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638-94834

Apr. 2021

Total Organic Carbon Analyzer

TOC-LCPH/CPN

User's Manual
LabSolutions TOC Volume
Read this manual thoroughly before you use the product.
Keep this manual for future reference.
This page is intentionally left blank.
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.

ã 2021 Shimadzu Corporation. All rights reserved.


Original version is approved in English.

TOC-LCPH/CPN LabSolutions TOC Volume i


Introduction

Indications Used in This Manual


Cautions and Notes are indicated using the following conventions:

n Precautionary Conventions Used in this Manual

The following precautionary conventions are used 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.

n Other Conventions Used in this Manual

Instrument Model Names


Descriptions in this documentation pertain to two models of the TOC-L Total Organic
Carbon Analyzer, namely the TOC-LCPH and TOC-LCPN. These models will be referred to in
relevant descriptions as the H Type and N Type, respectively.

Supplementary Conventions
The following symbols are used in this manual:

Convention Description

Indicates an action that must not be performed.

Indicates an action that must be performed.

Indicates information provided to improve product performance.

Indicates the location of related reference information.

ii TOC-LCPH/CPN LabSolutions TOC Volume


Safety Instructions

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

This instrument is a total organic carbon analyzer.


Use this instrument ONLY for the intended purpose.
Using this instrument for any other purpose could cause accidents.

n Installation Site

Do not install this product at a site where fire is prohibited.

n Installation

To ensure safe operation, contact your Shimadzu representative if product


installation, adjustment, or re-installation (after the product is moved) is
required.

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.

Do not measure or inject explosive, ignitable, or flammable materials into the


instrument.

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Introduction

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.

Emergency Stop Procedure

1 Close the main valves on the gas cylinders.

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.

3 Unplug the power cable.

n During a Power Outage

Take the following measures in the event of a power outage.

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.

n Warning Labels and Residual Risks

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.

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Safety Instructions

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Introduction

No. Description Protective Measure


The area near the center of the electric
furnace becomes extremely hot when the
furnace is heating up and when the furnace
has reached operating temperature (680 °C
High temperature caution
1 or 720 °C). Do not touch the electric furnace
Risk of burn
as this could result in burns. Allow the
furnace to cool before performing any
maintenance on the combustion tube or
catalyst.
High temperature caution Cool down the furnace sufficiently before
2
Risk of burn performing maintenance.
Electric shock caution
3 Do NOT remove the panel.
Risk of electric shock

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Safety Instructions

No. Description Protective Measure


Corrosion hazard Soda lime is a corrosive chemical substance.
4 Soda lime is a corrosive chemical Be careful not to touch or spill it. For details,
substance. see "8.9 Safety Data Sheets (SDS)" P.433.
During operation, the pressure in the CO2
absorber of the gas purifier is about 200 kPa.
To prevent injuries, turn off the carrier gas
High pressure caution and switch off the power to the TOC main
5
Risk of injury unit. Wait until the pressure inside the
container and the instrument flow lines
return to normal atmospheric pressure
before performing any maintenance.

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Introduction

No. Description Protective Measure


Acid and other corrosive substances are
present in the liquid waste drained from this
instrument. Be careful to not touch or spill
the liquid waste. Liquid waste may have a
pH level less than 2.0 depending on
measurement conditions. Liquid waste with a
Corrosion hazard pH less than 2.0 is classed as industrial waste
6 The liquid waste may contain subject to special control. Request transfer by
corrosive substances. an authorized industrial waste transporter to
an authorized industrial waste processing
facility to process any industrial waste
subject to special control.
If you wish to perform deacidification on
your own premises, contact the
environmental agency in your jurisdiction.

No. Description Protective Measure


Acid and other corrosive substances are
present in the liquid waste drained from this
instrument. Be careful to not touch or spill
the liquid waste. Liquid waste may have a
pH level less than 2.0 depending on
measurement conditions. Liquid waste with a
Corrosion hazard pH less than 2.0 is classed as industrial waste
7 The liquid waste may contain subject to special control. Request transfer by
corrosive substances. an authorized industrial waste transporter to
an authorized industrial waste processing
facility to process any industrial waste
subject to special control.
If you wish to perform deacidification on
your own premises, contact the
environmental agency in your jurisdiction.

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Safety Instructions

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Introduction

No. Description Protective Measure


There is a risk of corrosive substance leakage.
Corrosion hazard
Securely connect the Y-shaped fitting to the
8 The liquid waste may contain
tip of the tubing. Be careful not to contact
corrosive substances.
or spill the liquid.
The IC reaction solution contains corrosive
Corrosion hazard
(acidic) phosphoric acid. Be careful not to
9 The IC reaction solution is a corrosive
touch or spill it. For details, see "8.9 Safety
chemical substance.
Data Sheets (SDS)" P.433.
Hydrochloric acid is a corrosive chemical
Corrosion hazard
substance. Be careful not to touch or spill it.
0 Hydrochloric acid is a corrosive
For details, see "8.9 Safety Data Sheets
chemical substance.
(SDS)" P.433.

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Warranty

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.

(1) Improper product handling

(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

(7) Reasons unrelated to the product itself

(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

(10) Product movement or transportation after installation

(11) Consumable items


Recording media such as floppy disks and CD-ROMs are considered consumable items.

* 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.

TOC-LCPH/CPN LabSolutions TOC Volume xi


Introduction

After-Sales Service and Availability of Replacement Parts


n After-Sales Service

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.

n Replacement Parts Availability

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.

Maintenance, Inspections, and Adjustment


In order to maintain the instrument's performance and obtain accurate measurement
data, daily inspection and periodic inspection are necessary.
• For daily maintenance and periodic inspection, see "7 Maintenance".
• For consumable parts and maintenance parts, see "8 Reference Information".
The replacement cycle for each part is given at a rough estimate.
Replacement may be required earlier than the replacement cycle depending on the
environment and frequency of usage.

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Disposal Precautions

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.

For California, USA Only


This product contains a battery that contains perchlorate material.
Perchlorate Material - special handling may apply.
See www.dtsc.ca.gov/hazardouswaste/perchlorate

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Introduction

Electromagnetic Compatibility
This instrument complies with European standard EN50011 class A for electromagnetic
emission and EN61326-1 for electromagnetic immunity.

EN55011 Emissions (Electromagnetic Interference)


This instrument complies with European EMI (Electro Magnetic Interference) standard
EN55011 class A equipment. This instrument can be used in any environment except in
the home.

When an electromagnetic disturbance occurs due to nearby this instrument,


provide an appropriate distance between instruments to eliminate the
disturbance.
In addition, please connect this instrument to a large power supply of the
capacity as much as possible.

EN61326-1 Immunity (Electromagnetic Susceptibility)


This instrument complies with European standard EN61326-1 for electromagnetic
immunity.
Stated below are the test conditions.

IEC 61000-4-2 Electrostatic Discharge Air: 8 kV, Direct: 4 kV


IEC 61000-4-3 Radiated, Radio-Frequency, 10 V/m (0.08-1 GHz), 3 V/m (1.4-2 GHz),
Electromagnetic Field 1 V/m (2-2.7 GHz)
IEC 61000-4-4 Transient/Burst
2.0 kV to AC power line and ground
(Electrical Fast Transients)
IEC 61000-4-5 Voltage Surge 1.0 kV line to line, 2 kV line to ground
IEC 61000-4-6 Conducted RF Immunity 3 Vrms (150 kHz-80 MHz)
0 % UT 1 cycles (20 ms),
IEC 61000-4-11 Voltage Variations/Dips/Interrupts 70 % UT 25 cycles (500 ms),
0 % UT 250 cycles (5000 ms)

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.

To above electromagnetic disturbances, follow the recommendations below.

(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.

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Contents of This Manual

Contents of This Manual

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.

3 Preparation for Measurement


This chapter describes the procedures for preparing the instrument, optional accessories
and samples for measurement.

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.

6 Analysis with Special Options


This chapter describes measurement procedures using the optional manual injection kit.

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.

TOC-LCPH/CPN LabSolutions TOC Volume xv


Contents
Introduction Indications Used in This Manual ......................... ii
Safety Instructions ............................................. iii
Warranty .......................................................... xi
After-Sales Service and Availability of
Replacement Parts ............................................ xii
Maintenance, Inspections, and Adjustment ......... xii
Disposal Precautions ........................................ xiii
Electromagnetic Compatibility .......................... xiv
Contents of This Manual .................................. xv

1 Overview 1.1 Overview ............................................................ 1


1.2 Operational Precautions ....................................... 2

2 System Description 2.1 TOC-LCPH/CPN Construction ..................................... 6


2.1.1 Front View ...................................................... 6
2.1.2 Right Side View ................................................. 7

2.1.3 Left Side View .................................................. 8


2.1.4 Rear View ....................................................... 8
2.1.5 Front Internal View (Left Diagonal) ............................ 9
2.1.6 Top Internal View (Left Diagonal) .............................. 9

2.1.7 Flow Diagram ................................................. 10


2.2 Autosampler ASI-L (Option) ................................ 15
2.2.1 Front View (Left Diagonal) .................................... 15

2.2.2 Rear View (Left Diagonal) .................................... 15


2.3 8-Port Sampler OCT-L (Option) ........................... 16
2.3.1 Front View (Left Diagonal) .................................... 16

2.3.2 Rear View (Right Diagonal) ................................... 16


2.4 TN Unit TNM-L (Option) .................................... 17
2.4.1 Front View (Right Diagonal) .................................. 17
2.4.2 View Inside the Door on the Right Side .................... 17
2.4.3 Rear View ..................................................... 18

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Preparation for 19
3 Measurement
3.1 Instrument and Sample Preparation ....................

3.1.1 Catalyst Filling ................................................. 19

3.1.2 Installing the Cooling Tube Unit (H Type Only) ............. 25


3.1.3 Connecting the Combustion Tube ............................ 26

3.1.4 Connecting the Halogen Scrubber ............................ 38

3.1.5 Installing the Syringe .......................................... 39

3.1.6 Water Supply to the Cooler Drain Vessel .................... 43

3.1.7 Filling the Humidifier with Water ............................ 44


3.1.8 Preparation of Dilution Water ................................ 45
3.1.9 Acid Preparation ............................................... 46

3.1.10 Installation of the CO2 Absorber ............................. 48

3.1.11 Adjusting Sparge Gas Flow Rate ............................. 49


3.1.12 Installing the Suspended Solids Kit ........................... 51
3.1.13 Preparing the High Suspension Kit (When Using the
Optional High Suspension Kit) ................................ 53

3.1.14 IC Analysis Preparations ....................................... 55


3.1.15 Preparation for POC Analysis (When Using the Optional
POC Kit) ....................................................... 58
3.1.16 TN Analysis Preparation (When Using the Optional
TNM-L TN Unit) ............................................... 60
3.1.17 B-Type Halogen Scrubber (When Using the Optional
B-Type Halogen Scrubber) .................................... 61
3.1.18 Preparation and Storage of Standard Solutions .............. 64

3.1.19 Sample Preparation ............................................ 68

3.1.20 Sample Preparation for Autosampler Measurement .......... 80

3.1.21 OCT-L (8-Port Sampler) Measurement ........................ 92


3.1.22 Starting Up the Instrument ................................... 94

4 Analysis Procedure 4.1 Analysis Flow .................................................... 99


4.1.1 Checks Before Analysis ....................................... 99
4.1.2 Turning on the Instrument .................................. 100

4.1.3 Opening the Sample Table Editor .......................... 101


4.1.4 Creating a Sample Table .................................... 103

4.1.5 Creating an Analysis Parameters File ....................... 104


4.1.6 Editing the Sample Table ................................... 114
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4.1.7 Entering the Vial Numbers .................................. 116

4.1.8 Connecting to the Instrument .............................. 117


4.1.9 Conducting Analysis ......................................... 118

4.1.10 Viewing and Outputting Analysis Results ................... 121

4.1.11 Ending Analysis .............................................. 123

5 Software Operation 5.1 System Configuration ....................................... 124


5.1.1 Creating a New System Configuration ..................... 124
5.1.2 Reviewing and Editing a System Configuration ............ 134
5.1.3 Deleting a System Configuration ........................... 137
5.1.4 Viewing the System Configuration File Log ................ 138

5.2 Sample Table Editor ......................................... 139


5.2.1 Opening the Sample Table Editor .......................... 139
5.2.2 Exiting the Sample Table Editor ............................ 139
5.2.3 Sample Table Editor Window Components ................. 140

5.2.4 Sample Table Columns ...................................... 141

5.2.5 Sample Window Columns ................................... 143

5.2.6 File Types Used .............................................. 145

5.3 Creating and Editing Files ................................ 146


5.3.1 Creating a Sample Table .................................... 146

5.3.2 Creating a Calibration Curve File ........................... 147

5.3.3 Creating a Method .......................................... 158

5.3.4 Creating a Control Sample File ............................. 166

5.3.5 Creating a Schedule ......................................... 174

5.3.6 Reviewing and Editing a Sample Table ..................... 175

5.3.7 Reviewing and Editing a Calibration Curve ................ 176


5.3.8 Reviewing and Editing a Method ........................... 183

5.3.9 Reviewing and Editing a Control Sample .................. 188


5.3.10 Reviewing and Editing a Schedule .......................... 190

5.3.11 Opening an Existing File .................................... 190


5.4 Editing a Sample Table .................................... 194
5.4.1 Inserting a Standard Solution ............................... 194

5.4.2 Inserting a Sample .......................................... 195

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5.4.3 Inserting a Control Sample ................................. 202


5.4.4 Inserting Multiple Samples with the Same Analysis
Parameters ................................................... 203

5.4.5 Inserting a Schedule ......................................... 208

5.4.6 Vial Numbers ................................................ 210


5.4.7 Editing Sample Analysis Parameters ......................... 214

5.4.8 Copying, Cutting and Pasting Data ........................ 217


5.4.9 Deleting a Sample ........................................... 220

5.4.10 Adding a Comment to File Information .................... 221

5.5 Reviewing and Editing Measurement Data ........ 222


5.5.1 Sample Window ............................................. 222

5.5.2 Reviewing and Editing Sample Analysis Parameters ........ 226

5.5.3 Reviewing the Calibration Curve ............................ 227

5.5.4 Editing the Calibration Curve ............................... 228

5.5.5 Excluding Injection Results .................................. 231


5.5.6 Recalculating Results ........................................ 231
5.5.7 Clearing Analysis Results .................................... 233
5.6 Sample Table Data Output and Printing ............ 234
5.6.1 Selecting Content to Print .................................. 234
5.6.2 Print Setup .................................................. 239
5.6.3 Print Preview ................................................ 239
5.6.4 Printing ...................................................... 243
5.6.5 Selecting Content for ASCII Export ......................... 246

5.6.6 Exporting to ASCII Format .................................. 249


5.6.7 Exporting a Schedule File ................................... 251
5.6.8 Exporting a Runtime Report ................................ 252
5.7 Operation and Analysis .................................... 253
5.7.1 Instrument Connection and Disconnection ................. 253
5.7.2 Background Monitor ......................................... 257

5.7.3 Analysis with an ASI-L or OCT-L ........................... 261


5.7.4 Analysis without an ASI-L or OCT-L ........................ 263

5.7.5 Stopping Analysis ............................................ 269

5.7.6 Editing the Sample Table during Analysis .................. 270

5.7.7 Instrument Shutdown ....................................... 271


5.7.8 Instrument Validation ........................................ 276

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5.7.9 Maintenance Operations ..................................... 282

5.8 Display Options ............................................... 282


5.8.1 Sample Table ................................................ 282
5.8.2 Sample Window Display Options ........................... 285
5.8.3 File Viewer Display Options ................................. 288

5.8.4 Setting the Display Font of the Output Window .......... 289

5.8.5 Display of Selected Windows ............................... 291


5.8.6 Display Font ................................................. 292
5.8.7 Decimal Point Display ....................................... 293
5.9 Security Functions ............................................ 294
5.9.1 Login ......................................................... 294

5.9.2 Locking the Sample Table Editor ........................... 294


5.9.3 Releasing Time Out Lock ................................... 295
5.9.4 Recording the Operation History ............................ 296

5.9.5 Other Security Functions .................................... 296


5.10 Other Functions ............................................... 297
5.10.1 Default Analysis Parameters ................................. 297

5.10.2 Converting and Outputting Measurement Values .......... 298


5.10.3 Online Manual ............................................... 300

5.10.4 Version Information ......................................... 301

Analysis with 302


6 Special Options
6.1 Manual Injection Measurement (H Type Only) ...

6.1.1 Analysis Preparation ......................................... 302


6.1.2 Measurement ................................................ 304
6.1.3 Precautions for Low Concentration Samples ............... 308
6.1.4 Manual Injection Kit Maintenance .......................... 309
6.2 Gas Sample Analysis ......................................... 310
6.2.1 Precautions for Gas Sample Analysis ....................... 310
6.2.2 Analysis Preparation ......................................... 310
6.2.3 Measurement ................................................ 311
6.2.4 Manual Injection Kit Maintenance .......................... 315

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7 Maintenance 7.1 Daily Inspection ............................................... 317


7.1.1 Checking Dilution Water .................................... 317

7.1.2 Checking Acid ............................................... 317

7.1.3 Checking Drain Vessel Water Level ......................... 318

7.1.4 Checking Humidifier Water Level ........................... 318


7.1.5 Inspecting the Liquid in the B-Type Halogen Scrubber
(Option) ...................................................... 319

7.2 Periodic Inspections .......................................... 320


7.2.1 Catalyst Regeneration ....................................... 320
7.2.2 Washing or Replacing Catalyst ............................. 322
7.2.3 Replacing the Carrier Gas Purification Tube and
Catalyst ...................................................... 325
7.2.4 Washing/Replacing the Combustion Tube and Carrier
Gas Purification Tube (Option) .............................. 326

7.2.5 Replacing the High Purity Air (Filling the Cylinder) ........ 327

7.2.6 Replacing the CO2 Absorber ................................ 327

7.2.7 Replacing the Halogen Scrubber ............................ 327

7.2.8 Syringe Replacement ........................................ 329


7.2.9 Syringe Plunger Tip Replacement ........................... 331
7.2.10 Replacing the Sliding Sample Injector O-rings ............. 333
7.2.11 Replacing the Syringe Pump 8-port Valve Rotor ........... 334
7.2.12 Replacing the CO2 Absorber for the Optional Carrier
Gas Purifier .................................................. 336

7.2.13 Replenishing IC Reaction Solution .......................... 338


7.2.14 Replacing the Pump Head of the IC Reaction Solution
Pump ........................................................ 338
7.2.15 Replacing the Filler of the Optional POC Analysis CO2
Absorber ..................................................... 339
7.2.16 Replacing the Liquid in the B-Type Halogen Scrubber
(Option) ...................................................... 340

7.3 Autosampler (ASI-L) Maintenance ...................... 341


7.3.1 Rinse Bottle Inspection ...................................... 341
7.3.2 Sample Catcher Inspection .................................. 341

7.3.3 Replacing the Pump Head of the Rinse Pump ............. 342

7.4 8-Port Sampler (OCT-L) Maintenance ................. 343


7.4.1 Replacing the 8-Port Valve Rotor ........................... 343

7.5 TN Unit (TNM-L) Maintenance .......................... 346


7.5.1 Replacing the Catalyst in the Ozone Treatment Unit ...... 346
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7.5.2 Inspecting the Chemiluminescence Detector and


Replacing the Ozone Generator ............................ 348
7.5.3 Replacing the NOx Absorber ................................ 350

7.6 Maintenance Menus ......................................... 351


7.7 Troubleshooting ............................................... 359
7.7.1 Error Messages .............................................. 359
7.7.2 Troubleshooting .............................................. 367

Reference 381
8 Information
8.1 Principles of Analysis ........................................

8.1.1 Principles of TC (Total Carbon) Analysis ................... 381


8.1.2 Principles of IC (Inorganic Carbon) Analysis ................ 382
8.1.3 Principles of NPOC (Non-Purgeable Organic Carbon)
Analysis ...................................................... 383
8.1.4 Principles of POC (Purgeable Organic Carbon) Analysis ... 384
8.1.5 Principles of Measuring TOC ................................ 385

8.1.6 Principles of Measuring TN (Total Nitrogen) ............... 386


8.2 Analysis-Related Technical Information .............. 387
8.2.1 Peak Area Analysis .......................................... 387
8.2.2 Peak Shape .................................................. 388
8.2.3 Calibration Curves ........................................... 389

8.2.4 Sparging During Standard Solution Analysis ................ 391

8.2.5 Automatic Selection of Optimum Calibration Curve ....... 392


8.2.6 Automatic Correction for Injection Volume and Dilution
Factor ........................................................ 393
8.2.7 Multi-Stage Injection ........................................ 393
8.2.8 Pharmaceutical Water Testing ............................... 394

8.3 Specifications ................................................... 395


8.3.1 TOC-LCPH/CPN ................................................. 395
8.3.2 ASI-L ......................................................... 396
8.3.3 OCT-L 8-Port Sampler ....................................... 397

8.3.4 TNM-L ....................................................... 397


8.3.5 POC Measurement Kit ...................................... 397
8.3.6 Carrier Gas Purifier Kit ...................................... 398

8.3.7 Manual Injection Kit (Gas Sample Injection Kit) ........... 398
8.3.8 B-Type Halogen Scrubber ................................... 399

xxii TOC-LCPH/CPN LabSolutions TOC Volume


Contents

8.3.9 External Sparge Kit .......................................... 399

8.3.10 High Suspension Kit for High Concentrations .............. 399

8.3.11 High Suspension Kit for Low Concentrations .............. 400


8.3.12 Recommended PC Specifications ............................ 400

8.4 Standard Accessories ........................................ 401


8.5 Special Accessories ........................................... 403
8.6 Consumable Parts List ...................................... 405
8.6.1 Consumable Parts List ....................................... 405

8.6.2 Recommended Consumable Part Replacement Period ...... 408

8.7 Maintenance Parts List ..................................... 409


8.8 Installation ...................................................... 411
8.8.1 Before Installation ........................................... 411
8.8.2 Installation Site .............................................. 411
8.8.3 Installation Procedure ........................................ 413

8.8.4 Installing the ASI-L .......................................... 419


8.8.5 OCT-L Installation ............................................ 425

8.8.6 Installing the TNM-L ......................................... 429

8.9 Safety Data Sheets (SDS) .................................. 433


8.9.1 Hydrochloric Acid (HCl) ..................................... 433
8.9.2 Phosphoric Acid ............................................. 440
8.9.3 IC Reagent .................................................. 447
8.9.4 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime ......... 457
8.9.5 Ceramic Fiber ................................................ 464

8.9.6 Halogen Scrubber ........................................... 469


8.9.7 High Sensitivity Catalyst ..................................... 471

8.9.8 Normal Sensitivity Catalyst .................................. 473


8.9.9 Catalyst Platinum Black ..................................... 476
8.9.10 NH3 Absorbent .............................................. 486

8.9.11 Silica Glass Wool ............................................ 492

Index ......................................................... 501

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This page is intentionally left blank.
1 Overview
This chapter provides an overview of the instrument and operational precautions for its
use. 1

1.1 Overview

The TOC-LCPH/TOC-LCPN (hereinafter referred to as TOC-L) instrument measures the amount


of total carbon (TC), inorganic carbon (IC) and total organic carbon (TOC) in water.
Purgeable organic carbon (POC) can also be measured when the POC accessory is installed.
"Oxidative combustion-infrared analysis" is a widely-used TOC measurement method that
has been adopted by the JIS*1 and other international standards. The TOC-L instrument can
also measure total water-borne nitrogen (TN) if the optional TNM-L is installed. TN is
measured using the principles of "oxidative combustion-chemiluminescence."

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

Safety may be compromised if the instrument is used in a fashion other than


that indicated in this USER'S MANUAL.
Pay particular attention to the CAUTION sections to ensure safety when using
the instrument.

TOC-LCPH/CPN LabSolutions TOC Volume 1


1 Overview

1.2 Operational Precautions


Take the following precautions when using this instrument.

• This instrument is used for measuring the amount of organic and


nitrogenous substances in water (additional options allow gaseous and solid
sample measurement). Do NOT measure liquids other than water samples.
<Part damage prevention>
• Do not touch the electric furnace while it is heating. The center of the
electric furnace (near the combustion tube insertion opening) reaches very
high temperatures, and burns may result. <Burn prevention>
• To prevent high sensitivity catalyst from being forced upward in the
combustion tube, verify that carrier gas is flowing when heating the electric
furnace. <Prevents the floating of high sensitivity catalyst>
• 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 or exchanging the combustion tube. Burns may
result if this procedure is attempted when the furnace is at a high
temperature. <Burn prevention>
• Do not heat the electric furnace without the combustion tube installed.
The parts of the TC injection port will be exposed to radiant heat from
the center of the electric furnace and may become deformed. If the furnace
must be heated without the combustion tube installed, either remove the
TC injection port parts from the instrument in advance to prevent
deformation or cover the furnace core opening with quartz wool or
another suitable insulator. <Part damage prevention>
• To reduce back pressure, verify that the external drain tubing connected
to the waste port on the right side of the instrument does not touch the
surface of the liquid in the waste container. The height of the external
tube must always be lower than the height of the drain port. Note that
excessive back pressure will prevent sufficient drainage and cause
overflowing from the drain pot.

Figure 1.1 External Drain Tubing

2 TOC-LCPH/CPN LabSolutions TOC Volume


1.2 Operational Precautions

• 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.

Carrier gas is Never turn the lever to


discharged to the front this position.
of the IC reaction
vessel. (Turn the lever
to this position only
when detaching an IC
reaction vessel that
contains liquid.)

Figure 1.2 Lever Position of 3-Way Valve on the IC Reaction Vessel

• 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>

TOC-LCPH/CPN LabSolutions TOC Volume 3


1 Overview

• The optional POC measurement circuit incorporates a carbon dioxide (CO2)


absorber packed with lithium hydroxide for removal of carbon dioxide gas.
Misuse of lithium hydroxide can cause bodily harm. During packing or
replacing the CO2 absorber container, exercise adequate precaution. After
use, treat the material as industrial waste. The properties and handling
guidelines for lithium hydroxide are described in the material safety data
sheets (MSDS) in "8.9 Safety Data Sheets (SDS)" P.433.
• To clean the instrument, wipe the surface with a soft cloth moistened with
water. Do not use chemicals.
• Repairs to the inside of the instrument can be dangerous. Contact your
Shimadzu representative to have a trained service engineer perform repairs.
• Keep samples and chemicals away from the PC and printer.
• Do not disassemble or modify the instrument beyond the scope of the
maintenance procedures described in this manual, as safety may be
compromised.
• Do not use the instrument in hazardous areas (where fire is prohibited)
because the construction of the instrument is not explosion-proof. Also, the
instrument cannot be used in cleanroom environments.
• Select an installation site with a stable ambient temperature and clean
surroundings free from corrosive gas, organic gas, and dust. Dirty
surroundings in particular can cause measurement errors when performing
high sensitivity measurements. Install the instrument on a sturdy, horizontal
bench free from vibrations and physical impacts.
• In order to obtain favorable measurement values, do not install the
instrument near windows subject to direct sunlight, other sources of heat, or
locations directly subject to cool air from air conditioning, or near equipment
that generates strong magnetic fields, electric fields, or high frequency waves.
• Use the instrument with a grounded power supply of AC 100 ± 10 V.
• Do not use the following characters when naming files or systems to be
saved:
/ , . \ (back slash) : ; (these are all normal-width characters), space (normal
width, em width)
• Turn OFF the Power Management function of the PC to prevent shutdown
of the PC power while it is controlling the TOC analyzer. A shutdown of this
nature would adversely affect performance.
• Hand-tighten the connectors to the 8-port valve of the OCT-L.
Over-tightening with a tool may exert excessive force to the internal valve
body, causing deformation and internal leakage. <Part damage prevention>
• Shut down the instrument before connecting or disconnecting tubing to the
8-port valve or performing maintenance to the drive parts. Liquid may be
discharged from tubes during operation. <Part corrosion prevention>)
• When utilizing the software's printing function, set the paper size to letter
or A4 and printer graphic resolution to 600 dpi.
• Analysis parameter files including calibration curves and methods, as well as
system configuration settings created in the previous version, in addition to
all measurement data can be loaded and edited. However, please be
informed that some of these data may not be able to be loaded and edited.

4 TOC-LCPH/CPN LabSolutions TOC Volume


1.2 Operational Precautions

• 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.

TOC-LCPH/CPN LabSolutions TOC Volume 5


2 System Description
This chapter describes the components of the TOC-LCPH/CPN, autosampler (ASI-L), 8-port
sampler (OCT-L), and the TN unit (TNM-L).

2.1 TOC-LCPH/CPN Construction


This section shows the construction of the TOC-L main unit using front, right, left, rear,
and internal front and top views depicted diagonally from the left of the instrument, as
well as flow diagrams.

2.1.1 Front View

Figure 2.1 Front View

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2.1 TOC-LCPH/CPN Construction

2.1.2 Right Side View

Figure 2.2 Right Side View

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2 System Description

2.1.3 Left Side View

Figure 2.3 Left Side View

2.1.4 Rear View

Figure 2.4 Rear View

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2.1 TOC-LCPH/CPN Construction

2.1.5 Front Internal View (Left Diagonal)

Figure 2.5 Front Internal View (Left Diagonal)

2.1.6 Top Internal View (Left Diagonal)

Figure 2.6 Top Internal View (Left Diagonal)

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2 System Description

2.1.7 Flow Diagram

Figure 2.7 Flow Diagram (TOC-LCPH)

Figure 2.8 Flow Diagram (TOC-LCPH + TNM-L + External Sparge Kit)

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2.1 TOC-LCPH/CPN Construction

Figure 2.9 Flow Diagram (TOC-LCPH + N2 Carrier Gas Kit)

Figure 2.10 Flow Diagram (TOC-LCPH + POC Kit)

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2 System Description

Figure 2.11 Flow Diagram (TOC-LCPH + Manual Injection Kit)

Figure 2.12 Flow Diagram (TOC-LCPN)

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2.1 TOC-LCPH/CPN Construction

Figure 2.13 Flow Diagram (TOC-LCPN + TNM-L + External Sparge Kit)

Figure 2.14 Flow Diagram (TOC-LCPN + POC Kit)

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2 System Description

Figure 2.15 Flow Diagram (TOC-LCPN + TNM-L + Carrier Gas Purification Kit)

14 TOC-LCPH/CPN LabSolutions TOC Volume


2.2 Autosampler ASI-L (Option)

2.2 Autosampler ASI-L (Option)


This section shows the construction of the ASI-L unit using front and rear views depicted
diagonally from the left.

2.2.1 Front View (Left Diagonal)

Figure 2.16 Front View (Left Diagonal)

2.2.2 Rear View (Left Diagonal)

Figure 2.17 Rear View (Left Diagonal)

TOC-LCPH/CPN LabSolutions TOC Volume 15


2 System Description

2.3 8-Port Sampler OCT-L (Option)


This section shows the construction of the OCT-L unit using front and rear views depicted
diagonally from the left and right.

2.3.1 Front View (Left Diagonal)

Figure 2.18 Front View (Left Diagonal)

2.3.2 Rear View (Right Diagonal)

Figure 2.19 Rear View (Right Diagonal)

16 TOC-LCPH/CPN LabSolutions TOC Volume


2.4 TN Unit TNM-L (Option)

2.4 TN Unit TNM-L (Option)


This section shows the construction of the TNM-L unit using a front view depicted
diagonally from the right, a right view showing inside the door, and a rear view.

2.4.1 Front View (Right Diagonal)

Figure 2.20 Front View (Right Diagonal)

2.4.2 View Inside the Door on the Right Side

Figure 2.21 View Inside the Door on the Right Side

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2 System Description

2.4.3 Rear View

Figure 2.22 Rear View

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3 Preparation for Measurement
This chapter describes the instrument preparations required prior to conducting analysis.

3.1 Instrument and Sample Preparation


This section describes the preparation of catalyst, connection of the combustion tube,
mounting of the syringe and other procedures that must be performed prior to
conducting actual analysis.

3.1.1 Catalyst Filling


3
Three types of catalyst are available: TOC standard catalyst, TOC high sensitivity catalyst
(H Type only), and TOC/TN catalyst (option). The procedures for filling the combustion
tube with catalyst are described in this section. For TOC standard and high sensitivity
catalyst filling, follow the procedure in "Catalyst for TOC Analysis" P.20. For TOC/TN
catalyst filling, follow the procedure in "TOC/TN Catalyst (Option)" P.23.

Exercise caution when handling the combustion tube to prevent breakage, as


it is made of quartz glass.

When filling the combustion tube, verify that the catalyst does not become
contaminated. Contamination will cause high blank values and abnormal analysis
values.

Using New Catalyst


Broad blank peaks are obtained when using new catalyst for the first time. The blank
peaks will become progressively smaller and more stable with repeated injections, and
their size will stabilize. If calibration or analysis is performed while the blank peaks are
large, the measurements are affected by the changing magnitude of the blank peaks,
resulting in errors in the analysis values. Such errors are especially significant for high
sensitivity TC analysis.

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3 Preparation for Measurement

TC Analysis Using New Catalyst


Catalyst regeneration should be conducted 1-2 times for TC analysis using new catalyst.
This reduces the size of the blank peaks. Use continuous injections of pure water until
the blank peak area becomes small and stable. The blank peak magnitude depends on
the quality of the water (TC impurity concentration) and the TC analysis range used for
analysis. For example, a blank peak of 1 mg/L has little influence on results greater than
100 mg/L but has a significant influence on results equal to or less than 10 mg/L. Analyses
for expected concentrations around 10 mg/L must have stable blank peaks of 0.5 mg/L
or less.
For TOC high sensitivity catalyst, conduct the TC blank check analysis described in "TC
Blank Check Analysis" P.71.

TN Analysis Using New Catalyst


Blank peak magnitude poses no practical problems for TN analysis using new catalyst.
The blank peaks are fairly small and stable. Perform analysis with distilled or deionized
water to confirm the size of the blank peaks.

n Catalyst for TOC Analysis

Either standard or high sensitivity catalyst can be used for TOC analysis. The furnace
temperature is set to 680 °C for TOC analysis.

