Toc-L CP

638-94602B
Apr. 2012
TOTAL ORGANIC CARBON ANALYZER

TOC-LCPH/CPN
USER'S MANUAL
Read the instruction manual thoroughly before you use the product.
Keep this instruction manual for future reference.
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Introduction
Read this Instruction Manual thoroughly before using the product.
Thank you for purchasing this product. This USER'S MANUAL describes how to use this
product in addition to any accessories and options related to this product. Read this manual
thoroughly before using the product and operate the product in accordance with the
instructions in this manual.
Also, keep this manual for future reference.
IMPORTANT
• If the user or usage location changes, ensure that this Instruction Manual is always kept
together with the product.
• If this manual or a product warning label is lost or damaged, immediately contact your
Shimadzu representative to request a replacement.
• To ensure safe operation, read all Safety Instructions before using the product.
• To ensure safe operation, contact your Shimadzu representative if product installation,
adjustment, or re-installation (after the product is moved) is required.
Notice
• Information in this manual is subject to change without notice and does not represent a commitment on the
part of the vendor.
• Any errors or omissions which may have occurred in this manual despite the utmost care taken in its
production will be corrected as soon as possible, although not necessarily immediately after detection.
• All rights are reserved, including those to reproduce this manual or parts thereof in any form without
permission in writing from Shimadzu Corporation.
• Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States and/or other
countries.
Microsoft®, Windows® XP Operating System is expressed as Windows XP.
Microsoft® Windows 7® Operating System is expressed as Windows 7.
Microsoft®and Windows® are either registered trademarks or trademarks of Microsoft Corporation in the
United States and/or other countries.
• PALAFILM are registered trademarks 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.
© 2011-2012 Shimadzu Corporation. All rights reserved.

Indications Used in This Manual
Cautions and Notes are indicated using the following conventions:
Precautionary Conventions Used in this Manual
The following precautionary conventions are used in this manual.
Convention Description
CAUTION Indicates a potentially hazardous situation which, if not avoided, may

result in minor to moderate injury or equipment damage.
Note: Emphasizes additional information that is provided to ensure the proper

use of this product.
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
In addition to the precautionary conventions, the "Tip" and "Reference" conventions are
used to supply additional information.
Convention Description
TIP » Indicates a particular technique, alternative means of operation, or useful advice.
Reference: Indicates a reference location in the manual where more detailed information can
be found.
ii TOC-LCPH/CPN
Safety Instructions
To ensure safe product operation, read these important safety instructions carefully before
use and follow all CAUTION instructions given in this section.
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.
Installation Site
Do not install this product at a site where fire is prohibited.
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.
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.
TOC-LCPH/CPN iii
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.
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.
Warning Labels
High Temperature Warning

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 or 720 °C). Do
not touch the electric furnace as this could result in burns. Allow the furnace to cool before
performing any maintenance on the combustion tube or catalyst.
iv TOC-LCPH/CPN
Electric Shock Warning
Do not remove this panel, as there is danger of electric shock.
TOC-LCPH/CPN v
Injury Warning
During operation, the pressure in the CO2 absorber of the gas purifier is about 200kPa. To
prevent injuries, turn off the carrier gas and switch off power to the TOC main unit. Wait
until the pressure inside the container and the instrument flow lines return to normal
atmospheric pressure before performing any maintenance.
Corrosion Warning
Acid and other corrosive substances are present in the liquid waste drained from this
instrument. Be careful not to 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 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.
vi TOC-LCPH/CPN
The soda lime in the CO2 absorber of the carrier gas purifier is a corrosive chemical
substance. Be careful not to touch or spill this substance.
TOC-LCPH/CPN vii
The liquid discharged from the drain tube connected to the TC injector contains acid and
other corrosive substances. Verify that the tip of the drain tube is securely inserted into the
Y-shaped fitting when connecting the combustion tube and sample injector.
The IC reaction solution is acidic. Be careful not to touch or spill the IC reaction solution.
viii TOC-LCPH/CPN
Hydrochloric acid is a corrosive chemical substance. Be careful not to touch or spill the
hydrochloric acid.
TOC-LCPH/CPN ix
Warranty
Shimadzu provides the following warranty for this product.
Period:
Please contact your Shimadzu representative for information about the period of this
warranty.
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.
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.
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
x TOC-LCPH/CPN
10) Product movement or transportation after installation
11) Consumable items
Note: 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 xi
After-Sales Service and Availability of Replacement Parts
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.
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.
Note, however, that the availability of units or parts not manufactured by Shimadzu shall be
determined by the relevant manufacturers. 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 individual manufacturer
conditions 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.
xii TOC-LCPH/CPN
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.
Action for Environment (WEEE)
To all users of Shimadzu equipment in the European Union:

