gas.

[Flame Setup]
Click on this button after entering a value in [Fuel Gas Flow Rate], then the flow rate is set to the entered value.

[Auto Zero]
The current indicated value is shifted to zero.

5-40 AA-6800/6650 Instruction


5.5 [Parameters]

[Increase]
Each time this button is clicked on, the fuel gas flow rate increases by 0.1 L/min.

[Decrease]
Each time this button is clicked on, the fuel gas flow rate decreases by 0.1 L/min.

5.5.9 [Furnace Program] Page (for Furnace Method)


This is used to display or edit the conditions such as furnace heating temperature, furnace coating with reagent
and concentration boost cycle. The furnace program may be displayed graphically in the screen. In the graph
displaying real time waveform, the right mouse button menu can be used.

Figure 5.37 [Furnace Program] Page

[Temp.] and [Time]


Enter the furnace target temperature (0 to 3000 qC) and heating time (0 to 300 seconds).

[Heat Mode]
Select "RAMP" or "STEP" by double-clicking. When [RAMP] is set, the target temperature is attained at the end
of this stage using fixed uniform heating throughout the stage. When [STEP] is set, heating is conducted so as
to attain the target temperature immediately and maintain that temperature until the end of the stage.

[Sensitivity]
A high-sensitivity measurement is enabled by controlling the inner gas flow during the sample atomization.
[Sensitivity] is a switch to set a high-sensitivity mode. To perform a high-sensitivity measurement, put a
checkmark to the sensitivity field of atomization stage (at this time, the [Flow Rate] is fixed to 0 L/min) and
delete checkmarks from other stages.
In the report printing, this sensitivity switch status may be indicated as "HIGH" when it is [On], and as
"REGULAR" when it is [Off].

AA-6800/6650 Instruction 5-41


Chapter 5 Functions of Operation Menu

[Gas Type]
Select "#1" or "#2" by doubleclicking. The GFA-6500 incorporates 2 gas line systems. Select the gas line
system which you are going to use. Heating may be conducted by switching the gases at each stage. For
example, when analyzing samples in an organic solvent, connecting oxygen to the Gas #2 line will allow you to
use oxygen during the ashing stage to completely combust the organic materials.
The gas lines are specified as follows.
#1: Ar on GFA rear panel
#2: ALT on GFA rear panel
When #2 is to be used, verify that gas tubing is connected to the ALT connector. Only Ar can be used for #1.

[Flow Rate]
This sets the inner gas flow rate in the range of 0 to 1.5 L/min (0.1 L/min increments). When [Sensitivity] is
check-marked, this is fixed at 0 L/min. The outer gas flow rate is fixed.

[Sample]
Select "ON" or "OFF" by doubleclicking. When set to "ON", data is acquired during the heating time of that
stage. Normally, this is set to "ON" in the atomization stage. Note that the "ON" setting can be used for only one
stage.

[Max. No. of Stages]


Enter a numeric value (up to 20). The heating stages as many as the number can be programmed.

[Sampling Stage No.]


The data sampling is performed during the heating time of the stage specified here. Usually, the atomization
stage is specified.

[Graphite Tube Type]


Select a type of graphite tube. Note, however, that the setting here has no effect on actual instrument operation.
This is used only to be printed as a measurement parameter on the report.

[Load]
A furnace program file (*.fur) which has been already created can be loaded. Clicking on this opens [Open]
dialog box. Specify [Look in] and [File name] and click on [Open].

[Save]
The furnace program created in [Furnace Program] page is saved with a new file name. Clicking on this opens
the [Save As] dialog box. Specify [Save in] and [File name] and click on [Save].

[Insert Row]
A row is inserted just before the selected row in the furnace program.

[Delete Rows]
The selected row in the furnace program is deleted.

5-42 AA-6800/6650 Instruction


5.5 [Parameters]

5.5.9.1 [Coating/Boost Cycle] Button


Clicking this button opens the [Coating and Boost Cycles] dialog box.

Figure 5.38 [Coating and Boost Cycles] Dialog Box.

Coating refers to injecting a specified reagent into the furnace and drying it prior to the sample injection (coating
the tube surface). First, the check-marked reagent is injected in the furnace, and heating is executed up to the
furnace program stage specified in [Last Coating Cycle]. After this, the sample is injected.
Furnace boost cycle refers to the repetitive cycle of sample injection into the furnace, and drying and ashing of
the sample in order to raise the concentration of the target element in the sample. Repeating this boost cycle
enables measurement of the sample whose concentration is lower than the quantitation range by concentrating
it and raising its absorbance to the quantitative range of the calibration curve.

[Coating by Reagent]
This specifies a reagent to be injected into the furnace and dried prior to the sample injection.
The reagent volume used for coating is displayed/printed in parentheses on the MRT or data print to show that
this volume is not used for sample preparation.

NOTE
The coating setup is saved for each row on the MRT. This setup is reflected on the row when a new row is
added on the MRT or when the sample or reagent volume is edited on the MRT. To change the coating
setup for each row directly, use [Collective Edit] from [Edit] menu.

[Last Coating Cycle]


This specifies the stage to which the injected preceding reagent is heated and dried up in the furnace program.

[Number of Boost Cycles]


This specifies the number of boost cycles. In normal analysis without boost cycles, set this value to "1".

AA-6800/6650 Instruction 5-43


Chapter 5 Functions of Operation Menu

[Last Boost Cycle]


Enter the last stage number of boost cycle. From the sample injection stage #1 to the last stage specified here,
the concentration is boosted by the heating process for the specified number of sample injections. Note that a
data sampling stage cannot be included during the concentration boost cycles.

[Coating Reagent]
This displays reagents to be injected precedent to coating and their intake order to the ASC if plural reagents
are used.

[Sample]
This displays reagents to be injected together with the sample and their intake order to the ASC.

(Setup Example)
Coating by Reagent: Reagent 1, Reagent 2
Last Coating Cycle: 2
Number of Boost Cycles: 3
Last Boost Cycle: 4
Sampling Stage #: 6

With the above setting, the furnace program proceeds as below.


Injection of Reagent 1 and Reagent 2 o Stage 1 o Stage 2 o
Injection of Sample, Dilutent and Reagent 3 o Stage 1 o Stage 2 o Stage 3 o Stage 4 o
Injection of Sample, Dilutent and Reagent 3 o Stage 1 o Stage 2 o Stage 3 o Stage 4 o
Injection of Sample, Dilutent and Reagent 3 o Stage 1 o Stage 2 o Stage 3 o Stage 4 o
Stage 5 o Stage 6 (Measurement)

5.5.9.2 [Test Meas.] Button


Clicking on this button opens the [Test Measurement] dialog box.

Figure 5.39 [Test Measurement] Dialog Box

A test measurement is conducted in the [Test Measurement] dialog box to check whether the furnace program
is appropriate or not. A peak profile of measurement result is displayed in the graph on the screen, but the data
is not acquired.
In the [Test Measurement] dialog box, you can select either of manual measurement or autosampler
(measurement) by clicking on the radio button. When selecting the autosampler (measurement), enter the
position of test sample and the preparation parameters. When completing the settings, click on [Measure]. To
rinse the mixing port, press the [Rinse] button. The [Rinse] button is displayed only when the [Mixing] is set to
ON in the ASC parameters.

5-44 AA-6800/6650 Instruction


5.5 [Parameters]

5.5.9.3 [Cleaning] Button


Clicking on this button opens the [Cleaning] dialog box.

Figure 5.40 [Cleaning] Dialog Box

When [Start] is pressed, the graphite tube is baked for cleaning according to the built-in heating program. Use
[Test Measurement] together, if necessary.

5.5.9.4 [Change Graphite Tube] Button


Clicking on this button opens the [Change Graphite Tube] dialog box.

Figure 5.41 [Change Graphite Tube] Dialog Box.

[Graphite Tube Heat Cycle Count]


This indicates the heating times of the graphite tube. This number increases every after the tube is heated. After
changing the graphite tube, reset it to "0".

[Change Graphite Tube]


This starts the procedure for changing the graphite tube and adjusting the sample injection position of ASC
nozzle.

[Graphite Tube Conditioning]


A new pyrolytic coating graphite tube and a new platform tube must be heated repeatedly for conditioning. Be
sure to perform the conditioning after a replacement for a new pyrolytic coating graphite tube (or a new platform
tube). This conditioning is not necessary for high density graphite tube. After the conditioning, "10" is added to
the furnace heating number.

[Stop Tube Conditioning]


This stops the heating cycle of conditioning. Note, however, that "10" is added to the furnace heating number
even if the conditioning is quitted halfway.

AA-6800/6650 Instruction 5-45


Chapter 5 Functions of Operation Menu

[Auto Temp. Calib.]


To obtain a precise temperature control in low temperature range, the heating temperature of the graphite tube
is calibrated using an optical temperature sensor. Execute the temperature calibration immediately after
replacing the graphite tube, or after executing the conditioning of pyrolytic coating graphite tube (or platform
tube).

5.5.9.5 [Temp. Search] Button


Clicking on this button opens the dialog box in Figure 5.40. Here, the measurement is automatically performed
while changing the heating temperature condition little by little, and the data is automatically plotted in the graph
on the screen. With this function, optimum atomization and ashing temperatures can be searched. In both of the
right and left graphs on the screen, the right mouse button can be used.

Figure 5.42 [Optimum Furnace Program Search] Dialog Box

[Objective Stage]
Enter the stage No. for searching the heating temperature.

[Single Stage] [2-Stage Link] [3-Stage Link]


Successive stages up to 3 can be selected for search. Use the radio button for selection.
This is used, for example, to set an ashing temperature when using a RAMP heating stage to raise it to a
particular temperature and using a STEP heating stage to maintain the temperature.

[Start] and [End]


Set the search range.

[Step Width]
Enter the increment step for search to change the heating temperature.

5-46 AA-6800/6650 Instruction


5.5 [Parameters]

[Current Value]
Current temperature of the objective stage in the furnace program is indicated.
In the temperature search measurement, you can select either of [Manual Measurement] or [Autosampler]
(measurement) by clicking on the radio button. When selecting [Autosampler] (measurement), enter the
position of test sample and the preparation parameters. When completing all the settings, execute the
measurement. The measurement result is plotted in the right graph on the screen. Judge the optimum heating
temperature from this graph. The peak profiles are overwritten in the graph in center.

[Measure]
Before starting the measurement, the temperature calibration is executed. Note that heating is performed when
the temperature calibration is executed. After setting the sample, click on this button.

[Stop]
This stops the search.

NOTE
After finding the optimum heating temperature, it is necessary to set and edit the table in [Furnace Program]
page.

AA-6800/6650 Instruction 5-47


Chapter 5 Functions of Operation Menu
5.6 [Edit Parameters]

Executing this opens the [Edit Parameters] dialog box. This is used to set each parameter individually without
using Wizard. In this case, you can change the settings for the element of the MRT worksheet which you can
select by clicking on the tab in the left lower of the main window.

NOTE
In the [Edit Parameters] dialog box, you can make a change or reference only for the element selected on
the MRT worksheet.

When completing the setup for all the pages, click on [OK]. To cancel the setting halfway, click on [Cancel].
Then the settings return to the previous conditions before changed.

5.6.1 [Measurement Parameters] Page


Figure 5.43. is displayed. The displayed contents are different according to the selection of flame/furnace.

Figure 5.43 [Measurement Parameters] Page

(The upper figure is for flame measurement and the lower one is for furnace measurement.)

5-48 AA-6800/6650 Instruction


5.6 [Edit Parameters]

Flame
At the start of sample suction, the signal is not stable. The time required for introducing sample to the flame until
the signal becomes stable is referred to as pre-spray time.

Pre-Spray (Time) Integration Time

Figure 5.44 Pre-Spray and Integration Time

[Repetition Sequence]
This will set whether pre-spray is conducted during repeat measurement. There are 2 types of settings.
(S: Spray, M: Measure)
SM-SM-.. In repetition sequence, pre-spray is conducted prior to each repetition of sample
measurement.

Figure 5.45 Repetition Sequence (SM-SM-...)

SM-M-M-... In repeat measurement, pre-spray is conducted only prior to the first repetition of sample
measurement. Select this type when it is appropriate to continue spraying sample throughout
the repeat measurements.

Figure 5.46 Repetition Sequence (SM-M-M-...)

AA-6800/6650 Instruction 5-49


Chapter 5 Functions of Operation Menu

NOTE
In the case of automatic measurement with the ASC, the instrument always operates as "SM-M-M-..." even if
"SM-SM..." is selected as the repetition sequence.

[Pre-Spray Time] and [Integration Time]


Enter the time interval to be used for pre-spraying and for signal integration (measurement time). The
integration time (measurement time) will start directly after elapse of the pre-spray time. There is no integration
of the signal during the pre-spray.

[Response Time]
This selects the time constant of signal response. The time constant of signal response corresponds to time
constant set for [Real Time Graph Monitor]. That is to say, the signal profile displayed on the graph is affected
by the response. In the case of #1, the profile is close to the actual signal profile. As the value increases from #1
to #4, the profile becomes more and more processed, as if a filter is applied.
When excessive noise is a problem, settings in the direction of #4 will provide better repeatability.

NOTE
[Pre-Spary Time] must be changed depending on the property of the sample. For example, take long [Pre-
Spray Time] for sample with viscosity. If the absorbance of the sample is low, and liable to be affected by
noise, take a long [Response time]. In this case also, since it takes a long time to become stable after spray
of the sample, set the following time as [Pre-Spray Time] in standard operation.

Time until stabilization


Response Time 1: 3 sec.
Response Time 2: 5 sec.
Response Time 3: 10 sec.
Response Time 4: 20 sec.

Furnace
[Signal Processing]
As a measured value, you can select the peak height or peak area of the obtained waveform.

5-50 AA-6800/6650 Instruction


5.6 [Edit Parameters]

5.6.2 [Repeat Measurement Conditions] Page


Number of repeat measurements is set here.

Figure 5.47 [Repeat Measurement Conditions] Page

[Blank]
This row is for setting the repeat conditions for blank measurement.

[Standard]
This row is for setting the repeat conditions for standard measurement and standard addition measurement.

[Sample]
This row is for setting the repeat conditions for unknown sample measurement and simple standard addition
measurement.

[Reslope]
This row is for setting the repeat conditions for sensitivity correction measurement.

[Num. of Reps.] and [Max. Num. of Reps]


The number of repetitions refers to the minimum number of measurement repetitions to be used in acquiring
data. After completing this set number of measurement repetitions, the average value, relative standard
deviation (RSD) and standard deviation are calculated. Then, the measurement repetitions will continue until (1)
the RSD value limit is satisfied, (2) the standard deviation limit is satisfied, or (3) the maximum number of
repetition is reached.
Setup is possible up to 20 for each item.

AA-6800/6650 Instruction 5-51


Chapter 5 Functions of Operation Menu

[RSD Limit] and [SD Limit]


Both the RSD (Relative Standard Deviation) limit and the SD (Standard Deviation) limit are indicators of data
scattering. If these values are small enough, the data is considered to be stable and the measurement results
reliable.
Normally, set the SD limit value to "0" and use only the RSD limit. However, since the average value is used as
the denominator for the RSD limit, as shown in the following equations, a small value is difficult to attain when
samples of low concentration are measured. In such cases, use the SD limit in addition to the RSD limit.
After the set repetition number [Num. of Reps] is over, the average value, RSD and SD are calculated using the
combination of set number of measured data which provides the smallest amount of data scattering.
n: Number of measurement data
Xi: Measured data (i = 1 to n)

Average value: μ= ΣXi


n

SD: nΣXi2 − (ΣXi)2


σ=
n (n-1)

RSD: RSD = σ
μ × 100 (%)

5-52 AA-6800/6650 Instruction


5.6 [Edit Parameters]

5.6.3 [Weight Correction Factors] Page


The following are set here.
• Factors used in actual concentration calculation
• Actual concentration unit
• Decimal place of the factors and actual concentration to display and print

Figure 5.48 [Weight Correction Factors] Page

NOTE
Actual concentration is calculated with the following equation.
Actual Conc. = (Measured Conc.) u [Volume Factor] u [Dilution Factor] u [ASC Dilution Factor] u [Correction
Factor] / [Weight Factor]
However, there is no particular function to set units for [Weight Factor] and [Volume Factor]. Note that the
entered values are only calculated using the above equation. Use [Correction Factor] to convert the unit.
[ASC Dilution Factor] is a value automatically set by the software to correct a change of the actual dilution
factor when the preparation parameters are changed automatically by the software in the case of "Auto
dilution and Remeasurement" (refer to 5.6.9 (4)).

[Weight Factor]
Enter the sampling weight or sampling volume.

[Volume Factor]
Enter the weight or volume after the sample is dissolved or processed and brought up to a specific volume.

[Dilution Factor]
Enter the dilution factor when the sample solution is diluted after brought up to the above specific volume.

AA-6800/6650 Instruction 5-53


Chapter 5 Functions of Operation Menu

[Correction Factor]
Arbitrary factor necessary for unit conversion can be set.

[Actual Conc. Unit]


Enter a unit for actual concentration.

[Decimal Place]
Set a decimal place for displaying and rounding [Weight Factor], [Volume Factor], [Dilution Factor], [Correction
Factor] and [Actual Conc]. This decimal place is used for actual concentration calculation, the display on the
screen and data print.
In the case of [Auto Dilution] (Dilution factor for automatic dilution and remeasurement), the decimal place is
fixed to "6" for both the display and actual concentration calculation.

5.6.4 [Y-axis Print Range] Page


Enter the graph scale to print the peak profile with [File]-[Print Data/Parameters...].

5.6.5 [Analyst] Page


Enter the analyst name and file comment.
They are output when printing the parameter, and saved together with the file.

5.6.6 [Comment] Page


Comment is added to the element name. When the same element is measured with different parameters, you
can identify them with this comment. This comment is displayed in the element combo box on the main window
and on the MRT worksheet tab together with the element name. Up to 10 characters can be displayed on the
tab. If a line feed is included, however, only the characters before the line feed are displayed.

5-54 AA-6800/6650 Instruction


5.6 [Edit Parameters]

5.6.7 [Sequence] Page

Figure 5.49 [Sequence] Page

[Using ASC]
Put a check mark in the check box when using the ASC.

[At the End of Measurement]


When measuring plural elements successively, you can select to stop the measurement once at the end of
each element or to continue the measurement.

[Lamp Warmup Time]


Set the hollow cathode lamp warmup time, which is a waiting time after lighting on the lamp and before starting
the measurement, in the unit of minute.
To select the lamp warmup time, check the time from lighting the lamp to stabilizing the signal while observing
the real time graph in the flame measurement. Usually it is set to 5 to 30 minutes depending on the element and
the lamp condition such as deterioration degree.

AA-6800/6650 Instruction 5-55


Chapter 5 Functions of Operation Menu

5.6.8 [ASC Parameters] Page


This page is displayed only for the furnace method.

Figure 5.50 [ASC Parameters] Page

[Rinse with Sample]


This sets the type of rinsing to be conducted in this mixing port prior to mixing. Rinsing with sample refers to the
use of sample to rinse the mixing port based on the set mixing conditions, after first rinsing with rinse liquid. This
sample liquid is discarded and is not used for measurement. This method is used in high accuracy
measurement to prevent the diluting of measurement sample with the very small amount of rinse liquid
remaining after rinsing with rinse liquid. With this method, however, the rinse time is doubled and the amount of
sample required is increased.

[Mixing ON]
If a check mark is put in the check box, the sample and reagent are mixed after being introduced into the mixing
port.