TOC Standard Catalyst


The TOC standard catalyst is appropriate for both the TC-IC method and NPOC method
of analysis.

Analyze TOC high precision samples (with expected concentrations of about


1 mg/L) using the TOC high sensitivity catalyst because smaller blank peaks are
generated.

Filling Combustion Tube with TOC Standard Catalyst

1 Insert two sheets of platinum mesh into the combustion tube.

2 Layer about 5 mm of quartz wool onto the platinum mesh using the catalyst
filling rod.

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3.1 Instrument and Sample Preparation

3 Fill the TOC standard catalyst to a height of about 100 mm.

Figure 3.1 Combustion Tube with TOC Standard Catalyst

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.

TOC High Sensitivity Catalyst (H Type only)


Use the TOC high sensitivity catalyst for low level TC analysis. The blank values are
controlled to negligible levels, and analysis is performed primarily for trace TOC in pure
water (1 mg/L or less).

Samples containing IC in excess of 5mg/L


The detection rate for IC decreases with increasing concentration. As a result, use the
NPOC method instead of the TC-IC method when analyzing samples that contain IC
concentrations in excess of 5 mg/L.

Filling Combustion Tube with TOC High Sensitivity Catalyst


Two cylindrical containers of catalyst are required for a single load.

1 Place two sheets of platinum mesh in the combustion tube.

2 Fit together the combustion tube opening and the opened end of the cylindrical
catalyst container.

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3 Preparation for Measurement

3 Use the catalyst filling rod to push catalyst into the combustion tube from the
other opened end of the cylindrical catalyst container.

4 Transfer the contents of the two cylindrical catalyst containers to achieve a


catalyst layer height of 110 mm in the combustion tube.

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.

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3.1 Instrument and Sample Preparation

n TOC/TN Catalyst (Option)

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.

Filling Combustion Tube with Catalyst for TN Analysis

1 Insert two sheets of platinum mesh into the combustion tube.

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.

4 Introduce 0.2 (±0.1) g of ceramic fiber to cover the catalyst.

TOC-LCPH/CPN LabSolutions TOC Volume 23


3 Preparation for Measurement

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.

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3.1 Instrument and Sample Preparation

3.1.2 Installing the Cooling Tube Unit (H Type Only)

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.

Figure 3.4 Installing the Cooling Tube Unit

TOC-LCPH/CPN LabSolutions TOC Volume 25


3 Preparation for Measurement

3.1.3 Connecting the Combustion Tube

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.

Installation for the H Type

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.

26 TOC-LCPH/CPN LabSolutions TOC Volume


3.1 Instrument and Sample Preparation

3 Loosen the two knurled screws on the sample injector and remove the sample
injector in the upward direction.

Figure 3.5 Sample Injector

4 Securely insert the top end of the combustion tube filled with catalyst into the
hole on the bottom of the sample injector.

TOC-LCPH/CPN LabSolutions TOC Volume 27


3 Preparation for Measurement

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.

Figure 3.6 Installing the Combustion Tube

6 Secure the sample injector to the instrument body using the knurled screws.

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3.1 Instrument and Sample Preparation

7 Reattach the slider and carrier gas introduction tubing to their original positions.

Figure 3.7 Securing the Sample Injector to the Instrument Body

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.

TOC-LCPH/CPN LabSolutions TOC Volume 29


3 Preparation for 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 3.8 Connecting the Combustion Tube and Cooling Tubing

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.

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3.1 Instrument and Sample Preparation

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)

TOC-LCPH/CPN LabSolutions TOC Volume 31


3 Preparation for Measurement

Installation for the N Type

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.

Figure 3.12 Sample Injector

4 Securely insert the top end of the combustion tube filled with catalyst into the
hole on the bottom of the sample injector.

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3.1 Instrument and Sample Preparation

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.

Figure 3.13 Installing the Combustion Tube

6 Secure the sample injector to the instrument body using the knurled screws.

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3 Preparation for Measurement

7 Reattach the slider and carrier gas introduction tubing to their original positions.

Figure 3.14 Securing the Sample Injector to the Instrument Body

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.

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3.1 Instrument and Sample Preparation

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 3.15 Connecting the Combustion Tube and Cooling Tubing

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3 Preparation for Measurement

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)

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When installing or moving the instrument, insulation material powder may


drop under the electric furnace. Since insulation material contains ceramic
fibers, follow these precautions:
• When cleaning dust under the electric furnace, wipe with dampened cloths
to prevent dust or powder from being dispersed.
• Ceramic fibers are contained in the material used inside the electric furnace.
Never dismantle 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.

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3 Preparation for Measurement

3.1.4 Connecting the Halogen Scrubber

Connection Procedure

1 Remove the film at both ends of the new halogen scrubber and connect it to
the Viton connectors.

2 Secure the halogen scrubber with two white plastic clamps.

Figure 3.18 Halogen Scrubber

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.

Figure 3.19 Halogen Scrubber Connection

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3.1 Instrument and Sample Preparation

3.1.5 Installing the Syringe

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

The syringe is installed according to the following procedure.

A system configuration must be created before syringe installation. Refer to "5.


1.1 Creating a New System Configuration" P.124 to set up a new system
configuration.
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.

Installation Procedure

1 Open the Sample Table Editor.


The procedure for opening the Sample Table Editor is described in "5.2.1 Opening the
Sample Table Editor" P.139.

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3 Preparation for Measurement

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.

3 Right-click on the instrument icon, and select Maintenance – Change Syringe.

The Syringe Change window opens.

4 Click Preparation Start.

Syringe replacement preparation operation begins. The progress bar blinks while the
syringe moves into the replacement position.

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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.

Figure 3.20 Installing the Syringe

6 Click to move the syringe to its uppermost position.

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3 Preparation for Measurement

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 the plunger retaining screw, do not use any tools.


Over-tightening can deform the plastic components of the 8-port valve and
cause leaks.
• As a guide, tighten the screw until it stops snugly and make one quarter
turn further.
• The plunger is secured to the plunger holder with the plunger fixing screw
via a spring washer. Be careful not to lose the spring washer.

8 Click Finish Replacement. The syringe pump zero point detection operation is
executed automatically.

9 Click Close.

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3.1.6 Water Supply to the Cooler Drain Vessel

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.

Do not bend drain tubing, as this may prevent drain discharge.

Figure 3.21 Filling the Cooler Drain Vessel with Water

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3 Preparation for Measurement

3.1.7 Filling the Humidifier with Water

Water is supplied to the humidifier using the following procedure.

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.

Figure 3.22 Filling the Humidifier with Water

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3.1 Instrument and Sample Preparation

3.1.8 Preparation of Dilution Water

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.

5 Place the cap on the dilution water bottle.

Verify that the tip of the intake tubing nearly reaches the bottom of the
container.

Figure 3.23 Preparing Dilution Water

About pure water:


• Use the purest water that can be obtained.
• Refer to "Preparation of Standard Solutions" P.64 on page 64 for details on the degree
of purity of "pure water".

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3.1.9 Acid Preparation

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

1 Dilute commercially available special grade concentrated hydrochloric acid


(12 mol/L) with 12 parts pure water to prepare 1 mol/L hydrochloric acid. A
concentration accuracy of approximately ±2 % is acceptable.
The pure water used as the diluent must have a TOC concentration no greater
than 0.5 mg/L. Since the TOC value of the diluent pure water can have a large
effect on the analysis result with high sensitivity analysis (low TOC
concentrations), it is necessary to use pure water having a very low TOC
concentration.

Hydrochloric acid is a hazardous chemical. Use precautions to avoid contact


when handling this substance.
For details, refer to "8.9 Safety Data Sheets (SDS)" P.433.

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.

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5 Place the cap on the container.

Verify that the tip of the acid intake tubing nearly reaches the bottom of the
container.

Figure 3.24 Acid Preparation

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3 Preparation for Measurement

3.1.10 Installation of the CO2 Absorber

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.

The flexible tubing should not be bent.

3 Place the CO2 absorber in the holder on the upper rear of the instrument.

Figure 3.25 Installation of the CO2 Absorber

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3.1.11 Adjusting Sparge Gas Flow Rate

The gas flow rate must be adjusted before conducting sparging during measurement.

A system configuration must be created before syringe installation. Refer to "5.


1.1 Creating a New System Configuration" P.124 to set up a new system
configuration.

Adjustment Procedure

1 Open the Sample Table Editor.


The procedure for opening the Sample Table Editor is described in "5.2.1 Opening the
Sample Table Editor" P.139.
3
2 Right-click on the appropriate instrument icon in the Sample Table tab of the
file viewer, and click Connect.

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.

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3 Preparation for Measurement

4 Click Open for Ext. Sparge.

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.

Figure 3.26 Adjusting the Sparge Gas Flow Rate

6 Close the front door of the instrument.

7 Click Close for Ext. Sparge and then click OK to close the window.

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3.1 Instrument and Sample Preparation

3.1.12 Installing the Suspended Solids Kit

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.

Replacing the Flow Line Parts and Slider


This procedure is used for both kits.

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.

4 Reinstall the sliders on the sample injection blocks.

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.

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Replacing Sample Tubing

For TOC-L (TOC-L main unit only)

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.

For TOC-L + ASI-L (TOC-L and ASI-L)


Refer to "8.8.4 Installing the ASI-L" P.419 to remove the ASI-L sample needle and sample
tubing. Replace these with the sample needle and tubing provided in the Suspended
Solids Kit.

Precautions for Measuring Suspended Solids


When performing measurement of solid samples using the Suspended Solids Measurement
kit, follow the precautions below to ensure the best possible conditions for measurement.
Refer to "Analysis of Samples Containing Suspended Solids" P.76.

(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.

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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.

Replacing the Injection Tubing

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.

3 Reinstall the sliders onto the sample injection blocks.

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.

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3 Preparation for Measurement

Precautions when using the High Suspension Kit


When analyzing samples with suspended solids using the High Suspension Kit for High
Concentrations, observe the following precautions. These are general precautions to
ensure that analysis of samples with suspended solids is performed under the best
possible conditions.

(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.

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3.1 Instrument and Sample Preparation

3.1.14 IC Analysis Preparations

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.

Preparation and Placement of the IC Reagent 3


Procedure

1 Prepare the IC reagent by diluting 50 mL of commercially available 85 %


phosphoric acid (ACS Reagent grade) with pure water to a final volume of
250 mL.
Since the specific gravity of 85 % phosphoric acid is about 1.7, dilution results in a
concentration of phosphoric acid of about 25 % (weight%) in the prepared IC reagent.
A concentration accuracy of approximately ±2 % is acceptable.

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.

5 Replace the cap on the container.

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3 Preparation for Measurement

Replenishing IC Reaction Vessel with IC Reagent


Use the following procedure to replenish the IC reagent.

A system configuration must be created before syringe installation. Refer to "5.


1.1 Creating a New System Configuration" P.124 to set up a new system
configuration.

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".

Figure 3.27 Lever Position of IC Reaction Vessel 3-Way Valve

2 Open the Sample Table Editor.


The procedure for opening the Sample Table Editor is described in "5.2.1 Opening the
Sample Table Editor" P.139.

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.

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3.1 Instrument and Sample Preparation

4 Right-click on the instrument icon, and select Maintenance – Regeneration of the


IC Solution.

The Regeneration of IC Solution window opens.

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.

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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.

Installation of the CO2 Absorber for POC Analysis

1 Remove the CO2 absorber.

Figure 3.28 CO2 Absorber Container for POC Analysis

2 Insert about 5 mm of quartz wool into the bottom of the container.

3 Add commercially available anhydrous lithium hydroxide to the container on top


of the quartz wool until it reaches just below the screw threads of the container.

About 6 g of anhydrous lithium hydroxide is required for a single load.

4 Place about 5 mm of quartz wool on top of the lithium hydroxide.

5 Attach the O-ring and nipple to the top of the container, and firmly tighten the
cap.

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6 Install the CO2 absorber for POC analysis in the original position.

• Lithium hydroxide is available in anhydrous and hydrated forms. Since the


ability of the hydrated form to absorb carbon dioxide is slightly inferior to
that of the anhydrous form, use anhydrous lithium to fill the CO2 absorber
container.
• When introducing the quartz wool and lithium hydroxide into the container,
do not pack too tightly.
• The CO2 absorber container is constructed of glass. Handle it carefully to
prevent breakage.

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.

Figure 3.29 Preparing the CO2 Absorber for POC Analysis

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3 Preparation for Measurement

3.1.16 TN Analysis Preparation (When Using the Optional TNM-L TN Unit)

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.

n Installation of the NOx Absorber

Procedure

1 Cut the tips of the rigid tubes (2) in the lid of the CO2 absorber with a knife.

2 Connect the Viton tubing to the 2 rigid tubes as follows:


• Tubing labeled "L": Connect to tube labeled "L" on the CO2 absorber.

• 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.

Make sure there are no kinks in the flexible tubing.

Figure 3.30 Connecting the NOx Absorber

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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.

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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.

Figure 3.31 Removing the B-Type Halogen Scrubber

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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.

Figure 3.32 Preparing the B-Type Halogen Scrubber

4 Close the screw cap and return the B-type halogen scrubber to its original
position in the instrument.

Hydrochloric acid is a deleterious substance and must always be handled with


care to prevent spills and contact with the skin.
For details, refer to "8.9 Safety Data Sheets (SDS)" P.433.
The vessel of the B-type halogen scrubber is made of glass. Handle the vessel
with care to prevent breakage due to impact with other objects.

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3.1.18 Preparation and Storage of Standard Solutions

n Preparation of Standard Solutions

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.

Preparation of TC Standard Solutions

1 Accurately weigh 2.125 g of reagent grade potassium hydrogen phthalate.

2 Transfer the weighed amount into a 1 L volumetric flask.

3 Add zero water to the 1 L mark, and stir the solution.


The carbon concentration of the solution is 1000 mgC/L (1000 mgC/L = 1000 ppmC). This
solution is the standard stock solution.

• The standard stock solution may be prepared at other concentrations.


• Although this example describes the preparation of a 1000 mgC/L standard
stock solution, the standard stock solution may be prepared at other
concentrations within the range of solubility.

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4 Accurately dilute this standard stock solution with zero water to prepare
standard solutions at the required concentrations.

• The TC standard solution reagent need not be potassium hydrogen phthalate.


Other substances (such as sucrose) are also acceptable depending on the
application.
• Although this example describes the preparation of a 1000 mgC/L standard
stock solution, the standard stock solution may be prepared at other
concentrations within the range of solubility.
• A variety of official drying methods for standard substances are defined. Use
a suitable method for drying, if required.

Preparation of the IC Standard Solution


3
1 Accurately weigh 3.497 g of reagent grade sodium hydrogen carbonate and
4.412 g of sodium carbonate.

2 Transfer the weighed amount into a 1 L volumetric flask.

3 Add zero water up to the 1 L marker and mix well.


The carbon concentration of this liquid solution is equivalent to 1000 mgC/L (1000 mgC/L
= 1000 ppmC). Keep this solution as a standard stock solution.

The following procedure is the same as for preparing TC standard solution.

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Preparation of TN Standard Solution

1 Accurately weigh 7.219 g of reagent grade potassium nitrate.

2 Transfer the weighed material to a 1 L volumetric flask.

3 Add zero water up to the 1 L marker and mix well.


The nitrogen concentration of this liquid solution is equivalent to 1000 mgN/L
(1000 mgN/L = 1000 ppmN). Keep this solution as a standard stock solution.

The following procedure is the same as for preparing TC standard solution.

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.

TC/TN Mixed Standard Solution Preparation Procedure


When TC (or NPOC) and TN analyses are performed simultaneously, a mixed TC and TN
standard solution is prepared.
The mixed standard solution is prepared by mixing the TC standard solution and TN
standard solution. The mixed standard solution must contain 0.05 M hydrochloric acid.

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Preparation of 100 mgC/L TC - 100 mgN/L TN Mixed Standard Solution

1 Prepare 1 L of 1000 mgC/L TC standard solution using the preparation method


described above.

2 Prepare 1 L of 1000 mgN/L TN standard solution using the preparation method


described above.

3 Introduce 100 mL of each of the prepared standard solutions into a 1 L volumetric


flask.

4 Add 50 mL of 1 M hydrochloric acid to the flask.


3

5 Add zero water up to the 1 L marker and mix well.


The hydrochloric acid concentration will be about 0.05 M after dilution.

n Storage of Standard Solutions

The standard solutions undergo concentration changes, particularly when


low-concentration solutions are stored even for short periods. As a result,
high-concentration standard stock solutions (for example, 1000 mgC/L) should be stored
in airtight containers in a cool, dark place. Glass bottles are suitable storage containers.
Dilute the stock solution prior to each use.

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.

IC standard solution absorbs atmospheric carbon dioxide and undergoes


concentration changes. As a result, it is particularly important to store IC
standard solution in a sealed container.

Prepare fresh standard solutions:


• If reproducibility of analysis values is poor or concentration fluctuates.
• If contaminants, including even small amounts of dust, are present in the standard
solution.

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3.1.19 Sample Preparation

n High Sensitivity Analysis

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.

Precautions for High Sensitivity Analysis

Use TOC high sensitivity catalyst.


Carefully fill the combustion tube with high sensitivity catalyst to prevent contamination
of the combustion tube. Measuring high-concentration samples using TOC high sensitivity
catalyst that is intended for the analysis of ultra-pure water will influence the results of
subsequent analyses on ultra-pure water samples. This is primarily caused by remaining
sample residue. The residue may be removed by running repeated analyses of zero water.
Since removal is difficult with residual salt, alkali or highly acidic samples, a separate
combustion tube containing TOC high sensitivity catalyst should be prepared for use only
with ultra-pure water samples.
Verify that both ends of the combustion tube are sealed when storing catalyst that is to
be used only for ultra-pure water samples.

Measure samples immediately.


Samples containing trace carbon (such as ultra-pure water) should be measured
immediately after collection. If analysis cannot be performed immediately, store the
sample in a dark location at 0-10 °C (without freezing) and perform analysis as soon as
possible.
To collect the water, introduce water into a well-washed container, leaving no headspace,
and seal the container.

Use glass sample containers.


Glass containers are optimal for samples containing trace carbon. Commercially-available
500 mL to 1 L glass screw-lid jars with PTFE seals (generally referred to as heat-resistant
screw-top jars or hermetic jars) are appropriate for use as water collection and transport
containers.

Exercise caution with plastic containers, as elution of TOC-containing components


can occur.

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Use NPOC analysis for ultra-pure water samples.


Use the NPOC method for analysis of ultra-pure water samples. Measuring TOC in
ultra-pure water samples by using the difference between TC and IC is prone to large
analysis errors for the following reasons:
• The TOC value is significantly affected since a large portion of TC often comprises IC.
Errors in TC analysis and IC analysis are additive.
• Carbon dioxide is absorbed from the atmosphere during sample collection and analysis.
During the elapsed time between TC analysis and IC analysis, the sample absorbs more
carbon from the atmosphere, causing the IC result to be higher than the IC content in
the TC result. As a result, subtracting the elevated IC result from the TC result yields
a biased TOC value.
• Since a calibration curve must be generated for both TC and IC, TOC values are
significantly affected if the standard solutions for TC and IC are not prepared and
measured with a high degree of accuracy. 3
• In NPOC analysis, POC may be volatilized from the sample during sparging for IC
removal. This is not a problem since the ultra-pure water contains practically no POC.

Cautions in Calibration Curve Generation and Sample Measurement Using High


Sensitivity Analysis
The case below describes the generation of a 2-point calibration curve shifted through
the origin. The calibration standard concentrations are 0 µg/L and 400 µg/L.

Preparation of Standard Solutions


A 2-point calibration curve using 0 µg/L and 400 µg/L is generated. The calibration curve
is shifted through the origin to correct for the TC contained in purified water used for
preparation of the standard solutions.
The 0 µg/L and 400 µg/L TC standard solutions should be prepared at the same time
using the same purified water. Wash well, two 250 mL volumetric flasks with purified
water (preferably water containing low TC concentration). Carefully introduce 1 mL of
100 mg/L TC standard stock solution (for a 400 µg/L solution) into one of the volumetric
flasks. Distilled water is introduced up to the graduation line in both volumetric flasks.
Standard preparation procedures should be performed as quickly as possible, using
caution to avoid inclusion of external contaminants. If a water purification apparatus is
the source of purified water, allow the water to flow for a few minutes prior to use, as
the initial water will have a higher TC concentration. Alternate the flasks a number of
times while filling them with water to equalize, as much as possible, the TC concentration
of the purified water.
Use fresh purified water when filling the volumetric flask to the graduation line. Do not
use rinse bottle water that has been standing for a long period of time because the TC
concentration continually increases with time.

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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.

Calibration Curve Analyses


Calibration curves are generated using the following two methods.

(1) Using standard solution in a 250 mL volumetric flask


Insert the sample tubing directly into the volumetric flask until it reaches the bottom
of the flask. Perform analyses quickly. Four to five repeated analyses can be made with
almost no effects from the absorption of atmospheric carbon dioxide. Cover the
opening of the volumetric flask with sealing film or paraffin to prevent contamination.
Use this method when the IC value of the purified water used for standard solution
preparation (specifically, 0 µg/L standard solution) is about 50 µg/L or less.
(2) Sparging the standard solution
To sparge in the sample injection syringe, set the acid addition ratio to 0.5%, and the
sparge time to 1.5 minutes. To sparge using the optional external sparge kit, transfer
about 60 mL of the standard solution to a clean sample container, add 1-2 drops of
1 M hydrochloric acid, sparge for 10 minutes and analyze.
Cover the sample container with paraffin or sealing film to prevent contamination. A
glass container with an external diameter of 24-25 mm and a height of 200-250 mm
is appropriate. Test tubes, stopper-equipped test tubes and chromatography tubes of
suitable size are available commercially. If the outer diameter of the container is too
large, the air-to-water contact efficiency is decreased, requiring a longer sparge time.
Ensuring that the tip of the sparge tube is near the bottom of the container will
improve the sparging efficiency.

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.

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n TC Blank Check Analysis

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.

Practically no blank peaks are generated in the IC measurement. Also, because 3


the IC value will become zero for water that has been acidified and sparged,
this phenomenon can be easily verified by analyzing such water in the IC
measurement. However, normally, such a procedure is not necessary. For this
reason, a special program similar to the TC blank measurement is not provided
for IC measurement.

Blank Check Measurement Procedure

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.

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3 Select Instrument – Maintenance – Blank Check.

The Blank Check Parameters dialog box is displayed.

4 Enter the appropriate injection volume value.

5 Click Start.
The Measurement Start screen is displayed.
Refer to "Connection" P.253 for the procedure for connecting to the Instrument.

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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.

TC Blank Check Analysis Sequence

(1) Washing the inside of the trap


First, the blank check ultra-pure water trap is washed with water from the dilution
water bottle. A 6 mL aliquot of dilution water is drawn into and then expelled from
the ultra-pure water trap (twice), leaving the trap nearly empty. Then 2 mL of dilution
water is injected into the TC injector Finally, the remaining water in the trap is drawn
into the syringe and expelled (4 times).
(2) Preparation of ultra-pure water for blank check
Six separate 2 mL aliquots of dilution water bottle are injected into the TC injector.
Then, the water in the trap is injected into the TC injector five more times in 2 mL
aliquots.

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(3) Blank check analysis


The ultra-pure water collected in the trap for blank check analysis is used to conduct
5 repeat TC analyses at the set injection volume. Steps 2 and 3 are then repeated 9
times. The measurement result for each analysis is displayed, enabling assessment of
the magnitude and stability of the system blank value from the area values. If the
magnitude of the blank value must be read in terms of concentration, compare these
area values with those obtained through calibration curve measurement.

If the flow lines, syringe pump or catalyst is contaminated with foreign


substances, the blank values may not become small until the blank check
procedure is repeated multiple times.

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n Pretreatment for IC Removal (Sparging)

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.

(1) Sparging in the sample injector syringe


The sparge gas flow rate is variable on the H Type instrument and fixed to 80 mL/min
on the N Type instrument.
(2) Independent sparging of sample using the optional external sparge kit
A glass container with an external diameter of 24-25 mm and a height of 200-250 mm
is appropriate for use as the sample container. Test tubes, stopper-equipped test tubes
and chromatography tubes of suitable size are available commercially. If the outer
diameter of the container is too large, the air to water contact efficiency is decreased,
requiring a longer sparge time. As a guide, the sparge time should be about 5 to 10
minutes for a sample of 20 to 40 mL.

Sparge Procedure

1 Refer to "3.1.11 Adjusting Sparge Gas Flow Rate" P.49 for the sparge gas delivery
procedure.

2 Add 1 M hydrochloric acid to the sample to adjust the pH to 2-3.

3 Insert the sparge tubing into the sample.


To improve the sparging efficiency, the tip of the sparge tubing should be as close to
the bottom of the sample container as possible.

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.

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n Analysis of Samples Containing Suspended Solids

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.

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Countermeasures
The following types of processing operations are normally used for measuring samples
containing suspended solids.

(1) TOC Analysis of Supernatant


In situations when the suspended solids are of no great concern, sedimentation occurs
in the sample container, and the supernatant sample is used. Results depend on the
sedimentation and separation properties of the suspended solids, but usually the
dissolved TOC (DOC: dissolved organic carbon) is measured.
(2) TOC Analysis of Filtrate
The suspended solids are removed using glass fiber filter paper or a membrane filter,
and only the dissolved TOC is measured. Because the filter paper or filter itself is likely
to contain TOC, thorough washing with water or sample is performed prior to use
until no TOC is present in the eluate. Perform heat treatment on the filter for glass
fiber filter paper.
(3) TOC Analysis of Stirred Samples 3
To perform intentional analysis of suspended solids, the sample is stirred using a
magnetic stirrer or other instrument. Simple stirring can lead to extreme variability in
the results because the suspended solids contained in the sample may not be
distributed uniformly throughout the suspension.
(4) TOC Analysis after Homogenization of the Sample
If the application requires that the suspended solids be included in the analysis, it is
critical that the solids are as fine as possible and distributed uniformly throughout the
suspension. Accurate and reproducible TOC results can be obtained when the sample
is highly homogenized to form uniform micro-size particles.
Homogenizing systems may include a mixer to perform high-speed stirring or an
ultrasonic system. (These are homogenizers with outputs of 150-300 W. Typical washing
sonicators do not have sufficient output for this use.) Ultrasonic systems are generally
more powerful, though performance varies with the type of suspended solids.
Uniform suspension cannot always be achieved with all types of suspended solids.
Sludge-like materials are comparatively easy to process while fibrous materials are more
difficult.

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n Handling Samples Containing Acids, Bases or Salts

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.

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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.

Identifying Salt Accumulation


The following situations arise when salts accumulate and clog the catalyst:
• The sound of gas release is heard when the slider moves during analysis.
• A dramatic fluctuation in carrier gas flow is noticed after the sample is injected.

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3.1.20 Sample Preparation for Autosampler Measurement

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.

Table 3.1 Sample Volume for Each Vial Type

Sample Volume When Sparging ASI-L Vials


Vial Type Sample Volume
with the External Sparge Kit
9 mL 8.5 mL2 6.4 mL1
24 mL 22 mL4 20 mL3
40 mL 38 mL4 35 mL3

• Note1: Sample volume when sample is introduced up to about 17 mm from


the top of the vial.
• Note2: Sample volume when sample is introduced up to about 10 mm from
the top of the vial.
• Note3: Sample volume when sample is introduced to about 10 mm from the
bottom of vial cap.
• Note4: Sample volume when sample is introduced to about 5 mm from the
bottom of vial cap.

The following restrictions apply when using 9 mL vials.


• This vial size is not suited to high sensitivity analysis, such as pure water analysis,
because the maximum sensitivity range becomes 0 to 1 mg/L (analysis using a calibration
curve full scale of 1 mg/L).
• Commercially available aluminum foil should be used to seal the vial because dedicated
septums are not provided.
• The magnetic stirrer cannot be used.
• TC-IC analysis, NPOC-IC analysis, and NPOC+POC analysis cannot be performed.

Wash any new vials using laboratory glassware detergent and then rinse them
thoroughly with water before use.

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Maximum Number of Measurements by Vial Type


The tables below indicate the full scale values of the calibration curve and the maximum
number of measurements possible under those conditions for the 24 mL and 40 mL vials,
respectively, when they are filled with the specified volume of sample. This assumes use
of the software-recommended injection volume, and the default 2 washes. As for TC-IC
measurement, the calibration curve full scale is the same for both TC and IC. As for
NPOC-IC measurement, the calibration curve full scale for IC is about 1/10 of NPOC
(because the concentration of IC to measure is expected to be significantly less than
NPOC). The values in the table are the calibration full scale values for NPOC.
When TC measurement, TC-IC measurement and NPOC measurement are all performed
from a 40 mL vial, the maximum number of measurements is shortened by 1 – 3
measurements.

Table 3.2 24 mL Vials

Maximum Number of Measurements


Calibration 3
Full Scale NPOC-IC
NPOC Analysis TC Analysis TC-IC Analysis
Analysis
100 µg/L 2 3 1 1
500 µg/L 4 5 1 1
1 mg/L 5 6 2 1
5 mg/L 6 7 3 1
10 mg/L More than 6 More than 7 More than 3 2

Table 3.3 40 mL Vials

Maximum Number of Measurements


Calibration
Full Scale NPOC-IC
NPOC Analysis TC Analysis TC-IC Analysis
Analysis
100 µg/L 2 3 1 3
500 µg/L 4 5 1 3
1 mg/L 5 6 2 4
5 mg/L 6 7 3 4
10 mg/L More than 12 More than 17 More than 8 7

When using a TOC-LCPN, perform measurement using a calibration curve full scale
greater than 1 mg/L.

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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.

Table 3.4 Maximum Number of Measurements Using 9 mL Vials

Analyte Measurement Range Maximum Number of Measurements


When sparging with the sample injector
NPOC Range over 0 to 1 mg/L syringe: 3
When sparging with the ASI-L vials: 2
TC Range over 0 to 1 mg/L 3
IC Range over 0 to 2 mg/L 3
TN All ranges 3

n Filling Vials with Sample

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:

(1) sparging with the ASI-L for NPOC analysis


(2) measuring acidic samples
(3) IC analysis
(4) POC analysis
(5) low-concentration samples (as a guideline, less than 10 mg/L)
(6) alkaline samples (pH 7 or higher)
(7) samples that contain volatile organic hydrocarbon components
(8) a large number of samples to be measured
(9) standard solutions

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.

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Sealing Sample Vials


There are two acceptable methods for sealing vials: (1) using the caps provided with the
vials, or (2) using aluminum foil or commercially available sealing material.
However, because the airtightness of aluminum foil seals are poor, their use may cause
corrosion inside the ASI-L due to the vaporization of acid in NPOC analysis and acidic
sample measurement, which both use the ASI-L to perform sparging. For these types of
measurements, use seals that are airtight.
Note that Shimadzu does not recommend using Parafilm seals because pieces of this seal
can become attached to the needle and prevent normal sample extraction.

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.

1 Place a seal over the vial opening.

2 Cap the vial over the seal.

Because the seals are perforated during injection, discard the seals after use.

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n Placing Vials in the Vial Rack

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.

Installing the Vial Rack


Install the rack using the following procedure.

1 Insert the vials into the vial rack and place the rack on the ASI-L turntable.

2 Place the cover over the turntable.

During analysis, the turntable must be covered. The ASI-L will not operate if the
turntable cover is not detected.

n Rinse Water Preparation

Replenishing the Rinse Water


Replenish the rinse water in the rinse bottle. Ensure that the rinse water level reaches
above the 2 L indication on the rinse bottle.

Inserting the Rinse Tubing


Insert the rinse tubing as shown in "Figure 3.33 Rinse Tubing Placement". Place the
provided tubing ring-band over the end of the tubing, and slide the ring band up the
tubing until it reaches the bottle cap and about 200 mm of the tubing extends into the
rinse bottle. Verify that the end of the rinse tubing descends to a point just above the
bottom of the bottle.

Rinse water will not flow properly if the rinse tube is not inserted correctly, and
measurement values may be adversely affected.

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Figure 3.33 Rinse Tubing Placement

Rinse Water Usage


The required volume of rinse water will vary depending on the measurement parameters.
The information in Table 3.5 can serve as a guide, ensure that there is always a sufficient
volume of rinse water. If the capacity of the provided 2 L bottle is insufficient, use a
container with greater capacity.

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3 Preparation for Measurement

Table 3.5 Rinse Water Usage Examples

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.

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n High Sensitivity ASI-L Analysis

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.

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n Acid Addition in NPOC Analysis

Installation of the optional external sparge kit allows sample acidification/sparging to be


conducted in the ASI-L during NPOC measurement. In this case, acid addition for
acidification can be performed automatically in the ASI-L.
When analysis is started, acid is first drawn from the acid bottle into the syringe and
then the set amount of acid is added from the sampling needle into all vials that have
been designated for acid addition. Use 1 mol/L hydrochloric acid as the standard acid for
addition. While the acid addition ratio (ratio of acid with respect to the sample) should
normally be set to about 1 to 3 %, purified water analysis can use a setting as low as
about 0.5 %.
The hydrochloric acid concentration or amount added should be adjusted in accordance
with the sample pH or buffering strength to bring the sample pH to 2-3. Prior to analysis,
verify that the pH is 2-3 using pH paper. The pH need not be checked each time if the
same type of sample is routinely measured.

Hydrochloric acid is a hazardous chemical. Exercise caution when handling to


prevent contact and spills.
For details, refer to "8.9 Safety Data Sheets (SDS)" P.433.

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.

n Sparging in NPOC Analysis

Installation of the optional external sparge kit allows sparging to be performed on


samples in vials in the ASI-L. This allows sparging of the next sample while the sample
in the vial at the sampling position is being analyzed. The recommended sparging time
settings 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.
The standard sparge gas flow rate is 100 mL/min. If the sparge gas flow rate is set too
high, sample will be spattered onto the cap seal. Adjust the sparge gas flow rate to
avoid spattering.
To verify that enough IC is removed during sparging using the ASI-L to enable unhindered
NPOC analysis, perform IC analysis on the remaining sample following NPOC analysis.

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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.

2 Select the ASI tab.

3 Place a check mark next to Activate Stirrer to enable this option.

4 Click OK.

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Adjusting the Rotation Speed

1 Adjust the rotation speed by turning the stirrer rotation speed adjustment dial
at the bottom of the right side of the ASI-L.