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

equipment has reached the end of its life. They will advise
WEEE Mark you regarding the equipment take-back.
With your co-operation we are aiming to reduce contamination from waste electronic and
electrical equipment and preserve natural resource through re-use and recycling.
Do not hesitate to ask Shimadzu service representative, if you require further information.
TOC-LCPH/CPN xiii
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.
Note: 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)
IEC 61000-4-11 Voltage Variations/Dips/Interrupts 0 % UT 1 cycles (20 ms),
70 % UT 25 cycles (500 ms),
0 % UT 250 cycles (5000 ms)
Note: 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.
xiv TOC-LCPH/CPN
Regulatory Information
For Europe:
The product complies with the following requirements.
EMC Directive 2004 / 108 / EC

Low Voltage Directive 2006 / 95 / EC
Product name Total Organic Carbon Analyzer
Model Name TOC-LCPH / CPN
SHIMADZU CORPORATION
Manufacturer ANALYTICAL & MEASURING
INSTRUMENTS DIVISION
1 NISHINOKYO-KUWABARACHO
Address
NAKAGYO-KU KYOTO 604-8511 JAPAN
Authorized Representative in EU SHIMADZU EUROPA GmbH
Alberlt-Hahn-Strasse 6-10, 47269
Address
Duisburg F.R. Germany
TOC-LCPH/CPN xv
Contents of This Manual
Chapter 1 Overview
This chapter provides an overview of the instrument and operational precautions for its use.
Chapter 2 System Description

This chapter briefly describes the TOC-L system components, their names and optional
accessories.
Chapter 3 Preparation for Measurement

This chapter describes the procedures for preparing the instrument, optional accessories
and samples for measurement.
Chapter 4 Analysis Procedure

This describes the measurement operations using the software in direct sequential order.
Chapter 5 Software Operations

This chapter describes the in-depth software operations used for creating files, conducting
measurement and printing reports.
Chapter 6 Analysis with Special Options

