638-94834 Toc-L CPH-CPN Um en Labsolutionstoc
638-94834 Toc-L CPH-CPN Um en Labsolutionstoc
638-94834 Toc-L CPH-CPN Um en Labsolutionstoc
Apr. 2021
TOC-LCPH/CPN
User's Manual
LabSolutions TOC Volume
Read this manual thoroughly before you use the product.
Keep this manual for future reference.
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Introduction
Read this Instruction Manual thoroughly before using
the product.
Thank you for purchasing this product. This USER'S MANUAL describes how to use this
product in addition to any accessories and options related to this product. Read this
manual thoroughly before using the product and operate the product in accordance with
the instructions in this manual.
Also, keep this manual for future reference.
IMPORTANT
• If the user or usage location changes, ensure that this Instruction Manual is always
kept together with the product.
• If this manual or a product warning label is lost or damaged, immediately contact
your Shimadzu representative to request a replacement.
• To ensure safe operation, read all Safety Instructions before using the product.
• To ensure safe operation, contact your Shimadzu representative if product
installation, adjustment, or re-installation (after the product is moved) is required.
Notice
• Information in this manual is subject to change without notice and does not represent
a commitment on the part of the vendor.
• Any errors or omissions which may have occurred in this manual despite the utmost
care taken in its production will be corrected as soon as possible, although not
necessarily immediately after detection.
• All rights are reserved, including those to reproduce this manual or parts thereof in
any form without permission in writing from Shimadzu Corporation.
• Microsoft and Windows are registered trademarks of Microsoft Corporation in the
United States and/or other countries.
Microsoft®, Windows® XP Operating System is expressed as Windows XP.
Microsoft® Windows 7® Operating System is expressed as Windows 7.
Microsoft® and Windows® are either registered trademarks or trademarks of Microsoft
Corporation in the United States and/or other countries.
• PARAFILM is a registered trademark of American National Can.
• Other company names and product names mentioned in this manual are trademarks or
registered trademarks of their respective companies.
The TM and ® symbols are omitted in this manual.
Convention Description
Indicates a potentially hazardous situation which, if not
avoided, may result in minor to moderate injury or equipment
damage.
Emphasizes additional information that is provided to ensure
the proper use of this product.
Supplementary Conventions
The following symbols are used in this manual:
Convention Description
Safety Instructions
To ensure safe product operation, read these important safety instructions carefully
before use and follow all CAUTION instructions given in this section.
n Product Applications
n Installation Site
n Installation
When lifting the instrument, lift from the bottom and at both sides of the
instrument.
Do not lift it by the front access door, as this may cause instrument damage.
n Operation
The contents of the hard disk of the personal computer may be lost as the
result of an unforeseen accident.
Always create a backup to protect critical data from such accidents.
n In an Emergency
In an emergency, turn OFF the main power switch on the left side towards the top of
the TOC-L. Also, turn OFF the power switch on the left side of the ASI-L.
Also, when the product is used again, inspect the product and, if necessary, contact your
Shimadzu representative to request servicing.
2 Turn OFF the main power switch on the left side towards the top of the TOC-L.
Also, turn OFF the power switch on the left side of the ASI-L.
1 Turn OFF the main power switch on the left side towards the top of the TOC-L.
If the main power switch is not turned OFF, the instrument automatically restarts
when power is restored. The power switch on the ASI-L does not need to be
turned OFF.
2 After power is restored, turn ON the main power switch on the left side towards
the top of the TOC-L. Confirm that the instrument operates properly before use.
In order to ensure safety, warning labels are attached in places requiring caution.
If a warning label is lost or damaged, obtain a new label through your Shimadzu
representative and attach it in the correct position. A residual risk indicates a risk that
could not be reduced or eliminated in the process of design and manufacture. Be sure
to thoroughly read and understand the contents in "Description" before using the
product.
Warranty
Shimadzu provides the following warranty for this product.
1. Period:
Please contact your Shimadzu representative for information about the period of this warranty.
2. Description:
If a product/part failure occurs for reasons attributable to Shimadzu during the warranty period,
Shimadzu will repair or replace the product/part free of charge. However, in the case of products
which are usually available on the market only for a short time, such as personal computers and
their peripherals/parts, Shimadzu may not be able to provide identical replacement products.
3. Limitation of Liability:
(1) In no event will Shimadzu be liable for any lost revenue, profit or data, or for special, indirect,
consequential, incidental or punitive damages, however caused regardless of the theory of
liability, arising out of or related to the use of or inability to use the product, even if Shimadzu
has been advised of the possibility of such damage.
(2) In no event will Shimadzu's liability to you, whether in contract, tort (including negligence), or
otherwise, exceed the amount you paid for the product.
4. Exceptions:
Failures caused by the following are excluded from the warranty, even if they occur during the
warranty period.
(2) Repairs or modifications performed by parties other than Shimadzu or Shimadzu designated
companies
(3) Product use in combination with hardware or software other than that designated by Shimadzu
(4) Computer viruses leading to device failures and damage to data and software, including the
product's basic software
(5) Power failures, including power outages and sudden voltage drops, leading to device failures
and damage to data and software, including the product's basic software
(6) Turning OFF the product without following the proper shutdown procedure leading to device
failures and damage to data and software, including the product's basic software
(8) Product use in harsh environments, such as those subject to high temperatures or humidity levels,
corrosive gases, or strong vibrations
(9) Fires, earthquakes, or any other act of nature, contamination by radioactive or hazardous
substances, or any other force majeure event, including wars, riots, and crimes
* If there is a document such as a warranty provided with the product, or there is a separate contract
agreed upon that includes warranty conditions, the provisions of those documents shall apply.
If any problem occurs with this product, perform an inspection and take appropriate
corrective action as described in this manual's troubleshooting section. If the problem
persists, or the symptoms are not covered in the troubleshooting section, contact your
Shimadzu representative.
Replacement parts for this product will be available for a period of seven (7) years after
the product is discontinued. Thereafter, such parts may cease to be available.
If Shimadzu receives notice of the discontinuation of units or parts, the necessary quantity
for the above period is immediately calculated and secured. However, such units or parts
may cease to be available within seven years after the discontinuation of the product,
depending on the conditions of individual manufacturers and on changes in the quantity
required.
Disposal Precautions
• Dispose of this instrument according to local regulations for the relevant area and
request processing by an industrial waste disposal company. Gather and seal insulation
material waste into plastic bags and request disposal by an industrial waste disposal
company licensed to process glass, concrete, and ceramic waste.
• All used catalyst should be sent to a licensed industrial waste disposal company.
• All used CO2 absorbers should be sent to a licensed industrial waste disposal company.
• All used halogen scrubbers should be sent to a licensed industrial waste disposal
company.
• All used catalyst from the ozone treatment unit should be sent to a licensed industrial
waste disposal company.
• The optional measurement circuit for purgeable organic carbon (POC) uses a CO2
absorber filled with lithium hydroxide to remove carbon dioxide. All used lithium
hydroxide crystals should be sent to a licensed industrial waste disposal company.
• Wear protective glasses and gloves when handling quartz wool.
Inhaling it may cause health impairment.
Electromagnetic Compatibility
This instrument complies with European standard EN50011 class A for electromagnetic
emission and EN61326-1 for electromagnetic immunity.
Compliance to the standard does not ensure that the instrument can work with
any level of Electromagnetic interference stronger than the level tested.
Interference greater than the value specified in the condition above may cause
malfunction of the instrument.
(1) Before touching the instrument, discharge the electro static charged in operator's
body to ground touching metallic structure connected to ground.
(2) Do not install this instrument in such environment where strong electromagnetic
fields are generated near by.
1 Overview
This chapter provides an overview of the instrument and operational precautions for its
use.
2 System Description
This chapter briefly describes the TOC-L system components, their names and optional
accessories.
4 Analysis Procedure
This describes the measurement operations using the software in direct sequential order.
5 Software Operations
This chapter describes the in-depth software operations used for creating files, conducting
measurement and printing reports.
7 Maintenance
This chapter describes maintenance procedures and periodic checks required to ensure
that the instrument provides consistently high accuracy analyses. Troubleshooting
procedures and error messages are also included in this chapter.
8 Reference Information
This chapter describes principles of analysis and lists specifications, standard and optional
accessories, and specialized terms associated with this instrument. This chapter also
includes the installation procedure, for use in the event that instrument is moved to
another site.
Preparation for 19
3 Measurement
3.1 Instrument and Sample Preparation ....................
5.8.4 Setting the Display Font of the Output Window .......... 289
7.2.5 Replacing the High Purity Air (Filling the Cylinder) ........ 327
7.3.3 Replacing the Pump Head of the Rinse Pump ............. 342
Reference 381
8 Information
8.1 Principles of Analysis ........................................
8.3.7 Manual Injection Kit (Gas Sample Injection Kit) ........... 398
8.3.8 B-Type Halogen Scrubber ................................... 399
1.1 Overview
Moreover, when the ASI-L Autosampler or OCT-L 8-Port Sampler is used in combination with
the main unit, a fully automatic system is created, allowing automatic analysis of multiple
samples.
This instrument is a qualified product in Shimadzu's ecolabel program.
The power consumption of this instrument has been reduced by 36 %
for a supply voltage of 100 V and 43 % for a supply voltage of 200 V
compared to previous TOC-V models. (Usage conditions: (8 hours of
operation per day) ´ (5 hours of operation per week))
*1 JIS K-0102 "Industrial Waste Water Testing", JIS K-0551: "Total organic carbon (TOC) testing methods
for ultra-pure water", U.S. Pharmacopoeia, EPA 415.1, EPA 9060A, ASTM D7573-09, Standard
Methods for Examination of Water and Waste Water 5310B
• Hand tighten the various connectors to the 8-port valve. Use of a tool may
cause deformation and leakage in the valve. <Part damage prevention>
1
• Stop operation of the instrument when performing maintenance on any of
the drive components, such as connecting lines to the 8-port valve, or
connecting/disconnecting lines on the sample injector. If these parts are
manipulated or if the lines are disconnected during operation, the drive
component could move and cause injury or discharge of liquid. <Injury
prevention, corrosion prevention>
• Specify the Shut down instrument option in the Shutdown window to shut
down the instrument. The electric furnace turns OFF and the power supply
shuts off after 30 minutes except for a minimum amount of power
necessary to keep the software running. This shutdown process extends the
life of the TC injection port parts by preventing unnecessary wear. This
procedure does not apply to emergency shutdown. <Maintaining durability
of TC injection port parts>
• The lever of the 3-way valve at the bottom of the IC reaction vessel should
normally be turned to the left position. Refer to "Figure 1.2 Lever Position
of 3-Way Valve on the IC Reaction Vessel". The lever should never be
turned to the lower position. The lower position allows carrier gas to flow
at a pressure of 200kPa upstream from the 3-way valve, causing possible
disconnection of joints and damage to parts such as the combustion tube.
• Always verify that the ozone air source is supplying air at a rate of
0.5 L/min when using the TNM-L. This helps to prevent ozone leaks and
line corrosion. <Ozone leak prevention, line corrosion prevention>
• If an ozone odor is detected while using the TNM-L, immediately stop the
current measurement (without turning off the gas supply) and contact your
Shimadzu representative to request maintenance. Ozone can cause
respiratory organ injury and equipment damage. <Prevention of respiratory
organ injury and equipment damage>
• Do not write on the periphery of the vial rack or stick adhesive tape onto
the vial rack. If aluminum foil or water droplets are adhered to the periphery
of the vial rack, remove them. These may prevent the vial rack from rotating
1
correctly.
• At the start of measurement, the ASI-L rotates the vial rack by one revolution
to detect its home position and performs initialization. In order to perform
measurement correctly, the ASI-L may also detect shift in the vial rack
position during measurement and perform correction by rotating the vial rack
by one revolution. This does not mean that an abnormality has occurred.
Figure 2.15 Flow Diagram (TOC-LCPN + TNM-L + Carrier Gas Purification Kit)
When filling the combustion tube, verify that the catalyst does not become
contaminated. Contamination will cause high blank values and abnormal analysis
values.
Either standard or high sensitivity catalyst can be used for TOC analysis. The furnace
temperature is set to 680 °C for TOC analysis.
2 Layer about 5 mm of quartz wool onto the platinum mesh using the catalyst
filling rod.
Take care not to inhale any quartz wool when filling the combustion tube.
Inhaling quartz wool may cause health impairment. Handle with care. For
details, see "8.9 Safety Data Sheets (SDS)" P.433.
2 Fit together the combustion tube opening and the opened end of the cylindrical
catalyst container.
3 Use the catalyst filling rod to push catalyst into the combustion tube from the
other opened end of the cylindrical catalyst container.
A TC high sensitivity catalyst kit, including a combustion tube filled with TOC high
sensitivity catalyst in advance, is also available.
Figure 3.2 Filling of TOC Combustion Tube with High Sensitivity Catalyst
Wear protective glasses and gloves when handling high sensitivity catalyst.
Inhaling it may cause health impairment.
TOC/TN catalyst is used for TN analysis and TOC/TN simultaneous analysis. The detection
rate is low for the IC component when it exceeds 10 mg/L; as a result, TOC in samples
containing more than 10 mg/L IC cannot be measured using the TC-IC method and should
be measured using the NPOC method. The furnace temperature is set to 720 °C for
TOC/TN and TN analysis.
2 Layer about 5 mm of quartz wool onto the platinum mesh using the catalyst
filling rod.
3
3 Introduce the TOC standard catalyst into the combustion tube to a height of
140 mm from the top end of combustion tube.
5 Lightly press down on the ceramic fiber using the catalyst filling rod to attain a
thickness of 10 mm.
• The thickness of the ceramic fiber must be uniform, covering the entire surface
of the catalyst, or a poor TN detection rate may result.
• The filling heights of the catalyst and ceramic fiber influence the TN detection
rate, so it is important that the dimensions are close to those indicated below.
Catalyst: 140 mm from the top end of combustion tube
Ceramic fiber: 10 mm
Figure 3.3 Filling Combustion Tube with Catalyst for TOC/TN Analysis
Take care not to inhale any quartz wool or ceramic fiber when filling the
combustion tube.
Inhaling quartz wool may cause health impairment. Handle with care. For
details, see Section "8.9 Safety Data Sheets (SDS)" P.433.
Install the cooling tube unit to the outlet of the combustion tube.
• The cooling tube unit is made of hard glass. Handle the unit with care to
prevent breakage.
• Tighten the hexagon cap nut while holding the PTFE coupling in place with
your finger when connecting the outlet tube to the cooling tube. The cooling
tube with break if the hexagon nut is tightened without holding the PTFE
coupling in place.
3
1 Open the front door on the instrument and connect the PTFE tube attached to
the pure water trap to the outlet of the cooling tube unit (the smaller PTFE
coupling). At this point, carefully tighten the hexagon cap nut while holding the
PTFE coupling in place with your finger.
2 Loosen and remove the two fastening screws on the cooling tube unit located
on the lower section of the electric furnace and insert the screws into each of
the two holes on the upper section of the cooling tube unit and tighten them.
The installation procedure for the combustion tube differs for the H Type and N Type
instruments.
• Allow the electric furnace to cool to room temperature for at least six hours
after switching off the power supply by shutting down the instrument before
performing maintenance on the combustion tube or catalyst. Burns may result
if this task is attempted when the furnace is at a high temperature.
• Combustion tubes are made of quartz glass. Always wear protective leather
gloves when handling combustion tubes to prevent injuries due to breakage.
• When connecting the combustion tube, handle it carefully to avoid breakage.
The combustion tube is constructed of quartz glass, and injury is possible.
• Do not use a wrench or other tool. Injury could result if the combustion tube
breaks.
1 Open the door on top of the instrument, remove the slider retaining screws
(knurled screws) from the sample injector, and pull the slider towards you and
out of the sample injector.
2 Loosen the hexagon cap nut that joins the carrier gas introduction tubing (PTFE
tubing) to the right side of the sample injector and then remove the tubing.
3 Loosen the two knurled screws on the sample injector and remove the sample
injector in the upward direction.
4 Securely insert the top end of the combustion tube filled with catalyst into the
hole on the bottom of the sample injector.
5 Fit the combustion tube into the hole in the center of the electric furnace and
then insert the bottom end of the combustion tube into the PTFE coupling of
the cooling tubing inlet. At this point, securely connect the drain tubing, which
protrudes out of the sample injector, to the Y-shaped fitting.
6 Secure the sample injector to the instrument body using the knurled screws.
7 Reattach the slider and carrier gas introduction tubing to their original positions.
Do not allow organic substances, such as grease or oil, to contaminate any parts
exposed to gas including the inner surfaces on the tip of the combustion tube
as well as joints. This is especially important for high sensitivity measurement.
8 Connect the bottom of the combustion tube to the PTFE coupling of the cooling
tubing inlet. Carefully tighten the hexagon cap nut while holding the PTFE
coupling in place with your finger.
Figure 3.9 Connecting the Bottom End of the Combustion Tube to the PTFE Coupling
The quartz glass combustion tube will break if the hexagon cap nut is
overtightened.
Tightening the PTFE coupling without holding it in place will break the cooling
tubing because it is made of hard glass.
9 When using catalyst for TOC measurement and TOC/TN catalyst, use the provided
quartz wool (0.6 g and more) to fill the gap between the bottom of the electric
furnace and the combustion tube as well as the two notches in the insulator on
top of the electric furnace.
• When using TOC high sensitivity catalyst, do not fill the gap at the bottom
of the electric furnace with quartz wool.
• Take care not to inhale any quartz wool when filling the gap and the
notches.
• Inhaling quartz wool may cause health impairment. Handle with care. For
details, see "8.9 Safety Data Sheets (SDS)" P.433.
Figure 3.10 Filling With Quartz Wool (Bottom of the Electric Furnace)
Figure 3.11 Filling With Quartz Wool (Top of the Electric Furnace)
1 Open the door on top of the instrument, remove the slider retaining screws
(knurled screws) from the sample injector, and pull the slider towards you and
out of the sample injector.
2 Loosen the hexagon cap nut that joins the carrier gas introduction tubing (PTFE
tubing) to the right side of the sample injector and then remove the tubing.
3 Loosen the two knurled screws on the sample injector and remove the sample
injector in the upward direction.
4 Securely insert the top end of the combustion tube filled with catalyst into the
hole on the bottom of the sample injector.
5 Fit the combustion tube into the hole in the center of the electric furnace and
then insert the bottom end of the combustion tube into the PTFE coupling of
the cooling tubing inlet. At this point, securely connect the drain tubing, which
protrudes out of the sample injector, to the Y-shaped fitting.
6 Secure the sample injector to the instrument body using the knurled screws.
7 Reattach the slider and carrier gas introduction tubing to their original positions.
Do not allow organic substances, such as grease or oil, to contaminate any parts
exposed to gas including the inner surfaces on the tip of the combustion tube
as well as joints. This is especially important for high sensitivity measurement.
The quartz glass combustion tube will break if the compression fitting is
over-tightened.
8 Connect the bottom of the combustion tube to the PTFE coupling of the cooling
tubing inlet. Carefully tighten the hexagon cap nut while holding the PTFE
coupling in place with your finger.
9 In order to prevent heat from escaping from the furnace, use the provided quartz
wool (0.6 g and more) to fill the gap between the bottom of the electric furnace
and the combustion tube as well as the two notches in the insulator on top of
the electric furnace.
• When using TOC high sensitivity catalyst, do not fill the gap at the bottom
of the electric furnace with quartz wool.
• Take care not to inhale any quartz wool when filling the combustion tube.
• Inhaling quartz wool may cause health impairment. Handle with care. For
details, see "8.9 Safety Data Sheets (SDS)" P.433.
Figure 3.16 Filling With Quartz Wool (Bottom of the Electric Furnace)
Figure 3.17 Filling With Quartz Wool (Top of the Electric Furnace)
Refractory ceramic fibers (RCF) are fire-resistant inorganic fibers mainly consisting of
alumina (Al2O3) and silica (SiO2). This material is chemically stable and can be used as
insulation material in a high temperature range exceeding 1000 °C.
With this instrument, the dispersibility of fibrous mineral under normal conditions of use 3
is measured and is proven to be sufficiently low with respect to the maximum permissible
dust concentration level.
Connection Procedure
1 Remove the film at both ends of the new halogen scrubber and connect it to
the Viton connectors.
The baseline may fluctuate immediately after connection. Allow the instrument to run
for a short time until the baseline stabilizes. Stabilization normally occurs within one
hour.
This section describes how to install the syringe into the instrument.
Each port of the 8-port valve for the syringe pump type sample injector is connected to
certain streams depending on the state of the instrument. Installing and removing the
syringe without following the correct procedure may cause acid and other substances to
be discharged from the syringe connection port. Always follow the procedure described
below.
• If the syringe is installed using a procedure other than that described below,
there is a danger that acid, or other solutions may leak from the syringe
connection port. Ensure that the syringe is installed according to the
procedure below.
3
• To avoid injury, keep hands away from the sample injector during operation
of the syringe pump sample injector.
• The syringe barrel is made of glass, handle it carefully to avoid breakage.
n Syringe Installation
Installation Procedure
2 Right-click on the appropriate instrument icon in the Sample Table tab of the
file viewer, and click Connect.
Connection is established with the Sample Table Editor, and the Ready indicator
illuminates.
Syringe replacement preparation operation begins. The progress bar blinks while the
syringe moves into the replacement position.
5 Attach the syringe to the syringe connection port (downward facing port) of the
8-port valve and then connect the sparge gas line.
At this point, the plunger retaining screw is not completely tightened. Tighten the
retaining screw so that the plunger can still be slightly moved forwards and backwards
as well as left and right.
7 Once the syringe reaches the top position, hold the plunger vertical and tighten
the plunger retaining screw to secure it to the plunger holder.
8 Click Finish Replacement. The syringe pump zero point detection operation is
executed automatically.
9 Click Close.
The drain vessel must be filled with water to prevent carrier gas from being released
from the drain tubing.
Procedure
1 Remove the cooler drain vessel from the mounting clip and then remove the
rubber cap from the vessel.
2 Using a wash bottle, pour pure water (deionized water is acceptable) into the
cooler drain vessel up to the level of the drain discharge tubing on the side of
the drain vessel.
3
3 Reattach the rubber cap onto the cooler drain vessel and return the vessel to its
position in the mounting clip.
4 Verify that the cooler drain tubing is inserted straightly in the drain vessel
without being bent.
Procedure
1 Remove the cap from the water supply port at the top of the humidifier.
2 Introduce water through the water supply port to the "Hi" marking on the side
of the humidifier.
Use pure water that contains as little TC as possible when performing high
sensitivity measurement.
This section describes how to prepare the dilution water required to automatically dilute
the sample inside the instrument.
Filling Procedure
1 Wash the provided dilution water bottle (2 L capacity) with laboratory detergent,
rinse well with tap water and then a number of times with pure water.
2 Fill the dilution water bottle with pure water and place it to the left of the
instrument.
3
3 Pass the dilution water intake tubing, labeled DILUTION, through the hole in the
cap.
4 Attach a wiring band about 250 mm from the end of the dilution water intake
tubing to prevent the tubing from separating from the cap.
Verify that the tip of the intake tubing nearly reaches the bottom of the
container.
This section describes the preparation of acid used for IC removal in NPOC measurement
and IC measurement with the N Type instrument.
Although the concentration of hydrochloric acid is normally 1 mol/L as described below,
adjust the concentration according to the properties of the sample.
Preparation Procedure
2 Pour the prepared acid into the 250 mL acid container provided standard with
the instrument, and secure the acid container in the mounting clip on the left
side of the instrument.
3 Pass the acid intake tubing through the hole in the cap.
4 Secure the tubing, using a wire clamp about 100 mm from the end of the tubing,
to prevent the tubing and cap from separating.
Verify that the tip of the acid intake tubing nearly reaches the bottom of the
container.
A CO2 absorber is required to remove CO2 from carrier gas because carrier gas is used
to purge the optical system of the detector. Install the CO2 absorber by following the
procedure described below.
Procedure
1 Cut the tips of the 2 rigid tubes in the lid of the CO2 absorber with a knife.
2 Connect the flexible tubing that exits the rear panel of the instrument (near the
top) as follows:
Tubing labeled "L": Connect to tube labeled "L" on CO2 absorber.
Tubing labeled "S": Connect to tube labeled "S" on CO2 absorber.
3 Place the CO2 absorber in the holder on the upper rear of the instrument.
The gas flow rate must be adjusted before conducting sparging during measurement.
Adjustment Procedure
3 The Sample Table Editor connects to the instrument. Right-click the relevant
system configuration on the Sample Table tab in the file viewer and then click
Maintenance – Mechanical Check.
5 This opens the sparge gas solenoid valve. Open the front door of the instrument
and adjust the flow rate using the sparge gas flow rate adjustment knob.
Adjust the flow rate to suit the size and shape of the sample container. A flow
rate of about 100 mL/min is appropriate.
7 Click Close for Ext. Sparge and then click OK to close the window.
To analyze samples containing suspended solids, the sample flow line diameter can be
increased from 0.5 mm to 0.8 mm by installing the optional Suspended Solids Kit.
This section describes the installation of the Suspended Solids Kit.
There are two kits available:
(1) For TOC-L (TOC-L main unit only)
(2) For TOC-L + ASI-L (used with TOC-L and ASI-L)
Switch OFF the TOC-L before attempting to install the Suspended Solids Kit.
Procedure
1 Remove the bushing from port 7 of the 8-port syringe pump valve, and
disconnect the TC injection tubing. For the H-type, remove the bushing from port
5, and disconnect the IC injection tubing.
2 Remove the slider mounting screws from the TC and IC injection blocks, and
detach the sliders.
3 Remove the slider bushings and replace the sample injection tubing with the
0.8 mm diameter sample injection tubing provided in the kit.
5 Connect the TC injection tubing and the IC injection tubing to port 7 and port
5, respectively.
During analysis, verify that the sample flow is normal. Refer to "Corrective
Actions for Poor Reproducibility" P.377.
If the sample stream is not normal, the tip of the PTFE tubing may be deformed
or scratched. Use a knife to cut off a portion of the tube.
1 Remove the bushing from port 1 of the 8-port syringe pump valve and replace
the sample tubing with the 0.8 mm diameter tubing provided in the kit.
2 Connect the new sample tubing to the 8-port valve in the original position.
(1) Before measurement, use a homogenizer, etc. to make the sample as uniform as
possible. After homogenizing the sample, depending on the type of suspended
substance, precipitation and coagulation may occur after a period of time. Prior to
measurement, mix the sample again using a magnetic stirrer to ensure that
precipitated/coagulated material is well dispersed throughout the sample.
(2) If the suspended material is present in large quantities, clumping of the material and
obstruction may occur inside the sample flow line even if the particles are of smaller
diameter that the sample flow line diameter. Take measures such as sample dilution
to prevent flow line obstruction,
(3) The suspended solids measurement kit employs a 0.8 mm PTFE tubing for sample
injection. Diminished reproducibility may occur with small sample injection volumes.
Make injection volumes as large as possible.
(4) When conducting IC measurement of suspended solid samples using the H type
instrument, obstruction of the IC measurement flow line drain tube may occur.
Sufficiently pulverize the suspended particles to allow free flow through the drain tube.
3.1.13 Preparing the High Suspension Kit (When Using the Optional High Suspension Kit)
To analyze samples that contain a high concentration of suspended solids, analysis can
be performed with greater accuracy by using the optional High Suspension Kit for High
Concentrations or High Suspension Kit for Low Concentration. Analysis with the High
Suspension Kit for High Concentrations uses 80 µL capacity tubing for the TC sample
injector tubing and IC sample injector tubing, and the injection volume is set to 80 µL.
Meanwhile, analysis with the High Suspension Kit for Low Concentrations uses 150 µL
capacity tubing for the TC sample injector tubing and IC sample injector tubing, and the
injection volume is set to 150 µL.
This section describes the installation procedure for each type of the High Suspension Kits.
3
Always switch OFF power to the TOC-L before attempting to install the High
Suspension Kit for High Concentrations.
Procedure
1 For the H-type, remove the slider mounting screws from the TC and IC injection
blocks and detach the sliders. For the N-type, remove the slider mounting screws
from the TC injection block and detach the slider.
2 Remove the slider bushings and replace the connected sample injection tubing
with the provided tubing.
During analysis, verify that the sample flow is normal. If the sample flow is not
normal, refer to "Corrective Actions for Poor Reproducibility" P.377 and take
the described measures.
(1) Before analysis, use a homogenizer to make the suspended solids in the sample as
uniform as possible. After homogenizing the suspended solids in the sample,
precipitation and coagulation may occur after a period of time depending on the type
of suspended substance. Agitate the sample again prior to analysis and use a magnetic
stirrer during analysis to prevent precipitation and coagulation of the suspended
substance.
(2) If the suspended substance is present in high quantities, clumping of the substance
and blockage may occur inside the sample flow line even when particles are smaller
in diameter than the diameter of the sample flow line. Take measures, such as diluting
the sample, to prevent the suspended substance from causing blockages in the flow
line.
(3) The High Suspension Kit improves accuracy in the analysis of samples that contain
suspended solids when performing TC and TN analyses, H-type IC analysis, and NPOC
analysis using the external sparge kit. Accuracy is unaffected for N-type IC analysis and
POC analysis in this mode. While an increase in accuracy can be expected by performing
NPOC analysis using the optional external sparge kit, accuracy is unaffected when
sparge processing is performed within the syringe.
(4) When analyzing samples that contain high quantities of suspended solids, these solids
may remain in the tubing or syringe and cause contamination by mixing with a
subsequent analysis sample of low concentration. To prevent such contamination,
repeatedly perform purified water analysis after analyzing a sample that contains
suspended solids and verify that contamination will not occur.
The following measures can be taken when the effect of contamination is significant.
• Syringe flushing
Suspended solids may collect on the plunger tip of the syringe and adhere to the
syringe interior. Remove the syringe and flush the plunger tip and syringe interior.
The procedure for flushing the syringe is described in "7.2.8 Syringe Replacement"
P.329.
• Needle flushing
If suspended solids are adhered to the surface and tip of the sampling needle of
the autosampler, remove and flush the needle.
The procedure for removing the needle is described in "8.8.4 Installing the ASI-L"
P.419.
• Tube flushing
If suspended solids are adhered to the water sampling tube, remove and flush the
tube.
Certain preparations are necessary for the H Type instrument. These include installing
and replenishing the IC reagent in the IC reaction vessel. This section describes the
procedures for installing and replenishing the IC reagent.
The IC reagent contains corrosive phosphoric acid. Always handle acid with
care to prevent spills and contact with the skin.
For details, refer to "8.9 Safety Data Sheets (SDS)" P.433.
2 Pour the prepared IC reagent into the 250 mL container provided standard with
the instrument, and secure the container in the mounting clip on the left side
of the instrument.
3 Pass the tip of the IC reagent tubing through the hole in the cap.
4 Secure the tubing, using a wire clamp at a point about 100 mm from the end
of the tubing tip, to prevent the tubing and cap from separating.
Procedure
1 Verify that the lever of the 3-way valve at the bottom of the IC reaction vessel
is positioned to the left as shown in "Figure 3.27 Lever Position of IC Reaction
Vessel 3-Way Valve".
3 Right-click on the appropriate instrument icon in the Sample Table tab of the
file viewer, and click Connect.
Connection is established with the Sample Table Editor, and the Ready indicator
illuminates.
5 Click Start.
IC reagent is pumped to the IC reagent bottle by the IC reagent delivery pump. The
progress bar at the center of the window blinks during this process.
6 Repeat step 5 until the IC reagent level reaches the lower branch of the IC
reagent drain tube.
7 Click Close.
3.1.15 Preparation for POC Analysis (When Using the Optional POC Kit)
POC analysis can be performed if the optional POC analysis kit is installed on the
instrument. This section describes preparations required for POC analysis.