Precautions for Using an ASI-L Equipped with a Magnetic Stirrer


Follow these precautions when using an ASI-L equipped with a magnetic stirrer.

(1) When conducting measurement of a sample containing suspended solids, perform


pretreatment homogenization of the sample to obtain a uniform distribution of the
smallest possible particles. Apply a powerful enough homogenization process such as,
ultrasonication, to crush the suspended particles as much as possible. The magnetic
stirrer is not designed to perform such homogenization.
Stirring a non-homogeneous sample will not provide a uniform suspension. This will
result in poor measurement reproducibility.
(2) Depending on the characteristics of the suspended particles such as, shape, specific
gravity, size, strength and degree of cohesion, the stirrer bar may not be able to
sufficiently agitate the sample. For example, solid particles with a high specific gravity
sink to the bottom and prevent formation of a good mixture.

Magnetic Stirrer Operation


• Two types of magnetic stirrers are available, one for the 24 mL and one for the 40 mL
size vials. 9 mL vials cannot be used.
• Only the outermost four rows of the vial tray are accessible to the magnetic stirrer.

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.

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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.

2 Select the ASI tab.

3 Remove the check mark from the Activate Stirrer item.

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.

7 After the motor speeds are appropriated reset, click OK.


If the speeds do not reset, repeat the procedure from step 3.

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3 Preparation for Measurement

3.1.21 OCT-L (8-Port Sampler) Measurement

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.

n Loading the Sample

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.

(1) when performing IC measurement


(2) when performing POC measurement
(3) when performing measurement of low concentration samples (e.g., 10 mg/L)
(4) when performing measurement of alkali samples of pH 7 or higher
(5) when performing measurement of samples containing volatile organic carbon
compounds
(6) when the number of samples is so great as to require a long measurement time
(7) when performing measurement of standard solutions

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.

Sealing the Sample Containers


Sample containers may be sealed using commercial sealing films such as Parafilm. It is
also possible to pierce the lid of the container and insert the sample tubing into the
container through this opening.

In either case, wash the container with a laboratory detergent, and rinse it
thoroughly with water before use.

Sealing the Container with Parafilm

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.

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3 Press the overlapping portions of the Parafilm around the neck of the opening.

Figure 3.34 Sealing the Container 3

n High Sensitivity Using the OCT-L

If samples such as purified water or ultra-pure water, having a TOC concentration of


100ppb or less, are to be measured using the OCT-L, it is necessary to consider the
following precautions associated with high sensitivity analysis. Refer to "High Sensitivity
Analysis" P.68 in the TOC-LCPH/CPN USER'S MANUAL for more information.

(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.

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3.1.22 Starting Up the Instrument

n Turning on the Power

Turn on power to the instrument to perform measurements.

Main power switch


I mark: ON
O mark: OFF

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.

Turning on Power to the Instrument

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.

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Table 3.6 Relationship Between Power Switch and Indicator Lit States and Instrument State

Indicator in the Middle of the


Instrument State Power switch
Front Door
Ready condition not
Lit orange Lit green
established
Ready condition established Lit green Lit green
Measurement in progress Lit blue Lit green
In editing mode Flashing orange Lit green
Sleep state Flashing blue Lit green
Firmware update in progress Flashing green Lit green
Error occurred Flashing red Lit green
Warning occurred Lit red Lit green
Shutting down Off Flashing orange 3
Shut down Off Lit orange
Main power switch OFF Off Off

n Carrier Gas Pressure and Flow Rate Settings

This section describes how to set the pressure and flow rate of carrier gas in the TOC-L.

Setting Procedure

1 Refer to "5.1.1 Creating a New System Configuration" P.124 to create a new


system configuration. In the system configuration, set the carrier gas flow rate
to 150 mL/min (default value), unless another value is required for a special
purpose.

2 Set the carrier gas supply pressure to 200±10 kPa.

• 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.

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4 Display the Background Monitor window.

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

1 Refer to "5.1.1 Creating a New System Configuration" P.124 to create a new


system configuration. In the system configuration, set the carrier gas flow rate
to 150 mL/min (default value), unless another value is required for a special
purpose.

2 Set the carrier gas supply pressure to 300±10 kPa.

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.

4 Display the Background Monitor window.

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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.

Figure 3.35 Carrier Gas Pressure Settings

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.

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n Electric Furnace Power

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.

Electric Furnace Power

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.

2 Select the TOC tab.

3 For TN measurement, set the furnace temperature to 720 °C, and for all other
measurements, set it to 680 °C.

4 Click OK.

Allow 30 minutes for the furnace to reach the set temperature.

n TNM-L Ozone Air Gas Pressure Settings (Option)

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.

3 Display the TN tab in the Background Monitor window.

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.

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4 Analysis Procedure
This chapter presents a general description of the overall analysis flow.

4.1 Analysis Flow


Describes the series of operations from the preliminary checks before analysis to shutting
down the instrument after analysis.
For more detailed descriptions, refer to the indicated reference destinations.

4.1.1 Checks Before Analysis

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.

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4.1.2 Turning on the Instrument

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.

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4.1.3 Opening the Sample Table Editor

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.

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Procedure

1 Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon) in the Instruments tab.

The Sample Table Editor application starts up.

The Sample Table Editor can also be started directly from the Windows Start menu and
from the shortcut icon created on the desktop.

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4.1.4 Creating a Sample Table

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

1 Click in the Sample Table tab of the file viewer, or click

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.

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3 Click OK.
A new Sample Table is created, and opened in the Sample Table Editor.

4.1.5 Creating an Analysis Parameters File

• 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.

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Calibration Curve File


The procedure for entering the main parameters of the calibration curve file is described
below.
Only the basic parameters are described here.
Refer to "5.3.2 Creating a Calibration Curve File" P.147 for more details.

Procedure

1 Click in the Calibration Curve tab of the file viewer.

The Calibration Curve Wizard (Page 1) System Information page is displayed.

4
2 Select the System and click Next.

The Calibration Curve Wizard (Page 2) Calibration Curve Type page is displayed.

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3 Select Normal and then click Next.

The Calibration Curve Wizard (Page 3) Analysis Information page is displayed.

4 Select the type of analysis and place a check mark next to Zero Shift according
to the method. Click Browse.

The Save As dialog box is displayed.

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5 Enter a file name and click Save.

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.

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8 Click Add.

The Edit Calibration Point Parameters window is displayed.

9 Enter the calibration point concentration in the Cal. Point Conc. field, and click
OK.

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10 Repeat steps 6 and 7 to set all of the calibration points, and click Next.

The Calibration Curve Wizard (Page 6) Additional Settings page is displayed. 4

11 Click Finish to complete the calibration curve setup.

A calibration curve file is created based on the calibration curve parameters.

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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

1 Click in the Method tab of the file viewer.

The Method Wizard (Page 1) System Information page is displayed.

2 Select the System and click Next.

The Method Wizard (Page 2) Analysis Information page is displayed.

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3 Select the type of analysis according to the method. Click (Browse).

The analysis type "TOC" indicates TOC measurement using TC-IC.

4
The Save As dialog box is displayed.

4 Enter a file name and click Save.

5 Click Next.
The Method Wizard (Page 3) Calibration Curves page is displayed.

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6 Select the calibration curve to use in measurement and then click Next.

The Method Wizard (Page 4) Injection Parameters page is displayed.

7 The default values entered for the settings on this page may be used for
conducting basic analysis. Verify the settings, and click Next.

The Method Wizard (Page 5) Peak Time Parameters page is displayed.

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8 Check the settings and then click Next.

The Method Wizard (Page 6) Pharmaceutical water testing window is displayed. 4

9 Click Finish to complete the settings.

A method file is created based on these parameters.

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4.1.6 Editing the Sample Table

Insert the sample measurement parameters into the Sample Table.


Refer to "5.4 Editing a Sample Table" P.194 for more details.

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.

2 Insert the unknown samples into the Sample Table.


Drag the method file from the Method 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.

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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.

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4.1.7 Entering the Vial Numbers

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.

If the ASI-L or OCT-L is not used, this step is omitted.

Procedure

1 Click in the Sample Table.

The Vial Settings window is displayed.

2 Enter the vial numbers.

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.

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4.1.8 Connecting to the Instrument

Communication is established between the Sample Table Editor and the instrument to
enable sample analysis.
Refer to "Connection" P.253 for more details.

Procedure

1 Open the Sample Table to be used, and click .

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.

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4.1.9 Conducting Analysis

The instrument performs analysis based on the information in the Sample Table. The
operation differs depending on whether an ASI-L is being used.

Analysis with an ASI-L or OCT-L


Refer to "5.7.3 Analysis with an ASI-L or OCT-L" P.261 for more details.

Procedure

1 Open the Sample Table to be used, and click .

The Measurement Start window is displayed.

2 Select the procedure to be performed when the analysis sequence is complete.


• Keep running: The instrument remains in the Ready state at the completion of the
analysis sequence even after analysis is completed.
• Shut down instrument: The instrument automatically turns off at the completion of the
analysis sequence (although the main power remains on).
• Sleep: The instrument enters the sleep state, and restarts at a specified date and time.

Selecting TOC-L Quit the application will shut down the Sample Table Editor
after a Keep running, Shut down instrument, or Sleep process.

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3 Click Start to begin the analysis sequence.

4 After a peak appears, click to open the Sample window.

Analysis without an ASI-L or OCT-L


Refer to "5.7.4 Analysis without an ASI-L or OCT-L" P.263 for more details.

Procedure

1 Open the Sample Table to be used, and click .

The Meas Mode window is displayed.

2 Select Single Measurement and then click OK.


For the differences between each measurement mode, see the following page.
Refer to "5.7.4 Analysis without an ASI-L or OCT-L" P.263 for more details.

The TOC Measurement window is displayed.

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3 Click Start to begin the analysis.

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.

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4.1 Analysis Flow

4.1.10 Viewing and Outputting Analysis Results

The sample analysis results can be reviewed in the Sample Window, and output to a
printer or file.

Displaying the Sample Window


Refer to "5.5.1 Sample Window" P.222 for more details.

Procedure

1 Click .

The Sample window is displayed. Each of the sample analyses can be reviewed.

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Output to a Printer or File


Refer to "5.6 Sample Table Data Output and Printing" P.234 for more details.

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

screen and print it out in the same format.

• 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.

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4.1 Analysis Flow

4.1.11 Ending Analysis

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 .

The Shutdown dialog box is displayed.


4

2 Select the appropriate shutdown process.


• Shut down instrument: The instrument power turns off after about 30 minutes
(although the main power remains on).
• Sleep: The instrument enters a sleep state, and restarts automatically at a specified date
and time.

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.

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5 Software Operation
This chapter describes the use of the LabSolutions TOC software to set analysis parameters
and conduct analysis operations.

5.1 System Configuration


Describes the procedures for creating system configurations necessary for performing
analysis.

5.1.1 Creating a New System Configuration

Before starting analysis, it is necessary to create the system configuration to enable


instrument control by the PC. System configuration is how the information about the
optional accessories connected to the instrument are registered with the PC.

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.

The Sample Table Editor application starts up.

2 In the menu bar, select Options and click H/W Setting List.

The H/W Setting List window is displayed.

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3 Click the Create a New Setting button.

The Instrument Setup Wizard - System Information window is displayed.

4 Enter the system information.

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.

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5 Click Next.
The Instrument Setup Wizard - Options window is displayed.

6 Set the TOC instrument type and any options.

Item Description
Model Select the type of TOC instrument you are using.

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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.

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8 Enter the settings related to TOC measurement.

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.

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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.

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10 Enter the ASI-L-related settings.

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.

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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.

12 Enter the SSM-5000A-related settings.

Refer to the "SSM-5000A USER'S MANUAL for details on the SSM-5000A".


If the SSM-5000A will not be used, click Next without making any selections on this page.

13 Click Next.
The Instrument Setup Wizard-Communication window is displayed.

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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.

15 Enter a system configuration file name.


The created system configuration file is saved in Data Manager.

It is displayed when creating a system configuration file.

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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.

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5.1.2 Reviewing and Editing a System Configuration

System configurations may be viewed and edited as necessary. Some items cannot be
edited after the system configuration is created.

Access from the H/W Setting List

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.

The Sample Table Editor application starts up.

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.

The Instrument Properties window is displayed.

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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.

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Access from File View

Procedure

1 Open the Sample Table Editor.


Refer to "5.2.1 Opening the Sample Table Editor" P.139 to display the Sample Table Editor.

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.

The Instrument Properties window is displayed.


The window content and operations are the same at those described in "Access from the
H/W Setting List" P.134.

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.

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5.1 System Configuration

5.1.3 Deleting a System Configuration

If an existing system configuration becomes unnecessary, it can be deleted.

A deleted system configuration cannot be restored.

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.

The Sample Table Editor application starts up.

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.

A delete confirmation window is displayed.

4 Click Yes.
The system configuration is deleted.

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5.1.4 Viewing the System Configuration File Log

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.

The Sample Table Editor application starts up.

2 In the menu bar, select Options and click H/W Setting List.
The H/W Setting List window is displayed.

3 Click History.

The system configuration file log appears.

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5.2 Sample Table Editor

5.2 Sample Table Editor


Describes the basic operations of the Sample Table Editor analysis application.
Measurement is performed according to the analysis-related information contained in the
Sample Table. The Sample Table is created using the Sample Table Editor application.
This section describes operations of the Sample Table Editor.

5.2.1 Opening the Sample Table Editor

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.

The Sample Table Editor application starts up.

5.2.2 Exiting the Sample Table Editor

Procedure
5
1 Select File – Exit.

The Sample Table Editor closes.

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5.2.3 Sample Table Editor Window Components

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.

Indicates the connection status with the instrument and the


operational status of the instrument.
: Connection is not established with the instrument.

: Connection is established and the instrument is in READY


state.
Ready Indicator
: Connection is established but, the instrument is not in
READY state.
: Analysis is in progress.

: Operation has shifted to Editing mode and the Sample


Table being used for analysis can be edited.

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.

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5.2 Sample Table Editor

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

operations described below.

• : Minimizes the window.

• : Maximizes the window.

• : Exits the Sample Table Editor.

5.2.4 Sample Table Columns

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.

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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.

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5.2 Sample Table Editor

5.2.5 Sample Window Columns

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.

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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.

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5.2 Sample Table Editor

5.2.6 File Types Used

The types of files created and used in the Sample Table Editor are described below.

Sample Table File (*.tlxl)


The measurement parameters and results for each sample are recorded in this file.
A template containing the measurement parameters is inserted into the sample table file,
and measurement is conducted.

Calibration Curve File (*.cals, *.cald)


The calibration curve file is a template file containing the calibration curve generation
parameters.
A file (Example: ABC.cals) is created consisting of the calibration curve generation
parameters set using the calibration curve wizard, and is inserted into the sample table.
When measurement is conducted, a separate date and time appended file having the
same name (Example: ABC.2020_06_19_11_46_37.cald), is created.
The file containing the calibration curve generation parameters, such as the
above-mentioned ABC.cals, is distinguished by the sample table editor as a calibration
curve parameter file.
Selecting the calibration curve parameters file as the calibration curve to be used to
calculate the concentration of unknown samples ensures that the most recently generated
calibration curve, identified by the file name and date, is used for calculation.

Method File (*.metl)


The method file is a template file that contains the measurement parameters for the
unknown sample. This file is inserted into the sample table, and unknown sample 5
measurement is conducted.

Control Sample File (*.tpll)


A control sample is a known sample used to verify the instrument operation. The control
sample file is a template file that contains the control sample measurement parameters,
and the regular measurement parameters such as, error limit values (upper, lower limits),
and actions to be taken (re-analysis, stop, etc.) when such limits are exceeded.
This file is inserted into the sample table, and measurement of the control sample is
conducted.

Schedule File (*.tscl)


The schedule file is template file that contains the measurement parameters for multiple
samples and their order of measurement.
The sample table format schedule file (*.tsc) can be edited in the same way as a sample
table file (*.tlx) using the sample table editor. The measurement parameters,
measurement sequence, vial to be used, etc. can all be edited. The created schedule file
can be imported to the sample table file. The schedule file can also be output from the
created sample table file.

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5.3 Creating and Editing Files


Describes the procedures used for creating and editing the various files necessary for
conducting analysis.

5.3.1 Creating a Sample Table

A Sample Table is a file in which analysis information is entered in sequential order and
is used to conduct analysis.

Procedure

1 Click in the Sample Table tab of the file viewer, or in the


tool bar.

The Select H/W Settings window is displayed.

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.

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5.3 Creating and Editing Files

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.

5.3.2 Creating a Calibration Curve File

A Calibration Curve File is used to generate a calibration curve. This file includes standard
solution concentrations and measurement parameters.

Procedure

1 Click in the Calibration Curve tab of the file viewer.

The Calibration Curve Wizard (Page 1) System Information page is displayed.


5
The Calibration Curve Wizard (Page 1) System Information page can also be displayed by
selecting File – New – Calibration Curve.

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2 Select the system configuration to be used.

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.

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4 Enter the type of calibration curve.

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.

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6 Enter the basic analysis parameters and click (Browse).

Some items may not be displayed depending on the Analysis settings.

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.

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.
File Name Enter the calibration curve file name.

The Save As dialog box is displayed.

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7 Enter a file name and click Save.

8 Click Next.
The Calibration Curve Wizard (Page 4) Calibration Measurement Parameters page is
displayed.

9 Enter the advanced parameters.


Depending on the Analysis type, some items may not be displayed.

Item Description
Units Select the concentration unit from ppm, ppb, mg/L, µg/L, no unit.

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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.

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11 Enter the advanced parameters for each calibration point.


Depending on the settings, some items may not be 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.

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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.

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• When 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.
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.

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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.

Analysis Type Maximum Concentration


Normally: 30,000 mg/L
TC, NPOC
If using Dilution from Standard Solution*1: 2,500 mg/L
Using TOC-LCPH: 35,000 mg/L
IC Using TOC-LCPN: 3,000 mg/L
If using Dilution from Standard Solution*1: 3,000 mg/L
Normally: 4,000 mg/L
TN
If using Dilution from Standard Solution*1: 200 mg/L
POC 500 mg/L
Manual injection
20,000 mg/L
TC
Manual injection
Using TOC-LCPH: 20,000 mg/L
IC

*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.

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15 Enter the remaining parameters.

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.

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5.3.3 Creating a Method

A Method is a file used to set the analysis parameters used for measuring unknown
samples.

Procedure

1 Click in the Method tab of the file viewer.

The Method Wizard (Page 1) System Information page is displayed.

The Method Wizard (Page 1) System Information page can also be displayed by selecting
File – New – Method.

2 Select the system to be used.

Item Description
System Select the system to be used for measurement.
The name of the User conducting the operation is automatically
User
entered.

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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.

4 Enter the basic method information and click (Browse).

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.

The Save As dialog box is displayed.

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5 Enter a file name and click Save.

6 Click Next.
The Method Wizard (Page 3) Calibration Curves page is displayed.

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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.

You cannot select multiple identical calibration curve files.

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.

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9 Set the advanced analysis parameters.


Depending on the Analysis type setting, some items may not be 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.

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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.

11 Enter the peak detection parameters. 5

Item Description
Displays the analysis type selected in the Method Wizard (Page 2)
Analysis Analysis Information page. "TOC" indicates TOC measurement using
TC-IC.

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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.

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14 Configure the settings related to the acceptance of measurement values when


using pharmaceutical water control. (Refer to "8.2.8 Pharmaceutical Water
Testing" P.394.)

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.

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5.3.4 Creating a Control Sample File

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

1 Click in the Control Sample tab of the file viewer.

The Control Sample Wizard (Page 1) System Information page is displayed.

The Control Sample Wizard (Page 1) System Information page can also be displayed by
selecting File – New – Control Sample.

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2 Select the system to be used.

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.

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4 Select the Control Sample type and click (Browse).

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

The Save As dialog box is displayed.

5 Enter a file name and click Save.

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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.

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8 Click Next.
The Control Sample Wizard (Page 4) Analysis Parameters page is displayed.

9 Enter the basic control sample information.

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.

Click to locate the calibration curve folder, and select the


Calibration Curve 1
appropriate file using the Open dialog box.

10 Click Next.
The Control Sample Wizard (Page 5) Injection Parameters page is displayed.

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11 Enter the advanced analysis parameters.

Depending on the Analysis settings, some items may not be 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.

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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.

13 Enter the peak detection parameters.

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.

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14 Click Next.
The Control Sample Wizard (Page 7) Control Checking page is displayed.

15 Enter the control sample evaluation parameters.

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

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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.

5.3.5 Creating a Schedule

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.

Analysis based on the information in a schedule is conducted by loading the


information into a sample table. Analysis cannot be conducted using the schedule
file alone.

Creating a Schedule File in Sample Table Format


Editing of a schedule file in the format of a sample table is conducted using the same
operations as in a sample table.

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Procedure

1 Click in the Schedule tab of the file viewer.

The Select H/W Settings window is displayed.

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.

5.3.6 Reviewing and Editing a Sample Table

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.

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5.3.7 Reviewing and Editing a Calibration Curve

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.

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2 Review and edit the items by clicking on the desired tabs.

Some items cannot be edited.

• The Common tab is described below.

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.

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• The Parameter tab is described below.

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.

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• The Analysis tab is described below.

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.

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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.

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5.3 Creating and Editing Files

• The Data tab is described below.

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.

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• The Graph tab is displayed below.

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).

• The History tab is displayed below.

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5.3 Creating and Editing Files

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.

5.3.8 Reviewing and Editing a Method

An existing method can be reviewed and edited by opening the Sample/Method


Properties window.
The parameters in the Sample/Method Properties window were entered when the method
was created. For details regarding these items, refer to "5.3.3 Creating a Method" P.158.

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.

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2 Review and edit the items by clicking on the desired tabs.

Some items cannot be edited.

• The Common tab is described below.

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.

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• The Parameters tab is described below.

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.

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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.

• The TC tab is described below.


Depending on the analysis type, five different tabs may be displayed.
• TC
• IC
• NPOC
• POC
• TN

Depending on the type of tab, some items may not be displayed.

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.

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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.

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• The History tab is described below.

Item Description
Displays the Print screen. You can edit the settings and print out
Print
the information on the History screen.

3 After viewing and editing the method properties, click OK.


The changes are saved, and the window closes.

5.3.9 Reviewing and Editing a Control Sample

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.

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2 Click on the Control Parameters tab view and edit the control sample parameters.

Some items cannot be edited.

• The Control Parameters tab is described below.

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

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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.

3 After checking and editing the Control Parameters, click OK.


The changes are saved, and the window closes.

5.3.10 Reviewing and Editing a Schedule

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.

5.3.11 Opening an Existing File

Files are opened in several different ways.


Sample table and schedule files are displayed in the Sample Table Editor. Calibration
curve, method and control sample files are displayed in their respective Properties
windows.
For details, refer to the following pages.
• Calibration Curve: "5.3.7 Reviewing and Editing a Calibration Curve" P.176
• Method: "5.3.8 Reviewing and Editing a Method" P.183
• Control Sample: "5.3.9 Reviewing and Editing a Control Sample" P.188

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5.3 Creating and Editing Files

n From the File Viewer

Procedure

1 Click the file view tabs to switch to the desired file category.

2 Double-click on the desired file.


The file opens.

n From the Tool Bar

Procedure

1 Click in the tool bar.

The Open dialog box is displayed.

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2 Select the type of file you wish to open.

3 Select the desired file, and click Open.


The file opens.

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5.3 Creating and Editing Files

n From the File Menu

Procedure

1 Click File – Open.

2 Select the type of file you wish to open.


• Sample Table
• Cal. Curve Setting (calibration curve file)
• Calibration curve data files (calibration curve file and calibration curve analysis results)
• Method
5
• Control Sample
• Schedule
The Open dialog box is displayed.

3 Select the desired file, and click Open.


The file opens.

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5.4 Editing a Sample Table


Describes the procedures for entering analysis information into the Sample Table.

5.4.1 Inserting a Standard Solution

From the File Viewer


The standard is inserted into the sample table by dragging the calibration curve file from
the file viewer.

Calibration curve files are displayed as Standard when they are inserted into the
sample table.

Procedure

1 Display the Calibration Curve tab in the file viewer.

2 Select the calibration curve file, and drag it into position in the sample table.

The file is inserted in the position to which it was dragged.

If the row above the insertion position is empty, the row is filled with the new
content.

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5.4 Editing a Sample Table

From the Right-Click Menu


The calibration curve is inserted into the sample table using the right-click menu.

Procedure

1 Right-click in the left cell of the row where the calibration curve is to be inserted.

2 Click Insert – Calibration Curve.

The Open dialog box is displayed. 5

The Open dialog box can also be displayed by selecting Insert – Calibration Curve from the
menu bar.

3 Select the calibration curve to be inserted, and click Open.


The selected calibration curve is inserted in the sample table.

5.4.2 Inserting a Sample

From the File Viewer


The sample is inserted into the sample table by dragging the method file from the file
viewer.

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.

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Procedure

1 Display the Method tab of the file viewer.

2 Select the file, and drag it into position in the sample table.

The file is inserted in the position to which it was dragged.

If the row above the insertion position is empty, it is filled with the new content.

From the Right-Click Menu


Sample analysis parameters can be inserted directly into the Sample Table.

Procedure

1 Right-click in the left cell of the row where the sample is to be inserted.

2 Click Insert – Sample.

The Sample Wizard (Page 1) Parameter Source page is displayed.

The Sample Wizard (Page 1) Parameter Source page can also be displayed by selecting Insert
– Sample from the menu bar.

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5.4 Editing a Sample Table

3 Select the sample parameter source file.

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.

Create the sample by • Calibration Curve


Analysis parameters are from an existing calibration curve file.
using parameters
from: Click to display the Open dialog box, and select the
calibration curve file to use.
• Edit parameters manually
Allows setting of the analysis parameters manually rather than
using those in an existing 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

4 Click Next.
The Sample Wizard (Page 2) Analysis Information page is displayed.

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5 Set the basic sample information.

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.

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7 Select the calibration curve files to be incorporated with the sample.

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.

Displays the calibration curves files incorporated with the sample,


Calibration Curve 1,
Calibration Curve 2, and their location. Click and select the calibration curve file
Calibration Curve 3
from the Open dialog box.

8 Click Next.
The Sample Wizard (Page 4) Injection Parameters page is displayed.

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9 Enter the advanced analysis conditions.


Depending on the Analysis type, some items may not be 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.

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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.

11 Enter the peak detection parameters.


5

Item Description
Displays the analysis type selected in Sample Wizard (Page 2)
Analysis
Analysis Information.

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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.

5.4.3 Inserting a Control Sample

From the File Viewer


Control samples are inserted into the sample table by dragging the control sample file
from the file viewer.

Procedure

1 Display the Control Sample tab in the file viewer.

2 Select the file, and drag it into position in the sample table.

The file is inserted in the position to which it was dragged.

If there is an empty row above the insertion position, it is filled with the new
content.

From the Right-Click Menu

Procedure

1 Right-click in the left cell of the row where the control sample will be inserted.

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2 Click Insert – Control Sample.

The Open dialog box is displayed.

The Open dialog box can also be displayed by selecting Insert – Control Sample from the
menu bar.

3 Select the control sample to be inserted, and click Open.


The selected control sample is inserted into the sample table.
5
5.4.4 Inserting Multiple Samples with the Same Analysis Parameters

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.

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2 Select Insert – Multiple Samples.

The Open dialog box can also be displayed by selecting Insert – Multiple Samples from the
menu bar.

The Sample Group Wizard (Page 1) Select Source page is displayed.

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5.4 Editing a Sample Table

3 Select the parameter source file.

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.

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5 Enter the necessary parameters.

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

6 Click Finish or Next.


Click Finish to insert the group of samples into the sample table.
If Insert Cal. Curve / Control Samples was selected, the Next button is displayed to enable
proceeding to the next step in the wizard.

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7 Select the control samples to be inserted.

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.

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5.4.5 Inserting a Schedule

From the File Viewer


The contents of a schedule can be inserted into the sample table by dragging the
schedule file from the file viewer.

Procedure

1 Display the Schedule tab of the file viewer.

2 Select the file, and drag it into position in the sample table.

The file is inserted in the position to which it was dragged.

If there is an empty row above the insertion position, it is filled with the new
content.

From the Menu

Procedure

1 Select the row of the sample table where the schedule content is to be added.

The schedule content will be inserted above the selected row.

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2 Select File – Import Schedule File in the menu bar.

The Open dialog box is displayed.

3 Select the schedule file, and click Open.


The schedule content is inserted into the sample table.

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5.4.6 Vial Numbers

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

1 Open a completed sample table and click .

The Vial Settings dialog box is displayed.

The Vial Settings dialog box can also be displayed by selecting View – Vial Settings from
the menu bar.

2 Enter the sample vial numbers.


This diagram represents using the ASI-L to analyze samples in 24 mL vials.

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.

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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.

3 After all of the parameters are entered, click OK.


The vial numbers are entered into the sample table and the window closes.

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Entering Vial Numbers


Vial numbers can be entered using one of the following procedures.
• Keyboard Entry
Select the relevant cell, and enter the number using the keyboard.
• Entry by Dragging
After entering a vial number directly into a cell, the cell itself can be dragged to enter
sequential numbers in the cells of the "dragged" range.

Procedure

1 Select the cell where a number was entered.


Position the cursor precisely over the lower right corner of the selected cell until "+" is
displayed.

2 Click and drag.


• Dragging down or to the right will enter a series of ascending numbers.
• Dragging up or to the left will enter a series of descending numbers.

Dragging while holding down the Ctrl key, will enter numbers identical to that in the
original cell.

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Entry by Double-Clicking the Vial Arrangement Drawing

Procedure

1 Select the cell where the number will be entered.

2 Double-click on the vial in the vial arrangement drawing.

The number is entered in the cell.

Vial Arrangement Drawing Types


The following types of vial arrangement drawings are displayed in the Vial Settings
window.

ASI-L
5
These images are dependant on the number of vials and vial type.

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Single OCT-L Unit

Dual OCT-L Units

5.4.7 Editing Sample Analysis Parameters

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.

Sample Name, Sample ID and Comment of Samples


Text can be entered directly into the cells of the Sample Name, Sample ID and Comment
columns in the sample table.

Entry using the Keyboard


Click in the relevant cell, and enter text from the keyboard.

Sample Name, Sample ID Entry by Dragging


After entering content in a Sample Name or Sample ID cell, the cell itself can be dragged
to enter the same text in cells. If the end of the initially entered text is a number,
dragging the cell will copy that text and affix sequentially-ordered numbers over the
range.

Dragging while holding down the Ctrl key, will enter numbers identical to that in the
original cell.

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5.4 Editing a Sample Table

1 Select a cell and enter the desired text.


Position the cursor over the lower right corner of the selected cell until "+" is displayed.

2 Click and drag.


• Dragging down or to the right will enter a series of ascending numbers.
• Dragging up or to the left will enter a series of descending numbers.

Dragging while holding down the Ctrl key, will enter numbers identical to that in the 5
original cell.

Editing the Sample Analysis Parameters


Open the sample properties window to edit the analysis parameters. The properties
window is the same window used to insert the sample into the sample table. The type
of properties window differs according the sample Type.
• Standard
Displays the Calibration Curve Properties window. Refer to "5.3.7 Reviewing and Editing
a Calibration Curve" P.176.
• Unknown
Displays the Sample / Method Properties window. Refer to "5.3.8 Reviewing and Editing
a Method" P.183.
• Control
Displays the Control Sample Properties window. Refer to "5.3.9 Reviewing and Editing
a Control Sample" P.188.

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Using Double-Click

Procedure

1 Double-click on the left cell of the sample row.


The Properties window of the sample is displayed.

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

1 Select the left cell of the sample row.

2 Click .

The sample properties window is displayed.

Using Right-Click Menu

Procedure

1 Right-click on the left cell of the sample row.

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5.4 Editing a Sample Table

2 Select Measurement Settings.

The sample properties window is displayed.

5.4.8 Copying, Cutting and Pasting Data

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.

Copying, Cutting and Pasting a Cell

Procedure

1 Select the cell to be cut or copied.

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2 Select Edit – Cut or Edit – Copy.

The data is saved to the clipboard.

3 Select the cell where you wish to paste the data.

Valid cells include cells in the Sample Name, Sample ID or Comment columns
(cells in which keyboard entry is possible).

4 Click Edit – Paste.

The data is pasted into the selected cell.

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5.4 Editing a Sample Table

Copying, Cutting and Pasting a Sample


The sample row can be copied, cut and pasted to another row in the sample table. The
pasted content consists of the original sample analysis parameters only. Analysis results
cannot be pasted.

When a measured sample is cut, the measured data is deleted. Be careful when
cutting data, because the deleted data cannot be restored.

Procedure

1 Select the row to be cut or copied.

2 Click Edit – Cut or Edit – Copy.

The data is saved to the clipboard.

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.

4 Click Edit – Paste.

The data is pasted into the selected row.

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5.4.9 Deleting a Sample

Rows in the sample table can be deleted.

Use caution when deleting data, once deleted sample data cannot be restored.

Procedure

1 Select the row to be deleted.

2 Click Edit – Delete Row.

A deletion confirmation box is displayed.

3 Click OK. The selected row is deleted.

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5.4 Editing a Sample Table

5.4.10 Adding a Comment to File Information

Comments can be added by displaying the File Information dialog box for the opened
sample table or schedule.

Procedure

1 Click View – File Information.

The File Information window is displayed.

2 Confirm the file information.

3 Enter a comment in the Comment box, and click OK.


The window closes.

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5.5 Reviewing and Editing Measurement Data


Describes the procedures for checking and conducting re-calculation of previously
acquired data.

5.5.1 Sample Window

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.

n Opening the Sample Window

Procedure

1 Click .

The Sample Window is displayed.

The Sample Window can also be displayed by selecting View – Sample Window.

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Item Description

Set the graph format to Current Peak, All Peaks, or Cal. Curve.

• : Displays the peak profile of the selected injection in the


table.
Graph Format
• : Displays all the injection peaks in the table.

• : Displays the calibration curve peak. This is not enabled


during analysis.