[Intake Speed] and [Discharge Speed]


When the ASC-6100 is connected, the setting of [Intake Speed] is ignored. Mixing strength is set by [Discharge
Speed]. Change the setting if necessary while considering the sample viscosity. Ordinarily, "150" is appropriate.
This parameter is valid only when the [Mixing ON] is check-marked.

[Volume]
When the mixing is ON, the volume of mixed sample set here is drawn into the ASC nozzle and injected into the
graphite tube. Determine the injection volume in consideration of the total volume of mixed sample in the mixing
port and the maximum number of repeat measurement. When mixing is set to OFF, the [Total Vol] (PL) in the
sample preparation parameters becomes the volume to be injected into the graphite tube.

5-56 AA-6800/6650 Instruction


5.6 [Edit Parameters]

[Speed]
This sets the speed at which the sample is injected into the furnace. The default value is 25 (PL/sec).

[Diluent/Reagent Name and Position]


The ASC-6100 can mix one diluent and three reagents automatically. Set the prepared reagents on the
turntable and enter the position number.

NOTE
When [NONE] is selected for the reagent position, the reagent is not used in the setting and not displayed on
the MRT, and it is excluded from the calculation of total volume of the preparation. This change has an effect
on the entire one schedule. If the reagent position is changed to or from [NONE] in the middle of the
schedule measurement, the displayed/printed total volume in the sample data already measured is also
changed to be different from the actual volume. Therefore, when quitting a use of the reagent in the middle of
one schedule, do not use [NONE] but set the reagent volume to zero.

[Intake Order]
This specifies the intake order of sample and reagents to the ASC nozzle. The order can be changed using the
upward/downward arrow keys. The upper one is taken in (to the ASC earlier and injected later). Set the order
considering the mixing of the reagents and sample.

5.6.9 [QA/QC Setup] Page


In this page, select the ON/OFF of checking with each QC type, set the standard value, and select the action
when the result is out of standard range.

NOTE
After the data evaluation based on the QA/QC setup is executed, the calibration curve order, zero intercept
and signal processing mode settings cannot be changed after the measurement. When these settings are
expected to be changed after the measurement, set all the check boxes to OFF before starting the
measurement.

Figure 5.51 [QA/QC Setup] Page

AA-6800/6650 Instruction 5-57


Chapter 5 Functions of Operation Menu

(1) The followings are the QC types.


Correlation coefficient (= r)
This factor indicates the degree of agreement of the measured point (data) with the calibration curve
obtained by the least squares method. A value closer to "1" is desirable.
The "r" is calculated using the following equation.

r= NΣxiyi − ΣxiΣyi
[NΣxi2 − (Σxi)2] [NΣyi2 − (Σyi)2]
1 1
2 2

Put a check mark in this check box, and set "CAL-CHK" in [Action] field after a series of STD
measurements on the MRT worksheet to execute the evaluation by correlation coefficient.

NOTE
"CAL-CHK" setting is necessary only in the calibration curve method. In standard addition method and
simple standard addition method, this setting is not necessary because the evaluation is done at "MSA-
RES".

LCS (QC Standard)


(Laboratory Control Sample: Evaluation by standard sample)
This is the evaluation using a standard sample with known concentration. The ratio between certified value
and obtained value is calculated for evaluation.

Concentration
%R = u 100
True Value
In this case, "True Value" means a certified value. Set this value in [True Value] field on the MRT
worksheet. Put a check mark in this check box, and set "QC" in [Action] field on the MRT worksheet to
execute the evaluation by LCS.

SPK (Spike)
(Pre-Digestion Spike: Addition and recovery without pretreatment)
This evaluates the recovery degree of the amount added to the sample. It is calculated by the following
equation.

%R = SSR − SR × 100
SA
SR: Measured result of sample without addition ([Conc.] value of UNK on the MRT worksheet)
SSR: Measured result of sample with addition ([Conc.] value of SPIKE on the MRT worksheet)
SA: Amount of addition (Calculated value) (Enter this value in [True Value] field of SPIKE on the
MRT worksheet)
Put a check mark in this check box, and set "SPIKE" in the [Action] field after "UNK" whose recovery
degree you wish to get on the MRT worksheet. It executes the evaluation by SPK.

Sample Upper Limit


Put a check mark in the [Sample Upper Limit] check box, the software evaluates whether the concentration
of each sample is within the standard value.

5-58 AA-6800/6650 Instruction


5.6 [Edit Parameters]

%RSD (Relative Standard Deviation)


Put a check mark in the [%RSD] check box, the software evaluates whether the deviation of repeat
measurement results of each sample is within the standard value.

NOTE
[RSD Limit] and [SD Limit] on the [Repeat Measurement Conditions] page are used as the standard value of
%RSD.

(2) The default (initial) standard values displayed on the screen are the values recommended by EPA (United
States Environmental Protection Agency) method. However, the values can be changed.

(3) Also, in the [Out of Control Remark], you can set [Stop Measurement] or [Mark and Continue] when each
QC type value exceeds the range of standard value. Only for the [Sample Upper Limit], you can select
[Auto Dilution and Remeasurement] in addition to [Stop Measurement] or [Mark and Continue].

NOTE
[Auto Dilution and Remeasurement] is valid only in furnace measurement.

(4) Auto Dilution and Remeasurement


The function of auto dilution and remeasurement is described here.
The auto dilution and remeasurement is a function to change the ASC preparation parameters
automatically and perform a remeasurement so that the concentration may be near the center of the
calibration curve (mean value of the highest and lowest concentrations of the standard sample). The
change of preparation parameters at this time is automatically reflected on the [Auto DF] value in the MRT
to correct the actual concentration calculation value.
The actual functions are as below.
1. The ratio of the current value to the concentration of calibration curve center is obtained as an integral
number.
2. When the order of the calibration curve is 2nd, and if the absorbance exceeds the top of the 2nd order
equation and the concentration cannot be calculated, the above integral number is set to "10".
3. The sample volume is reduced according to the auto-dilution ratio.
When the sample volume is reduced to the minimum value 2 PL,
a. the value is used as it is when [Mixing] is OFF.
b. the diluent volume and reagent volume are increased when [Mixing] is ON.
In addition to the limitation that the minimum sample volume is 2 PL when [Mixing] is OFF, the
following items are also limited.
(1) The maximum auto-dilution factor is "100".
(2) When the solution of the 2nd-order calibration curve equation is not found, the 10-time dilution
is not repeated.

AA-6800/6650 Instruction 5-59


Chapter 5 Functions of Operation Menu

5.6.10 [Calibration Curve Parameters] Page

Figure 5.52 [Calibration Curve Parameters] Page

[Order]
Select an order of calibration curve equation. You can select 1st, 2nd or 3rd.

[Zero Intercept]
Putting a check mark in the check box will create the calibration curve equation that forcibly intercepts the
origin. When the standard addition method or simple standard addition method is selected, setup is made
automatically to "1st" and "no zero intercept", and these items are not displayed.

Correlation Coefficient calculation of calibration curve when Zero Intercept is selected


When the order of the calibration curve is 1st, the correlation coefficient of the calibration curve is not
changed by changing the selection of zero intercept. This may seem unnatural, but can be understood as
follows.
The correlation coefficient shows the relation of "increasing way" of two quantities. When the order of the
calibration curve is 1st, the increase is linear whether the zero is intercepted or not. Therefore, the relation of
increasing way is also not changed (the slope of linear line has no relation with "Correlation").

[Conc. Unit]
Unit of concentration used in MRT worksheet is set here.

5-60 AA-6800/6650 Instruction


5.6 [Edit Parameters]

5.6.11 [Optics Parameters] Page


The contents are the same as the [Optics Parameters] page in Wizard (refer to 5.5.6).

5.6.12 [Atomizer/Gas Flow Rate Setup] Page (Flame Method)


The contents are the same as the [Atomizer/Gas Flow Rate Setup] page in Wizard (refer to 5.5.7, 5.5.8).

5.6.13 [Furnace Program] Page (Furnace Method)


The contents are the same as the [Furnace Program] page in Wizard (refer to 5.5.9).

AA-6800/6650 Instruction 5-61


Chapter 5 Functions of Operation Menu
5.7 [Default Parameters]

This sets the parameters which are read in as initial values when creating a new file. The parameters for QA/
QC setup, calibration curve parameters, repeat measurement conditions, measurement parameters and
sequence can be set here.
Contents and operation of each page are completely the same as those of the property sheet. Refer to section
5.6.

5.7.1 [Flame]
The property sheet for flame default parameters is opened.

5.7.2 [Furnace]
The property sheet for furnace default parameters is opened.

5.7.3 [Graph]
The [Graph Default Scale] dialog box is opened. The ordinate scale and the time width for real time graph can
be set here.

Figure 5.53 [Graph Default Scale] Dialog Box

5.7.4 [Analyst]
The [Default Analyst] dialog box opens. Enter [Analyst] and [File Comment] newly, then the entered contents
are used when creating a new file next time.

5-62 AA-6800/6650 Instruction


5.8 [Instrument]
5.8 [Instrument]

The functions related to instrument hardware are summarized in this menu.

Figure 5.54 [Instrument] Drop-Down Menu

AA-6800/6650 Instruction 5-63


Chapter 5 Functions of Operation Menu

5.8.1 [Connect]
If this menu is selected, communication between the instrument and personal computer will be performed. After
starting communication, first [Initialize] screen is displayed, where the instrument information (model, ROM
version, serial No.) of AA/ASC/GFA and the progress of hardware initialization is sequentially displayed. Item
under check is indicated in yellow, items successfully completed are indicated in green, items with failure are
indicated in red. In takes several minutes to finish the initialization.
The item [Start Leak Check] is displayed on the [Initialize] screen when the instrument applicable to a flame
measurement (AA-6800F/AA-6650F) is initialized.
Since a message prompting to check the fuel/support gas set pressure and the fuel gas flow rate is displayed
before executing this item, check them when a flame measurement is to be used (refer to section 3.1.6).
If all items are indicated in green, the initialization is correctly completed. Click on the [OK] button to close the
screen. The items of [ASC Check] and [GFA Check] are indicated in red even if they are not connected with the
AA main unit. When the ASC or GFA is not used from the first, it doesn't mean an abnormal status.
When the communication is performed again while the power of instrument is ON, the slit, turret, burner up/
down, burner fore/back and C2H2 valve are not checked. Also, when the gas leak check has been already
finished, the gas leak check is not started and the item is indicated in green.
In the case of AA-6800G or AA-6650G, the indications of C2H2 valve origin search, gas leak check start, gas
pressure monitor ON and flame monitor ON are not displayed.
In the case of AA-6650, the items [Atomizer Up/Down] and [Atomizer Fore/Back] are not displayed.

Figure 5.55 [Initialize] Screen

5-64 AA-6800/6650 Instruction


5.8 [Instrument]

After the [Initialize] screen is closed, [Instrument Check List for Flame Analysis] is displayed.

Figure 5.56 [Instrument Check List for Flame Analysis]

This screen is always displayed when the instrument applicable to a flame measurement (AA-6800F/AA-
6650F) is used (except when the GFA is connected and the gas leak check was not started).
To use the instrument safely, always check these items displayed on this screen before igniting a flame. Put a
check mark to the item already checked. When all the items have been checked, [OK] can be selected.

5.8.2 [Option Connect]


This indicates the connection status between the AA main unit and the peripheral attachments (ASC, GFA).

Figure 5.57 [Option Connect] Screen

[Connect]
Click on this button when turning on the power of peripheral attachment (ASC, GFA) after the communication
between the personal computer and AA main unit are completed.

AA-6800/6650 Instruction 5-65


Chapter 5 Functions of Operation Menu

5.8.3 [Configuration]
The PC communication port and the type of AA main unit are set here. Selecting this menu opens
[Configuration] dialog box.

Figure 5.58 [Configuration] Dialog Box

[COM Port]
The communication port on the PC is set here. Set the number of port to which the communication cable with
the AA main unit is connected.

[Instrument Type]
This indicates the AA main unit model with which this software can be connected.

[Check instrument type at initialization]


Putting a check mark in the check box will give an alarm if the connected instrument is different from
[Instrument Type].

[Flame ASC Rinse Time]


Enter a numeric value from 0 to 600 (seconds). When a numeric value except "0" is entered, the ASC executes
the rinse for every sample.

5-66 AA-6800/6650 Instruction


5.8 [Instrument]

[Flame ASC Autozero in Rinsing]


This function is used to set the baseline to zero frequently in the flame measurement with ASC.
When this check box is set to ON, the auto zero is executed every after the rinse for each sample while keeping
the rinse liquid suctioned. For example, when [Flame ASC rinse time] is set to "10 seconds", the auto zero is
executed (for 10 seconds) after executing the rinse for 10 seconds. So the rinse liquid is aspirated for approx.
20 seconds in total.

NOTE
If the auto zero is executed with an insufficient rinse, the zero set is executed before the signal has not go
back to the base, as the result, the measurement cannot be performed properly after that. Before using this
function, check that the signal in the real time graph goes down to the base within the time set in [Flame ASC
rinse time].

[Action setup when measurement is finished]


This sets the [Automatic Flame Extinction Yes/No] and [Automatic Lamp Extinction Yes/No] when the
measurement is finished. This action is also applied when [Stop] is selected for switching the element in
measuring plural elements. This is valid only when using ASC.

[Action setup when measurement is stopped]


The measurement is stopped by QA/QC judging process. In this case, you can set [Automatic Flame Extinction
YES/NO] and [Automatic Lamp Extinction YES/NO]. These are valid only when using ASC.

[Automatic Flame Extinction]


Put a check mark in the check box to extinguish the flame automatically.

[Wait Time]
Enter a numeric value (minute) to wait before extinguishing the flame. In the automatic continuous
measurement using the ASC and HVG, the hydrides are generated for a while after the measurement. If these
hydrides are left in the absorption cell, the life of the absorption cell will be shortened. In order to purge the
hydrides remaining in the cell, it is necessary to heat the absorption cell for a while after the measurement.
Usually, 3 minutes is sufficient.

[Automatic Lamp Extinction]


Put a check mark in the check box to turn off the lamp automatically.

AA-6800/6650 Instruction 5-67


Chapter 5 Functions of Operation Menu

[Show Instrument Check List for Furnace Analysis]


When this check box is set to ON, the list of the items to be noted before the furnace measurement is displayed
at the start time of the software.

Figure 5.59 [Instrument Check List for Furnace Analysis]

[Show performing temp. calib. warning message at start of furnace measurement]


The temperature calibration is executed when starting the furnace measurement with the [Start] button in the
main window or when starting the optimum furnace program search.
When this check box is check-marked, a message appears to indicate a caution on executing this temperature
calibration program or heating the furnace. When the check mark is deleted, the message is not displayed, but
the temperature calibration itself is always executed.

[Show lamp used time over operating life message]


Put a check mark in the check box to check whether the lamp used time is over the specified lamp life or not.

[Use Rounded ABS for calculation]


The absorbance data is displayed or printed down to the fourth decimal place. The absorbance data kept in the
internal memory is a little more precise. When [Use Rounded ABS for calculation] is check-marked, the
displayed rounded value is used for the calculations such as "Average", "% RSD value", "Standard deviation",
"Calibration curve polynomial expression" and "Quantitation of unknown sample". When the check mark is
deleted, the value kept in the internal memory is used for these calculations.
Although the calculation is performed more precisely when the check mark is deleted, the value kept in the
internal memory cannot be known instead. As the result, the WizAArd software processing is like a black box,
and the calculation process cannot be verified from the outside. If [Use Rounded ABS for calculation] is check-
marked, the processing contents in the WizAArd software can be verified by a manual calculation with a
calculator.

5-68 AA-6800/6650 Instruction


5.8 [Instrument]

CAUTION
If this setting is changed, the calibration curve and quantitation result of the measured data are also
changed. Take note of this when changing the setting. When [Rounded absorbance is used for calculation]
and [Decimal place] are changed, the calibration curve and quantitation results of the data measured before
will be changed. Also, if the QA/QC judgement is already executed at the time of data acquisition, the file of
the data cannot be read in. Note this when changing these settings. In both cases, to recover the data at the
time of the measurement, read in the file after changing the rounding settings back to the original ones used
at the time of measurement.

[Decimal place]
This sets a decimal place to which the absorbance is rounded.
The rounding method is as follows.
When the figure below the specified place is just "5", it is rounded down if the specified figure is even and
rounded up if the specified figure is odd. In other cases, it is rounded off normally.

Example: When the specified decimal place is 4


• Average between 0.1234 and 0.1235 is calculated as follows.
(0.1234 + 0.1235) y 2 = 0.12345000  o 0.1234
• Average between 0.1233 and 0.1234 is calculated as follows.
(0.1233 + 0.1234) y 2 = 0.12335000  o 0.1234

[Show meas. file created by older version WizAArd message]


When an old measurement file created in old version WizAArd (ver.1.x) is opened, the values such as
absorbance and concentration on the MRT worksheet are not completely compatible and may have some
differences in decimal fraction. To keep a complete compatibility, it is necessary to open the measurement file
from the old version WizAArd in which the file was created.
To check whether the measurement file was created in old version WizAArd or not, set the [Show meas. file
created by older version WizAArd message] check box to ON. Then a message appears when an old
measurement file is opened.

AA-6800/6650 Instruction 5-69


Chapter 5 Functions of Operation Menu

5.8.4 [Lamp Position Setup]


Selecting this menu opens the [Lamp Position Setup] dialog box. Enter the element symbol to be set to each
socket number. "*" is used as a wild card. When using multi-element lamp, enter "*" instead of the element
symbol. Clicking on the cell of the [Element] opens the drop-down list, from which you can select the element.
Set the correct type of hollow cathode lamp to be used in [Lamp Type].
Setting the element and lamp type allows you to select a lamp ID in [Lamp ID] field. Select the lamp to be used.
Selecting the lamp displays the judgement whether the lamp life is over or not, lamp life, used time and unit of
used time.
When the unit of the used time is mA*hrs, the use degree is calculated by the lamp current and the lighting time.
When the lamp is lit at 10 mA for 10 hours for example, the used time is as follows.
10 (mA) u 10 (hrs) = 100 (mA*hrs)
When the unit of used time is hrs, the lighting hour is directly used, and the use degree is 10 (hrs) in this
example.
If there is no item to select in [Lamp ID] field after you specify the element and lamp type, register the data for
the lamp in the [Lamp History] dialog box (refer to section 5.8.5).
To clear the selected lamp, select [None] at the top of the drop-down list.
Editing is not available for the lamp which is lit on. Turn off the lamp before editting.

[OK]
This closes the dialog box after changing and saving the lamp position setting. At this time, if the lamp whose
use time exceeds the lamp life is selected, a warning message for checking appears.

[Cancel]
This cancels changing the lamp position setup and closes the dialog box.

[Print]
This prints the table of lamp position setup.

Figure 5.60 [Lamp Position Setup] Dialog Box

5-70 AA-6800/6650 Instruction


5.8 [Instrument]

5.8.5 [Lamp History]


Selecting this menu opens the [Lamp History] dialog box to register/delete/edit the lamp informations for the
lamp life management in the data base.