5 Attach the O-ring and nipple to the top of the container, and firmly tighten the
cap.
6 Install the CO2 absorber for POC analysis in the original position.
Wear protective glasses, gloves, and mask when handling anhydrous lithium
hydroxide.
3
Anhydrous lithium hydroxide is a corrosive (strongly alkaline) powder.
Direct contact or inhaling it causes injury.
Inhaling lithium hydroxide may cause health impairment. Handle with care.
or details, check the contents of the safety data sheet (SDS) available from the
lithium hydroxide manufacturer.
Inhaling quartz wool may cause health impairment. Handle with care.
For details, see "8.9 Safety Data Sheets (SDS)" P.433.
TN analysis can be performed if the optional TNM-L is installed on the instrument. The
NOx absorber also must be connected to perform TN analysis. The CO2 absorber (soda
lime) is used as the NOx absorber. Connect it to the instrument using the following
procedure.
Procedure
1 Cut the tips of the rigid tubes (2) in the lid of the CO2 absorber with a knife.
• Tubing labeled "S": Connect to tube labeled "S" on the CO2 absorber.
3 Once connected, place the NOx absorber at the back right of the instrument.
3.1.17 B-Type Halogen Scrubber (When Using the Optional B-Type Halogen Scrubber)
The optional B-type halogen scrubber can help protect the NDIR cell from corrosion when
analyzing samples that contain a high amount of salt (concentration up to about 3 %).
The B-type halogen scrubber connects to the IC reaction vessel outlet (downstream of
the carrier gas flow) on the H Type instrument and to the pure water trap outlet
(downstream of the carrier gas flow) on the N Type instrument.
Follow the procedure described below to introduce the stainless mesh for absorption and
dilute hydrochloric acid into the B-type halogen scrubber.
The B-type halogen scrubber is filled with 0.05 mol/L hydrochloric acid. The liquid level
of hydrochloric acid gradually decreases when the instrument is waiting for analysis to
start (and the carrier gas is flowing), the sample injection volume is small, or the interval
between analyses is large during analysis. Always verify that the liquid level is up to the
height of the branching tube in the vessel of the B-type halogen scrubber before starting 3
analysis. If the liquid level is lower than the branching tube, fill the vessel to the correct
height with 0.05 mol/L hydrochloric acid (this is important when performing continuous
analysis over an extended period of time using the autosampler).
The ability to absorb halogen stops if the amount of liquid in the B-type halogen
scrubber decreases enough to prevent the carrier gas from bubbling or if the
stainless mesh for absorption dissolves completely. Before starting analysis, always
verify that the liquid level is up to the height of the branching tube in the
vessel of the B-type halogen scrubber and the scrubber contains stainless mesh
for absorption.
Preparation Procedure
1 Prepare 0.05 mol/L hydrochloric acid by either diluting 1 mol/L hydrochloric acid
with 20 parts pure water or diluting concentrated hydrochloric acid (12 mol/L)
with 240 parts pure water.
A concentration accuracy of approximately ±2 % is acceptable. As a guide, the TOC value
of the pure water used for dilution should be less than 0.5 mg/L.
2 Release the clamps that secure the B-type halogen scrubber in place, remove the
B-type halogen scrubber from the instrument, and open the screw cap.
3 Insert a stainless mesh for absorption into the B-type halogen scrubber and then
fill the vessel with 0.05 mol/L hydrochloric acid up to the height of the branching
tube.
4 Close the screw cap and return the B-type halogen scrubber to its original
position in the instrument.
Zero water refers to a standard solution with zero concentration of TC, IC, and TN, or
the water used to prepare these standard solutions of various concentrations. Although
zero water is absolutely free of carbon (TC) and nitrogen (TN) in theory, in practice, this
type of water is difficult to attain. Even ultra-pure water attained using a high
performance membrane technique or water that has been repeatedly distilled will have
a TC content of about 10 µg/L, which will increase as the water moved and stored in a
container. Carbon dioxide is present in the atmosphere at concentrations ranging from
300 to 500 mg/L. The carbon dioxide content of ambient air is even higher in a room
with many people or where combustion equipment is used. Carbon dioxide in ambient
air dissolves in water, taking the form of IC. The dissolved amount is generally about
0.2 mg/L, but depends on the water temperature and carbon dioxide content of the air
in contact with the water (refer to "Table 8.2 CO2 Content (ppm) in Distilled Water
Equilibrated with Atmosphere Temperature (°C)").
Not all water distillation and purification instruments incorporate mechanisms that
prevent contact with air during water uptake, retention, or storage processes. For this
reason, IC is present in most types of distilled and purified water. In some cases, the TC
content of commercially available distilled water stored in plastic or glass containers is
near 1 mg/L.
The degree of purity required for zero water varies depending on the
measurement range. For example, commercially available purified water is
acceptable when measuring samples with TC concentrations of a few hundred
mg/L. The quality of the zero water should be considered along with the
measurement range.
4 Accurately dilute this standard stock solution with zero water to prepare
standard solutions at the required concentrations.
Preparation of POC Standard Solution (using the optional POC analysis kit)
IC standard solution is used as the POC standard solution with this instrument for the
following reasons.
• In POC analysis, the measured substance is an organic material that is volatile and
poorly soluble in water (for example, benzene or chloroform). Preparing a standard
solution at an appropriate concentration using these types of organic substances is
difficult.
• Volatile and poorly soluble organic substances tend to undergo changes in
concentration during storage or handling after preparation.
• Standard solutions that are produced using volatile and poorly soluble organic
substances are difficult to use.
Consequently, the IC standard solution is used for this instrument. The preparation
method is listed above.
Storage Time
The limitation on storage of standard solutions is about 2 months for 1000 mgC/L
standard stock solutions and about 1 week for diluted standard solutions (for example,
100 mgC/L). The limitations are for cold storage in sealed containers.
High sensitivity analysis refers to use of the high sensitivity analysis kit to measure trace
amounts (commonly 0.5 mg/L or less) of TOC in samples such as ultra-pure water. The
precautions described in the sections below should be followed when conducting trace
analysis on the order of 10 - 100 µg/L.
Instrument Preparation
The blank peaks present at the start of high sensitivity analysis will become progressively
smaller and gradually stabilize. As a result, calibration curves generated too soon after
the start of analysis may be inaccurate because they contain data collected during
unstable conditions. For this reason, perform NPOC analysis at least five times on pure
water using the same measurement parameters (injection volume, sparge time) to be
used for analyzing the sample prior to analyzing the standard solution, and verify that
the peaks have stabilized.
Sample Analysis
Use the calibration curve generated in the previous section to measure NPOC in the
sample. Measure the sample using the same method used for the calibration standards.
If the values gradually decrease with each repeated analysis using the optional external
sparge kit, extend the sparge time to ensure sufficient sparging. The shape of the sample
container, the sample amount, the amount of sparge gas and the IC content of the
sample all have a bearing on the required sparge time. Determine the appropriate sparge
time in accordance with these parameters.
A TOC system invariably contains substances in the instrument flow lines that produce
peaks. These peaks are referred to as blank values or system blank values, and are present
even in water samples containing absolutely no carbon. The magnitude of peaks in the
blanks differs based on various factors such as system construction and the catalyst used.
For the TOC-L, every effort has been made to minimize these peaks, which can affect
the accuracy of TC analyses. Accuracy is particularly affected when trace TOC is measured
(such as in high sensitivity analysis of ultra-pure water samples); for this type of analysis,
the blank peaks must be small and stable. To check and correct for the magnitude of
the system blank peaks, use the TOC-Control L Blank Check procedure described below.
When using high-sensitivity TOC catalyst with this instrument, blank check measurement
is conducted using blank check water which is produced within the instrument itself.
1 Select an instrument in which the Catalyst type has been set for High Sensitivity,
and create a new Sample Table.
Do not enter anything into the Sample Table. The blank check sample will be
inserted automatically upon completion of the blank check setup operation.
Refer to "5.1.1 Creating a New System Configuration" P.124 to set up a new system
configuration. Refer to "5.3.1 Creating a Sample Table" P.146 to create a Sample Table.
2 Press Connect to establish communication between the Sample Table Editor and
the instrument.
Refer to "Connection" P.253 to connect the Sample Table Editor to the Instrument.
5 Click Start.
The Measurement Start screen is displayed.
Refer to "Connection" P.253 for the procedure for connecting to the Instrument.
6 Click either Keep running, Shut down instrument or Sleep to determine the
action to be taken following the blank check analysis.
• Keep running: The instrument remains operational after the blank check.
• Shut down instrument: The instrument is switched OFF after the blank check.
• Sleep: The instrument enters the 'sleep' state after the blank check. The restart date
and time are set in the Auto Restart Time fields.
Selecting Qut the appliction will shut down the Sample Table Editor after a Keep
running, Shut down instrument, or Sleep process.
7 Fill the dilution water bottle to capacity with distilled water, and place it in the
specified position.
Although blank check measurement requires only about 200 mL, fill the bottle
to capacity.
8 Click Start.
The sample is inserted into the Sample Table, and blank check analysis begins.
Errors for TC and IC analyses are additive. For samples that have a comparatively large
IC concentrations relative to TOC concentrations, the TOC analysis error is large if it is
determined by the difference between TC and IC results. Samples of this type include
samples from water treatment facilities or from the natural environment, such as rivers,
lakes, swamps, oceans and groundwater.
Using the difference between TC and IC to determine TOC is not appropriate for purified
water or ultra-pure water samples. The CO2 in air dissolves in the sample and is measured
as IC, causing the concentration to vary.
In such cases, the sample is pretreated with aeration or sparging before analysis to
remove the IC. The sample is then subjected to TC analysis, immediately followed by TOC
analysis using the NPOC method.
Sparge Sequence 3
There are two methods for sparging with this instrument.
Sparge Procedure
1 Refer to "3.1.11 Adjusting Sparge Gas Flow Rate" P.49 for the sparge gas delivery
procedure.
In this method, sparge gas can be used independently. While the first sample is
being measured, another sample can be sparged, thereby improving analysis
efficiency.
Effect on Analysis
Large variations sometimes occur in TOC analyses of samples containing suspended solids
because TOC is often contained in the suspended material. This effect is evident when
the same sample is analyzed on two different TOC analyzers. Good results are not
obtained if the suspended solids are handled differently in the gathering of biochemical
oxygen demand (BOD) and TOC correlative data.
The suspended solids described here are primarily considered impurities in the sample
that will pass through a 50 mesh strainer (openings of approximately 0.28 mm). When
larger solid particles are present, analysis should be performed without drawing water
into the instrument.
The procedure described below is for TOC analysis, but is also valid for TN analysis.
Analysis Restrictions
Since PTFE tubing with an inner diameter of about 0.5 mm is used in the instrument for
injecting the sample, suspended solids that do not pass through cannot be measured.
Analysis reproducibility is poor for samples that do not uniformly contain such solids even
if they should pass through the tubing.
Solids that are heavy and readily form sediment, such as silt, can accumulate at the
bottom of the syringe. This can scratch the rotor of the sample injector 8-port valve,
causing leaks. Sedimentation and separation should be performed to as great an extent
as possible prior to analysis.
Countermeasures
The following types of processing operations are normally used for measuring samples
containing suspended solids.
Various problems can be encountered when measuring samples that contain acids, bases
or salts. Such problems include corrosion of the NDIR analysis cell as well as detrimental
effects on analysis values and the life of the combustion tube and catalyst. If corrosion
of the inner surface of the NDIR cell occurs, baseline stability will decline and noise will
increase. Samples containing acids, bases or salts should be handled as described below.
The concentration at which adverse effects are produced varies depending on the type
of acid or salt and the TOC or TN concentration. Prior to analysis, dilute the sample so
that acid, base and salt concentrations are reduced to 1000 mg/L or less. Neutralization
is also required for bases. The TOC-L is equipped with an automatic dilution function to
perform these dilutions.
The optional B-type halogen scrubber is effective at protecting the NDIR cell with respect
to the analysis of samples that contain a concentration of salt equal or equivalent to
that of sea water. For details on B-type halogen scrubber specifications, refer to Section
8.3.8.
Acid
Dilution to a concentration of 1000 mg/L or less is desirable for acids. Concentrations up
to 5000 mg/L can be used if this level of dilution cannot be attained. Note that there
are also methods to reduce the acidity of hydrochloric acid or sulfuric acid to a more
neutral pH of 2 to 3 using potassium hydroxide or sodium hydroxide. This process
produces thermally stable sodium chloride or sodium sulfate, which prevent the
generation of acidic gas during sample combustion. Acid neutralization should be stopped
at a pH of about 2 to 3 and TOC direct analysis (NPOC analysis) should then be performed
after sparging to remove any IC. It is necessary to consider the TOC associated with
impurities contained in the alkali reagents used for neutralization. All salts of nitric acid
generate acidic gas under thermal decomposition; as a result, neutralization is ineffective.
When the sample contains hydrochloric or hypochlorous acid, hydrochloric acid gas is
generated from salts that are readily subject to thermal decomposition, such as
ammonium chloride, calcium chloride and magnesium chloride. The instrument is
equipped with a halogen scrubber; however, the scrubber's main function is absorb
hydrochloric acid gas generated by corrosion of the gold plating on the internal surface
of the NDIR cell.
Alkaline samples
When performing TC analysis on alkaline samples, the following problems can arise:
• Rapid decrease in sensitivity and loss of reproducibility
• Rapid degradation of catalyst or wear of the combustion tube
• Likelihood that IC will be high due to absorption of carbon dioxide
For these reasons, the NPOC analysis is suitable for alkaline samples.
In NPOC analysis, dilute hydrochloric acid is added first to adjust the solution to a pH
of 2 to 3. This causes a reaction that generates salt. For example, calcium chloride will
be formed as a salt if the sample contains calcium hydroxide as the base. Since it is
preferable for this salt concentration to be low, alkaline samples should be diluted as
much as possible.
Salt accumulation
Samples should be diluted as much as possible to reduce the salt concentration and
extend the life of the combustion tube and catalyst. Conducting a large number of
analyses on samples containing salts will allow the salts to accumulate in the combustion
tube, gradually increasing resistance to the flow of carrier gas and resulting in decreased
analysis reproducibility. When decreased reproducibility is observed, perform the
combustion tube maintenance procedure described in "7.2.4 Washing/Replacing the
Combustion Tube and Carrier Gas Purification Tube (Option)" P.326.
n Vial Types
The three types of ASI-L vial are 9 mL, 24 mL, and 40 mL vials. There are two models
of ASI-L unit, one is dedicated to 24 mL vials and the other supports both 9 mL and
40 mL vials. The sample volume associated with each vial type is shown below. Introduce
the specified volume of sample into each vial to basically attain the sample volume shown
in Table 3.1. When using the external sparge kit to sparge ASI-L vials in NPOC analysis,
reduce the sample volume to minimize contact between sample droplets and the vial cap
caused by sparging.
Wash any new vials using laboratory glassware detergent and then rinse them
thoroughly with water before use.
When using a TOC-LCPN, perform measurement using a calibration curve full scale
greater than 1 mg/L.
The target measurement range for three repeated measurements using 9 mL vials is
shown in "Table 3.4 Maximum Number of Measurements Using 9 mL Vials".
The table indicates the maximum number of measurements when using TOC standard
catalyst, the automatic setting for the sample injection volume, and stream washing is
set to once only. If residual removal is insufficient between vial usages when washing is
set to once only, performing analysis with vials of pure water placed between every other
vial can improve residual problems.
In most cases, vials can be placed in the ASI-L turntable and analyzed without being
sealed. Vials must be sealed in the following situations:
In situations (1) and (2) above, corrosion of the instrument may occur due to spattering
of sample, which contains acid.
In situations (3) through (9), results may be affected by either volatilization of the TOC
components in the sample or contamination from substances that absorb CO2 from the
atmosphere. If aluminum foil is used to cap the sample vial for NPOC or acidic sample
measurement, there is a danger of acid volatilization through the hole caused by
insertion of the needle. Do not use aluminum foil to cap the vials.
Regardless of the type of seal used, always use vials after washing them with
water or laboratory glassware detergent and then rising them thoroughly with
water.
Using Caps 3
For 24 mL and 40 mL vials
Caps and seals are provided with these vials.
Because the seals are perforated during injection, discard the seals after use.
Remove the vial rack from the ASI-L before inserting the sample vials. There are three
different types of vial racks, each accommodating a different vial size.
The ASI-L permits random access of vials in the vial rack. Vials are measured according
to the sequence set in the Sample Table Editor, thus enabling analysis to start from any
position number in the vial rack, and for analysis to occur in non-sequential vial positions.
Ensure that the vials are placed into the vial rack vertically and that they remain straight
during analysis.
When samples are to be sparged using the optional external sparge kit, analysis is
performed more efficiently if the vials are placed in sequential rack positions without gaps.
This allows a vial to be sparged while an adjacent vial is being measured.
1 Insert the vials into the vial rack and place the rack on the ASI-L turntable.
During analysis, the turntable must be covered. The ASI-L will not operate if the
turntable cover is not detected.
Rinse water will not flow properly if the rinse tube is not inserted correctly, and
measurement values may be adversely affected.
No. of Flow
No. of Flow
Wash (after Rinse Water
Wash Remarks
all meas. Usage
(between vials)
completion)
Approx.1.3 L Analyzing 93 samples with standard model.
1 1 Conducting NPOC analysis of 93 samples
Approx.2.3 L
with external sparge kit.
Approx.2.6 L Analyzing 93 samples with standard model.
2 2 Conducting NPOC analysis of 93 samples
Approx.3.6 L
with external sparge kit.
If samples with TOC concentrations of 100 µg/L or less (such as purified water or
ultra-pure water) are measured using an ASI-L, the following precautions associated with
high sensitivity analysis must be considered. Refer to "High Sensitivity Analysis" P.68 for
additional information.
• NPOC analysis is recommended. TOC (TC-IC) analysis tends to have a greater variation
in measured values than the NPOC analysis because IC often accounts for a significant
portion of the TC, and the errors in the two values are additive, which significantly
affects TOC analysis.
• To generate a calibration curve, fill well-washed vials with standard solutions to about
5-10 mm from the top of the vial, and immediately seal each vial.
Use a cap that has been washed with purified water prior to use.
When placing the vial in the rack, handle the vial carefully to avoid contact between
the standard solution and the cap. 3
Low-concentration standard solutions must be prepared each time they are used.
• To stabilize the peaks, perform 4 to 5 injections using the same analysis parameters
prior to analyzing the calibration standard solutions. For example, to generate a
400 µg/L calibration curve, place a 0 µg/L standard solution in vial position 1 and
measure it 4 to 5 times using the same analysis parameters that were selected for the
calibration curve. Refer to "5.3.2 Creating a Calibration Curve File" P.147. The objective
at this point is not to generate a calibration curve, but to inject water using the same
injection volume used for the calibration curve that is to be generated. This not only
stabilizes peaks but also thoroughly washes the sample needle and sparge needle with
purified water.
After the stabilizing injections are complete, place the 0 µg/L and 400 µg/L calibration
standard solutions in vial positions 2 and 3, insert the calibration standards into the
Sample Table Editor, and start measurement. Refer to "5.3.2 Creating a Calibration
Curve File" P.147.
• Acid addition for NPOC analysis can be performed automatically using the ASI-L. It is
best to perform manual addition of hydrochloric acid for NPOC analysis on the order
of 10 µg/L. This is because, automatic acid addition pierces the vial seal and allows CO2
contamination from the air.
• In the ASI tab of the Instrument Properties window, ensure that needle washing is not
conducted by setting the No. of Flow Wash (between vials) to 0.
Even if ultra-pure water is used as rinse water, the TOC concentration of the rinse
water will increase during the time it is exposed. For best results, do not rinse the
needle for analyses on the order of 100 µg/L.
• Do not use the analysis value acquired from the first sample vial. In sample analysis,
particularly analysis on the order of 10 µg/L, the first sample measured may yield high
results.
• When using the optional external sparge kit, use the standard sparge gas flow rate of
100 mL/min. The recommended sparging times are displayed as 3 minutes for 9 mL
vials, 6 minutes for 24 mL vials, and 10 minutes for 40 mL vials. If sparging is
insufficient, increase the gas flow rate or the sparging time accordingly.
If the sample pH does not reach a value between 2 and 3, increase the acid addition
ratio or the acid concentration. Excessively increasing the acid addition ratio will result
in dilution of the sample. On the other hand, if the acid amount is too small, the size
of the acid droplet on the tip of the needle will not be large enough to drop from the
needle.
Visually observe the process through the glass vial to determine if the acid droplet is
actually added to the sample.
The needle will be rinsed following each acid addition by placing a check mark next to
the Needle Rinse (after acid addition) item in the ASI tab of the Instrument Properties
window. To save time during the analysis sequence, rinsing of the needle is unnecessary
if the variation in NPOC concentration among the samples is not large.
When the vials are capped and sparging is performed without automatic acid
addition via ASI-L, pierce the caps before analysis by using the tip of a
provided needle or other instrument. This allows the sparge gas to vent. If
sparge gas is not vented from the vials, pressure will build inside the vials
and prevent effective sparging.
Note that the inside surfaces of the sparging needle may corrode due to
unwanted sample entry when conducting measurements other than NPOC
measurement that involve acidification and sparging of vials in the ASI-L
(including TC measurement, IC measurement, and NPOC measurement that
performed acidification and sparging within the TOC-L) over long periods of
time. For this reason, Shimadzu recommends removing the sparging needle
when performing these types of measurements.
n Stirrer Preparation 3
When using the optional magnetic stirrer on the ASI-L, perform the following procedure
to enable the magnetic stirrer. After attaching the optional magnetic stirrer, use the
following procedure to enable use of the stirrer.
The rotation speed can also be set as necessary.
Procedure
1 Display the Instrument Properties screen associated with the instrument settings
that will be used for measurement.
Refer to "5.1.2 Reviewing and Editing a System Configuration" P.134, to display the
Instrument Properties window.
4 Click OK.
1 Adjust the rotation speed by turning the stirrer rotation speed adjustment dial
at the bottom of the right side of the ASI-L.
When using 24 mL vials, the innermost row of vials are inaccessible to the stirrer.
When using 40 mL vials, all vials are accessible to the stirrer.
• The magnetic stirrer only agitates vials in the current sampling position and the next
sampling position. Proper mixing is not performed even if the stirrer bar can rotate at
other vial positions. For example, if vial number 20 is selected, stirring is performed for
vial 20 (sampling position) and vial 21 (next sampling position).
• Depending on the shape of the vial bottom, the stirrer bar rotation axis may shift.
However this has almost no effect on the effectiveness of the stirring.
• Adjust the stirrer rotation speed according to the sample properties. Use the stirrer
speed control dial on the right side of the ASI-L. Be careful not to increase the speed
excessively, as this can cause the stirrer bar to jump around instead of rotate.
• Turning the stirrer on and off repeatedly while the stirrer is set at the lowest speed
may cause fluctuations to occur in the motor speeds. This is due to the relationship
between the resistance values inside the motor and the impressed voltage, and only
occurs when the motor voltage is small. If this occurs, readjust the rotation speed using
the following procedure.
Procedure
1 Open the Instrument Properties window associated with the instrument used for
measurement.
Refer to "5.1.2 Reviewing and Editing a System Configuration" P.134, to display the
Instrument Properties screen.
4 Turn the stirrer speed control dial on the right side of the ASI-L to the maximum
speed position.
3
5 Replace the check mark next to the Activate Stirrer item. Clicking this item
several more times to turn it on and off repeatedly
6 Ensure that the check mark remains next to Activate Stirrer and reduce the
rotation speed using the control dial.
n Sample Container
There are no restrictions on the type of sample containers that can be used with the
OCT-L. It is only necessary that the containers be placed so the sample tubing from the
various ports can be inserted directly into the containers.
Wash all sample containers with an appropriate laboratory detergent, and rinse
them thoroughly with water before using them for the first time.
Open sample containers can be used to perform sample measurement with the OCT-L.
However, in the following situations, it is necessary to seal the sample container.
If the sample container openings are not sealed in the situations listed above,
measurement values may be influenced by such factors as absorption of
atmospheric CO2, contamination with carbon containing substances, and
evaporation of TOC constituents from the samples.
In either case, wash the container with a laboratory detergent, and rinse it
thoroughly with water before use.
1 Cut a piece of Parafilm to size according to the size of the sample vessel opening.
2 Insert the tip of the sampling tube into the vessel, cover the opening with the
prepared Parafilm, and seal the opening of the vessel, stretching the Parafilm
over the edges. Be sure that a very small gap in the seal is formed to prevent
creation of negative pressure inside the vessel.
3 Press the overlapping portions of the Parafilm around the neck of the opening.
(1) NPOC analysis is recommended because TOC (TC-IC) analysis tends to have a greater
variation in measured values than NPOC. This is because IC often accounts for a
significant portion of the TC, and the errors in the two values are additive using TOC
(TC-IC) analysis. This affect significantly influences TOC analysis.
(2) For calibration measurement of standard solutions, fill well-washed containers with
standard solutions to about 5-10 mm from the top of the container, and immediately
seal each container. When placing the container below the OCT-L, handle it carefully
to avoid the standard solution contacting the sealing surface. Low-concentration
standard solutions must be prepared each time they are used.
(3) To ensure that the peaks are stable for generating the calibration curve, perform 4-5
injections using the same analysis parameters prior to performing the calibration curve
analysis. For example, to generate a 400 ppb calibration curve, set 400 ppb as the 1st
standard solution concentration, and enter 1 as the container number. Actually place
a 0 µg/L solution in the vial for port No. 1. The objective of these settings at this point
is not to generate a calibration curve, but to inject water using the same injection
volume that will be used to generate the calibration curve. This allows stabilized peaks
to be obtained.
In the 2nd row of the settings screen and using the same calibration curve number as
above, set the analysis parameters for 0 ppb and 400 ppb. When sample measurement
starts, the calibration curve to be used will be created with the correct standard
solutions.
The TOC-L has two power switches: a power switch for everyday use (on the left side of
the front door of the instrument), and a main power switch (on the right side towards
the top of the instrument) for turning off power to the instrument over extended idle
periods. With the exception of extended idle periods, leave the main power switch turned
on and use the power switch on the front of the instrument start and stop the instrument
on a daily basis. The instrument consumes the minimum amount of energy required to
keep the software running (about 15 W) when the main power switch is left on.
When using the ASI-L or OCT-L, connect these units to the TOC-L using the corresponding
connection cables before turning on the main power switch on the TOC-L main unit.
Leave the power switch on the ASI-L turned on at all times.
1 Turn on the main power switch on the left side towards the top of the TOC-L.
The power switch on the left of the front door of the TOC-L lights up orange. While
the power switch is lit orange, it is not possible to connect the instrument to the PC.
2 Turn on the power switch on the left of the front door of the TOC-L.
The power switch lights up green and the instrument starts up. After start-up the
instrument can be connected to the PC.
Electric furnace heating and carrier gas supply will not start until the instrument starts up
and communication is established between the instrument and the Sample Table Editor.
The lit states of the power switch and the indicator in the middle of the TOC-L front
door represent the instrument states shown in Table 3.6.
Table 3.6 Relationship Between Power Switch and Indicator Lit States and Instrument State
This section describes how to set the pressure and flow rate of carrier gas in the TOC-L.
Setting Procedure
• Never allow the carrier gas supply pressure to exceed 250 kPa.
• Always keep the carrier gas tubing exclusive to this instrument. Branching the
tubing and connecting it to other equipment may adversely affect
measurement performance due to fluctuations in supply pressure.
• If the carrier gas supply pressure drops below 170 kPa, a warning message is
displayed.
If a warning message is displayed, verify the carrier gas supply source.
3 Right-click the system configuration on the Sample Table tab in the file viewer
and then click Connect. The Sample Table Editor connects to the instrument and
the Ready indicator lights up.
5 Verify that carrier gas flow rate displayed on the TOC tab in the Background
Monitor window becomes 150 mL/min.
Do not change the carrier gas flow rate during analysis. The peak area changes
in an inversely proportional relationship and may cause errors in analysis
precision.
n Carrier Gas Pressure and Flow Rate Settings (When Using the Carrier Gas Regulator
Option)
This section describes how to set the pressure and flow rate of carrier gas in the TOC-L.
Setting Procedure
If the carrier gas supply pressure must be set higher than 300 kPa, never allow
the pressure to exceed 600 kPa.
3 Right-click the system configuration on the Sample Table tab in the file viewer
and then click Connect. The Sample Table Editor connects to the instrument and
the Ready indicator lights up.
5 The supply gas pressure is displayed on the TOC tab in the Background Monitor
window. Watch the display while turning the carrier gas pressure adjustment
knob on the pressure adjustment unit (at the top right inside the instrument
front door) to attain a supply gas pressure of 200 kPa.
6 Verify that carrier gas flow rate displayed on the TOC tab in the Background
Monitor window becomes 150 mL/min.
Do not change the carrier gas flow rate during analysis. The peak area changes
in an inversely proportional relationship and may cause errors in analysis
precision.
The electric furnace power must be turned on for TC, TOC, NPOC, POC and TN analyses.
The electric furnace does not need to be turned on if only IC analysis is performed.
1 Open the Instrument Properties window associated with the instrument used for
measurement.
Refer to "5.1.2 Reviewing and Editing a System Configuration" P.134, to display the
Instrument Properties window.
3 For TN measurement, set the furnace temperature to 720 °C, and for all other
measurements, set it to 680 °C.
4 Click OK.
This section describes how to set the air gas pressure for supplying ozone when using
the optional TNM-L TN unit.
Setting Procedure
1 Set the air gas supply pressure for ozone to 200 to 300 kPa.
Never allow the air supply pressure for ozone to exceed 300 kPa.
2 Right-click the system configuration on the Sample Table tab in the file viewer
and then click Connect. The Sample Table Editor connects to the instrument and
the Ready indicator lights up.
4 The supply gas pressure is displayed on the TN tab in the Background Monitor
window. Watch the display while turning the carrier gas pressure adjustment
knob on the pressure adjustment unit (inside the door on the right side of the
TNM-L) to attain a supply gas pressure of 200 kPa.
Perform the following daily inspections before switching on power to the instrument.
• Remaining dilution water: Refer to "7.1.1 Checking Dilution Water" P.317.
• Remaining acid: Refer to "7.1.2 Checking Acid" P.317.
• Drain vessel water level: Refer to "7.1.3 Checking Drain Vessel Water Level" P.318. 4
• Humidifier water level: Refer to "7.1.4 Checking Humidifier Water Level" P.318.
Procedure
• When the main power switch is OFF (when the main power switch is not lit)
Turn on the main power switch on the right side towards the top and turn on the
power switch on the left side towards the front to start up the instrument.
• When the main power switch is ON (when the main power switch is lit orange)
Press the power switch on the left side towards the front to start up the instrument.
The Sample Table Editor is an application used for analyzing samples from the PC by
performing software operations.
Refer to "5.2.1 Opening the Sample Table Editor" P.139.
To perform the following operations, the instrument settings must first be created. If the
required instrument settings have already been created, this is not necessary.
Refer to "5.1.1 Creating a New System Configuration" P.124.
Procedure
1 Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon) in the Instruments tab.
The Sample Table Editor can also be started directly from the Windows Start menu and
from the shortcut icon created on the desktop.
The Sample Table is a file used for setting analysis parameters and sequence of analyses.
The Sample Table can also display the analysis results.
Refer to "5.3.1 Creating a Sample Table" P.146.
Procedure
on the toolbar.
4
The Select H/W Settings window is displayed.
2 Click the System drop down menu and select the system configuration to use
and then click the Table Type drop down menu and select Normal.
3 Click OK.
A new Sample Table is created, and opened in the Sample Table Editor.
• A calibration curve file is created to set the analysis parameters for measuring known
standard solutions and generating a calibration curve.
• A method file is created to set the analysis parameters for measuring unknown samples.