Select the sample (row) for display from the sample table.
• Sample number/Row number: Select a sample to display.

• : Display the first sample.

Sample Selection • : Display the sample above the current one.

• : Display the sample below the current one.

• : Display the last sample.

Graph Area Displays the peak profile.


Sample Information Displays the injection information. Click on a cell to display the peak
List profile for that sample in the graph area.
If the sample was analyzed by more than one analysis method, 5
several tabs are displayed at the bottom of the Injection Table
Injection Table window. Click a tab to display the respective injection data.
Example: For analysis type TOC, both the TC and IC tabs are
displayed at the bottom of the injection table.

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.

2 To close the Sample Window, click again.

The Sample Window closes.

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n Changing the Graph Display

The graph display can be manipulated using the following procedures.

Enlarging or Reducing the Graph Display


The size of the graph display can be enlarged or reduced.

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.

• Using the / buttons:

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.

Changing the magnification manually

1 Right-click on the graph.

2 Click Manual.
The Graph Limits window is displayed.

3 Set the display range and click OK.

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.

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Full Scale
Use the following procedure to adjust the graph scale to enlarge the largest peak to
full scale.

Procedure

1 Right-click on the graph.

2 Select Scale - Full Scale.

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

1 Right-click on the graph.

2 Select Auto Adjust.

3 Click X Axis, Y Axis or X,Y Axis, as appropriate. 5


The display range is adjusted automatically.

Default
If the graph display has been changed, it can be returned to the default range with
the following procedure.

Procedure

1 Right-click on the graph.

2 Select Scale - Default.


The display range returns to the default parameters.

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.

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Procedure

1 Right-click on the graph.

2 Select Copy to Clipboard.


The graph is copied to the clipboard.

5.5.2 Reviewing and Editing Sample Analysis Parameters

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

1 Double-click on the left cell of the sample row.

The properties window of the sample is displayed.

The properties window can also be displayed by clicking the left cell of the sample row,
and then selecting View – Measurement Settings.

Using the Icon

Procedure

1 Click on the left cell of the sample row.

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2 Click .

The properties window is displayed.

Using Right-Click Menu

Procedure

1 Right-click on the left cell of the sample row.

2 Select Measurement Settings.

The properties window is displayed.

5.5.3 Reviewing the Calibration Curve

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.

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2 Click View Cal. 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.

5.5.4 Editing the Calibration Curve

The calibration curve file associated with the unknown sample or control sample can be
edited.

Changing from the Menu Bar

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.

2 Click View – Select Cal. Curve to Use.

The Select Cal. Curve to Use dialog box is displayed.

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5.5 Reviewing and Editing Measurement Data

3 Confirm or change the calibration curve.

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.

Select this item to change the calibration curve. Click to


Cal. Curve for Conc.
Calculation display the Open dialog box, and select the new calibration curve
file.

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.

Changing from the Calibration Curve Properties Screen

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.

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2 Select Measurement Settings.

3 Click the carbon condition tab.


There are five types of carbon analysis condition tabs: TC, IC, NPOC, POC, and TN. The
tab displayed depends on the analysis type. The following uses the TC tab as an example.

4 Click (Browse) and change the calibration curve.

5 Click OK.
The settings are saved, and the concentration is automatically recalculated based on the
new calibration curve information.

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5.5 Reviewing and Editing Measurement Data

5.5.5 Excluding Injection Results

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.

2 Click Exclude to remove the result from the calculation.

An exclusion confirmation box is displayed.

3 Click Yes.
The selected injection result is excluded.
Remove the exclusion by performing the procedure again.

5.5.6 Recalculating Results

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.

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Recalculating All the Analysis Results

Procedure

1 Select Edit – Recalculate – All.

The recalculate confirmation box is displayed.

2 Click Yes.
All of the results in the sample table are recalculated.

Recalculating Selected Analysis Results

Procedure

1 Select the sample to be recalculated.

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.

2 Select Edit – Recalculate – Highlighted.

The recalculate confirmation box is displayed.

3 Click Yes.
The selected results are recalculated.

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5.5.7 Clearing Analysis Results

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.

Clearing All Results

1 Select Edit – Clear Measured Data – All.

The clear confirmation box is displayed.

2 Click Yes.
All of the results in the sample table are cleared.

Clearing Selected Results

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.

2 Select Edit – Clear Measured Data – Highlighted.

The clear confirmation box is displayed.

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3 Click Yes.
The selected analysis results are cleared.

5.6 Sample Table Data Output and Printing


Describes the procedures for printing analysis results and outputting data.

5.6.1 Selecting Content to Print

Items such as page margins can be specified when printing a sample report.

Procedure

1 Select File - Page Setup.

The Page Setup dialog box is displayed.

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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.

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• Calibrations tab

• Samples tab

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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.

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4 Select the Miscellaneous tab to review the remaining parameters.

Item Description
Margin parameters Enter the print margins in these boxes.

Select the items to be printed in the report header.


• Organization: Enter the name of the organization.

• Logo: Enables printing of a .bmp format image. Click to


Header parameters
display the Open dialog box, and select the appropriate image file.
• Date/Time, User, Document name: Select these options to print the
date and time, user name or document name at the top of the
sample report.

Select this item to print a page number at the bottom of each


Footer / Page No.
sample report page.
Page Break / After Select this item to print information for each sample on a separate
every sample page of the report.
• Set the font used for column headings in sample reports.
Report Font Settings
• Set the font used for the information contained in sample reports.
Click this button to display a preview of the sample report before
Preview
printing. Refer to "Sample Report Preview" P.241.

5 Click OK.
The changes are saved, and the dialog box closes.

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5.6 Sample Table Data Output and Printing

5.6.2 Print Setup

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

1 Click File – Print Setup.

The Print Setup dialog box is displayed.

2 Make the necessary changes, and click OK. 5

5.6.3 Print Preview

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.

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n Sample Table Preview

Procedure

1 Click .

2 Select Sample Table.

The print preview is displayed.

The preview can also be displayed by selecting File - Print Preview - Sample Table.

3 Examine the preview.

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.

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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.

n Sample Report Preview

All

Procedure

1 Click .

2 Select Sample Report – All.

The preview is displayed.

The preview can also be displayed by selecting File – Print Preview – Sample Report - All.

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3 Check the displayed Preview.

The operations available while displaying this are the same as those described in "Sample
Table Preview" P.240.

Highlighted

Procedure

1 Select the samples to be previewed from the sample table.

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 .

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3 Select Sample Report – Highlighted.

The print preview is displayed.

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 .

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2 Select Sample Table.

The Print dialog box is displayed.

3 Make any necessary changes and print the sample table.

The sample table can also be printed by selecting File - Print - Sample Table.

n Sample Report

All

1 Click .

2 Select Sample Report - All.

The Print dialog box is displayed.

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3 Make any necessary changes and print the sample report.

The entire sample report can also be printed by selecting File - Print - Sample Report - All.

Highlighted

Procedure

1 Select all of the samples to be included in the report.

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 .

3 Select Sample Report - Highlighted.

The Print dialog box is displayed.

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.

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5.6.5 Selecting Content for ASCII Export

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

1 Click File - Ascii Export Setting and then Normal or Detail.

The ASCII Export Options dialog box is displayed.

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5.6 Sample Table Data Output and Printing

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.

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• System tab

• Data tab

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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.

5.6.6 Exporting to ASCII Format

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.

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Procedure

1 Click File - Ascii Export.

2 Click Normal (Meas Data Only) or Detail (Include injection data).


The Save As dialog box is displayed.

3 Enter a file name and save destination, then click the Save button.
The text file is saved.

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5.6 Sample Table Data Output and Printing

5.6.7 Exporting a Schedule File

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

1 Click File - Export Schedule File.

The Save As dialog box is displayed.

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.

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5.6.8 Exporting a Runtime Report

Setting up a runtime report enables measurement reports to be export automatically.

Procedure

1 Click Runtime Report Settings on the Options menu.

The Runtime Report Settings window is displayed.

2 Set the export settings for the runtime report.

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.

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5.7 Operation and Analysis

5.7 Operation and Analysis


Describes the procedures for operating the instrument and conducting analysis.

5.7.1 Instrument Connection and Disconnection

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

1 Open the sample table to be used for analysis.

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5 Software Operation

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.

Connection is also possible by selecting Instrument - Connect.

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5.7 Operation and Analysis

To Perform Maintenance or Monitor Operation


Connection is made without opening the sample table. Use this convenient method to
perform instrument maintenance and monitor instrument operation.

Procedure

1 Open the Sample Table tab of the file viewer. Right-click the instrument
configuration and select Connect.

The instrument is connected, and the Ready indicator illuminates.

The icon of the connected instrument configuration also illuminates.

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n Disconnection

With an Open Sample Table

Procedure

1 While connected, click .

The Disconnect box is displayed.

The Disconnect box can also be displayed by clicking Instrument – Connect while the
instrument is connected.

2 Click OK.

The connection is broken, and the Ready indicator goes out.

Without an Open Sample Table

1 Open the Sample Table tab of the file viewer. Right-click on the instrument
configuration and select Connect.

The Disconnect box is displayed.

2 Click OK.

The connection is broken, and the Ready indicator goes out.


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5.7 Operation and Analysis

5.7.2 Background Monitor

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.

From an Open Sample Table

Procedure

1 Establish instrument connection.

2 Click .

Refer to "Connection" P.253 to connect the instrument.

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.

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• The following screenshot shows the TOC tab.

Item Description

Indicates the analysis status. indicates a Ready status and


NDIR indicates a Not Ready status for Baseline Pos., Baseline Fluc., and
Baseline Noise.

Displays the current temperature for the Furnace, Dehumidifier, and


Temp.
NDIR.
Supply Gas Pressure Displays the current supply pressure of the carrier gas.
Carrier Gas Flow Displays the current flow rate of the carrier gas.
Sparge Gas Flow Displays the current flow rate of the sparge gas.
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.

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• 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.

Indicates the analysis status. indicates a Ready status and


Chemiluminescence indicates a Not Ready status for Baseline Pos., Baseline Fluc., and
5
Baseline Noise.

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.

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• The following screenshot shows the ASI tab. This tab is displayed when configuring
settings to use the ASI-L.

Item Description

Indicates the analysis status. indicates a Ready status and


ASI Power/ASI Cover
indicates a Not Ready status for ASI Power and ASI Cover.

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.

3 To close the Background Monitor window, click the .


The window closes.

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Not from an Open Sample Table

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.

The Background Monitor window is displayed.

5.7.3 Analysis with an ASI-L or OCT-L 5


Procedure

1 Open the sample table to be used and place the samples in the ASI-L accordingly.

2 Establish instrument connection.


Refer to "Connection" P.253 to connect the instrument.

3 Click .

The Measurement Start window is displayed.

Analysis can also be started by selecting Instrument – Start Measurement after connection
is established.

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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.

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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.

5.7.4 Analysis without an ASI-L or OCT-L

n Single Sample Analysis

Procedure

1 Open the sample table to be used for analysis, and place the sample in the
instrument.

2 Establish instrument connection.


Refer to "Connection" P.253 to connect the instrument.

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3 Click .

The Meas Mode dialog box is displayed.

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.

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5 Select Normal or Non-stop Mode.

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.

The Analysis starts.

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.

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9 Examine the results, and select the type of processing to be conducted.

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.

2 Establish instrument connection.


Refer to "Connection" P.253 to connect the instrument.

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3 Click .

The Meas Mode dialog box is displayed.

Analysis can also be started by selecting Instrument – Start Measurement after connection
is established.

4 Click Batch Measurement.

5 Click OK.
The Measurement Start window is displayed.

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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.

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5.7.5 Stopping Analysis

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

1 Click while analysis is in progress, and then select Peak Stop.

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

n Stop (after current sample is completed)

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).

All analysis stops after the current sample analysis is complete.

This option can also be accessed by clicking Instrument - Stop - Stop (after current sample
is completed).

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n Stop (stop all processes immediately)

This option immediately interrupts the current analysis.

Procedure

1 Click while analysis is in progress, and then select Stop (stop all

processes immediately).

The analysis stops.

This option can also be accessed by clicking Instrument - Stop - Stop (stop all processes
immediately).

5.7.6 Editing the Sample Table during Analysis

The sample table can be edited during analysis by changing to the Edit Mode and
temporarily suspending analysis.

Procedure

1 During analysis, select Instrument - Edit Mode.

The sample table is placed in the Edit Mode.


In the Edit Mode, the indicator at the right end of the tool bar changes to read "Edit."
This mode allows the following operations to be conducted in the sample table in the
same way as when analysis is not being conducted.
• Adding and deleting samples
• Changing analysis parameters and vial numbers
• Printing reports for samples that are already analyzed

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2 Click to cancel the Edit Mode and restart analysis.

The restart analysis confirmation window is displayed.

3 Click OK.
The Edit Mode is cancelled, and analysis continues.

The Edit Mode can also be cancelled by selecting Instrument - Edit Mode.

5.7.7 Instrument Shutdown

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.

From an Open Sample Table

Procedure

1 Establish instrument connection.


5
Refer to "Connection" P.253 to connect the instrument.

2 Click .

The Shutdown dialog box is displayed.

The Shutdown dialog box can also be displayed by selecting Instrument – Shutdown.

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3 Select Shut down instrument.

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.

From the File Viewer

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.

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2 Right-click on the instrument icon in the Sample Table tab of the file viewer,
and select Shutdown.

The Shutdown dialog box is displayed.

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

1 Establish instrument connection.


Refer to "Connection" P.253 to connect the instrument.

2 Click .

The Shutdown dialog box is displayed.

The Shutdown dialog box can also be displayed by selecting Instrument – Shutdown.

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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.

5 Enter the restart time in the Auto Restart Time boxes.

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.

From the File Viewer

Procedure

1 Establish instrument connection.


Refer to "Connection" P.253 to connect the instrument.

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2 Right-click on the instrument icon in the Sample Table tab of the file viewer,
and select Shutdown.

The Shutdown dialog box is displayed.

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.

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5.7.8 Instrument Validation

The performance of an instrument, such as repeatability and linearity, can be verified by


measuring standard solution under preset conditions.

Procedure

1 Click New on the Sample Table tab in the file viewer or New on the tool bar.

The Select H/W Settings window is displayed.

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.

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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.

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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.

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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.

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Linearity and Repeatability


The instrument's linearity and repeatability can be verified from the results of measuring
three samples: blank water, span, and an intermediary. 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.
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.

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5.7 Operation and Analysis

Quantitative Lower Limit


The instrument's quantitative lower limit can be verified by measuring blank water, span,
and a sample designated as the target.
The settings related to this measurement can be changed by clicking the Settings button
to open the following window.

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.

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5.7.9 Maintenance Operations

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.

5.8 Display Options


Describes the procedure for changing the Sample Table display.

5.8.1 Sample Table

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

1 Click Options – Display Settings – Sample Table/Schedule File.

The Sample Table/Schedule File window is displayed.

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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.

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• Display Items 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.

3 After all necessary changes are complete, click OK.


The changes are saved, and the window closes.

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5.8.2 Sample Window Display Options

Display options for the Sample window, such as row height, can be changed using the
following procedure.

Procedure

1 Select Options – Display Settings – Sample Window.

The Sample Window dialog box is displayed.

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.

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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.

• Display Items tab

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• 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.

3 After all of the settings are complete, click OK.


The changes are saved, and the window is closed.

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5.8.3 File Viewer Display Options

Display options for the File Viewer, such as tab position, can be changed using the
following procedure.

Procedure

1 Click Options – Display Settings – File View.

The File View dialog box is displayed.

2 Select the tabs that will be displayed.

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.

3 Click OK after the settings are complete.


The changes are saved, and the window is closed.

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5.8.4 Setting the Display Font of the Output Window

The display font of the output window can be set as desired.

Procedure

1 Click Options – Display Settings – Output Window.

The Output Window dialog box is displayed.

2 Select the font to be used.

Item Description

The currently selected font is displayed in the dialog box. Click


Font
to display the Font dialog box and select the desired font.

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• 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.

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5.8.5 Display of Selected Windows

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.

2 Deselect any items that are to be hidden.

Remove the check mark to conceal the item(s). Click a hidden item to replace the check
mark, and display the item. 5

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5.8.6 Display Font

The font used in the Sample Table, Schedule and Sample Window can be set as desired.

Procedure

1 Click Options – Display Settings – Font.

The Font dialog box is displayed.

2 Select the display font.

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 After the font settings are complete, click OK.


The changes are saved, and the dialog box is closed.

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5.8.7 Decimal Point Display

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

1 Click Options – Display Settings – Floating Point Number Format.

The Floating Point Format dialog box is displayed.

2 Enter the number of decimal places to be displayed.

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.

3 After completing the settings, click OK.


The changes are saved, and the dialog box is closed.

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5.9 Security Functions


Describes the login procedures such as, using passwords, screen lock release and other
software administration functions.

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

1 Enter the User ID and Password provided by the system administrator.

2 Click OK.
If the User ID and Password are recognized, the user is logged in and gains access to
the software functions.

5.9.2 Locking the Sample Table Editor

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.

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Procedure

1 Click Tools – Screen Lock.

The Sample Table Editor is locked, and the Re-enter Password window is displayed.

2 Enter the User ID and Password to release the screen lock.

5
3 Click OK.
The window closes, and the lock is released.

5.9.3 Releasing Time Out Lock

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

1 Enter the User ID and Password.

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2 Click OK.
The lock is released, and the window closes.

5.9.4 Recording the Operation History

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

1 In the menu bar, select Tools and click Add log.

2 Enter your message in message or submessage as necessary.

3 Click OK.
The history item is added.

5.9.5 Other Security Functions

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]".

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5.10 Other Functions

5.10 Other Functions


Describes supplementary functions.

5.10.1 Default Analysis Parameters

The default measurement parameters can be changed. The default values can be edited
when the parameters are entered.

Procedure

1 Click Options – Default Measurement Parameters.

The Default Measurement Parameters window is displayed.

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.

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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.

3 When the changes are complete, click OK.


The changes are saved, and the dialog box closes.

5.10.2 Converting and Outputting Measurement Values

Conversion can be performed with respect to data from completed measurements using
a set mathematical formula.

Procedure

1 Click Measurement Result Conversion on the Options menu.

The Measurement Result Conversion window is displayed.

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5.10 Other Functions

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.

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5 Software Operation

5.10.3 Online Manual

This documentation can be displayed and viewed on the PC screen.

The online manual is in PDF format. The Adobe Reader is required to display
this manual.

n Selecting the Online 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

by selecting Help – Online Manual.

Procedure

1 Click Help – Select Online Manual.

The Select Online Manual dialog box is displayed.

2 Select TOC-L CPH/CPN.

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.

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5.10 Other Functions

n Displaying the Online Manual

The online manual is displayed using the following procedure.

Procedure

1 Click Help – Online Manual.

The online manual is displayed.

5.10.4 Version Information

The following procedure is used to verify the Sample Table Editor version information.

Procedure

1 Click Help – About TOC-Control L.

The About TOC-Control L window is displayed.

2 Verify the information and click OK.

The window closes.

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6 Analysis with Special Options
This chapter describes measurement using the optional manual measurement kit.

6.1 Manual Injection Measurement (H Type Only)


This section describes the measurement of water samples using the optional manual
injection kit.
The optional manual injection kit allows the sample to be injected manually using an
external syringe, instead of using the built in sample injector syringe.

6.1.1 Analysis Preparation

n Installation

Procedure

1 Remove the knurled thumbscrew that secures the slider then remove the TC/TN
injector slider.

Figure 6.1 Removing the Slider

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6.1 Manual Injection Measurement (H Type Only)

2 Install the TC/TN block provided in the kit.

Figure 6.2 Installing the TC/TN Block

3 Remove the slider of the IC injector in the same manner and install the IC block
provided with the manual injection kit.

Figure 6.3 Installing the IC Block

When installing the block, be sure that it is properly aligned with the injection
port.

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6 Analysis with Special Options

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

n Calibration Curve Measurement

Use the following procedure to perform calibration curve measurement.


• Refer to "5.3.2 Creating a Calibration Curve File" P.147 for details on generating a
calibration curve.

• Refer to "5.3.1 Creating a Sample Table" P.146 for information on creating a sample table.

Procedure

1 Use the following parameters to create the calibration curve.


• System
This item is found on the Calibration Curve Wizard (Page 1) System Setup page. Select
the system configuration created in "System Configuration" P.304.
• No. of Injections
This item is found on the Calibration Curve Wizard (Page 4) Plot Settings page. Enter
a 1 for this value.
• Enter the other parameters as appropriate.

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6.1 Manual Injection Measurement (H Type Only)

2 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 "System Configuration" P.304.

3 Drag the created calibration curve from the file viewer into the Sample Table.

4 Click to connect to the instrument.

5 Click to start the analysis.

The Manual Injection Parameter dialog box is displayed.

6 Draw an appropriate amount of sample into the syringe.

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.

8 Verify that the instrument status is READY, and click Set.


6
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.

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n Sample Measurement

Use the following procedure to perform sample measurement.


• Refer to "5.3.3 Creating a Method" P.158 for details on creating a method.

• Refer to "5.3.1 Creating a Sample Table" P.146 or information on creating a sample table.

Procedure

1 Use the following parameters to create the method.


• System Name
This item is found on the Method Wizard (Page 1) System Setup page. Select the system
configuration created in"System Configuration" P.304.
• Calibration Curve 1
This item is found on the Method Wizard (Page 3) Calibration Curve page. Select the
calibration curve file created in "Calibration Curve Measurement" P.304.
• No. of Injections
This item is found on the Method Wizard (Page 4) Analysis Parameters page. Enter a
1 for this value.
• The other parameters may be set as appropriate.

2 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 "System Configuration" P.304.

3 Drag the created method from the file viewer into the Sample Table.

4 Click to connect to the instrument.

5 Click to start the analysis.

The Manual Injection Parameter dialog box is displayed.

6 Draw an appropriate amount of sample into the syringe.

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.
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6.1 Manual Injection Measurement (H Type Only)

8 Verify that the instrument status is READY 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.

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6.1.3 Precautions for Low Concentration Samples

In manual injections of sample concentrations lower than 1 mg/L, it is necessary to take


the following precautions to prevent contamination of the sample and the measurement
process.
• Injecting Sample into the Injection Port
Use a separate micro syringe (500 µL) for high sensitivity measurement. Any
contamination on the sample injection port may affect the result for high sensitivity
measurement.The inside of the injection port can be contaminated by sample solution
that adheres to the tip of the micro syringe needle. When inserting the micro syringe
into the injection port, use extreme care to avoid touching the tapered portion of the
inside of the sample injection port. After filling the syringe, wipe the excess solution
from the needle surface with soft tissue paper. Prevent excess drops of solution from
forming on the tip of the needle by gently pulling back on the plunger.
• Cleaning the Sample Injection Port
Under normal operating conditions, fill a 500 µL micro syringe with pure water and
insert it into the injection port. Keep the bottom of the syringe barrel 8-10 mm above
the injection port. Under normal operation, the bottom of the syringe barrel is inserted
until it comes into contact with the injection port allowing the needle tip to protrude
from the needle guide pipe by about 5-6 mm. With the needle 8-10 mm higher than
normal operation, the tip of the needle inside the needle guide pipe. Slowly dispense
the pure water. The pure water does not flow into the combustion tube. It is driven
out of the injection port by the carrier gas flowing through the needle guide pipe.
Wipe off the water coming out of the injection tube with soft tissue paper. The internal
injection port and inside of the needle guide pipe are now clean.
• Measurement of service water or contamination free environmental water, such as river
water, often reveals that IC is the major part of TC when the TOC content is around
1 mg/L. For these types of samples it is preferable to remove the IC content before
measuring TOC through the TC channel.
Errors for TC and IC analyses are additive. For samples that have a comparatively high
IC content relative to the TOC content, the TOC analysis error will be large if it is
determined by the difference between TC and IC results.

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6.1 Manual Injection Measurement (H Type Only)

6.1.4 Manual Injection Kit Maintenance

n Replacing the IC Injection Port Septum (Cushion O-Ring)

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

1 Loosen and remove the injection port bushing.

2 Remove the old septum, and insert a new one.

3 Replace the bushing and tighten it.

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)

Part Name P/N Capacity


Gas-tight syringe set 25 uL S638-60733-02 25 µL *1

Gas-tight syringe set 50 µL S638-60733-03 50 µL *1

Gas-tight syringe set 100 µL S638-60733-04 100 µL *1

Gas-tight syringe set 250 µL S638-60733-05 250 µL *1

Gas-tight syringe set 500 µL S638-60733-06 500 µL *1

Gas-tight syringe 1 mL S046-00026-02 1 mL


Gas-tight syringe set 5 mL S638-60733-03 5 mL
Gas-tight syringe set 10 mL S638-60733-04 10 mL

*1 Set comprises one replacement gas-tight syringe needle and one plunger.

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6 Analysis with Special Options

6.2 Gas Sample Analysis


This section describes the measurement of gas samples using the optional manual
injection kit.
If the optional manual injection kit is installed, analysis of TC and IC in gaseous samples
can be performed by using gas-tight syringes or other applicable injectors to inject the
gaseous samples.

6.2.1 Precautions for Gas Sample Analysis

• Do not inject a large quantity of sample at one time when measuring


combustible or explosive gases. The combustion tube could break. The
injection volume should not exceed 10 mL.
• Use caution when measuring combustible or explosive gases.
• Do not analyze samples that can release toxic substances during combustion.
The exhaust gas released during analysis passes through the CO2 detector to
the CO2 absorber, after which it is used as NDIR purge gas, and then is
vented inside the instrument. Take appropriate countermeasures if there is a
possibility that toxic substances could be included in the exhaust gas. If
appropriate countermeasures cannot be taken, do not perform such analyses.

• 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.

6.2.2 Analysis Preparation

n Installation of the Manual Injection Kit

Install the manual injection kit by referring to "6.1 Manual Injection Measurement (H
Type Only)" P.302 and then create a system configuration.

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6.2 Gas Sample Analysis

6.2.3 Measurement

n Calibration Curve

Use the following procedure to perform calibration curve measurement.

Procedure

1 Prepare a standard gas sample with a known carbon concentration.

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.

2 Create the calibration curve using the following parameters.


• 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.
• No. of Injections
This item is found on the Calibration Curve Wizard (Page 4) Plot Settings page. Enter
a 1 for this value.
• Enter the other parameters as appropriate.
• Refer to "5.3.2 Creating a Calibration Curve File" P.147 for details on generating a
calibration curve.

• 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.

5 Click to connect to the instrument.

6 Click to start the analysis.

The Manual Injection Parameter dialog box is displayed.

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6 Analysis with Special Options

7 Draw an appropriate amount of sample into the gas-tight syringe.

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.

9 Verify that the instrument status is READY, 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

Use the following procedure to perform sample measurement.


• Refer to "5.3.3 Creating a Method" P.158 for details on creating a method.

• Refer to "5.3.1 Creating a Sample Table" P.146 for information on creating a sample table.

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6.2 Gas Sample Analysis

Procedure

1 Use the following parameters to create the method.


• System Name
This item is found on the Method Wizard (Page 1) System Setup page. Select the system
configuration created in "5.1.1 Creating a New System Configuration" P.124.
• Calibration Curve 1
This item is found on the Method Wizard (Page 3) Calibration Curve page. Select the
calibration curve file created in "Calibration Curve" P.311.
• No. of Injections
This item is found on the Method Wizard (Page 4) Analysis Parameters page. Enter a
1 for this value.
• The other parameters may be set as appropriate.

2 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.

3 Drag the created method from the file viewer into the Sample Table.

4 Click to connect to the instrument.

6
5 Click to start the analysis.

The Manual Injection Parameter dialog box is displayed.

6 Draw an appropriate amount of sample into the gas-tight syringe.

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.

8 Verify that the instrument status is READY, and click Set.

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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.

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6.2 Gas Sample Analysis

6.2.4 Manual Injection Kit Maintenance

n Replacing the IC Injection Port Septum (Cushion O-Ring)

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

1 Loosen and remove the injection port bushing.

2 Remove the old septum, and insert a new one.

3 Replace the bushing and tighten it.

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)

Part Name P/N Capacity


Gas-tight syringe set 25 µL S638-60733-02 25 µL *1

Gas-tight syringe set 50 µL S638-60733-03 50 µL *1

Gas-tight syringe set 100 µL S638-60733-04 100 µL *1

Gas-tight syringe set 250 µL S638-60733-05 250 µL *1

Gas-tight syringe set 500 µL S638-60733-06 500 µL *1

Gas-tight syringe 1 mL S046-00026-02 1 mL


Gas-tight syringe set 5 mL S638-60733-03 5 mL
Gas-tight syringe set 10 mL S638-60733-04 10 mL

*1 Set comprises one replacement gas-tight syringe needle and one plunger.

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6 Analysis with Special Options

Table 6.3 Relationship Between Appropriate Peak Height and (CO2) Gas
Concentration / Injection Volume *1

Gas Concentration (CO2) Gas Injection Volume


TC 100 ppm 10 mL
1000 ppm 1 mL
1 % 500 µL
10 % 300 µL
100 % 30 µL
IC 100 ppm 6 uL
1000 ppm 600 µL
1 % 300 µL
10 % 200 µL
100 % 20 µL
*1 The values listed in this table should be regarded as reference values only as slight differences in
data may occur between individual instruments.

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7 Maintenance
Inspection and maintenance of the TOC-L instrument are required to ensure normal
operation and reliable and accurate data acquisition.

7.1 Daily Inspection


Describes the daily inspection procedures that should be performed before instrument
startup.
Check the levels of dilution water, acid, drain vessel water, and humidifier water each
day before starting the instrument.

7.1.1 Checking Dilution Water

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.

7.1.2 Checking Acid

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.

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7 Maintenance

7.1.3 Checking Drain Vessel Water Level

Figure 7.1 Drain Vessel Water Level

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.

7.1.4 Checking Humidifier Water Level

Figure 7.2 Humidifier Water Level

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.

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7.1 Daily Inspection

7.1.5 Inspecting the Liquid in the B-Type Halogen Scrubber (Option)

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.

Hydrochloric acid is a deleterious substance and must always be handled with


care to prevent spills and contact with the skin. For details, refer to "8.9 Safety
Data Sheets (SDS)" P.433.
The vessel of the B-type halogen scrubber is made of glass. Handle the vessel
with care to prevent breakage due to impact with other objects.
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.

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7 Maintenance

7.2 Periodic Inspections


Describes periodic inspection procedures for the TOC-L.
Periodically inspect the items listed in this section to maintain instrument performance
quality.

7.2.1 Catalyst Regeneration

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.

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7.2 Periodic Inspections

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.

The Regeneration of TC-Catalyst window is displayed.

The Regeneration of TC-Catalyst window can also be displayed by selecting Instrument –


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.

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7 Maintenance

7.2.2 Washing or Replacing Catalyst

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.

Removing the Combustion Tube


Remove the combustion tube according to the following procedure.
For details on installing the combustion tube, refer to "3.1.3 Connecting the Combustion
Tube" P.26.

• 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.

Figure 7.3 Sample Injector

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7.2 Periodic Inspections

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.

Figure 7.4 Removing the Combustion Tube


7

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7 Maintenance

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.

2 Neutralize the alkalis with dilute hydrochloric acid (5:1).

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).

2 Rinse with water.

3 Dry, and reuse these items.

4 Fill the combustion tube as described in "3.1.1 Catalyst Filling" P.19.

TOC High Sensitivity Catalyst


TOC high sensitivity catalyst cannot be washed and reused like standard catalyst. If
analysis sensitivity and reproducibility are not restored after catalyst regeneration, replace
the deteriorated high sensitivity catalyst with new high sensitivity catalyst. The platinum
mesh and combustion tube can be washed with hydrochloric acid and reused.

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7.2 Periodic Inspections

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.

7.2.3 Replacing the Carrier Gas Purification Tube and Catalyst

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.

Removing the Carrier Gas Purification Tube (Option)

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.

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7 Maintenance

Procedure

1 Remove the catalyst from the carrier gas purification tube through the opening
at the top.

2 Remove the quartz wool using a thin tube or other instrument.

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.

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7.2 Periodic Inspections

7.2.5 Replacing the High Purity Air (Filling the Cylinder)

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.

7.2.6 Replacing the CO2 Absorber

Replace the entire CO2 absorber located in the holder on top of the instrument once a
year.

CO2 Absorber Disposal Procedure


Used CO2 absorbers should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the used
CO2 absorber contains soda lime.
For details on replacing the CO2 absorbers, refer to "3.1.10 Installation of the CO2 Absorber"
P.48.

7.2.7 Replacing the Halogen Scrubber

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.

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7 Maintenance

4 Secure the halogen scrubber with the two clips in its original position.

Figure 7.5 Halogen Scrubber

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.

Figure 7.6 Halogen Scrubber Replacement

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7.2 Periodic Inspections

7.2.8 Syringe Replacement

Use the procedure below to replace the syringe.

• 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

1 Connect the Sample Table Editor to the instrument.


Refer to "Connection" P.253 for the connection procedure.

2 Open the Sample Table tab of the file viewer. Right-click on the connected
system configuration icon, and click Maintenance – Change Syringe.

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7 Maintenance

The Syringe Change window is displayed.

The Syringe Change window can also be displayed by selecting Instrument – Maintenance
– Change Syringe.

3 Click Preparation Start.


The syringe replacement preparation process begins. The progress bar blinks while the
operation is in progress.

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.

Figure 7.7 Plunger Retaining Screw

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.

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7.2 Periodic Inspections

6 Click to move the syringe to its uppermost position.

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

7.2.9 Syringe Plunger Tip Replacement

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

1 Remove the syringe referring to "7.2.8 Syringe Replacement" P.329.

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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.

Figure 7.8 Removing the Old Plunger Tip

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.

Figure 7.9 Installing the New Plunger Tip (cross-section)

• 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.

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7.2 Periodic Inspections

7.2.10 Replacing the Sliding Sample Injector O-rings

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)

Figure 7.10 Replacing the Sliding Sample Injector O-rings

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.

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7.2.11 Replacing the Syringe Pump 8-port Valve Rotor

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.