Figure 5.61 [Lamp History] Dialog Box

A new lamp can be registered by entering a new lamp ID in [Lamp ID]. Firstly, set the element of the lamp in
[Element]. The "*" mark is used as a wild card. When using a multi-element lamp, enter "*" instead of element
symbol. Also, an element can be selected from the drop-down list opened by clicking [Element]. In [Lamp Type],
select the correct type of the hollow cathod lamp to be used. Next, set [Lamp Life] and [Unit] referring to the
manuals provided with the lamp to be used. The unit can be selected from "mA*/hrs" and "hrs". In the case of
SR lamp, however, the unit is fixed to "hrs". Use [Comment] freely for anything such as date.
When the unit of the used time is "mA*hrs", the use degree is calculated by the lamp current and the lighting
time. When the lamp is lit at 10 mA for 10 hours for example, the use degree is as follows.
10 (mA) u 10 (hrs) = 100 (mA*hrs)
When the unit of used time is "hrs", the lighting hour is directly used, and the use degree is 10 (hrs) in this
example.
Then the registered lamps can be selected in the [Lamp Position Setup] dialog box. When the lamp is selected
in the [Lamp Position Setup] dialog box, the used time of the lamp is accumulated.
Once the accumulation of use time is started, [Lock] is check-marked for the lamp, and editing the fields except
[Comment] is prohibited. For an edit, delete the check mark from [Lock] or use the [Clear] button to clear the
accumulation content.
For the lamp set to be used in the [Lamp Position Setup] dialog box, the accumulation cannot be cleared with
[Clear] button, and the setting cannot be deleted with [Delete] button. To clear or delete the setting, delete the
lamp from the [Lamp Position Setup] dialog box.

[OK]
This saves the changed contents of the database and closes the dialog box.

AA-6800/6650 Instruction 5-71


Chapter 5 Functions of Operation Menu

[Cancel]
This cancels the changed contents of the database and closes the dialog box.

[Clear]
This clears the accumulation records of the lamps in the selected range, then the lamp information can be
edited. The data of the lamp selected in the [Lamp Position Setup] dialog box cannot be deleted.

[Print]
This prints a table of the lamp registration data base.

5.8.6 [Maintenance]
Selecting this menu allows you to use the functions for maintenance of the instrument.

5.8.6.1 [D2 Lamp Position]


This is used to adjust the position of deuterium lamp when replaced. For the replacing procedures, refer to
section 6.4.2. Selecting this menu displays the message "Adjust D2 lamp. First, adjust D2 lamp position
roughly.". Set the D2 lamp approximately to the center position using the adjusting screw. Then the deuterium
lamp is lit and the [D2 Lamp Adjustment] dialog box opens.

Figure 5.62 [D2 Lamp Adjustment] Dialog Box

The bar graph and [Current] indicate the current absorbance value of D2 lamp. Adjust the D2 lamp position so
that the absorbance value may become minimum.
[Reset Max Min]
Clicking on this button resets the values of [Max] and [Min].

5.8.6.2 [Wavelength Adjustment]


This executes the wavelength correction of monochromator automatically. It takes several minutes to execute
this correction.
Before execution, a message is displayed to check whether there is nothing interrupting the light beam in the
atomizer unit. Click on [OK] to execute.

5-72 AA-6800/6650 Instruction


5.8 [Instrument]

5.8.6.3 [Burner Origin Position Adjustment] (AA-6800)


This menu is used to adjust the burner up/down and fore/back positions. For the actual procedures, refer to
section 6.1.1.1.

Figure 5.63 [Burner Origin Position Adjustment] Dialog Box

[Moving Rate]
This indicates pulse number for one movement. Select [Fast], [Middle] or [Slow].

[Fore] and [Back]


Clicking on this button moves the burner by the pulse number set in [Moving Rate].
1 pulse = 0.024 mm

[Up] and [Down]


Clicking on this button moves the burner by the pulse number set in [Moving Rate].
1 pulse = 0.012 mm

[Origin Memory]
The current burner position is memorized as "fore/back = 0, up/down = 0" in the AA main unit.

[Autozero]
This shifts the current indicated value to zero.

AA-6800/6650 Instruction 5-73


Chapter 5 Functions of Operation Menu

5.8.6.4 [Furnace Origin Position Adjustment] (AA-6800)


This menu is used to adjust the furnace up/down and fore/back positions. For the actual procedures, refer to
section 6.1.2.1.

Figure 5.64 [Furnace Origin Position Adjustment] Dialog Box

[Moving Rate]
This indicates pulse number for one movement. Select [Fast], [Middle] or [Slow].

[Fore] and [Back]


Clicking on this button moves the burner by the pulse number set in [Moving Rate].
1 pulse = 0.024 mm

[Up] and [Down]


Clicking on this button moves the burner by the pulse number set in [Moving Rate].
1 pulse = 0.012 mm

[Origin Memory]
The current furnace position is memorized as "fore/back = 0, up/down = 0".

[Autozero]
This shifts the current indicated value to zero.

[Line Search]
This executes line search.

5-74 AA-6800/6650 Instruction


5.8 [Instrument]

[Move the furnace down to the lower position at the time of Line Search]
Check-marking the check box will move down the furnace beforehand at the time of line search so that the
optical path may not be obstructed. Use this function when the furnace is out of position too much to execute
[Line Search].
When the [Line Search/Beam Balance] dialog box is closed, the furnace position returns to the origin.

5.8.6.5 [Burner Origin Position Adjustment] (AA-6650)


In the case of AA-6650, the [Burner Origin Position Adjustment] dialog box cannot be used. Use [Atomizer/Gas
Flow Rate Setup] page when adjusting the burner position by observing the photometric value (refer to 6.1.1.2).

5.8.6.6 [Furnace Origin Position Adjustment] (AA-6650)


This menu is used to adjust the furnace up/down and forward/back positions. For the actual procedures, refer to
section 6.1.2.2.

Figure 5.65 [Furnace Origin Position Adjustment] Dialog Box

[Autozero]
This shifts the current indicated value to zero.

[Line Search]
This executes line search.

AA-6800/6650 Instruction 5-75


Chapter 5 Functions of Operation Menu

5.8.6.7 [ASC Maintenance]


This menu is used for maintenance related to the ASC. The maintenance related to the ASC is also described
in the instruction manual for ASC-6100.

• [Set Syringe Volume]


After replacing the syringe, set the upper and lower position limits of the syringe plunger and the syringe
volume.

Figure 5.66 [Set Syringe Volume] Dialog Box

Setting Procedures
(1) Setting the upper position
1. Move the plunger by using the [Up] or [Down] button of [Move Plunger] so that it is set near 0 PL,
as seen by the eye.
2. Click on the [Set Upper Limit] button to set the upper limit position. Note that the last position step
must be finish on an up-stroke before clicking on the [Set Upper Limit] button. This is to prevent
backlash.
(2) Setting the lower position
1. Move the plunger by using the [Up] or [Down] button of [Move Plunger] so that it is set near
230 PL, as seen by the eye.
2. Click on [Set Lower Limit] to set the lower limit position. Note that the last position step must be
finish on an up-stroke before clicking on the [Set Lower Limit] button. This is to prevent backlash.
(3) Volume setting
1. Enter the syringe volume for [Volume]. Enter a value determined by reading the syringe scale to
find the difference between the plunger upper and lower limit positions.
2. After entering the value for [Volume], click on [Set Volume] to fix the set syringe volume. Note
that the volume setting is not executed if this button is not pressed.

NOTE
If the plunger is moved beyond the syringe upper and lower limits, the syringe motor gets out of step and as
the result the syringe volume cannot be set properly after then. In this case, close this screen and power on
the ASC again. After completing the option connection, set the syringe volume setup again.

5-76 AA-6800/6650 Instruction


5.8 [Instrument]

[Move Plunger]
Select the plunger moving rate from [Fine (10 pulses)], [Coarse (600 pulses)] and [Specified Pulse]. When
[Specified Pulse] is selected, you can enter and set the pulse number for one moving step.

[Go to Upper Limit]


This moves the plunger to the set upper limit position. After setting the upper limit position, you can use this
to check whether the upper limit position is correctly set.

[Go to Lower Limit]


This moves the plunger to the set lower limit position. After setting the lower limit position, you can use this
to check whether the lower limit position is correctly set.

• [Change Syringe]

Figure 5.67 [Change Syringe] Dialog Box

[Change]
This is used to replace the syringe. Replace the syringe following the messages displayed on the screen
sequentially.
"Remove the syringe."
p
"Fill the syringe with water and mount it to the instrument."

[Fill]
This is used to fill the rinse liquid in the syringe. Use this function after replacing the syringe or when
bubbles are present in the syringe. Follow the messages displayed on the screen sequentially. The
message "Is the tube tip soaked in the rinse bottle liquid?" appears. After checking, click on [OK], then the
plunger moves upward to finish filling.

5.8.6.8 [Maintenance only for Service Engineer]


Only the service engineers can use this menu.

AA-6800/6650 Instruction 5-77


Chapter 5 Functions of Operation Menu

5.8.7 [Lamp Status]


Selecting this menu opens the [Lamp Status] dialog box and the status of the lamp currently used is displayed.
This dialog box indicates how long the lamp has been lit.

Figure 5.68 [Lamp Status] Dialog Box

[Lamp Status]
The lighting ON/OFF of the lamp is displayed. If the checkmark is deleted, the hollow cathode lamp can be
turned off but cannot be lit.
D2 lamp can be lit or turned off.

[Lighting Time]
Elapsed time of the lamp lighting is displayed. Once the lamp is turned off, it resets to "0".

[Wait Time]
When the warmup time is set, the rest of warmup time is displayed. If the measurement is started before the
wait time becomes "0", the [Hollow Cathode Lamp Warmup Waiting] dialog box is opened to indicates the wait
time. Clicking on [Start Measurement] in this dialog box ignores the waiting time and starts measurement.

Figure 5.69 [Warmup Waiting] Dialog Box

[Warmup Lamp Status]


When the rest waiting time becomes "0", "Completed" is displayed to indicate that warmup of the lamp is
completed.
When the lamp is not lit or when the specified warmup has not been completed, "Not Completed" is displayed.

5-78 AA-6800/6650 Instruction


5.8 [Instrument]

[D2 Lamp Warmup Time (min)]


Enter the time necessary for warming up the D2 lamp in the unit of minute. Since the D2 lamp is once turned off
when the line search is executed, the wait time set here is started after the line search/beam balance at the
measurement start time is finished.
During the wait time, the [Hollow Cathode Lamp Warmup Waiting] (or [D2 Lamp Warmup Waiting]) dialog box is
displayed.
The sequence of the lamp warmup and line search/beam balance at the measurement start time is as follows.

Hollow cathode lamp and D2 lamp are lit.


p
Hollow cathode lamp is warmed up.
p
Line search/beam balance is executed.
p
D2 lamp is warmed up.
p
Measurement is started.

NOTE
The warmup time of the hollow cathode lamp is set by selecting [Parameters]-[Edit Parameters]-[Sequence]
page from the menu.

5.8.8 [Change Graphite Tube]


The [Change Graphite Tube] dialog box is opened. For details, refer to section 5.5.9.4 for explanation of the
dialog box.

Figure 5.70 [Change Graphite Tube] Dialog Box

AA-6800/6650 Instruction 5-79


Chapter 5 Functions of Operation Menu

5.8.9 [Gas Controller Status]


This displays the state of the gas leak check, the drain level and the fuel gas pressure.

Figure 5.71 [Gas Controller Status] Dialog Box

[Gas Leak Check]


Displays the result of gas leak check.

[Drain Level]
Displays the status of drain tank level.

[Fuel Gas Pressure]


Displays whether the fuel gas pressure is appropriate or not.

[Flame Monitor ON]


When the check box is check-marked, the extinguished flame safety device is valid. Normally, set the flame
monitor "ON". Only in the case of Ar-H2 flame, however, set it off because the flame has no color and cannot be
detected.
When the AA software and the AA main unit are connected, the flame monitor is always set to ON at the time of
initialization. Therefore, if you wish to invalidate the flame monitor safety device, set the flame monitor to OFF in
this dialog box at every time of using the instrument.

NOTE
When the flame monitor is OFF, the extinguished flame safety device doesn't operate. Stay near the
instrument and always check that the flame is not extinguished. If the flame should be extinguished, press
the EXTINGUISH button.

5.8.10 [Gas Leak Check]


This checks a gas leakage of the piping inside the gas controller. The gas leak check is usually performed at the
initialization time of instrument, but can be performed by selecting this menu at any time if necessary.
The message "Gas leak check will be started. Press the EXTINGUISH button on the instrument." is displayed.
Following this instruction, press the EXTINGUISH button at the right of the combustion chamber, then click on
[OK] on the message box to close the message. The instrument automatically starts the gas leak check of 10
minutes. After 10 minutes, the check result is indicated in a pop-up message box. If the gas leak check is
finished before this, however, you can always ignite a flame within 10 minutes by pressing the IGNITE button.

5-80 AA-6800/6650 Instruction


5.8 [Instrument]

5.8.11 [Remaining Gas Combustion]


This menu is used to burn up acetylene gas in the piping from the gas main valve to the instrument by closing
the main valve of acetylene gas during the combustion of Air-C2H2 flame. If the flame type is set to N2O-C2H2,
you can't execute this procedure. Change the flame type to Air-C2H2 and retry it.

CAUTION
Be sure to follow the procedure below to perform the remaining gas combustion. If the procedure is
compromised, a flashback may occur.

(Procedure of Remaining Gas Combustion)


(1) Set the supply pressure and setting pressure of the acetylene gas and air properly (refer to 4.8).
(2) Select [Parameters]-[Edit Parameters] menu to open the [Atomizer/Gas Flow Rate Setup] page when the
measurement type of the current measurement element is set to flame in AA software.
Select the [Fuel Gas Flow Rate] radio button here, set "Air-C2H2" for [Flame Type] and click on [OK] to
close the page.
When using the high temperature burner, change the burner select key switch back to [AIR-C2H2] in the
AA main unit.

CAUTION
Be sure to use Air-C2H2 flame to perform the remaining gas combustion. Using N2O-C2H2 flame may cause
a flashback.

(3) Press the IGNITE button to ignite a flame.


(4) Select [Instrument]-[Remaining Gas Combustion] menu. The message in Figure 5.72 appears. Click on
[OK].

Figure 5.72 Remaining Gas Combustion - Message 1

(5) Next, the message shown in Figure 5.73 is displayed. Click on [OK] and close the main valve of the
acetylene gas cylinder. At this time, don't stop the support gas (air) and continue to supply it in the proper
pressure. As the acetylene gas decreases, the gas pressure lowering alarm sounds (stop the gas pressure
lowering alarm in the next (6)). Also, the AA software displays the message "Fuel gas pressure is too low".
Click on [OK] to close it.

NOTE
When stopping the remaining gas combustion, click on [Cancel] in the message of Figure 5.73 without
closing the main valve of the acetylene gas cylinder.

AA-6800/6650 Instruction 5-81


Chapter 5 Functions of Operation Menu

Figure 5.73 Remaining Gas Combustion - Message 2

(6) Next, the message shown in Figure 5.74 is displayed. Since the support gas (air) flows out after the flame
goes out, press the EXTINGUISH button of the AA main unit to stop the support gas (air). Also, press the
[BUZZER OFF] button on the gas controller panel to stop the gas pressure lowering alarm.

Figure 5.74 Remaining Gas Combustion - Message 3

(7) Click on [OK] in the message of Figure 5.74 to close the message.
With the above procedure, the remaining gas combustion is finished.

5.8.12 [Execute Line Search]


This is used to execute the line search for the element currently set. This function is the same as that of [Line
Search] button in the [Optics Parameters] page.

5.8.13 [Cleaning]
By selecting this menu, cleaning of the graphite tube is performed. This function is the same as that of
[Cleaning] button in the [Furnace Program] page.

5.8.14 [Rinse Nozzle]


The ASC nozzle rinse is executed in furnace measurement.
This menu is disabled when current measurement is flame measurement.

5.8.15 [Flame Nozzle Position]


This is used to adjust the sample uptake position. Adjust the position of suction nozzle following the messages
displayed step by step. To quit the position adjustment halfway, press the [Cancel]. Note, however, that the
proper adjustment cannot be performed when the nozzle position adjustment is quitted halfway.

"Please set the ASC turntable for flame measurement and remove the sample suction nozzle from the arm.
The ASC nozzle moves to sample intake position if you press OK button."
p
"Please mount the sample suction nozzle and adjust the nozzle vertical position. Please press OK button
after you finish the adjustment."

5-82 AA-6800/6650 Instruction


5.8 [Instrument]

5.8.16 [Furnace Nozzle Position]


Firstly, the sample uptake position is adjusted. Adjust the position of suction nozzle following the messages
displayed step by step. To quit the position adjustment halfway, press [Cancel]. Note, however, that the proper
adjustment cannot be performed when the nozzle position adjustment is quitted halfway.

"Please set the ASC turntable for furnace measurement and remove the sample suction nozzle from the
arm. The ASC nozzle moves to sample intake position if you press OK button."
p
"Please mount the sample suction nozzle and adjust the nozzle vertical position. Please press OK button
after you finish the adjustment. The ASC arm moves to furnace position."
p
"Loosen the arm guide screw mounted onto the furnace and release the arm guide. Be careful not to
change the arm guide position too much."

Next, the [ASC Furnace Nozzle Position Adjustment] dialog box is displayed. The injection position is adjusted
here.

Figure 5.75 [ASC Furnace Nozzle Position Adjustment] Dialog Box

Lower the nozzle to near the injection hole of the graphite tube, using the [Move Upward] or [Move Downward]
button. Then, adjust the horizontal position forward, backward, rightward and leftward using the injection
position adjusting knob of the ASC table so that the tip of the nozzle comes almost to the center of the injection
hole. After adjusting the horizontal position in every direction, move the nozzle to a proper injection position
using the [Move Upward] or [Move Downward] button then click on the [OK] button. The position is set as the
injection position. Clicking on the [Cancel] button cancels setting the injection position. When quitting the setting
at this step, note that the injection position is not set although the suction position is set.
The message "Tighten the fixing screw of the arm guide" is displayed before this screen is closed. Tighten the
screw of the arm guide previously loosened carefully so that the arm is not moved.

[Fine (1 pulse)] [Coarse (30 pulses)] [Specified Pulses]


Select a moving rate from these. When [Specified Pulses] is selected, a value "1" to "30" can be entered.

[Current Pos.]
The current nozzle position is displayed.

AA-6800/6650 Instruction 5-83


Chapter 5 Functions of Operation Menu

[Injection Pos.]
The sample injection position currently selected is displayed.

[Move Near to Tube]


The nozzle is moved straight to the vicinity of graphite tube. When the injection position is largely shifted by a
change of the furnace position, care must be taken so that the tip of the nozzle may not be damaged.

[Move Upward] [Move Downward]


The nozzle is moved up or down at a specified rate.

5-84 AA-6800/6650 Instruction


5.9 [Help]
5.9 [Help]

Select this menu when using the help function.

5.9.1 [Search for Help on...]


By entering a keyword in the [Search for Help on...] dialog box, the help of a specified item can be searched.

5.9.2 [About WizAArd...]


Version and system information of this software are displayed.

AA-6800/6650 Instruction 5-85


Chapter 5 Functions of Operation Menu

This page is intentionally left blank.

5-86 AA-6800/6650 Instruction


Chapter 6
Maintenance

CONTENTS

6.1 Atomizer Position Adjustment........................................................................................................ 6-2


6.2 Burner Maintenance ...................................................................................................................... 6-5
6.3 Checking for Gas Leaks in Tubing................................................................................................. 6-9
6.4 Replacing the Deuterium Lamp ................................................................................................... 6-10
6.5 Maintenance Parts....................................................................................................................... 6-12
6.6 Special Accessories..................................................................................................................... 6-13

AA-6800/6650 Instruction 6-1


Chapter 6 Maintenance
6.1 Atomizer Position Adjustment

6.1.1 Burner Positioning Adjustment


6.1.1.1 AA-6800
In the case of flame method, the burner moves automatically so that the burner head slot is positioned directly
beneath the optical path. However, when the burner is dismantled for cleaning etc., the burner position must be
readjusted. The procedure is described below.