If these files already exist, the operations described below are unnecessary.
• Use a method to set measurements conducted with a combination of multiple
measurement items, such as TOC measurement using TC-IC (Analysis at the top of the
Method Wizard (Page 2) Analysis Information window).
If these analysis parameter files have already been created, this step does not need to
be performed.
Procedure
4
2 Select the System and click Next.
The Calibration Curve Wizard (Page 2) Calibration Curve Type page is displayed.
4 Select the type of analysis and place a check mark next to Zero Shift according
to the method. Click Browse.
6 Click Next.
The Calibration Curve Wizard (Page 4) Calibration Measurement Parameters page is
displayed.
4
7 Select the Units, and click Next.
The Calibration Curve Wizard (Page 5) Calibration Points List page is displayed.
8 Click Add.
9 Enter the calibration point concentration in the Cal. Point Conc. field, and click
OK.
10 Repeat steps 6 and 7 to set all of the calibration points, and click Next.
Method File
The procedure for entering the main parameters of the method file is described below.
Only the basic parameters are described here.
Refer to "5.3.3 Creating a Method" P.158 for more details.
Procedure
4
The Save As dialog box is displayed.
5 Click Next.
The Method Wizard (Page 3) Calibration Curves page is displayed.
6 Select the calibration curve to use in measurement and then click Next.
7 The default values entered for the settings on this page may be used for
conducting basic analysis. Verify the settings, and click Next.
Procedure
1 Insert the calibration curve (standard solutions) into the Sample Table.
Drag the calibration curve file from the Calibration Curve tab of the file viewer.
When analyzing multiple samples using the same conditions, the inserted sample can be
reproduced by copying and pasting. Select the inserted sample, right-click in the cell at
the left end of the row, and click Copy.
Select the rows in the Sample Table corresponding to the number of samples to set,
right-click in the cell at the left end of the row, and click Paste.
When the ASI-L or OCT-L is used for measurement, the sample vial numbers used are
entered as follows.
Refer to "5.4.6 Vial Numbers" P.210 for more details.
Procedure
Enter a number in a Vial column cell, click on the lower right part of the cell, and drag
downward to enter a series of sample vial numbers all at once.
3 Click OK to close the window and automatically set all of the vial numbers in
the Sample Table.
Communication is established between the Sample Table Editor and the instrument to
enable sample analysis.
Refer to "Connection" P.253 for more details.
Procedure
The ready state of the instrument is shown at the right end of the toolbar. 4
Approximately 30 - 40 minutes are required for the temperature of the furnace to rise
and the baseline to stabilize.
The instrument performs analysis based on the information in the Sample Table. The
operation differs depending on whether an ASI-L is being used.
Procedure
Selecting TOC-L Quit the application will shut down the Sample Table Editor
after a Keep running, Shut down instrument, or Sleep process.
Procedure
As each sample measurement is finished, the results are displayed in the TOC
Measurement window. Click Next to begin analysis of the next sample.
4 When a peak appears during analysis, click to open the Sample window.
The sample analysis results can be reviewed in the Sample Window, and output to a
printer or file.
Procedure
1 Click .
The Sample window is displayed. Each of the sample analyses can be reviewed.
Procedure
• Click , and then click Sample Report – All to print the analysis results report.
• Click , and then click Sample Table to display the Sample Table on the
• Click File – Ascii Export – ASCII Export Norm(Meas Data Only) to output the contents
of the Sample Table in text format.
The file that is output can be opened in a text editor or Microsoft Excel to view the
content.
This procedure describes the end of analysis and post-analysis instrument settings.
Refer to "5.7.7 Instrument Shutdown" P.271 for more details.
Procedure
1 Click .
After selecting shutdown and clicking the OK button, the power of the PC can be turned
off without waiting for the instrument power to turn off.
After sleep is selected and the OK button is clicked, the power of the PC can be turned
off after the connection between the PC and the instrument is broken.
System Configuration
1 Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon) in the Instruments tab.
When the User window is displayed, log in referring to "5.9.1 Login" P.294.
2 In the menu bar, select Options and click H/W Setting List.
Item Description
Enter a system name using up to 32 single-byte characters. Entry is
System mandatory. Use of a name that is already assigned to an existing
system configuration is not permitted.
Enter the serial number of the instrument. Entry is mandatory. The
Instr Serial No. serial number is printed on the plate attached to the lower right
side of the instrument.
The name of the current user is automatically entered into the User
User
field.
The current date is automatically entered into the Date of Creation
Date of Creation
field.
Enter additional system information in the Comment text box. The
Comment
Comment field is optional and can contain up to 512 characters.
5 Click Next.
The Instrument Setup Wizard - Options window is displayed.
Item Description
Model Select the type of TOC instrument you are using.
Item Description
Set any options you are using by selecting the corresponding
checkboxes.
• ASI-L: Select this checkbox if using the ASI-L Autosampler.
• OCT-L(1): Select this checkbox if using a single OCT-L 8-Port
Sampler.
• OCT-L(2): Select this checkbox in addition to the OCT-L(1) checkbox
if using two OCT-L 8-Port Samplers.
• SSM-5000A: Select this checkbox if using the SSM-5000A Solid
Sample Module for Total Organic Carbon Analyzer. For details on
the SSM-5000A, refer to the "SSM-5000A USER'S MANUAL".
• TNM-L: Select this checkbox if using the TNM-L TN Unit.
• POC Kit: Select this checkbox if using the POC Kit.
• External Sparge Kit: Select this checkbox if using the External
Options Sparge Kit.
• Manual Injection Kit: Select this checkbox if using the Manual
Injection Kit. Selecting this checkbox disables the ASI-L, SSM-5000A,
and POC Kit options.
• Small Syringe Kit: Select this checkbox if using the Small Syringe
Kit.
• High Suspension Kit (High Conc.): Select this checkbox if using the
High Suspension Kit for High Concentrations. For details on the
High Suspension Kit for High Concentrations, refer to "3.1.13
Preparing the High Suspension Kit (When Using the Optional High
Suspension Kit)" P.53.
• High Suspension Kit (Low Conc.): Select this checkbox if using the
High Suspension Kit for Low Concentrations. For details on the 5
High Suspension Kit for Low Concentrations, refer to "3.1.13
Preparing the High Suspension Kit (When Using the Optional High
Suspension Kit)" P.53.
7 Click Next.
The Instrument Setup Wizard - TOC window is displayed.
Item Description
Selecting this checkbox will cause the instrument to automatically
regenerate IC reagent in the following situations. Normally, this
checkbox should be selected.
Auto regeneration of • When the instrument power is turned on
IC solution
• Before the initial IC measurement, following a preset number of
injections and preset volume of injected samples
• If peak tailing occurs in IC measurement
Selecting this checkbox will supply power to the optional TNM-L. If
the TNM-L is installed, ensure that this checkbox is selected.
TN Power
This option is only enabled if the TNM-L checkbox was selected
under Options in the Instrument Setup Wizard Options window.
Set the analysis operations to perform prior to sample injection.
The operation types available for analysis are Normal, Stir
Suspension Solids, and High Suspension Mode.
• Normal: Perform a standard injection operation.
• Stir Suspension Solids: Agitate the sample in the syringe
Measurement
immediately before injection.
Method
• High Suspension Mode: Perform an operation appropriate to the
analysis of precipitative suspended solids.
This option is selected if the High Suspension Kit (High Conc.) or
High Suspension Kit (Low Conc.) checkbox was selected under
Options in the Instrument Setup Wizard Options window.
Selecting this checkbox in the system configuration for the added
Ext. Sparge Valve
external sparge kit allows sparge gas to continue flowing while the
OPEN
Sample Table Editor is connected to the instrument.
Item Description
Enable ready status Selecting this checkbox enables the instrument's Ready Status Check
check function. Normally, this checkbox should be selected.
Selecting this checkbox agitates the sample extracted with the
Stir Suspended Solids syringe of the sample injector with sparge gas immediately before
injecting it into the combustion tube (or IC reaction vessel).
Set the carrier gas flow rate. Normally, this should be set to
Carrier Gas Flow
150 mL/min (default value).
Select the type of carrier gas to supply to the TOC instrument. The
Carrier Gas available types of carrier gas are Air, Oxygen, and Nitrogen. The
optional N2 carrier gas kit is required to use nitrogen gas.
Select the catalyst type. Click on the box, and select either Regular,
Catalyst Type
High Sense, or TC/TN.
Select the type of tubing installed in the TOC-L main unit. Click on
the box and select either Regular or Suspended Particle. For typical
Tubing Diameter
measurements, select Regular. Select Suspended Particle if the
optional Suspended Solids kit will be used.
This item sets the detector cell length. Click the box, and select
Cell Length
either Long or Short. Normally, Long is selected.
This item sets the TC furnace temperature. Select 680 for Regular or
TC Furnace
High Sense catalyst, and 720 for TC/TN catalyst.
9 Click Next.
If ASI-L was selected in the Options page of the Instrument Setup Wizard, the Instrument 5
Setup Wizard-ASI window is displayed.
Item Description
Select the vial rack type. Click on the box, and select 9 mL Vial,
Vial Type
24 mL Vial or 40 mL Vial.
Set the needle type. Click the box and then click the needle type
to be used from the list. These items are only enabled if the Sparge
Kit item was selected on the Options page of the Instrument Setup
Needle Type Wizard.
• Sample: for analysis using only a sample needle
• Sample + Sparge: for analysis using a sample needle and sparge
needle
No. of Flow Wash Select the number of times (0 - 10) the outside of the needle will
(between vials) be washed with dilution water, after each sample analysis.
Select the number of times (0 - 10) the flow line will be washed
No. of Flow Wash with dilution water from the needle to the injection tube, at the
(after all meas. completion of the sample sequence. A single wash is acceptable for
completion) typical samples. Select 3 – 4 washes when analyzing samples
containing acid, alkali or salt.
Select this item to rinse the sampling needle with dilution water
between each sample. If the difference in concentration among
samples in the sample run is negligible, this rinse may be omitted.
Needle Rinse (after Better results are obtained by not rinsing between samples when
sampling) analyzing ultra-pure water with a concentration of less than a few
100 µg/L.This happens because the concentration of the dilution
water becomes greater than the sample as it is exposed to the
atmosphere.
Select this item to rinse the sampling needle with dilution water
Needle Rinse (after
after each acid addition. If the difference in NPOC content among
acid addition)
the samples is not large, this rinse may be omitted.
Item Description
Activate Stirrer Select this item to enable use of the magnetic stirrer.
11 Click Next.
The Instrument Setup Wizard-SSM window is displayed.
13 Click Next.
The Instrument Setup Wizard-Communication window is displayed.
14 Enter the parameters for communication between the PC and the instrument.
Item Description
Enter the communication port. Click on the box, and select from
Com1 to Com10.
Select the port number to be used by the USB device driver for
Com Port
TOC-L.
For information on the USB device driver, refer to "LabSolutions
DB/CS Installation & Maintenance [for LabSolutions TOC]".
This item is entered automatically and is dependent on the Com
Stop Bits
Port selection.
This item is entered automatically and is dependent on the Com
Parity
Port selection.
16 Click Finish.
The system configuration is created.
The newly created system configuration is displayed as an icon in the H/W Setting List
window. The system name is displayed with the icon.
System configurations may be viewed and edited as necessary. Some items cannot be
edited after the system configuration is created.
Procedure
1 Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon) in the Instruments tab.
When the User window is displayed, log in referring to "5.9.1 Login" P.294.
2 In the menu bar, select Options and click H/W Setting List.
The H/W Setting List window is displayed.
3 Select the icon of the system configuration element to be viewed or edited, and
click Open.
4 Click the tabs at the top of the window to view or edit the content as necessary.
Click Print to open the Print window and enable printing of the Instrument Properties
window settings.
5
The tabs are described below.
Depending on the system configuration, the ASI tab may not be present.
• System: Same as the Instrument Setup Wizard-System Information window. The system
name and serial number cannot be edited.
• Options: Same as the Instrument Setup Wizard Options window. The items on this tab
cannot be edited.
• TOC: Same as the Instrument Setup Wizard-TOC window.
• ASI: Same as the Instrument Setup Wizard-ASI window.
• SSM: Same as the Instrument Setup Wizard-SSM window.
• Communication: Same as the Instrument Setup Wizard-Communication window. If these
items are edited, the changes are reflected at the next instrument connection.
• History: All modifications made to the system configuration are displayed in a list
format. Click the Ascii Export button to output the history to an ASCII format text file.
5 Click OK.
Any changes to the system configuration are saved, and the window closes.
Procedure
2 In the Sample Table tab of the file viewer, right-click on the system configuration
to be viewed or edited and select Instrument Settings.
If a sample table is open, click Instrument – H/W Settings to display the Instrument
Properties window for the system associated with the sample table.
Procedure
1 Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon) in the Instruments tab.
When the User window is displayed, log in referring to "5.9.1 Login" P.294.
2 In the menu bar, select Options and click H/W Setting List.
The H/W Setting List window is displayed.
3 Select the icon of the system configuration element to be deleted, and click
Delete.
4 Click Yes.
The system configuration is deleted.
1 Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon).
When the User screen is displayed, refer to "5.9.1 Login" P.294 and log in.
2 In the menu bar, select Options and click H/W Setting List.
The H/W Setting List window is displayed.
3 Click History.
Procedure
1 Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon) in the Instruments tab.
When the User window is displayed, log in referring to "5.9.1 Login" P.294.
Procedure
5
1 Select File – Exit.
The Sample Table Editor window consists of the components shown below.
Item Description
Menu Bar Many operations can be performed from the menus.
Tool Bar Primary operations can be performed from the icons.
The file viewer has 5 tabs to display the files that can be processed
using the Sample Table Editor. Click a tab to change the displayed
files.
is a sorting button. Click this button to sort the file list according
to one of the 4 options:
File Viewer • file name, ascending order
• file name, descending order
• creation date, ascending order
• creation date, descending order
Click once on file to display a file summary in the tool tip, and
double-click the file to open that file.
Item Description
Displays the name, ID, measurement results, etc. associated with the
Status Monitor
sample in the table.
Displays a brief description of selected menu items and the user's
Status Bar
name.
Output Window Displays information regarding the instrument operation.
Common Operations
Click in the upper right corner of the Sample Table Editor to execute the
The Sample Table column headings describe the information listed in that column.
Refer to "5.3.1 Creating a Sample Table" P.146 for details on creating a Sample Table.
Sample table rows that contain unmeasured samples are indicated with an
asterisk next to the row number.
When a sample is inserted into the Sample Table, the following columns may displayed.
The columns displayed vary depending on the display settings. To change the
settings, refer to "5.8.1 Sample Table" P.282.
Column Description
Displays the sample type.
• Standard is displayed for standard solutions.
Type
• Unknown is displayed for unknown samples.
• Control is displayed for control samples.
Analysis Displays the type of analysis (TC, IC, etc.).
Sample Name Displays the sample name.
Column Description
Sample ID Displays the sample ID.
Displays the object ID. Depending on the software, a unique number
Object ID
may be allocated to each sample.
Origin Displays the name of the file from which the settings are referenced.
Manual Dilution Displays the manual dilution factor. This item is entered by the user.
Result Displays the measured concentration result.
Displays information such as whether the assessment is based on a
Notes
control sample or on USP/EP measurement.
Comment Displays any entered comment.
Displays the sample status.
• Defined
Status • Measuring
• Completed
• Aborted
Action Displays the remedial action to be taken if an error occurs.
Date / Time Displays the date and time of analysis.
Vial Displays the sampled vial number.
The Sample Window column headings describe the information listed in that column.
The Sample Window includes an Injection Table containing injection-related information.
Refer to "5.5.1 Sample Window" P.222 for details regarding the Sample Window.
When a sample is selected in the Sample Table, the following information is displayed
in the Sample Window.
The columns displayed vary depending on the sample type and display item
settings. Refer to "5.8.2 Sample Window Display Options" P.285 to change the
settings.
Column Description
Displays the sample or standard number.
Spl. No./Std. No. Spl. No. is used for Unknown and Control samples.
Std. No. is used for calibration curve samples. 5
Std. Solution Conc. Displays the concentration of the standard solution.
Injection No. Displays the injection number.
Area Displays the area value.
Mean Area Displays the mean area value.
Conc. Displays the concentration.
Mean Conc. Displays the mean concentration.
Result Displays the measured concentration result.
Displays a remark. Remarks consist of the following types.
• Tailing occurred in the detector output.
• H: Saturated signal occurred in the detector output.
Remarks • h: The measured value exceeded the calibration curve range.
• S: IC reagent automatic regeneration was conducted. (Displayed
only with TOC-LCPH)
• R: Analysis parameters were changed due to software settings.
SD Area Displays the area SD value.
CV Area Displays the area CV value.
SD Conc. Displays the concentration SD value.
CV Conc. Displays the concentration CV value.
Column Description
Displays the injection status.
• Defined
Status • Measuring
• Completed
• Aborted
Vial Displays the vial number of the sample.
Displays the exclusion flag (E) for exclusion of the injection. If
Excluded analysis parameters were changed due to software settings, R is
displayed.
Inj. Vol. Displays the injection volume
Auto Dil. Displays the dilution factor.
Displays the name of the calibration curve file referenced to obtain
Calibr. Curve
the calibration curve calculation.
Date / Time Displays the date and time the analysis was conducted.
The types of files created and used in the Sample Table Editor are described below.
A Sample Table is a file in which analysis information is entered in sequential order and
is used to conduct analysis.
Procedure
The Select H/W Settings window can also be displayed by selecting File – New – Sample
Table.
2 Click the System drop down menu and select the system configuration to use
and then click the Table Type drop down menu and select Normal.
Enter a comment in the Comment box, as necessary.
3 Click OK.
A new Sample Table is created, and opens inside the Sample Table Editor.
Refer to "5.4 Editing a Sample Table" P.194 for the procedure for inserting information
into the Sample Table.
A Calibration Curve File is used to generate a calibration curve. This file includes standard
solution concentrations and measurement parameters.
Procedure
Item Description
System Select the system to be used for measurement.
The name of the User conducting the operation is automatically
User
entered.
Date of Creation The current date and time are automatically entered.
A comment (using up to 512 single-byte characters) regarding the
Comment
system configuration may be entered as necessary.
3 Click Next.
The Calibration Curve Wizard (Page 2) Calibration Curve Type page is displayed.
Item Description
• Normal:
Normally, use this option. Selecting the Use dilution from standard
5
solution checkbox sets the usage of standard solution
automatically prepared inside the instrument.
• USP/EP Support:
Type settings
Sets the creation of a calibration curve according to USP/EP
specifications.
• JP Support:
Sets the creation of a calibration curve according to JP
specifications.
5 Click Next.
The Calibration Curve Wizard (Page 3) Analysis Information page is displayed.
Item Description
Analysis Click the box, and select the analysis type from the list.
Default Sample Name Enter a sample name using up to 65 single-byte characters.
Default Sample ID Enter a sample ID using up to 65 single-byte characters.
Calculation Method Click the box, and select either Point-to-Point or Linear Regression.
Select this item to shift the calibration curve through the origin.
Zero Shift For information on the zero shift setting, refer to "Shifting of
Calibration Curves" P.390.
8 Click Next.
The Calibration Curve Wizard (Page 4) Calibration Measurement Parameters page is
displayed.
Item Description
Units Select the concentration unit from ppm, ppb, mg/L, µg/L, no unit.
Item Description
Select the number of injections (1 – 20). The left box indicates the
number of analysis injection and the right box indicates the
maximum number of injections. The result is calculated using the
mean value of the total number of analysis injections. If the
No. of Injections
resulting value exceeds the SD Max. and CV Max. limits, additional
injections are performed for confirmation. The maximum number of
injections includes the analysis injections and the additional
injections.
Select the number of times (1 – 10) the flow line will be washed
No. of Washes
before the first injection.
Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used
to assess the analysis result. This parameter is activated if the No.
SD Max.
of Injections setting has a larger maximum number of injections than
the number of analysis injections.
Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is
used to assess the analysis result. This parameter is activated if the
CV Max.
No. of Injections setting has a larger maximum number of injections
than the number of analysis injections.
Enter the sparge gas flow rate (50 – 200). Normally, a flow rate of
Sparge Gas Flow
80 to 100 mL/min is appropriate.
Sparge Time Enter the sparge time (0 – 20).
Acid Addition Enter the percentage (0 – 20) of acid to be added to the sample.
10 Click Next.
The Calibration Curve Wizard (Page 5) Calibration Points List page is displayed.
Item Description
5
Auto Dilution Displays the calculated automatic dilution factor.
Inj. Volume Displays the calculated injection volume.
Calibration point list Displays the information associated with each calibration point.
Opens the Edit Calibration Point Parameters dialog box to allow
Edit
editing of the selected calibration point.
Opens the Edit Calibration Point Parameters dialog box to add a
Add
new calibration point.
Delete Deletes the selected calibration point.
Delete All Deletes all of the calibration points in the Calibration point list.
12 Change the calibration point parameters as necessary using the Edit Calibration
Point Parameters dialog box.
Depending on the settings in the Calibration Curve Wizard (Page 2) Calibration Curve
Type page, the contents of the Edit Calibration Point Parameters dialog box may differ.
• When not using the dilution of stock solution function
Item Description
Displays the calibration point number that corresponds to the
Calibration Point No.
number in Calibration Curve Wizard (Page 5) Calibration Points List.
Cal. Point Conc. Enter the calibration point concentration.
Select the number of injections (1 – 20). The left box indicates the
number of analysis injection and the right box indicates the
maximum number of injections. The result is calculated using the
mean value of the total number of analysis injections. If the
No. of Injections
resulting value exceeds the SD Max. and CV Max. limits, additional
injections are performed for confirmation. The maximum number of
injections includes the analysis injections and the additional
injections.
Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used
to assess the analysis result. This parameter is activated if the No.
SD Max.
of Injections setting has a larger maximum number of injections than
the number of analysis injections.
Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is
used to assess the analysis result. This parameter is activated if the
CV Max.
No. of Injections setting has a larger maximum number of injections
than the number of analysis injections.
Item Description
Displays the calibration point number that corresponds to the
Calibration Point No.
number in Calibration Curve Wizard (Page 5) Calibration Points List.
Standard Solution
Enter the standard solution concentration.
Conc.
Cal. Point Conc. Enter the calibration point (concentration) for calibration.
Displays the automatic dilution factor calculated from Auto.
Dilution / Standard Solution Conc..
Auto. Dilution Set values that ensure the dilution factor is greater
than 1.25. If the dilution factor is less than 1.25, the
dilution factor precision of the instrument may be
impaired. 5
Select the number of injections (1 – 20). The left box indicates the
number of analysis injection and the right box indicates the
maximum number of injections. The result is calculated using the
mean value of the total number of analysis injections.
No. of Injections
If the resulting value exceeds the SD Max. and CV Max. limits,
additional injections are performed for confirmation. The maximum
number of injections includes the analysis injections and the
additional injections.
Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used
to assess the analysis result. This parameter is activated if the No.
SD Max.
of Injections setting has a larger maximum number of injections than
the number of analysis injections.
Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is
used to assess the analysis result. This parameter is activated if the
CV Max.
No. of Injections setting has a larger maximum number of injections
than the number of analysis injections.
Refer to the following table to ensure that the concentration does not exceed
the maximum concentration specified for the respective analysis type. If the
concentration exceeds the maximum value, the instrument performance may be
adversely affected.
*1 If the Dilution from Standard Solution item is selected in the Calibration Curve Wizard
(Page 2) Calibration Curve Type page.
13 Click OK.
The Calibration Curve Wizard (Page 5) Calibration Points List page is displayed.
14 Click Next.
The Calibration Curve Wizard (Page 6) Additional Settings page is displayed.
Item Description
If this item is selected, the software default values are used for peak
Use default settings detection and the Min. integration time and Max. integration items
are disabled.
Enter the minimum time the instrument signal will continue to be
Min. integration time
detected.
Enter the maximum time the instrument signal will be detected
Max. integration
when no peak is found.
If this item is selected, the calibration curve error judgment is based
on the correlation coefficient. When this item is selected, Failure
Correlation Coeff. Action (1st time), Failure Action (2nd time) and Lower limit items
Check are also activated.
If the calibration curve contains less than 3 calibration points, error
judgement is not possible, and this option will have no effect.
Select the process to be conducted if an error occurs.
Continue: Records the error in the Sample Table, and allows analysis
Failure Action (1st to continue.
time) Stop: Records the error in the Sample Table, and stops analysis.
Repeat: Records the error in the Sample Table, and re-analyzes the
calibration curve.
Select the process to be conducted if a second error occurs.
Failure Action (2nd Continue: Records the error in the Sample Table, and allows analysis
time) to continue.
Stop: Records the error in the Sample Table, and stops analysis.
5
Enter the minimum correlation coefficient value. If the calculated
Lower Limit correlation coefficient is less than the value entered, an error is
assessed.
16 Click Finish.
The calibration curve file is saved.
A Method is a file used to set the analysis parameters used for measuring unknown
samples.
Procedure
The Method Wizard (Page 1) System Information page can also be displayed by selecting
File – New – Method.
Item Description
System Select the system to be used for measurement.
The name of the User conducting the operation is automatically
User
entered.
Item Description
Date of Creation The current date and time are automatically entered.
A comment (using up to 512 single-byte characters) regarding the
Comment
system configuration may be entered as necessary.
3 Click Next.
The Method Wizard (Page 2) Analysis Information page is displayed.
Item Description
Select the analysis type from the list. "TOC" indicates TOC
Analysis
measurement using TC-IC.
Default Sample Name Enter a sample name using up to 65 single-byte characters.
Default Sample ID Enter a sample ID using up to 65 single-byte characters.
Enter the sample preparation dilution factor if the sample was
Manual Dilution diluted manually. The entered value will be used in the
concentration calculation. The default value is 1.
Enter the number of times each sample is to be injected. If the
No. of multiple injections item is selected one aliquot will be drawn into
Determinations the syringe and all of the required injections are made from this
aliquot.
File Name Enter a method file name.
6 Click Next.
The Method Wizard (Page 3) Calibration Curves page is displayed.
7 Select the calibration curve files that will be incorporated into the method. Up
to 3 calibration curve files can be selected.
If multiple calibration curve files are selected, the software selects the most suitable
calibration curve during the analysis.
For information on this function, refer to the following page.
Refer to "8.2.5 Automatic Selection of Optimum Calibration Curve" P.392 for more details.
Item Description
Displays the analysis type selected in the Method Wizard (Page 2)
Analysis Analysis Information page. "TOC" indicates TOC measurement using
TC-IC.
Calibration Curve 1,
Click to locate the calibration curve folder, and select the file
Calibration Curve 2,
Calibration Curve 3 using the Open dialog box.
8 Click Next.
The Method Wizard (Page 4) Injection Parameters page is displayed.
Item Description
Displays the analysis type selected in the Method Wizard (Page 2)
Analysis Analysis Information page. "TOC" indicates TOC measurement using
TC-IC.
Units Select the concentration unit from ppm, ppb, mg/L, µg/L, no unit.
Injection Volume The injection volume is automatically entered.
Enter the expected concentration value if one is known. This item
is not required. A range value is automatically entered based on the
Expected Conc. Range
calibration curve selected on Method Wizard (Page 2) Calibration
Curves.
Select the number of injections (1 – 20). The left box indicates the
number of analysis injections and the right box indicates the
maximum number of injections. The result is calculated using the
mean value of the total number of analysis injections.
No. of Injections
If the resulting value exceeds the SD Max. and CV Max. limits,
additional injections are performed for confirmation. The maximum
number of injections includes the analysis injections and the
additional injections.
Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used
to assess the analysis result. This parameter is activated if the No.
SD Max.
of Injections setting has a larger maximum number of injections than
the number of analysis injections.
Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is
used to assess the analysis result. This parameter is activated if the
CV Max.
No. of Injections setting has a larger maximum number of injections
than the number of analysis injections.
Enter the number of times (1 – 10) the flow line will be washed
No. of Washes
before the first analysis injection.
Item Description
Auto. Dilution Enter the sample dilution factor.
Enter the sparge gas flow rate (50 – 200). Normally, a flow rate of
Sparge Gas Flow
80 to 100 mL/min is appropriate.
Sparge Time Enter the sparging time (0 – 20).
Acid Addition Enter the percentage (0 – 20) of acid to be added to the sample.
If this item is selected, multiple injections are made from a single
sample aliquot. This larger aliquot is drawn in the syringe in one
Multiple Injections
aspiration and is sufficient to accommodate all of the repeat
injections.
If selected, the blank analysis value is subtracted from the analysis
Use blank check area
result.
If selected, the instrument will automatically adjust the injection
Correction of inj. Vol volume and conduct re-analysis when the measurement result
exceeds the calibration curve range.
If selected, the instrument will automatically adjust the dilution
Correction of dilution factor and conduct re-analysis when the measurement result exceeds
the calibration curve range.
10 Click Next.
The Method Wizard (Page 5) Peak Time Parameters page is displayed.
Item Description
Displays the analysis type selected in the Method Wizard (Page 2)
Analysis Analysis Information page. "TOC" indicates TOC measurement using
TC-IC.
Item Description
If this item is selected, the software default values are used for peak
Use default settings detection and the Min. integration time and Max. integration items
are disabled.
Enter the minimum time the instrument signal will continue to be
Min. integration time
detected.
Enter the maximum time the instrument signal will be detected
Max. integration
when no peak is found.
12 Click Next.
If the analysis type is set to TC, IC, NPOC, POC or TN, the Method Wizard (Page
6) Pharmaceutical water testing window is displayed.
The other analysis types consist of combinations of the above five types (for
example, TOC is a combination of TC and IC). Repeat the setting procedure from
step 6 for any analysis types for which the parameters have not been set because
the analysis parameter settings here are performed with respect to the above
five types. When the settings are complete for all the analysis types, proceed to
the Method Wizard (Page 6) Pharmaceutical water testing window.
13 Click Next.
The Method Wizard (Page 6) Pharmaceutical water testing window is displayed.
Item Description
• None: Do not test measurement values.
• USP/EP system suitability test: Test whether measurement values
conform to the USP (United States Pharmacopeia) / EP (European
Pharmacopoeia) system suitability test standards.
• USP/EP TOC test: Test whether measurement values conform to the
Testing method
USP (United States Pharmacopeia) / EP (European Pharmacopoeia)
settings
pharmaceutical water test standards.
• JP recovery rate test: Test whether measurement values conform
to the JP (Japanese Pharmacopoeia) resolvability test standards.
• JP TOC test: Test whether measurement values conform to the JP
(Japanese Pharmacopoeia) pharmaceutical water test standards.
When performing pharmaceutical water testing, set the injection volume and
automatic dilution factor to the same values as the calibration curve used for
calculating concentration.
Do not set multiple calibration curves to use in calculating concentration or select
the [Auto. Correction of inj. Vol. and dilution] checkbox. Doing so may change
the injection volume and automatic dilution factor.
15 Click Finish. 5
The method file is saved.
The control sample is a sample with a known concentration that is used for evaluating
the accuracy of the instrument.
A control sample file is a file used for entering the control sample analysis parameters.
Procedure
The Control Sample Wizard (Page 1) System Information page can also be displayed by
selecting File – New – Control Sample.
Item Description
System Select the system to be used for measurement.
The name of the User conducting the operation is automatically
User
entered.
5
Date of Creation The current date and time are automatically entered.
A comment (using up to 512 single-byte characters) regarding the
Comment
system configuration may be entered as necessary.
3 Click Next.
The Control Sample Wizard (Page 2) Control Sample Type page is displayed.
Item Description
Control sample types Control Sample: Specifies use of a typical control sample.
Save the data in a
Enter a file name that will become the name of the control sample
control sample
file.
template
6 Click Next.
The Control Sample Wizard (Page 3) Parameter Source page is displayed.