This chapter describes measurement procedures using the optional manual injection kit.
Chapter 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.
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.
xvi TOC-LCPH/CPN
Table of Contents
Introduction............................................................................................... i
Indications Used in This Manual................................................................. ii
Precautionary Conventions Used in this Manual ........................................... ii
Other Conventions Used in this Manual ........................................................ ii
Safety Instructions ...................................................................................... iii
Product Applications..................................................................................... iii
Installation Site.............................................................................................. iii
Installation..................................................................................................... iii
Operation....................................................................................................... iii
In an Emergency ............................................................................................ iv
During a Power Outage.................................................................................. iv
Warning Labels .............................................................................................. iv
Warranty ...................................................................................................... x
After-Sales Service and Availability of Replacement Parts...................... xii
After-Sales Service....................................................................................... xii
Replacement Parts Availability.................................................................... xii
Maintenance, Inspections, and Adjustment............................................... xii
Disposal Precautions................................................................................. xiii
Action for Environment (WEEE)................................................................ xiii
Electromagnetic Compatibility................................................................. xiv
Regulatory Information ............................................................................. xv
Contents of This Manual .......................................................................... xvi
1 Overview ................................................................................................... 1
1.1 Overview ..................................................................................................... 2
1.2 Operational Precautions............................................................................... 3
2 System Description................................................................................... 7
2.1 TOC-LCPH/CPN Construction ...................................................................... 8
2.1.1 Front View ...................................................................................................... 8
2.1.2 Right Side View .............................................................................................. 8
2.1.3 Left Side View ................................................................................................ 9
2.1.4 Rear View...................................................................................................... 10
2.1.5 Front Internal View (Left Diagonal) ............................................................. 11
2.1.6 Top Internal View (Left Diagonal) ............................................................... 11
2.1.7 Flow Diagram................................................................................................ 12
2.2 Autosampler ASI-L (Option)..................................................................... 17
2.2.1 Front View (Left Diagonal) .......................................................................... 17
2.2.2 Rear View (Left Diagonal)............................................................................ 17
2.3 8-Port Sampler OCT-L (Option) ............................................................... 18
2.3.1 Front View (Left Diagonal) .......................................................................... 18
2.3.2 Rear View (Right Diagonal) ......................................................................... 18
2.4 TN Unit TNM-L (Option) ......................................................................... 19
2.4.1 Front View (Right Diagonal) ........................................................................ 19
TOC-LCPH/CPN xvii
Table of Contents
2.4.2 View Inside the Door on the Right Side....................................................... 19
2.4.3 Rear View ..................................................................................................... 20
3 Preparation for Measurement.............................................................. 21

3.1 Instrument and Sample Preparation ........................................................... 22
3.1.1 Catalyst Filling ............................................................................................. 22
3.1.1.1 Catalyst for TOC Analysis ................................................................ 23
3.1.1.2 TOC/TN Catalyst (Option) ............................................................... 25
3.1.2 Installing the Cooling Tube Unit (H Type Only) ......................................... 26
3.1.3 Connecting the Combustion Tube ................................................................ 27
3.1.4 Connecting the Halogen Scrubber................................................................ 37
3.1.5 Installing the Syringe.................................................................................... 38
3.1.5.1 Syringe Installation ........................................................................... 38
3.1.6 Water Supply to the Cooler Drain Vessel .................................................... 41
3.1.7 Filling the Humidifier with Water ................................................................ 42
3.1.8 Preparation of Dilution Water ...................................................................... 43
3.1.9 Acid Preparation........................................................................................... 44
3.1.10 Installation of the CO2 Absorber.................................................................. 45
3.1.11 Adjusting Sparge Gas Flow Rate ................................................................. 46
3.1.12 Installing the Suspended Solids Kit.............................................................. 49
3.1.13 IC Analysis Preparations .............................................................................. 51
3.1.14 Preparation for POC Analysis (When Using the Optional POC Kit)........... 54
3.1.15 TN Analysis Preparation (When Using the Optional TNM-L TN Unit)...... 55
3.1.15.1 Installation of the NOx Absorber...................................................... 55
3.1.16 B-Type Halogen Scrubber
(When Using the Optional B-Type Halogen Scrubber) ............................... 56
3.1.17 Preparation and Storage of Standard Solutions ............................................ 59
3.1.17.1 Preparation of Standard Solutions..................................................... 59
3.1.17.2 Storage of Standard Solutions........................................................... 61
3.1.18 Sample Preparation....................................................................................... 61
3.1.18.1 High Sensitivity Analysis.................................................................. 61
3.1.18.2 TC Blank Check Analysis................................................................. 64
3.1.18.3 Pretreatment for IC Removal (Sparging) .......................................... 66
3.1.18.4 Analysis of Samples Containing Suspended Solids.......................... 67
3.1.18.5 Handling Samples Containing Acids, Bases or Salts........................ 68
3.1.19 Sample Preparation for Autosampler Measurement..................................... 70
3.1.19.1 Vial Types ......................................................................................... 70
3.1.19.2 Filling Vials with Sample.................................................................. 72
3.1.19.3 Placing Vials in the Vial Rack .......................................................... 73
3.1.19.4 Rinse Water Preparation ................................................................... 74
3.1.19.5 High Sensitivity ASI-L Analysis ...................................................... 75
3.1.19.6 Acid Addition in NPOC Analysis ..................................................... 76
3.1.19.7 Sparging in NPOC Analysis.............................................................. 77
3.1.19.8 Stirrer Preparation ............................................................................. 77
3.1.20 OCT-L (8-Port Sampler) Measurement........................................................ 80
3.1.20.1 Sample Container .............................................................................. 80
3.1.20.2 Loading the Sample........................................................................... 80
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Table of Contents
3.1.20.3 High Sensitivity Using the OCT-L .................................................... 81
3.1.21 Starting Up the Instrument ............................................................................ 82
3.1.21.1 Turning on the Power ........................................................................ 82
3.1.21.2 Carrier Gas Pressure and Flow Rate Settings .................................... 83
3.1.21.3 Carrier Gas Pressure and Flow Rate Settings
(When Using the Carrier Gas Regulator Option) .............................. 84
3.1.21.4 Electric Furnace Power...................................................................... 85
3.1.21.5 TNM-L Ozone Air Gas Pressure Settings (Option)........................... 85
4 Analysis Procedure ............................................................................... 87