(1) Select an element which you usually use in flame method.


(2) In the [Optics Parameters] page, set the lamp mode to "EMISSION" and light the lamp to perform line
search.
(3) Returning to the main window displays the current measured photometric value. Rotate the lamp mounted
in the turret and adjust the rotating position so that the indicated value may become maximum.
(4) Select [Instrument]-[Maintenance]-[Burner Origin Position Adjustment] from the menu. Then [Burner Origin
Position Adjustment] dialog box opens.
(5) Verify that the burner head is securely mounted. Then click on [Down] to lower the burner so that the
burner may not interrupt the light beam. In addition, set the burner angle to "0".
(6) Set the provided burner positioning jig at the center of the burner head so that the scale is facing the lamp.
By using the [Fore] and [Back] buttons, adjust front/back position of the burner so that the photometric data
is at its maximum.
(7) Without changing the direction of the adjustment jig, move it to the right end of the burner head and fix it in
place. Then using the burner head angle adjustment lever, gradually rotate the burner head until you
obtain the position where the displayed photometric value is at its maximum.
(8) Once again, secure the positioning jig at the center of the burner head, and move the burner head front
and back by the [Fore] and [Back] buttons to determine the position where the photometric data is at its
maximum.
(9) Click on [Up] to set the burner height to 0 mm. Set a piece of white paper on the burner facing the lamp.
Adjust the burner height so that the beam spot on the paper is semicircular (Figure 6.2).
(10) Click on [Origin Memory]. Then the current burner position is memorized as "Fore/back = 0, Up/down = 0".

Burner head positioning jig

Burner head

Burner head angle adjusting lever

Figure 6.1 Burner Position Adjustment

6-2 AA-6800/6650 Instruction


6.1 Atomizer Position Adjustment

White paper

Beam spot

Burner head

Figure 6.2 Burner Height Adjustment

6.1.1.2 AA-6650
The adjustment procedure, searching the most sensitive position of the burner front/back direction by using
knobs for adjusting burner position (refer to section 3.1.4.2), is described below.
(1) Select an element which you usually use in flame method.
(2) In the [Optics Parameters] page, set the lamp mode to "EMISSION" and light the lamp to perform line
search.
(3) Returning to the main window displays the current measured photometric value.
Rotate the lamp mounted in the turret and adjust the rotating position so that the indicated value may
become maximum.
(4) Select [Parameters] - [Edit Parameters...] from the menu, open [Atomizer / Gas Flow Rate Setup] page,
and select [Atomizer Position] radio button.
(5) Verify that the burner head is securely mounted. Then turn the knob for adjusting burner vertical position to
lower the burner so that the burner may not interrupt the light beam. In addition, set the burner angle to "0".
(6) Set the provided burner positioning jig at the center of the burner head so that the scale is facing the lamp.
By using knob for adjusting burner horizontal position, adjust front/back position of the burner so that the
photometric value is at its maximum.
(7) Without changing the direction of the adjustment jig, move it to the right end of the burner head and fix it in
place. Then using the burner head angle adjustment lever, gradually rotate the burner head until you
obtain the position where the displayed photometric value is at its maximum.
(8) Once again, secure the positioning jig at the center of the burner head, and move the burner head front
and back by the knob for adjusting burner horizontal position to determine the position where the
photometric value is at its maximum.
(9) At this time, the most sensitive position of the burner front/back direction is specified. And adjust the burner
height in accordance with each measurement parameter.

AA-6800/6650 Instruction 6-3


Chapter 6 Maintenance

6.1.2 Furnace Position Adjustment


6.1.2.1 AA-6800
(1) Select an element which you usually use in furnace method.
(2) In the [Optics Parameters] page, set the lamp mode to "EMISSION". Although the message "Line Search/
Beam Balance is necessary" appears, press [Cancel].
(3) From the menu, execute [Instrument]-[Maintenance]-[Furnace Origin Position Adjustment]. Then the
[Furnace Origin Position Adjustment] dialog box is opened.
(4) Next, after check-marking the [Move the furnace down to the lower position at the time of Line Search.]
check box, click on [Line Search].
(5) After the furnace gets out of the optical axis position, the [Line Search/Beam Balance] dialog box is opened
and the line search is executed.
(6) When both line search and beam balance results are indicated as "OK", click on [Close].
(7) Using [Fore], [Back], [Up] and [Down] buttons, adjust the vertical and horizontal position so that the
photometric data indicates the maximum value.
(8) After adjusting the position, click on [Origin Memory]. Then the current furnace position is memorized as
"Lateral = 0, Height = 0".

6.1.2.2 AA-6650
When changing the atomizer from the burner to the graphite furnace, it is necessary to adjust the furnace
position.
First, start the following procedure before mounting the graphite furnace on the optical path.
(1) Select an element that you usually use. It doesn't matter which of the furnace method or flame method is
selected.
(2) In the [Optics Parameters] page, set the lamp mode to "EMISSION". Although the message "Line Search/
Beam Balance is necessary" appears before returning to the main screen, press [Cancel].
(3) From the menu, execute [Instrument]-[Maintenance]-[Furnace Origin Position Adjustment]. Then the
[Furnace Origin Position Adjustment] dialog box is opened.
(4) Next, click on [Line Search]. The [Line Search Beam Balance] dialog box is opened and the line search is
executed.
(5) When both line search and beam balance results are "OK", click on [Close].
Then mount the graphite furnace (equipped with the graphite tube) on the light path.
(6) Adjust the vertical and horizontal positions with the knobs manually so that the photometric data in the
[Furnace Origin Position Adjustment] dialog box may indicates a maximum value.
(7) Then the furnace position is adjusted properly.

When only the graphite furnace is used without switching between the burner and the graphite furnace, the
furnace position is not changed so much. Therefore, the procedure from (1) to (6) may be performed while
keeping the graphite furnace mounted.

6-4 AA-6800/6650 Instruction


6.2 Burner Maintenance
6.2 Burner Maintenance

If foreign matter sticks to the burner head, nebulizer, and inside of the chamber, the signal becomes unstable or
absorbance sensitivity decreases. Periodic cleaning of these components is recommended.
The connector between the burner head and nebulizer is sealed with O-rings. If the O-rings are deformed or
deteriorated, immediately replace them.

NOTE
1. When analysis is complete, do not immediately extinguish the flame. Spray distilled water for about
three to five minutes to purge the capillary of the nebulizer, burner head, and the inside of the chamber.
2. If it is difficult to remove or install the burner head and the nebulizer, apply a small amount of grease
(available as an accessory) on the O-rings.

CAUTION
1. O-rings are inserted into the connector between the burner head and nebulizer to prevent a gas leak.
When reassembling the burner, ensure that the O-rings are correctly installed.
2. Deteriorated O-rings cause gas leaks. O-rings should be replaced on a yearly basis.

6.2.1 Cleaning the Burner Head


If the slot of the burner head is slightly clogged, the reduction flame will have fine irregularities.
When the slot is more heavily clogged, the flame splits as shown in Figure 6-3. If such a flame is produced,
extinguish the flame, then remove the adhering matter by scraping the inner wall of the slot with thick paper or
thin plastic plate.
Sometimes an orange colored flame may flicker when the burner is ignited again after cleaning the slot. In this
case, spray pure water until there is no flickering. If the flickering does not stop quickly, remove the burner head
from the chamber and wash the inside with distilled water. The burner head can be removed by pulling upward.
If it is extremely dirty, soak it in acid or appropriate detergent over night then brush the slot inner wall.

Clogged Normal

Figure 6.3 Flame Symptoms due to Clogged Slot

AA-6800/6650 Instruction 6-5


Chapter 6 Maintenance

When measuring samples with high concentrations of coexistent components, such as salts, these will adhere
to the inner wall of the slot. After measuring such samples, be sure to clean the slot thoroughly.

CAUTION
1. Don't use metal brushes that may scratch the burner head.
2. If the width of the slot become wider or the inner surface of the slot become coarse, replace the burner
head with a new one. In the case of a high temperature burner, usage under such conditions may cause
a flashback. The typical life time of burner head is about 3 years.

6.2.2 Nebulizer Maintenance


6.2.2.1 Cleaning the Nebulizer
If the indication value fluctuates or the absorbance sensitivity decreased during measurement, the capillary of
the nebulizer may be clogged by some contaminant. Clean the nebulizer in the following procedure.

(1) When the flame is extinguished completely, insert the cleaning wire into the capillary <1> to clean its inner
wall (refer to Figure 6.5).
(2) After removing the cleaning wire, spray distilled water.
(3) Use a standard sample solution or the like to check the sensitivity and stability.
(4) If the performance is not improved after performing the above operations (1) through (3), contaminants
may stick between the capillary and the plastic jacket <2> at the tip of the nebulizer. In this case, perform
the following procedure (refer to Figure 6.5).
(5) When the flame is extinguished completely, loosen the fixing screws <1> for the nebulizer <4> to draw out
the nebulizer retaining plate <2> in the right direction. Remove the SPRAY joint <3> inserted into the
nebulizer and then remove the nebulizer from the chamber <5> (refer to Figure 6.4).
(6) After removing the nebulizer, dip the nebulizer tip into hydrochloric acid (1:1). At this time, hold the
nebulizer so that only the jacket <2> is immersed and make sure that the metal part <3> is not immersed in
the hydrochloric acid (refer to Figure 6.3). Subsequently, immerse the same part in distilled water to
completely eliminate hydrochloric acid.

CAUTION
1. Do not remove the disperser unit.
2. Do not apply the ultrasonic cleaner to the nebulizer. Otherwise, the adhesion between the capillary and
the main body may be damaged.

(7) Mount the nebulizer and then spray pure water. Use a standard sample solution or the like to check the
absorption sensitivity and stability.

6-6 AA-6800/6650 Instruction


6.2 Burner Maintenance

<4> Nebulizer

<3> SPRAY joint


Burner head

<2> Retaining plate

<1> Fixing screw

<4> Nebulizer
<5> Chamber
<6> Mixer
<7> Spray unit

Figure 6.4 Burner Unit

<1> Capillary

<7> Polyethylene tube

<2> Plastic jacket


<6> Cap

<3> Body (Metal part)

Figure 6.5 Nebulizer

AA-6800/6650 Instruction 6-7


Chapter 6 Maintenance

6.2.2.2 Replacing the Polyethylene Tube


The PTFE sampling tube used to suction samples is held in place by a polyethylene tube wedged into the
nebulizer capillary. If the polyethylene tube deteriorates or comes loose, it cannot hold the PTFE sampling tube
in place. Should this happen, use the following procedure to replace the polyethylene tube.
Refer to Figure 6.5.

(1) Remove the cap <6> shown in Figure 6.5 by rotating it to the left.
(2) If the old polyethylene tube is still in the capillary <1>, remove it.
(3) Cut the new polyethylene tube <7> to the length of the old tube (about 5 mm) and insert the new tube into
the capillary. Do not bend the capillary.
(4) Replace the cap.

NOTE
If it is difficult to fit the polyethylene tube in the capillary, enlarge the opening by inserting a pen or other thin
object.

6.2.3 Washing the Chamber


Disassembling the chamber unit following the procedures below and completely wash it with distilled water or
alcohol.

(1) Remove the burner head and the nebulizer (refer to 6.2.1 and 6.2.2).
(2) Remove the spray unit fixing screws <1> to remove the spray unit. Then you can take the mixer out from
the chamber inside.
(3) Remove the chamber fixing screws <3> and remove the chamber. Then loosen the strap of the drain port
<4> at the lower chamber floor and remove the U-tube.

CAUTION
1. When assembling the chamber after cleaning it, be sure to check the direction of the mixer. Since the
outer diameter of the mixer is slightly tapered, push it in the direction, which fits the taper of the chamber
inside.
2. Before pouring water or alcohol from the burner socket, be sure to remove the nebulizer. Otherwise, the
nebulizer may sink in the liquid and the adhesive may be damaged.
3. When disassembling the chamber unit, pay attention not to break the disperser.

6-8 AA-6800/6650 Instruction


6.3 Checking for Gas Leaks in Tubing
6.3 Checking for Gas Leaks in Tubing

Regular checks are automatically conducted for gas leaks in the fuel gas tubing within the gas controller. Gas
leaks at other locations may also be conducted using the following procedure. This procedure should be
performed regularly at monthly intervals.
(1) Disconnect the White tube between the nebulizer and L-coupling joint. And disconnect the Red tube and
Black tube from the Y joint of the burner unit.
(2) Connect these tubes to the provided leak check seal joint and supply air 0.35 MPa and acetylene at
0.09 MPa.

Figure 6.6 Seal Joint for Gas Leak Check

(3) Execute [Instrument]-[Gas Controller Status] from the menu. Then the [Gas Controller Status] dialog box is
displayed. Click on the [Flame Monitor ON] check box to delete the check mark.
(4) Press the IGNITE button on the front of the instrument for 2 or 3 seconds. Since the burner is not supplied
with the gas, a flame is not ignited. However, the instrument gets in a dummy combustion status because
the flame monitor is set to OFF. As the result, all the solenoid valves in the gas controller open.
(5) Close the main valve of the cylinder and turn the secondary pressure control handle of the air compressor
sufficiently counterclockwise and close it.
(6) Confirm the pressure drop in 30 minutes is less than 0.015 MPa for fuel gas and less than 0.03 MPa for
support gas, viewing the gas control gauges. If the drop in pressure exceeds these values, it should be
concluded that gas is leaking.
(7) If gas is judged to be leaking, apply soapy water or commercial leak check liquid to each of the connecting
joints of the cylinder, compressor, gas controller and burner to ascertain the location of the leak.
(8) Reconnect any joints where a gas leak is discovered. If it is concluded that gas is leaking inside the gas
controller, contact your service representative immediately.
(9) Check for leaking in the drain tube by filling water inside and checking visually.
(10) When the gas leak check is finished, press the EXTINGUISH button. Then detach the three tubes from the
seal joint and reconnect them to the burner as described under 2.4.4.

NOTE
To stop this gas leak check halfway, press the EXTINGUISH button at the front of instrument.

AA-6800/6650 Instruction 6-9


Chapter 6 Maintenance
6.4 Replacing the Deuterium Lamp

6.4.1 Specifications of Deuterium Lamp


Table 6.1 Specifications of Deuterium Lamp

Part No 062-65063-01

Type L6382

Average 500 hours

Characteristics Discharge voltage 70 - 90 V

Discharge current 300 mA

Discharge starting voltage 300 - 600 V

6.4.2 Replacing Procedures of Deuterium Lamp

WARNING
HIGH TEMPERATURE
The deuterium lamp and deuterium lamp house are very hot. Before replacing the lamp, turn OFF the power
and check that the lamp has cooled sufficiently.

CAUTION

1. Handle the new lamp using gloves so as not to leave fingerprints on the light beam window. Otherwise,
the window is stained with the fingerprints when it is hot, and as the result the light transmission will be
reduced. If contaminated, clean it with alcohol or the like.
2. When detaching or attaching the cover of the deuterium lamp house, be very careful not to hit the
protrudent upper edge of the deuterium lamp against the cover rear side. It may cause a vacuum leak of
the bulb.

Protrudent part on upper edge

Light beam window

Figure 6.7 Interior of Deuterium Lamp House Unit

6-10 AA-6800/6650 Instruction


6.4 Replacing the Deuterium Lamp

(1) As shown in Figure 6.8, remove the two screws to detach the lamp cover. When the cover is removed, the
deuterium lamp will appear as shown in Figure 6.7.

Deuterium lamp cover

Hole for adjustment

Figure 6.8 Deuterium Lamp Cover

(2) Pull the deuterium lamp slowly upward and out of its socket.
(3) Insert a new deuterium lamp into the socket. At this time check that the lamp is fully seated in the socket.
(4) Turn on the power of the instrument. Start up the PC software and select [Instrument]-[Connect] from the
menu to make the connection for communication with the instrument.
(5) Select [Instrument]-[Maintenance]-[D2 Lamp Position] from the menu. The message "D2 lamp position
adjustment procedure is going to start. Please adjust D2 lamp position roughly first." is displayed. Set the
deuterium lamp to almost center with the adjusting screw.
(6) Click on [OK] and close the lamp cover.
(7) Next, the deuterium lamp intensity in absorbance is displayed in the [D2 Lamp Adjustment] dialog box.
Adjust the position using the adjusting knob so that the indicated value may become minimum.
(8) After completing the deuterium lamp adjustment, click on [OK] to close the [D2 Lamp Adjustment] dialog
box.

AA-6800/6650 Instruction 6-11


Chapter 6 Maintenance
6.5 Maintenance Parts

Standard
Name P/N Remarks Replacement
Interval

Lamp, D2 L6382 062-65063-01 Deuterium lamp 1 year

Nebulizer set 206-52300-91 With impact bead 2 years

Chamber ASSY 206-50363-91 Made of polypropylene 6 years

Burner head ASSY 206-50370-92 Made of titanium (10 cm) 3 years

Burner socket ASSY 206-50762-91 3 years

O ring, AS568-116-4D 036-15551-16 Used at the burner head side of the 1 year
burner socket

O ring, 4D P22 036-11222 Used at the chamber side of the 1 year


burner socket

O ring, 4D P5 036-11203 Used in the nebulizer 1 year

O ring, 4D P16 036-11217 Used with the nebulizer and chamber 1 year
plugs

O ring, 4D P14 036-11215 Used in the drain joint 1 year

O ring, 4D P35 036-11237 Used between the chamber and the 1 year
jacket

Cleaning wire 201-79229-01 For capillary cleaning 


Sampling tube 204-05899-01 PTFE* tube for sample suction 
Sampling tube ASSY 206-50772-91 Polyethylene tube for sample suction 
Drain ASSY 206-80771-91 Overflow-type waste liquid trap 3 years

Gas tube ASSY 206-65112 Nylon tube set for gas supply 3 years

Hose, 8 u 2B-BK 016-02101-04 For air (black) 3 years


Specify the necessary length.
(Standard length: 5 m)

Hose, 8 u 2B-R 016-02101-03 For fuel gas (red) 3 years


Specify the necessary length.
(Standard length: 5 m)

Hose, 8 u 2B-G 016-02101-01 For N2O (green) 3 years


Specify the necessary length.
(Standard length: 5 m)

Wire band for 16 mm 037-61019 Hose clamp 


diameter

6-12 AA-6800/6650 Instruction


6.5 Maintenance Parts

Standard
Name P/N Remarks Replacement
Interval

Tube super cone, 9 u 13 016-43200-08 Drain hose (under the chamber) 3 years
Specify the necessary length.
(Standard length: 80 cm)

Vinyl tube, R3603 3/8 u1/16 016-31409 Connected to the Taigon tube and 3 years
drainage bottle
(For water-soluble samples)
Specify the necessary length.
(Standard length: 2.4 m)

Si rubber tube, 9 u12 016-31350-22 Silicone rubber tube, connected to 3 years


the drainage bottle
(For samples in organic solvents
other than oil-based solvents)
Specify the necessary length.
(Standard length: 2.4 m)

Seal joint ASSY 206-52826-91 For checking for gas leakage 


Polyethylene capillary tube 200-31328-01 For capillary seals 
No. 3 Specify the necessary length.
(Standard length: 30 cm)

Fixed block 206-52217 For securing the nebulizer 6 years

Elbow, 31020600 035-65268-02 Connects the nebulizer to the spray 1 year


tube

Vinyl cover 206-64902 Body cover made of vinyl 


Mixer 206-50486 6 years

Burner positioning jig 202-38757-02 


Wiring band 072-60315-01 For fixing the drain hose 
Fuse, 313.250 0.25 A 072-01664-11 For HCL lamp 3 years

Fuse, 189100 072-01667-12 For D2 lamp 3 years

Fuse, ULCS-61ML6 072-01661-24 For 6 A, 100 V system 3 years

Fuse, 3313.003 072-01664-30 For 3 A, 200 V system 3 years

* Throughout this manual, polytetrafluorethylene is abbreviated to PTFE.