7 Select the source file type to be used for creating the control sample.
Item Description
• Method: The analysis parameters in an existing method file are
referenced. Click to locate the method folder, and select the
appropriate method file using the Open dialog box.
• Calibration Curve: The analysis parameters in an existing
Parameter sources
calibration curve file are referenced. Click to locate the
calibration curve folder, and select the appropriate file using the
Open dialog box.
• Edit parameters manually: The analysis parameters are entered
manually without obtaining them from a source file.
Skip remaining
wizard pages and use Select this item to skip the remaining Wizard pages. A Finish button
measurement is displayed at the bottom of the page. Click it to save the control
parameters from the sample file.
source
If the analysis parameters are obtained from a Method or Calibration Curve file,
those parameters are automatically entered. However, some of the parameters
can be edited as necessary.
8 Click Next.
The Control Sample Wizard (Page 4) Analysis Parameters page is displayed.
Item Description
Analysis Click the box, and select the analysis type from the list.
Default Sample Name Enter a sample name using up to 64 single-byte characters.
Default Sample ID Enter a sample ID using up to 64 single-byte characters.
Enter the sample preparation dilution factor if the sample was
Manual Dilution diluted manually. The entered value will be used in the
concentration calculation. The default value is 1.
10 Click Next.
The Control Sample Wizard (Page 5) Injection Parameters page is displayed.
Item Description
Analysis
Displays the analysis type selected in Control Sample Wizard (Page 5
4) Analysis Parameters.
Units Select the concentration unit from ppm, ppb, mg/L, µg/L, no unit.
Enter the expected concentration value if one is known. Input is not
Expected Conc. Range
mandatory.
Injection Volume The injection volume is automatically entered.
Select the number of injections (1 – 20). The left box indicates the
number of analysis injections and the right box indicates the
maximum number of injections. The result is calculated using the
mean value of the total number of analysis injections.
No. of Injections
If the resulting value exceeds the SD Max. and CV Max. limits,
additional injections are performed for confirmation. The maximum
number of injections includes the analysis injections and the
additional injections.
Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used
to assess the analysis result. This parameter is activated if the No.
SD Max.
of Injections setting has a larger maximum number of injections than
the number of analysis injections.
Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is
used to assess the analysis result. This parameter is activated if the
CV Max.
No. of Injections setting has a larger maximum number of injections
than the number of analysis injections.
Enter the number of times (1 – 10) the flow line will be washed
No. of Washes
before the first analysis injection.
Auto. Dilution Enter the sample dilution factor.
Item Description
Enter the sparge gas flow rate (50 – 200). Normally, a flow rate of
Sparge Gas Flow
80 to 100 mL/min is appropriate.
Sparge Time Enter the sparging time (0 – 20).
Acid Addition Enter the percentage (0 – 20) of acid to be added to the sample.
If this item is selected, multiple injections are made from a single
Multiple Injections aliquot. This larger aliquot is drawn in the syringe in one aspiration
and is sufficient to accommodate all of the repeat injections.
Use area retrieved If selected, the blank analysis value is subtracted from the analysis
from the blank check result.
12 Click Next.
The Control Sample Wizard (Page 6) Peak Time Parameters page is displayed.
Item Description
Displays the analysis type that was selected for Analysis Type in the
Analysis
Control Sample Wizard (Page 4) Analysis Type page.
If this item is selected, the software default values are used for peak
Use default settings detection and the Min. integration time and Max. integration items
are disabled.
Enter the minimum time the instrument signal will continue to be
Min. integration time
detected.
Enter the maximum time the instrument signal will be detected
Max. integration
when no peak is found.
14 Click Next.
The Control Sample Wizard (Page 7) Control Checking page is displayed.
Item Description
• Recovery %
Select this parameter to evaluate the recovery percent of the
control sample.
Enter the original sample concentration in the Original Conc. field.
Select Spiked and enter a Spiked Conc. value to calculate the
recovery by comparing the original control sample concentration
to the spiked concentration.
• Mean Value (Concentration)
Evaluation type Select this parameter to evaluate the mean concentration of the
control sample.
• Blind Value (Area)
Select this parameter to evaluate the mean area of the control
sample.
• Spanwidth (Concentration)
Select this parameter to evaluate the deviation of the control
sample concentration. If this item is selected, the Max Dev% must
also be entered.
Enter the lower limits for the selected control sample evaluation
Low Lmt.
procedure.
Enter the upper limits for the selected control sample evaluation
Up. Lmt.
procedure.
Ignore Zero Shift of
Select this item to ensure that the concentration calculation is
Cal. Curve in Conc.
conducted while ignoring the calibration curve shift to origin setting.
Calculation
Item Description
Select the action to be taken the first time a control sample exceeds
the control limits. Click the box, and select the appropriate action
from the following options:
• Continue (notify)
Records failure in Sample Table, and allows the analysis to
continue.
Action when the • Stop (whole sample run)
failure event occurs Records the failure in the Sample Table, and stops the analysis.
the first time
• Repeat (from last control or calibration)
Records the failure in the Sample Table, and re-analyzes the
samples following the prior control sample or calibration curve.
• Re calibrate and Repeat
Records the failure in the Sample Table, re calibrates the
calibration curve and re-analyzes the samples following the last
control sample.
Select the action to be taken if a control sample exceeds the control
limits when during repeat analysis as specified for the 1st failure
action. Click the box, and select the appropriate action from the
Action when the following options:
failure event occurs • Continue (notify)
the second time Records failure in Sample Table, and allows the analysis to
continue.
• Stop (whole sample run)
Records the failure in the Sample Table, and stops the analysis.
16 Click Finish.
The Control Sample file is saved.
A schedule is a stored file which contains measurement parameters for multiple samples,
including the specified sequence of analyses. The saved content of the file can be called
up as desired, and loaded into a sample table.
Procedure
The Select H/W Settings window can also be displayed by selecting File – New – Schedule.
2 Click the System drop down menu and select the system configuration to use
and then click the Table Type drop down menu and select Normal.
Enter a comment in the Comment box, as necessary.
3 Click OK.
A new schedule is created, and opens in the Sample Table Editor.
• Enter information in the schedule in the same manner as in the Sample Table.
For details, refer to "5.4 Editing a Sample Table" P.194.
• A sample file can export a schedule file with the same content. For details,
refer to "5.6.7 Exporting a Schedule File" P.251.
For details on opening an existing Sample Table and entering information, refer to "5.4
Editing a Sample Table" P.194, and "5.5 Reviewing and Editing Measurement Data"
P.222.
An existing calibration curve can be viewed and edited by opening the Calibration Curve
Properties window.
The parameters in the Calibration Curve Properties window were entered when the
calibration curve was generated. For details regarding these items, refer to "5.3.2 Creating
a Calibration Curve File" P.147.
Procedure
1 Display the Calibration Curve tab in the file viewer, and double-click the
calibration curve to view the detailed information.
The Calibration Curve Properties window is displayed.
The Calibration Curve Properties window can also be displayed by selecting the row of the
Sample Table that contains the calibration curve, and then selecting View - Measurement
Settings.
Item Description
System Displays the system used for analysis and cannot be edited.
Displays the name of the user who created the file and cannot be
User
edited.
Date of Creation Displays the current date and time and cannot be edited.
Comment Enter a comment using up to 512 single-byte characters.
Opens the Print dialog box. Make the necessary print settings, and
Print
then print the contents of the Calibration Curve Properties Window.
Item Description
Analysis Displays the analysis type.
Displays the measurement status of the calibration curve. If
Measured is displayed, most of the Calibration Curve Properties can
be edited.
Status • Defined: not measured
• Completed: measured
• Aborted: measurement cancelled in progress
Units Displays the concentration unit.
Sample Name Displays the sample name.
Sample ID Displays the sample ID.
No. of Cal. Points Displays the number of calibration points and cannot be edited.
Calculation Method Displays the calculation method.
Zero Shift Displays the Zero Shift selection.
Multiple Injections Displays the selection for Multiple Injections.
Displays the file name and directory folder. This item cannot be
Calibration Curve File
edited.
Item Description
Displays the number of times (1 – 10) the flow line will be washed
No. Washes
before the first analysis injection. 5
Acid Add Displays the percentage of acid to be added to the sample.
If this item is selected, the software default values are used for peak
Use default settings detection and the Min. integration time and Max. integration items
are disabled.
Enter the minimum time the instrument signal will continue to be
Min. integration time
detected.
Enter the maximum time the instrument signal will be detected
Max. integration
when no peak is found.
If this item is selected, the calibration curve error judgment is based
on the correlation coefficient. When this item is selected, Failure
Correlation Coeff. Action (1st time), Failure Action (2nd time) and Lower limit items
Check are also activated.
If the calibration curve contains less than 3 calibration points, error
judgement is not possible, and this option will have no effect.
Displays the process to be conducted if an error occurs.
• Continue
Records the error in the Sample Table, and allows analysis to
continue.
Failure Action (1st
time) • Stop
Records the error in the Sample Table, and stops analysis.
• Repeat
Records the error in the Sample Table, and re-analyzes the
calibration curve.
Item Description
Displays the process to be conducted if a second error occurs.
• Continue
Failure Action (2nd Records the error in the Sample Table, and allows analysis to
time) continue.
• Stop
Records the error in the Sample Table, and stops analysis.
Enter the minimum correlation coefficient value. If the calculated
Lower Limit correlation coefficient is less than the value entered, an error is
assessed.
Item Description 5
Auto. Dilution Displays the automatic dilution factor.
Injection Volume Displays the calculated injection volume.
Calibration points list Displays the information associated with each calibration point.
Displays the Edit Calibration Point Parameters dialog box to allow
Edit
editing of the selected calibration point parameters.
Displays the Edit Calibration Point Parameters dialog box to allow
Add addition of a new calibration point. Select the position the point
will be added by selecting the calibration number.
Delete Deletes the selected calibration point.
Delete All Deletes all of the calibration points in the Calibration Points List.
Exclude the selected calibration point from the analysis results. This
Exclude function is enabled only if the Status in the Parameter tab is
Completed.
Item Description
Slope / Intercept / Displays the slope, y-intercept and coefficient of determination,
r^2 / r / RSE(%) correlation coefficient values and RSE (Relative Standard Error).
Item Description
Displays the Print screen. You can edit the settings and print out
History
the information on the History screen.
3 After reviewing and editing the calibration curve properties, click OK.
The changes are saved, and the window closes.
Procedure
1 Display the Method tab in the file viewer, and double-click the method to view
the detailed information.
The Sample/Method Properties window is displayed.
Item Description
System Displays the system used for analysis and cannot be edited.
Displays the name of the user who created the file and cannot be
User
edited.
Date of Creation Displays the current date and time and cannot be edited.
Comment Enter a comment using up to 512 single-byte characters.
Opens the Print dialog box. Make the necessary print settings, and
Print
then print the contents of the Sample/Method Properties window.
Item Description
Displays the type of analysis. "TOC" indicates TOC measurement
Analysis
using TC-IC. 5
Status Displays the measurement status of the method file.
Displays the dilution factor that was entered when the method was
Manual Dilution
created.
Sample Name Displays the sample name.
Sample ID Displays the sample ID.
No. of
Displays the number of injections for each sample.
Determinations
Configure the settings related to the acceptance of measurement
values when using pharmaceutical water control.
• None: Do not test measurement values.
• USP/EP system suitability test: Test whether measurement values
conform to the USP (United States Pharmacopeia) / EP (European
Pharmacopoeia) system suitability test standards.
Pharmaceutical water
testing • USP/EP TOC test: Test whether measurement values conform to the
USP (United States Pharmacopeia) / EP (European Pharmacopoeia)
pharmaceutical water test standards.
• JP recovery rate test: Test whether measurement values conform
to the JP (Japanese Pharmacopoeia) resolvability test standards.
• JP TOC test: Test whether measurement values conform to the JP
(Japanese Pharmacopoeia) pharmaceutical water test standards.
Displays the method file name and storage location. This item
Current Method
cannot be edited.
When performing pharmaceutical water testing, set the injection volume and
automatic dilution factor to the same values as the calibration curve used for
calculating concentration.
Do not set multiple calibration curves to use in calculating concentration or select
the [Auto. Correction of inj. Vol. and dilution] checkbox. Doing so may change
the injection volume and automatic dilution factor.
Item Description
Units Displays the concentration unit.
Displays the number of injections (1 – 20). The left box indicates the
No. of Injections number of analysis injections and the right box indicates the
maximum number of injections.
No. of Washes Displays the number of flow line washes.
Displays the standard deviation (SD) limit (0.0 – 9999). used to assess
SD Max.
the analysis result.
Item Description
Displays the coefficient of variation (CV) limit (0.0 – 100) used to
CV Max.
assess the analysis result.
Acid Addition Displays the percentage of acid added to the sample.
Enter the sparge gas flow rate (50 – 200). Normally, a flow rate of
Sparge Gas Flow
80 to 100 mL/min is appropriate.
Sparge Time Displays the sparge time.
Displays whether or not the software default values will be used for
Use default settings
the peak detection time.
Displays the time allowed for signal detection from the instrument
Min. integration time
to continue.
Displays the time at which signal detection from the instrument will
Max. integration
stop.
If this item is selected, multiple injections are made from a single
aliquot of standard solution. This larger standard aliquot is drawn
Multiple Injections
in the syringe in one aspiration and is sufficient to accommodate all
of the repeat injections.
Auto. Dilution Displays the automatic dilution factor.
Injection Volume Displays the injection volume.
Expected Conc. Range Displays the expected concentration.
Use area retrieved If selected, the bank analysis value is subtracted from the analysis
from the blank check result.
Calibration Curve 1,
Calibration Curve 2,
Displays the file names of the calibration curves incorporated in the 5
method, and the project name under which they are stored.
Calibration Curve 3
If selected, the instrument will automatically adjust the injection
Correction of inj. Vol volume and conduct re-analysis when the measurement result
exceeds the calibration curve range.
If selected, the instrument will automatically adjust the dilution
Correction of dilution factor and conduct re-analysis when the measurement result exceeds
the calibration curve range.
Item Description
Displays the Print screen. You can edit the settings and print out
Print
the information on the History screen.
The control sample information also accessed through the Sample/Method Properties
window. The Sample/Method Properties window displays the same information as was
accessed in the method with one addition, a Control Parameters tab devoted exclusively
to Control Sample information.
The control sample parameters in the Sample/Method Properties window were entered
when the control sample was created. For details regarding these items, refer to "5.3.4
Creating a Control Sample File" P.166.
Procedure
1 Display the Control Sample tab in the file viewer, and double-click the control
sample to view the detailed information.
The Sample/Method Properties window is displayed.
Click the Sample Table row where the control sample is inserted, and click View –
Measurement Parameters to display the Sample/Method Properties window.
2 Click on the Control Parameters tab view and edit the control sample parameters.
Item Description
Control Sample / The selected radio button indicates the type of control sample used
Control Chart Sample in measurement.
Control Checking Selected radio buttons indicate the type of control sample
Type evaluation that will be conducted.
Original
Displays the concentration of the original control sample.
Concentration
Spiked Concentration Displays the concentration of the of the spiked control sample.
Displays the upper limit of the allowed concentration deviation in
Max. Dev.
span width determination.
Low Lmt. Displays the lower acceptable limit.
Up. Lmt. Displays the upper acceptable limit.
Control Chart Displays the file name and path of the referenced control chart file.
Ignore Zero Shift of
If selected, this item allows the calibration curve shift to the zero
Cal. Curve in Conc.
point to be ignored when calculating the concentration.
Calculation
Item Description
Action when the
failure event occurs
the first time / Action Read-only display of the measures to be taken if the control sample
when the failure exceeds any of the limit values.
event occurs the
second time
For details regarding tabs other than the Control Parameters tab, refer to "5.3.8 Reviewing
and Editing a Method" P.183.
The schedule file is accessed in the same manner as the Sample Table. For details, refer
to "5.4 Editing a Sample Table" P.194, and "5.5 Reviewing and Editing Measurement
Data" P.222.
Procedure
1 Click the file view tabs to switch to the desired file category.
Procedure
Procedure
Calibration curve files are displayed as Standard when they are inserted into the
sample table.
Procedure
2 Select the calibration curve file, and drag it into position in the sample table.
If the row above the insertion position is empty, the row is filled with the new
content.
Procedure
1 Right-click in the left cell of the row where the calibration curve is to be inserted.
The Open dialog box can also be displayed by selecting Insert – Calibration Curve from the
menu bar.
Method files are displayed as Unknown when they are inserted into the sample
table.
Unknown samples can also be added to the sample table by clicking a calibration curve
file from the file viewer and while pressing the SHIFT key, dragging the calibration curve
into the sample table.
Procedure
2 Select the file, and drag it into position in the sample table.
If the row above the insertion position is empty, it is filled with the new content.
Procedure
1 Right-click in the left cell of the row where the sample is to be inserted.
The Sample Wizard (Page 1) Parameter Source page can also be displayed by selecting Insert
– Sample from the menu bar.
Item Description
• Method 5
Analysis parameters are from an existing method file. Click
to display the Open dialog box, and select the method file to use.
Skip remaining
wizard pages and use Select this item to skip the remaining Wizard pages. A Finish button
measurement is displayed at the bottom of the page. Click it to save the control
parameters from the sample file.
source
4 Click Next.
The Sample Wizard (Page 2) Analysis Information page is displayed.
Item Description
Analysis Select the analysis type from the list.
Default Sample Name Enter a sample name using up to 64 single-byte characters.
Default Sample ID Enter a sample ID using up to 64 single-byte characters.
Enter the sample preparation dilution factor if the sample was
Manual Dilution diluted manually. The entered value will be used in the
concentration calculation. The default value is 1.
No. of
Enter the number of times each sample is to be injected.
Determinations
6 Click Next.
The Sample Wizard (Page 3) Calibration Curve page is displayed.
Up to 3 calibration curve files can be assigned to the sample. If multiple calibration curves
are assigned, the software selects the optimum curve.
Item Description
5
Displays the type of analysis selected in Sample Wizard (Page 2)
Analysis
Analysis Information.
8 Click Next.
The Sample Wizard (Page 4) Injection Parameters page is displayed.
Item Description
Displays the analysis type selected in Sample Wizard (Page 2)
Analysis
Analysis Information.
Units Select the concentration unit from ppm, ppb, mg/L, µg/L, no unit.
Injection Volume The injection volume is automatically entered.
Enter the expected concentration value if one is known. This item
is not required. A range value is automatically entered based on the
Expected Conc. Range
calibration curve selected on Method Wizard (Page 3) Calibration
Curves.
Select the number of injections (1 – 20). The left box indicates the
number of analysis injections and the right box indicates the
maximum number of injections. The result is calculated using the
mean value of the total number of analysis injections.
No. of Injections
If the resulting value exceeds the SD Max. and CV Max. limits,
additional injections are performed for confirmation. The maximum
number of injections includes the analysis injections and the
additional injections.
Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used
to assess the analysis result. This parameter is activated if the No.
SD Max.
of Injections setting has a larger maximum number of injections than
the number of analysis injections.
Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is
used to assess the analysis result. This parameter is activated if the
CV Max.
No. of Injections setting has a larger maximum number of injections
than the number of analysis injections.
Enter the number of times (1 – 10) the flow line will be washed
No. of Washes
before the first analysis injection.
Item Description
Auto. Dilution Enter the sample dilution factor.
Enter the sparge gas flow rate (50 – 200). Normally, a flow rate of
Sparge Gas Flow
80 to 100 mL/min is appropriate.
Sparge Time Enter the sparging time (0 – 20).
Acid Addition Enter the percentage (0 – 20) of acid to be added to the sample.
If this item is selected, multiple injections are made from a single
Multiple Injections aliquot. This larger aliquot is drawn in the syringe in one aspiration
and is sufficient to accommodate all of the repeat injections.
If selected, the blank analysis value is subtracted from the analysis
Use blank check area
result.
If selected, the instrument will automatically adjust the injection
Correction of inj. Vol volume and conduct re-analysis when the measurement result
exceeds the calibration curve range.
If selected, the instrument will automatically adjust the dilution
Correction of dilution factor and conduct re-analysis when the measurement result exceeds
the calibration curve range.
10 Click Next.
The Sample Wizard (Page 5) Peak Time Parameters page is displayed.
Item Description
Displays the analysis type selected in Sample Wizard (Page 2)
Analysis
Analysis Information.
Item Description
If this item is selected, the software default values are used for peak
Use default settings detection and the Min. integration time and Max. integration items
are disabled.
Enter the minimum time the instrument signal will continue to be
Min. integration time
detected.
Enter the maximum time the instrument signal will be detected
Max. integration
when no peak is found.
12 Click Finish.
The sample is inserted into the sample table.
Procedure
2 Select the file, and drag it into position in the sample table.
If there is an empty row above the insertion position, it is filled with the new
content.
Procedure
1 Right-click in the left cell of the row where the control sample will be inserted.
The Open dialog box can also be displayed by selecting Insert – Control Sample from the
menu bar.
Multiple samples are inserted into the sample table as a group by selecting an existing
or new method. Calibration curves and control samples may also be inserted.
This procedure may be performed during analysis while reviewing analysis accuracy.
Procedure
1 Right-click in the left cell in the row where multiple samples are to be inserted.
The Open dialog box can also be displayed by selecting Insert – Multiple Samples from the
menu bar.
Item Description
• Method
The analysis parameters of an existing method file are used to
5
create the samples. Click to display the Open dialog box,
and select the method file to use.
Parameter source
• Calibration Curve
The analysis parameters of an existing calibration curve file are
used to create the samples. Click to display the Open dialog
box, and select the calibration curve file to use.
4 Click Next.
The Sample Group Wizard (Page 2) Sample Parameter page is displayed.
Item Description
No. of Samples Enter the number of samples (1 – 100) to be inserted in the group.
Enter the number of the first vial to be sampled. This number is
entered into the Vial column in the sample table. The subsequent
vial numbers are entered automatically.
Start Vial
Example: If 1 is entered, and No. of Samples is 5, the series of
numbers 1 – 5 is entered into the vial column. This field is disabled
if the system does not contain an ASI-L.
Sample Name / Enter the sample name and sample ID using up to 64 single-byte
Sample ID characters.
Select this option to append the sample names and Sample IDs with
Index Start sequential numbers. Enter a desired starting number in the field at
right.
Insert Control
Select this option to insert control samples along with the samples.
Samples
Item Description
At the beginning of
the sample group
Select this item to insert a control sample before sample
measurement.
5
Always, after Select this item to insert a control sample after every fixed number
"number" Samples of samples. Enter that number in the box.
At the end of the Select this item to insert a control sample at the and of the sample
sample group measurements.
Displays the information related to the added control samples. Up
Control Templates
to three separate Control Samples may be added.
Displays the Open dialog box. Select the control sample and click
Add
Open to add the control sample to the control sample list.
Delete Deletes a selected control sample.
8 Click Finish.
The group of samples are inserted into the sample table.
Procedure
2 Select the file, and drag it into position in the sample table.
If there is an empty row above the insertion position, it is filled with the new
content.
Procedure
1 Select the row of the sample table where the schedule content is to be added.
After inserting the samples in the sample table, the vial numbers of vials to be sampled
in the ASI-L must be associated with the samples.
If the system does not contain an ASI-L, this item is not displayed.
Procedure
The Vial Settings dialog box can also be displayed by selecting View – Vial Settings from
the menu bar.
Item Description
The sample table displays the row, sample name and attribute of
the inserted samples. Content in the Row, Sample Name and
Attribute columns cannot be edited.
Enter the number of the vial to be sampled in the Vial column.
Table Refer to "Entering Vial Numbers" P.212 for the methods for
entering numbers in the Vial column.
The Ex. 1, Ex. 2 and Ex. 3 columns are used to enter vials numbers
for re-analysis of samples. These vials are used if the control sample
results exceed the set limits and are not mandatory.
Item Description
Designated vials are marked blue. If the total injection volume
exceeds the capacity the vial is marked red. If the cursor is
positioned over a vial in the drawing, the vial number is displayed.
Vial arrangement
The arrangement drawing differs depending on the ASI-L type and
connection condition. Refer to "Vial Arrangement Drawing Types"
P.213.
Move the mouse pointer over a vial icon and click to display the
Vial vial's number.
is displayed if the total injection volume exceeds the vial capacity.
Displays the amount of sample required for the vial displayed in the
Required
above Vial field.
Select a cell in the Vial, Ex. 1, Ex. 2, or Ex. 3 columns, and enter a
Off-Line "0" to conduct sampling from the sampling tube on the left side
of the instrument.
Procedure
Dragging while holding down the Ctrl key, will enter numbers identical to that in the
original cell.
Procedure
ASI-L
5
These images are dependant on the number of vials and vial type.
Standard solutions and samples inserted into the sample table are referred to as
"sample". The sample analysis parameters are the same as those in the calibration curve
and method files. Sample information can be edited individually in the sample table.
Dragging while holding down the Ctrl key, will enter numbers identical to that in the
original cell.
Dragging while holding down the Ctrl key, will enter numbers identical to that in the 5
original cell.
Using Double-Click
Procedure
The properties window can also be displayed by clicking the left cell of the sample row,
and then selecting View – Measurement Settings.
By Clicking Button
Procedure
2 Click .
Procedure
Copy, Cut and Paste operations can be performed with data in a selected cell in the
sample table.
• Copy
Copies a selected cell or sample data from the sample table and saves it to the 5
clipboard.
• Cut
Deletes a selected cell or sample data from the sample table and saves it to the
clipboard.
• Paste
Pastes content that is saved in the clipboard into the sample table.
Procedure
Valid cells include cells in the Sample Name, Sample ID or Comment columns
(cells in which keyboard entry is possible).
When a measured sample is cut, the measured data is deleted. Be careful when
cutting data, because the deleted data cannot be restored.
Procedure
5
3 Select the row where the data is to be pasted.
If there is already data in the paste destination row, the data is shifted down
to allow the data to be pasted into the selected row.
Use caution when deleting data, once deleted sample data cannot be restored.
Procedure
Comments can be added by displaying the File Information dialog box for the opened
sample table or schedule.
Procedure
The Sample Window displays the data associated with each analysis injection. The
injection peaks and detailed information can be displayed. If this window is open during
analysis, real-time peak verification is possible.
Procedure
1 Click .
The Sample Window can also be displayed by selecting View – Sample Window.
Item Description
Set the graph format to Current Peak, All Peaks, or Cal. Curve.
Select the sample (row) for display from the sample table.
• Sample number/Row number: Select a sample to display.
The boundary lines of the Peak Profile, Sample Information List and Injection Table can be
dragged to change the size of the segments as desired.
Operating Procedure
• Using the / buttons:
Click the and buttons on the vertical or horizontal axes on the graph.
Each click either enlarges or reduces the size of the corresponding axis display.
Click or and then select and click the full scale for modification.
The full scale of the corresponding axis becomes the selected value.
• Enlarging part of the graph:
Drag out the range on the graph to enlarge.
The dragged out range is enlarged.
2 Click Manual.
The Graph Limits window is displayed.
Item Description
X axis (Min. / Max.) Enter the minimum and maximum values for the X axis range.
Y-axis (Min. / Max.) Enter the minimum and maximum values for the Y axis range.
Click this to return the graph display to the default parameters, and
Cancel
close the dialog box.
Full Scale
Use the following procedure to adjust the graph scale to enlarge the largest peak to
full scale.
Procedure
Auto Adjust
The graphic display range can be automatically adjusted to fully accommodate the peak
shape. This adjustment may be made in three ways, X axis only, Y axis only or both X
and Y axes.
Procedure
Default
If the graph display has been changed, it can be returned to the default range with
the following procedure.
Procedure
Double-clicking anywhere on the graph will also return to the default display parameters.
n Copy to Clipboard
The graph can be copied to the clipboard. The copied graph can then be used by pasting
it into another software application.
Procedure
Open the properties window to edit the analysis parameters of a measured sample.
Depending on the sample Type designation, different types of properties windows are
displayed.
• Standard
Displays Calibration Curve Properties window. Refer to "5.3.7 Reviewing and Editing a
Calibration Curve" P.176.
• Unknown
Displays Sample / Method Properties window. Refer to "5.3.8 Reviewing and Editing a
Method" P.183.
• Control
Displays Control Sample Properties window. Refer to "5.3.9 Reviewing and Editing a
Control Sample" P.188.
Using Double-Click
Procedure
The properties window can also be displayed by clicking the left cell of the sample row,
and then selecting View – Measurement Settings.
Procedure
2 Click .
Procedure
Open the sample window to access the information related to the calibration curve.
Procedure
1 Right-click on the left cell of the injection table row that contains the calibration
curve.
The Calibration Curve Properties window is displayed. refer to "5.3.7 Reviewing and
Editing a Calibration Curve" P.176 for details regarding the Calibration Curve Properties
window.
The calibration curve file associated with the unknown sample or control sample can be
edited.
Procedure
1 Select the sample table row that is associated with the calibration curve you
wish to view.
Multiple contiguous samples can be selected by selecting the first sample, and holding down
on the Shift key, selecting the last sample in the range. These samples and all of the
samples in between are selected.
Additional samples can be added to those already selected by holding down the Ctrl key
and selecting the sample to be added.
Item Description
Select a tab to view the calibration curve for each tab.
Tab The number of tabs displayed depends on the Analysis Type. In the
above example, the Analysis Type is TC.
If the check mark is omitted, the new calibration curve will not be reflected in
the concentration calculation. 5
4 Click OK.
The changes are saved, and the dialog box closes.
1 In the sample table, right-click the leftmost cell (number) of the row of the
unknown sample or control sample that you want to display the calibration curve
for.
5 Click OK.
The settings are saved, and the concentration is automatically recalculated based on the
new calibration curve information.
If multiple injections are used in the analysis, specific injections can be excluded.
The exclusion can be cancelled and the injection again, included in the concentration
calculation.
Procedure
1 In the Sample Window, right-click on the left cell of the injection table row that
includes the injection to be excluded.
The exclusion confirmation box can also be displayed by selecting the relevant row, and
clicking Edit – Exclude/Include Injections.
3 Click Yes.
The selected injection result is excluded.
Remove the exclusion by performing the procedure again.
After changing the calibration curve or the shift to zero parameter, the analysis results
can be recalculated. Recalculation can include all of the analysis results in the sample
table, or only a selected few.
Procedure
2 Click Yes.
All of the results in the sample table are recalculated.
Procedure
Multiple contiguous samples can be selected by selecting the first sample, and while holding
down the Shift key, selecting the last sample in the range. These samples and all of the
samples in between are selected.
Additional samples can be added to those already selected by holding down the Ctrl key
and clicking on the sample to be added.
3 Click Yes.
The selected results are recalculated.
The analysis results in the sample table can be returned to the unmeasured state. Clearing
of results can be applied to all of the results in the sample table, or only a selected few.
2 Click Yes.
All of the results in the sample table are cleared.
Procedure 5
1 Select the sample that you wish to clear. To select a sample, click the left cell
of the sample row.
Multiple contiguous samples can be selected by selecting the first sample and while holding
down the Shift key, selecting the last sample in the range. These samples and all of the
samples in between are selected.
Additional samples can be added to those already selected by holding down the Ctrl key
and clicking on the samples to be added.
3 Click Yes.
The selected analysis results are cleared.
Items such as page margins can be specified when printing a sample report.
Procedure
2 Select the Instrument, Calibrations and Samples tabs to change the content
selection pages, and select the items to be printed. These pages are described
below.
• Instrument tab
Item Description
Select this option to print the selected items in the sample report.
Print system
information
Items selected in the frame below are not printed unless this item 5
is selected.
Press this button to display a preview of the sample report. Refer
Preview
to "Sample Report Preview" P.241.
Select All All items in the frame are selected.
Select None All items in the frame are deselected.
Default Default system items are selected.
• Calibrations tab
• Samples tab
3 Click the Graph tab to change the peak profile print options.
Item Description
Black & White Select this item to print the report in black and white.