4.1 Analysis Flow ............................................................................................ 88
Step 1 Checks Before Analysis ................................................................................ 88
Step 2 Turning on the Instrument............................................................................. 89
Step 3 Opening the Sample Table Editor ................................................................. 90
Step 4 Creating a Sample Table ............................................................................... 91
Step 5 Creating an Analysis Parameters File ........................................................... 92
Step 6 Editing the Sample Table ............................................................................ 100
Step 7 Entering the Vial Numbers.......................................................................... 102
Step 8 Connecting to the Instrument ...................................................................... 103
Step 9 Conducting Analysis ................................................................................... 104
Step 10 Viewing and Outputting Analysis Results .................................................. 106
Step 11 Ending Analysis .......................................................................................... 108
5 Software Operation.............................................................................. 109

5.1 System Configuration .............................................................................. 110
5.1.1 Creating a New System Configuration ....................................................... 110
5.1.2 Reviewing and Editing a System Configuration......................................... 116
5.1.3 Deleting a System Configuration ................................................................ 118
5.2 Sample Table Editor ................................................................................ 119
5.2.1 Opening the Sample Table Editor ............................................................... 119
5.2.2 Exiting the Sample Table Editor ................................................................. 119
5.2.3 Sample Table Editor Window Components................................................ 120
5.2.4 Sample Table Columns ............................................................................... 121
5.2.5 Sample Window Columns........................................................................... 122
5.2.6 File Types Used........................................................................................... 123
5.3 Creating and Editing Files ....................................................................... 125
5.3.1 Creating a Sample Table ............................................................................. 125
5.3.2 Creating a Calibration Curve File ............................................................... 126
5.3.3 Creating a Method....................................................................................... 133
5.3.4 Creating a Control Sample File................................................................... 139
5.3.5 Creating a Schedule..................................................................................... 145
5.3.6 Reviewing and Editing a Sample Table ...................................................... 146
5.3.7 Reviewing and Editing a Calibration Curve ............................................... 146
5.3.8 Reviewing and Editing a Method................................................................ 152
5.3.9 Reviewing and Editing a Control Sample................................................... 156
5.3.10 Reviewing and Editing a Schedule ............................................................. 157
TOC-LCPH/CPN xix
Table of Contents
5.3.11 Opening an Existing File ............................................................................ 157
5.3.11.1 From the File Viewer ...................................................................... 158
5.3.11.2 From the Tool Bar........................................................................... 158
5.3.11.3 From the File Menu......................................................................... 159
5.4 Editing a Sample Table............................................................................ 160
5.4.1 Inserting a Standard Solution ..................................................................... 160
5.4.2 Inserting a Sample ...................................................................................... 162
5.4.3 Inserting a Control Sample......................................................................... 167
5.4.4 Inserting Multiple Samples with the Same Analysis Parameters............... 168
5.4.5 Inserting a Schedule ................................................................................... 172
5.4.6 Vial Numbers.............................................................................................. 173
5.4.7 Editing Sample Analysis Parameters.......................................................... 177
5.4.8 Copying, Cutting and Pasting Data ............................................................ 180
5.4.9 Deleting a Sample....................................................................................... 182
5.4.10 Adding a Comment to File Information ..................................................... 183
5.5 Reviewing and Editing Measurement Data ............................................. 184
5.5.1 Sample Window ......................................................................................... 184
5.5.1.1 Opening the Sample Window ......................................................... 184
5.5.1.2 Changing the Graph Display........................................................... 185
5.5.1.3 Copy to Clipboard ........................................................................... 187
5.5.2 Reviewing and Editing Sample Analysis Parameters ................................ 187
5.5.3 Reviewing the Calibration Curve .............................................................. 190
5.5.4 Editing the Calibration Curve..................................................................... 191
5.5.5 Excluding Injection Results........................................................................ 192