NOTE
The cross-hatching in the table indicates parts that are related to the safety of the product. You must replace
these parts at regular intervals.

AA-6800/6650 Instruction 6-13


Chapter 6 Maintenance
6.6 Special Accessories

6.6.1 For Flame Analysis

Part Name Part No. Remarks


Flame conversion unit ACF-6800 206-64843-92
Cover, flame 206-50554 Required when mounting ACF-6800 on
AA-6650G
High temperature burner head 206-50300-92 Titanium
Silent-type air compressor 208-91750-36 For 220/230 VAC, 50/60 Hz
Air compressor 208-91742-91 For 100 VAC, 50/60 Hz
Mist separator kit 206-52458-91 Use with air compressors other than
described above
Precision gas pressure regulator YR-71 040-72020-01 For acetylene gas
Precision gas pressure regulator MAF-85S 040-72019-11 For nitrous oxide gas
Precision gas pressure regulator MAF-76S 040-72019-01 For hydrogen gas
Precision gas pressure regulator MAF-106S 040-72019-21 For argon gas
Hose ASSY 206-50389-91 For argon gas
Hose ASSY 206-50389-92 For hydrogen gas

6.6.2 For Furnace Analysis (for GFA-EX7)

Part Name Part No. Remarks


Graphite Furnace Atomizer GFA-EX7 206-51000-xx
Furnace base 206-51141 Required when mounting GFA-EX7 on
AA-6650F
High-density graphite tube 206-50587
Pyrolytic coated graphite tube 206-50588
Platform tube 206-50887-02

6.6.3 Autosampler

Part Name Part No. Remarks


Autosampler ASC-6100 206-50100-xx
Unit for furnace ASK-6100 206-50200-91
Nozzle ASSY, HVG 206-67563 Required when using ASC-6100 with
HVG-1

6-14 AA-6800/6650 Instruction


6.6 Special Accessories

6.6.4 Hollow Cathod Lamps (Single Element Lamps)


HAMAMATSU PHOTONICS Co. LTD L233 Series (Not usable for SR method)

Element Symbol Element Name Part No. Product Name


Ag Silver 200-38422-02 L233-47NQ
Al Aluminum 200-38422-01 L233-13NB
As Arsenic 200-38422-42 L233-33NQ
Au Gold 200-38422-25 L233-79NQ
B Boron 200-38422-39 L233-5NQ
Ba Barium 200-38422-03 L233-56NB
Be Beryllium 200-38422-04 L233-4NQ
Bi Bismuth 200-38422-43 L233-83NQ
Ca Calcium 200-38422-05 L233-20NU
Cd Cadmium 200-38422-06 L233-48NQ
Co Cobalt 200-38422-09 L233-27NU
Cr Chromium 200-38422-07 L233-24NB
Cs Cesium 200-38422-27 L233-55NB
Cu Copper 200-38422-08 L233-29NB
Dy Dysprosium 200-38422-60 L233-66NB
Er Erbium 200-38422-61 L233-68NB
Eu Europium 200-38422-62 L233-63NB
Fe Iron 200-38422-10 L233-26NB
Ga Gallium 200-38422-40 L233-31NU
Gd Gadolinium 200-38422-63 L233-64NB
Ge Germanium 200-38422-11 L233-32NU
Hf Hafnium 200-38422-64 L233-72NU
Hg Mercury 200-38422-28 L233-80NU
Ho Holmium 200-38422-65 L233-67NB
In Indium 200-38422-48 L233-49NB
Ir Iridium 200-38422-66 L233-77NQ
K Potassium 200-38422-22 L233-19NB
La Lanthanum 200-38422-29 L233-57NB
Li Lithium 200-38422-30 L233-3NB
Lu Lutetium 200-38422-67 L233-71NB
Mg Magnesium 200-38422-12 L233-12NU
Mn Manganese 200-38422-13 L233-25NU
Mo Molybdenum 200-38422-31 L233-42NB
Na Sodium 200-38422-14 L233-11NB
Nb Niobium 200-38422-32 L233-41NB

AA-6800/6650 Instruction 6-15


Chapter 6 Maintenance

Element Symbol Element Name Part No. Product Name


Nd Neodymium 200-38422-68 L233-60NB
Ni Nickel 200-38422-15 L233-28NQ
Os Osmium 200-38422-69 L233-76NU
Pb Lead 200-38422-21 L233-82NQ
Pd Palladium 200-38422-41 L233-46NQ
Pr Praseodymium 200-38422-70 L233-59NB
Pt Platinum 200-38422-20 L233-78NU
Rb Rubidium 200-38422-33 L233-37NB
Re Rhenium 200-38422-44 L233-75NB
Rh Rhodium 200-38422-49 L233-45NB
Ru Ruthenium 200-38422-45 L233-44NB
Sb Antimon 200-38422-24 L233-51NB
Sc Scandium 200-38422-71 L233-21NB
Se Selenium 200-38422-46 L233-34NB
Si Silicon 200-38422-16 L233-14NU
Sm Samarium 200-38422-72 L233-62NB
Sn Tin 200-38422-18 L233-50NQ
Sr Strontium 200-38422-34 L233-38NB
Ta Tantalum 200-38422-35 L233-73NU
Tb Terbium 200-38422-73 L233-65NB
Te Tellurium 200-38422-47 L233-52NQ
Ti Titanium 200-38422-17 L233-22NB
Tl Thallium 200-38422-74 L233-81NU
Tm Thulium 200-38422-75 L233-69NB
V Vanadium 200-38422-19 L233-23NB
W Tungsten 200-38422-36 L233-74NU
Y Yttrium 200-38422-76 L233-39NB
Yb Ytterbium 200-38422-77 L233-70NB
Zn Zinc 200-38422-23 L233-30NQ
Zr Zirconium 200-38422-37 L233-40NB

6-16 AA-6800/6650 Instruction


6.6 Special Accessories

6.6.5 Hollow Cathode Lamps (Single Element Lamps, Usable for SR


Method)
HAMAMATSU PHOTONICS Co. LTD L2433 Series

Element Symbol Element Name Part No. Product Name


Ag Silver 200-38456-01 L2433-47NB
Al Aluminum 200-38456-02 L2433-13NB
As Arsenic 200-38456-03 L2433-33NQ
Au Gold 200-38456-04 L2433-79NQ
B Boron 200-38456-05 L2433-5NB
Ba Barium 200-38456-06 L2433-56NB
Be Beryllium 200-38456-07 L2433-4NQ
Bi Bismuth 200-38456-08 L2433-83NQ
Ca Calcium 200-38456-09 L2433-20NU
Cd Cadmium 200-38456-10 L2433-48NQ
Co Cobalt 200-38456-11 L2433-27NU
Cr Chromium 200-38456-12 L2433-24NB
Cu Copper 200-38456-14 L2433-29NB
Dy Dysprosium 200-38456-15 L2433-66NB
Er Erbium 200-38456-16 L2433-68NB
Eu Europium 200-38456-17 L2433-63NB
Fe Iron 200-38456-18 L2433-26NQ
Ga Gallium 200-38456-19 L2433-31NU
Ge Germanium 200-38456-21 L2433-32NU
Hf Hafnium 200-38456-22 L2433-72NU
Ho Holmium 200-38456-24 L2433-67NB
K Potassium 200-38456-26 L2433-19NB
La Lanthanum 200-38456-27 L2433-57NB
Li Lithium 200-38456-28 L2433-3NB
Mg Magnesium 200-38456-30 L2433-12NU
Mn Manganese 200-38456-31 L2433-25NU
Mo Molybdenum 200-38456-32 L2433-42NB
Na Sodium 200-38456-33 L2433-11NB
Ni Nickel 200-38456-35 L2433-28NQ
Pb Lead 200-38456-37 L2433-82NQ
Pd Palladium 200-38456-38 L2433-46NQ
Pt Platinum 200-38456-40 L2433-78NU
Ru Ruthenium 200-38456-43 L2433-44NB
Sb Antimon 200-38456-44 L2433-51NQ

AA-6800/6650 Instruction 6-17


Chapter 6 Maintenance

Element Symbol Element Name Part No. Product Name


Se Selenium 200-38456-46 L2433-34NQ
Si Silicon 200-38456-47 L2433-14NQ
Sm Samarium 200-38456-48 L2433-62NB
Sn Tin 200-38456-49 L2433-50NQ
Sr Strontium 200-38456-50 L2433-38NB
Te Tellurium 200-38456-53 L2433-52NQ
Ti Titanium 200-38456-54 L2433-22NB
V Vanadium 200-38456-56 L2433-23NB
Y Yttrium 200-38456-58 L2433-39NB
Yb Ytterbium 200-38456-59 L2433-70NB
Zn Zinc 200-38456-60 L2433-30NQ

6.6.6 Hollow Cathod Lamp (Multi-element Lamps)


(Not usable for SR method)

Element Part No. Product Name


Ca, Mg 200-38422-51 L733-202NU
Fe, Ni 200-38422-53 L733-204NQ
Na, K 200-38422-50 L733-201NB
Si, Al 200-38422-52 L733-203NU
Si, Ba 200-38422-54 L733-205NU

6.6.7 Other Accessories

Part Name Part No. Remark


Mercury vaporizer unit MVU-1A 204-21932-01
Gas flow cell 201-98687
Cell holder for gas flow cell 202-35867
Hydride vaporizer unit HVG-1 206-17143
Cooling water circulating unit CA-1112 044-01809-03 Working temperature range: -10 to +40 qC
Cooler connection kit 206-84373-91 Required when the GFA is connected with
the cooling water circulator
Regulator ASSY 206-86147-91 Pressure reducing valve for GFA cooling
water

6-18 AA-6800/6650 Instruction


Chapter 7
Appendix

CONTENTS

7.1 Measurement Conditions Table for Flame Atomic Absorption Analysis ........................................ 7-2
7.2 Analysis Line Wavelength Table for Flame Emission Analysis ..................................................... 7-5
7.3 Graphite Tube Type Selection in Furnace Method ........................................................................ 7-6
7.4 Error Messages ........................................................................................................................... 7-10

AA-6800/6650 Instruction 7-1


Chapter 7 Appendix
7.1 Measurement Conditions Table for Flame
Atomic Absorption Analysis

Wave length L233 L2433 Flow Burner. H


Element Slit (nm) Flame Type
(nm) (mA) (mA) (l/min) (mm)
Ag 328.1 10 10/400 0.5 Air-C2H2 2.2 7
Al 309.3 10 10/600 0.5 N2O-C2H2 7.0 11
As (H) 193.7 12 12/500 1.0 Air-C2H2 2.0 <HVG-1>
As 193.7 12 12/500 1.0 Ar-H2 [3.7] 15
Au 242.8 10 10/400 0.5 Air-C2H2 1.8 7
B 249.7 16 10/500 0.2 N2O-C2H2 7.7 11
Ba 553.5 16 12/600 0.2 N2O-C2H2 6.7 11
Be 234.9 16 10/600 1.0 N2O-C2H2 7.0 11
Bi (H) 223.1 10 10/300 0.5 Air-C2H2 2.0 <HVG-1>
Bi 223.1 10 10/300 0.5 Air-C2H2 2.2 7
Ca (1) 422.7 10 10/600 0.5 Air-C2H2 2.0 7
Ca (2) 422.7 10 10/600 0.5 N2O-C2H2 6.5 11
Cd 228.8 8 8/100 1.0 Air-C2H2 1.8 7
Co 240.7 12 12/400 0.2 Air-C2H2 1.6 7
Cr 357.9 10 10/600 0.5 Air-C2H2 2.8 9
Cs 852.1 16  1.0 Air-C2H2 1.8 7
Cu 324.8 6 10/500 0.5 Air-C2H2 1.8 7
Dy 421.2 14 15/600 0.2 N2O-C2H2 7.0 11
Er 400.8 14 15/500 0.5 N2O-C2H2 7.0 11
Eu 459.4 14 10/600 0.5 N2O-C2H2 7.0 11
Fe 248.3 12 12/400 0.2 Air-C2H2 2.2 9
Ga 287.4 4 4/400 0.2 Air-C2H2 1.8 7
Gd 368.4 12  0.2 N2O-C2H2 7.0 11
Ge 265.2 18 20/500 0.2 N2O-C2H2 7.8 11
Hf 307.3 24 20/600 0.2 N2O-C2H2 7.0 11
Hg 253.7 4  1.0 By the cold vapor mercury technique
Ho 410.4 14 10/600 0.2 N2O-C2H2 7.0 11
Ir 208.8 20  0.2 Air-C2H2 2.2 7
K 766.5 10 8/600 0.5 Air-C2H2 2.0 7
La 550.1 18 18/600 0.5 N2O-C2H2 7.5 11
Li 670.8 8 8/500 0.5 Air-C2H2 1.8 7
Lu 360.0 14  0.5 N2O-C2H2 7.0 11
Mg 285.2 8 8/500 0.5 Air-C2H2 1.8 7
Mn 279.5 10 10/600 0.2 Air-C2H2 2.0 7
Mo 313.3 10 10/500 0.5 N2O-C2H2 7.0 11
Na 589.0 12 8/600 0.2 Air-C2H2 1.8 7

7-2 AA-6800/6650 Instruction


7.1 Measurement Conditions Table for Flame Atomic Absorption
Analysis

Wave length L233 L2433 Flow Burner. H


Element Slit (nm) Flame Type
(nm) (mA) (mA) (l/min) (mm)
Nb 334.9 24  0.2 N2O-C2H2 7.0 11
Ni 232.0 12 10/400 0.2 Air-C2H2 1.6 7
Os 290.9 14  0.2 N2O-C2H2 7.0 11
Pb (1) 217.0 12 8/300 0.5 Air-C2H2 2.0 7
Pb (2) 283.3 10 8/300 1.0 Air-C2H2 2.0 7
Pd 247.6 10 10/300 0.5 Air-C2H2 1.8 7
Pr 495.1 14  0.5 N2O-C2H2 7.0 11
Pt 265.9 14 10/300 0.5 Air-C2H2 1.8 7
Rb 780.0 14  0.2 Air-C2H2 1.8 7
Re 346.0 20  0.2 N2O-C2H2 7.0 11
Ru 349.9 20 20/600 0.2 Air-C2H2 1.8 7
Sb (H) 217.6 13 15/500 0.5 Air-C2H2 2.0 <HVG-1>
Sb 217.6 13 15/500 0.5 Air-C2H2 2.0 7
Sc 391.2 10  0.2 N2O-C2H2 7.0 11
Se (H) 196.0 23 15/300 1.0 Air-C2H2 2.0 <HVG-1>
Se 196.0 23 15/300 1.0 Ar-H2 [3.7] 15
Si 251.6 15 10/500 0.5 N2O-C2H2 7.7 11
Sm 429.7 14 15/600 0.2 N2O-C2H2 7.0 11
Sn (H) 286.3 10 20/500 1.0 Air-C2H2 2.0 <HVG-1>
Sn (1) 224.6 10 20/500 0.5 Air-C2H2 3.0 9
Sn (2) 286.3 10 20/500 1.0 Air-C2H2 3.0 9
Sn (3) 224.6 10 20/500 0.5 N2O-C2H2 6.8 11
Sn (4) 286.3 10 20/500 1.0 N2O-C2H2 6.8 11
Sr 460.7 8 6/500 0.5 Air-C2H2 1.8 7
Ta 271.5 18  0.2 N2O-C2H2 7.0 11
Tb 432.6 10  0.2 N2O-C2H2 7.0 11
Te (H) 214.3 14 15/400 0.2 Air-C2H2 2.0 <HVG-1>
Te 214.3 14 15/400 0.2 Air-C2H2 1.8 7
Ti 364.3 12 10/600 0.5 N2O-C2H2 7.8 11
Tl 276.8 6  0.5 Air-C2H2 1.8 7
V 318.4 10 10/600 0.5 N2O-C2H2 7.5 11
W 255.1 24  0.2 N2O-C2H2 7.7 11
Y 410.2 14 10/600 0.5 N2O-C2H2 7.5 11
Yb 398.8 10 5/200 0.5 N2O-C2H2 7.5 11
Zn 213.9 8 10/300 0.5 Air-C2H2 2.0 7
Zr 360.1 18 0.2 N2O-C2H2 7.5 11

AA-6800/6650 Instruction 7-3


Chapter 7 Appendix

NOTE
1. These measurement parameters are handled in the program as standard analysis parameters, but the
optimum measurement parameters may vary depending on the properties of the sample.
2. When hydrogen gas is used as the fuel gas, the actual flow rate of the hydrogen is larger than the
displayed fuel gas flow rate. The fuel gas flow rate in the brackets for the As or Se in this table is the
displayed value. Use this value in the brackets as the parameter for fuel gas flow rate. The actual flow
rate can be calculated as below.
Actual hydrogen gas flow rate # Displayed fuel gas flow rate u 3.5
3. <HVG-1> represents the special accessory Hydride Vapor Generator.
4. Ar-H2 flame for As and Se is used for normal measurement, not for hydrogen vapor generating method.

7-4 AA-6800/6650 Instruction


7.2 Analysis Line Wavelength Table for Flame Emission
7.2 Analysis Line Wavelength Table for Flame Analysis
Emission Analysis

Wavelength Wavelength Wavelength


Element Element Element
(nm) (nm) (nm)

Ag 328.1 Hf 531.2 Re 346.1

Al 396.2 Hg 253.7 Rh 343.5

As 193.7 In 451.1 Ru 372.8

Au 267.6 Ho 410.4 Sc 402.4

B 518.0* Ir 550.0 Si 251.6

Ba 455.4 K 766.5 Sm 476.0

Be 234.9 La 442.0 Sn 317.5

Bi 306.8 Li 670.8 Sr 460.7

Ca 422.7 Lu 451.9 Ta 474.0

Cd 326.1 Mg 285.2 Tb 534.0*

Ce 494.0* Mn 403.3 Te 486.6

Co 345.4 Mo 390.3 Ti 334.9

Cr 425.4 Na 589.0 Th 492.0

Cs 455.5 Nb 405.9 Tl 377.6

Cu 324.8 Nd 492.5 U 544.8

Dy 404.6 Ni 352.5 V 437.9

Er 400.8 Os 442.1 W 430.2

Eu 459.4 Pb 405.8 Y 597.2

Fe 372.0 Pd 363.5 Yb 398.8

Ga 417.2 Pr 495.1 Zn 636.2

Gd 622.0 Pt 265.9 Zr 360.1

Ge 265.1 Rb 794.8

*: Band spectrum

AA-6800/6650 Instruction 7-5


Chapter 7 Appendix
7.3 Graphite Tube Type Selection in Furnace
Method

In furnace method, it is effective to select a graphite tube according to the element and sample. There are three
graphite tube types widely used at present; high density graphite tube (hereinafter referred to as high density
tube), pyrolytic coating graphite tube (hereinafter, pyro-coated tube) and platform type graphite tube
(hereinafter, platform tube). The high density tube is made of ordinary graphite and most widely used. Since the
graphite has a porous characteristic, the injected sample solution permeates into the graphite wall in some
degree. On the other hand, the pyro-coated tube has a metalic luster on its surface, because it is made by
forming a pyrolitic layer on the surface of high density tube by the CVD method. Since the density of the surface
is higher than that of high density tube, the sample permeation into the wall is less. The platform tube refers to
a graphite tube in which a plate with a basin for containing the sample (platform) is mounted. The Shimadzu
platform tube has a platform made of 100 % pyrolitic carbon.
In this chapter, how to select these graphite tubes is described.