Enter the scale of the peak profile. The X axis and Y axis values are
entered separately.
5
Chart scale settings
• Auto: Allows the software to set suitable scale values.
• Manual: The scale is the value in the box relative to the zero point.
Press this button to display a preview of the sample report. Refer
Preview
to "Sample Report Preview" P.241.
Select this item to reset all of the Graph tab items to the default
Default
values.
Item Description
Margin parameters Enter the print margins in these boxes.
5 Click OK.
The changes are saved, and the dialog box closes.
Use this function to select the printer parameters for the selected printer. Print setup
options differ depending on the type printer, refer to the printer instruction manual for
specific details.
Procedure
Print Preview allows for on screen verification of the report content before actually
printing the report. The 3 print preview modes are described below.
• Sample Table
Previews all content in the sample table in a table format similar to that displayed on
the screen.
• Sample Report (All)
Previews all content in the sample table in a detailed report format.
• Sample Report (Highlighted)
Previews selected content in the sample table in a detailed report format.
Procedure
1 Click .
The preview can also be displayed by selecting File - Print Preview - Sample Table.
Item Description
Displays the Print dialog box. If there are no problems with the
Print
preview, make the necessary settings and print the report.
Displays the next page of the report. This button is disabled when
Next Page
viewing the last page of the report.
Displays the previous page of the report. This button is disabled
Prev Page
when viewing the first page of the report.
Item Description
Displays two pages, side by side on 1 screen. When in the Two Page
Two Page view, this button is displayed as One Page, and returns the display
to one page per screen.
Increases the magnification of the displayed page. There are three
Zoom In
levels of Zoom In.
Decreases the magnification of the displayed page. There are three
Zoom Out
levels of Zoom Out.
Close Closes the print preview window.
All
Procedure
1 Click .
The preview can also be displayed by selecting File – Print Preview – Sample Report - All.
The operations available while displaying this are the same as those described in "Sample
Table Preview" P.240.
Highlighted
Procedure
Multiple contiguous samples can be selected by selecting the first sample and while holding
down the Shift key, selecting the last sample in the range. These samples and all of the
samples in between are selected.
Additional samples can be added to those already selected by holding down the Ctrl key
and clicking on the samples to be added.
2 Click .
The preview can also be displayed by selecting File – Print Preview – Sample Report -
Highlighted.
5.6.4 Printing
The sample table content can be printed using any of the following procedures.
• Sample Table
Prints the content of the sample table in a table format similar to that displayed on
the screen.
• Sample Report (All)
Prints the content of the sample table in a detailed report format. 5
• Sample Report (Highlighted)
Prints the selected content of the sample table in a detailed report format.
n Sample Table
The contents of a sample report can be selected prior to printing. Refer to "5.6.1 Selecting
Content to Print" P.234.
Procedure
1 Click .
The sample table can also be printed by selecting File - Print - Sample Table.
n Sample Report
All
1 Click .
The entire sample report can also be printed by selecting File - Print - Sample Report - All.
Highlighted
Procedure
Multiple contiguous samples can be selected by selecting the first sample in a range, and
while holding down the Shift key selecting the last sample in the range. These samples
and all of the samples in between are selected.
Additional samples may be added to those already selected by holding down the Ctrl key
and clicking on the sample to be added.
2 Click .
4 Make any necessary changes and print the sample report selections.
The sample report selections can also be printed by selecting File - Print - Sample Report -
Highlighted.
Before data can be exported in ASCII format, the items to be output to the file must
first be selected. Either of the following two types of output methods can be used.
Refer to "5.6.6 Exporting to ASCII Format" P.249 for more information on the ASCII Export
procedure.
• Normal:
Output the measurement results for each analysis type in ASCII format. While this
method cannot output data for individual injections, normal output data is ideal for
use and manipulation in spreadsheet software.
• Detail:
Output the measurement results for each analysis type as well as data for individual
injections of each measurement in ASCII format.
Operating Procedure
2 Select the Header, System and Data tabs to switch between the content selection
pages, and select all of the items to be exported in ASCII format.
• Header tab
Item Description
Export header Select this option to export the selected items. The items selected
information in the frame below are not exported unless this item is selected.
5
Select All Selects all items in the frame.
Select None Deselects all items in the frame.
Default Selects only the software default items.
• System tab
• Data tab
3 Click the Misc. tab to enter the other export option parameters such as the
separator type and whether to use quotation marks.
• Misc tab display
Item Description 5
Select the character that will separate items in the text file. This
Separator character separates the items that reside in adjacent sample table
cells. Select from among Tabulator, Comma, Semicolon, and Space.
Select this item to enclose text strings inside quotation marks in the
export text file. When selected, numerical data may be read as text.
Export strings in
This may prevent calculations with this data. If a spreadsheet or
quotation marks
other software is used to process the output data, ensure this item
is NOT selected.
4 Click OK.
The changes are saved, and the dialog box closes.
The sample table contents can be exported to an ASCII format text file. Two different
export procedures are described below.
• Normal:
Analysis results are output in ASCII format by analysis type. Although the data cannot
be separated by injection, spreadsheet software can be used to reformat the data.
• Detail:
Analysis results that include the injection data are output in ASCII format by analysis
type.
Procedure
3 Enter a file name and save destination, then click the Save button.
The text file is saved.
The contents of a sample table can be exported as a Schedule file. Loading an exported
Schedule facilitates the analysis setup procedure. The Schedule file can be exported in
either sample table format or text format.
• Sample Table format
The contents may edited as a Sample Table.
• Text format
The sample name, sample ID and method used can be edited with a text editor. Vial
numbers are not noted when the schedule file written to text format.
Procedure
2 Enter the file name and destination path, and click Save.
The file is saved.
Refer to "5.4.5 Inserting a Schedule" P.208 for details on inserting an existing schedule file
into a sample table.
Procedure
This window allows you to check whether the currently configured printer is available
by clicking on Printer Settings.
3 Click OK.
When Enable runtime report is set to Yes, the sample table (corresponding single row
from the sample table) is printed every time a measurement completes.
n Connection
The Sample Table Editor must be connected to the instrument before analysis can be
conducted. Depending on the purpose, select one of the two procedures described below.
To Perform Analysis
Connection is made after opening the sample table to be used for analysis.
Procedure
2 Click .
The sample table editor connects to the instrument and the ready state of the instrument
is shown at the right end of the toolbar.
The icon of the connected instrument in the Sample Table tab of the file viewer also
illuminates.
Procedure
1 Open the Sample Table tab of the file viewer. Right-click the instrument
configuration and select Connect.
n Disconnection
Procedure
The Disconnect box can also be displayed by clicking Instrument – Connect while the
instrument is connected.
2 Click OK.
1 Open the Sample Table tab of the file viewer. Right-click on the instrument
configuration and select Connect.
2 Click OK.
The Background Monitor window is used to check the instrument temperature and signal
intensity. The Background Monitor window can only be displayed while the instrument
is connected. The Background Monitor window can remain open during analysis and
other operations.
Two methods for displaying the Background Monitor window are described below.
Procedure
2 Click .
5
The Background Monitor window is displayed. Click the tabs to select the various content
pages.
The Background Monitor window can also be displayed by clicking Instrument – Background
Monitor while connected to the instrument.
Item Description
• The following screenshot shows the TN tab. This tab is displayed when configuring
settings for TN analysis.
Item Description
TN Reactor Displays the current TN reactor temperature.
Ozone Gas Displays the current supply pressure of the gas for TN ozone.
Enlarges the Y axis scale to 50 times that of the default value. Note
X1 to X50
that the X axis scale does not change.
Displays the signal intensity from the time the Monitor window is
Graph
opened. The display is updated every second.
• The following screenshot shows the ASI tab. This tab is displayed when configuring
settings to use the ASI-L.
Item Description
Enlarges the Y axis scale to 50 times that of the default value. Note
X1 to X50
that the X axis scale does not change.
Displays the signal intensity from the time the Background Monitor
Graph
window is opened. The display is updated every second.
Procedure
1 In the File view and under the Sample Table tab, right-click System Configuration
and click Connect.
Refer to "Connection" P.253 to connect the instrument.
2 Right-click on the instrument configuration in the Sample Table tab of the file
viewer, and select Background Monitor.
1 Open the sample table to be used and place the samples in the ASI-L accordingly.
3 Click .
Analysis can also be started by selecting Instrument – Start Measurement after connection
is established.
4 If the sample table name is not set, the Save as screen appears.
5 Set the vial numbers in the sample table if they are not already configured.
This screen is not displayed if the vial numbers have been configured in the sample table.
To return to the sample table, click Cancel to close the Measurement Start window.
6 Select the processing that will take place after analysis is complete.
Item Description
Keep running After analysis, the system maintains the current status.
Shut down
After analysis, the instrument is turned off.
instrument
After analysis, the instrument enters the sleep state. The instrument
Sleep restarts automatically at the specified time. Enter the date and time 5
for the instrument to restart in the Auto Restart boxes.
If the Sleep option is selected, set the units to leave running while
Extra Settings the instrument is sleeping. Select the units to remain on even during
the sleep state.
7 Click Start.
Analysis starts. When measurement is complete, the results are displayed in the sample
table, and analysis ends.
Procedure
1 Open the sample table to be used for analysis, and place the sample in the
instrument.
3 Click .
Analysis can also be started by selecting Instrument – Start Measurement after connection
is established.
4 If the sample table name is not set, the Save as screen appears.
Item Description
Measurement stops after a single sample measurement and the
measurement results are displayed. If the analysis type is a
compound type, such as TOC (which is a combination of TC and IC),
measurement stops after each type of analysis and the measurement
Single Measurement
results are displayed.
If the Continuous Measurement checkbox is selected, measurement
continues regardless of analysis type when processing compound
types, such as TOC (which is a combination of TC and IC).
Batch Measurement All samples in the sample table are measured without stopping.
6 Click OK.
The TOC Measurement window is displayed.
5
7 Click Start.
To return to the sample table, click Stop to close the TOC Measurement window.
8 The results are displayed in the window after the measurement is complete.
Item Description
Results display list Displays the analysis results for each injection.
Select an injection result in the list and click the Exclude button.
Exclude If the result is not currently excluded, it will be excluded, and if the
result is currently excluded, the exclude setting is cancelled.
Repeat This repeats the same analysis once more.
Next Starts the next analysis.
Stop Stops analysis and closes the window.
After all of the samples are complete, the results are displayed in the sample table, and
analysis ends.
n Continuous Analysis
Procedure
1 Open the sample table to be used for analysis, and place the sample in the
instrument.
3 Click .
Analysis can also be started by selecting Instrument – Start Measurement after connection
is established.
5 Click OK.
The Measurement Start window is displayed.
6 Select the processing that will take place after analysis is complete.
Item Description
Keep running After analysis, the system maintains the current status.
Shut down
After analysis, the instrument is turned off.
instrument
After analysis, the instrument enters the sleep state. The instrument
Sleep restarts automatically at the specified time. Enter the date and time
for the instrument to restart in the Auto Restart boxes.
If the Sleep option is selected, set the units to leave running while
Extra Settings the instrument is sleeping. Select the units to remain ON even
during the sleep state.
To return to the sample table, click Cancel to close the Measurement Start window.
7 Click Start.
Analysis starts.
When measurement is complete, the results are displayed in the sample table, and
analysis ends.
n Peak Stop
This option interrupts processing of the current injection, and analysis proceeds to the
next injection measurement.
This option can also be accessed by clicking Instrument - Stop - Peak Stop.
Procedure
Analysis of the current injection stops and processing continues to the analysis of the
next injection.
This option can also be accessed by clicking Instrument - Stop - Peak Stop. 5
This option stops analysis after all of the scheduled injections of the current sample have
been analyzed.
Procedure
1 Click while analysis is in progress, and then select Stop (after current
sample is completed).
This option can also be accessed by clicking Instrument - Stop - Stop (after current sample
is completed).
Procedure
1 Click while analysis is in progress, and then select Stop (stop all
processes immediately).
This option can also be accessed by clicking Instrument - Stop - Stop (stop all processes
immediately).
The sample table can be edited during analysis by changing to the Edit Mode and
temporarily suspending analysis.
Procedure
3 Click OK.
The Edit Mode is cancelled, and analysis continues.
The Edit Mode can also be cancelled by selecting Instrument - Edit Mode.
n Shutdown
Instrument shutdown processing takes place. The connection to the device is released
when the instrument is shut down, and thus the sample table editor can be closed and
the PC can be turned off.
Procedure
2 Click .
The Shutdown dialog box can also be displayed by selecting Instrument – Shutdown.
4 Click OK.
The furnace is switched off, carrier gas flow is stopped, and 30 minutes later, power to
the instrument is switched off (although the main power remains on).
The instrument can be restarted by holding down the power switch for three seconds during
a shutdown (while the power switch's LED is flashing orange) before the power to the
instrument is switched off.
Procedure
1 In the File view and under the Sample Table tab, right-click System Configuration
and click Connect.
Refer to "Connection" P.253 to connect the instrument.
2 Right-click on the instrument icon in the Sample Table tab of the file viewer,
and select Shutdown.
n Sleep
The instrument can be put in the sleep state with a restart setting to enable
measurement at a set date and time. The instrument will automatically wake from the
sleep state about one hour prior to the set time to allow use at the set time.
After sleep processing has been set and the connection between the PC and the
instrument is released, the power of the PC can be turned off.
The two methods for implementing the Sleep status are described below.
5
From an Open Sample Table
Procedure
2 Click .
The Shutdown dialog box can also be displayed by selecting Instrument – Shutdown.
3 Select Sleep.
4 If any units should remain on during the sleep state, click Extra Settings and
select the checkboxes corresponding to each unit name. Normally, checkboxes do
not need to be selected.
The instrument can be brought out of the Sleep state by clicking End Sleep mode.
6 Click OK.
The power of the instrument will automatically turn off. About one hour before the set
time, the power will turn on and analysis preparation will begin.
Procedure
2 Right-click on the instrument icon in the Sample Table tab of the file viewer,
and select Shutdown.
When a carrier gas purification kit is used, if the power switch is turned OFF or
the instrument is shut down or put into the sleep state, an air hissing sound
may be heard from the inside of the instrument at the time of carrier gas
stopping. This is the sound of releasing residual pressure of carrier gas from
within the CO2 absorber and is normal.
Procedure
1 Click New on the Sample Table tab in the file viewer or New on the tool bar.
2 Click the System drop down menu and select the system configuration to use.
3 Click the Table Type drop down menu and select Validation.
Note that validation cannot be performed if the manual injection kit options are
set in the selected system configuration.
4 Click OK.
The Validation Settings window is displayed.
Selecting the checkboxes of the items to validate and clicking OK automatically creates
a sample table configured with the necessary measurement conditions. Start an analysis
using the normal method of sample measurement.
If using the ASI-L or OCT-L, measurement of the selected items is performed automatically
if measurement is started after setting standard solution according to the conditions
configured in the sample table.
Once measurement is complete, an index for the validation items, such as sensitivity and
linearity, is displayed in the Notes column in the sample table.
Preliminary Measurement
Execute a preliminary measurement by measuring blank water in order to stabilize the
instrument before performing validation or between measurements of each validation
item. The settings related to preliminary measurement can be changed by clicking the
Settings button.
Setting Description
Analysis Select the measurement type.
Number of samples Set the number of samples to measure.
Default Return the settings to their default state.
Sensitivity
The instrument's sensitivity can be verified by measuring blank water and a 30 mg/L
sample and calculating the difference between the two resulting peak areas. The settings
related to this measurement can be changed by clicking the Settings button to open the
following window.
Setting Description
Analysis Select the measurement type.
Default Return the settings to their default state.
The sensitivity index is calculated in the following manner and output to the Notes 5
column in the sample table.
(Mean peak area of the 30 mg/L sample) - (Mean peak area of the blank water)
A sensitivity index greater than 210 for H Type and greater than 130 for N Type is
acceptable.
Sensitivity will vary as the instrument ages and according to the deterioration of
consumable parts. Even if the measurement results are below these values, the
measurement performance will not be adversely affected if the results are stable and the
results of other evaluation items are acceptable.
Setting Description
Analysis Select the measurement type.
Set the span concentration. An intermediate concentration point is
Span
automatically determined based on this value.
Default Return the settings to their default state.
The linearity index is calculated in the following manner and output to the Notes column
in the sample table.
((B - A) - (C - A) / 2) / (C - A) ´ 100(%)
A: Mean peak area of the zero point (blank water)
B: Mean peak area of the intermediate point
C: Mean peak area of the span point
The CV value of the intermediate point is output to the Notes column in the sample
table as the repeatability index.
A linearity of less than ± 2.0 % and a repeatability of less than 1.5 % is acceptable.
Setting Description
Method Select the evaluation method.
Analysis Select the measurement type.
Set the span concentration. When the Verify CV value of target
5
Span conc. is selected, the concentration of Target is automatically
calculated to be 1/10th of Span.
Default Return the settings to their default state.
When Tenfold SD value of blank water is set, the value calculated using the following
method is taken as the instrument's quantitative lower limit and output to the Notes
column in the sample table.
A 2-point calibration curve is derived from the zero point (blank water) and span point
(set concentration) measurement results. The quantitative lower limit value is tenfold that
of the CV value of the concentration calculated from the target (blank water)
measurement result using the calibration curve.
When Verify CV value of target conc. is set, repeatability is evaluated in the following
manner for the set target concentration value and the result is output to the Notes
column in the sample table.
A 2-point calibration curve is derived from the zero point (blank water) and span point
(set concentration) measurement results. The repeatability is the CV value of the
concentration calculated from the target (1/10 of the set concentration) measurement
result using the calibration curve.
The quantitative lower limit is significantly affected by instrument usage. The instrument
is considered to be in an acceptable condition if the quantitative lower limit is less than
30 µg/L when using TOC high sensitivity catalyst for the H Type, and less than 150 µg/L
in all other cases.
Refer to "7 Maintenance" P.317 for specific maintenance procedures on the various
instrument components. Refer to "7.6 Maintenance Menus" P.351 for descriptions of the
Maintenance menus.
The display options for the Sample Table, such as row height, can be changed using the
following procedure.
These options also apply to the schedule table.
Procedure
2 Click the tabs to switch the displayed page, and make any necessary changes to
the display parameters.
• General tab
Item Description
Enter the number of columns (0 – 14) to be displayed counting from
Columns to freeze the left. This number of columns will always be displayed even when
scrolling horizontally. 5
Default row height Enter the default row height (10 – 100) setting.
Show full path for Select this item to display the full filename and path for the file in
"Origin" the Reference Source File column.
Select this item to allow the text in a cell to flow to the next line
Wrap text
without being truncated.
Bold characters for
Select this item to display the column header using bold text.
column headers
This button selects the default settings for all of the items on this
Default
tab.
Item Description
The selected items are displayed as column headers in the sample
table and schedule.
Display Items
If the system does not include an ASI-L, the Vial column is not
displayed even if it is selected.
Select All Selects all of the items in the list.
Select None Deselects all of the items in the list.
Default Selects only the default items in the Display Item List.
Display options for the Sample window, such as row height, can be changed using the
following procedure.
Procedure
2 Click the tabs to switch the pages, and make any necessary changes to the
display settings.
• General tab
Item Description
Enter the number of columns (0 – 15) to be displayed counting from
Columns to freeze the left. This number of columns will always be displayed even when
scrolling horizontally.
Default row height Enter the default row height (10 – 100) setting.
Show full path for Select this item to display the full filename and path for the file in
Cal. Curve the Cal. Curve column.
Item Description
Select this item to allow the text in a cell to flow to the next line
Wrap text
without being truncated.
Bold characters for
Select this item to display the column header using bold text.
column headers
Select this item to ensure that when the Sample Window is opened
Auto fit to viewable it does not overlay the Sample Table.
area • Initial height: Enter an integer (100 – 1000) to set the initial height
of the Sample Window.
This button selects the default settings for all of the items on this
Default
tab.
• Graph tab
Item Description
Use these items to set the X axis and Y axis scales.
• Auto: The appropriate scale is determined by the software.
Chart scale settings
• Manual: The scale is set to range from the zero point to the value 5
entered in the box.
Show Crosshair Select this item to display the cursor point crosshairs.
This button selects the default settings for all of the items on this
Default
tab.
Display options for the File Viewer, such as tab position, can be changed using the
following procedure.
Procedure
Item Description
Select each tab to be displayed in the File Viewer. The Sample Table
Select File Types to
tab is always displayed.
Select whether to display the tabs at the top of the File Viewer or
Tab Position
the bottom.
Procedure
Item Description
• Change the font setting and click OK to validate the change and close the dialog box.
Item Description
Select the font to be used. The available fonts vary according to the
Font
fonts installed.
Select the font style to be used. The available font styles vary
Font style
according to the fonts installed.
Select the font size to be used. The available font sizes vary
Size
according to the fonts installed.
Select the character set and language to be used. The available
Script
character sets vary according to the fonts installed.
3 Make any necessary changes and click OK in the Output Window dialog box.
The changes are saved, and the dialog box is closed.
The File Viewer, Output Window, Toolbar and Status Bar can be hidden or displayed.
Hiding an item is rarely used but can allow a larger display area for the Sample Table.
Procedure
1 Select View.
Remove the check mark to conceal the item(s). Click a hidden item to replace the check
mark, and display the item. 5
The font used in the Sample Table, Schedule and Sample Window can be set as desired.
Procedure
Item Description
Select the font to be used. The available fonts vary according to the
Font
fonts installed.
Select the font style to be used. The available font styles vary
Font style
according to the fonts installed.
Select the font size to be used. The available font sizes vary
Size
according to the fonts installed.
Select the character set and language to be used. The available
Script
character sets vary according to the fonts installed.
The number of decimal places to be used for number display in the Sample Table,
Schedule and Sample Window can be set as appropriate.
Procedure
Item Description
• Number of significant digits: Select this item to set the total
number of digits to be displayed. Enter that number in the box.
Common Floating
Point Numbers • Number of digits after the decimal point: Select this item to set
the total number of digits to be displayed after the decimal point.
Enter that number in the box.
• Number of significant digits: Select this item to set the total
number of digits to be displayed. Enter that number in the box.
Percent Values • Number of digits after the decimal point: Select this item to set
the total number of digits to be displayed after the decimal point.
Enter that number in the box.
5.9.1 Login
Depending on the System Policy settings, the User dialog box is displayed for verification
to use functions of TOC-Control L software. The user is verified by entering the
appropriate User ID and Password into the User dialog box.
Procedure
2 Click OK.
If the User ID and Password are recognized, the user is logged in and gains access to
the software functions.
The Sample Table Editor screen can be locked to protect the data from improper or
malicious operations in the event that the user must temporarily leave the PC during
measurement.
Once locked, the screen can only be unlocked by the user who locked it or by a user
with Release Screen Lock authority. Enter the appropriate User ID and Password to unlock
the Sample Table Editor screen.
Procedure
The Sample Table Editor is locked, and the Re-enter Password window is displayed.
5
3 Click OK.
The window closes, and the lock is released.
Depending on the System Policy settings, the Sample Table Editor locks after a specified
period of inactivity. Release the lock by entering the User ID and Password of either the
user who was logged in when the screen locked or by a user with Release Screen Lock
authority.
Operation Procedure
2 Click OK.
The lock is released, and the window closes.
Comments may be added to the Operation History to record various operations such as
catalyst replacement, that are not automatically recorded by the software.
This function is only available to users who have Add Event Logs authority.
Procedure
3 Click OK.
The history item is added.
The functions described in this documentation represent only a portion of the security
functions. For general information on security features, refer to "LabSolutions DB/CS
Administration [for LabSolutions TOC]".
The default measurement parameters can be changed. The default values can be edited
when the parameters are entered.
Procedure
2 Enter the following items on each of the TC, IC, NPOC, POC and TN tabs.
5
These parameters can only be edited in the SSM-TC tab and SSM-IC tab when
the SSM-5000A is included in the system configuration. For details, refer to the
"SSM-5000A USER'S MANUAL".
Item Description
Units Select the concentration unit from ppm, ppb, mg/L, µg/L, no unit.
Item Description
Select the number of injections (1 – 20). The left box indicates the
number of analysis injection and the right box indicates the
maximum number of injections. The result is calculated using the
mean value of the total number of analysis injections.
No. of Injections
If the resulting value exceeds the SD Max. and CV Max. limits,
additional injections are performed for confirmation. The maximum
number of injections includes the analysis injections and the
additional injections.
Select the number of times (1 – 10) the flow line will be washed
No. of Washes
before the first injection.
Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used
to assess the analysis result. This parameter is activated if the No.
Max SD
of Injections setting has a larger maximum number of injections than
the number of analysis injections.
Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is
used to assess the analysis result. This parameter is activated if the
Max CV
No. of Injections setting has a larger maximum number of injections
than the number of analysis injections.
Conversion can be performed with respect to data from completed measurements using
a set mathematical formula.
Procedure
2 Set the Item to Convert, Item Name, Conversion a, and Conversion b fields.
Setting Description
Item to Convert Select the measurement type of the target for conversion.
Item Name Enter the item name.
Conversion a Enter the X coefficient of the formula.
Conversion b Enter the intercept of the formula. 5
3 Click OK.
This sets the conversion formula, closes the window, and displays the conversion result
in the Result column in the sample table.
The online manual is in PDF format. The Adobe Reader is required to display
this manual.
Two volumes of online manuals are provided with TOC-Control L. The online manual that
contains the same material as this manual is the "TOC-LCPH/CPN". By selecting "TOC-LCPH/
CPN" according to the following operation, the online manual can thereafter be displayed
Procedure
After clicking View Manual, a confirmation window may appear to verify the online manual
to be displayed.
3 Click OK.
The "TOC-LCPH/CPN" manual will now be displayed each time Help – Online Manual is
selected.
The window closes.
Procedure
The following procedure is used to verify the Sample Table Editor version information.
Procedure
n Installation
Procedure
1 Remove the knurled thumbscrew that secures the slider then remove the TC/TN
injector slider.
3 Remove the slider of the IC injector in the same manner and install the IC block
provided with the manual injection kit.
When installing the block, be sure that it is properly aligned with the injection
port.
n System Configuration
Select Manual Injection Kit in the Instrument Setup Wizard Options page during initial
system configuration.
Refer to "5.1.1 Creating a New System Configuration" P.124 for information on creating a
system configuration.
The sample injector syringe will not operate when the Manual Injection Kit item
is selected.
6.1.2 Measurement
• Refer to "5.3.1 Creating a Sample Table" P.146 for information on creating a sample table.
Procedure
3 Drag the created calibration curve from the file viewer into the Sample Table.
Draw in and discharge the sample 3 or 4 times before filling the syringe for
analysis.
7 Enter the injection volume in the Manual Injection Parameter dialog box, and
click Set.
Insert the syringe needle as far as possible into the injection port. Use the same
injection technique such as plunger speed, to ensure that the results are
reproducible.
10 Remove the syringe from the injection port. For TC or TN measurement, close
the injection port valve. The results are displayed after the measurement is
complete.
Click Next to perform more measurements. Repeat the procedure. Click Stop when all of
the measurements are complete.
n Sample Measurement
• Refer to "5.3.1 Creating a Sample Table" P.146 or information on creating a sample table.
Procedure
3 Drag the created method from the file viewer into the Sample Table.
Draw in and discharge the sample 3 or 4 times before filling the syringe for
analysis.
7 Enter the injection volume in the Manual Injection Parameter dialog box, and
click Set.
306 TOC-LCPH/CPN LabSolutions TOC Volume
6.1 Manual Injection Measurement (H Type Only)
9 For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into
the injection port septum.
Insert the syringe needle as far as possible into the injection port. Use the same
injection technique such as plunger speed, to ensure that the results are
reproducible.
10 Remove the syringe from the injection port. For TC or TN measurement, close
the injection port valve. The results are displayed after the measurement is
complete.
Click Next to perform more measurements. Repeat the procedure. Click Stop when all of
the measurements are complete.
The septum used with the IC injection port is a consumable item. The septum is typically
useful for 200 or more injections; however, it should be replaced if reproducibility or
peak shape deterioration is detected.
Part number for replacement cushion O-ring (20 pcs.): P/N S630-01559-01
Replacement Procedure
IC reaction solution may spatter close to the injection port septum and
injection port. This poses no problem during analysis. When replacing the
septum, wipe away any liquid, taking care to avoid contact.
n Gas-Tight Syringe
For analysis, use a needle length of 50 mm, or a 2-inch gas-tight syringe. The following
gas-tight syringes are available from Shimadzu. Order replacement syringes as necessary.
6
Table 6.1 Gas-Tight Syringes (Option)
*1 Set comprises one replacement gas-tight syringe needle and one plunger.
• The sample analysis results are displayed according to the gas concentration used in
calibration. For example, if CO2 is used to generate the calibration curve, the sample
analysis result is displayed based on a conversion using the CO2 gas concentration.
• Gaseous samples have certain properties such as adsorption, condensation and reactivity,
and some gaseous samples are partially liquid or contain a solid component. Depending
on the properties, certain conditions may occur that cannot be ignored. Some of these
conditions are residual substances and contamination in the flow line, which may result
in peak tailing, carryover, baseline fluctuation, or other analytical problems.
• High concentrations of NOx or SOx in the sample or in the post combustion-oxidized
sample can interfere with the NDIR activity. To evaluate the degree of the interference,
combine the analysis of the base gas without the TOC component together with the
sample analysis.
Install the manual injection kit by referring to "6.1 Manual Injection Measurement (H
Type Only)" P.302 and then create a system configuration.
6.2.3 Measurement
n Calibration Curve
Procedure
For IC (carbon dioxide) analysis, prepare a standard gas with a known carbon
dioxide concentration. For TC analysis, another organic gas (for example,
methane) of known concentration can be used.
• Refer to "5.3.1 Creating a Sample Table" P.146 for information on creating a sample table.
6
3 Create a Sample Table.
System
This item is found on the Calibration Curve Wizard (Page 1) System Setup page. Select
the system configuration created in "5.1.1 Creating a New System Configuration" P.124.
4 Drag the created calibration curve from the file viewer into the Sample Table.
Draw in and discharge the sample 3 or 4 times before filling the gas-tight syringe
for analysis.
8 Enter the injection volume in the Manual Injection Parameter dialog box, and
click Set.
10 For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into
the injection port septum.
Insert the syringe needle as far as possible into the injection port. Use the same
injection technique such as plunger speed, to ensure that the results are
reproducible.
11 Remove the syringe from the injection port. For TC or TN measurement, close
the injection port valve. The results are displayed after the measurement is
complete.
Click Next to perform more measurements. Repeat the procedure. Click Stop when all of
the measurements are complete.
n Sample Measurement
• Refer to "5.3.1 Creating a Sample Table" P.146 for information on creating a sample table.
Procedure
3 Drag the created method from the file viewer into the Sample Table.
6
5 Click to start the analysis.
Draw in and discharge the sample 3 or 4 times before filling the gas-tight syringe
for analysis.
7 Enter the injection volume in the Manual Injection Parameter dialog box, and
click Set.
9 For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into
the injection port septum.
Insert the syringe needle as far as possible into the injection port. Use the same
injection technique such as plunger speed, to ensure that the results are
reproducible.
10 Remove the syringe from the injection port. For TC or TN measurement, close
the injection port valve. The results are displayed after the measurement is
complete.
Click Next to perform more measurements. Repeat the procedure. Click Stop when all of
the measurements are complete.
The septum used with the IC injection port is a consumable item. The septum typically
can be used for 200 or more injections; however, it should be replaced if there is
deterioration in reproducibility or peak shapes.
Part number for replacement cushion O-ring (20 pcs.): P/N S630-01559-01
Replacement Procedure
IC reaction solution may spatter close to the injection port septum and
injection port. This poses no problem during analysis. When replacing the
septum, wipe away any liquid, taking care to avoid contact.
n Gas-Tight Syringe
For analysis, use a needle length of 50 mm., or a 2-inch gas-tight syringe. The following
gas-tight syringes are available from Shimadzu. Order replacement syringes as necessary.