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7.2 Periodic Inspections

2 Remove the nut using the provided wrench.

Figure 7.11 Removing the Nut

3 Pull up to remove the rotor drive component. Hang it on the screw on the right
side of the plunger.

4 Loosen the retaining nut using the provided wrench.

Figure 7.12 Removing the Retaining Nut

5 Remove the spring-equipped rod.

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6 Grasp the rotor with pliers and pull it out.

Figure 7.13 Removing the Rotor

7 Insert a new rotor, taking care that the rotor hole matches original orientation.

8 Reinsert the spring-equipped rod and tighten the retaining nut.

9 Replace the rotor drive component, and tighten the nut.

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.

Soda Lime Replacement Procedure

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.

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7.2 Periodic Inspections

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.

2 Invert the CO2 absorber and remove the screw cap.

3 Remove the used soda lime.

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.

To maintain an airtight seal, a rubber o-ring is placed between the container


and the screw cap. Inspect the o-ring to verify that it is not scratched or
twisted, then attach the cap.

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"

• Tubing labeled "S"


Affixed to the connection port of the CO2 absorber container labeled "S"

Only tighten the nuts on the elbow joints by hand. Do not use tools.

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7 Maintenance

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.

Soda lime is a corrosive chemical substance. Be careful not to touch it with


bare hands. For details, refer to "8.9 Safety Data Sheets (SDS)" P.433.

7.2.13 Replenishing IC Reaction Solution

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.

7.2.14 Replacing the Pump Head of the IC Reaction Solution Pump

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.

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7.2 Periodic Inspections

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.

4 Attach the pump head by following the above procedure in reverse.

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.

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• Wear protective glasses and gloves when handling quartz wool.


Inhaling it may cause health impairment.
• Lithium hydroxide is a corrosive (strongly alkali) powder. Be carefully not to
spill or touch it during handling.
• Used lithium hydroxide should be disposed of by a certified industrial waste
handler according to local industrial waste disposal regulations. It must be
clearly disclosed using an industrial waste manifest that the waste is lithium
hydroxide.
• Lithium hydroxide crystal is found in both anhydrous and hydrated forms.
Because the carbon dioxide gas absorbance properties of the hydrated form
are slightly inferior to those of the anhydrous form, use anhydrous lithium
hydroxide to fill the CO2 absorber.

• The life of the CO2 absorber will be shortened by performing POC analysis
on samples with high concentrations of IC.

7.2.16 Replacing the Liquid in the B-Type Halogen Scrubber (Option)

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.

Hydrochloric acid is a deleterious substance and must always be handled with


care to prevent spills and contact with the skin. For details, refer to "8.9 Safety
Data Sheets (SDS)" P.433.
The vessel of the B-type halogen scrubber is made of glass. Handle the vessel
with care to prevent breakage due to impact with other objects.
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.

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7.3 Autosampler (ASI-L) Maintenance

7.3 Autosampler (ASI-L) Maintenance


Describes periodic inspection procedures for the ASI-L.
Maintenance of the ASI-L includes periodic inspection of the rinse bottle, sample catcher
and rinse pump.

7.3.1 Rinse Bottle Inspection

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.

Figure 7.15 Rinse Bottle Inspection

7.3.2 Sample Catcher Inspection


7
Examine the turntable (black plate) and the sample catcher tray below the turntable
when installing or removing the ASI-L vial rack. If they are wet or dirty, wipe them clean.

Corrosion of the instrument may occur if spilled sample is allowed to remain


in the sample catcher. Keep the sample catcher clean.

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7.3.3 Replacing the Pump Head of the Rinse Pump

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.

Figure 7.16 Replacing the Pump Head of the Rinse Pump

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7.4 8-Port Sampler (OCT-L) Maintenance

7.4 8-Port Sampler (OCT-L) Maintenance


Describes periodic inspection procedures for the OCT-L.

7.4.1 Replacing the 8-Port Valve Rotor

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.

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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.

Figure 7.17 Removing the Nut

4 Remove the 8-port valve by pulling it downward.

5 Loosen the retaining nut using the provided wrench.

Figure 7.18 Removing the Retaining Bracket

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.

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7.4 8-Port Sampler (OCT-L) Maintenance

7 Note the orientation of the rotor hole position. Grasp the rotor with forceps,
and remove by pulling upwards.

Figure 7.19 Removing the Rotor

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.

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7.5 TN Unit (TNM-L) Maintenance


Describes periodic inspection procedures for the TNM-L.
Maintenance of the TNM-L includes periodic inspection of the ozone treatment unit
catalyst, chemiluminescence detector and ozone generator.

7.5.1 Replacing the Catalyst in the Ozone Treatment Unit

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.

The interior of the ozone treatment unit is heated to 50°C. Perform


maintenance only after cooling for at least two hours.

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.

Figure 7.20 Removing the Ozone Treatment Unit

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7.5 TN Unit (TNM-L) Maintenance

2 Remove the larger diameter fluoro rubber plug and take out the used catalyst
and polypropylene packing material.

3 Insert a small amount of new polypropylene packing material at the bottom of


the vessel and then fill with catalyst to about 2 cm below where the vessel
hollows. Insert another small amount of polypropylene packing material on top
of the catalyst and then reattach the fluoro rubber plug. (The amount of catalyst
is about 150 g.)

Figure 7.21 Filling the Ozone Treatment Unit with Catalyst

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.

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7 Maintenance

5 Return the ozone treatment unit to its original position in the instrument and
reconnect the tubing to each end of the unit.

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 catalyst contains manganese dioxide.

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.

Checking the Operation Time of the Ozone Generator

1 Connect the Sample Table Editor to the instrument.


Refer to "Connection" P.253 for the connection procedure.

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 is displayed.

The Maintenance History Dlg window can also be displayed by selecting Instrument –
Maintenance – History.

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7.5 TN Unit (TNM-L) Maintenance

3 Examine the number in the Current field for Ozone Generator.

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.

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7.5.3 Replacing the NOx Absorber

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.

Discarding the NOx Absorber (CO2 Absorber)


Place a request to an authorized industrial waste contractor to process the used NOx
absorber (CO2 absorber). Clearly indicate in the industrial waste material manifest that
the absorber contains soda lime.

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7.6 Maintenance Menus

7.6 Maintenance Menus


Describes maintenance menu functions controlled by the TOC-Control L software.
This section describes the Maintenance operations used to conduct instrument
maintenance and checking instrument operation.

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.

Display from the Menu Bar


Open a Sample Table and establish connection with the instrument. From the menu
bar, Select Instrument – Maintenance.

Display from the File Viewer


Open the Sample Table tab of the file viewer. Right-click on the connected system
configuration icon, and select Maintenance.

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Zero Point Detection


Use this function to determine the zero point of the syringe.

Regeneration of the TC Catalyst


Use this function to restore the sensitivity and efficiency of the TC catalyst. During the
regeneration process, 1 mol/L of hydrochloric acid is injected into the TC combustion
tube. This process is repeated several times. For details, refer to "7.2.1 Catalyst
Regeneration" P.320.

Regeneration of the IC Solution


Use this function to restore acidity to the IC reagent solution. This function is not
accessible with the TOC-LCPN instrument. For details, refer to "3.1.14 IC Analysis
Preparations" P.55.

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7.6 Maintenance Menus

Replace Flowline Content


Use this function to remove bubbles from the dilution water tubing and hydrochloric
acid tubing connected to the 8-port valve.

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.

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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.

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7.6 Maintenance Menus

• ASI/8 Port Sampler Tab


The enabled items will vary depending on the optional accessories connected.

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.

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Initialize ASI/8Port Sampler


This function initializes the ASI-L or OCT-L. This option is disabled if an ASI-L or OCT-L
is not connected to the system.

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.

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7.6 Maintenance Menus

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

• Number of 8-port valve operations


• Volume of sample injected into the combustion tube
• Volume of acid used
• Number of syringe operations
• IC pump operation time (recommended warning value: 300 hours)
• Ozonizer (ozone generator) operation time (enabled when using the TNM-L)
• ASI-L wash pump operation time (recommended warning value: 300 hours)
• Number of ASI-L magnetic stirrer operations
• OCT-L 8-port valve operation time

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.

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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.

Sparge Gas Valve


Select this item to sparge with the external sparge kit. Deselect to turn the sparge flow
off.

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7.7 Troubleshooting

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.

7.7.1 Error Messages

Take the corrective action indicated in the table below when any of the following error
messages are displayed.

Table 7.1 Error and Warning Messages

Message Description Corrective Action


Switch off power to the
instrument. Switch on the
Failed to detect the syringe
ERROR: Find zero point power again, operate the
zero point.
instrument, and verify whether
the same error occurs again.
Operation cannot continue Mount the vial rack in the
ERROR: No vial rack because the vial rack is not turntable and execute the
mounted in the turntable. operation again.
Measurement cannot be
ERROR: Rack type performed because the vial rack Verify the type of vial rack
mismatch specified in the settings differs mounted in the instrument.
from the detected vial rack.
Switch off power to the
ERROR: Battery The battery voltage has instrument. Contact your
replacement depleted. Shimadzu representative as this
problem requires servicing.
Replenish the hydrochloric acid
The volume of hydrochloric acid
in the acid vessel and then
used has exceeded the
ERROR: No Acid reset the Total Acid Vol counter
threshold value set in the
in the Maintenance History
Maintenance History window.
window.
The volume of sample injected Regenerate or replace the
ERROR: Sample volume
into the combustion tube has catalyst, replace the combustion 7
exceeded the threshold value tube, and then reset the Total
count
set in the Maintenance History TC Inj Vol counter in the
window. Maintenance History window.
The number of syringe strokes Replace the plunger tip and
ERROR: Move syringe has exceeded the threshold then reset the Syringe Strokes
count value set in the Maintenance counter in the Maintenance
History window. History window.
Wait for the electric furnace to
ERROR: TC furnace The temperature of the TC
rise to the set temperature
temperature during furnace is too low to
before executing catalyst
regeneration regenerate catalyst.
regeneration.
The ASI needle cover or sample Close the ASI needle cover or
ERROR: ASI cover open
cover is open. sample cover.

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Message Description Corrective Action


The operation time of the IC Replace the IC pump tube and
pump has exceeded the then reset the IC Unit Pump
ERROR: IC acid pump
threshold value set in the (hour) counter in the
Maintenance History window. Maintenance History window.
The operation time of the ASI Replace the ASI pump tube and
pump has exceeded the then reset the ASI Rinse Pump
ERROR: ASI rinse pump
threshold value set in the (hour) counter in the
Maintenance History window. Maintenance History window.
The number of operations of Replace the 8-port valve rotor
WARNING: 8port valve the 8-port valve has exceeded and then reset the 8Port Valve
rotor operation the value set in the Operation (no.) counter in the
Maintenance History window. Maintenance History window.
Replace the ozone generator
The operation time of the
and then reset the Ozonizer
WARNING: Ozonizer ozone generator has exceeded
Operation Time (hour) counter
operation time the value set in the
in the Maintenance History
Maintenance History window.
window.
Replace the CO2 absorber and
The CO2 absorber has exceeded then reset the date for CO2
WARNING: CO2 absorber
its expiry date. Absorber, replaced on in the
Maintenance History window.
The operation time of stirrer Replace stirrer motor 1 and
WARNING: ASI stirrer motor 1 has exceeded the value then reset the ASI Stirrer(1)
motor 1 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.
The operation time of stirrer Replace stirrer motor 2 and
WARNING: ASI stirrer motor 2 has exceeded the value then reset the ASI Stirrer(2)
motor 2 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.
The operation time of stirrer Replace stirrer motor 3 and
WARNING: ASI stirrer motor 3 has exceeded the value then reset the ASI Stirrer(3)
motor 3 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.
The operation time of stirrer Replace stirrer motor 4 and
WARNING: ASI stirrer motor 4 has exceeded the value then reset the ASI Stirrer(4)
motor 4 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.
The operation time of stirrer Replace stirrer motor 5 and
WARNING: ASI stirrer motor 5 has exceeded the value then reset the ASI Stirrer(5)
motor 5 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.
The operation time of stirrer Replace stirrer motor 6 and
WARNING: ASI stirrer motor 6 has exceeded the value then reset the ASI Stirrer(6)
motor 6 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.
The operation time of stirrer Replace stirrer motor 7 and
WARNING: ASI stirrer motor 7 has exceeded the value then reset the ASI Stirrer(7)
motor 7 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.

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7.7 Troubleshooting

Message Description Corrective Action


The operation time of stirrer Replace stirrer motor 8 and
WARNING: ASI stirrer motor 8 has exceeded the value then reset the ASI Stirrer(8)
motor 8 set in the Maintenance History Operation (hour) counter in the
window. Maintenance History window.
Replace the OCT-L (1) 8-port
The number of operations of
valve and then reset the
WARNING: OCT(1) 8port the OCT-L (1) 8-port valve has
OCT-L(1) 8 Port Valve Operation
valve operation exceeded the value set in the
(no.) counter in the
Maintenance History window.
Maintenance History window.
Replace the OCT-L (2) 8-port
The number of operations of
valve and then reset the
WARNING: OCT(2) 8port the OCT-L (2) 8-port valve has
OCT-L(2) 8 Port Valve Operation
valve operation exceeded the value set in the
(no.) counter in the
Maintenance History window.
Maintenance History window.
WARNING: TOC-L carrier The carrier gas pressure is too Check the condition of the
gas pres low low. carrier gas supply.
Before starting measurement
If the vial cover opened state is
based on a schedule, open the
not recognized although
vial cover once and check that
measurement has been
an error message is displayed,
conducted for more than 200
ERROR: ASI vial cover to ensure that the sensor is
vials, the sensor may be faulty.
sensor working correctly.
This error may also occur due
If the sensor is not working
to false recognition when vials
correctly, contact your
are changed while the power is
Shimadzu representative as this
off.
problem requires servicing.

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.

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7 Maintenance

Table 7.2 Fatal Error Messages

Message Description Corrective Action


Switch off power to the
An error occurred while writing instrument. Contact your
ERROR: Flash ROM
to memory. Shimadzu representative as this
problem requires servicing.
With the power on, wait
approximately 20 minutes for
the temperature of the electric
furnace to decrease and then
ERROR: Furnace
The electric furnace overheated. switch off the instrument.
overheat
Switch on the power again,
operate the instrument, and
verify whether the same error
occurs again.
Switch off power to the
instrument. Switch on the
The temperature of the electric
ERROR: Furnace error power again, operate the
furnace does not rise.
instrument, and verify whether
the same error occurs again.
ERROR: Carrier gas flow The carrier gas flow rate does Check the condition of the
control error ! not reach the set value. carrier gas supply.
Switch off power to the
instrument and remove any
The syringe is not operating
foreign particles from the
normally due to clogging of the
ERROR: Syringe pump tubing. Switch on the power
tubing connected to the 8-port
again, operate the instrument,
valve.
and verify whether the same
error occurs again.
Switch off power to the
instrument. Switch on the
ERROR: Syringe pulse A problem occurred during
power again, operate the
count syringe operation.
instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Remove the rotor
ERROR: 8Port valve A problem occurred during
from the 8-port valve, remove
position 8-port valve operation.
any particles found in the valve,
and wash the valve.
Switch off power to the
The 8-port valve is not
instrument. Remove the rotor
ERROR: 8Port valve operating normally due to
from the 8-port valve, remove
pulse count clogging inside the sample
any particles found in the valve,
injector 8-port valve.
and wash the valve.
Switch off power to the
The TC slider is not operating
instrument and remove any
ERROR: TC slider normally due to particles
particles. Switch on power
position trapped between its moving
again after removing the cause
parts.
of the error.
Switch off power to the
The IC slider is not operating
instrument and remove any
normally due to particles
ERROR: IC slider position particles. Switch on power
trapped between its moving
again after removing the cause
parts.
of the error.

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7.7 Troubleshooting

Message Description Corrective Action


Switch off power to the
instrument. Switch on the
A problem occurred during
ERROR: Zero detection power again, operate the
syringe operation.
instrument, and verify whether
the same error occurs again.
The ASI arm is not operating Switch off power on the TOC-L
ERROR: ASI arm vertical
normally in the vertical main unit. Switch on the power
position
direction. again, operate the instrument,
The ASI arm is not operating and verify whether the same
ERROR: ASI arm vertical error occurs again.
normally in the vertical
pulse count Since the problem is unrelated
direction.
to the TOC-L main unit,
The ASI arm is not operating disconnect the ASI-L from the
ERROR: ASI arm
normally in the horizontal main unit, and perform
horizontal position
direction. operations using the TOC-L
The ASI arm is not operating main unit alone until normal
ERROR: ASI arm operation of the ASI-L is
normally in the horizontal
horizontal pulse count restored.
direction.
Switch off power to the
instrument. Switch on the
The ASI turntable is not
ERROR: ASI tray position power again, operate the
operating normally.
instrument, and verify whether
the same error occurs again.
Switch off power on the TOC-L
main unit.
Make sure the rack is properly
The rotation direction of the
seated on the ASI-L turntable
ASI turntable could not be
and remove any objects that
detected. Either the rack is not
ERROR: ASI tray pulse may be blocking the position
properly seated in the turntable
count detection notch on the
or some object may be blocking
periphery of the rack. After
a position detection notch on
eliminating the cause of the
the periphery of the rack.
problem, close the ASI-L cover
and switch on power to the
instrument again.
The photocouplers (two
locations) for detecting the Switch off power to the
ERROR: SSM_TC sample position of the TC sample boat instrument. Contact your
boat position are not operating correctly. Shimadzu representative as this 7
(Both photocouplers are problem requires servicing.
detecting that light is blocked.)
The photocouplers (two
locations) for detecting the Switch off power to the
ERROR: SSM-IC sample position of the IC sample boat instrument. Contact your
boat position are not operating correctly. Shimadzu representative as this
(Both photocouplers are problem requires servicing.
detecting that light is blocked.)
Switch off power to the
instrument. Remove the rotor
The OCT-L (1) 8-port valve is
ERROR: 8Port Sampler1 - from the OCT-L (1) 8-port valve
not operating normally due to
8Port Valve Position and either remove any particles
clogging inside the valve.
found in the valve or wash the
valve.

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7 Maintenance

Message Description Corrective Action


Switch off power to the
instrument. Remove the rotor
The OCT-L (2) 8-port valve is
ERROR: 8Port Sampler2 - from the OCT-L (2) 8-port valve
not operating normally due to
8Port Valve Position and either remove any particles
clogging inside the valve.
found in the valve or wash the
valve.
Switch off power to the
instrument. Remove the rotor
The OCT-L (1) 8-port valve is
ERROR: 8Port Sampler1 - from the OCT-L (1) 8-port valve
not operating normally due to
8Port Valve Position and either remove any particles
clogging inside the valve.
found in the valve or wash the
valve.
Switch off power to the
instrument. Remove the rotor
The OCT-L (2) 8-port valve is
ERROR: 8Port Sampler2 - from the OCT-L (2) 8-port valve
not operating normally due to
8Port Valve Position and either remove any particles
clogging inside the valve.
found in the valve or wash the
valve.
Switch off power to the
instrument. Switch on the
ERROR: Dehumidifier The fan on the electronic cooler
power again, operate the
fan stopped ! has stopped.
instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Switch on the
ERROR: ASI emergency The ASI encountered an
power again, operate the
stopped ! emergency stop.
instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Switch on the
ERROR: Main fan The instrument fan has
power again, operate the
stopped ! stopped.
instrument, and verify whether
the same error occurs again.
Switch off power to the
The power supply to the instrument. Switch on the
ERROR: TC Furnace
electric furnace is not operating power again, operate the
power error!
normally. instrument, and verify whether
the same error occurs again.
Switch off power to the
The temperature controller of instrument. Switch on the
ERROR: Dehumidifier
the cooler is not operating power again, operate the
temperature error !
normally. instrument, and verify whether
the same error occurs again.
Switch off power to the
The temperature controller of instrument. Switch on the
ERROR: TOC detector
the TOC detector is not power again, operate the
temperature error !
operating normally. instrument, and verify whether
the same error occurs again.
Switch off power to the
The motor drive of the TOC instrument. Switch on the
ERROR: TOC detector
detector is not operating power again, operate the
motor error !
normally. instrument, and verify whether
the same error occurs again.

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7.7 Troubleshooting

Message Description Corrective Action


Switch off power to the
instrument. Switch on the
ERROR: TOC detector A memory error occurred inside
power again, operate the
memory error ! the TOC detector.
instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Switch on the
ERROR: TOC detector The TOC detector is not
power again, operate the
connection error ! connected properly.
instrument, and verify whether
the same error occurs again.
Switch off power to the
The temperature controller of instrument. Switch on the
ERROR: TN detector
the TN detector is not power again, operate the
temperature error !
operating normally. instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Switch on the
ERROR: TN detector A memory error occurred inside
power again, operate the
memory error ! the TN detector.
instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Switch on the
ERROR: TN detector The TN detector is not
power again, operate the
connection error ! connected properly.
instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Switch on the
ERROR: TN detector fan The TN detector fan has
power again, operate the
stopped ! stopped.
instrument, and verify whether
the same error occurs again.
Switch off power to the
An error occurred in the instrument. Switch on the
ERROR: Ozone pressure
pressure sensor for the ozone power again, operate the
sensor error !
stream of the TN detector. instrument, and verify whether
the same error occurs again.
Switch off power to the
An error occurred related to
instrument. Switch on the
the sparge gas stream. There is
ERROR: Sparge gas line
a possibility that the stream
power again, operate the 7
instrument, and verify whether
line is clogged.
the same error occurs again.
Switch off power to the
An error occurred in the instrument. Switch on the
ERROR: Pressure sensor
pressure sensor for supplying power again, operate the
1 error !
gas. instrument, and verify whether
the same error occurs again.
Switch off power to the
An error occurred in the instrument. Switch on the
ERROR: Pressure sensor
pressure sensor for detecting power again, operate the
2 error !
the carrier gas flow rate. instrument, and verify whether
the same error occurs again.

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Message Description Corrective Action


Switch off power to the
An error occurred in the instrument. Switch on the
ERROR: Pressure sensor
pressure sensor for detecting power again, operate the
3 error !
the sparge gas flow rate. instrument, and verify whether
the same error occurs again.
Switch off power to the
instrument. Remove the rotor
ERROR: 8 port valve A problem occurred during
from the 8-port valve, remove
retry 8-port valve operation.
any particles found in the valve,
and wash the valve.
Switch off power to the
The instrument main unit's data
instrument. Contact your
ERROR: CF Card storage device is not operating
Shimadzu representative as this
normally.
problem requires servicing.
ERROR: Protocol Check the protocol version of
The protocol version of the
mismatched. Please the firmware and PC software.
firmware does not match that
check the software The PC software must be
of the PC software.
version. upgraded.
Switch off power to the
Firmware is old, so Firmware is old, so update is instrument. Contact your
update is required. required. Shimadzu representative as this
problem requires servicing.

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7.7 Troubleshooting

7.7.2 Troubleshooting

n TOC-L

(1) An error message is displayed.


→ Refer to error message.
(2) The Ready lamp will not light.
→ Access the Background Monitor screen by selecting Background Monitor from the
Instrument menu. Refer to the screen to see which parameters are not satisfied.
(3) The baseline stays over the auto zero range. Baseline position never reaches the ready
state.

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(4) The baseline is unstable.

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7.7 Troubleshooting

(5) Poor reproducibility with standard solution.

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7 Maintenance

(6) No peaks appear after sample injection.

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.

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7.7 Troubleshooting

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.

(7) If the NPOC measurement value is higher than anticipated

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

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n ASI-L

(1) The ASI-L does not operate.

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7.7 Troubleshooting

(2) Rinse water is not delivered from the rinse port.

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(3) Reproducibility is poor.

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7.7 Troubleshooting

n OCT-L, 8-Port SamplerL

(1) OCT-L does not operate.

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(2) Reproducibility is poor.

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7.7 Troubleshooting

n Corrective Actions for Poor Reproducibility

Corrective Action for Poor Sample Injection


The manner in which sample is discharged from the TC or IC sample injection tubing has
a large influence on reproducibility. The sample should be injected as vertically as possible
onto the TC catalyst or into the IC reaction vessel. If the sample is scattered or injected
obliquely, detach the sample injection tubing from the slider, and remove any obstruction
that may be adhering to the opening at the tip of the sample tubing.

Figure 7.22 Sample Injection Patterns from Sample Tubing

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

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7 Maintenance

Figure 7.23 Slider Assembly

Corrective Action to Eliminate Bubbles Inside the Syringe


Small bubbles that adhere to the inside of the syringe by the plunger tip will have little
effect on analysis values. Larger bubbles inside the syringe will affect values and result
in poor reproducibility. Large bubbles form easily inside a dirty syringe. This is evident
when sample is mixed with dilution water in the syringe and when sparging with carrier
gas inside the syringe for IC removal pretreatment for NPOC analysis. In this case, detach
the syringe from the syringe pump. Repeatedly draw in and discharge laboratory
glassware detergent to wash the inside of the syringe. Then draw in a full-stroke volume
of the cleaning agent and let it sit for about 20 minutes, or overnight if the syringe is
extremely dirty. Thoroughly rinse away all of the detergent and reattach the syringe to
the syringe pump.

Decreased Reproducibility Due to Plunger Tip Backlash


The plunger tip is a consumable item and, as it is used, wears in the following ways:

(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.

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7.7 Troubleshooting

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.

1 By reversing the procedure described in "Connecting the Combustion Tube" ("3.


1.3 Connecting the Combustion Tube" P.26), remove the sample injector from the
instrument together with the broken upper end of the combustion tube.

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.

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7 Maintenance

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.

2 Open the Sample Table Editor again.


For details, refer to "5.2.1 Opening the Sample Table Editor" P.139.

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.

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8 Reference Information
This chapter describes the principles of analysis and lists instrument specifications,
accessories, and parts. This chapter also includes installation procedures, for use in the
event that the instrument is relocated.

8.1 Principles of Analysis


The principles for TC, IC, POC, NPOC, TOC and TN analysis are described in this section.
Two types of carbon are present in water: organic carbon and inorganic carbon. Organic
carbon (TOC) bonds with hydrogen or oxygen to form organic compounds. Inorganic
carbon (IC or TIC) is the structural basis for inorganic compounds such as gas carbonates
and carbonate ions. Collectively the two forms of carbon are referred to as total carbon
(TC) and the relationship between them is expressed TOC=TC-IC.
Nitrogen is also present in water in two types: organic and inorganic. The sum of these
is referred to as total nitrogen (TN).
The principles underlying TC and TN analysis are explained in the following sections.

8.1.1 Principles of TC (Total Carbon) Analysis

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.

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8.1.2 Principles of IC (Inorganic Carbon) Analysis

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.

Analysis Using the IC Reaction Vessel (H Type Instrument)


The TOC-L IC reactor kit is used to sparge the IC reaction solution (acidified reaction
liquid) with carrier gas. Sample is injected into the IC reaction vessel and the IC in the
sample is converted to carbon dioxide, which is volatilized by the sparging process and
detected by the NDIR.

Analysis Within the Syringe (N Type Instrument)


The sample is acidified to pH 3 or lower in the syringe, using hydrochloric acid. The
sample is sparged with carrier gas and the IC in the sample is converted to carbon dioxide
and detected by the NDIR.

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8.1 Principles of Analysis

8.1.3 Principles of NPOC (Non-Purgeable Organic Carbon) Analysis

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)

Pre-Sparging Conc. Post-Sparging Conc. Residual Rate


Organic Substance
(ppm) (ppm) (%)
Methanol 117.5 116 98.6
Ethanol 106.5 105 98.5
Isopropyl alcohol 129 127 98.5
n-butyl alcohol 117 115 98.3
Acetone 106 101 95.3
Acetaldehyde 130 117 90.0
Ethyl acetate 102 88 86.3
Tyrosine 117 116.5 99.5
Benzene 85 2.5 2.9
Cyclohexane 79 2 2.5

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8.1.4 Principles of POC (Purgeable Organic Carbon) Analysis

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.

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8.1 Principles of Analysis

8.1.5 Principles of Measuring TOC

TOC can be measured using the following 3 methods:


• TC-IC Method
• NPOC Method
• POC+NPOC Method

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.

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8.1.6 Principles of Measuring TN (Total Nitrogen)

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.

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8.2 Analysis-Related Technical Information

8.2 Analysis-Related Technical Information


This section summarizes technical information related to analysis, including peak area
analysis and calibration curve selection.

8.2.1 Peak Area Analysis

When a sample is analyzed, the TOC-Control L software automatically detects the


beginning and end of each peak produced, and calculates the peak areas. Detection of
the beginning and end of each peak is based on the slope of the tangent, which changes
from moment to moment. Peak detection begins when that slope exceeds a
predetermined value and ends when a negative slope falls below a specified value.

• 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.

Figure 8.1 Determining Peak Area

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8.2.2 Peak Shape

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.

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8.2 Analysis-Related Technical Information

8.2.3 Calibration Curves

n Types of Calibration Curves

1-Point and 2-Point Calibration Curves


The output signals of the TOC-L are linearized. As a result, there are almost no factors
in the reaction systems of the TC/TN combustion and IC reaction components that might
cause the concentration-output characteristic to deviate from linearity. Consequently,
calibration curves are commonly generated as 1-point curves consisting of 1 span point,
or 2-point curves consisting of 1 span point and the zero point.
The concentration of TC and IC, or of TN, varies with standard solutions prepared with
pure water. A calibration curve generated using concentrations greater than
50 - 100 mg/L will pass very close to the zero point. In this case, it is practical to generate
a 1-point calibration curve.
Use a 2-point calibration curve when the concentration of TC and IC or TN in the pure
water used to prepare the standard solutions cannot be disregarded with respect to the
standard solution concentration. For information on handling of this type of curve, refer
to "Shifting of Calibration Curves" P.390.

Multi-Point Calibration Curves


Calibration curves can be generated using up to 10 points. Calibration curves consisting
of 3 or more points can be generated as a point-to-point curve or as a regression line
using the least squares method. With the least squares regression curve, a correlation
coefficient is displayed.

Multi-Point Calibration Curve Function for Dilution of Stock Solution


This function creates multi-point calibration curves through the dilution of standard
solution. The use of this function enables the creation of multi-point calibration curves
with a single batch of standard solution. Activate the function by selecting the Use
dilution from standard solution checkbox in the Calibration Curve Wizard (Page 2)
Calibration Curve Type window.
Supported analysis types: TC, IC (CPH only), and TN

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.

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8 Reference Information

n Shifting of Calibration Curves

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.

Shift to Blank Point


The "shift to blank point" procedure is performed for high sensitivity analyses when the
system blank value could have a significant effect on the measurement value.
By selecting the "shift to blank point" option, a TC blank check analysis is performed
using the same injection volume that will be used for sample measurement. The
calibration curve zero point is shifted to the TC blank check value.

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8.2 Analysis-Related Technical Information

Figure 8.2 Shifting of Calibration Curve

8.2.4 Sparging During Standard Solution Analysis

Standard solutions that have TC concentrations so low as to be affected by the amount


of dissolved carbon dioxide in the solution should be sparged with carrier gas prior to
measurement. Sparging eliminates the dissolved carbon dioxide, thereby preventing it
from affecting the concentration of the standard solution.
The amount of dissolved carbon dioxide in water used for standard solution preparation
is affected by factors such as water purification method, length and condition of storage,
and the concentration of carbon dioxide in the atmosphere. Concentrations of dissolved
carbon dioxide increase when the water is exposed to the atmosphere during the
standard solution preparation process. Refer to "Table 8.2 CO2 Content (ppm) in Distilled
Water Equilibrated with Atmosphere Temperature (°C)" for the dissolution rates of
atmospheric carbon dioxide in water.
It is important to consider both the concentration of the standard solution and the
concentration of TOC contained in the preparation water when deciding whether to use
the sparging function. Use of sparging is appropriate if the TOC contained in the water
is low enough to not substantially affect the standard solution concentration, but not
low enough to be ignored.

Do not use sparging with IC standard solutions, as sparging decreases the IC


concentration.

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

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8.2.5 Automatic Selection of Optimum Calibration Curve

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

By setting the concentration ratio between calibration curves to a factor of


approximately 10, the automatic selection function can be effectively utilized for
analyses covering a wide range of concentrations. For example, use a
concentration of 10 mg/L for Calibration Curve 1, 100 mg/L for Calibration Curve
2, and 1000 mg/L for Calibration Curve 3.

Considerations for the Automatic Selection Function


• The automatic selection process rules do not change when multi-point calibration curves
are included.
• When more than one injection is performed, the calibration curve is selected based on
the measured value of the first injection.
• Because the measured value is always calculated first using Calibration Curve 1, specify
the most commonly used calibration curve in this field.
• The priority of the second and third calibration curves is determined based on the
calibration curve concentrations and the sample concentration.

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8.2 Analysis-Related Technical Information

8.2.6 Automatic Correction for Injection Volume and Dilution Factor

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.

Automatic Correction Function for Injection Volume and Dilution Factor


The injection volume and dilution factor are automatically adjusted when the
measurement results exceed the concentration of the calibration curve. In these
adjustments, the injection volume is corrected so that, based on the measurement results,
the peak area value becomes about 80 % of the corresponding calibration curve. The
measurement is performed again after the correction.

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.

8.2.7 Multi-Stage Injection

Activate the multi-stage injection function by selecting the Multiple Injections checkbox
in the Method Wizard (Page 4) Injection Parameters window.

Multi-Stage Injection Function


This function extracts multiple injections worth of sample at once into the syringe and
measures the sample over multiple injections. This enables rapid measurement because
acid addition and dilution can all be performed at once within the syringe. This function
only supports the following analysis types.
Supported analysis types: TC, IC (CPH only), NPOC, and TN

Notes on the Multi-Stage Injection Function


• Reproducibility may deteriorate compared to normal measurement.
• The measurement process may restart from water sampling when measurement
conditions are changed automatically by the automatic selection function for optimum
8
calibration curves, automatic correction function for injection volume, or automatic
correction function for dilution factor.

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8.2.8 Pharmaceutical Water Testing

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.

n USP (United States Pharmacopeia) and EP (European Pharmacopoeia) Support

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.

n JP (Japanese Pharmacopoeia) Support

A recovery rate test and pharmaceutical water test are defined in the JP standards.

