Aa-6800 Im 01
Aa-6800 Im 01
Aa-6800 Im 01
Sep. 2011
Read the instruction manual thoroughly before you use the product.
Keep this instruction manual for future reference.
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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.
Do not disassemble or modify the equipment without the express approval of an authorized 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.
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)
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.
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.
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.
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.
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.
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.
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.
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
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
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
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.
<10> Nebulizer
<12> Mixer
<6> Chamber fixing screw
<13> O-ring
<7> Drain tube
(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.
(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.
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.
(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.
(1) Do not use the flame for any purpose other than analysis.
(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.
(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.
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.
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.
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.
(*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.
(2) Nebulizer
(*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.
(*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.
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
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.
Before ignition
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.
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.
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.
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.
1 Water is drained from the air The scupper of the air compressor is certainly performed after
compressor. using instrument.
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.
xxvi
xxiv AA-6800/6650 Instruction
Contents
Precautions for Safe Operation
Emergency Action
General Precautions
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
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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
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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
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
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xxx AA-6800/6650 Instruction
Chapter 1
Overview
CONTENTS
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.
Range
Spectro-
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
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
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)
AA-6800F Specifications
Chamber Polypropylene
AA-6800G Specifications
Range
Spectro-
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
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
Baseline Correction Automatic baseline drift correction using electrical double beam
signal processing (Furnace)
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.
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)
AA-6650F Specifications
Chamber Polypropylene
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
CONTENTS
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.
AA-6800F (206-50500)
AA-6800G (206-50700) −
AA-6650F (206-51200)
AA-6650G (206-51300) −
Q'ty
Item No. Parts Name Part No.
6800 6650
2 Standard Accessories 1 1
-6 CD-ROM㧘WizAArd 1 1 206-58458-91
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>
<2-9>
<2-6>
<2-10>
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.
<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>
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.
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.
Front view
Duct
About 700
Plane view
(Unit: mm)
AA-6800/6650
• When the power voltage of AA-6800/6650 changes 5 %, absorbance changes approx. 0.005 Abs.
Air 0.35 MPa 24 L/min Free from oil, moisture and dust
WARNING
Use only gases in Table 2.4 for flame analyses.
Do not use oxygen gas.
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.
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.
Stop cock
Analysis room
Out- Drain
doors separator Air
compressor
Damper
Fan
About 700
(Unit: mm)
<4> <3>
<9>
<8>
<11>
<7>
<5> <6>
6 Drain cock
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
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.
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.)
Connecting nut
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.)
Specifications
Screen resolution SVGA (800 s 600 or higher) (1024 s 768 or higher resolution recommended)
Peripherals Monitor
Keyboard
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 side PC side
D sub 25-pin D sub 9-pin
male connector female connector
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.).
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
Drain tube
Drain container
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.
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.
Burner head
O-ring
Chamber
O-ring
Retaining plate
Nebulizer
Impact bead
AA rear side
PC RS-232C
(PC)
RS-232C
cable
SERIAL1
SERIAL2
COM1
COM2
RS-232C
etc. AC cable AC
(called by various name.) ~
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.
Black
Tube connectors
White
Red
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) 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.
Graphite furnace atomizer GFA 206-51000-93 (220 V), -34 (230 V), -35 (240 V)
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.
Graphite furnace
Burner head
Four screws
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.
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.
(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.
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.
CONTENTS
<1>
<4> <3>
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.
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.
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
Deuterium lamp
Adjusting screw
<4>
<3>
<1>
<2>
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.
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.
<1>
<2>
<3>
Height indicating position
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
3.1.5 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>
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.
5 Spray chamber The particles of sprayed sample solution are mixed with the
combustion gas in this chamber.
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.
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.
<5>
<2>
<6> <12>
<1>
<8>
<7>
<4> <3>
<10>
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
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.
Lamp power
supply
Monochromator
Deuterium lamp
Hollow cathode Analog signal processor
Burner Detector
lamp
Half mirror
CPU
Gas control PC
unit
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
<1>
1 Power switch
<2>
<1>
1 Power switch
2 Heat switch
<1>
1 Power switch
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.
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.
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.
(1) First, click on [Select Elements]. Then the [Load Parameters] page will appear.
(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.
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.
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.
(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]
(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.
4.2.1.5 Sample ID
(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.
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.
In this [Sample Selection] page, the samples to be measured for each element are selected.
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.
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.
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.
(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.
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.
(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.
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.
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.
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.
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.
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.
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.
(1) First, click on the [Select Elements] button. Then the [Load Parameters] page will appear.
(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.
(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.
First, click on the element row to highlight it, then click on [Edit]. The [Preparation Parameters] page will appear.
Set the parameters as below.
(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.
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].
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.
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.
(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".
(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.
Parameters Screens
(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.
4.2.2.5 Sample ID
(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.
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.
In this [Sample Selection] page, the samples to be measured for each element are selected.
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.
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.
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.
(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.
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.
(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.
(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.
Flow Rate
STAGE# Temp (qC) Time (sec) Heat Mode Sensitivity GAS Type
(L/min)
(1) Click on [File] in the menu bar and select [Save As].
(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.
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.
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.
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.
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.
[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.
(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.
<8>
<2>
<5>
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.
(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.
(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.
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.
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.
Symbol Meaning
Abs Absorbance
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"
(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>
(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.
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.
AUTO ZERO
BLANK
START
TEST MEAS.
RINSE
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.
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.
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.
(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.
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.
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.
(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.
(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.
(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.
[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).
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.
NOTE
Insertion and deletion of a row next to current measuring row can't be done during measurement.
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.
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.
Slot length 10 cm 5 cm
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.
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.
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) 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.
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.
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.
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
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
Dark blue
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.
(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.