6
Table 6.2 Gas-Tight Syringes (Option)
*1 Set comprises one replacement gas-tight syringe needle and one plunger.
Table 6.3 Relationship Between Appropriate Peak Height and (CO2) Gas
Concentration / Injection Volume *1
Verify that the dilution water volume is sufficient for analysis. If necessary, replenish the
dilution water as described in "3.1.8 Preparation of Dilution Water" P.45.
Verify that the acid volume is adequate for analysis. If necessary, replenish the acid as
described in "3.1.9 Acid Preparation" P.46. Any container such as a small-mouth glass 1
liter bottle can be used.
Verify that the water level in the drain vessel on the left side of the instrument is near
the position of the overflow tube on the side of the drain vessel (within 10 mm) before
using the instrument. Replenish as necessary with purified water (ion-exchange water).
Refer to "3.1.6 Water Supply to the Cooler Drain Vessel" P.43 for details on adding purified
water.
Confirm that the carrier gas does not leak from the tip of the drain tubing when the
flow rate is 150 mL/min.
Verify that the water level in the humidifier is above the "Lo" mark. If the level is below
the "Lo" mark, replenish by adding purified water through the water supply port on top
of the vessel. Add water until the level reaches the "Hi" mark.
Check the level of liquid (0.05 mol/L hydrochloric acid) in the B-type halogen scrubber
and amount of remaining stainless mesh before using the instrument, and if necessary,
top up the liquid or replace the stainless mesh.
The liquid level in the B-type halogen scrubber decreases over time when the instrument
is waiting for analysis to start (and the carrier gas is flowing), the sample injection volume
is small, or the interval between analyses is large during analysis. Always check the liquid
level before starting analysis and, if necessary, refill the vessel with 0.05 mol/L
hydrochloric acid (this is important when performing continuous analysis over an
extended period of time using the autosampler). Although the liquid color turns blue or
brown with use, this is normal.
Inorganic substances contained in the samples accumulate in the catalyst as salts and
oxides. Buildup of these residues decreases the sensitivity and reproducibility of analyses.
(Catalyst performance can be checked by measuring a standard solution.) This type of
catalyst contamination occurs when measuring alkaline samples and samples that contain
high concentrations of IC compounds. When catalyst contamination occurs, performance
can be restored by regenerating the catalyst. Catalyst regeneration is also an effective
means of reducing the system blank peaks that are present when using new catalyst or
catalyst that has not been used for a long time. The catalyst regeneration procedure has
little effect on TN analysis.
Catalyst is regenerated by injecting dilute hydrochloric acid onto the catalyst. The acid
used in the procedure is 1 M hydrochloric acid obtained from the instrument reservoir
(acid used during IC and NPOC analysis). The catalyst regeneration process is the same
for both TOC standard catalyst and TOC high sensitivity catalyst. If performance is not
restored after the regeneration process has been conducted, replace the catalyst. Refer
to "7.2.2 Washing or Replacing Catalyst" P.322.
Regeneration Procedure
Perform catalyst regeneration according to the following procedure.
1 Verify that the Ready indicator lights up once the Sample Table Editor connects
to the instrument.
Refer to "Connection" P.253 for the procedure for connecting to the Instrument.
2 Open the Sample Table tab of the file viewer. Right-click on the connected
system configuration icon, and select Maintenance – Regeneration of the TC
Catalyst.
3 Click Start.
The catalyst regeneration process begins. A progress bar is active until the TC catalyst
has been regenerated.
7
4 After the process is complete, click Close.
The window closes.
Dilute hydrochloric acid is the only type of acid that can be used to regenerate
TC catalyst. Other acids, particularly phosphoric acid, cause abnormally high
peaks and scattered peak values to occur. If this happens, the catalyst must
be replaced.
Large quantities of salts accumulate in the catalyst when measuring samples with high
salt concentrations. If sensitivity and reproducibility do not improve after catalyst
regeneration, wash or replace the catalyst. Refer to "7.2.1 Catalyst Regeneration" P.320.
Note that TOC high sensitivity catalyst cannot be washed or reused.
• Allow the electric furnace to cool to room temperature for at least six hours
after switching off the power supply by shutting down the instrument before
performing maintenance on the combustion tube or catalyst. Burns may result
if this task is attempted when the furnace is at a high temperature.
• Combustion tubes are made of quartz glass. Always wear protective leather
gloves when handling combustion tubes to prevent injuries due to breakage.
• Do not use wrenches or other such tools. Doing so could break the
combustion tube and cause injury.
Removal Procedure
1 Open the door on top of the instrument, remove the slider retaining screws
(knurled screws) from the sample injector, and pull the slider towards you and
out of the sample injector.
2 Loosen the hexagon cap nut that joins the carrier gas introduction tubing (PTFE
tubing) to the right side of the sample injector and then remove the tubing.
3 Loosen the hexagon cap nut on the PTFE coupling located on the cooling tubing
inlet at the bottom end of the combustion tube.
4 Loosen the two knurled screws on the sample injector and remove the sample
injector together with the combustion tube in the upward direction.
Washing Catalyst
Standard catalyst can be washed and reused several times using the following procedure.
High sensitivity catalyst cannot be washed and reused.
Procedure
1 Thoroughly wash the catalyst with tap water to remove any accumulated salts.
3 Thoroughly wash the catalyst with tap water to remove the hydrochloric acid.
4 Rinse with pure water (ion exchange water acceptable) and then dry.
• Dry the catalyst at a temperature lower than 700°C to avoid the degradation
of catalyst activity that occurs at higher temperatures.
• A large quantity of steam is produced when the regenerated catalyst is
placed in the oven and heated. Due to the danger of burn injury, leave the
outlet of the combustion tube open until no more steam is released.
Replacing Catalyst
If performance does not improve even after washing the catalyst as described above,
replace the TOC standard catalyst with a new one. For this reason, always have platinum
catalyst on hand as a maintenance consumable. One bottle of platinum catalyst is enough
for one replacement.
Use the following procedure to replace the platinum catalyst.
Procedure
1 Wash the platinum mesh and the inside of the combustion tube with (1:2)
hydrochloric acid (1 part concentrated HCl and 2 parts water).
Disposal of Catalyst
Used catalyst should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the used
catalyst contains platinum.
The carrier gas purification tube burns the carrier gas and oxidizes carbon-based
impurities, converting them to carbon dioxide. The carbon dioxide is absorbed and
eliminated by the CO2 absorber. The carrier gas purification tube is filled with oxidation
catalyst (same as TOC standard catalyst).
The procedure for replacing the purification tube and catalyst is as follows.
Allow the electric furnace to cool to room temperature for at least six hours
after switching off the power supply by shutting down the instrument before
removing the carrier gas purification tube. Burns may result if this task is
attempted when the furnace is at a high temperature.
Removal Procedure
1 Remove the combustion tube together with the TC sample injector from the
electric furnace.
2 Release the swage locks on the top and bottom of the carrier gas purification
tube.
Refer to "3.1.3 Connecting the Combustion Tube" P.26.
3 Extract the carrier gas purification tube from the electric oven by pulling upward.
7
Replacing Catalyst
The top nut of the compression fitting joint is hand-tightened. Do not use
tools to tighten or loosen this nut.
Because the tube is constructed of quartz glass, over-tightening or aggressive
handling may result in damage.
Inhaling quartz wool may cause health impairment. Handle with care. For
details, see "8.9 Safety Data Sheets (SDS)" P.433.
Procedure
1 Remove the catalyst from the carrier gas purification tube through the opening
at the top.
3 Insert a small amount of new TOC standard catalyst into the combustion tube
from the bottom (straight end).
4 Pack a small amount of quartz wool into the tube from the bottom.
The quartz wool is inserted to prevent the catalyst from falling out of the
bottom. Packing too much quartz wool into the tube will greatly impede airflow,
so do not use too much quartz wool. To prevent contamination of the catalyst
or the inclusion of foreign particles, use the same precautions used when filling
the combustion tube with TOC platinum catalyst.
5 Insert the straight end of the carrier gas purification tube down into the front
8 mm diameter hole in the oven.
6 Using the compression fitting joints, restore the tubing connections to their
original condition.
7 Return the combustion tube and the TC sample injector to their original positions
on the electric furnace.
7.2.4 Washing/Replacing the Combustion Tube and Carrier Gas Purification Tube (Option)
The inner surface of the combustion tube devitrifies (becomes crystalline in texture and
turns white) when it reacts with salts contained in the samples. The tube can continue
to be used in this condition until it breaks or cracks.
During the catalyst washing or replacing process, wash the interior of the combustion
tube and carrier gas purification tube with (1:2) hydrochloric acid (1 part concentrated
HCl and 2 parts water) to remove the contaminants and accumulated salts. Rinse with
water, dry, and then reuse the tube(s).
For details on removing the combustion tube, refer to "7.2.2 Washing or Replacing
Catalyst" P.322.
A 47-liter cylinder of high-purity air used as the carrier gas will last for approximately
three months using the H Type instrument, and two months using the N Type.
• Replace the cylinder when the residual pressure diminishes to a few hundred kPa. Do
not wait until it is completely empty.
• When connecting a new cylinder, clean the connections thoroughly. After connecting
the cylinder, do not allow dust or other matter to enter the instrument.
• Keep a spare cylinder available at all times.
Replace the entire CO2 absorber located in the holder on top of the instrument once a
year.
The absorbent inside the halogen scrubber turns black as it absorbs chlorine. The
discoloration band advances toward the outlet as the amount of chlorine absorbed
increases. Replace the scrubber with a new halogen scrubber when the front of the
discoloration band reaches the position shown in "Figure 7.5 Halogen Scrubber".
Replacement Procedure
1 Unclip the upper and lower clips that secure the halogen scrubber.
7
2 Disconnect the Viton connectors and remove the halogen scrubber. Release the
white plastic clamp that secures the Viton connector while twisting it in the
vertical direction.
3 Remove the film at both ends of the new halogen scrubber and connect it to
the Viton connectors.
4 Secure the halogen scrubber with the two clips in its original position.
The baseline may fluctuate immediately after replacement. Allow the instrument to run
for a short time until the baseline stabilizes. Stabilization normally occurs within one
hour.
Used halogen scrubbers should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the
halogen scrubber contains copper.
• Install the syringe according to the procedure to avoid the danger of acid
leaking from the syringe connection port.
• Keep hands away from the sample injector during operation of the syringe
pump sample injector.
• The syringe barrel is made of glass, handle it carefully to avoid breakage.
Procedure
2 Open the Sample Table tab of the file viewer. Right-click on the connected
system configuration icon, and click Maintenance – Change Syringe.
The Syringe Change window can also be displayed by selecting Instrument – Maintenance
– Change Syringe.
4 Disconnect the sparge gas line from the syringe, remove the plunger retaining
screw, and remove the syringe.
5 Reverse the above procedure to install the new syringe and connect the sparge
gas line. At this point, the plunger retaining screw is not completely tightened.
Tighten the retaining screw so that the plunger can still be slightly moved
forwards and backwards as well as left and right.
The plunger is secured to the plunger holder with the plunger retaining screw through
a spring washer. Be careful not to lose the spring washer.
7 Once the syringe reaches the top position, hold the plunger vertical and tighten
the plunger retaining screw to secure it to the plunger holder.
Hand-tighten only. Do not use a tool tighten the plunger retaining screw.
Over-tightening may deform the resin components of the 8-port valve and
cause leaks.
8 Click Finish Replacement. The syringe pump zero point detection operation is
executed automatically.
9 Click Close.
7
The syringe plunger tip is constructed of fluororesin and wears with use. Gaps will
eventually form between the plunger and the inner wall of the syringe barrel (glass
tube), causing leaks. When leaks occurs, bubbles are produced near the syringe tip when
sample is drawn into the syringe or sample may leak from the bottom of the barrel
when the sample is discharged. When these problems are observed, replace the plunger
tip.
Replacement Procedure
2 Use a sharp knife to make two or three incisions at the bottom of the plunger
tip, as shown in "Figure 7.8 Removing the Old Plunger Tip".
3 Grasp the plunger tip with a pair of pliers and remove it from the plunger. The
O-ring that is held in place by the plunger tip also comes off. DO NOT reuse
this O-ring.
4 Pushing down on the plunger, press the leading edge of the new plunger tip
straight into the plunger tip seat, as shown in "Figure 7.9 Installing the New
Plunger Tip (cross-section)". Save the syringe for future use since the plunger tip
seat is enclosed inside the syringe.
• Do not scratch the perimeter of the plunger tip. This could cause leaks.
• Use only Shimadzu-specified plunger tips. Use of unspecified parts may result
in malfunction and/or diminished performance.
Two types of o-rings are stacked between the injection block and the slider of the sample
injector. If a gas leak develops in this area, replace both o-rings.
• White Upper O-ring: O-ring, PTFE (P/N S638-15025)
• Black Lower O-ring: O-ring, 4DP10A (P/N S0936-11209-84)
If a gas leak develops between the injector block and the combustion tube, replace the
o-ring there as well.
Do not scratch the o-rings or the o-ring seat when replacing the o-rings.
To prevent gas leaks, install the o-rings (PTFE) in the correct orientation as
shown in Figure 4.10 when replacing the O-rings.
The fluororesin rotor of the syringe pump 8-port valve gradually becomes worn and
scratched after prolonged use due to suspended particles in the samples. This wear
eventually causes leaks from the 8-port valve.
The following symptoms are associated with leaks from the 8-port valve and indicate that
rotor replacement is necessary.
• Droplets of liquid around the 8-port valve (especially around the upper shaft)
• Decreased analysis reproducibility
• Presence of bubbles in the syringe
If the leakage is great, sample remaining in the tubing after it is drawn into the syringe
may flow back into the sample container. This is most likely due to a sampling tubing
flange or connection problem.
Switch OFF the instrument before replacing the 8-port valve rotor.
Procedure
1 The mark on the 8-port valve interrupt plate indicates the orientation of the
rotor hole (stream direction). Take note of which port number the mark is
pointing towards.
3 Pull up to remove the rotor drive component. Hang it on the screw on the right
side of the plunger.
7 Insert a new rotor, taking care that the rotor hole matches original orientation.
Perform the syringe pump zero detection procedure before analysis. Refer to "7.
6 Maintenance Menus" P.351.
7.2.12 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier
The NDIR baseline becomes unstable with a decrease in the carbon dioxide absorption
in the carrier gas purifier CO2 absorber. The baseline position rises and reproducibility
diminishes, making analysis impossible.
The soda lime must be replaced when this occurs.
The frequency with which soda lime must be replaced depends on the frequency of
analysis, quantity of organic impurities in the carrier gas, and the TOC content of the
samples. It is recommended that soda lime be replaced once every four months.
The carrier gas pressure applied to the carrier gas purifier CO2 absorber is
approximately 200 kPa. It is dangerous to perform this maintenance procedure
under these conditions. Before replacing the soda lime, lower the carrier gas
pressure in the instrument to normal as follows:
• Turn the supply valve of carrier gas source OFF.
• Switch OFF the instrument.
Procedure
1 Remove the elbow joints on the CO2 absorber for carrier gas purification, which
is located in the holder on top of the instrument.
4 Refill the absorber container with about 500 g of new soda lime until it reaches
about 5 mm from the interior screw threads.
Do not allow any soda lime to enter the tube in the center of the container
when refilling the CO2 absorber.
5 Fill the hollow in the screw cap with quartz wool and screw the cap back on
the container.
6 Using the elbow joints, connect the carrier gas purifier CO2 absorber to the two
tubes exiting the back of the instrument as follows:
7
• Tubing labeled "L"
Affixed to the connection port of the CO2 absorber container labeled "L"
Only tighten the nuts on the elbow joints by hand. Do not use tools.
7 Place the CO2 absorber for carrier gas purification in the holder on top of the
instrument.
Used soda lime should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the
material contains soda lime.
For the H Type, verify that there is sufficient IC reaction solution in the IC reaction
solution vessel before performing IC analysis. If not, replenish the IC reaction solution
referring to "3.1.14 IC Analysis Preparations" P.55.
The IC reaction solution is acidic. Use care not to spill or touch the fluid when
handling it.
For details, refer to "8.9 Safety Data Sheets (SDS)" P.433.
The IC reaction solution pump is a roller type pump that uses a rotating roller to flatten
the rubber tube carrying the IC reaction solution, thereby feeding solution into the
system. This rubber tubing gradually deteriorates, requiring periodic replacement of the
pump head.
The life of the rubber tubing is generally about 300 hours of pump operation. It is
recommended that 300 hours be entered as the warning value in the Maintenance History
Dlg window.
The pump head and rubber tubing inside the IC reagent pump are filled with
IC reagent solution. This solution is acidic. Use care to avoid touching or
spilling the solution when changing the pump heads. For details refer to "8.9
Safety Data Sheets (SDS)" P.433.
Replacement Procedure
Use the following procedure to replace the pump head.
1 Pinch the pump head (plastic) of the IC reaction liquid feed pump with your
fingers, turn the pump head counterclockwise, and pull it out from the pump
(motor side).
2 Disconnect the rubber tubing ties of the pump head and remove the connected
PTFE tubing.
3 Connect the PTFE tubing to the rubber tubing of the new pump head and secure
it with the included ties.
Figure 7.14 Replacing the Pump Head of the IC Reaction Solution Pump
7.2.15 Replacing the Filler of the Optional POC Analysis CO2 Absorber
The CO2 absorber for POC analysis is filled with about 6 grams of lithium hydroxide, 7
which is sufficient to absorb carbon dioxide gas for several hundred analyses under
normal conditions. Airflow resistance gradually increases with use and may become
excessive irrespective of adequate carbon dioxide absorbency.
Replace the lithium hydroxide in the CO2 absorber with a new batch if analysis values
become unstable or carrier gas flow is impeded. For the procedure on filling the CO2
absorber with lithium hydroxide, refer to "3.1.15 Preparation for POC Analysis (When
Using the Optional POC Kit)" P.58.
• The life of the CO2 absorber will be shortened by performing POC analysis
on samples with high concentrations of IC.
Replace the liquid in the B-type halogen scrubber every three months with 0.05 mol/L
hydrochloric acid.
The stainless mesh for absorption can be used until it dissolves. Note that the ability to
absorb halogen stops after the stainless mesh for absorption has dissolved completely.
Perform the following inspections before conducting analysis with the ASI-L. If the
following inspections are not properly conducted, air will be drawn into the ASI-L
injection pump, preventing the delivery of rinse water.
• Check the rinse water level
Verify that the water in the rinse bottle is above the 2-liter level mark. Add water if
necessary.
• Check the rinse tubing
Verify that the tip of the rinse tubing reaches nearly to the bottom of the rinse bottle.
Adjust the tubing position if necessary.
The rinse pump is located inside the ASI-L and supplies rinse water to the rinse port. The
rinse pump is a roller type pump that uses a rotating roller to flatten the rubber tubing
carrying the rinse water, thereby feeding rinse water into the system. This rubber tubing
gradually deteriorates, requiring periodic replacement.
The life of the rubber tubing is generally about 300 hours of pump operation. It is
recommended that 300 hours be entered as the warning value in the Maintenance History
Dlg window.
Replacement Procedure
Use the following procedure to replace the pump head.
1 Remove the rectangular pump access cover on the back left side of the ASI-L.
2 Pinch the pump head (plastic) of the rinse water pump with your fingers, turn
the pump head counterclockwise, and pull it out from the pump (motor side).
3 Disconnect the rubber tubing ties of the pump head and remove the connected
PTFE tubing.
4 Connect the PTFE tubing to the rubber tubing of the new pump head and secure
it with the included ties.
5 Attach the pump head by following the above procedure in reverse and then
attach the pump access cover.
The OCT-L uses a fluororesin 8-port valve rotor. The valve rotor may become worn or
scratched after prolonged use due to the suspended particles in the samples. This wear
eventually causes leaks from the 8-port valve.
The following symptoms are associated with leaks from the 8-port valve and indicate that
it is necessary to replace the rotor.
• Droplets of liquid around the 8-port valve (especially, around the upper shaft)
• Decreased analysis reproducibility.
• Presence of bubbles in the TOC-L syringe.
If the leak is large, sample remaining in the tubing after the syringe has been filled may
flow back into the sample container. This is most likely due to a sample tubing or flange
connection problem.
Switch OFF the power before replacing to the 8-port valve rotor.
Replacement Procedure
1 Remove the four screws on the top of the OCT-L and take off the cover.
2 Verify that the mark on the 8-port valve cover is directed toward port No.1.
If the mark is not directed toward port No.1, the instrument was not shut
down properly. If this is the case, turn the TOC-L on again, and shut it down
properly.
3 Remove the nut using the wrench supplied with the TOC-L.
6 Note the orientation (toward port No. 1) of the flat surface of the
spring-equipped rod. Remove the spring-equipped rod and retaining nut.
7 Note the orientation of the rotor hole position. Grasp the rotor with forceps,
and remove by pulling upwards.
8 Insert a new rotor, positioning the rotor hole to the original position.
9 Reinsert the spring-equipped rod and retaining nut with the flat surface directed
toward port No. 1. Tighten the retaining nut.
10 Replace the 8-port valve in its original position, and secure it using the nut.
11 Replace the cover of the OCT-L and secure it with four screws.
The ozone treatment unit breaks down ozone gas produced by the ozone generator. The
catalyst inside the ozone treatment unit must periodically be replaced. Replace the
catalyst once a year for an instrument that runs 8 hours a day and 5 days a week.
Perform maintenance to the ozone treatment unit only after stopping the instrument as
described in "5.7.7 Instrument Shutdown" P.271.
Replacement Procedure
Use the following procedure to replace the catalyst in the ozone treatment unit.
1 Disconnect the tubing (Viton tubing) from each end of the ozone treatment unit
and pull out the ozone treatment unit in the upward direction.
2 Remove the larger diameter fluoro rubber plug and take out the used catalyst
and polypropylene packing material.
4 Remove the ozone exhaust tubing that connects the detector exhaust port and
the ozone treatment unit inlet.
The ozone exhaust tubing must be replaced with a new one each time the
catalyst is replaced.
5 Return the ozone treatment unit to its original position in the instrument and
reconnect the tubing to each end of the unit.
7.5.2 Inspecting the Chemiluminescence Detector and Replacing the Ozone Generator
The light receiving window of the chemiluminescence detector may become dirty with
components of the sample for measurement. Inspect the window contamination and
packing at least once a year.
Replace the ozone generator with a new one after the operation time exceeds 4000
hours.
Replacement of these parts must be carried out by an authorized Shimadzu service
engineer, or someone who has been properly trained in the procedure. Contact your
Shimadzu representative to request replacement.
2 Open the Sample Table tab of the file viewer. Right-click on the connected
system configuration icon, and click Maintenance – History.
The Maintenance History Dlg window can also be displayed by selecting Instrument –
Maintenance – History.
If the ozone generator is used after 4000 hours of operation, ozone generation
may not be sufficient for analysis, or ozone may leak from inside the
generator. Replace the ozone generator without fail.
The NOx absorber is used to absorb NOx gas generated by the TNM-L. Although the CO2
absorber used to purge the optical system of the NDIR detector is used in the NOx
absorber (the spent absorber from "7.2.6 Replacing the CO2 Absorber" P.327), this CO2
absorber is still effective for NOx absorption.
During the annual replacement of the CO2 absorber used to purge the optical system of
the NDIR detector, replace the NOx absorber for the TNM-L with the used CO2 absorber
from the TOC-L.
Refer to "Installation of the NOx Absorber" P.60 for more details.
During the annual replacement of the CO2 absorber used to purge the optical system of
the NDIR detector, replace the NOx absorber for the TNM-L with the used CO2 absorber
from the TOC-L.
The Sample Table editor must be connected to the instrument to access the
Maintenance menu. Refer to The Sample Table editor must be connected to the
instrument to access the Maintenance menu. Refer to "Connection" P.253 for
details on the connection procedure. for details on the connection procedure.
The Maintenance menu can be accessed using two different methods. It should be noted
that the Blank Check operation is only available from the menu bar.
Click Start to begin the procedure. The progress bar continues blinks while the operation
is in progress.
When the process is complete, click Close to close the window.
Washing...
Use this function to wash of the selected flow lines.
Click the Select Flow Lines button to display the Wash Flow Lines dialog box.
Select the flow lines to be washed. The available items will vary depending on the
connected optional accessories. Click Washing to close this dialog box, return to the
Washing window and begin the flow line wash operation.
The progress bar blinks while the operation is in progress.
When the washing process is complete, click Close to close the window.
Mechanical Check
This function is used to check the mechanical operation of the system components. This
is normally used by Shimadzu service engineers to conduct instrument inspections. To
close the window, click OK.
• TOC tab
Item Function
Click the buttons to move the syringe pump to the Zero, Home and
Syringe Pump Sparge positions.
Click the Reset button to move the plunger to the highest position.
Use the Open and Close buttons to open and close the following
solenoid valves.
Solenoid Valves • IC Drain
(Combustion and
• Carrier gas
Option)
• Sparge Gas
• POC
Click a numbered button to open the flow line between the syringe
Port Select and the injection port. The numbered buttons correspond to the
port numbers of the 8-port valve.
Click Open to turn the IC reagent delivery pump on, and Close to
Acid Pump
turn it off.
Click Drain or Meas to move the TC slider to the drain or injection
TC Inj. Port
position.
Click Drain or Meas to move the IC slider to the drain or injection
IC Inj. Port
position.
Item Function
Click On and Off to start and stop the ASI-L flow line rinsing
Rinse
operation.
Click the left and right buttons to move the ASI-L vial rack left and
Move Tray
right. Click Reset to return the rack to the home position.
Click the up and down buttons to move the arm up and down. Click
Reset to return the arm to the home position.
Arm Use the Horizontal drop-down box to move the arm horizontally to
the Rinse, Needle Change Pos, Drain Port or Vial 1st (to 5th) Line
positions.
Enter a vial position number, and then click the Move button to
Vial Position
move the arm to the specified position.
Magnetic Stirrer Click On and Off to start and stop the magnetic stirrer operation.
Click Start to begin the initialization process. The progress bar blinks while the operation
is in progress.
When the initialization is complete, click Close to close the window.
Change Syringe
This function is used when installing and replacing a syringe. For details of the procedure,
refer to "3.1.5 Installing the Syringe" P.39, or "7.2.8 Syringe Replacement" P.329.
Blank Check
This function is used to measure the system blank value before conducting high sensitivity
measurement and before using new TOC high sensitivity catalyst. For details of the
procedure, refer to "TC Blank Check Analysis" P.71.
History
Threshold values can be set for the items below. If a threshold value is exceeded, a
warning message is displayed (except for the total operation time).
• CO2 absorber last replacement date
Enter a value in each of the Preset Limit boxes to set the warning threshold. Click Reset
to clear the Current value.
After all of the parameters are entered, click OK to close the dialog box.
It is recommended to set the warning threshold for Dilution water and Total Acid Vol to
a value that is slightly less than the actual remaining volume to display the warning
message before the dilution water or acid run dry.
Error List
The errors occurring to the instrument are displayed in list form. These errors can be
reset at one time.
Place a check mark next to the Reset All Error item on the Error List dialog box, and
click OK. The displayed errors will be reset.
7.7 Troubleshooting
Describes the error messages and troubleshooting procedures.
This section describes the error messages displayed by the TOC-Control L software and
the actions recommended to resolve the underlying causes.
Take the corrective action indicated in the table below when any of the following error
messages are displayed.
The following error messages indicate that an error has occurred that prevents the
measurement operation from continuing. Take the appropriate corrective action indicated
in the table below when any of these error messages are displayed.
If the cause of an error cannot be determined or the error persists after taking the
prescribed corrective action, contact your Shimadzu representative as the problem
requires servicing.
7.7.2 Troubleshooting
n TOC-L
Reference
The following procedure can be used to check whether carrier gas is flowing to the
infrared gas analyzer. However, this procedure cannot determine the existence of minute
gas leaks. Note that checks using this procedure cannot be performed when the TNM-L
is connected to the instrument.
Procedure
1 Block the carrier gas flow by firmly folding over the flexible tubing labeled with
an "L" that is connected to the CO2 absorber, which is located in the holder on
top of the instrument.
2 If carrier gas bubbles out from the bottom of the drain tubing inside the drain
container, which is located on the left side of the instrument, this means that
carrier gas is flowing to the infrared gas analyzer.
For the H Type instrument, whether carrier gas is flowing to the IC reaction vessel can
be determined by visually checking for bubbling of IC reagent in the IC reaction vessel.
Reference
When using a TOC high sensitivity catalyst, peaks will not be output or the peak shape
will deteriorate if the catalyst filling in the combustion tube becomes loose (rises up). In
this case, remove the combustion tube from the instrument and check the filling state
of the catalyst. If the filling height is more than 110 mm, use the catalyst filling rod to
push the catalyst down from the top of the combustion tube to a height of 110 mm.
When performing sample acidification and sparging in NPOC measurement using the
syringe pump type sample injector in the TOC-L, the acid used for sample acidification
must completely fill the PTFE tubing used to supply the acid. If bubbles are present in
the tube, acid addition with respect to the sample will not occur properly and will lead
to only partial IC removal. This will result in a higher NPOC measurement value than
anticipated.
This problem will occur noticeably if the connection between the PTFE tubing for
supplying acid and the 8-port valve decreases in airtightness. If this is the suspected cause,
executing the stream bubble removal function, retightening the bush on the connection
of the PTFE tubing for supply acid, and replacing the rotor in the 8-port valve are all
effective methods to resolve this problem.
In addition, it is possible to check whether any sample has acidified inside the syringe
by measuring the pH level of discharge from the TOC-L drain tubing with pH test paper.
7
n ASI-L
Ensure that the tip of the tubing does not protrude beyond the bottom surface of the
slider. The O-ring or other seal parts will be scratched if the tubing protrudes, resulting
in gas leaks. The sample is not properly injected unless the tip of the tubing extends
into the depression in the bottom of the slider.
Check the state of the injection for TC analysis by looking through the TC combustion
tube while it is attached to the instrument. The sample injection tubing can be detached
from the slider, and water can be injected for inspection using the functions available
in the Instrument>Maintenance>Mechanical Check screen.
Salt or other substances adhering to the tip of the tubing after rinsing can allow large
droplets of sample to remain on the tip of the tubing after injection. A deformed tip
on the sample injection tubing (a beard-like protrusion, for example) may cause the
sample to be injected obliquely. In either case, reproducibility is adversely affected and
the sample injection tubing should be replaced. Another option available only if there
is sufficient length of tubing remaining is to use a sharp cutting tool at a 90° angle to
cut off 2 - 3 mm from the tip of the currently used sample injection tubing.
7
(1) The surface of the plunger tip becomes worn and the seal between the plunger tip
and the inside of the glass syringe barrel deteriorates, allowing slight amounts of water
to leak out with vertical movements of the plunger.
(2) The contact site of the plunger tip and plunger becomes loose, causing a slight backlash
with vertical movement of the plunger.
As the above conditions start to occur, repeatability of sample injection volume decreases,
resulting in diminished analysis reproducibility. Item (2) above rapidly leads to decreased
reproducibility. Since it is very difficult to determine backlash by inspecting movement
of the plunger tip, inspect as follows.
Before sample injection, observe the wash injection used to replace the previous sample
in the syringe and flow line with the new sample. After injection, if a droplet forms at
the tip of the injection tubing and increases in size, there is a strong possibility that
backlash has increased. The corrective action in this case is to replace the plunger tip.
The effect of backlash increases with smaller sample injection volumes. Poor
results might be obtained with a sample injection volume of 10 µL, while the
effect might be negligible with a 100 µL sample injection volume.
n Corrective Action for Combustion Tube Breakage Inside the Electric Furnace
Allow the electric furnace to cool to room temperature for at least six hours after
switching off the power supply by shutting down the instrument and then perform
corrective measures according to the following procedure.