Pyro-coated

Platform

High density

Pyro-coated

Pyro-coated : High-density Pyro-coated : Platform


(Cu : 6 ppb) : (Cu : 60 ppb) (Cu : 6 ppb) : (Cu : 6 ppb)

Figure 7.1 Comparison of Peak Profiles (Left: between the pyro-coated tube and high density tube,
Right: between the platform tube and pyro-coated tube)

7.3.1 When Using a High Density Graphite Tube


The high density tube is used for measurements of various elements, and is often used especially for an
element whose atomization temperature is low. For example, Cd, Pb, Na, K, Zn and Mg are such elements. It is
also used to lower the measurement sensitivity in the case of a high concentration sample. For example, in the
case of Al, Fe and Cu, although a level of 1 ppb can be measured when the pyro-coated tube is used, the
measurement sensitivity can be lowered to a level of 100 ppb by using the high density tube. Figure 7.2 shows
an example of calibration curves for Cu measurements using the high density tube and pyro-coated tube. The
measurement points are 20, 40 and 60 ppb in the case of high density tube and 2, 4 and 6 ppb in the case of
pyro-coated tube, although the similar absorbances are shown.

7-6 AA-6800/6650 Instruction


7.3 Graphite Tube Type Selection in Furnace Method

7.3.2 When Using a Pyrolitic Coating Graphite Tube


Generally, the pyro-coated graphite tube is effective for elements which are easily combined with carbon or the
major component of graphite tube (carbide is easily formed). Ni, Ca, Ti, Si, V and Mo are the typical elements.
In the high density tube, a sample easily permeates into the graphite, resulting in a larger contact area between
the element and carbon. In the pyro-coated tube, however, a smaller contact area can suppress the carbide
formation, and as the result, a higher sensitivity is obtained.
When the peak profiles are compared, a sharp peak is observed in the case of pyro-coated tube, while a broad
peak is observed in the case of high density tube. Figure 7.1 shows the example in Cu. In the case of pyro-
coated tube, however, the result is easily affected by an acid concentration in sample and a sample spreading
in the tube varies widely. As the result, the reproducibility is tend to be inferior to that of the high density tube.
The effect of acid concentration on sensitivity is shown in Figure 7.3. The sensitivity varies more drastically as
the acid concentration changes, when compared with those of platform tube or high density tube.

7.3.3 When Using the Platform Type Tube


As a feature of the platform tube, the sample solution is injected onto the platform and heated as shown in
Figure 7.4. In the furnace method, the graphite tube is heated firstly from the wall, therefore, in normal tube, the
sample is heated and atomized as the wall is heated. In platform tube, however, the sample is atomized after
the temperature of entire tube reaches the atomization temperature (see Figure 7.5). In the measurement with
platform tube, the atomization peak becomes more broad in spite that the platform material is pyrolitic graphite
(see Figure 7.1). Also, it is more effective to set the temperature a little higher, compared with normal pyro-
coated tube. With this difference of heating sequence, however, using the platform tube can minimize the
influence of the sample liquid nature. This is because a recombination of atoms after atomization does not
easily occur in the platform tube, while it easily occurs with a low temperature of tube center in the case of wall
heating. As shown in Figure 7.3, the sensitivity change is small when the acid concentration changes largely.
Also, when a background signal is generated, a timing of atomization signal can be shifted from it. Therefore,
this is effective for samples with complicated matrix, such as biological sample, waste water and sea water.
This feature of platform tube often makes the latter part of peak profile not get down to baseline level within the
atomization stage. Set the time of atomization stage a little bit longer in such case.

AA-6800/6650 Instruction 7-7


Chapter 7 Appendix

Sensitivity comparison among graphite tubes

Absorbance

Pyro-coated
Platform
High density

Cu Concentration/ ppb

Figure 7.2 Sensitivity Comparison among Graphite Tube Types

Graphite tube types and acid concentration

High density
Pyro-coated
Platform
Absorbance

HNO3 Concentration/%

Figure 7.3 Effect of Nitric Acid Concentration on Pb Sensitivity among Graphite Tube Types
(Pb: 5 ppb, 10 PL injection)

7-8 AA-6800/6650 Instruction


7.3 Graphite Tube Type Selection in Furnace Method

Figure 7.4 Platform Type Graphite Tube

Platform type Pyro-coated (or high density)


graphite tube graphite tube

Figure 7.5 Temperature Distribution Image in Atomization Stage


(Low temperature is indicated in dark color.)

AA-6800/6650 Instruction 7-9


Chapter 7 Appendix
7.4 Error Messages

NOTE
Before contacting your Shimadzu service representative, record the following items.
• Content of error message
• Status in which the error message is displayed (indication screen, performed operation, measurement
file, "wizaa.ini" file in windows folder, etc.)
• Instrument information displayed at the upper in the initialization screen (model names of AA/ASC/GFA,
ROM version and serial No.)
• AA software version No. ([Help]-[About WizAArd] menu)

Error Message Cause/Details Remedial Measure

Number

x,x,x,...This lamp ID is • Select [None] for the Element field to clear


already in use. Please the overlapped lamp in [Lamp Position
select another ID. Setup] dialog box.
• When using plural lamps of the same
element and type simultaneously, register
each of the lamps in [Instrument]-[Lamp
History].

ACK has not been Communication protocol with ASC Verify the ASC power supply and the cable
accepted from ASC. was not completed. (:A) connection between ASC and AA main unit,
then connect the ASC in [Instrument]-[Option
Connect] menu.

ACK has not been Communication protocol with GFA Verify the GFA power supply and the cable
accepted from GFA. was not completed. (:A) connection between GFA and AA main unit,
then connect the GFA in [Instrument]-[Option
Connect] menu.

After leak check is Residual gas combustion was tried Residual gas combustion cannot be done
finished, ignite flame while executing the gas leak check. during execution of gas leak check. After
again. finishing the gas leak check, ignite a flame and
execute the residual gas combustion.

Analytical Line is not Line Search has failed. (1) Verify that the lamp is correctly mounted
found. The following causes are to the socket and the lamp turret position.
considerable. (2) Perform the wavelength correction in
(1) The lamp is not properly [Instrument]-[Maintenance]-[Wavelength
mounted to the lamp turret. Adjustment].
(2) The wavelength shift has
occurred in the
monochromator.

Another error No. was - The ROM program of the AA main unit has a
issued from GFA. problem.
Record the instrument information displayed
on the initialization screen and the status in
which this error occurs. Then contact your
Shimadzu service representative.

7-10 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Another error occurred - The ROM program of the AA main unit has
while recovering ASC a problem.
error. Record the instrument information
displayed on the initial screen and the
status in which this error occurs. Then
contact your Shimadzu service
representative.

ASC arm motor - • Verify that the ASC arm movement is


slipped. not impeded.
• Switch on the ASC again and connect
the ASC in [Instrument]-[Option
Connect] menu.

ASC arm rotation (1) The origin detector didn't detect (1), (2) Switch on the ASC main unit again.
position cannot be the origin correctly. If the error occurs again, record the status
initialized. (2) The arm rotation drive motor in which this error message appears and
doesn't operate. contact your Shimadzu service
representative.

ASC arm vertical (1) The origin detector didn't detect (1), (2) Switch on the ASC main unit again.
position cannot be the origin correctly. If the error occurs again, record the status
initialized. (2) The vertical arm drive motor in which this error message appears and
doesn't operate. contact your Shimadzu service
representative.

ASC cannot be Connection with ASC was interrupted. Verify the ASC power supply and the cable
detected. connection between ASC and AA main
unit, then connect the ASC in [Instrument]-
[Option Connect] menu.

ASC Error occurred - Remove the cause of error and switch on


during action. Press the ASC power again. Then connect the
Cancel to close this ASC in [Instrument]-[Option Connect]
dialog box. Resolve the menu and try this operation again.
ASC problem then
retry.

ASC I/F port is used for Communication with ASC is unstable. Verify the ASC power supply and the cable
another device. connection between ASC and AA main
unit, then connect the ASC in [Instrument]-
[Option Connect] menu.

ASC is disconnected, The ASC is not connected or the setup • Switch on the ASC and use
or ASC is set not to be for using ASC is not made, although [Instrument]-[Option Connect] menu
used in sequence [ASC Sample Pos. for EMISSION Line to connect the ASC.
parameter settings. Search] for Emission mode is selected • To make a setting to use the ASC,
in the Optics Parameters page to select [Using ASC] check box in the
execute the Line Search/Beam [Sequence] page.
Balance in Emission mode.

AA-6800/6650 Instruction 7-11


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

ASC Syringe 1 cannot (1) The origin detector didn't detect (1), (2) Switch on the ASC main unit again.
be initialized. the origin correctly. If the error occurs again, record the status
(2) The syringe drive motor doesn't in which this error message appears and
operate. contact your Shimadzu service
representative.

ASC table cannot be (1) The origin detector didn't detect (1), (2) Switch on the ASC main unit again.
initialized. the origin correctly. If the error occurs again, record the status
(2) The turntable drive motor doesn't in which this error message appears and
operate. contact your Shimadzu service
representative.

ASC table motor - • Verify that rotation of the ASC table is


slipped. not impeded.
• Switch on the ASC again and connect
the ASC in [Instrument]-[Option
Connect] menu.

ASC Timeout. The ASC doesn't response on the way Verify the ASC power supply and the cable
of the communication. connection between ASC and AA main
The communication cable with ASC unit, then connect the ASC in [Instrument]-
has a problem. [Option Connect] menu.

Atomizer cannot be The AA software tried to send the Verify that the [Instrument Type] (the main
moved from the automatic atomizer setup command to unit) is properly set in [Instrument]-
program with this the instrument but the atomizer [Configuration].
instrument. position setup of the instrument type is
manual.

Automatic burner/ The AA software has sent a command Verify that [Instrument Type] (Main Unit) is
furnace change system of atomizer automatic change, properly selected from [Instrument]-
does not exist. although the instrument is the manual [Configuration].
type of atomizer change.

Background signal is Beam Balance failed because the light (1)


too large to execute intensity of BG measurement is too • Increase the hollow cathode lamp
Beam Balance. greater than the light intensity of current (Low) (pay attention to the
hollow cathode lamp. max. current).
The following causes are
• When the lamp mode is BGC-D2,
considerable.
narrow the slit width.
(1) The light intensity of the hollow
cathode lamp becomes too (2)
smaller than the light intensity of • Set [Wavelength] correctly in [Optics
BG measurement as the result of Parameters] page.
change in the Optics Parameters, • If the wavelength shift has occurred in
etc. the monochromator, perform the
(2) The Line Search failed to catch wavelength correction in [Instrument]-
the correct analytical line. [Maintenance]-[Wavelength
(3) The light intensity becomes Adjustment].
smaller because of the
(3) Change the hollow cathode lamp.
exhaustion of hollow cathode
lamp.

7-12 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Background signal is Beam Balance failed because the light (1)


too small to execute intensity of hollow cathode lamp is too • Decrease the hollow cathode lamp
Beam Balance. greater than the light intensity of BG current (Low).
measurement.
• When the lamp mode is BGC-D2,
The following causes are
widen the slit width (pay attention to
considerable.
the neighboring line).
(1) The light intensity of hollow
cathode lamp becomes too (2)
greater than the light intensity of • Set [Wavelength] correctly in [Optics
BG measurement as the result of Parameters] page.
change in the Optics Parameters, • Narrow the slit width so as not to
etc. catch the neighboring line.
(2) The Line Search failed to catch
• If the wavelength shift has occurred in
the correct analytical line.
the monochromator, perform the
(3) The light intensity becomes
wavelength correction in [Instrument]-
greater because of the
[Maintenance]-[Wavelength
exhaustion of hollow cathode
Adjustment].
lamp.
(3) Change the hollow cathode lamp.
<When the lamp mode is BGC-D2>
(4) The light intensity of BG (4) Change the D2 lamp.
measurement becomes smaller (5) Adjust the D2 lamp position in
because of the exhaustion of D2 [Instrument]-[Maintenance]-[D2 Lamp
lamp. Position].
(5) The optical axis of D2 lamp is
shifted.

BG signal is too large. Beam Balance failed because the light (1)
intensity of BG measurement is too • Increase the hollow cathode lamp
greater than the light intensity of current (Low) (pay attention to the
hollow cathode lamp. max. current).
The following causes are
• When the lamp mode is BGC-D2,
considerable.
narrow the slit width.
(1) The light intensity of the hollow
cathode lamp becomes too (2)
smaller than the light intensity of • Set [Wavelength] correctly in [Optics
BG measurement as the result of Parameters] page.
change in the Optics Parameters, • If the wavelength shift has occurred in
etc. the monochromator, perform the
(2) The Line Search failed to catch wavelength correction in [Instrument]-
the correct analytical line. [Maintenance]-[Wavelength
(3) The light intensity becomes Adjustment].
smaller because of the
(3) Change the hollow cathode lamp.
exhaustion of hollow cathode
lamp.

AA-6800/6650 Instruction 7-13


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

BG signal is too small. Beam Balance failed because the light (1)
intensity of hollow cathode lamp is too • Decrease the hollow cathode lamp
greater than the light intensity of BG current (Low).
measurement.
• When the lamp mode is BGC-D2,
The following causes are
widen the slit width (pay attention to
considerable.
the neighboring line).
(1) The light intensity of hollow
(2)
cathode lamp becomes too
greater than the light intensity of • Set [Wavelength] correctly in [Optics
BG measurement as the result of Parameters] page.
change in the Optics Parameters, • Narrow the slit width so as not to
etc. catch the neighboring line.
(2) The Line Search failed to catch • If the wavelength shift has occurred in
the correct analytical line. the monochromator, perform the
(3) The light intensity becomes wavelength correction in [Instrument]-
greater because of the [Maintenance]-[Wavelength
exhaustion of hollow cathode Adjustment].
lamp.
(3) Change the hollow cathode lamp.
<When the lamp mode is BGC-D2>
(4) Change the D2 lamp.
(4) The light intensity of BG
measurement becomes smaller (5) Adjust the D2 lamp position in
because of the exhaustion of D2 [Instrument]-[Maintenance]-[D2 Lamp
lamp. Position].
(5) The optical axis of D2 lamp is
shifted.

Blank cannot be Inserting a blank measurement row Execute the blank measurement after the
inserted here. between the repeat measurement repeat measurements are finished.
rows was tried.

Buffer Overflow. Amount of the acquired data is larger Switch on the PC power and the
than the communication buffer of AA instrument power again. If the error occurs
software. again, check the following items.
• Set all of the PC BIOS setup and the
electric power saving function of
control panel to OFF.
• Don't start up other application
software simultaneously.

Calibration Curve The calibration curve order doesn't When the Zero Intercept is not selected,
cannot be created. match with the number of standard set the calibration curve order below the
samples. number of standard samples.
When the Zero Intercept is selected, set
the calibration curve order below the
number of standard samples or the same.

7-14 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Calibration Curve does Standard samples (STD or MSA) have Set up STD, in the case of calibration
not exist! not been measured. curve method, and MSA, in the case of
standard addition method or simple
standard addition method, on the MRT
worksheet and measure them.

Calibration Curve is not The calibration curve order doesn't When the Zero Intercept is not selected,
valid! match with the number of standard set the calibration curve order below the
samples. number of standard samples.
When the Zero Intercept is selected, set
the calibration curve order below the
number of standard samples or the same.

Cannot load file. - Change the current setting of


Measurement Type [Measurement Type] to other type in [Edit
(Calibration/SMSA) is Preparation Parameters] dialog box then
different. read out the target file.

Cannot load file. Mixing - Change the current setting of [Mixing ON]
ON/OFF status is check box to the opposite one in [Edit
different. Preparation Parameters] dialog box then
read out the target file.

Can't find drive X: The setup disk of AA software is Try to recover the setup disk using the
broken (at the time of installation). scan disk of Windows.

Can't heat furnace Heating was tried before the GFA Wait until the GFA transformer is cooled
during the GFA transformer had been cooled sufficiently, and then try the operation
transformer cooling sufficiently. again.
period. Please wait for
transformer to cool then
retry the operation.

Can't set temperature Sending the command to change the Set the furnace program after the heating
program when the GFA furnace program was tried during is finished.
heats furnace. heating.

Communication The communication between AA Switch on the PC power and the


Timeout. software and AA main unit has a instrument power again. If the error occurs
problem. again, check the following items.
• Switch on the power of the AA-6800/
6650 main unit and wait until a peep
sounds three times. Then set
[Connect] to ON.
• Set all of the PC BIOS setup and the
electric power saving function of
control panel to OFF.
• Fix all the communication cables (AA-
PC, AA-ASC, AA-GFA-EX7) with
screws to avoid an insufficient contact
and ground level mismatch of
communication port.

AA-6800/6650 Instruction 7-15


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

Communication was The communication between AA Switch on the PC power and the
aborted from the software and AA main unit has a instrument power again. If the error occurs
spectrophotometer problem. again, check the following items.
side. • Set all of the PC BIOS setup and the
electric power saving function of
control panel to OFF.
• Fix all the communication cables (AA-
PC, AA-ASC, AA-GFA-EX7) with
screws to avoid an insufficient contact
and ground level mismatch of
communication port.

Current measurement The lamp of current measurement Select [Lamp ON] check box in the [Optics
schedule cannot be element cannot be selected as warm- Parameters] page to light on the lamp of
selected. up lamp. current measurement element.

D2 lamp energy is too (1) The light intensity becomes (1) Change the D2 lamp.
low smaller as the result of D2 lamp (2) Adjust the D2 lamp position in
exhaustion. [Instrument]-[Maintenance]-[D2 Lamp
(2) The optical axis of D2 lamp is Position].
shifted.

D2 lamp energy is too Beam balance failed. (1) Change the D2 lamp.
low The following causes are (2) Adjust the D2 lamp position in
considerable. [Instrument]-[Maintenance]-[D2 Lamp
(1) The light intensity becomes Position].
smaller as the result of D2 lamp
exhaustion.
(2) The optical axis of D2 lamp is
shifted.

Drain tank water level is A flashback may be caused by an Fill water via the breather at the top of
too low. ignition without sufficient water in drain drain tank little by little until the water
tank. Therefore, be sure to fill the drain overflows from the drain tank to waste
tank with water before igniting a flame. container.

Emission vial position Although the ASC is to be used to Set the position of sample to be sprayed at
has not been set in the execute Line Search/Beam Balance in the time of Line Search/Beam Balance in
following Emission mode in the setting, [ASC [ASC Sample Pos. for EMISSION Line
measurement. Sample Pos. for EMISSION Line Search]. Entry for [ASC Sample Pos. for
Search] in [Optics Parameters] page is EMISSION Line Search] is available when
set to [NONE]. the [Lamp Mode] is set to "EMISSION" and
[Lamp Current (Low)] to "0".