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8.3 Specifications

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

Analyte TC, IC, TOC (TC-IC), NPOC

Measurement 680 °C catalytically-aided combustion oxidation/non-dispersive


principle infrared detection (NDIR)
TC: 0 - 30000 mg/L
IC:
Measuring range
TOC-LCPH: 0 - 35000 mg/L
TOC-LCPN: 0 - 3000 mg/L
TC:
TOC-LCPH: 4 µg/L
Detection limits
TOC-LCPN: TC: 50 µg/L
IC:4 µg/L
TC: Approx. 3 min
IC:
Measurement time
TOC-LCPH: Approx. 3 min
TOC-LCPN: Approx. 4 min
TOC-LCPH:
TC, IC, NPOC CV 1.5 % or ±4 µg/L max.
(Option: TN: CV 3.0 % or ±5 µg/L max.)
Repeatability TOC-LCPN:
TC, NPOC CV 1.5 % or ±50 µg/L max.
IC CV 1.5 % or ±4 µg/L max.
(Option: TN: CV 3.0 % or ±20 µg/L max.)
Sample introduction Auto injection using syringe pump/slider
TC:
• TOC-LCPH: 10 to 2000 µL (variable)

Sample injection • TOC-LCPN: 10 to 150 µL (variable)


volume IC: 8
• TOC-LCPH: 10 to 2000 µL (variable)
• TOC-LCPN: 10 to 4500 µL (variable)
Sample dilution
Dilution within syringe, dilution factor 2 - 50 times
function
Pretreatment for IC Automatic acid addition and sparging

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8 Reference Information

High purity air (from cylinder)


High purity nitrogen (with addition of the N2 carrier gas kit)
Carrier gas
Pressurized air (with addition of the carrier gas purification kit (only
applicable to the TOC-LCPN))
Approx. 200 ± 10 kPa (300 to 600 kPa when using the carrier gas
Carrier gas pressure
regulator option)
TOC-LCPH: 150 mL/min (230 to 250 mL/min when sparging)
Carrier gas flow rate
TOC-LCPN: 230 mL/min
Ambient temperature 5 - 35 °C
Power requirements AC 100-120V ±10 % or AC 220-240V ±10 %, 600 VA, 50/60 Hz
Fuse 10A LAG x 2, Interrupting capacity: 100A
Approximate
(W) 340 ´ (D) 660 ´ (H) 480 mm (excluding projections)
dimensions
Weight Approx. 35 kg

8.3.2 ASI-L

9 mL vial rack: 9 mL (External diameter 13 x Height 100 mm),


100 vials
24 mL vial rack: 24 mL (External diameter 23 x Height 85 mm),
Sample containers
100 vials, 100 septum-equipped caps
40 mL vial rack: 40 mL (External diameter 27 x Height 95 mm),
72 vials, 72 septum-equipped caps
9 mL vial rack: 93 vials
Vial rack capacity 24 mL vial rack: 93 vials
40 mL vial rack: 68 vials
• Acid addition and sparging possible for NPOC analysis
(with addition of the external sparge kit)
Sample pretreatment • Needle rinse possible
• Stirring with magnetic stirrer
(with addition of the magnetic stirrer, excluding 9 mL vials)
Ambient temperature 5 - 35 °C
Approximate
(W) 370 ´ (D) 540 ´ (H) 490 mm (excluding projections)
dimensions
Weight Approx. 14 kg

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8.3 Specifications

8.3.3 OCT-L 8-Port Sampler

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

Analyte TN (total nitrogen)


Measurement Thermal decomposition / NO detection
principle (chemiluminescence method)
Measuring range 0 - 10000 mg/L
• TOC-LCPH: 5 µg/L
Detection limit
• TOC-LCPN: 20 µg/L
Measurement time Approx. 4 min
Repeatability Higher value of within CV3 % or ± 5 µg/L

Sample injection • TOC-LCPH: 10 to 300 µL (variable)


volume • TOC-LCPN: 10 to 150 µL (variable)
Ambient temperature 5 - 35 °C
Approximate
(W) 270 ´ (D) 240 ´ (H) 160 mm (excluding projections)
dimensions
Weight Approx. 6 kg

8.3.5 POC Measurement Kit

Analyte POC (volatile organic carbon)


Sparging / CO2 removal / 680 °C combustion oxidation /
Measurement method
nondispersive infrared detection (NDIR)
CO2 removal method Absorption via lithium hydroxide, removal
Measuring range 0 - 500 mg/L
8
Detection limit 4 µg/L
Measurement time Approx. 4 min
Repeatability CV within 1.5%

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8 Reference Information

8.3.6 Carrier Gas Purifier Kit

Gas purification Combustion oxidation / CO2 removal


method
Carrier gas supply Pressurized air or oxygen (free of dust, oil mist, water droplets, etc.)
Carrier gas supply
200±10 kPa
pressure

8.3.7 Manual Injection Kit (Gas Sample Injection Kit)

Liquid samples: TC, IC, TOC (TC-IC)


Gas samples: TC, carbon dioxide, TOC (determined by TC-carbon
dioxide; Carbon monoxide and other inorganic carbon containing
Analyte
gases aside from carbon dioxide are also measured as TOC)
Measurement of IC, TOC and carbon dioxide is possible with the
TOC-LCPH

Measurement 680 °C catalytically-aided combustion oxidation/non-dispersive


principle infrared detection (NDIR)
Liquid sample:
TC: 0 - 20000 mg/L
Measuring range IC: 0 - 20000 mg/L
Gas sample:
6 ppm - 100 % CO2

Sample injection Liquid sample: 1 - 150 µL


volume Gas sample: 20 µL - 10 mL
Liquid sample:
TC: Approx. 3 min
Measuring time
IC: Approx. 3 min
Gas sample: 2 - 4 min
Liquid sample: CV within 2 % (CV is within 3 % when sample
Repeatability concentration is 8000 mg/L or greater)
Gas sample: CV within 2 %
Sample introduction Manual injection using microsyringe

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8.3 Specifications

8.3.8 B-Type Halogen Scrubber

TC: 60 µg/L
Detection limit IC: 4 µg/L
TN: 30 µg/L
TC: 10 to 150 µL

Sample injection IC:


volume • TOC-LCPH: 10 to 2000 µL (variable)
• TOC-LCPN: 10 to 4500 µL (variable)
Repeatability CV within 3 %

8.3.9 External Sparge Kit

Flow rate adjustment


0 to 300 mL/min
range

8.3.10 High Suspension Kit for High Concentrations

TC: 0 to 300 mg/L


Analysis range IC: 0 to 300 mg/L
(Optional TN: 0 to 100 mg/L)
TC: 100 µg/L
Detection limit IC: 100 µg/L
(Optional TN: 40 µg/L)

Sample injection TC, IC: 80 µL


volume (Optional TN: 80 µL)
TC, IC, NPOC: CV within 1.5 %
Repeatability
(Optional TN: CV within 3.0 %)

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8 Reference Information

8.3.11 High Suspension Kit for Low Concentrations

TC: 0 to 150 mg/L


Analysis range IC: 0 to 150 mg/L
(Optional TN: 0 to 50 mg/L)
TC: 50 µg/L
Detection limit IC: 50 µg/L
(Optional TN: 20 µg/L)

Sample injection TC, IC: 150 µL


volume (Optional TN: 150 µL)
TC, IC, NPOC: CV within 1.5 %
Repeatability
(Optional TN: CV within 3.0 %)

8.3.12 Recommended PC Specifications

Windows 10 Pro (64bit),


OS
Windows 10 Enterprise LTSC (64bit)
CPU 3.0 GHz or faster
Memory 8 GB or greater
Hard drive 200 GB or greater
Monitor resolution 1280 ´ 1024 pixels or greater

DVD drive
Other
USB port

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8.4 Standard Accessories

8.4 Standard Accessories


The standard accessories are listed in this section.

Table 8.3 Standard Accessories List 1 (TOC-LCPH/CPN)

Part Number Part Name TOC-LCPH TOC-LCPN


S638-41323 Combustion tube, in case 2 1
S638-92069-02 TOC regular catalyst set 1 1
S638-92070-01 TOC high sensitivity catalyst set 1 -
638-42100-01 Cooling tubing unit 1 -
S638-16023 Catalyst filling rod 1 1
S638-59296-01 Plunger tip 1 1
S638-59296 Syringe 1 1
S072-60320-01 Wiring band 2 2
S072-02004-26 Fuse (100-127V) 2 2
S072-02004-27 Fuse (220-240V) 2 2
S631-78002 Wrench, for 8-port valve 1 1
S638-53152 Rinse water bottle 1 1
S638-20072 Cap 2 1
S638-64091-91 DVD-ROM "TOC-Control L" 1 1
S088-52859-65 USB cable 1 1
S038-00292-04 Plastic bottle 2 1
S630-00557 Quartz wool, 1 g 1 1
S630-00992 Halogen scrubber 1 1
638-94843-41 User's Manual (Disk provided) 1 1

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8 Reference Information

Table 8.4 Standard Accessories List 2 (ASI-L Autosampler)

Part Number Part Name 9 mL 24 mL 40 mL


S638-52337 Rinse water bottle 1 1 1
S072-60310-03 Wiring band, TM-53M 2 2 2
S631-51869-20 Name plate, SAMPLE 1 1 1
S631-51869-21 Name plate, GAS 1 1 1
S072-60301 Wiring band, Nylon TY-23M 1 1 1
S638-74492 Connection cable 1 1 1
S638-41472-01 Water sampling needle 1 1 1
S638-26022 9 mL vial rack 1 - -
S638-26021 24 mL vial rack - 1 -
S638-26020 40 mL vial rack - - 1

Table 8.5 Standard Accessories List 3 (OCT-L 8-Port Sampler)

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)

*1 Flanged tubing in C and C2 sets have an inner diameter of 1.0 mm.


*2 Connect this tubing to the common (COM) port of the OCT-L (1) and port 2 on the TOCL unit.
*3 Connect this tubing to the common (COM) port of the OCT-L (2) and port 1 on the TOCL unit.

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8.5 Special Accessories

8.5 Special Accessories


The optional accessories are listed in this section.

Table 8.6 Special Accessories List

Part Number Part Name Comment


S638-93199-58 Auto Sampler ASI-L Dedicated 24 mL vial model
S638-93200-58 Auto Sampler ASI-L Common 9 mL/40 mL vial model
S638-92327-58 ASI Accessories (9 mL)
S638-92325-58 ASI Accessories (24 mL)
S638-92326-58 ASI Accessories (40 mL)
S638-53044-06 9 mL vial rack set for ASI 9 mL vial rack + 9 mL vial set
24 mL vial rack + set of 24 mL vials,
S638-53044-04 24 mL vial rack set for ASI
caps and septums
40 mL vial rack + set of 40 mL vials,
S638-53044-05 40 mL vial rack set for ASI
caps and septums
S638-67099-41 Stirrer (for 24 mL vials) Autosampler for 24 mL vials
S638-67100-41 Stirrer (for 40 mL vials) Autosampler for 40 mL vials
1 stirring bar for 24 mL vials,
S046-00617-02 Stirring bar (for 24 mL vials) 1 is required for sample
measurement
1 stirring bar for 40 mL vials,
S046-00617-03 Stirring bar (for 40 mL vials) 1 is required for sample
measurement
S638-53096 9 mL ASI vial 100 pcs.
S638-41462 24 mL ASI vial 100 pcs.
72 pcs.
S038-00158-11 40 mL ASI vial
Includes caps and septums
S638-20074-01 Cap (for 24 mL vials) 100 pcs.
S038-00165-61 Septum (for 24 mL vials) 100 pcs.
S638-93201-58 8-Port sampler OCT-L (first unit)
8-Port sampler OCT-L
S638-93202-58 For expanding to a second unit
(second unit)
S638-91108-58 TN unit TNM-L For AC 100-127V
SSM-5000A Solid Sample
S638-93210-41 or -41: For AC 100~120 V
Module for Total Organic Carbon
S638-93210-58 -58: For AC 220~240 V
Analyzer 8
S638-56239-41 Cell switching valve set Option for SSM-5000A
Required when using TNM-L and
S638-56281-41 Changeover valve set, TN-SSM
SSM-5000A together.
POC measurement kit
S638-42101 "-01" is for N Type,
Required when using TNM-L and
-01,-02 "-02" is for H Type
SSM-5000A together.
S638-41447 Carrier gas purifier kit

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8 Reference Information

Part Number Part Name Comment


S638-77183-40 External sparge kit Only when using TOC-L
S638-77183-41 External sparge kit (with ASI-L) When using ASI-L Autosampler
S638-93149-03 Manual injection kit
Suspended solids kit (when used
S638-41586 Only when using TOC-L
with TOC-L alone)
Suspended Solids Kit (when ASIL is
S638-93151-04 When using ASI-L Autosampler
used)
Enables use of high purify nitrogen
gas with less than 1 ppm each of
CO, CO2 and HC as carrier gas.
S638-42054-02 Nitrogen currier gas kit
TN measurement cannot be
performed when using this kit with
the TNM-L.
S638-52572-03 B-type halogen scrubber
S638-59328 Small syringe kit
S638-93176 Combustion tube kit for high salt "-01" is for N Type,
-01,-02 samples "-02" is for H Type
"-41" is for TC, and "-42" is for IC.
S638-42167 High Suspension Kit for High
When using the H-type, TC and IC
-41,-42 Concentrations
require one kit each (i.e. two kits).
"-43" is for TC, and "-44" is for IC.
S638-42167 High Suspension Kit for Low
When using the H-type, TC and IC
-43,-44 Concentrations
require one kit each (i.e. two kits).
S630-08585-05 Cylinder pressure regulator User can provide this item.
Air supply tubing set (with 20
S638-41204 User can provide this item.
meters of tubing)
S638-52344 Drain bottle (for ASI)
Use this regulator when the
pressure from the carrier gas supply
S638-56255-41 Carrier gas regulator
source cannot be stably maintained
at 200 ± 10 kPa.
LabSolutions DB TOC installation LabSolutions TOC and LabSolutions
S638-64172-91
disc DB Manager 2-disc set
Required when connecting to
LabSolutions CS TOC installation LabSolutions CS.
S638-64173-91
disc LabSolutions TOC and LabSolutions
CS Manager 2-disc set
S638-64165-94 TOC control license (DB) 10-year (3650 days) license
S638-64165-91 TOC control license (CS) 10-year (3650 days) license
1-year extended license for TOC
S638-64165-95 1-year (365 days) license
(DB)
1-year extended license for TOC
S638-64165-92 1-year (365 days) license
(CS)

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8.6 Consumable Parts List

8.6 Consumable Parts List


The consumable parts are listed in this section.

8.6.1 Consumable Parts List

Table 8.7 Consumable Parts List 1 (TOC-LCPH)

Part Number Part Name Comment


S638-41323 Combustion tube, in case
S638-60246 TOC regular catalyst
S630-00105-01 Platinum mesh To support catalyst, 2 included
S630-00557 Quartz wool To support catalyst, 1 g
S630-00996 TOC high sensitivity catalyst
A set of TC high sensitivity catalyst
and combustion tube, where the
S638-92380-41 TC high sensitivity catalyst kit
tube is filled with TC high
sensitivity catalyst in advance
S630-00999 CO2 absorber

S630-00992 Halogen scrubber


S036-11209-84 O-ring, 4D P 10A For slider, 5 pcs.
S638-15025 O-ring, PTFE For slider, 1 pc.
S036-11222-84 O-ring, 4D P22 For IC reaction tube, 5 pcs.
S036-11219-84 O-ring, 4D P20 For TC reaction tube, 5 pcs.
IC reaction solution supply pump
S638-59390-41
head
S046-00042-12 Membrane filter
S638-56251-01 8-port valve rotor Type name: Plug, XT24-197-1-4
S638-59296-01 Plunger tip
Refer to "Table 8.9 TOC-LCPH, CPN
S638-92464-04 TOC-LCPH consumable parts set Consumable Parts Set Breakdown"
for an itemized list

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8 Reference Information

Table 8.8 Consumable Parts List 2 (TOC-LCPN)

Part Number Part Name Comment


S638-41323 Combustion tube, in case
S638-60246 TOC regular catalyst
S630-00105-01 Platinum mesh To support catalyst, 2 included
S630-00557 Quartz wool To support catalyst, 1 g
S630-00999 CO2 absorber Contains 500 mL
S630-00992 Halogen scrubber
S036-11209-84 O-ring, 4D P 10A For slider, 5 pcs.
S638-15025 O-ring, PTFE For slider, 1 pc.
S036-11219-84 O-ring, 4D P20 For TC reaction tube, 5 pcs.
S046-00042-12 Membrane filter
S638-56251-01 8-port valve rotor
S638-59296-01 Plunger tip
Refer to "Table 8.9 TOC-LCPH, CPN
S638-92464-05 TOC-LCPN consumable parts set Consumable Parts Set Breakdown"
for contents

Table 8.9 TOC-LCPH, CPN Consumable Parts Set Breakdown

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 8.10 Consumable Parts List 3 (ASI-L Autosampler)

Part Number Part Name Comment


S038-00158-11 40 mL vial set 40 mL, 72 vials, septa and caps
S638-41462 24 mL vial 24 mL, 100 pcs.
S638-53096 9 mL vial 9 mL, 100 pcs.
S638-43034-42 Septum 24 mL, 100 pcs.
S638-43034-41 Septum 40 mL, 100 pcs.
S638-20074-01 Cap 24 mL, 100 pcs.
S038-00165-40 Cap 40 mL, 200 pcs.

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8.6 Consumable Parts List

Part Number Part Name Comment


S638-59390-41 Rinse pump head

Table 8.11 Consumable Parts List 4 (8-Port Sampler OCT-L)

Part Number Part Name Comment


S638-56251-01 8-Port valve rotor

Table 8.12 Consumable Parts List 5 (TNM-L TN Unit)

Part Number Part Name Comment


S638-65232 Ozone treatment - catalyst 300 g included
S638-60074 Ceramic fiber
S638-42127 Ozone exhaust tubing

Table 8.13 Consumable Parts List 6 (Carrier Gas Purifier Kit)

Part Number Part Name Comment


S630-00556 CO2 absorber, absorbent 500 g included
S638-60246 TOC regular catalyst

Table 8.14 Consumable Parts List 7 (B-Type Halogen Scrubber)

Part Number Part Name Comment


S631-60069 Stainless mesh for absorption

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8 Reference Information

8.6.2 Recommended Consumable Part Replacement Period

"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.

Table 8.15 Recommended Consumable Part Replacement Period

Part Number Part Name Comment


S638-41323 Combustion tube (case included) 6 months
S638-60246 TOC standard catalyst 6 months
S630-00557 Quartz wool 1 year
S630-00999 CO2 absorber 1 year
S630-00992 Halogen scrubber 6 months
S638-15025 O-ring, PTFE (1 pc.) 1 year
S036-11209-84 O-ring, 4D P10 A (5 pcs.) 1 year
S036-11219-84 O-ring, 4D P20 (5 pcs.) 6 months
S638-56251-01 8-port valve rotor 1 year
S638-59296-01 Plunger tip 6 months

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8.7 Maintenance Parts List

8.7 Maintenance Parts List


The maintenance parts are listed in this section.

Table 8.16 Maintenance Parts List 1 (TOC-LCPH/CPN)

Part Number Part Name Comment


S638-56251 8-port valve
S638-59296 Syringe
For port number 1 on the 8-port
S638-42119-01 Tube 1
valve
For port number 2 on the 8-port
S638-42029-07 Tube set (sampling)
valve (for ASI connection)
For port number 3 on the 8-port
S638-42119-03 Tube 3
valve
For port number 4 on the 8-port
S638-42119-04 Tube 4
valve
For port number 5 on the 8-port
S638-42119-05 Tube 5
valve
For port number 6 on the 8-port
S638-42119-06 Tube 6
valve
For port number 7 on the 8-port
S638-42119-07 Tube 7
valve
For port number 8 on the 8-port
S638-42119-08 Tube 8
valve

Table 8.17 Maintenance Parts List 2 (ASI-L Autosampler)

Part Number Part Name Comment


The sparging needle is identical to
S638-41472-01 Water sampling needle
this part.
For use with 24 mL and 40 mL vials
S638-41450-01 Needle for suspended solids kit and the suspended solids kit,
0.8 mm, 1 included
1 tube, retainer, and tube seal for
S638-42029-07 Tube set
both sampling and sparging
1 sampling tube for the suspended
Tube set (sampling for the
S638-42029-04 solids kit, with retainer and tube
suspended solids kit)
seal
S638-67095-41 Motor (for 24 mL vials) For stirrer 24 mL vials
S638-67095-42 Motor (for 40 mL vials) For stirrer 40 mL vials
8
S638-67099-41 Stirrer (for 24 mL vials) For autosampler 24 mL vials
S638-67100-41 Stirrer (for 40 mL vials) For autosampler 40 mL vials

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8 Reference Information

Table 8.18 Maintenance Parts List 3 (OCT-L 8-Port Sampler)

Part Number Part Name Comment


S638-56251-01 8-port valve rotor Spare rotor
S638-42119-01 Water sampling tubing Water sampling tubing for TOC-L
S638-42119-21 OCT connection tubing TOC-L to OCT-L connection tubing

Table 8.19 Maintenance Parts List 4 (Manual Injection Kit)

Part Number Part Name Comment


Open / Close valve, TC injection
S630-02621
port
S638-60733-01 Microsyringe, MANU10 10 µL
S638-60733-02 Microsyringe, MANU25 25 µL
S638-60733-03 Microsyringe, MANU50 50 µL
S638-60733-04 Microsyringe, MANU100 100 µL
S638-60733-05 Microsyringe, MANU250 250 µL
S638-60733-06 Microsyringe, MANU500 500 µL

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8.8 Installation

8.8 Installation
The installation site requirements and installation procedures for future relocation of the
instrument are described here.

8.8.1 Before Installation

Parts Inspection
Confirm that all of the components listed in "8.4 Standard Accessories" P.401 have been
included in the shipping package.

8.8.2 Installation Site

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.

n Installation Site Selection

The instrument is designed for use on a desk or bench.


The external dimensions of the instrument are shown in "Figure 8.3 External Dimensions
of Instrument with ASI-L". A space of at least 200 mm is required on either side of and
behind the instrument to enable unhindered operation and maintenance. In order to
prevent any interference during operation, be aware that the main power switch of the
TOC instrument is located on the right side of the main unit and the power switch of
the ASI-L is located on the left side of the device.

Figure 8.3 External Dimensions of Instrument with ASI-L

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8 Reference Information

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.

n Installation Site Conditions

The ambient temperature specification for this instrument is 5 to 35 °C (10 to 35 °C for


the OCT-L). Install the instrument in an environment that can maintain this temperature
range in order to obtain stable measurement results.
Prevent condensation from occurring due to changes in ambient temperature and
humidity.

Select an installation site with the following conditions:


• A clean environment free of corrosive gases, organic gases, and dusts.

Contamination in the atmosphere will cause analysis errors, especially for high
sensitivity analyses.

• A strong, level bench, free of vibration and shock.


• An indoor location with a stable ambient temperature.
• A location with access to a completely grounded, stable power supply.
• Installation category: II
• Pollution degree: 2
• Altitude: up to 2000 m

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8.8 Installation

Avoid locations where flames are prohibited. Some internal parts reach high
temperatures and could cause a fire hazard.

Avoid the following kinds of locations:


• Locations close to heat sources, windows in direct sunlight, or in direct contact with
drafts from air conditioning vents.
• Near equipment that generates intense magnetic fields, electrical fields, or high
frequency waves.

8.8.3 Installation Procedure

n Connecting Power Supply and Ground

Connecting Power Supply


Connect the instrument to a stable, AC 100-127V (100V System) or AC 220-240V (200V
System), 50 Hz or 60 Hz (single phase) power supply with sufficient capacity to
accommodate 600 VA or greater current.

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.

The instrument is compatible with both 50 Hz and 60 Hz power supplies and


can be used with either frequency.
And, use the power code that meet the following condition.
* Power supply of each country
* Standard of each country
* Power supply inlet of TOC-L(standard : IEC-60320-C14)
* Power supply specifications of TOC-L

For position on the power supply inlet, refer to "2.1.4 Rear View" P.8.

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8 Reference Information

Grounding
The power cord is a three-conductor cable including a ground wire.
Be sure to completely ground the ground wire of the cable.

• In addition to the consideration of safety, complete grounding of the


instrument is very important and necessary in order to prevent malfunctions
due to the interference of signal noise in the instrument's electrical circuitry.
A Type-3
ground (ground resistance: 100 Ω or less) is recommended.
• Perform grounding separately and avoid contact with water supply pipes, gas
pipes, and lightning rods.

n Changing the Power Supply Voltage

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)

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8.8 Installation

High Purity Air Cylinders


High purity air is synthetic air manufactured from pure nitrogen and pure oxygen. It
must be guaranteed to contain less than one 1 ppm of each of the following impurities:
carbon dioxide, carbon monoxide, and hydrocarbons.
The cylinder must be equipped with a pressure regulator to supply it at 200 ± 10 kPa
to the gas connection inlet of the instrument.

If the carrier gas contains excessive impurities, analysis accuracy is diminished and
good results will not be obtained.

Precautions for Handling Gas Cylinders


The handling and safety management of high-pressure gases is strictly
regulated by high-pressure gas control laws, general high-pressure gas safety
codes, and fire laws.
The gas used in the instrument is not dangerous, but mistakes in handling of
high-pressure gas cylinders can be extremely hazardous. Carefully read and
obey the following precautions.
• Place gas cylinders in a well-ventilated location out of direct sunlight.
• Ensure that gas cylinders never reach temperatures higher than 40 °C.

• 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.

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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.

Gas Supply Pressure


Ensure that the gas supplied to the gas inlet of the instrument maintains a constant,
stable pressure of 200 ± 10 kPa.
Use the optional carrier gas regulator if pressure cannot be stably supplied at 200 ± 10
kPa. In this case, set the carrier gas supply pressure to 300 ± 10 kPa.

Never allow the carrier gas supply pressure to exceed 600 kPa when using the
optional carrier gas regulator.

Gas Tubing Connections


The special accessory Air Supply Tubing Set includes nylon tubing and connectors (two
[2] half unions).

Procedure

Figure 8.6 Gas Tubing Connection

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8.8 Installation

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.

3 Verify that there are no gas leaks.

• Do not allow acute bends in the tubing.


• Clean the tubing and connectors to remove any oils or other contaminants
on their inner surfaces.
• Copper tubing or stainless steel tubing may also be used.
• Always keep the 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.

n Installing the Drain Container

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.

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Figure 8.7 How to Lead the Drain Tubing from the Instrument to the Drain Container

• Drain discharge contains acids and other corrosive substances so always


handle it with care to prevent spills and contact with the skin.
• Depending on measurement conditions, drain discharge may have a pH level
less than 2.0. Drain discharge with a pH less than 2.0 is classed as industrial
waste subject to special control. Request transfer by an authorized industrial
waste transporter to an authorized industrial waste processing facility to
process any industrial waste subject to special control. If you wish to perform
deacidification on your own premises, contact the environmental agency in
your jurisdiction.

n Connecting to the PC Using the Provided Cable

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.

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8.8 Installation

8.8.4 Installing the ASI-L

This section describes procedures for installing the ASI-L autosampler.

Positioning the ASI-L


Place the autosampler about 100 mm to the left of the TOC-L, as shown in "Figure 8.8
Installing the ASI-L".

Figure 8.8 Installing the ASI-L

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.

Removing the Shipping Screw


The ASI-L arm is secured with a shipping screw to prevent damage during shipment.
Before connecting power to the instrument, remove the ASI-L cover to access the shipping
screw, which is located on the retaining bracket. Remove the shipping screw and replace
the cover. Label the shipping screw and store it for future use.

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.

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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.

Figure 8.9 Connecting the Cables (TOC-L to ASI-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.

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8.8 Installation

2 If using the external sparge kit, attach the sparging tubing for ASI-L.

Figure 8.10 Attaching 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.

Installing the Needle


The water sampling needle and sparging needle (for use with the external sparge kit)
are of the same type. Insert the sparging needle into the opening on the right side of
the needle holder.

Verify that the TOC-L is switched OFF before performing the following
procedure.

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Installing the Water Sampling Needle and Sparging Needle

1 Open the needle cover door towards the left.

2 Remove the needle holder retaining screw and then remove the needle holder
from the arm.

Figure 8.11 Inside the Needle Cover

3 Insert the needle into the opening in the needle holder.

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.

Figure 8.12 Installing the Needle

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8.8 Installation

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.

8 Close the needle cover door.

Installing the Turntable, Vial Rack and Cover

Installing the Turntable

1 Place the turntable on the ASI-L.

There is no distinction between front and rear of the turntable, so placement


orientation is irrelevant.

2 Place the turntable so that the 3 guides on the ASI-L pass through the 3 holes
at the center of the turntable.

Figure 8.13 Installing the Turntable

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Installing the Vial Rack

1 Place the vial rack on top 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

Installing the Cover

1 Place the cover on the ASI-L.

There is a magnet at the left rear of the cover. Verify that the cover and ASI-L
are in contact at the magnet.

Installing the Rinse Bottle and Drain Container


This section describes how to install the rinse bottle and drain container.
The rinse tubing and drain tubing are attached to the ASI-L and each bear the name
tag "RINSE" and "DRAIN" respectively. The drain tubing should be cut to a suitable
length whereas the rinse tubing can be used without modification.

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.

Before Starting Analysis


Check the following before starting analysis.
• The rinse water bottle is filled to above the 2 L mark.
• The tip of the rinse tubing reaches nearly to the bottom of the rinse water 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.

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8.8 Installation

8.8.5 OCT-L Installation

The OCT-L is installed as described below.

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)".

Figure 8.14 Installation of the OCT-L

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.

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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.

Figure 8.15 Cable Connections (TOC-L and OCT-L)

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8.8 Installation

Installing Two OCT-L Units


When installing two OCT-L units, a signal cable (standard accessory) is connected between
OCT-L (1) and OCT-L (2).

Installation Procedure

1 Remove the covers from both OCT-L units.

2 Connect the signal cable exiting OCT-L (2) to the connector of OCT-L (1).

Figure 8.16 Connecting Two OCT-L Units

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.

4 Replace the covers on both of the OCT-L units.

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Connecting the Water Sampling Tubing


Connect the water sampling tubing according to the procedure described below.

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)).

Figure 8.17 COM Port and Water Sampling Tubing Connections

Connection to the TOC-L Main Unit


• OCT-L (1)
Connect the COM tubing to the common (COM) port of OCT-L (1) and port
No. 2 on the TOC-L unit.
• OCT-L (2)
Connect the COM tubing to the common (COM) port of OCT-L (2) and port
No. 1 on the TOC-L unit

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8.8 Installation

8.8.6 Installing the TNM-L

n TNM-L TN Unit Installation

A technician from Shimadzu or designated by Shimadzu will install this unit.

n Connecting Ozone Source Air

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 Compressor Air or Instrumentation Air


When using compressor air or instrumentation air for generation of ozone, be sure that
the following conditions are satisfied.
• Install an air filter in the air supply line to eliminate dust, oil mist and water droplets
from the air. If a compressor is used, install the air filter (equipped with drain
separation and discharge branch) close to the tubing connection at the instrument.
• If a compressor is used, select an oil-less type air compressor. Shimadzu offers the
SLP5D-2SV oilless and silent air compressor (P/N 042-70041-02) and AW30-02BG-N filter
regulator (P/N 040-82118-23) as options.

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.

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8 Reference Information

Precautions in Handling Gas Cylinders


The handling and safety management of high-pressure gases is strictly
regulated by high-pressure gas control laws, general high-pressure gas safety
codes, and fire laws.
The gas used in this instrument itself is not dangerous, but mistakes in the
handling of high-pressure gas cylinders can be extremely hazardous. Carefully
read and obey the following precautions.
• Place gas cylinders in a well-ventilated location out of direct sunlight.
• Ensure that gas cylinders never reach temperatures higher than 40 °C.

• 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.

Gas Supply Pressure


Supply gas at a constant, stable pressure of 300 to 600 kPa (87 PSI) at the gas inlet
connection of the TNM-L.

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.

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8.8 Installation

Gas Tubing Connections


The special accessory Air Supply Tubing Set includes nylon tubing and connectors (two
(2) half unions).

Figure 8.18 Gas Tubing Connection

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.

3 After connection, check to see that there are no gas leaks.

• Do not allow any acute bends in the tubing.


• When tubing and connectors are prepared by the user, be sure to use clean
components that are free of oils or other contaminants on their inner
surfaces.
• Copper tubing or stainless steel tubing may also be used.
8
Low Ozone Air Supply Pressure Safety Mechanism
As a safety measure, the TNM-L is equipped with an ozone air gas pressure sensor that
will automatically switch off the ozone generator if the ozone air gas pressure decreases
below the prescribed level. If an error message is displayed indicating this problem,
perform an inspection of the ozone air gas supply.

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Connecting Gas Exhaust Tubing


Because the unit uses a chemiluminescence system for the detection of TN components,
it is equipped with an internal ozone generator. The ozone and NOx generated are
removed by the ozone treatment unit and NOx absorber, and are then exhausted.
However, in the event that the performance of the ozone treatment catalyst and NOx
absorber deteriorate, ozone and NOx gas may be expelled in the exhaust gas. Be sure
to discharge exhaust gas to the outdoors or to an exhaust pit using a 5 mm I.D. flexible
vinyl hose.

• 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.

Expose the exhaust gas tubing to atmospheric pressure to reduce resistance.

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8.9 Safety Data Sheets (SDS)

8.9 Safety Data Sheets (SDS)


Material Safety Data Sheets are included for hydrochloric acid, phosphoric acid, IC regent,
the CO2 absorber, ceramic fiber and catalyst platinum black.

8.9.1 Hydrochloric Acid (HCl)

PRODUCT NAME Hydrochloric Acid


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
Skin corrosion/irritation :Category 1A
Serious eye damage/eye
:Category 1
irritation
Acute toxicity-Oral :Category 4
Acute toxicity-Inhalation :Category 1
GHS Sensitization-Respiratory :Category 1
CLASSIFICATION
Specific target organ systemic
:Category 1
toxicity Single exposure
Specific target organ systemic
:Category 1
toxicity Repeated exposure
Hazardous to the aquatic
:Category 1
environment -Acute hazard
SECTION II
HAZARDS
IDENTIFICATION HAZARD SYMBOL DANGER

Causes severe skin burns and eye damage


Causes serious eye damage
Harmful if swallowed 8
Fatal if inhaled
HAZARD May cause allergy or asthma symptoms or
STATEMENTS breathing difficulties if inhaled.
Causes damage to organs
Causes damage to organs through prolonged
or repeated exposure
Very toxic to aquatic life

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8 Reference Information

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.