2 With the utmost care to avoid injury, remove the broken upper end of the
combustion tube from the sample injector.
3 Remove the bottom end of the combustion tube from the cooling tube coupling,
loosen the two screws that secure the cooling tubing unit, and remove the
cooling tubing unit from the instrument.
4 With the utmost care to avoid injury, remove any catalyst and broken pieces of
combustion tube that have fallen inside the instrument.
Allow the electric furnace to cool to room temperature for at least six hours
after switching off the power supply by shutting down the instrument before
performing maintenance on the combustion tube or catalyst. Burns may result
if this task is attempted when the furnace is at a high temperature.
Combustion tubes are made of quartz glass. Always wear protective leather
gloves when handling combustion tubes to prevent injuries due to breakage.
n Corrective Action for Connection Failure between Sample Table Editor and Instrument
A connection failure may occur if the application is forcibly quit while connected
to the instrument.
1 Turn OFF the main power of the instrument and then turn it ON again.
For details, refer to "4.1.2 Turning on the Instrument" P.100.
3 Establish the connection between the Sample Table Editor and the instrument.
For details, refer to "5.7.1 Instrument Connection and Disconnection" P.253.
n Corrective Action When a Communication Failure Occurs with the Server (When Using
Client Server Version)
If a communication failure occurs with the server when using the client server version,
the application ends normally after the current sample measurement is completed.
Open the Sample Table Editor again after recovering from the communication failure.
For details, refer to "5.2.1 Opening the Sample Table Editor" P.139.
It may not be possible to save the sample information that was being measured
when the failure occurred.
Sample is introduced into the TC combustion tube, which is filled with an oxidation
catalyst and heated to 680 °C. The sample is burned in the combustion tube and, as a
result, the TC components in the sample are converted to carbon dioxide. Carrier gas,
which flows at a rate of 150 mL/min to the combustion tube, carries the sample
combustion products from the combustion tube to an electronic dehumidifier, where the
gas is cooled and dehydrated. The gas then carries the sample combustion products
through a halogen scrubber to remove chlorine and other halogens. Finally, the carrier
gas delivers the sample combustion products to the cell of a non-dispersive infrared
(NDIR) gas analyzer, where the carbon dioxide is detected. The NDIR outputs an analog
detection signal that forms a peak; the peak area is measured by the TOC-Control L
software.
The peak area is proportional to the TC concentration of the sample. A calibration curve
equation that mathematically expresses the relationship between peak area and TC
concentration can be generated by analyzing various concentrations of a TC standard
solution. The TC concentration in a sample can be determined by analyzing the sample
to obtain the peak area and then using the peak area in the calibration curve equation.
Two methods for measuring IC using the TOC-L are available: analysis within the injection
syringe and analysis using the optional IC reactor. In both methods, the measured IC
consists of carbon derived from carbonates, hydrogen carbonates and dissolved carbon
dioxide.
Defining IC
The IC measured by TOC analysis consists of the carbon contained in carbonates and in
carbon dioxide dissolved in water.
By acidifying the sample with a small amount of hydrochloric acid to obtain a pH less
than 3, all carbonates are converted to carbon dioxide (CO2) by the following reactions:
Me2CO3 + 2HCl → CO2 + 2MeCl + H2O
MeHCO3 + HCl → CO2 + MeCl + H2O
Carbon dioxide and dissolved carbon dioxide in the sample are volatilized by bubbling
(sparging) air or nitrogen gas that does not contain carbon dioxide through the sample.
After acidifying the sample to pH 2 to 3, sparge gas is bubbled through the sample to
eliminate the IC component. The remaining TC is measured to determine total organic
carbon, and the result is generally referred to as TOC. However, in the TOC-L, this analysis
value is referred to NPOC to distinguish it from the TOC value obtained by calculating
the difference between TC and IC. NPOC stands for non-purgeable organic carbon and
refers to organic carbon that is present in a sample in a non-volatile form.
NPOC and TOC (obtained by IC elimination) described in the TOC-related standard
methods and referred to in water quality-related test methods (JIS, ASTM, EPA, EN) are
identical. Purgeable organic substances in the sample can be lost during the sparging
process. Consequently, when the sample contains purgeable organic substances, TOC
should not be measured by the NPOC method. If the dissolved purgeable organic
component in the water sample is large, the amount volatilized during sparging is
relatively small. Generally, the amount of purgeable organic substances in natural
environmental, public and purified water is small; as a result, NPOC can be referred to
as TOC.
Table 8.1 Residual Rate of Volatile Organic Substances using Sparging (Nitrogen Gas)
POC analysis is used to measure the volatilized component of TOC, which is produced
during the NPOC sample sparging process. As a result, NPOC+POC is equivalent to TOC.
POC analysis is performed as follows.
Sparge gas containing the volatilized CO2 and POC components of the sample is carried
to the lithium hydroxide-filled CO2 absorber to eliminate the CO2 that was converted
from the IC in the sample. The gas, which now contains only the POC component of the
sample, then passes through the combustion tube to be oxidized. The POC component
is converted to CO2 during oxidation and the CO2 is detected by the NDIR. Data
processing is conducted in the same manner as for TC.
POC is not precisely defined. Factors that determine whether or not, or to what degree,
a volatile organic carbon component is volatilized during sparging include the type of
organic compound, the gas/liquid contact with the sparge gas, and the ambient
temperature during sparging. The target of POC analysis is the organic component
present in the aqueous phase. As a result, organic compounds that are highly soluble in
water (such as methanol or ethanol) and not easily volatilized by sparging produce almost
no peaks in POC analysis.
Organic compounds with low solubility in water (such as methylene chloride or
chloroform) produce sharp peaks in POC analysis. Over a long period of time, compounds
such as acetone and methyl isobutyl ketone generate extremely broad, tailing peaks with
no specific end time.
The lithium hydroxide-filled CO2 absorber eliminates the carbon dioxide that was
generated along with the POC substances. Therefore, POC components that are easily
caught in the CO2 absorber (such as esters) produce low values in POC analysis. POC
results obtained using this technique are not absolute. The user should take all the above
factors into consideration when measuring POC using this instrument.
TC-IC Method
In the TC-IC method, TOC is measured as the difference between the TC and IC analysis
values. The TC-IC method is not recommended for samples that contain more IC than TOC
(samples where TC consists almost entirely of IC); the NPOC method is recommended for
such samples. The TOC value determined using the TC-IC method includes errors
associated with each of the individual TC and IC measurements, and can therefore result
in a large error in the TOC value.
Because detection accuracy decreases with increasing IC concentration, the NPOC method
is also recommended for samples containing IC concentrations exceeding 10 ppm for
TOC/TN catalyst and 5 ppm for high sensitivity catalyst.
NPOC Method
The NPOC method is the most widely used TOC analysis method. The NPOC method is
not recommended for samples that foam during sparging. Samples that become foamy
during sparging tend to form bubbles that flow out of the syringe, which removes the
concentrated TOC sample components and leaves a small amount of TOC in the syringe.
The TC-IC method is recommend in this situation. Moreover, since TOC cannot be correctly
measured in samples that coagulate or precipitate when acidified, use the TC-IC method.
Note that with Shimadzu’s TOC analyzer, the recommended amount of acid added and
the recommended ventilation time in the IC removal process during NPOC measurement
are set so as to be able to accommodate a wide range of samples. However, depending
on the characteristics of the sample, including pH, the IC removal may not be complete,
and there may still be residue in the sample.
To check the effectiveness of the IC removal process, or to compensate for the effects
of the remaining IC, with NPOC-IC as the measurement type, IC measurement is
performed in conjunction with NPOC measurement, and result of subtracting the
measured IC value from the measured NPOC value is output. This feature is only available
with PC control and requires the ASI-L option and an external sparge kit.
POC+NPOC Method
The POC+NPOC method should be used when the amount of POC present in the sample
cannot be disregarded.
When a sample is introduced into the combustion tube (furnace temperature 720 °C),
the TN in the sample decomposes to nitrogen monoxide. Nitrogen gas does not become
nitrogen monoxide under these circumstances. The carrier gas, which contains the
nitrogen monoxide, is cooled and dehumidified by the electronic dehumidifier. The gas
then enters a chemiluminescence gas analyzer, where the nitrogen monoxide is detected.
The detection signal from the chemiluminescence gas analyzer generates a peak and the
TN concentration in the sample can then be measured.
TN Detection Rate
In TN analysis, the state (crystalline state) in which TN exists in the sample greatly
affects the TN detection rate. Nitrogen contained in nitrates, nitrites, ammonia
and the majority of other organic nitrogen compounds exhibit high detection
rates. Conversely, some organic nitrogen-containing compounds (such as
hydrazines, pyrazolones, and azide compounds) have detection rates ranging
from 10 % to 60 %, depending on the concentration.
• Separated Peaks
In TC analysis, multiple peaks may occur when a large quantity of sample is
injected. Only the end of the last peak is detected. The total area of the
multiple peaks is calculated.
• Baseline Correction
Baseline correction is performed for peaks produced with fluctuating baseline
to obtain the correct peak area.
Multiple peaks are especially prominent when using the high sensitivity catalyst with
sample injections greater than 100 µL. As sample is injected onto the catalyst, the easily
volatilized organic substances and the crystalline organic substances are combusted at
different rates. As a result, carbon dioxide is generated multiple times, resulting in the
formation of multiple peaks. Easily volatilized organic substances are organic compounds
that are volatilized with water when an aqueous solution of the compounds is heated;
ethanol is one example of such a compound. Crystalline organic compounds remain in a
solid form following the heating of an aqueous solution of the compound; glucose is
one example of such a compound.
The manner in which the sample is injected also has an effect on peak shape. If a portion
of the sample is injected into the center of the combustion tube while another portion
is injected at the periphery, combustion may occur at different times, resulting in multiple
peaks.
Peak shape does not affect the analysis results. Even if multiple peaks occur due to the
type of organic substance or injection manner described above, the TOC-Control L
calculates the total area of the peaks generated to determine the TOC (or TC) accordingly.
Set values that ensure the dilution factor is greater than 1.25. If the dilution
factor is less than 1.25, the dilution factor precision of the instrument may be
impaired.
Shift to Origin
The "shift to origin" function is used when the amount of TC and IC or TN in the pure
water used for standard solution preparation cannot be ignored with respect to the
standard solution concentration. A correction must be made by shifting the calibration
curve in a parallel fashion so that it passes through the origin. This corrects for the TC
and IC or TN concentration in the water used for standard solution preparation. An
example of a situation in which the "shift to origin" function is useful is described below.
When water containing 0.5 mg/L TC is used to prepare a 10 mg/L TC standard solution,
the actual TC concentration in the standard solution will be 10.5 mg/L (0.5 mg/L from
the water + 10 mg/L from the standard solution). The 2-point calibration curve generated
using such a solution is shown by the solid line in "8.2 Analysis-Related Technical
Information" P.387. If this curve is used without correction, the sample analysis values
will always be 0.5 mg/L less than the true value. By shifting the calibration curve so that
it passes through the origin, as shown by the broken line in "8.2 Analysis-Related
Technical Information" P.387, the calibration curve is effectively corrected.
A system blank is water that contains absolutely no carbon (zero water). When
measurement of a system blank produces a peak, the TC concentrations measured in
samples will be biased high by the amount of TC in the system blank. In most cases (with
the exception of high sensitivity analysis), this bias is not significant. Measurement error
resulting from the TC or TN content in the water used to prepare standard solutions is
typically much greater than measurement error resulting from the system blank value.
Correcting the calibration curve based on the TC or TN content in the standard solution
preparation water will produce satisfactory analyses. Using this correction method, the
value obtained for a system blank would be greater than zero by the amount of the
blank value.
The instrument allows shifting of calibration curves only to the extent of the system
blank value. The system blank peak height varies with such factors as the system
configuration and the type of catalyst used.
Table 8.2 CO2 Content (ppm) in Distilled Water Equilibrated with Atmosphere Temperature (°C)
Atmospheric CO2
(vol%)
0 5 10 15 20 25 30 8
0.030 1.00 0.83 0.79 0.59 0.51 0.44 0.38
0.033 1.10 0.91 0.76 0.65 0.56 0.48 0.42
0.044 1.47 1.22 1.02 0.87 0.74 0.64 0.56
The above CO2 content can be converted to IC using the following equation.
IC (ppm)=CO2 (mg/L) ´ 0.27
Up to three different calibration curves can be selected for use in a method. The curves
are specified in the Calibration Curve 1, Calibration Curve 2 and Calibration Curve 3 fields
on page 3 of the Method Wizard when the method is being created. When more than
one calibration curve is specified, the TOC-Control L software automatically selects the
optimum calibration curve to be used for calculating measurement results.
The automatic selection process occurs on a measurement-by-measurement basis.
Measurement values are always calculated first using Calibration Curve 1.
The TOCControl L software then evaluates the result, applies the optimum calibration
curve, and recalculates the value if necessary. The calibration curve with a concentration
range that is greater than and closest to the measured value is used. Examples are shown
below:
(1) If the measured value is less than the concentration of Calibration Curve 1 and greater
than the concentration of Calibration Curve 2 and Calibration Curve 3, Calibration
Curve 1 is used.
Conc. of Calibration Curve 1 > Measured Value > Conc. of Calibration Curves 2 and 3
→ Calibration Curve 1 is used
(2) If the measured value is less than the concentrations of Calibration Curve 1 and
Calibration Curve 2, and if the concentration of Calibration Curve 2 is less than that
of Calibration Curve 1, Calibration Curve 2 is used.
Conc. of Calibration Curve 1 > Conc. of Calibration Curve 2 > Measured Value →
Calibration Curve 2 is used
(3) If three calibration curves are specified, the calibration curve that is greater than and
closest to the measured value is used.
Conc. of Calibration Curve 1 > Conc. of Calibration Curve 3 > Measured Value > Conc.
of Calibration Curve 2 → Calibration Curve 3 is used
(4) If the measured value is greater than the concentration of all curves and the
concentration of Calibration Curve 1 is greater than the concentration of Calibration
Curves 2 and 3, Calibration Curve 1 is used.
Measured Value > Conc. of Calibration Curve 1 > Conc. of Calibration Curve 2 > Conc.
of Calibration Curve 3 → Calibration Curve 1 is used
Activate the automatic correction function for injection volume and dilution factor by
selecting the Auto. Correction of inj. Vol. and dilution checkbox in the Method Wizard
(Page 4) Injection Parameters window.
Notes on the Automatic Correction Function for Injection Volume and Dilution Factor
• When the number of injections is set to multiple, the first measurement value is used
to judge the above condition.
• This function will not work if TN simultaneous measurement and POC/NPOC identical
sample measurement are turned ON.
• The automatic selection function for optimum calibration curves and the automatic
correction function for injection volume take priority over this function.
• The dilution factor may not become exactly 80 % due to rounding to integer numbers.
• When this function activates, all previous data is erased and measurement starts again
after changing the measurement conditions. Note that measurement takes longer
because the number of injections is counted again from zero when the measurement
conditions are changed.
Activate the multi-stage injection function by selecting the Multiple Injections checkbox
in the Method Wizard (Page 4) Injection Parameters window.
The TOC-L is equipped with a program that automatically performs testing and judgment
of results for three types of pharmacopoeia in regard to testing the purity of
pharmaceutical water.
While a summary of the testing procedure is described below, refer to each
pharmacopoeia for a detailed explanation.
A system suitability test and pharmaceutical water test are defined in the USP and EP
standards.
The system suitability test is used to produce a pass or fail result for the organic substance
detection function of the TOC instrument. The test involves performing TOC
measurements of 0.5 mgC/L sucrose test solution and 1,4-benzoquinone. If the
measurement value of the latter is within the 85 % to 115 % range of the former, the
organic substance detection function is given a pass result.
The process also measures the TOC contained in the pure water used to prepare the test
solutions and this is used to correct measurement results.
The pharmaceutical water test is used to test the purity of pharmaceutical water. A TOC
measurement value for pharmaceutical water that is less than the TOC measurement
value for a 0.5 mgC/L sucrose test solution will result in a pass. The process also measures
the TOC contained in the pure water used to prepare the sucrose test solution an this
is used to correct measurement results.
A recovery rate test and pharmaceutical water test are defined in the JP standards.
8.3 Specifications
This section lists specifications for the TOC-LCPH/CPN main unit, ASI-L, TNM-L and the
various optional kits.
8.3.1 TOC-LCPH/CPN
8.3.2 ASI-L
No. of sample
8 containers
containers
accommodated 16 containers (using 2 OCT-L units)
Ambient temperature 10 - 35 ° C
Approx. (W) 245 ´ (D) 245 ´ (H) 440 mm
External dimensions
(excluding protruding parts)
Weight Approx. 3.5 kg
8.3.4 TNM-L
TC: 60 µg/L
Detection limit IC: 4 µg/L
TN: 30 µg/L
TC: 10 to 150 µL
DVD drive
Other
USB port
OCT-L OCT-L
Part Number Part Name Details
(1) (2)
Rotor (for replacement
S638-56251-01 8-port valve rotor 1 1
maintenance)
8 sample tubes, 1 tube for
S638-42106-01 Flared tubing set C 1*1
connection to main unit.*2
8 sample tubes, 1 tube for
S638-42106-02 Flared tubing set C2 1*1
connection to main unit.*3
Cable for connection to
S638-74492-01 Connection cable 1
the main unit
Second unit connection Cable for connecting
S638-74476-02 1
cable OCT-L (1) to OCTL (2)
Qty
Part No. Description Remark
TOC-LCPH TOC-LCPN
S638-41323 Combustion tube (in case) 2 2
S638-60246 TOC regular catalyst 2 2
S630-00996 TOC high sensitive catalyst 1 0
S630-00557 Quartz wool 1 1
S630-00992 Halogen scrubber 2 2
S036-11209-84 O-ring, 4D P 10A 1 1 5 pcs.
S638-15025 O-ring, PTFE 2 1 1 pc.
S036-11219-84 O-ring, 4DP 20 1 1 5 pcs.
S638-59390-41 IC reagent supply pump head 1 0
S638-56251-01 8-port valve rotor 1 1
S638-59296-01 Plunger tip 2 2
"Table 8.15 Recommended Consumable Part Replacement Period" indicates the guidelines
for the major recommended consumable part replacement periods when NPOC
measurement is performed on samples that are comparatively as clean as tap water, using
TOC standard catalyst and at a rate of about 500 samples per month (operating five days
a week).
Note that these are not guaranteed values and the replacement period changes according
to instrument usage. In particular, measuring samples that contain salt, acid, or alkalis
may shorten the replacement period of parts such as the combustion tube, catalyst, and
halogen scrubber.
8.8 Installation
The installation site requirements and installation procedures for future relocation of the
instrument are described here.
Parts Inspection
Confirm that all of the components listed in "8.4 Standard Accessories" P.401 have been
included in the shipping package.
Be sure to take into account the size of the instrument, how it will be used, and the
installation conditions indicated below when selecting an installation site. Instrument
damage or measurement errors may occur based on the conditions of the installation site.
Figure 8.4 External Dimensions of the Instrument with the OCT-L 8-Port Sampler and TNM-L TN Unit (Units: mm)
When lifting the instrument, lift from the bottom and at both sides of the
instrument.
Do not lift the instrument by the front access door, as this may cause damage.
Contamination in the atmosphere will cause analysis errors, especially for high
sensitivity analyses.
Avoid locations where flames are prohibited. Some internal parts reach high
temperatures and could cause a fire hazard.
The instrument may not operate properly if the power supply voltage exceeds
the range of AC100-127 V ±10 % or AC 220-240 V ±10 %. Unstable voltage
may cause problems during high sensitivity analysis.
For position on the power supply inlet, refer to "2.1.4 Rear View" P.8.
Grounding
The power cord is a three-conductor cable including a ground wire.
Be sure to completely ground the ground wire of the cable.
The instrument is set up before shipment to match the power supply voltage in the locale
where it will be used. In the event that it becomes necessary to change the power supply
voltage, please contact your Shimadzu representative. Depending on the voltage change,
an authorized Shimadzu service engineer may be required to rewire connections to the
terminal block to change the power supply voltage and/or perform changes to the main
board.
n Connecting Gas
Use one of the following as the carrier gas supply for this instrument.
• Cylinders filled with high purity air
• Compressed air or instrumentation air (requires the optional carrier gas purification kit
on the N Type instrument)
• Gas cylinder filled with high purity nitrogen or instrumentation high purity nitrogen
(requires the optional N2 carrier gas kit)
If the carrier gas contains excessive impurities, analysis accuracy is diminished and
good results will not be obtained.
• Make sure there are no open flames anywhere within 2 meters of a gas
cylinder.
• Secure cylinders with bands or other fasteners to prevent tipping and falling.
• Turn OFF, immediately and completely, all valves on the cylinder, when
finished using gas.
• Inspect the operation of the pressure gauge at least once every three (3)
months.
Compressed Air or Instrument Air Purified with the Carrier Gas Purification Kit
Using the carrier gas purification kit on the N Type instrument enables the use of
compressed air, instrumentation air, and air from gas cylinders that is generally impure.
Since there are limits to the capabilities of the Carrier Gas Purification Kit, the following
conditions must be met when supplying compressed air. This kit cannot be used with the
H Type instrument.
• Provide an air filter in the supply line to remove dust, oil mist, water drops, and other
contaminants. Place an air filter in the tubing near the gas connection inlet of the
instrument when a compressor is used.
• If you intend to use an air compressor, select an oilless air compressor. Shimadzu offers 8
the SLP5D-2SV oilless and silent air compressor (P/N 042-70041-02) and AW30-02BGN
filter regulator (P/N 040-82118-23) as options.
• There are cases where the organic gas concentration is too high to be removed
completely by the gas purifier. Analysis accuracy is poor in atmospheres containing high
concentrations of volatile gases from exposed organic solvents and gasoline, or high
concentrations of automobile and diesel engine exhaust. If the possibility of the
presence of these kinds of gases cannot be avoided, use a filter to remove organic
particles and/or gases.
Using Gas Cylinder High Purity Nitrogen or Instrumentation High Purity Nitrogen
High purity nitrogen gas must be guaranteed to contain less than 1 ppm of each of the
following impurities: carbon dioxide, carbon monoxide, and hydrocarbons.
Install a pressure regulator on the cylinder and supply gas to the gas connection inlet
on the instrument at 200 ± 10 kPa.
These specifications limit the upper measurement concentration to 100 mg/L for TC and
NPOC. For sample measurements that exceed this concentration, measurement is possible
using the automatic dilution function if the concentration of the sample is less than
100 mg/L after dilution. Also note that TN measurement cannot be performed using the
TNM-L with these specifications.
Excessive impurities in the carrier gas will diminish analysis accuracy and prevent
the acquisition of sound measurement results.
Never allow the carrier gas supply pressure to exceed 600 kPa when using the
optional carrier gas regulator.
Procedure
1 Connect the half unions to the carrier gas inlet on the instrument and the
connection outlet (¼" NPT) of the gas supply source.
2 Connect the nylon tubing (4 mm OD, 2.5 mm ID) between the gas supply source
and the instrument.
To connect the nylon tubing, firmly insert it into the half union. To disconnect
the tubing, pull the tubing off while pushing down firmly on the blue ring of
the half union with a screwdriver.
Place the drain container under the bench on which the TOC-L is installed. A suitable
drain container is a plastic container with a 10 to 20 L capacity. The drain tubing from
the TOC-L is inserted into this drain container. Take note of the following precautions.
• As the flow resistance of the drain is low, lead the drain tubing from the instrument
in such a way that prevents any part of the tubing from pointing upwards and do not
allow the end of the drain tubing to become submerged in the drain container.
Exposing the drain tubing to atmospheric pressure near the TOC-L is also effective. Note
that high flow pressure in the drain may inhibit drain discharge and cause an overflow
within the TOC-L.
Figure 8.7 How to Lead the Drain Tubing from the Instrument to the Drain Container
This section describes how to connect the TOC-L and PC using the provided USB cable.
Connection Procedure
1 Insert one plug on the provided USB cable into the USB terminal on the rear of
the TOC-L. (Refer to "2.1.4 Rear View" P.8.)
2 Insert the other plug on the cable into the USB connector on the PC.
If the distance from the instrument is more than 100 mm, the water sampling
tube may impede the movement of the ASI-L arm resulting in operation errors
or damage to the instrument.
To prevent instrument damage, verify that the ASI-L arm is firmly attached to
the retaining bracket with the shipping screw before shipping the instrument
or moving it to another location.
8
Connecting Cables
The TOC-L and ASI-L are connected using cables, as described below.
Verify that the TOC-L is switched OFF before performing the following
procedure.
Procedure
1 Connect the provided cable to the connectors on the rear of the ASI-L and rear
of the TOC-L.
Connecting the Sample Tubing and Sparge Tubing (External Sparge Kit)
The procedure for connecting the ASI-L sample tubing and sparge tubing for the External
Sparge Kit is as follows.
Procedure
1 Attach the bush on the end of the water sampling tubing to port number 2 on
the 8-port valve of the sample injector on the TOC-L.
2 If using the external sparge kit, attach the sparging tubing for ASI-L.
Do not use the flow meter knob to turn off the sparge gas flow.
The sparge gas flow meter may break if the flow adjustment knob is
overtightened.
Verify that the TOC-L is switched OFF before performing the following
procedure.
2 Remove the needle holder retaining screw and then remove the needle holder
from the arm.
4 Secure the needle by turning the retaining bracket and tightening the screw at
the top of the needle holder.
There are two openings; the left opening is for the sample tubing and the right
opening is for the sparge tubing.
5 Feed the water sampling tubing through the hole in the needle cover and pull
it inside the needle cover. When using the external sparge kit, pull the sparging
tubing inside the needle cover in the same manner.
6 Fit the water sampling tubing or sparging tubing to the top of the needle and
attach a retainer.
7 Insert the bottom of the needle into the needle guide hole, run the needle holder
through the arm pin, and then secure the needle holder with the retaining screw.
2 Place the turntable so that the 3 guides on the ASI-L pass through the 3 holes
at the center of the turntable.
2 Rotate the vial rack until the guides of the turntable fit into the vial rack. This
secures the vial rack in place
There is a magnet at the left rear of the cover. Verify that the cover and ASI-L
are in contact at the magnet.
Preparation
• Use the rinse bottle provided as a standard accessory.
• Use either the drain container from the optional drain container set or another suitable
container. For the latter, use a plastic container with a 10 to 20 L capacity. For details
on installation and precautions, refer to "Installing the Drain Container" P.417. Such a
container of sufficient capacity can be used in conjunction with the drain container for
TOC-L.
Installation Procedure
1 Place the rinse bottle on the same table or bench as the TOC-L and ASI-L.
2 Insert the rinse tubing from the ASI-L into the rinse bottle.
Perform the checks described above to ensure that rinse water will be
delivered and air will not be taken into the TOC-L injection pump.
Installation Procedure
Place the 8-port sampler about 50 mm to the left of the TOC-L main unit, as shown in
"Figure 8.14 Installation of the OCT-L".
The unit is set up to the left of the TOC-L main body as shown in "Figure 8.14 Installation
of the OCT-L".
When 2 OCT-L 8-Port Samplers are to be used, place both units to the left of the TOC-L
main unit as shown in the overhead view of "Figure 8.4 External Dimensions of the
Instrument with the OCT-L 8-Port Sampler and TNM-L TN Unit (Units: mm)".
Cable Connections
The cable is connected between the main unit of the TOC-L and the OCT-L.
Confirm that the power to the TOC-L main unit is switched OFF before
performing this procedure.
Connection Procedure
1 Remove the 4 screws at the top of the OCT-L, and take off the cover.
2 Connect the provided OCT-L cable to the connector on the OCT-L board. Attach
the ground terminal of the power cable to the screw positioned next to the
ground label.
3 Feed the cable under the rear cover as shown in Figure 8.15 Cable Connections
and then reattach the cover to its original position.
4 Connect the other end of the OCT-L cable to the OCT-L connector on the rear
of the TOC-L main unit.
Installation Procedure
2 Connect the signal cable exiting OCT-L (2) to the connector of OCT-L (1).
3 Remove the port number label from the OCT-L (2) unit and replace it with the
port number label provided with the unit.
The port that was originally labeled as port No. 1 should be labeled as port No.
9.
Connection Procedure
1 Connect the bushing on the end of provided tubing (tubing with bushes on both
ends) to the common (COM) port on the OCT-L.
2 Feed the bushing on the other end of the tubing through the hole in the left
side of the TOC-L main unit and connect it to port number 2 (or port number 1
for OCT-L (2)) on the 8-port valve of the syringe pump type sample injector.
3 Connect the bushing on the ends of the water sampling tubing to ports 1 to 8
on the OCT-L (or ports 9 to 16 for OCT-L (2)).
The TNM-L incorporates an internal ozone generator, requiring a source of air gas
(supplied at about 500 mL/min) separate from the carrier gas supplied to the TOC-L.
While it is possible to use TOC-L high purity carrier gas by providing branch tubing, the
consumption of the combined-use carrier gas would increase to about
150 - 250 mL/min.
Assuming operation at the rate of 8 hours/day, 5 days/week, the 47 L, 12 MPa air cylinder
would require monthly replacement (as compared to every 3 months when used for
carrier gas alone).
Because air gas for ozone generation is not required to be the high purity air used as
carrier gas, it is recommended to use instrumentation air or compressor-supplied air for
ozone generation, separate from the carrier gas.
Using a High Purity Air-Filled Cylinder (Via Branch Tubing from Carrier Gas)
High purity air is synthesized air using pure nitrogen and pure oxygen. Ensure that
contaminants, including carbon dioxide, carbon monoxide and total hydrocarbons, are
guaranteed not to exceed 1 ppm each.
Install a pressure regulator on the gas cylinder and supply gas to the instrument so that
the pressure is 300 kPa at the instrument gas connection port.
If there are excessive contaminants in the carrier gas, measurement results will
be adversely affected due to low measurement reproducibility, etc.
• Make sure there are no open flames anywhere within 2 meters of a gas
cylinder.
• Secure cylinders with bands or other fasteners to prevent tipping and falling.
• When finished using gas, immediately and completely turn OFF all valves on
the cylinder.
• Inspect the operation of the pressure gauge at least once every three (3)
months.
If a supply pressure higher than 300 kPa is required when using compressed air
or instrument air, always keep it at 600 kPa or less.
Procedure
1 Connect the half unions to the carrier gas inlet on the instrument and the
connection outlet (¼" NPT) of the gas supply source.
2 Connect the nylon tubing (4 mm O.D., 2.5 mm I.D.) between the gas supply
source and the instrument.
The nylon tubing can be connected simply by firmly inserting it into the half
union. When disconnecting the tubing, pull off the tubing while pushing down
firmly on the green-colored ring of the half union using a screwdriver.
• To minimize resistance, leave the gas exhaust tubing open to the atmosphere.
• Be sure to connect the gas exhaust tubing to the instrument and discharge
the exhaust gas to the outdoors or an exhaust pit.
• If the gas exhaust tubing is not connected, ozone and NOx gas may be
exhausted from the instrument, causing harm to the respiratory organs of
individuals in the vicinity.
PRECAUTIONARY STATEMENTS
Avoid breathing
dust/fume/gas/mist/vapours/spray.
Avoid release to the environment if this is not
the intended use.
Do not eat, drink or smoke when using this
product.
In case of inadequate ventilation wear
respiratory protection as specified by the
manufacturer/supplier or the competent
<Prevention> authority.
Use only outdoors or in a well-ventilated area.
Wash thoroughly after handling.
Wear protective gloves and eye/face protection
as specified by the manufacturer/supplier or
the competent authority.
Wear respiratory protection as specified by the
manufacturer/supplier or the competent
authority.
Collect spillage.
Get medical attention/advice if you feel unwell.