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
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
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.
(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).
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
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.
[Action] C#
[Action] C#
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.
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.
(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.
Table 4.5 Analysis Line Wavelength Table for Flame Emission Analysis
Ge 265.1 Rb 794.8
*: Band spectrum
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.
(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.
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.
(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.
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.
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].
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.
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.
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.
CONTENTS
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.
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").
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].
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].
[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.
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.
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.
(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.
NOTE
Only the data on the MRT worksheet can be output to text file. Measurement parameters and waveform data
cannot be output.
<1> <2>
<3> <4>
<5>
<6>
<7> <8>
<9>
<10> <13>
<11>
<12>
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.
NOTE
To perform the text file auto export in manual measurement, set a "FILEEXPORT" row in the MRT
worksheet.
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".
NOTE
When executing a program by command line in manual measurement, set up "COMMAND" row in the MRT
worksheet.
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.
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
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].
[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.
5.2.14 [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.
Functions to be used in editing the data row on MRT worksheet are summarized.
NOTE
Insertion and deletion of a row next to the current measuring row can't be done during measurement.
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.
Clicking on [Parameters] in the menu bar during the measurement opens a 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.
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.
[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.
[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.
[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.
This check box gets active when the element measured by the cold vapor mercury technique or the hydride
vapor technique is specified.
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.
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.
[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.
[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
(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.
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)).
[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.
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].
NOTE
When using the ASC, put a check mark in the check box of [Using ASC] in [Sequence] page of [Edit
Parameters] dialog box.
[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.
[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.
[Reagent Name], [Reagent Position] and the intake order of sample and reagents can be set here for four kinds
of reagents.
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.
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.
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.
[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.
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.
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.
[Name]
Enter a common sample name here.
[Start No.]
Enter the first number of successive number.
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].
[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.
[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.
[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 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.
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.
While this dialog box is displayed, you can turn the lamp turret and change the lamp.
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.
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.
[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.
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.
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.
[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.
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.
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.
[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.
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.
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.
[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.
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.
[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.
[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].
[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.
[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.
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.
[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
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.
When [Start] is pressed, the graphite tube is baked for cleaning according to the built-in heating program. Use
[Test Measurement] together, if necessary.
[Objective Stage]
Enter the stage No. for searching the heating temperature.
[Step Width]
Enter the increment step for search to change the heating temperature.
[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.
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.
(The upper figure is for flame measurement and the lower one is for furnace measurement.)
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.
[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.
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.
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.
[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.
Furnace
[Signal Processing]
As a measured value, you can select the peak height or peak area of the obtained waveform.
[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.
RSD: RSD = σ
μ × 100 (%)
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.
[Correction Factor]
Arbitrary factor necessary for unit conversion can be set.
[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.
[Using ASC]
Put a check mark in the check box when using the ASC.
[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.
[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.
[Speed]
This sets the speed at which the sample is injected into the furnace. The default value is 25 (PL/sec).
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.
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.
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".
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.
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.
[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.
[Conc. Unit]
Unit of concentration used in MRT worksheet is set here.
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.
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.
5.8.1 [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.
After the [Initialize] screen is closed, [Instrument Check List for Flame Analysis] is displayed.
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.
[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.
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.
[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.
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].
[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.
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.
[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.
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.
[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.
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].
[Moving Rate]
This indicates pulse number for one movement. Select [Fast], [Middle] or [Slow].
[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.
[Moving Rate]
This indicates pulse number for one movement. Select [Fast], [Middle] or [Slow].
[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.
[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.
[Autozero]
This shifts the current indicated value to zero.
[Line Search]
This executes line search.
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.
[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.
• [Change Syringe]
[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.
[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.
NOTE
The warmup time of the hollow cathode lamp is set by selecting [Parameters]-[Edit Parameters]-[Sequence]
page from the menu.
[Drain Level]
Displays the status of drain tank level.
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.
CAUTION
Be sure to follow the procedure below to perform the remaining gas combustion. If the procedure is
compromised, a flashback may occur.
CAUTION
Be sure to use Air-C2H2 flame to perform the remaining gas combustion. Using N2O-C2H2 flame may cause
a flashback.
(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.
(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.
(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.
5.8.13 [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.
"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."
"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.
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.
[Current Pos.]
The current nozzle position is displayed.
[Injection Pos.]
The sample injection position currently selected is displayed.
CONTENTS
Burner head
White paper
Beam spot
Burner head
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.
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.
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.
Clogged Normal
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.
(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.
<4> Nebulizer
<4> Nebulizer
<5> Chamber
<6> Mixer
<7> Spray unit
<1> Capillary
(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.
(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.
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.
(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.
Part No 062-65063-01
Type L6382
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.
(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.
(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.
Standard
Name P/N Remarks Replacement
Interval
O ring, AS568-116-4D 036-15551-16 Used at the burner head side of the 1 year
burner socket
O ring, 4D P16 036-11217 Used with the nebulizer and chamber 1 year
plugs
O ring, 4D P35 036-11237 Used between the chamber and the 1 year
jacket
Gas tube ASSY 206-65112 Nylon tube set for gas supply 3 years
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)
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.
6.6.3 Autosampler
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
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.
Ge 265.1 Rb 794.8
*: Band spectrum
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
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)
Absorbance
Pyro-coated
Platform
High density
Cu Concentration/ ppb
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)
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)
Number
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.
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 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 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.
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 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.
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.
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.
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. 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 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".
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.
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).
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 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.
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.
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.
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.
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.
(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.
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.
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.
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 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.
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.
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.
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.
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
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.
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].
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.
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.
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 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.
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.
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.
X, Y, Z
7/1997 New
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
3/2007 K Change of the Seal Joint and Gas Leak Check method.
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.