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8.9 Safety Data Sheets (SDS)

Store container tightly closed in well-ventilated


place -if product is as volatile as to generate
<Storage> hazardous atmosphere.
 SECTION II
HAZARDS   Store locked up.
IDENTIFICATION
Dispose of contents/container to a located
<Disposal> point (in accordance with
local/regional/national/international regulation).
CHEMILCAL
Hydrochloric acid (36 %)
IDENTITY
SYNONYMS Muriatic acid
FORMULA HCl
SECTION III
COMPOSITION/ MOLECULAR
36.46
INFORMATION ON WEIGHT
INGREDIENTS CAS NUMBER 7647-01-0
TSCA INVENTORY Listed
EINECS No. 231-595-7
EC INDEX NUMBER 017-002-00-2
Wash off immediately with soap and plenty of
water. In the case of respirable dust and/or
GENERAL ADVICE fumes, use self-contained 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. Never give anything by mouth to an
INGESTION
unconscious person.
Transport to a hospital immediately. 8

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8 Reference Information

EXTINGUISHING Carbon dioxide, dry chemical powder, foam,


MEDIA water
Toxic and irritating fumes or smoke may be
FIRE & EXPLOSION
SECTION V emitted. Explosive hydrogen gas is released
HAZARDS
FIRE FIGHTING upon contact with common metals.
MEASURES
SPECIAL Firemen should wear normal protective
PROTECTIVE equipment (full bunker gear) and
EQUIPMENT FOR positive-pressure self-contained breathing
FIREFIGHTERS apparatus.
Remove ignition sources and ventilate the
PERSONAL area. In case of insufficient ventilation, wear
PRECAUTIONS suitable respiratory equipment.
Avoid contact with skin and eyes.
ENVIRONMENTAL Prevent spills from entering sewers,
PRECAUTIONS watercourses or low areas.
Do not touch spilled material without suitable
SECTION VI
protection (See section 8). Take up spilled
ACCIDENTAL RELEASE
material with ashes or other incombustible
MEASURES
absorbents and dilute it with plenty of water
and neutralize with soda ash.
METHODS FOR
After material is completely picked up, wash
CLEANING UP
the spill site with soap and water and ventilate
the area. Put all wastes in a plastic bag for
disposal and seal it tightly.
Remove, clean, or dispose of contaminated
clothing.
Avoid contact with eyes, skin and clothing.
PRECAUTION FOR
Avoid prolonged or repeated exposure.
SAFE HANDLING
Handle material with suitable protection.
SECTION VII
HANDLING AND Store away from sunlight in well-ventilated dry
CONDITIONS FOR
STORAGE place at room temperature.
SAFE STORAGE
Keep container tightly closed.
INCOMPATIBILITIES Strong oxidizers, alkalis, amines, metals
Use exhaust ventilation to keep airborne
ENGINEERING
concentrations below exposure limits.
MEASURES
Use only with adequate ventilation.
Local Exhaust ; Necessary, Mechanical
VENTILATION (General) ; Necessary
Special; Closed system is recommended.
INDIVIDUAL PROTECTION MEASURES

SECTION VIII Respiratory NIOSH/MSHA or European Standard EN149


EXPOSURE protection approved respirator
CONTROLS/PERSONAL
  Hand protection Impervious gloves
PROTECTION
Eye protection Safety glasses (goggles)
Skin protection Protective clothing
CONTROL
as Hydrogen chloride
PARAMETER
OSHA Final
Ceiling = 5 ppm, 7 mg/m3; STEL = 2 ppm
  Limits
ACGIH TLV(s) Ceiling = 5 ppm, 7.5 mg/m3

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8.9 Safety Data Sheets (SDS)

APPEARANCE Colorless clear liquid


ODOUR Irritating odor
pH Not available
FREEZING POINT -46.2 °C = -51.2 °F (31.24 %)
INITIAL BOILING
108.58 °C = 227.44 °F
POINT
FLASH POINT Not available
FLAMMABILITY
-
(solid, gas)
SECTION IX EXPLOSIVE LIMITS Not available
PHYSICAL AND
CHEMICAL VAPOR PRESSURE Not available
PROPERTIES VAPOR DENSITY 1.3 (air = 1)
RELATIVE DENSITY 1.180 (35.39 %)
SOLUBILITY IN
WATER Miscible
  ETHANOL, ETHL
Miscible
ETHER
PARTITION
0.25
COEFFICIENT
DECOMPOSITION
Not available
TEMPERATURE
CHEMICAL
Will not occur.
STABILITY
CONDITIONS TO
Sunlight, heat
SECTION X AVOID
STABILITY AND INCOMPATIBILE
REACTIVITY Strong oxidizers, alkalis, amines, metals
MATERIALS
HAZARDOUS
DECOMPOSITION Hydrogen chloride gas may be formed.
PRODUCTS

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8 Reference Information

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

438 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

Cautiously add to a large stirred excess of water. Adjusting the pH


SECTION XIII to neutral, separate any insoluble solids or liquids and package them
DISPOSAL for hazardous-waste disposal.
CONSIDERATION Flush the aqueous solutions down the drain with plenty of water.
(INCLUDING Any disposal practice must be in compliance with country, local,
CONTAINER) state, and federal laws and regulations (contact country, local or
state environmental agency for specific rules).
IATA
UN NUMBER UN1789
UN PROPER
Hydrochloric acid
SHIPPING NAME
CLASS or
  Corrosives. (Class 8)
DIVISION

SECTION XIV PACKING GROUP PG II


TRANSPORT MARINE
INFORMATION Yes
POLLUTANT
DOT (Department of Transportation)
IDENTIFICATION
UN1789
NUMBER
  PROPER
Hydrochloric acid
SHIPPING NAME
HAZARD CLASS Corrosive material (Class 8)
CAA/112 1990 Amend., CAA/122(r) Acci.
Release Pre. Subst., CERCLA Haz. Subst., DOT
US REGULATIONS ; Haz. Mat., DOT Haz. Sub.
and Rep. Quant., Mass. Subst. List , New Jers.
RTK Haz. Subst. List , Penn. Haz. Subst. List
SECTION XV
REGULATORY CERCLA RQ= 5000 lb
INFORMATION
EPCRA TPQ= Not listed
EPA
  EPA FIFRA 1998 STATUS OF PESTICIDES: Red
Completed
OSHA TQ= Not listed
SECTION XVI
OTHER
INFORMATION
INCLUDING No specific notes
INFORMATION ON
PREPARATION AND
REVISION OF THE SDS
 
8
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.

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8 Reference Information

8.9.2 Phosphoric Acid

PRODUCT NAME Phosphoric Acid


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
Skin corrosion/irritation :Category 1A
Serious eye damage/eye
:Category 1
irritation
Acute toxicity-Oral :Category 4
GHS
Acute toxicity-Dermal :Category 5
CLASSIFICATION
:Category 3
Specific target organ systemic <the
toxicity respiratory
Single exposure tract
irritation>
SECTION II
HAZARDS
IDENTIFICATION
HAZARD SYMBOL DANGER

Causes severe skin burns and eye damage


Causes serious eye damage
Harmful if swallowed
HAZARD
STATEMENTS May be harmful in contact with skin
May cause respiratory irritation; or May cause
drowsiness and dizziness <the respiratory tract
irritation>

440 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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

SECTION III FORMULA H3PO4


COMPOSITION/ MOLECULAR
INFORMATION ON 98.00
WEIGHT
INGREDIENTS
CAS NUMBER 7664-38-2
TSCA INVENTORY Listed
EINECS No. 231-633-2
EC INDEX NUMBER 015-011-00-6

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8 Reference Information

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
INHALATION difficult, give oxygen. If irritation persists,
consult a physician.
Remove contaminated clothes and shoes, rinse
skin with plenty of water or shower. Use soap
SKIN CONTACT to help assure removal.
SECTION IV
If irritation persists, transport to a hospital
FIRST AID MEASURES
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. Never give anything by mouth to an
INGESTION
unconscious person.
Transport to a hospital immediately.
EXTINGUISHING Carbon dioxide, dry chemical powder, foam,
MEDIA water
Toxic, irritating fumes or smoke may be
FIRE & EXPLOSION
SECTION V emitted. Explosive hydrogen gas is released
HAZARDS
FIRE FIGHTING upon contact with common metals.
MEASURES
SPECIAL Firemen should wear normal protective
PROTECTIVE equipment (full bunker gear) and
EQUIPMENT FOR positive-pressure self-contained breathing
FIREFIGHTERS apparatus.
Remove ignition sources and ventilate the
PERSONAL area. In case of insufficient ventilation, wear
PRECAUTIONS suitable respiratory equipment.
Avoid contact with skin and eyes.
ENVIRONMENTAL Prevent spills from entering sewers,
PRECAUTIONS watercourses or low areas.
Do not touch spilled material without suitable
SECTION VI
protection (See section 8). Take up spilled
ACCIDENTAL RELEASE
material with ashes or other incombustible
MEASURES
absorbents and dilute it with plenty of water
and neutralize with soda ash. After material is
METHODS FOR
completely picked up, wash the spill site with
CLEANING UP
soap and water and ventilate the area.
Put all wastes in a plastic bag for disposal and
seal it tightly.
Remove, clean, or dispose of contaminated
clothing.

442 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

Avoid contact with eyes, skin and clothing.


PRECAUTION FOR Avoid prolonged or repeated exposure.
SAFE HANDLING Handle material with suitable protection.
SECTION VII This material is hygroscopic.
HANDLING AND
Store away from sunlight in well-ventilated dry
STORAGE CONDITIONS FOR
place at room temperature. Keep container
SAFE STORAGE
tightly closed.
INCOMPATIBILITIES Oxidizers, alkalis, metals
Use exhaust ventilation to keep airborne
ENGINEERING
concentrations below exposure limits. Use only
MEASURES
with adequate ventilation.
Local Exhaust ; Necessary, Mechanical
VENTILATION (General) ; Necessary
Special; Closed system is recommended.
INDIVIDUAL PROTECTION MEASURES ;
SECTION VIII
EXPOSURE Respiratory Use a NIOSH/MSHA or European Standard
CONTROLS/ protection EN149 approved respirator
PERSONAL Hand protection Impervious gloves
PROTECTION
Eye protection Safety glasses (goggles)
Skin protection Protective clothing
CONTROL PARAMETER
OSHA Final
TWA = 1 mg/m3
Limits
ACGIH TLV(s) TWA = 1 mg/m3; STEL = 3 mg/m3
APPEARANCE Colourless clear liquid
ODOUR Odourless
pH Not available
MELTING POINT Not available
INITIAL BOILING
213 °C = 415 °F
POINT
FLASH POINT Not available
FLAMMABILITY
-
(solid, gas)
SECTION IX
PHYSICAL AND EXPLOSIVE LIMITS Not available
CHEMICAL VAPOR PRESSURE 4.0 Pa (at 20 °C = 68 °F)
PROPERTIES
VAPOR DENSITY 3.4 (Air = 1)
SPECIFIC GRAVITY 1.685
8
SOLUBILITY IN ;
WATER Freely soluble (670 g/100 mL at 25 °C = 77 °F)

ETHANOL Freely soluble


PARTITION
Not available
COEFFICIENT
DECOMPOSITION
Not available
TEMPERATURE

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8 Reference Information

May occur. Violent polymerization can occur


CHEMICAL
with epoxides, azo compounds, and
STABILITY
polymerizable compounds.
CONDITIONS TO
SECTION X Sunlight, heat, moisture
AVOID
STABILITY AND
REACTIVITY INCOMPATIBILE
Oxidizers, alkalis, metals
MATERIALS
HAZARDOUS
DECOMPOSITION Phosphorous oxide may be formed.
PRODUCTS
ACUTE TOXICITY (oral/dermal/inhalation)
LD50 (orl, rat) 1.25 gm/kg (RTECS)
LD50 (orl,
1.25 gm/kg (RTECS)
mouse)
LC50 (ihl, rat) 25.5 mg/m3 (RTECS)
LD50 (orl, rat) 1530 mg/kg (IUCLID, 2000) (HSDB, 2006)
LD50 (skin,
2740 mg/kg (IUCLID, 2000) (HSDB, 2006)
rabbit)
SKIN CORROSION/IRRITATION
Skin; rabbit; 595 mg/24H; Severe (RTECS)
Skin; rabbit; 75-85 %/24H; Irritation (IUCLID, 2000)
EYE DAMAGE/EYE
Eye; rabbit; 119 mg; Severe (RTECS)
IRRITATION
RESPIRATORY OR
Not available
SKIN SENSITIZATION
SECTION XI GERM CELL
Not available
TOXICOLOGICAL MUTAGENICITY
INFORMATION
TOXIC TO
Not available
REPRODUCTION
STOST-SINGLE Human; mist, irritation of the upper respiratory
EXPOSURE tract (ACGIH 7th, 2001)
STOST-REPEATED
Not available
EXPOSURE
ASPIRATION
Not available
TOXICITY
CARCINOGENICITY Not available
ADDITIONAL INFORMATION ;
NTP Not listed
IARC Not listed
OSHA Not listed
ACGIH Not listed
EPA GENETOX PROGRAM 1988, Negative: Cell
transform.-SA7/SHE

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8.9 Safety Data Sheets (SDS)

ECOTOXICITY Not available


PERSISTENCE AND
Not available
DEGRADABILITY
SECTION XII
BIOACCUMULATIO
ECOLOGICAL Not available
N POTENTIAL
INFORMATION
MOBILITY IN SOIL Not available
OTHER ADVERSE
WGK;1
EFFECTS
Cautiously add to a large stirred excess of water. Adjusting the pH
to neutral, separate any insoluble solids or liquids and package them
for hazardous-waste disposal. Flush the aqueous solutions down the
SECTION XIII
drain with plenty of water.
DISPOSAL
Any disposal practice must be in compliance with country, local,
CONSIDERATION
state, and federal laws and regulations (contact country, local or
(INCLUDING
state environmental agency for specific rules).
CONTAINER)
After contents are completely removed, dispose of its container at
hazadous or special waste collection point.
(in accordance with local/regional/ national/international regulation).
IATA
UN NUMBER UN1805
UN PROPER
Phosphoric acid
SHIPPING NAME
CLASS or
Corrosives. (Class 8)
DIVISION

SECTION XIV PACKING GROUP PG III


TRANSPORT MARINE
INFORMATION No
POLLUTANT
DOT (Department of Transportation)
IDENTIFICATION
UN1805
NUMBER
PROPER
Phosphoric acid
SHIPPING NAME
HAZARD CLASS Corrosive material (Class 8)

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8 Reference Information

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.

446 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

8.9.3 IC Reagent

PRODUCT NAME IC reagent


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
Single
SINGLE PRODUCT OR COMPOUND CLASSIFICATION
product
Phosphoric
CHEMICAL OR GENERIC NAME
acid
SECTION II
CONTENT Phosphoric acid, 25 % aqueous solution
COMPOSITION/
INFORMATION ON CHEMICAL PROPERTIES (CHEMICAL FORMULA) H3PO4
INGREDIENTS
OFFICIAL GAZETTE REFERENCE NUMBER (CSCL/ISHL) 1-422
CAS NO. 7664-38-2
HAZARDOUS
Phosphoric acid
COMPONENTS
PRIMARY
HAZARDOUS Corrosive to skin.
PROPERTY
Strongly acidic liquid that causes irritation and
inflammation to the eyes, skin, and mucous
membrane.
Contact with the eyes causes irritation and
may cause blindness.
HAZARDS
In a mist or vapor state, causes irritation to the
eyes, skin, mucous membrane, respiratory tract,
SECTION III
and lungs.
SUMMARY OF
Oral ingestion may cause nausea, vomiting,
HAZARDOUS
abdominal pain, and bloody diarrhea.
PROPERTIES
ENVIRONMENTAL Hazardous to aquatic organisms due to strong
IMPACT acidity.
Contact with alkaline substances generates
PHYSICAL AND heat.
8
CHEMICAL Reacts with many types of metals to produce
HAZARDS hydrogen gas that mixes with air to form a
flammable and explosive gas.
CLASSIFICATION
Corrosive substance
NAME

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8 Reference Information

Immediately move the affected person to a


location with fresh air. Calm them and cover
their body with a blanket or
similar material to keep them warm. Instruct
them to blow their nose and gargle their
INHALATION throat.
If breathing is difficult, give oxygen. If
breathing stops, loosen clothing, secure the
respiratory tract, and perform artificial
respiration. Transport to a hospital
immediately.
Remove contaminated clothes and shoes and
rinse the affected area of skin with plenty of
water. Do NOT neutralize using alkaline
solutions.
Do NOT apply any type of oil or ointment to
SKIN CONTACT
the affected area without specific instruction
SECTION IV
from a physician.
FIRST AID MEASURES
If the appearance of the skin changes or
irritation and pain persist, transport to a
hospital immediately.
Immediately flush the affected eye with clean,
running water for at least 15 minutes and
promptly consult an eye physician. Ensure
adequate rinsing by separating the eyelids
with sterile fingers and flushing the eyeball
and all parts of the eyelid with water.
Do NOT apply any type of oil or ointment
EYE CONTACT
without specific instruction from a physician.
Always perform first aid measures immediately
because a delay in eye flushing or insufficient
flushing may cause permanent damage to the
affected eye. Continue flushing the affected
eye if medical attention from a physician is
delayed.

448 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

Calm the affected person and cover their body


with a blanket or similar material to keep
them warm.
Reassure the affected person if conscious. Rinse
out their mouth and give milk or water
dispersed with magnesium oxide
in small amounts. If these measures cannot be
INGESTION taken immediately, give large amounts of
water.
SECTION IV NEVER induce vomiting as this may have the
FIRST AID MEASURES opposite effect of damaging the stomach wall
due to the corrosive nature of the material.
Never give anything by mouth to an
unconscious person. Transport to a hospital
immediately.
The person who provides first aid should wear
PROTECTION FOR
protective equipment including protective
THE GIVER OF
eyewear and protective gloves to avoid contact
FIRST AID
with the hazardous substance.
This product does not ignite on its own.
EXTINGUISHING Use a suitable extinguishing media for the
MEDIA other materials caused to ignite by this
product.
Prohibit unauthorized personnel from entering
the area where fire has broken out and direct
them to a safe location.
While this substance is noncombustible,
immediately transfer the container to a safe
SECTION V SPECIFIC
location if fire breaks out.
FIRE FIGHTING EXTINGUISHING
If the container cannot be transferred to
MEASURES METHOD
another location, cool the container and
immediate area by spraying water.
Take suitable measures to prevent the runoff
of substances when extinguishing the fire that
may adversely affect the environment.
The molecules that comprise this substance
contain phosphorus. Avoid inhaling any smoke
SPECIFIC HAZARDS
produced due to contact with
fire as it contains irritants, toxic fumes and gas.

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8 Reference Information

Always wear suitable protective equipment


due to the strong acidity of the liquid.
SECTION V Perform firefighting from an up wind position
PROTECTION FOR
FIRE FIGHTING as mush as possible. Wear protective
FIREFIGHTERS
MEASURES equipment that covers the eyes, nose,
and mouth to prevent exposure and inhalation
of smoke that contains toxic gas.
Cordon off the area of spilled material with
rope, sound an alarm or similar warning, and
prohibit unauthorized personnel from entering
the area.
Sufficiently ventilate the area and perform
cleanup work from an up wind position. Do
PERSONAL not perform any work down wind from the
PRECAUTIONS spilled material.
Always wear protective equipment (protective
eyewear, protective gloves, protective shoes,
protective clothing, and a gas mask for acidic
gases) during cleanup work due to the
strongly acidity and corrosive nature of the
substance.
Take measures to prevent the discharge of this
product into rivers that will adversely affect
the environment.
When this substance is diluted with large
ENVIRONMENTAL
amounts of water, do not allow the discharge
PRECAUTIONS
of contaminated water into the
environment without suitable treatment. Do
not discharge spilled material directly into
rivers or the sewage system.
SECTION VI CLEANUP METHOD
ACCIDENTAL RELEASE
Clear away any spilled material after soaking
MEASURES
it up with dry sand or earth. Alternatively,
dilute the spilled material with water,
SMALL SPILLS
neutralize it with lime hydrate or soda ash,
and then wash the material away with a large
amount of water.
Enclose the spilled material with earth fill to
prevent run off and allow absorption and then
collect the material in a sealable, empty
container. Alternatively, gradually dilute the
spilled material with water from a safe
location at a distance, neutralize the spilled
material with lime hydrate or soda ash, and
then wash the material away with a large
amount of water.
LARGE SPILLS Rapid contact with water during dilution or
the neutralizing agent generates heat and may
cause acid to splatter. For this reason, take
care when performing dilution and always be
careful when performing gradual
neutralization after dilution.
If gas is produced during neutralization, spray
the gas with water mist to absorb it.
Do not allow the discharge of concentrated
liquid into rivers.

450 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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.

TOC-LCPH/CPN LabSolutions TOC Volume 451


8 Reference Information

• Directly mixing neutralizing agent with this


material generates heat and bubbles and
may cause the material to splatter. Always
perform neutralization after dilution with
water.
• Always perform dilution with water carefully
as this can generate heat.
• Handle alkaline substances, cyanide
TECHNICAL compounds, and metal powder at removed
MEASURES locations.
• Always wash your hands and eyes and gargle
after handling this material. Always wash
any used protective equipment with water
and allow to dry. Change your clothing
immediately if it comes into contact with the
material.
Wash the contaminated clothing with water
and allow to dry.
If there is a risk that mist or vapor may be
generated, handle the material
PRECAUTIONS
within local ventilation or at a location with
general ventilation equipment.
Avoid contact with alkaline substances due to
the material's strongly acidity.
PRECAUTIONS As this liquid reacts with metals, select a
SECTION VII
FOR SAFE suitable material for handling.
HANDLING AND
HANDLING As this material will cause metals such as iron
STORAGE
to rust, relevant facilities
require anti-rust treatment.
STORAGE
• Store away from sunlight in a dry,
well-ventilated location at room temperature.
• Keep container tightly sealed.
• Construct the floor of the storage location
with acid resistant material to prevent any
spillages from penetrating underground.
CONDITIONS
FOR SAFE • Install drainage prevention facilities to
STORAGE prevent the material from flowing out of the
storage location.
• Do not store in underground rooms or
locations with sources of heat, such as
boilers.
• Store away from alkaline substances, cyanide
compounds, and metal powder.
Due to a strong corrosive reaction with metals,
SAFE
select a suitable material to handle this liquid.
CONTAINERS
Cast iron containers cannot be used.
AND
Resin-based materials such as polyethylene,
PACKAGING
PTFE, and FRP as well as glass are resistant to
MATERIAL
this liquid.

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8.9 Safety Data Sheets (SDS)

In handling locations that generate mist or


vapor, seal the generation source or use local
FACILITY ventilation equipment.
MEASURES Install facilities for emergency eye and body
washing near the area of handling and clearly
indicate the position of such facilities.
CONTROL
Not set.
CONCENTRATION
Japan Society for Occupational
1 mg/m3
Health

SECTION VIII ACCEPTABLE 3 mg/m3


ACGIH1mg/m3 (TLV-TWA)
EXPOSURE CONTROL CONCENTRATION (TLV-STEL)
AND PERSONAL *) TWA : Time-weighted average value,
PROTECTION STEL : Short-term exposure limit
PROTECTIVE EQUIPMENT
RESPIRATORY
Gas mask for acidic gases
PROTECTION
HAND Protective gloves (impervious and acid
PROTECTION resistant)
Protective eyewear (normal glasses with side
EYE PROTECTION
protection, goggles)
SKIN Protective clothing (long-sleeved work clothes),
PROTECTION protective shoes, apron
PHYSICAL PROPERTIES
SHAPE Viscous liquid
COLOR Clear and colorless
ODOR Odorless
SECTION IX pH Strongly acidic
PHYSICAL AND
FLASH POINT Nonflammable.
CHEMICAL
PROPERTIES DENSITY (SPECIFIC
1.15 g/cm3 (20 °C)
GRAVITY)
Freely mixes
SOLUBILITY WITH RESPECT TO with water.
SOLUBILITY
SOLVENT Soluble in
ethyl alcohol.

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8 Reference Information

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

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8.9 Safety Data Sheets (SDS)

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.

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8 Reference Information

Dilute with a large amount of water before


carefully neutralizing with an aqueous solution
of lime hydrate (calcium hydroxide) or soda
ash (sodium carbonate). Separate from any
generated precipitates and discharge the
supernatant liquid according to wastewater
standard restrictions.
RESIDUAL WASTE Rapid contact with water during dilution or
the neutralizing agent generates heat and may
cause acid to splatter. For this reason, take
care when performing dilution and always be
careful when performing gradual
SECTION XIII neutralization after dilution.
DISPOSAL Always wear protective equipment suitable to
CONSIDERATIONS the task at hand.
Protective eyewear or face shield, impervious
protective gloves, protective shoes, protective
Protective clothing (impervious, long-sleeved work
equipment clothes),
gas mask for acidic gases (for sulfurous gas),
apron
Dispose of material according to local regulations for the relevant
area and request processing by an industrial waste disposal
company.
Dispose of containers after completely
CONTAINER
removing their contents.
UN CLASSIFICATION Class 8 (Corrosives), PG III
UN NUMBER 1805
Check that containers are not broken or
leaking. Pack containers to prevent shocks,
toppling over, falling, or breaking.
Take measures to prevent the cargo from
collapsing. Cover containers with a
SECTION XIV light-shielding cloth to avoid exposure to
TRANSPORTATION SPECIFIC SAFETY direct sunlight. Prevent containers from
INFORMATION MEASURES AND becoming wet with rain.
CONDITIONS FOR Carefully handle containers to prevent
TRANSPORTATION breakage, leakage, or splattering due to
shocks, toppling over, or falling.
Always wear the required protective
equipment when performing loading,
unloading, transport, and filling tasks.
Avoid contact and mixed loading with metals,
alkaline substances, and cyanide compounds.

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.

456 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

8.9.4 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime

PRODUCT NAME Soda Lime


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number

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8 Reference Information

GHS
Skin corrosion/irritation Category 1B
CLASSIFICATION

HAZARD SYMBOL DANGER

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.

SECTION II IF SWALLOWED: Rinse mouth. Do NOT induce


HAZARDS vomiting.
Response
IDENTIFICATION IF INHALED: Remove victim to fresh air and
keep at rest in a position comfortable for
breathing.
Immediately call a POISON CENTRE or
doctor/physician.
Wash contaminated clothing before reuse.
Specific measures (see MSDS).
Storage Store locked up.
Dispose of contents/container to a located
Disposal
point.
EU CLASSIFICATION according to Directive 67/548/EEC.
SYMBOL C
R-phrase R34 Causes burns.
S26 In case of contact with eyes, rinse
immediately with plenty of water and seek
medical advice.
S-phrase S36/37/39 Wear suitable protective clothing,
gloves and eye/face protection.
S45 In case of accident or if you feel unwell,
seek medical advice immediately.

458 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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.

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8 Reference Information

Remove ignition sources and ventilate the


area. In case of insufficient ventilation, wear
PERSONAL
suitable respiratory equipment.
PRECAUTIONS
Avoid raising dust and avoid contact with skin
and eyes.
ENVIRONMENTAL Prevent spills from entering sewers,
SECTION VI
PRECAUTIONS watercourses or low areas.
ACCIDENTAL RELEASE
MEASURES Do not touch spilled material without suitable
protection (See section 8). After material is
completely picked up, wash the spill site with
METHODS FOR
soap and water and ventilate the area. Put all
CLEANING UP
wastes in a plastic bag for disposal and seal it
tightly. Remove, clean, or dispose of
contaminated clothing.
Avoid contact with eyes, skin and clothing.
PRECAUTION FOR Avoid prolonged or repeated exposure. Handle
SAFE HANDLING material with suitable protection.
SECTION VII This material is hygroscopic.
HANDLING AND
Store away from sunlight in well-ventilated dry
STORAGE CONDITIONS FOR
place at room temperature. Keep container
SAFE STORAGE
tightly closed.
INCOMPATIBILITIES Strong acids
Use exhaust ventilation to keep airborne
ENGINEERING
concentrations below exposure limits. Use only
MEASURES
with adequate ventilation.
Local Exhaust:Necessary, Mechanical (General) ;
VENTILATION Necessary
Special:Closed system is recommended.
INDIVIDUAL PROTECTION MEASURES
SECTION VIII Respiratory
EXPOSURE NIOSH/MSHA approved respirator
protection
CONTROLS/PERSONAL
PROTECTION Hand protection Impervious gloves
Eye protection Safety glasses (goggles)
Skin protection Protective clothing
CONTROL PARAMETER
OSHA Final
None established
Limits
ACGIH TLV(s) None established

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8.9 Safety Data Sheets (SDS)

APPEARANCE White - slightly brown, shot


ODOUR Odorless
pH Not available
MELTING POINT Not available
INITIAL BOILING
Not available
POINT
FLASH POINT Not available

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

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8 Reference Information

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.

462 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

IATA
UN NUMBER UN3262
UN PROPER Corrosive solid, basic, inorganic, n.o.s.
SHIPPING NAME (Soda lime)
CLASS or
Corrosives. (Class 8)
DIVISION

SECTION XIV PACKING GROUP PG III


TRANSPORT MARINE
INFORMATION No
POLLUTANT
DOT (Department of Transportation)
IDENTIFICATION
UN3262
NUMBER
PROPER
Corrosive solid, basic, inorganic, n.o.s.
SHIPPING NAME
HAZARD CLASS Corrosive material (Class 8)
US REGULATIONS
New Jers. RTK Haz. Subst. List
CERCLA RQ= Not listed
EPA
EPCRA TPQ= Not listed
SECTION XV
REGULATORY OSHA TQ= Not listed
INFORMATION NFPA HR= health-2, flam.-0, react.-1
HMIS HR= health-2, flam.-0, react.-1
Use of this product must be restricted to
TSCA research or analysis for the development of a
product in accordance with the Act.
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

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8 Reference Information

8.9.5 Ceramic Fiber

PRODUCT NAME Ceramic Fiber


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
Alumina Ceramic Fiber
INGREDIENT [CAS# 675106-31-7]
Diameter about 3 µm
% 100
SECTION II
HAZARDOUS HAZARD DATA 0.2 f/cm3 [Notice of Intended Changes on
INGREDIENTS/ TLV-TWA ACGIH]
IDENTITY
Counting fibers;
INFORMATION
Longer ³ 5 µm
REMARKS
Diameter < 3 µm
Length/Diameter ³ 3

Hazard Data Source ACGIH Threshold Limit Values for 2002


Boiling Point No data
Solubility in Water N/A
Melting Point No data

SECTION III Appearance White, loose wool


PHYSICAL/CHEMICAL Evaporation Rate N/A
CHARACTERISTICS
Odor No odor-
Density (kg/m3) -
Service
1,300 - 1,700
Temperature (°C)

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

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8.9 Safety Data Sheets (SDS)

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.

SECTION VI Record details of operation and arrange


3.
HEALTH HAZARD training/education of workers.
DATA Workers should wash hand and rinse mouth
4.
after use.
Emergency and First Aid Procedures
First aid procedure is not necessary for
respiratory tract. May cause cough, phlegm,
Inhalation etc., in case continue to inhale more than
acceptable level as described below. Get
medical attention in such case.
Ingestion is unlikely. If ingested, drink
Ingestion sufficient water and vomit and get medical
attention.
Flush with water or slightly warm water and
Skin Contact wash with soap. Get medical attention if pain
and inflammation.
Flush eyes with water for a least 15 minutes.
Abrasive action may cause damage to the 8
Eye Contact
outer surface of the eye. Get medical attention
if irritating.

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8 Reference Information

Carcinogenicity (Refractory Ceramic Fiber)


NTP B2-Reasonably anticipated to be a carcinogen
IARC
2B-Possibly carcinogenic to humans
Monographs
EU 2-Probably carcinogenic to humans
Data of Experiments of Refractory Ceramic Fiber on Animals
Result of experiments depends on kinds of experimental animals,
volume/size distribution/process of exposure etc. of fiber dosed to
experimental animals and therefore a number of experiments are
necessary.
There is a report that increase of lung tumor
has been observed in rats exposed to the
1. inhalation of 8.4 mg/m3 of Alumina Silicate
Ceramic Fiber (RCF) into lung for twelve
months.
There is a report that pleural sarcoma has
been frequently observed in rats exposed to
SECTION VI
2. the dose of ceramic fiber into pleural cavity,
HEALTH HAZARD
especially be diameter less than 0.25 mm and
DATA
length more than 8 µm (8 µm exclusive).
There is a report that pleural interstitial
fibrosis has been observed in 3 rats out of 36
3.
rats exposed to one dose of 20 mg RCF into
pleura.
There is a report that one % of interstitial
fibrosis has been observed in hamsters exposed
to the inhalation of 12 mg/m3 RCF with 1.8
mm for 24 months (6 hours per day, 5 days
4. per week) not in rats.
Also there is a report that peritoneal
interstitial fibrous has been observed in
hamsters and rats exposed to one dose of
same 25 mg/m3 into pleural cavity.
There is a report that tumor has been
observed in 2.6-14.5 % of rats exposed to the
5. inhalation of RCF 3-30 mg/m3 with kaolin as
raw materials for 24 months (6 hours per day,
5 days per week).