5.5.6 Recalculating Results ................................................................................. 193
5.5.7 Clearing Analysis Results........................................................................... 194
5.6 Sample Table Data Output and Printing .................................................. 195
5.6.1 Selecting Content to Print........................................................................... 195
5.6.2 Print Setup .................................................................................................. 198
5.6.3 Print Preview .............................................................................................. 199
5.6.3.1 Sample Table Preview..................................................................... 199
5.6.3.2 Sample Report Preview................................................................... 200
5.6.4 Printing ....................................................................................................... 202
5.6.4.1 Sample Table................................................................................... 202
5.6.4.2 Sample Report................................................................................. 203
5.6.5 Selecting Content for ASCII Export........................................................... 204
5.6.6 Exporting to ASCII Format ........................................................................ 207
5.6.7 Exporting a Schedule File .......................................................................... 208
5.6.8 Exporting a Runtime Report....................................................................... 209
5.7 Operation and Analysis............................................................................ 210
5.7.1 Instrument Connection and Disconnection ................................................ 210
5.7.1.1 Connection ...................................................................................... 210
5.7.1.2 Disconnection.................................................................................. 212
5.7.2 Background Monitor .................................................................................. 213
5.7.3 Analysis with an ASI-L or OCT-L............................................................. 216
5.7.4 Analysis without an ASI-L or OCT-L........................................................ 218
5.7.4.1 Single Sample Analysis................................................................... 218
xx TOC-LCPH/CPN
Table of Contents
5.7.4.2 Continuous Analysis ........................................................................ 220
5.7.5 Stopping Analysis ....................................................................................... 221
5.7.5.1 Peak Stop ......................................................................................... 221
5.7.5.2 Stop (after current sample is completed) ......................................... 222
5.7.5.3 Stop (stop all processes immediately) ............................................. 222
5.7.6 Editing the Sample Table during Analysis.................................................. 223
5.7.7 Instrument Shutdown .................................................................................. 224
5.7.7.1 Shutdown ......................................................................................... 224
5.7.7.2 Sleep................................................................................................. 226
5.7.8 Instrument Validation.................................................................................. 228
5.7.9 Maintenance Operations.............................................................................. 233
5.8 Display Options ....................................................................................... 234
5.8.1 Sample Table............................................................................................... 234
5.8.2 Sample Window Display Options............................................................... 236
5.8.3 File Viewer Display Options....................................................................... 239
5.8.4 Setting the Display Font of the Output Window......................................... 240
5.8.5 Display of Selected Windows ..................................................................... 241
5.8.6 Display Font ................................................................................................ 242
5.8.7 Decimal Point Display ................................................................................ 243
5.9 Security Functions ................................................................................... 244
5.9.1 Login ........................................................................................................... 244
5.9.2 Locking the Sample Table Editor ............................................................... 244
5.9.3 Releasing Time Out Lock ........................................................................... 245
5.9.4 Recording the Operation History ................................................................ 246
5.9.5 Other Security Functions............................................................................. 247
5.10 Other Functions ....................................................................................... 248
5.10.1 Default Analysis Parameters ....................................................................... 248
5.10.2 Data Storage Folders ................................................................................... 249
5.10.3 Converting and Outputting Measurement Values....................................... 251
5.10.4 Searching for Files ...................................................................................... 252
5.10.5 File Organization......................................................................................... 253
5.10.6 Online Manual............................................................................................. 256
5.10.6.1 Selecting the Online Manual............................................................ 256
5.10.6.2 Displaying the Online Manual......................................................... 257
5.10.7 Version Information .................................................................................... 257
6 Analysis with Special Options............................................................. 259