7-16 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Error: Pressure Too (1) In the case of water pressure (1) In the case of water pressure
Low! • The water pressure supplied for Set the water pressure within the
the GFA-6500 is too low. range of specification.
• The water pressure supplied for
• In the case of GFA-6500, an error
GFA-EX7 is too low or too high.
message is not indicated when the
(2) In the case of Ar gas pressure
water pressure is too high. Since too
The Ar gas pressure supplied for
high water pressure may cause water
GFA is too low.
leak, be careful about it.
• In the case of GFA-EX7, note that the
message "ERROR: Pressure is too
low!" is also displayed even if the
water pressure is too high. Be careful
about it.
(2) In the case of Ar gas pressure
Open the stopcock of Ar gas and
adjust the pressure regulator so that
the supply pressure satisfies the
specification.

Error: Pressure Too The water pressure supplied for GFA- Set the water pressure within the range of
Low or Too High! EX7 is too low or too high. specification.

Expired Lamp is The lamp selected in [Lamp Position • Although the "Used Time" is one of
selected. Reestablish Setup] dialog box has a relation (Life the signs to change the lamp, a lamp
the setting? Time) < (Used Time). used for longer than the life time can
be used if Line Search/Beam Balance
is performed successfully and if the
noise level required for the analysis is
satisfied.
• Select [Instrument]-[Configuration]
menu and clear the check box of
[Show lamp used time over operating
life message] not to display this
message.

Failed to Add New When the number of Element Delete unnecessary Element Schedules in
Schedule. Schedules on the MRT worksheet [Element Selection] page. Also, clear the
exceeds 20, the excess schedules check box of unnecessary element in
cannot be read out on the MRT. [Element Selection] list when reading out
parameters in the Template page of [Load
Parameters] dialog box.

Failed to detect burner (1) The origin detector couldn't detect (1), (2) Switch on the AA main unit again.
moving motor (fore/ the origin correctly. If the error occurs again, record the status
back) origin. (2) The burner forward/back in which this error message appears and
movement motor doesn't operate contact your Shimadzu service
properly. representative.

AA-6800/6650 Instruction 7-17


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

Failed to detect burner (1) The origin detector couldn't detect (1), (2) Switch on the AA main unit again.
moving motor (up/ the origin correctly. If the error occurs again, record the status
down) origin. (2) The burner up/down movement in which this error message appears and
motor doesn't operate properly. contact your Shimadzu service
representative.

Failed to detect lamp (1) The origin detector couldn't detect (1), (2) Switch on the AA main unit again.
turret motor origin. the origin correctly. If the error occurs again, record the status
(2) The lamp turret motor doesn't in which this error message appears and
operate properly. contact your Shimadzu service
representative.

Failed to detect slit (1) The origin detector didn't detect (1), (2) Switch on the AA main unit again.
motor origin. the origin correctly. If the error occurs again, record the status
(2) The slit drive motor doesn't in which this error message appears and
operate. contact your Shimadzu service
representative.

Failed to detect (1) The origin detector couldn't detect (1), (2) Switch on the AA main unit again.
wavelength motor the origin correctly. If the error occurs again, record the status
origin. (2) The wavelength drive motor in which this error message appears and
doesn't operate properly. contact your Shimadzu service
representative.

Failed to execute Gas Gas leak check couldn't be started. Switch on the AA main unit again.
Leak Check command. If the error occurs again, stop using the
instrument and record the error messages
and status before and after this error. Then
contact your Shimadzu service
representative.

Failed to extinguish the EXTINGUISH button of the instrument Press the EXTINGUISH button following
flame. was not pressed while executing the the instruction displayed while executing
remaining gas combustion. the residual gas combustion.

Failed to load The "cookbook.ref" file in the folder in Delete the "cookbook.ref" file and install it
Cookbook which the AA software is installed again.
cannot be read in. The version of
"cookbook.ref" doesn't match the
execution file, or the file is broken.

Failed to load Measurement file or template file Check the following points.
document. cannot be read out in [Wizard • The file tried to load actually exists.
Selection] dialog box.
• The file name contains no period
except the period just before the
extension (for example, a file named
"Cu.Ag.aa" cannot read out).

7-18 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Failed to open the The PC serial port cannot be used. Check the following points.
serial port. • [COM port] in [Instrument]-
[Configuration] is properly set.
• Other application software
(communication software, FAX
software, etc.) is not used.
• The resource of the communication
port doesn't compete with other
device.

Failed to send - Close this message and wait until


parameters to the "READY" is displayed at the right lower of
instrument. Wait until the status bar. Then perform the target
the instrument operation again.
becomes READY then
retry it.

Failed to send the The GFA instrument type selected in Set the correct [GFA] in [Instrument]-
furnace program for the AA software is wrong. [Configuration] menu then start up the AA
GFA cleaning. software again.

Failed to send the The GFA instrument type selected in Set the correct [GFA] in [Instrument]-
temperature coefficient. the AA software is wrong. [Configuration] menu then start up the AA
software again.

Failed to send the The GFA instrument type selected in Set the correct [GFA] in [Instrument]-
temperature the AA software is wrong. [Configuration] menu then start up the AA
stabilization time. software again.

Failed to set Flame Flame monitor couldn't be set OFF Stop using the instrument, switch on the
Monitor Safety Device while executing the residual gas power again and connect it with the PC
to OFF. combustion. again. If the item [Flame Monitor ON]
becomes NG, contact your Shimadzu
service representative.

Failed to turn OFF the The gas pressure monitor couldn't be Stop using the instrument. Then switch on
gas pressure monitor. set OFF while executing the residual the power again and reconnect it with the
gas combustion. PC. If NG is displayed for the item [Gas
Pressure Monitor ON] on the initialization
screen, contact your Shimadzu service
representative.

Failed to turn ON the The gas pressure monitor couldn't be Stop using the instrument. Then switch on
gas pressure monitor. set ON when the residual gas the power again and reconnect it with the
combustion was finished or cancelled. PC. If NG is displayed for the item [Gas
Pressure Monitor ON] on the initialization
screen, contact your Shimadzu service
representative.

AA-6800/6650 Instruction 7-19


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

Flame has been (1) The flame monitor detected that (1) Verify that nothing obstructs the flame
extinguished. the flame is extinguished monitor.
although the EXTINGUISH button (2) When using Ar-H2 flame, clear [Flame
is not pressed. Monitor ON] check box in
(2) When using Ar-H2 flame, the [Instrument]-[Gas controller Status] to
flame monitor was activated invalidate the flame monitor. When
because the flame is colorless. performing a measurement in this
status, always stay near the
instrument and check the flame
doesn't go out.

Flame Monitor Safety Flame monitor couldn't be set ON Stop using the instrument, switch on the
Device was not set. while executing the residual gas power again and connect it with the PC
combustion. again. If the item "Flame Monitor ON"
becomes NG, contact your Shimadzu
service representative.

Fuel gas leak detected. As the result of gas leak check, a gas Stop using the instrument and contact your
leak from the tubing inside the gas Shimadzu service representative.
controller was detected.

Fuel gas pressure is (1) The supply pressure of fuel gas (1) Open the stopcock and check the
too low. (C2H2 or H2) or support gas (Air supply pressure of fuel/support gas by
or N2O) has decreased. the meter of pressure regulator. If the
required pressure is not satisfied,
(2) The PURGE button on the gas
change the fuel/support gas cylinder,
controller panel of AA main unit
check/adjust the air compressor
was pressed.
operation or perform other
(3) Automatic flame extinction was appropriate treatment.
executed at the end time of
(2), (3) This doesn't mean an abnormal
automatic measurement using the
status. Close the message and
ASC.
continue the operation.
(4) The flame monitor safety device
(4) Eliminate the cause with which the
was activated.
flame was extinguished. If the supply
(5) There was a momentary AC pressure of fuel/support gas is not
power outage. lowered and if an ignition is possible,
there is no problem.
(5) Start up the instrument again. If the
supply pressure of fuel/support gas is
not lowered and if an ignition is
possible, there is no problem.
If the error occurs again, record the status
in which this error is displayed and contact
the Shimadzu service representative.

7-20 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Furnace is not Heating was tried before the graphite • Wait until the graphite tube is cooled
sufficiently cooled. furnace is cooled sufficiently. The sufficiently, and then try the operation
Check that cooling temperature of cooling water is high or again.
water is supplied the flow of cooling water is not • Verify that the cooling water
properly. sufficient. temperature and pressure are within
the specifications of the instrument
and that the cooling tubes are not
pressed or bent.

Furnace program does Original furnace program for the Return to [Furnace Program] page and set
not exist. optimum furnace program search has up a furnace program.
not been set up.

Gas leak was found. (1) When the error message is (1) Stop using the instrument and contact
displayed within 10 minutes after your Shimadzu service
the gas leak check is started: representative.
As the result of gas leak check, a (2) Close this message and continue the
gas leak from the tubing in the operation.
gas control unit was detected.
(2) When the error message is
displayed after 10 minutes or
more from the starting of gas leak
check:
This doesn't mean any abnormal
status. In case of gas leak, an
error occurs immediately after the
starting of check.

Gas pressure was too - Check the gauge of the pressure regulator
low to execute gas leak and verify that the supply pressure
check. Please check satisfies the specification. If the required
that the fuel gas supply pressure is not detected, perform
pressure and execute appropriate measures such as
the gas leak check. replacement of fuel gas cylinder.

GFA-6500: Furnace is Heating was tried before the graphite • Wait until the graphite tube is cooled
not sufficiently cooled. furnace is cooled sufficiently. The sufficiently, and then try the operation
GFA-EX7: Furnace is temperature of cooling water is high or again.
not sufficiently cooled the flow of cooling water is not • Verify that the cooling tubes are not
or cooling water is too sufficient. pressed or bent.
cool. In the case of GFA-EX7, the lower limit
• Verify that the cooling water
Check that the cooling of cooling water temperature is also
temperature and pressure are within
water temperature are checked. Therefore, the error also
the specifications of the instrument.
within the specifications occurs when the cooling water is too
of the instrument and it cool.
is supplied properly.

GFA cannot be Connection with GFA was interrupted. Verify the GFA power supply and the cable
detected. connection between GFA and AA main
unit, then connect the GFA in [Instrument]-
[Option Connect] menu.

AA-6800/6650 Instruction 7-21


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

GFA gas pressure is - Open the Ar gas stopcock and verify that
too low. the supply pressure satisfies the
specification.

GFA heating is OFF. If this error occurs again after Open the graphite furnace and rotate the
1.Turn on the power executing the measures following the graphite tube forward and back while
switch (HEAT) of GFA. message, the contact between the pressing the end of the graphite tube to the
2.Make sure that a graphite cap or holder and the graphite graphite cap or holder. Through this
graphite tube is set and tube may be improper. procedure, the contact with the graphite
the graphite furnace is tube will be recovered.
fastened.

GFA I/F port is used for Communication with GFA is unstable. Verify the GFA power supply and the cable
other device. connection between GFA and AA main
unit, then connect the GFA in [Instrument]-
[Option Connect] menu.

GFA is NOT initialized. Although the initialization command of (1) Verify the GFA power supply and the
Please perform option GFA-EX7 had not been sent, other cable connections between GFA and
connect. If you see this command was sent. AA main unit, then connect the GFA
message during option (1) The power supply of GFA has in [Instrument]-[Option Connect]
connect, check GFA once failed then recovered. menu.
instrument type in (2) Set the correct [GFA] in [Instrument]-
(2) The initialization command was
[Instrument]- [Configuration] menu then start up the
not sent because the GFA
[Configuration]. AA software again.
instrument type selected in the
AA software was wrong.

GFA returns invalid The temperature calibration couldn't Switch on the GFA again. If the error
Temperature be performed correctly. occurs again, record the number indicated
Coefficient! -(Value of in this message and the status in which
Invalid Temperature this error message appears. Then contact
Coefficient)- your Shimadzu service representative.

GFA serial interface - The ROM program of the AA main unit has
cannot be opened. a problem.
Record the instrument information
displayed on the initialization screen and
the status in which this error occurs. Then
contact your Shimadzu service
representative.

GFA Temperature The graphite tube may have been Change the graphite tube for a good one.
Calibration Error. worn out. If the error occurs again, contact your
Or the optical temperature sensor has Shimadzu service representative.
a problem.

GFA timed out. The GFA doesn't response on the way Verify the GFA power supply and the cable
of the communication. connection between GFA and AA main
The communication cable with GFA unit, then connect the GFA in [Instrument]-
has a problem. [Option Connect] menu.

7-22 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

GFA water pressure is [GFA-6500] Set the water pressure within the range of
too low. The water pressure of GFA is too low. specification and use it.
[GFA-EX7] • In the case of GFA-6500, an error
The water pressure of GFA is too low message is not indicated when the
or too high. water pressure is too high. Since too
high water pressure may cause water
leak, be careful about it.
• In the case of GFA-EX7, note that the
message "ERROR: Pressure is too
low!" is also displayed even if the
water pressure is too high. Be careful
about it.

GFA water pressure is The water pressure of GFA-EX7 is too Set the water pressure within the range of
too low or too high. low or too high. specification and use it.

HC Lamp Energy is Sufficient light intensity of hollow (1)


insufficient. cathode lamp could not be obtained • Verify that the atomizer or any other
during the wavelength adjustment. thing doesn't obstruct the optical axis.
The following causes are
• Verify that the lamp is correctly
considerable.
mounted to the socket and the lamp
(1) The optical axis has a problem. turret position.
(2) The light intensity of the hollow • Rotate the hollow cathode lamp and
cathode lamp becomes too small adjust the optical axis.
as the result of change in the
(2)
Optics Parameters, etc.
• Increase the hollow cathode lamp
(3) The Line Search failed to catch
current (Low) (pay attention to the
the correct analytical line.
max. current).
(4) The light intensity becomes
• Widen the slit width (pay attention to
smaller because of the
neighboring lines).
exhaustion of hollow cathode
lamp. (3) Set [Wavelength] correctly in [Optics
Parameters] page.
(4) Change the hollow cathode lamp.

AA-6800/6650 Instruction 7-23


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

HC lamp energy is too The light intensity of the hollow (1)


low. cathode lamp (or emission intensity in • Verify that the socket to which the
the case of flame emission analysis) is lamp is mounted and the lamp turret
small and the Line Search/Beam position are correctly set.
Balance failed.
• Rotate the hollow cathode lamp to
The following causes are
adjust the optical axis.
considerable.
In the case of atomic absorption (2)
analysis: • Verify that there is no obstacle on the
(1) The hollow cathode lamp is not light path.
set in the lamp turret correctly. • If the burner head or furnace
(2) The optical path is obstructed. intercepts the light, adjust the origin
position.
(3) The light intensity of the hollow
cathode lamp becomes too (3) Increase the lamp current (Low) or
smaller as the result of change in widen the slit width in the [Optics
the Optics Parameters, etc. Parameters] page.

(4) The Line Search failed to catch (4)


the correct analytical line. • Set [Wavelength] correctly in [Optics
(5) The light intensity becomes Parameters] page.
smaller because of the • If the wavelength shift has occurred in
exhaustion of hollow cathode the monochromator, perform the
lamp. wavelength correction in [Instrument]-
<In the case of flame emission [Maintenance]-[Wavelength
analysis> Adjustment].

(6) The emission intensity of the (5) Change the hollow cathode lamp.
standard sample of the highest (6)
concentration is too small. • Use a proper flame type.
• Adjust the burner height so that the
maximum signal may be obtained.
• Use a standard sample of higher
concentration.

Invalid Temperature Starting up the AA software detected In the case of GFA-EX7, after connecting it
Coefficient is saved in that the temperature calibration with the instrument, mount the graphite
INI file! -(Value of coefficient (key: TempCoef) saved in tube to be used for measurement following
Iinvalid Temperature "wizaa.ini" file in "windows" folder is [Change GFA Tube] in [Furnace Program]
Coefficient)- out of the proper range. page then click [Temp.Calib] to execute
the temperature calibration.

Incorrect interface - The ROM program of the AA main unit has


handshake with ASC. a problem.
Record the instrument information
displayed on the initialization screen and
the status in which this error occurs. Then
contact your Shimadzu service
representative.

7-24 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Incorrect interface - The ROM program of the AA main unit has


handshake with GFA. a problem.
Record the instrument information
displayed on the initialization screen and
the status in which this error occurs. Then
contact your Shimadzu service
representative.

Instrument failed to Gas leak check start command was Switch on the PC power and instrument
execute the command. not executed properly. power again. If the error occurs again,
Please restart the contact your Shimadzu service
instrument and representative.
software and retry Leak
Check.

Instrument is not ready! (1) A send command was attempted (1) Set the communication with the
when the communication instrument to ON from [Instrument]-
between the instrument and PC is [Connect] menu.
OFF. (2) Close this message box and wait until
(2) While the instrument is executing the command currently executed in
the command, the next send the instrument is finished. Perform the
command was attempted. target operation again after "READY"
is displayed at the right lower of the
status bar.

Instrument is still busy. The operation that cannot be executed Close this message and wait until
during BUSY status of instrument was "READY" is displayed at the right lower of
attempted. the status bar. Then perform the target
operation again.

Invalid ASC Command. A command that is not supported by Verify that the AA software supports the
the ASC was sent from the AA your ASC.
software.

Invalid ASC Parameter. Parameters that are not supported by Verify that the AA software supports the
the ASC were sent from the AA your ASC.
software.

Invalid error No. has - The ROM program of the AA main unit has
been sent from ASC. a problem.
Record the instrument information
displayed on the initialization screen and
the status in which this error occurs. Then
contact your Shimadzu service
representative.

Invalid error No. was - The ROM program of the AA main unit has
sent from GFA. a problem.
Record the instrument information
displayed on the initialization screen and
the status in which this error occurs. Then
contact your Shimadzu service
representative.

AA-6800/6650 Instruction 7-25


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

Invalid GFA Command A command that is not supported by Verify that the [GFA] is correctly selected
the GFA was sent from the AA in the [Instrument]-[Configuration].
software.

Invalid GFA Parameters that are not supported by Verify that the [GFA] is correctly selected
Parameters the GFA were sent from the AA in the [Instrument]-[Configuration].
software.

J, K

Lamp energy is too low Beam Balance failed because the light (1)
to execute Beam intensity of hollow cathode lamp is too • Increase the hollow cathode lamp
Balance. small. current (Low) (pay attention to the
The following causes are max. current).
considerable.
• Widen the slit width (pay attention to
(1) The light intensity of the hollow neighboring lines).
cathode lamp becomes too small
(2)
as the result of change in the
Optics Parameters, etc. • Set [Wavelength] correctly in [Optics
Parameters] page.
(2) The Line Search failed to catch
the correct analytical line. • If the wavelength shift has occurred in
the monochromator, perform the
(3) The light intensity becomes
wavelength correction in [Instrument]-
smaller because of the
[Maintenance]-[Wavelength
exhaustion of hollow cathode
Adjustment].
lamp.
(3) Change the hollow cathode lamp.

Lamp History data file (1) "lamphist.ref" file doesn't exist in (1) Check whether the name
(lamphist.ref) cannot be the folder in which the AA "lamphist.ref" was changed or not and
found. software is installed. whether it has been moved to other
(2) Execution file (wizaa.exe) was folder or not. If so, set it back to
copied in the folder other than the original condition. If "lamphist.ref" file
installation folder and was doesn't exist in the install folder, the
executed. AA software creates a new file.
(2) Be sure to execute "wizaa.exe" from
the install folder.

Lamp ID is not valid. In [Lamp Position Setup] dialog box, Select [Instrument]-[Lamp History] menu
Register the proper select a lamp to be used from the and register the lamp to be used.
lamp in Lamp History lamps registered in [Lamp History]
dialog box, then set the dialog box. Therefore, register the
lamp turret position. lamp in [Lamp History] dialog box
when using a lamp that is not
registered.