466 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

Use vacuum suction with HEPA filters to clean


Step to be taken in
up spilled material suppressing generations of
case material is
airborne dust. Wear air purifying respirator or
released or spilled
mask when clean up.
Disposal of this waste material must be by
plastic bag with minimum 0.05mm thickness to
prevent generations of airborne dust.
Precaution on
The transportation, storage, treatment and
SECTION VII waste disposal
disposal of this waste material must be
PRECAUTION FOR
conducted in compliance with all applicable
SAFE HANDLING AND
local regulations.
USE
Avoid generations of airborne dust by
breakage of package during transportation.
Repair broken part of package by adhesive
Precaution on tape and also arrange new packing in case of
transportation breakage.
Refer "Step to be taken in case material is
released or spilled" in this MSDS for treatment
of spilled material.
Restrict and separate areas where this product
is used.
Close up tight and/or install/provide proper
Suppressive
general and/or local ventilation at the places
procedure
where dust concentrations exceeds TLV. Inspect
regularly such ventilation to maintain initial
functions.
Respiratory protection must be selected/used
according to airborne concentrations as
Respiratory described below.
Protection Respiratory protection must be checked for
(Specify Type): fitness to face and also arranged proper
maintenance on filter in case use Half-Face air
purifying respirator.
SECTION VIII Concentration (8-hours TWA) Minimum Acceptable Respirator
CONTROL MEASURES Type
0.1- 1 f/cm3 Disposable dust respirator.
Half-Face, air-purifying respirator equipped
1- 5 f/cm3 with high-efficiency particulate air (HEPA) filter
cartridges.
Full-Face, air purifying respirator with
high-efficiency particulate air (HEPA) filter
5-25 f/cm3
cartridges or powered air-purifying respirator
equipped with HEPA filter cartridges.
Greater than Full-Face, positive pressure supplied air
25f/cm3 respirator. 8
Wear proper eye protection such as chemical
Eye Protection
goggles, safety glasses with side seal.

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8 Reference Information

Wear gloves and long-sleeve work clothes to


prevent skin irritation as necessary. Remove
materials from area of contact of clothes by
Other Protective
SECTION VIII vacuum suction with HEPA filter or adhesive
Clothing or
CONTROL MEASURES tape avoiding generations of airborne dust.
Equipment
Recommended workers who may be sensitive
to a fiber not to engage in handling this
product.
Avoid smoking at the workplace.
Preparations containing RCF should not be sprayed.
This product does not contain crystalline silica. However product
which has been in service at elevated temperatures (greater than 1,
000 °C) may undergo partial conversion to cristobalite, a form of
crystalline silica. Cristobalite is classified as a GROUP 1 by IARC and
by definition the agent of GROUP 1 is carcinogenic to
humans. So special caution must be taken.
The information provided on this Material Safety Data Sheet is based
on ACGIH Threshold Limit Values 2002 as of the date of issuance of
the sheets. The purchaser shall follow the up-to-date rules and also
your local rules, laws, regulations, etc. Obey up-to-date local rules,
SECTION IX laws, regulations, etc.
SPECIAL The information presented herein is based on
PRECAUTIONS data considered to be accurate as of date of
preparation of this Material Safety Data Sheet.
However, no warranty or representation,
express or implied, is made as to the accuracy
or completeness of the foregoing data and
safety information, nor is any authorization
NOTICE
given or implied to practice any patented
invention without a license. In addition, no
responsibility can be assumed by vendor for
any damage or injury resulting from abnormal
use, from any failure to adhere to
recommended practices, or from any hazards
inherent in the nature of the product.

468 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

8.9.6 Halogen Scrubber

PRODUCT NAME Halogen Scrubber


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
Melt Point 1083 °C

Boil Point 2595 °C

Density N/A
Vapor Pressure N/A

SECTION II Vapor Density N/A


PHYSICAL DATA Evaporation Rate N/A
Odor N/A
Color Reddish
Phase Solid Malleable Metal
Water Solubility N/A
SECTION III
HAZARDS Dust, mist or fumes may cause eye and skin irritation. Avoid contact.
IDENTIFICATION
RAT/MOUSE LD50 N/A

SECTION IV RTECS# GL5325000


TOXICITY DATA OSHA PEL N/A
ACGIH TLV-TWA N/A
SECTION V
Exposure to large amounts can cause gastrointestinal disturbances,
HEALTH HAZARD
nausea, vomiting, headaches, or dizziness.
DATA
In case of contact, immediately flush eyes with copious amounts of
water for at least 15 minutes. in case of skin contact, immediately
SECTION VI
FIRST-AID MEASURES
wash skin with soap and copious amounts of water. if ingested and 8
subject is conscious, immediately give large amounts of water. get
medical attention.
SECTION VII Appropriate to surrounding fire. Possible
EXTINGUISHING
FIRE FIGHTING formation of toxic copper fumes. Use
MEDIA
MEASURES appropriate respiratory support.
SECTION VIII
ACCIDENTAL RELEASE N/A
MEASURES

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8 Reference Information

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.

470 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

8.9.7 High Sensitivity Catalyst

PRODUCT NAME High Sensitivity Catalyst


Manufacture/supplier SHIMADZU CORPORATION
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
Kyoto 604-8511, Japan
SECTION I
PRODUCT AND Department in Analytical & Measuring Instruments Division,
COMPANY charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
This product is specifically for use as a catalyst in the TOC 500,TOC
SECTION II
5000, and TOC 4000 series of TOC analyzers. Refer to the
PRODUCT USE
appropriate instruction manual for directions on proper use.
Melt Point N/A
Boil Point N/A
Density N/A
Vapor Pressure N/A

SECTION III Vapor Density N/A


PHYSICAL DATA Evaporation Rate N/A
Odor N/A
Color Grey
Phase Fibrous Solid
Water Solubility N/A
Possible sensitizer. Keep away from sources of
SECTION IV ignition - NO SMOKING. Take precautionary
HAZARDS FLAMMABLE measures against static discharges. Keep
IDENTIFICATION container tightly closed and in a
well-ventilated place.
May be harmful by inhalation or ingestion.
May cause eye irritation. May cause skin
irritation. Material may be irritating to mucous
ACUTE EFFECTS membranes and upper respiratory tract.
Prolonged or repeated exposure may cause
SECTION V allergic reactions in certain sensitive
TOXICITY DATA individuals.
Coughing, chest pains, difficulty in breathing. 8
EXPOSURE CAN To the best of our knowledge, the chemical,
CAUSE physical, and toxicological properties have not
been thoroughly investigated.
SECTION VI
HEALTH HAZARD SEE SECTION 5.
DATA

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8 Reference Information

In case of contact, immediately flush eyes or skin with copious


amounts of water for at least 15 minutes while removing
contaminated clothing and shoes. IF inhaled, remove to fresh air. If
SECTION VII
not breathing give artificial respiration. If breathing is difficult, give
FIRST-AID MEASURES
oxygen. If swallowed, wash out mouth with water provided
person is conscious. Call a physician. Remove and wash contaminated
clothing promptly.
SECTION VIII
EXTINGUISHING CARBON dioxide, dry chemical powder or
FIRE FIGHTING
MEDIA appropriate foam.
MEASURES
Shut off all sources of ignition. Wear self-contained breathing
SECTION IX
apparatus, rubber boots and heavy rubber gloves.
ACCIDENTAL RELEASE
Sweep up, place in a bag and hold for waste disposal. Ventilate area
MEASURES
and wash spill site after material pickup is complete.
INCOMPATIBILITIES Strong oxidizing agents, organic materials.
SECTION X HAZARDOUS
STABILITY AND COMBUSTION OR Nature of decomposition products not known.
REACTIVITY DECOMPOSITION Hazardous polymerization will not occur.
PRODUCTS
The above information is believed to be correct but does not
SECTION XI 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.

472 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

8.9.8 Normal Sensitivity Catalyst

PRODUCT NAME Normal Sensitivity Catalyst


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Ku wabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
This product is specifically for use as a catalyst in the TOC 500,TOC
SECTION II
5000, and TOC 4000 series of TOC analyzers. Refer to the
PRODUCT USE
appropriate instruction manual for directions on proper use.
Melt Point N/A
Boil Point N/A
Density N/A
Vapor Pressure N/A

SECTION III Vapor Density N/A


PHYSICAL DATA Evaporation Rate N/A
Odor N/A
Color Grey
Phase Solid Pellets
Water Solubility N/A
Possible sensitizer. keep away from sources of
ignition - no smoking. Take precautionary
measures against static discharges.
FLAMMABLE
Keep container tightly closed and in a
SECTION IV well-ventilated place. Harmful by inhalation.
HAZARDS Irritating to respiratory system.
IDENTIFICATION
Lungs, bones, do not breathe dust. In case of
insufficient ventilation, wear suitable
TARGET ORGAN(S)
respiratory equipment. Wear suitable
protective clothing.

TOC-LCPH/CPN LabSolutions TOC Volume 473


8 Reference Information

May be harmful by inhalation or ingestion.


May cause eye irritation. may cause skin
irritation. Material may be irritating to mucous
ACUTE EFFECTS membranes and upper respiratory tract.
prolonged or repeated exposure may cause
allergic reactions in certain sensitive
individuals.
EXPOSURE CAN Coughing, chest pains, difficulty in breathing,
CAUSE gastrointestinal disturbances.

SECTION V Prolonged exposure can cause damage to the


TOXICITY DATA lungs and bones. TO the best of our
CHRONIC EFFECTS knowledge, the chemical, physical, and
toxicological properties have not been
thoroughly investigated.
Lungs, thorax or respiration (tumors)
tumorigenic (neoplastic by RTECS criteria)
tumorigenic (equivocal tumorigenic agent by
TARGET ORGAN
RTECS criteria) tumorigenic (tumors at site of
DATA
application) only selected registry of toxic
effects of chemical substances (RTECS) data is
presented here. see actual entry in RTECS.
SECTION VI
8H TWA 5MG/ME respirable fraction; 8h TWA
HEALTH HAZARD OSHA PEL
10MG/M3 total dust
DATA
In case of contact, immediately flush eyes with copious amounts of
water for at least 15 minutes while removing contaminated clothing
and shoes. If inhaled, remove to fresh air. If not breathing give
SECTION VII artificial respiration. If breathing is difficult, give oxygen. If
FIRST-AID MEASURES swallowed, wash out mouth with water provided person is conscious.
Call a physician. Remove and wash contaminated clothing promptly.
In case of skin contact, immediately wash skin with soap and copious
amounts of water.
EXTINGUISHING Carbon dioxide, dry chemical powder or
SECTION VIII MEDIA appropriate foam.
FIRE FIGHTING UNUSUAL FIRE Material may have an exothermic reaction
MEASURES AND EXPLOSIONS above 200 c with halocarbon vapors and may
HAZARDS produce toxic hydrochloric acid and phosgene.
Shut off all sources of ignition. Wear self-contained breathing
SECTION IX
apparatus, rubber boots and heavy rubber gloves. Sweep up, place
ACCIDENTAL RELEASE
in a bag and hold for waste disposal.
MEASURES
Ventilate area and wash spill site after material pickup is complete.
Stability Stable.
Strong acids, strong bases, chlorine trifluoride,
ethylene oxide, halocarbons, oxygen difluoride,
SECTION X sodium nitrate, vinyl acetate, strong oxidizing
STABILITY AND agents, organic materials. Protect from
REACTIVITY Incompatibilities
moisture. Hazardous combustion or
decomposition products. Nature of
decomposition products not known. Hazardous
polymerization will not occur.

474 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

The above information is believed to be correct but does not


SECTION XI 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.

TOC-LCPH/CPN LabSolutions TOC Volume 475


8 Reference Information

8.9.9 Catalyst Platinum Black

PRODUCT NAME Catalyst Platinum Black


Manufacture/supplier SHIMADZU CORPORATION
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION 1: Kyoto 604-8511, Japan
Identification of the
Department in Analytical & Measuring Instruments Division,
substance/mixture
charge Environmental Business Unit
and of the
company/undertaking Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency telephone
81(75)-823-1207
number
This product does not
meet the classification
Classification of the Classification
and labelling criteria
substance or mixture information
SECTION 2: given in the Regulation
Hazards identification (EC) No 1272/2008 (CLP).
Label elements Not relevant
Other hazards No data available.
Not applicable. The product is not a
Substances
substance.
Hazardous ingredients

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.

Full Text for all H-phrases and EUH-phrases:


pls. see section 16

476 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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.

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8 Reference Information

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.

478 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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

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8 Reference Information

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.

480 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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.

TOC-LCPH/CPN LabSolutions TOC Volume 481


8 Reference Information

Reactivity No data available.


Chemical stability No data available.
Possibility of
No data available.
hazardous reactions
SECTION 10:
Stability and Conditions to avoid Heat; Keep away sources of ignition.
reactivity Incompatible
Oxidizing agents; Alkalis; Acids
materials
Hazardous
No hazardous decomposition products
decomposition
known.
products
Acute oral
No data available.
toxicity
Acute dermal
No data available.
toxicity
Acute
inhalational No data available.
toxicity
Skin corrosion/
No data available.
irritation
Serious eye
No data available.
damage/irritation
Respiratory or
No data available.
skin sensitisation
Germ cell
No data available.
mutagenicity
Reproduction
No data available.
toxicity
SECTION 11:
Information on Carcinogenicity No data available.
Toxicological
toxicological effects
information STOT - single
No data available.
exposure
STOT - repeated
No data available.
exposure
Aspiration
No data available.
hazard
Symptoms
related to the
Eye contact may cause
physical,
mechanical irritation
chemical and
through dust particles.
toxicological
characteristics
Delayed and
immediate
effects as well as Inhalation of dusts may
chronic effects irritate the respiratory
from short and tract.
long-term
exposure

482 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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.

SECTION 13: Residuals must be


Waste treatment removed from packaging
Disposal
methods and when emptied
considerations
completely disposed of in
accordance with the
Packaging regulations for waste
removal. Incompletely
emptied packaging must
be disposed of in the 8
form of disposal specified
by the regional disposer.

TOC-LCPH/CPN LabSolutions TOC Volume 483


8 Reference Information

Transport The product is not subject to ADR/RID/ADN


ADR/RID/AND regulations.
The product is not subject to IMDG
Transport IMDG
regulations.
Transport ICAO-TI / The product is not subject to ICAO-TI / IATA
IATA regulations.
Other information No data available.
SECTION 14:
Transport Information on environmental hazards, if
Environmental
information relevant, please see 「Transport
hazards
ADR/RID/AND」- 「Transport ICAO-TI / IATA」.
Special precautions
No data available
for user
Transport in bulk
according to Annex II
Not relevant
of Marpol and the
IBC Code
According to the data
available and/or
Regulation (EC)
specifications supplied by
No 1907/2006
upstream suppliers, this
(REACH) Annex
product does not contain
XIV (List of
any substances considered
substances
as substances requiring
subject to
authorisation as listed on
authorisation)
Annex XIV of the REACH
Safety, health and regulation (EC) 1907/2006.
environmental According to available
SECTION 15:
regulations/legislation data and the information
Regulatory
specific for the provided by preliminary
information
substance or mixture suppliers, the product
EU regulations REACH does not contain
candidate list of substances that are
substances of considered substances
very high meeting the criteria for
concern (SVHC) inclusion in annex XIV
for authorisation (List of Substances Subject
to Authorisation) as laid
down in Article 57 and
article 59 of REACH (EC)
1907/2006.

484 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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

TOC-LCPH/CPN LabSolutions TOC Volume 485


8 Reference Information

8.9.10 NH3 Absorbent

PRODUCT NAME NH3 ABSORBENT


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
Acute toxicity Oral Category 4
Skin corrosion/ irritation Category 1A
Serious eye damage/ eye
Category 1
GHS Classification irritation
Specific target organ systemic
Category 3
toxicity Single exposure
< the respiratory tract irritation >

Hazard Symbol DANGER

H302 Harmful if swallowed


H314 Causes severe skin burns and eye damage
Hazard Statements
H318 Causes serious eye damage
H335 May cause respiratory irritation

SECTION II P264 Wash hand thoroughly after handling.


HAZARDS P270 Do no eat, drink or smoke when using
IDENTIFICATION this product.
P260 Do not breathe
dust/fume/gas/mist/vapours/spray.
P280 Wear protective gloves/protective
clothing/eye protection/face protection.
P301+P330+P331 IF SWALLOWED: rinse mouth.
Do NOT induce vomiting.
P304+P340 IF INHALED: Remove victim to fresh
Precautionary air and keep at rest in a position comfortable
Statements for breathing.
P305+ P351+P338 IF IN EYES: Rinse cautiously
with water for several minutes. Remove
contact lenses, if present and
easy to do. Continue rinsing.
P271 Use only outdoors or in a well-ventilated
area.
P312 Call a POISON CENTER or doctor/physician
if you feel unwell.
P403+P233 Store in a well-ventilated place.
Keep container tightly closed.

486 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

Component Phosphoric acid


Formula H3PO4

CAS No. 7664-38-2


SECTION III
COMPOSITION / Content 20 - 25 %
INFORMATION ON Component Diatomaceous earth, (Calcined)
INGREDIENTS
Formula SiO2

CAS No. 91053-39-3


Content 75 - 80 %
Wash off immediately with soap and plenty of
water. In the case of respirable dust and/or
GENERAL ADVICE fumes, use self-contained breathing apparatus
and dust impervious protective suit. Use
personal protective equipment.
Move victim to fresh air. If breathing is
INHALATION difficult, give oxygen. If irritation persists,
consult a physician.
Remove contaminated clothes and shoes, rinse
skin with plenty of water or shower. Use soap
SECTION IV SKIN CONTACT
to help assure removal. If irritation persists,
FIRST AID MEASURES
consult a physician.
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,
consult a physician.
Rinse mouth, give plenty of water to dilute the
INGESTION substance. Never give anything by mouth to an
unconscious person. Consult a physician.
EXTINGUISHING Carbon dioxide, dry chemical powder, foam,
MEDIA water
FIRE & EXPLOSION Toxic and irritating dust, fumes or smoke may
SECTION V
HAZARDS be emitted.
FIRE-FIGHTING
MEASURES SPECIAL Firemen should wear normal protective
PROTECTIVE equipment (full bunker gear) and
EQUIPMENT FOR positive-pressure self-contained breathing
FIREFIGHTERS apparatus.

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8 Reference Information

Remove ignition sources and ventilate area. In


PERSONAL case of insufficient ventilation, wear suitable
PRECAUTIONS respiratory equipment. Avoid raising dust and
avoid contact with skin and eyes.
ENVIRONMENTAL Prevent spills from entering sewers,
SECTION VI PRECAUTIONS watercourses or low areas.
ACCIDENTAL RELEASE
Do not touch spilled material without suitable
MEASURES
protection (See section 8). After material is
completely picked up, wash the spill site with
METHODS FOR
soap and water and ventilate the area. Put all
CLEAN UP
wastes in a plastic bag for disposal and seal it
tightly. Remove clean or dispose of
contaminated clothing.
Avoid contact with eyes, skin and clothing.
HANDLING Avoid prolonged or repeated exposure. Handle
material with suitable protection.
SECTION VII
Store away from sunlight in well-ventilated dry
HANDLING AND
STORAGE place at room temperature (Preferably cool
STORAGE
place). Keep container tightly closed.
INCOMPATIBLE
Strong oxidizers, alkalis, metals
PRODUCTS
Use exhaust ventilation to keep airborne
ENGINEERING
concentrations below exposure limits. Use only
MEASURES
with adequate ventilation.
Local Exhaust; Necessary, Mechanical (General);
VENTILATION
Recommended
TWA=
OSHA Final Limits 1 mg/m3
(H3PO4)
CONTROL TWA=
PARAMETER 1 mg/m3;
SECTION VIII
EXPOSURE ACGIH TLV(s) STEL=
CONTROLS, 3 mg/m3
PERSONAL (H3PO4)
PROTECTION
NIOSH/MSHA
Respiratory protection approved
respirator
Chemical
PERSONAL Hand protection resistant
PROTECTION gloves
Safety glasses
Eye protection
(goggles)
Protective
Skin protection
clothing

488 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

APPEARANCE Brown or Red, Pellets


ODOR Odorless
pH Not available
BOILING POINT Not available
MELTING POINT Not available
FLASH POINT Non flammable
FLAMMABILITY
Non flammable
(solid, gas)
SECTION IX
PHYSICAL AND DECOMPOSITION
Not available
CHEMICAL TEMPERATURE
PROPERTIES
EXPLOSIVE LIMITS Not available
VAPOR PRESSURE Not available
SPECIFIC GRAVITY Not available
WATER Not soluble
ETHANOL Not soluble
SOLUBILITY IN ACETONE Not soluble
Phosphoric acid will be eluted when immersed
in water, ethanol and acetone
CONDITION TO
Sunlight, heat,
AVOID
INCOMPATIBILITY
(MATERIAL TO Strong oxidizer, Strong alkalis, Moisture
SECTION X AVOID)
STABILITY AND
REACTIVITY HAZARDOUS
DECOMPOSITION Not available
PRODUCTS
HAZARDOUS
Will not occur.
POLYMERIZATION

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8 Reference Information

Acute toxicity no data available


Skin
no data available
corrosion/irritation
Serious eye
damage/eye no data available
irritation
Respiratory or skin
no data available
sensitization
Germ cell
no data available
mutagenicity
Carcinogenicity
A4 - Not classifiable as a human carcinogen
(Diatomaceous earth (Calcined))
IARC 3 - Group 3: Not classifiable as to its
carcinogenicity to humans (Diatomaceous
earth(Calcined))
SECTION XI Group 3 Not Classifiable as to Carcinogenicity
IARC
TOXICOLOGICAL to Humans (Phosphoric acid)
INFORMATION
Reproductive
no data available
toxicity
Specific target
organ toxicity - no data available
single exposure
Specific target
organ toxicity - no data available
repeated exposure
Aspiration hazard no data available
Potential health effects
Harmful if inhaled. Causes respiratory tract
Inhalation
irritation.
Ingestion Harmful if swallowed.
Harmful if absorbed through skin. May cause
Skin
skin irritation.
Eyes Causes serious eye irritation.
BIODEGRADABILITY Not available
BIOACCUMULATIO
SECTION XII Not available
N POTENTIAL
ECOLOGICAL
INFORMATION AQUATIC TOXICITY Not available
OTHER
Not available
INFORMATION
Dispose in a hazardous-waste site in accordance with all applicable
SECTION XIII
regulations. Any disposal practice must be in compliance with
DISPOSAL
country, local, state, and federal laws and regulations (contact
CONSIDERATIONS
country, local or state environmental agency for specific rules)

SECTION XIV IATA Not Restricted


TRANSPORT DOT (Department
INFORMATION Non Hazardous Material for DOT shipping.
of Transportation)

490 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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.

TOC-LCPH/CPN LabSolutions TOC Volume 491


8 Reference Information

8.9.11 Silica Glass Wool

PRODUCT NAME Silica Glass Wool


Manufacture/
SHIMADZU CORPORATION
supplier
1 Nishinokyo-Kuwabara-cho, Nakagyo-ku,
Address
SECTION I Kyoto 604-8511, Japan
PRODUCT AND
Department in Analytical & Measuring Instruments Division,
COMPANY
charge Environmental Business Unit
IDENTIFICATION
Telephone number 81(75)-823-1207
Fax number 81(75)-823-4614
Emergency
81(75)-823-1207
telephone number
GHS classification
Explosives No classification
Flammable gases No classification
Flammable
No classification
aerosols
Oxidizing gases No classification
Gases under
No classification
pressure
Flammable
No classification
liquids
Flammable solids Not classified
Self-reactive
substances and No classification
mixtures
SECTION II
Pyrophoric
HAZARD No classification
liquids
IDENTIFICATION
Pyrophoric solids Not classified
Self-heating
substances and Not classified
mixtures
Substances and
mixtures which,
in contact with Not classified
water, emit
flammable gases
Oxidizing liquids No classification
Oxidizing solids Classification not possible
Organic
No classification
peroxides
Corrosive to
Classification not possible
metals

492 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

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

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8 Reference 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

494 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

SiO2 in a compact from is absolutely not dangerous, only in case of


dry dust use the following measures
Remove a victim to fresh air and keep at rest
in a position comfortable for breathing.
IF INHALED Make an arrangement to get medical attention
immediately.
If feel unwell, call a physician.
Wash with plenty of water and soap.
In case of cut, conduct treatments such as
IF ON SKIN
hemostasis and disinfection, and get medical
attention immediately.
Remove contact lenses, if present and not
firmly fixed. Get medical attention
SECTION IV immediately.
FIRST-AID MEASURES Wash eyes with clean water immediately.
IF IN EYES If eye irritation persists: Get medical advice/
attention.
Do not rub eyes or close eyes tightly, since eye
damage may occur by sharp edges such as
glass powder.
Call a physician immediately. Rinse mouth.
IF SWALLOWED
Do not induce vomiting.
Most important
effects and No information available.
symptoms
Protection for
No information available.
first-aid responders
Note to physician No information available.
Dry chemical powder, foam, carbon dioxide,
Extinguishing
sand.
media
This product itself will not burn.
Unsuitable Mist may be used for cooling purposes, but
extinguishing cylindrical water flow should not be used for
media extinguishing fire.
Specific hazards
SECTION V
arising from the No information available
FIRE-FIGHTING
chemical if burning
MEASURES
Fight fire from upwind side.
Specific fire Keep people away from around the fire
fighting measures generation site.
Evacuate people to a safe place.
Special protective During fire-fighting, wear heat resistance
equipment for fire gloves, safety goggles, and breathing 8
fighter apparatus.

TOC-LCPH/CPN LabSolutions TOC Volume 495


8 Reference Information

Personal Keep people away from around the leakage


precautions, site by encircling it with a rope.
protective During working, wear rubber gloves, safety
equipment and glasses, protective clothing, and a dust/mist
emergency filtering respirator so as to prevent adhering
procedures powder to the skin and inhalation of dust.

SECTION VI Exercise caution so as not to drain the leaked


Environmental
ACCIDENTAL RELEASE precautions product into rivers, etc. but to minimize the
MEASURES adverse events on the environment.
Sweep the scattered product and collect it into
Method of cleaning
an empty container which can be closed
up
tightly.
Prevention
measures of No information available
secondary disaster
Handling
Take facility measures stated in “Section 8.
Exposure controls and personal protection“
Appropriate and wear protective equipment.
engineering Exercise caution for fall, impulse, and weight
controls load, since the product is liable to damages.
Avoid use or handling which causes change in
forms, since this material is fragile.
Conduct local or entire exhaust ventilation
Local and entire
stated in “Section 8. Exposure controls and
ventilation
personal protection”.
General Ventilate when dust is generated during
SECTION VII
precautions processing.
HANDLING AND
STORAGE Safe handling To prevent the products from contamination,
advice do not touch with bare hands.
Storage
Appropriate
engineering No information available
controls
Appropriate
Store in stable conditions not to cause
storage
inversion, fall, and damage.
conditions
Safe containers
Use vinyl container and exercise caution for
and packaging
contamination (from view point of quality).
materials

496 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

In case of generation of dust by handling,


Facility measures install ventilation facility to keep the working
site under the threshold limit value.
Administrative
Not established
levels
Occupational Exposure Limits
1mg/m3
Silica, vitreous TWA
Japan Society for Occupational Health
SECTION VIII 0.1mg/m3
EXPOSURE
Silica, vitreous TWA
CONTROLS/PERSONAL
PROTECTION ACGIH
Personal protective equipment
Respiratory Dust/mist filtering respirator, air-supplied mask,
protection etc.
Hand protection Leather gloves
Eyes Protection Safety goggles or a face shield
Skin and body Long-sleeve shirts and long pants made of
protection thick cloth
Appropriate Wash hands thoroughly and gargle after
hygiene measures working, and eat and drink.

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8 Reference Information

Physical State Solid (Lumps)


Clear for Clear Slica Glass , White for Opaque
Colour
Silica Glass
Odour(Odour
Odor less
threshold)
pH Not applicable
Melting
point/Freezing There is no clear melting point
point
Boiling point 2227 °C
Initial boiling point Unknown
Boiling range Unknown
Flash point Unknown
Auto-ignition
Unknown
temperature
SECTION IX
Flammability (solid,
PHYSICAL AND Noncombustible
gas)
CHEMICAL
PROPERTIES Lower flammability
Unknown
or explosive limits
Upper flammability
Unknown
or explosive limits
Vapor pressure Unknown
Vapor density Unknown
Evaporation rate Unknown
Specific gravity 2.2 (15 °C) for Clear Silica Glass
(Relative density) 1.9~2.1 (15 °C) for Opaque Silica Glass
Solubility Unknown
Partition
coefficient; Unknown
n-octanol/water
Decomposition
Unknown
temperature
Other information No information available
Stable at ordinary storage and handling
Chemical stability
conditions.
Possibility of Stable at ordinary storage and handling
hazardous reactions conditions.
Extremely rapid heating, rapid cooling
SECTION X Fused or amorphous silica may become
Conditions to avoid
STABILITY AND crystalline if held at high temperatures for
REACTIVITY extended periods of time.
Incompatible
No information available
materials
Hazardous
decomposition No information available
products

498 TOC-LCPH/CPN LabSolutions TOC Volume


8.9 Safety Data Sheets (SDS)

Acute toxicity Unknown


Skin
Unknown
corrosion/Irritation
Serious eye
Unknown
damage/irritation
Respiratory
sensitization/skin Unknown
sensitization
Mutagenicity (Germ
Unknown
cell mutagenicity)
Carcinogenicity
SECTION XI IARC: Group 3 (Cannot be classified as to its
TOXICOLOGICAL Silica, vitreous
carcinogenicity to humans)
INFORMATION
Crystalline silica should be considered a possible human
carcinogen based on this association. Fused silica has not been
identified as a carcinogen.
Reproductive
Unknown
toxicity
Specific target
organ toxicity - Unknown
Single exposure
Specific target
organ toxicity - Unknown
Repeated exposure
Aspiration hazard Unknown
Ecotoxicity
Fish No information available
Crustacea No information available
Algae No information available
SECTION XII Persistence /
ECOLOGICAL No information available
Degradability
INFORMATION
Bioaccumulative
No information available
Potential
Mobility in soil No information available
Other adverse Do not dispose into a general environment
effects due to no data in many items.
Consign disposal to the disposal-specialized
services approved by a prefectural governor in
Residual wastes
accordance with “Waste Management and 8
Public Cleansing Law”.
SECTION XIII
DISPOSAL After removal of contents in the used
CONSIDERATIONS packaging container completely, consign
Contaminated
disposal to the disposal-specialized services
containers and
approved by a prefectural governor in
packaging
accordance with “Waste Management and
Public Cleansing Law”.

TOC-LCPH/CPN LabSolutions TOC Volume 499


8 Reference Information

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.

500 TOC-LCPH/CPN LabSolutions TOC Volume


Index
Numerics E
8-Port Sampler OCT-L 16 Edit Mode 270
Editing Sample Analysis Parameters 214
A Editing the Calibration Curve 228
Acid Preparation 46 Electric Furnace Power 98
Adjusting Sparge Gas Flow Rate 49 Error Messages 359
Analysis Flow 99 Excluding Injection Results 231
Analysis with an ASI-L or OCT-L 261 Exiting the Sample Table Editor 139
Analysis without an ASI-L or OCT-L 263 Exporting to ASCII Format 249
Analysis-Related Technical Information 387
Autosampler ASI-L 15 F
Autosampler Measurement 80 File Viewer 140
File Viewer Display Options 288
B Filling the Humidifier with Water 44
Background Monitor 257 Filling Vials with Sample 82
Blank Check Analysis 71 Flow Diagram 10
B-Type Halogen Scrubber 61 Font 292

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

TOC-LCPH/CPN LabSolutions TOC Volume 501


M Replacing the Syringe Pump 8-port Valve Rotor
Maintenance 317 334
Maintenance Parts List 409 Reviewing and Editing a Calibration Curve 176
Manual Injection Measurement 302 Reviewing and Editing a Control Sample 188
Mechanical Check 354 Reviewing and Editing a Method 183
Menu Bar 140 Reviewing and Editing a Sample Table 175
Reviewing and Editing a Schedule 190
N Reviewing and Editing a System Configuration 134
NOx Absorber 60, 350 Reviewing and Editing Sample Analysis Parameters
226
O Reviewing the Calibration Curve 227
Rinse Bottle Inspection 341
OCT-L Installation 425
Online Manual 300
Opening the Sample Table Editor 139
S
Output Window 141 Safety Data Sheets 433
Sample Catcher Inspection 341
P Sample Report Preview 241
Sample Report 244
Page Setup 234
Sample Table 243, 282
Peak Stop 269
Sample Table Preview 240
Periodic Inspections 320
Sample Window 222
Placing Vials in the Vial Rack 84
Sample Window Display Options 285
Preparation and Storage of Standard Solutions 64
SDS 433
Preparation for POC Analysis 58
Selecting Content for ASCII Export 246
Preparation of Dilution Water 45
Selecting Content to Print 234
Preparing the High Suspension Kit 53
Selecting the Online Manual 300
Principles of Analysis 381
Setting the Display Font of the Output Window
Print Setup 239
289
R Shutdown 271
Sleep 273
Ready Indicator 140
Sparging 75
Recalculating Results 231
Special Accessories 403
Recording the Operation History 296
Specifications 395
Regeneration of the IC Solution 352
Standard Accessories 401
Releasing Time Out Lock 295
Status Bar 141
Removing the Combustion Tube 322
Status Monitor 141
Replace Flowline Content 353
Stirrer Preparation 89
Replacing the 8-Port Valve Rotor 343
Stopping Analysis 269
Replacing the Carrier Gas Purification Tube and
Syringe Plunger Tip Replacement 331
Catalyst 325
Replacing the Catalyst in the Ozone Treatment Unit
T
346
Threshold values 357
Replacing the CO2 Absorber 327
TN Analysis Preparation 60
Replacing the CO2 Absorber for the Optional
TN Unit TNM-L 17
Carrier Gas Purifier 336
TOC-L 6
Replacing the Filler of the Optional POC Analysis
Tool Bar 140
CO2 Absorber 339
Troubleshooting 359
Replacing the Halogen Scrubber 327
Turning on 100
Replacing the Liquid 340
Replacing the Ozone Generator 348 V
Replacing the Pump Head of the IC Reaction
Version Information 301
Solution Pump 338
Vial Numbers 210
Replacing the Pump Head of the Rinse Pump 342
Vial Types 80
Replacing the Sliding Sample Injector O-rings 333

502 TOC-LCPH/CPN LabSolutions TOC Volume


W
Washing 353
Washing or Replacing Catalyst 322
Washing/Replacing the Combustion Tube and
Carrier Gas Purification Tube (Option) 326
Water Supply to the Cooler Drain Vessel 43

Z
Zero Point Detection 352

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