SECTION II
HAZARDS If experiencing respiratory symptoms call a
IDENTIFICATION POISON CENTER or doctor/physician.
IF exposed: Call a POISON CENTER or
doctor/physician.
IF IN EYES: Rinse cautiously with water for
several minutes. Remove contact lenses, if
present and easy to do. Continue rinsing.
IF INHALED: Remove victim to fresh air and
keep at rest in a position comfortable for
breathing.
<Resoponse> IF ON SKIN (or hair): Remove/Take off
immediately all contaminated clothing. Rinse
skin with water/shower.
IF SWALLOWED: Rinse mouth. Do NOT induce
vomiting.
IF SWALLOWED: Call a POISON CENTER or
doctor/physician if you feel unwell.
Rinse mouth.
Specific treatment is urgent (see ... on this
label) .. reference to supplemental first aid
instruction if immediate administration of
antidote is required.
Wash contaminated clothing before reuse.
as Hydrogen chloride;
LDLo (orl,woman): 420 µL/kg (JJTOEX
9,351,1996)
ACUTE TOXICITY
LC50 (ihl,rat): 7004 mg/m3/30M (VCVN5* -, 383,
(oral/dermal/
1989)
inhalation)
TCLo (ihl,human): 50 mg/m3 (VCVN5* -, 383,
1989)
SKIN CORROSION/ Skin; human; 4 %/24H; Mild (BJDEAZ
IRRITATION 68,192,1988)
EYE DAMAGE/EYE Eye; rabbit, rinsed; 5 mg/30S; Mild (TXCYAC 23,
IRRITATION 281,1982)
RESPIRATORY OR
Not available
SKIN SENSITIZATION
Cytogenetic analysis; hamster; ovary; 8 mmol/L
GERM CELL (MUREAV 225,55,1989)
MUTAGENICITY DNA repair; E.coli; 25 µg/well (ENMUDM 3,
429, 1981)
SECTION XI
TOXICOLOGICAL TCLo (ihl,rat): 450 mg/m3/1H (female 1D pre):
TOXIC TO
INFORMATION Effects on Embryo or Fetus - fetotoxicity
REPRODUCTION
(AKGIAO 53 (6), 69,1977)
STOST-SINGLE
Not available
EXPOSURE
STOST-REPEATED
Not available
EXPOSURE
ASPIRATION
Not available
TOXICITY
CARCINOGENICITY Not available
ADDITIONAL INFORMATION ;
NTP Not listed
Not Classifiable as to Carcinogenicity to
IARC
Humans (Group 3)
OSHA Not listed
ACGIH Not listed
EPA GENETOX PROGRAM 1988, Negative: Cell
transform.-SA7/SHE
LC50 (starfish): 100 to 330 ppm (as Hydrogen
ECOTOXICITY
chloride)
PERSISTENCE AND
Not available
DEGRADABILITY
SECTION XII
ECOLOGICAL BIOACCUMULATIO
Not available
INFORMATION N POTENTIAL
MOBILITY IN SOIL Not available
OTHER ADVERSE
WGK; 1
EFFECTS
PRECAUTIONARY STATEMENTS
Do not eat, drink or smoke when using this product.
Wash thoroughly after handling.
Get medical attention/advice if you feel unwell.
Rinse cautiously with water for several
IF IN EYES minutes. Remove contact lenses, if present and
easy to do. Continue rinsing.
IF ON SKIN Gently wash with plenty of soap and water.
SECTION II
IF SWALLOWED Rinse mouth. Do NOT induce vomiting.
HAZARDS
IDENTIFICATION Store container tightly closed in well-ventilated place -if product
is as volatile as to generate hazardous atmosphere.
Dispose of contents/container to a located point (in accordance
with local/regional/national/international regulation).
EU
according to EC Directives
CLASSIFICATIONS
SYMBOL C
HAZARD
STATEMENTS, R34 Causes burns.
including R-phrase
CHEMILCAL
Phosphoric acid (min.85.0 %)
IDENTITY
Orthophosphoric acid, Hydrogen phosphate ;
SYNONYMS
Phosphoric Acid, Ortho
US REGULATIONS ;
CWA/311 Haz., NIOSH Recommend. Subst.,
CERCLA Haz. Subst., SARA III/313 Tox. Chem.,
DOT Haz. Mat.,
as Phosphoric acid;
DOT Haz. Sub. and Rep. Quant., Mass. Subst.
List , New Jers. RTK Haz. Subst. List , Penn.
Haz. Subst. List , Canad. WHMIS IDL 1 % conc.
CERCLA RQ= 1000 lb
EPCRA SECTION 313 de minimis concentration
is 1.0 %.
EPA
FIFRA 1988 PESTICIDE SUBJECT TO
REGISTRATION OR RE-REGISTRATION FIFRA
1998 ; RED Completed
OSHA TQ= Not listed
SECTION XV
REGULATORY NFPA HR= health-2, flam.-0, react.-0
INFORMATION EU REGULATIONS according to EC Directives
SYMBOL C
HAZARD
STATEMENTS, R34 Causes burns.
including R-phrase
ADDITIONAL
Harmful if inhaled and ingested. React with
HAZARD
most metals to form flammable hydrogen gas.
STATEMENTS
PRECAUTIONARY STATEMENTS, including S-phrase
S26 In case of contact with eyes, rinse immediately with plenty
of water and seek medical advice.
S45 In case of accident or if you feel unwell, seek medical advice
immediately
SECTION XVI
OTHER
INFORMATION
INCLUDING
No specific notes
INFORMATION ON
PREPARATION AND
REVISION
OF THE SDS
The above information is believed to be correct to be the best of our knowledge and
information but does not purport to be all inclusive and shall be used only as a guide.
This product is intended to be used by expert persons having chemical knowledge and skill,
at their own discretion and risk and Wako shall not be held liable for any damage resulting
from handling or from contact with the above material.
8.9.3 IC Reagent
HANDLING
• Avoid contact with eyes, skin, and clothes
due to the strongly acidity of the substance.
• Avoid inhalation of mist and vapor.
• Always wear suitable protective equipment
when working with this substance.
(Protective eyewear or face shield, protective
gloves, protective shoes, protective clothing
(all of which are acid resistant), and
protective breathing
equipment such as a gas mask for acidic
gases.)
• Always handle this material in well
ventilated areas.
• Avoid inhalation of mist or vapor in
insufficiently ventilated areas.
SECTION VII • Prevent the generation of mist and vapor as
HANDLING AND TECHNICAL much as possible and keep the work
STORAGE MEASURES environment within exposure limits.
• In order to prevent the accumulation of mist
and vapor in locations that generate these
states, implement measures to seal up
instruments or remove contaminated air
using exhaust equipment.
• Always seal the container opening to prevent
airborne droplets entering from clothing and
openings in footwear.
• Install facilities for emergency eye and body
washing near the area of handling and
clearly indicate the position of such facilities.
• Handle the container with care to prevent
breakage. Do not hold the container by the
plug or mouth.
• Do not topple over, shock, drag, or handle
the container in a similarly rough manner.
CHEMICAL
Stable under normal handling conditions.
STABILITY
Violently generates heat when material comes
into contact with alkaline substances due to
strong acidity.
Very stable at room temperature, does not
change state due to oxidizing or reducing
agents, and generally resists reduction by
carbon and hydrogen under 350 to 400 °C.
Generates toxic phosphorus oxide when heated
CHEMICAL to the point of decomposition.
REACTIVITY While a comparatively weak acid as an
aqueous solution, it will react with iron,
SECTION X
aluminum, and zinc to produce hydrogen and
STABILITY AND
generate each type of salt.
REACTIVITY
While the action of highly concentrated
phosphorus acid with respect to most metals
around room temperature is weak, it reacts
violently with many types of metals and their
oxides at high temperatures.
CONDITIONS TO
Direct sunlight, heat
AVOID
INCOMPATIBLE
Metals, alkaline substances
MATERIALS
HAZARDOUS
DECOMPOSITION Phosphorus oxide, hydrogen gas
PRODUCTS
Oral ingestion may cause nausea, vomiting,
ACUTE TOXICITY
abdominal pain, and bloody diarrhea.
SECTION XI Rat, oral LD50 1,530 mg/kg
TOXICOLOGICAL
INFORMATION Rabbit, skin LD50 2,740 mg/kg
Human,
TCL0 100 mg/m3
inhalation
LOCAL EFFECTS
Contact with the eyes causes irritation and
may cause conjunctival
hyperemia, corneal impairment, and iritis.
Contact with the skin and mucous membrane
IRRITATION
causes itching and pain
(SKIN, EYES)
and may cause soreness and inflammation.
In a mist or vapor state, causes irritation to the
eyes, skin, mucous
SECTION XI membrane, respiratory tract, and lungs.
TOXICOLOGICAL
CHRONIC AND
INFORMATION Repeated inhalation of mist or vapor may
LONG-TERM
cause bronchitis.
TOXICITY
CARCINOGENICIT
Not included on IARC and NTP lists.
Y
MUTAGENICITY Not available
TERATOGENICITY Not available
REPRODUCTIVE
Not available
TOXICITY
From its physicochemical properties, this
MOBILITY material has the potential to move into
atmospheric, aquatic, and soil environments.
RESIDUAL/RESOLVABILITY Not available
SECTION XII
ENVIRONMENTAL BIOACCUMULATION POTENTIAL Not available
INFORMATION
ECOTOXICITY
Hazardous to aquatic organisms.
TOXICITY TO
LD50 over 96 hours is 100-10 mg/L.
FISH
The fatal dose for fish is 135 mg/L.
The above information is believed to be correct to the best of our knowledge and according
to the information available but does not purport to be all inclusive and should only be
used as a guide.
While the above stated precautions only describe normal handling procedures, users should
implement safety measures that apply to any new applications that necessitate special
handling requirements.
All chemicals require handling with utmost care as there is always the possibility of
unknown hazards and toxicity. This product is intended for use at your own discretion and
risk and we request that you implement any necessary conditions for safe use.
GHS
Skin corrosion/irritation Category 1B
CLASSIFICATION
HAZARD
Causes severe skin burns and eye damage
STATEMENTS
PRECAUTIONARY STATEMENTS
Wear protective gloves and eye/face
protection.
Prevention
Wash thoroughly after handling.
Do not breathe dust
IF ON SKIN (or hair): Remove/Take off
immediately all contaminated clothing. Rinse
skin with water/shower.
IF IN EYES: Rinse cautiously with water for
several minutes. Remove contact lenses, if
present and easy to do. Continue rinsing.
CHEMILCAL
Soda lime
IDENTITY
FORMULA -
SECTION III MOLECULAR
-
COMPOSITION/ WEIGHT
INFORMATION
CAS NUMBER 8006-28-8
ON INGREDIENTS
TSCA INVENTORY Not listed (See Section 15)
EINECS No. Not listed
EC INDEX NUMBER Not listed
Wash off immediately with soap and plenty of
water. In the case of respirable dust and/or
fumes, use self-contained
GENERAL ADVICE
breathing apparatus and dust impervious
protective suit. Use personal protective
equipment.
Move victim to fresh air. If breathing is
difficult, give oxygen. If breathing has stopped,
administer artificial respiration.
INHALATION
Maintain normal body temperature with a
blanket. If irritation persists, transport to a
hospital immediately.
Remove contaminated clothes and shoes, rinse
SECTION IV skin with plenty of water or shower. Use soap
FIRST AID MEASURES SKIN CONTACT to help assure removal. If
irritation persists, transport to a hospital
immediately.
Remove any contact lenses at once. Flush eyes
well with flooding amounts of running water
for at least 15 minutes.
EYE CONTACT
Assure adequate flushing by separating the
eyelids with sterile fingers. If irritation persists,
transport to a hospital immediately.
Rinse mouth, give plenty of water to dilute the
substance. Do not induce vomiting. Never give
INGESTION anything by mouth to an
unconscious person. Transport to a hospital
immediately.
EXTINGUISHING Not combustible. Use extinguisnig media
MEDIA appropriate to the surrounding fire.
FIRE & EXPLOSION Toxic and irritating dust, fumes or smoke may
SECTION V
HAZARDS be emitted.
FIRE FIGHTING
MEASURES SPECIAL Firemen should wear normal protective 8
PROTECTIVE equipment (full bunker gear) and
EQUIPMENT FOR positive-pressure self-contained breathing
FIREFIGHTERS apparatus.
SECTION IX FLAMMABILITY
Not available
PHYSICAL AND (solid, gas)
CHEMICAL EXPLOSIVE LIMITS Not available
PROPERTIES
VAPOR PRESSURE Not available
SPECIFIC GRAVITY 2.1
SOLUBILITY IN
WATER Practically insoluble
PARTITION
Not available
COEFFICIENT
DECOMPOSITION
Not available
TEMPERATURE
CHEMICAL
Stable under recommended storage conditions.
STABILITY
CONDITIONS TO
Sunlight, heat, moisture
SECTION X AVOID
STABILITY AND INCOMPATIBILE
REACTIVITY Strong acids
MATERIALS
HAZARDOUS
DECOMPOSITION Not available
PRODUCTS
ACUTE TOXICITY
(oral/dermal Not available
/inhalation)
TOXICITY DATA Harmful if inhaled and ingested.
SKIN CORROSION/ May be harmful if absorbed through skin.
IRRITATION Causese skin burns.
EYE DAMAGE/EYE
Causes burns.
IRRITATION
RESPIRATORY OR SKIN SENSITIZATION Not available
SECTION XI GERM CELL MUTAGENICITY Not available
TOXICOLOGICAL
TOXIC TO REPRODUCTION Not available
INFORMATION
STOST-SINGLE EXPOSURE Not available
ASPIRATION TOXICITY Not available
CARCINOGENICITY Not available
ADDITIONAL INFORMATION
NTP Not listed
IARC Not listed
OSHA Not listed
ACGIH Not listed
ECOTOXICITY Not available
PERSISTENCE AND DEGRADABILITY Not available
SECTION XII
ECOLOGICAL BIOACCUMULATION POTENTIAL Not available
INFORMATION
MOBILITY IN SOIL Not available
OTHER ADVERSE EFFECTS Not available
Cautiously add to a large stirred excess of water. Adjusting the pH
to neutral, separate any insoluble solids or liquids and package them
SECTION XIII for hazardous-waste disposal. Flush the aqueous solutions down the
DISPOSAL drain with plenty of water. Any disposal practice must be in
CONSIDERATION compliance with country, local, state, and federal laws and
(INCLUDING regulations (contact country, local or state environmental agency for
CONTAINER) specific rules).
After contents are completely removed, dispose of its container in
accordance with local/regional/national/international regulation.
IATA
UN NUMBER UN3262
UN PROPER Corrosive solid, basic, inorganic, n.o.s.
SHIPPING NAME (Soda lime)
CLASS or
Corrosives. (Class 8)
DIVISION
The above information is believed to be correct to be the best of our knowledge and
information but does not purport to be all inclusive and shall be used only as a guide.
This product is intended to be used by expert persons having chemical knowledge and skill,
at their own discretion and risk and Wako shall not be held liable for any damage resulting
from handling or from contact with the above material. 8
Flash Point
This product is not flammable.
(Method used)
Special Fire and
None
Fighting Procedures
SECTION IV
Explosion Point
FIRE AND EXPLOSION N/A
(Method used)
HAZARD DATA
Unusual Fire and
None
Explosion Hazards
Extinguishing
N/A
Media
Stability Stable
Hazardous
Decomposition or None
SECTION V By-products
REACTIVITY DATA
Incompatibility
None
(Materials to avoid)
Conditions to Avoid None
Acute Hazard
Skin Contact May cause irritation.
Eye Contact May cause irritation, inflammation and rash.
Repeated, prolonged or excessive inhalation of
fiber may cause respiratory disease.
Chronic Hazard At this time there are no known published
reports demonstrating negative health
outcomes of workers exposed to ceramic fiber.
Other Precautions on Health Hazard
Perform periodic medical examination by X-ray
1. of the lung function of the workers who
handle this product.
Perform periodic monitoring of individual
exposure of workers who handle this product
2.
to check if exposure level is in compliance with
TLV.
Density N/A
Vapor Pressure N/A
SECTION IX
Strong acids, active halogens such as chlorine,
STABILITY AND INCOMPATIBILITIES
fluorine, iodine, and bromine. ammonia.
REACTIVITY
The above information is believed to be correct but does not
SECTION X purport to be all inclusive. It shall serve only as a guide. Shimadzu
SPECIAL shall not be held liable for any damage resulting from handling or
PRECAUTIONS AND contact with the above product. Users should make their own
COMMENTS determinations regarding the suitability of this information for their
particular purposes.
Classifica
CAS/EC/
Substance tion (EC) Concen
SECTION 3: Index/
name 1272/2008 tration
Composition/ REACH no
(CLP)
information on
ingredients Mixtures Aluminium 1344-28-1 100.00
-
oxide 215-691-6 %-b.w.
7440-06-4 2.50
Platinum -
231-116-1 %-b.w.
In case of persisting
adverse effects, consult a
General
physician. Change
information
contaminated, saturated
clothing.
Remove affected person
After inhalation from the immediate area.
Ensure supply of fresh air.
After skin Wash off immediately
Description of first
contact with soap and water.
aid measures
Separate eyelids, wash the
After eye
eyes thoroughly with
contact
water (15 min.).
SECTION 4:
First aid measures Seek medical advice
immediately. Rinse mouth
thoroughly with water.
After ingestion
Never give anything by
mouth to an unconscious
person.
Most important
symptoms and
No data available.
effects, both acute
and delayed
Indication of any
immediate medical
No data available.
attention and special
treatment needed
Suitable Foam; Carbon dioxide;
extinguishing Extinguishing powder;
media Water spray jet
Extinguishing media
Unsuitable
extinguishing No data available.
media
SECTION 5:
Firefighting measures In the event of fire, the following can be
Special hazards released: Carbon dioxide (CO2); Carbon
arising from the monoxide (CO); Combustion products of this
substance or mixture material have to be classed invariably as
respiratory poison.
Advice for Use self-contained breathing apparatus.
firefighters Wear protective clothing.
Refer to protective
measures listed in sections
For
7 and 8. Ensure adequate
non-emergency
Personal precautions, ventilation. Avoid dust
personnel
protective equipment formation. Keep away
and emergency from ignition sources.
procedures No data available.
For emergency Personal protective
SECTION 6: responders equipment (PPE) - see
Accidental release Section 8.
measures
Environmental Do not discharge into the drains/surface
precautions waters/groundwater.
Methods and
Take up mechanically. When collected,
material for
handle material as described under the
containment and
section heading "Disposal considerations".
cleaning up
Reference to other
No data available.
sections
No special measures
necessary if stored and
handled as prescribed.
Avoid the formation and
Advice on safe
deposition of dust.
handling
Provide good ventilation
at the work area (local
exhaust ventilation, if
necessary).
Do not eat, drink or
smoke during work time.
Keep away from
SECTION 7: Precautions for safe General
foodstuffs and beverages.
Handling and storage handling protective and
Wash hands before breaks
hygiene
and after work. Provide
measures
eye wash fountain in
work area. Do not inhale
dust.
Dust can form an
explosive mixture with air.
Advice on
Take precautionary
protection
measures against static
against fire and
charges. Keep away from
explosion
sources of heat and
ignition.
Technical
Keep container tightly
measures and
closed and dry in a cool,
storage
well-ventilated place.
conditions
Conditions for safe Requirements
SECTION 7: storage, including for storage Store product in closed
Handling and storage any incompatibilities rooms and containers.
vessels
Do not store together
Incompatible
with: oxidizing agents;
products
Acids; Alkalis
Specific end use(s) No data available.
Occupational exposure limit values
CAS no.:1344-28-1
EC no.:215-691-6
List of approved workplace
exposure limits (WELs) /
EH40:Aluminium oxides
total inhalable dust
Aluminium WEL long-term (8-hr TWA
oxide reference period):10 mg/m³
List of approved workplace
exposure limits (WELs) /
SECTION 8: EH40:Aluminium oxides
Exposure respirable dust
Control parameters
controls/personal WEL long-term (8-hr TWA
protection reference period):4 mg/m³
CAS no.:7440-06-4
EC no.:231-116-1
List of approved workplace
exposure limits (WELs) /
EH40:Platinum metal
Platinum WEL long-term (8-hr TWA
reference period):5 mg/m³
91/322/EWG:Platinum
(metallic)
WEL long-term (8-hr TWA
reference period):1 mg/m³
Appropriate
engineering No data available.
controls
Respiratory protection
If workplace exposure
limits are exceeded, a
respiration protection
approved for this
particular job must be
worn. In case of dust
formation, take
appropriate measures for
breathing protection in
the event that workplace
threshold values are not
specified.
Eye / face protection
Safety glasses (EN 166)
Hand protection
In case of intensive
contact, wear protective
gloves (EN 374). Sufficient
protection is given
wearing suitable
protective gloves checked
SECTION 8: according to i.e. EN 374,
Exposure in the event of risk of
Exposure controls skin contact with the
controls/personal Personal
protection product. Before use, the
protective
protective gloves should
equipment
be tested in any case for
its specific work-station
suitability (i.e. mechanical
resistance, product
compatibility and
antistatic properties).
Adhere to the
manufacturer’s
instructions and
information relating to
the use, storage, care and
replacement of protective
gloves. Protective gloves
shall be replaced
immediately when
physically damaged or
worn. Design operations
thus to avoid permanent
use of protective gloves.
Other
Normal chemical work
clothing.
Environmental exposure
controls
No data available.
granules
Form/Colour
black; grey
Odour odourless
Odour threshold No data available.
pH value No data available.
Boiling
point/boiling No data available.
range
Melting
point/melting No data available.
range
Decomposition
point/
No data available.
decomposition
range
Flash point Not applicable.
Auto-ignition
No data available.
temperature
Oxidising
No data available.
properties
Explosive
No data available.
Information on basic properties
SECTION 9: physical and chemical
Physical and chemical properties Flammability
No data available.
properties (solid, gas)
Lower
flammability or No data available.
explosive limits
Upper
flammability or No data available.
explosive limits
Vapour pressure No data available.
Vapour density No data available.
Evaporation rate No data available.
Relative density No data available.
Density No data available.
Value
Bulk density
710-770 g/l
Solubility in Comments
water insoluble 8
Solubility(ies) No data available.
Partition
coefficient: No data available.
n-octanol/water
Viscosity No data available.
Other information No data available.
Toxicity to fish
No data available.
(acute)
Toxicity to fish
No data available.
(chronic)
Toxicity to
No data available.
Daphnia (acute)
Toxicity Toxicity to
No data available.
Daphnia (chronic)
Toxicity to algae
No data available.
(acute)
Toxicity to algae
No data available.
(chronic)
SECTION 12:
Bacteria toxicity No data available.
Ecological
information Persistence and
No data available.
degradability
Bioaccumulative
No data available.
potential
Mobility in soil No data available.
Results of PBT and
No data available.
vPvB assessment
Other adverse effects No data available.
Ecological data are not
available.
Other
Other information Do not discharge product
information
unmonitored into the
environment.
Allocation of a waste
code number, according
to the European Waste
Product Catalogue, should be
carried out in agreement
with the regional waste
disposal company.
Regulation (EC)
No 1907/2006
(REACH) Annex
According to the data
XVII:
available and/or
RESTRICTIONS
specifications supplied by
ON THE
upstream suppliers, this
MANUFACTURE,
product does not contain
PLACING ON
any substances
THE MARKET
Safety, health and requiring authorisation as
AND USE OF
environmental listed on Annex XVII of
CERTAIN
regulations/legislation DANGEROUS the REACH regulation (EC)
SECTION 15: specific for the 1907/2006.
SUBSTANCES,
Regulatory substance or mixture PREPARATIONS
information EU regulations AND ARTICLES
Directive
2012/18/EU on
the control of
major-accident This product is not subject
hazards to Part 1 or 2 of Annex I.
involving
dangerous
substances
Chemical safety
No data available.
assessment
Regulation (EC) No 1907/2006 (REACH),
1272/2008 (CLP) as amended in each case. EC
Directives 2000/39/EC, 2006/15/EC,
2009/161/EU
Sources of key data National Threshold Limit Values of the
used to compile the corresponding countries as amended in each
data sheet case. Transport regulations according to ADR,
RID, IMDG, IATA as amended in each case.
The data sources used to determine physical,
toxic and ecotoxic data, are indicated directly
in the corresponding chapter.
UMCO GmbH
Georg-Wilhelm-Str. 187, D-21107 Hamburg
SECTION 16:
Tel.: +49 40 / 555 546 300 Fax: +49 40 / 555
Other information
546 357 e-mail: umco@umco.de
This information is based on our present
knowledge and experience.
The safety data sheet describes products with
Department issuing a view to safety requirements.
safety data sheet It does not however, constitute a guarantee
for any specific product properties and shall
not establish a legally valid contractual
relationship.
8
Document protected by copyright.
Alterations or reproductions require the
express written permission of UMCO GmbH.
Prod-ID 40074
Japanese regulations
Fire Service Act Not applicable
Substances Control
CAS No. 7664-38-2
Harmful Substances Whose Names Are to be
Indicated on the Label (Law Art.57, Para.1,
Act Industrial Enforcement Order Art.18)
SECTION XV Safety and CAS No. 7664-38-2
REGULATORY Health Act Notifiable Substances (Law Art.57-2,
INFORMATION Enforcement Oder Art.18-2 Attached Table No.
9)
No.618
Pneumoconiosis CAS No. 91053-39-3
Act Law number: Act No. 30 of 1960
Ship Safety Act Not applicable
Civil Aeronautics
Not applicable
Law
SECTION XVI
No specific notes
OTHER INFORMATION
The above information is believed to be correct to be the best of our knowledge and
information but does not purport to be all inclusive and shall be used only as a guide. This
product is intended to be used by expert persons having chemical knowledge and skill, at
their own discretion and risk and We shall not be held liable for any damage resulting
from handling or from contact with the above material.
Acute toxicity
Oral Classification not possible
Dermal Classification not possible
nhalation
No classification
(Gases)
Inhalation
No classification
(Vapors)
Inhalation
Classification not possible
(Dusts/Mists)
Skin corrosion/
Classification not possible
Irritation
Serious eye
damage/eye Classification not possible
irritation
Sensitization
Respiratory Classification not possible
Skin Classification not possible
Germ cell
Classification not possible
mutagenicity
Carcinogenicity Not classified
Reproductive
SECTION II Classification not possible
toxicity
HAZARD
IDENTIFICATION Specific target
organ systemic
Classification not possible
toxicity (Single
exposure)
Specific target
organ systemic
toxicity Classification not possible
(Repeated
exposure)
Aspiration
Classification not possible
hazard
Aquatic environment
Acute hazard Classification not possible
Chronic hazard Classification not possible
Other hazards
which do not result No information available
in GHS classification 8
Important
No information available
symptoms
Summary of
No information available
assumed emergency
National or
regional Refer to [15. Regulatory Information]
information
Classification of the
chemical substance Single product
or/mixture
Chemical name or
Silica, vitreous
common name
Synonyms Silica Glass
Concentration or concentration range
Chemical name
or common Silica, vitreous
name
Abbreviation -
Concentration or
concentration More than 99.99 %
range
Japanese Chemical Substances
(1)-548
Reference Control Law (JCSCL)
SECTION III
number in Existing
COMPOSITION / Japanese Industrial Safety and
Gazetted List chemical
INFORMATION ON Health Law
INGREDIENTS substances
CAS No 60676-86-0
Chemical formula <Silica, vitreous> SiO2
Component subject to regulation
Ingredient Silica, vitreous
Japanese Japanese Industrial Safety and Health Law
Industrial Safety (Article 57-2 of the Law) -MSDS require
and Health Law Number 312
Japanese PRTR
Law (Pollutant Not applicable to the specified chemical
Release and substances of Japanese PRTR Law
Transfer Register
Impurities and
stabilizing additives
which contribute to No information available
the classification of
GHS
Domestic
Refer to laws and regulation that are applied.
regulations
Special precautions No information available
Load so that there will be no tumbling,
dropping or damaging, and securely conduct
SECTION XIV load collapse prevention.
TRANSPORT At the time of transportation by vehicles,
INFORMATION Special precautions always have the driver carry yellow cards.
and conditions in In order to prevent mingling of foreign matter
transport and wetting with water, cover the goods with
a sheet.
In case of bulky loading, in order to prevent
load collapse, keep the stack lower or fix the
goods in position
Substances to be notified, which are specified
SECTION XV in Article 57 Item 2 of the Japanese Law on
REGULATORY <Silica, vitreous> Industrial Safety and Hygiene
INFORMATION Waste Management and Public Cleansing Law
(Industrial Wastes)
References
Journal of Occupational Health Vol. 55 (2013)
List of Chemical Substances Classified based on
GHS Classification - GHS Classification Results,
SECTION XVI National Institute of Technology and
OTHER INFORMATION <Silica, vitreous> Evaluation (NITE)
ACGIH,TLVs and BEls Based on the
Documentation of the Threshold Limit Values
for Chemical Substances and Physical Agents &
Biological Exposure Indices (2013)
The information contained herein is prepared based on the available information to Tosoh
that is believed to be reliable: however the information is provided by Tosoh WITHOUT
ANY REPRESENTATION OR WARRANTY, EXPRESSED OR IMPLIED, AS TO ITS COMPLETENESS,
COMPREHENSIVENESS AND ACCURACY.
Since the conditions of handling, storage and disposal of this material are beyond our
control, it is the responsibility of the user to determine whether the material is fit for a
particular purpose and / or suitable for the user’s method of use or application, and to
determine safe conditions for use of the material, and to assume full responsibility for loss,
injury and expense arising out of or in connection with the use of material. NO
REPRESENTATION OR WARRANTY, EXPRESS OR IMPLIED, REGARDING THE MATERIAL
DESCRIBED HEREIN SHALL BE CREATED BY OR INFERRED FROM ANY STATEMENT OR
OMISSION FROM THIS MSDS.
Various government agencies and local authorities may have general or specific regulations
applicable to the material which may not be covered in this MSDS. It is sole responsibility
of the user to examine and confirm for its full compliance with any such regulations.
When the revision of this SDS is received, please dispose of the old one.
C G
Carrier Gas Pressure and Flow Rate Settings 95 Gas Sample Analysis 310
Catalyst Filling 19
Catalyst Regeneration 320 H
Changing the Graph Display 224 High Sensitivity Analysis 68
Checking Acid 317 High Sensitivity ASI-L Analysis 87
Checking Dilution Water 317 High Sensitivity Using the OCT-L 93
Checking Drain Vessel Water Level 318 History 357
Checking Humidifier Water Level 318
Clearing Analysis Results 233 I
Connecting 117 IC Analysis Preparations 55
Connecting the Combustion Tube 26 Initialize ASI/8Port Sampler 356
Consumable Parts 405 Inserting a Control Sample 202
Copying, Cutting and Pasting 217 Inserting a Sample 195
Creating a Calibration Curve File 147 Inserting a Schedule 208
Creating a Control Sample File 166 Inserting a Standard Solution 194
Creating a Method 158 Inserting Multiple Samples with the Same Analysis
Creating a New System Configuration 124 Parameters 203
Creating a Sample Table 146 Inspecting the Chemiluminescence Detector 348
Creating a Schedule 174 Inspecting the Liquid 319
Installation 411
D Installation of the CO2 Absorber 48
Daily Inspection 317 Installing the ASI-L 419
decimal places 293 Installing the Needle 421
Decimal Point Display 293 Installing the Suspended Solids Kit 51
Default Analysis Parameters 297 Installing the TNM-L 429
Deleting a Sample 220 Instrument Connection 253
Deleting a System Configuration 137
Disconnection 253 L
Display of Selected Windows 291 Locking the Sample Table Editor 294
displaying the File Information 221 Login 294
during analysis by changing to the Edit Mode 270
Z
Zero Point Detection 352