7-26 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Lamp Socket # is not [Socket #] in the [Optics Parameters] Set up the Socket # in the [Optics
selected in this page of the element for warm-up is set Parameters] page of the element for
schedule. to [NONE]. warm-up. When the Socket # you wish to
set is not displayed in the list, set up the
lamp mounted to the Socket # in [Lamp
Pos. Setup]. (If the Lamp ID of the lamp
you wish to set is not displayed in the
[Lamp Position Setup] dialog box, register
the lamp in [Instrument]-[Lamp History]).

Lamp Socket # is [Socket #] of the element for warm-up Set up the Socket # in the [Optics
wrong. This schedule in the [Optics Parameters] page is set Parameters] page. When the Socket # you
cannot be selected for to [NONE]. wish to set is not displayed in the list, set
warmup lamp. up the lamp mounted to the Socket # in
[Lamp Pos. Setup]. (If the Lamp ID of the
lamp you wish to set is not displayed in the
[Lamp Position Setup] dialog box, register
the lamp in [Instrument]-[Lamp History].)

Lamp socket# is not - In the [Optics Parameters] page of the


specified! Please set element named in the message, set the
socket# for the socket number. If the aimed socket
following elements. number is not displayed on the list, set the
lamp mounted to the aimed socket number
in [Lamp Pos. Setup]. (Furthermore, if the
lamp of aimed element and type is not
displayed on the list in [Lamp Position
Setup] dialog box, register the lamp in
[Instrument]-[Lamp History].)

Lamp Used Time In [Lamp History] dialog box, the lamp • Although the "Used Time" is one of
exceeded the Life Time to be used has a relation "(Life Time) < the sign to change the lamp, a lamp
(Used Time)". used for longer than the life time can
be used if Line Search/Beam Balance
is performed successfully and if the
noise level required for the analysis is
satisfied.
• Select [Instrument]-[Configuration]
menu and clear the check box of
[Show lamp used time over operating
life message] not to display this
message.

Memory Lock Failure The memory reserved for Switch on the PC power and the
communication by AA software instrument power again. If the error occurs
couldn't be locked. again, check the following items.
• Set all of the PC BIOS setup and the
electric power saving function of
control panel to OFF.
• Don't start up other application
software simultaneously.

AA-6800/6650 Instruction 7-27


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

Mixing is OFF and If the injection volume is too large, the Select an appropriate injection volume
Injection volume is sample overflows from the graphite after checking that the sample doesn't
more than 100 PL. Are tube. overflow from the graphite tube.
you sure?

Momentary electric Momentary power failure of the AC Switch on the AA main unit again.
shutdown occurred in power supply was detected. If the error occurs again, record the status
the gas controller. in which this error occurs. Then contact
Forcibly support gas your Shimadzu service representative.
type is changed to Air
and flame monitor is set
to ON.

No lamps which can be [Socket #] in the [Optics Parameters] Set up the Socket # in the [Optics
used for this page is set to [NONE]. Parameters] page. When the Socket # you
measurement are set. wish to set is not displayed in the list, set
Set a lamp which is up the lamp mounted to the Socket # in
suitable for [Lamp Pos. Setup]. (If the Lamp ID of the
measurement element lamp you wish to set is not displayed in the
and lamp mode. [Lamp Position Setup] dialog box, register
the lamp in [Instrument]-[Lamp History].)

No. of Mixing Cycles is The setting of [Mixing ON] is not Set up [Mixing ON] in [ASC Parameters]
Invalid. properly saved in the measurement page again.
parameters.

Other program is using "lamphist.ref" file is a data file for lamp (1) "lamphist.ref" can be renewed from
lamphist.ref file. Lamp history. The following causes are the AA software firstly started up but
data will not be saved. considerable when this message is cannot be renewed from the AA
displayed. software secondly started up.
(1) The second AA software has Therefore, use the AA software firstly
been started up. started up to perform measurement.
There is no problem to use the AA
(2) The file attribute of "lamphist.ref"
software secondly started up to edit
is read-only.
parameters.
(2) Turn the read-only attribute of
"lamphist.ref" file in AA software
folder OFF.

7-28 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Other program is using "lampplace.ref" file is a data file for (1) "lampplace.ref" can be renewed from
lampplace. ref file. lamp position setup. The following the AA software firstly started up but
Lamp data will not be causes are considerable when this cannot be renewed from the AA
saved. message is displayed. software secondly started up.
(1) The second AA software has Therefore, use the AA software firstly
been started up. started up to perform measurement.
There is no problem to use the AA
(2) The file attribute of
software secondly started up to edit
"lampplace.ref" is read-only.
parameters.
(2) Turn the read-only attribute of
"lampplace.ref" file in AA software
folder OFF.

Periodic Blank - If an invalid value that is not usually


Preparation entered has been entered in the Blank
Parameters is Invalid. Samples table of the [Edit Preparation
Parameters] dialog box, enter a correct
value.

Please connect ASC. (1) Although the autosampler is (1) Verify the ASC power supply and the
necessary for the operation, the cable connection between ASC and
ASC is not connected. AA main unit, then connect the ASC
(2) Although the ASC is used in the in [Instrument]-[Option Connect]
measurement conditions, the menu.
ASC is not connected. (2) When the ASC is necessary for the
measurement, connect the ASC in the
procedure as above. When the ASC
is not necessary, clear the [Using
ASC] check box in the [Parameters]-
[Edit Parameters]-[Sequence].

Please connect GFA The GFA power is set OFF or the Verify the GFA power supply and the cable
serial interface. communication cable between GFA connection between GFA and AA main
and AA main unit is disconnected. unit, then connect the GFA in [Instrument]-
[Option Connect] menu. Fix the
communication cable between GFA-EX7
and AA main unit with the screws.

Please connect GFA. The GFA is not connected although Verify the GFA power supply and the cable
the GFA is necessary for the operation connection between GFA and AA main
or measurement. unit, then connect the GFA in [Instrument]-
[Option Connect] menu.

Please connect the The ASC power is set OFF or the Verify the ASC power supply and the cable
ASC serial interface. communication cable between ASC connection between ASC and AA main
and AA main unit is disconnected. unit, then connect the ASC in [Instrument]-
[Option Connect] menu. Fix the
communication cable between ASC and
AA with the screws.

Please select the Flame type is not selected properly in Select a correct flame type in [Atomizer/
Flame Type. [Atomizer/Gas Flow Rate Setup] page. Gas Flow Rate Setup] page.

AA-6800/6650 Instruction 7-29


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

Please set the socket # The lamps cannot be lit on • Change the order of measurements in
combining even/odd in simultaneously when their socket # the [Element Selection] page so that
turn. combination is even/even or odd/odd. the socket number combination may
Therefore, when measuring many be even/odd in turn.
elements, it is recommended to set up • When you wish not to change the
the even/odd of the socket # in turn to order of measurements or when
perform efficient warm-up. changing the measurement order
cannot make the even/odd
combination, change the lamp
mounting position by [Lamp Pos.
Setup] in [Optics Parameters] page.

Please set the total - Change the furnace program so that the
time of Furnace total time of the furnace program may be
Program less than 300 within 300 seconds.
(sec).

Please set the total Since the data sampling is started When the sampling stage is in the first row:
time before the before executing the sampling stage in Insert a stage of 3 seconds or longer
sampling stage more the furnace program, a stage of 3 before the sampling stage.
than 3 (sec). seconds or longer is always necessary When the sampling stage is in the second
prior to the sampling stage. row or after:
Change the program so that the total time
of the stages before the sampling stage
may be 3 seconds or longer.

Please specify the lamp Line Search/Beam Balance couldn't Set up the Socket # in [Optics Parameters]
socket#. be executed because [Socket #] in the page of the current measurement element.
[Optics Parameters] page is set to When the Socket # you wish to set is not
[NONE]. displayed in the list, set up the lamp
mounted to the Socket # in [Lamp Pos.
Setup]. (If the Lamp ID of the lamp you
wish to set is not displayed in the [Lamp
Position Setup] dialog box, register the
lamp in [Instrument]-[Lamp History].)

Q, R

Sample Preparation - If an invalid value that is not usually


Parameters is Invalid. entered has been entered, enter a correct
value in the Unknown Samples table in the
[Edit Preparation Parameters] dialog box.

Schedule does not In the measurement using the ASC, Select the measurement element and set
exist! Element schedule has not been up the measurement procedure in [Action]
selected, or the measurement fields on the MRT worksheet.
procedure has not been set up
although the element schedule exists.

7-30 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Serial interface cannot - The ROM program of the AA main unit has
be opened. a problem.
Record the instrument information
displayed on the initialization screen and
the status in which this error occurs. Then
contact your Shimadzu service
representative.

Serial Port Error. The PC serial port has a problem. Switch on the PC power and the
instrument power again. If the error occurs
again, check the following items.
• Set all of the PC BIOS setup and the
electric power saving function of
control panel to OFF.
• Fix all the communication cables (AA-
PC, AA-ASC, AA-GFA-EX7) with
screws to avoid an insufficient contact
and ground level mismatch of
communication port.
• To avoid overrun of PC serial port,
lower the receive buffer of FIFO on
the control panel.

Set the flame The attempted operation cannot be After changing the measurement mode of
measurement as a executed unless the flame the instrument to flame, execute the target
current measurement. measurement mode is set in the operation. Perform the following operation
instrument. to change the measurement mode of the
instrument to flame.
When the flame measurement exists on
the MRT:
Select the flame measurement from the
measurement element tool bar.
When the flame measurement doesn't
exist on the MRT:
Select [Parameters]-[Element Selection
Wizard] and add a flame measurement by
[Select Elements] in the [Element
Selection] page. Then select the
measurement from the [Meas. Element]
drop-down list as current measurement
element and click on [Finish].

AA-6800/6650 Instruction 7-31


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

Set the furnace The attempted operation cannot be After changing the measurement mode of
measurement as a executed unless the furnace the instrument to furnace, execute the
current measurement. measurement mode is set in the target operation. Perform the following
instrument. operation to change the measurement
mode of the instrument to furnace.
When the furnace measurement exists on
the MRT:
Select the furnace measurement from the
measurement element tool bar.
When the furnace measurement doesn't
exist on the MRT:
Select [Parameters]-[Element Selection
Wizard] and add a furnace measurement
by [Select Elements] in the [Element
Selection] page. Then select the
measurement from the [Meas. Element]
drop-down list as current measurement
element and click on [Finish].

Since odd/even of the The measurement element is edited Close the message and set up the warm-
socket # was the same when the warm-up lamp is lit on, and up lamp again in [Optics Parameters] page
as that of measurement as the result, the warm-up lamp socket of the current measurement element.
lamp, the warmup lamp # and the measurement element lamp
was lit off and the socket # become the same odd/even
setting was cleared. number.

Spectrophotometer has - Switch on the PC power and the


not been turned ON or instrument power again. If the error occurs
cable is disconnected. again, check the following items.
• Verify that the communication cables
between AA main unit and PC are
connected properly and fixed with
screws.
• Set all of the PC BIOS setup and the
electric power saving function of
control panel to OFF.

Standard Preparation - If an invalid value that is not usually


Parameters is Invalid. entered has been entered in the STD
Samples table of the [Edit Preparation
Parameters] dialog box, enter a correct
value.

Support gas pressure is (1) The supply pressure of support (1) Open the stopcock and check the
too low. gas (Air or N2O) has decreased. supply pressure of support gas by the
(2) The support gas pressure was meter of the pressure regulator. If the
lowered from the gas controller required pressure is not satisfied,
panel on the right side of the AA change the support gas cylinder,
main unit. check/adjust the air compressor
operation or perform other
appropriate treatment.
(2) Set the proper pressure.

7-32 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Switch the Flame Type When the support gas is N2O, Set [Flame Type] to [AIR-C2H2] in
to AIR-C2H2 before the executing the residual gas combustion [Atomizer/Gas Flow Rate Setup] page and
remaining gas may cause a flashback. switch [BURNER SELECT] (burner
combustion. selection key switch) of the AA main unit to
[AIR-C2H2] side. Then execute the
residual gas combustion.

Termination has not Communication protocol with ASC Verify the ASC power supply and the cable
been accepted from was not completed. (:T) connection between ASC and AA main
ASC. unit, then connect the ASC in [Instrument]-
[Option Connect] menu.

Termination has not Communication protocol with GFA Verify the GFA power supply and the cable
been accepted from was not completed. (:T) connection between GFA and AA main
GFA. unit, then connect the GFA in [Instrument]-
[Option Connect] menu.

The following lamps The data mismatching between the Click on [Yes] and delete the data from the
exist in the Lamp lamp history and the lamp position lamp position setup. Register the
Position Setup Dialog setup was detected at the time of necessary lamps in [Instrument]-[Lamp
Box, but do not exist in starting up the AA software. History]. Next, make a setting of the lamp
the Lamp History mounted to each socket in [Instrument]-
Dialog Box. Please [Lamp Position Setup].
update the Lamp
History Dialog Box or
delete lamps from the
Lamp Position Setup
Dialog Box. Socket
#x,x,x,...

The GFA instrument The GFA instrument type selected in Set the correct [GFA] in [Instrument]-
type is not selected the AA software is wrong. [Configuration] menu then start up the AA
correctly. Please select software again.
proper GFA instrument
type and restart this
software.

The instrument fail to The gas flow rate setup command has When an error occurs to the fuel gas flow
adjust the gas flow rate failed. rate setup in [Atomizer/Gas Flow Rate
to the optimal position. Setup] page, stop using the instrument
and contact your Shimadzu service
representative.

The instrument fail to The burner movement command has Remove the obstacles that disturb the
move the burner to the failed. burner movement then switch on the
optimal position. instrument power again.

The selected area - In [Instrument]-[Lamp Position Setup]


cannot be cleared as menu, select [NONE] for [Element] field of
the information is the lamp ID you wish to clear, and click on
stored in the Lamp [OK]. Then clear the target lamp in [Lamp
Position Setup Dialog History] dialog box.
Box.

AA-6800/6650 Instruction 7-33


Chapter 7 Appendix

Error Message Cause/Details Remedial Measure

The selected area - In [Instrument]-[Lamp Position Setup]


cannot be deleted as menu, select [NONE] for [Element] field of
the information is the lamp ID you wish to delete, and click
stored in the Lamp on [OK]. Then delete the target lamp in
Position Setup Dialog [Lamp History] dialog box.
Box.

The selected area Deleting the first row for D2 lamp in The first row for D2 lamp is fixed and
contains the D2 lamp. "Lamp History" table was attempted. cannot be deleted.
D2 lamp row cannot be
deleted.

This file cannot be Measurement file (*.aa) measured in Use the software that corresponds with the
loaded because different model (AA main unit) may not same (or compatible) model to read out
instrument type is be read out because of parameter the file. When reading out only the
different.***Flow Rate X mismatch. parameters, use the template file (*.taa).
isn't suitable for this The parameters are read out after
instrument. converted to match with the model.

This file cannot be Measurement file (*.aa) measured in Use the software that corresponds with the
loaded because different model (AA main unit) may not same (or compatible) model to read out
instrument type is be read out because of parameter the file. When reading out only the
different.***Slit Width X mismatch. parameters, use the template file (*.taa).
isn't suitable for this The parameters are read out after
instrument. converted to match with the model.

This file is not to be The extension of file is wrong. Load a file that has the extension indicated
loaded. Software in [Files of type] in [Open] dialog box.
doesn't support this file.

This operation cannot The attempted operation cannot be Close this message and wait until
be executed during executed when the instrument is "READY" is displayed at the right lower of
action or measurement. BUSY status or while the the status bar. Then perform the target
measurement is executed. operation again.

This operation cannot - Turn off the lamp in [Optics Parameters]


be executed while the page of the current measurement element.
hollow cathode lamp is Use [Lamp ON] check box in the case of
lit ON. Please retry it measurement lamp and [Warmup Lamp]
after you turn off the button in the case of warm-up lamp. Then,
lamp. execute the aimed operation.

Time out occurred The GFA is in waiting status for Switch on the GFA and PC again. If the
during the GFA cooling transformer and cannot error occurs again, record the status in
transformer is cooling recover. which this error occurs. Then contact your
down. Shimadzu service representative.

Timer cannot be The number of timers currently used Start up the PC again. Also, don't start
created. After closing exceeds the limit of the Windows other applications.
other applications, try it system.
again.

7-34 AA-6800/6650 Instruction


7.4 Error Messages

Error Message Cause/Details Remedial Measure

Too many schedules. When executing [File]-[Additional When the Element schedule you wish to
Failed to add all Load], the excess schedules cannot add is located in the latter part of the
schedules. be read out on the MRT worksheet if original file of adding, start up another AA
the number of Element Schedules on software and load the original file for
the MRT worksheet exceeds 20. adding and move the order of target
Element schedule. Or take out only the
element schedule and save it as different
file name to create an original file for
adding.

Unexpected file format. The extension of file is wrong. Load a file that has the extension indicated
in [Files of type] in [Open] dialog box.

Unknown Status Code: An error that is not defined in the AA Switch on the PC power and the
/(Error Code) software inside has occurred. instrument power again. If the error occurs
again, record the number indicated in the
error message and the status in which the
errors occurred. Then contact your
Shimadzu service representative.

Usage time has exceed When registering the lamp in [Lamp It is possible to input the values as "(Life
lamp life time. History] dialog box, the input values Time) < (Used Time)".
has a relation "(Life Time) < (Used If the values are not wrong, continue the
Time)". input.

Valid Injection position The injection position is set higher Set the injection position properly then
is not set. Use [Move than the destination nozzle position in [Move near to Tube] can be used.
Upward]/[Move [ASC Furnace Nozzle Position
Downward] button to Adjustment] dialog box, and as the
move the nozzle to result, [Move Near to Tube] cannot be
proper position. executed.

Wizard cannot be - Close this message and wait until


executed during "READY" is displayed at the right lower of
measurement or when the status bar. Then perform the target
the instrument is operation again.
BUSY.

X, Y, Z

AA-6800/6650 Instruction 7-35


Chapter 7 Appendix

This page is intentionally left blank.

7-36 AA-6800/6650 Instruction


Record of Revision

Date Revision Changed Page Description

7/1997 New

6/1998 A A: yellow p3, p5


2-9, 2-18, 2-20, 6-19 or later
Clerical error correction p6-20

4/1999 B It corresponds to upgrade.

7/1999 C Explanation addition for AA-6650

10/1999 D Explanation addition

5/2000 E The addition of the check procedure after reverse fire. Ver2.10 o 2.11
It corresponds to upgrade.

6/2000 F Change of an ignition switch and the ignition method. Ver2.11 o 2.20
It corresponds to upgrade.

2/2004 G A related illustration and a document are improved with Hardware change
nebulizer change. IVDD
A: Record of Revision

3/2006 H Note for WEEE Mark was added.


Yellow page p8
• Supply period of replacement parts
10 years o 7 years

7/2006 J Add notes for the following items on yellow pages:


• "Handling Waste Liquid"
• One warning label
• Two items added to "General Precautions"
2.4.1 Connecting Drain Tube
• Addition to the notes
6.5 Maintenance Parts
• Standard replacement intervals added

3/2007 K Change of the Seal Joint and Gas Leak Check method.

4/2007 L Change of the burner unit and procedure in case of


flashback.

3/2008 M Add a note for "Action in the Case of Fuel Gas Leakage" on
yellow pages.

8/2008 N "Safety Service Parts List" and "Daily Check List" added in
the yellow pages.
Flow rate changed from 8.0 to "7.0 to 8.0 L/min" for [N2O-
C2H2] on page 4-64.

Note) A ... Added Page No.


D ... Deleted Page No.
2011, 06 3500-06110-1TD (D-1194)

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