6.1 Manual Injection Measurement (H Type Only) ...................................... 260
6.1.1 Analysis Preparation ................................................................................... 260
6.1.1.1 Installation ....................................................................................... 260
6.1.1.2 System Configuration ...................................................................... 261
6.1.2 Measurement ............................................................................................... 262
6.1.2.1 Calibration Curve Measurement...................................................... 262
6.1.2.2 Sample Measurement....................................................................... 263
6.1.3 Precautions for Low Concentration Samples.............................................. 264
6.1.4 Manual Injection Kit Maintenance.............................................................. 265
TOC-LCPH/CPN xxi
Table of Contents
6.1.4.1 Replacing the IC Injection Port Septum (Cushion O-Ring)............ 265
6.1.4.2 Gas-Tight Syringe ........................................................................... 265
6.2 Gas Sample Analysis ............................................................................... 266
6.2.1 Precautions for Gas Sample Analysis......................................................... 266
6.2.2 Analysis Preparation................................................................................... 266
6.2.2.1 Installation of the Manual Injection Kit .......................................... 266
6.2.3 Measurement .............................................................................................. 267
6.2.3.1 Calibration Curve ............................................................................ 267
6.2.3.2 Sample Measurement ...................................................................... 268
6.2.4 Manual Injection Kit Maintenance............................................................. 269
6.2.4.1 Replacing the IC Injection Port Septum (Cushion O-Ring)............ 269
6.2.4.2 Gas-Tight Syringe ........................................................................... 270
7 Maintenance......................................................................................... 271
7.1 Daily Inspection ....................................................................................... 272
7.1.1 Checking Dilution Water............................................................................ 272
7.1.2 Checking Acid ............................................................................................ 272
7.1.3 Checking Drain Vessel Water Level .......................................................... 272
7.1.4 Checking Humidifier Water Level ............................................................. 273
7.1.5 Inspecting the Liquid in the B-Type Halogen Scrubber (Option) .............. 274
7.2 Periodic Inspections ................................................................................. 275
7.2.1 Catalyst Regeneration................................................................................. 275
7.2.2 Washing or Replacing Catalyst .................................................................. 277
7.2.3 Replacing the Carrier Gas Purification Tube and Catalyst ........................ 279
7.2.4 Washing/Replacing the Combustion Tube
and Carrier Gas Purification Tube (Option) ............................................... 281
7.2.5 Replacing the High Purity Air (Filling the Cylinder)................................. 281
7.2.6 Replacing the CO2 Absorber ...................................................................... 281
7.2.7 Replacing the Halogen Scrubber ................................................................ 281
7.2.8 Syringe Replacement.................................................................................. 283
7.2.9 Syringe Plunger Tip Replacement.............................................................. 286
7.2.10 Replacing the Sliding Sample Injector O-rings.......................................... 287
7.2.11 Replacing the Syringe Pump 8-port Valve Rotor....................................... 288
7.2.12 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier........... 290
7.2.13 Replenishing IC Reaction Solution ............................................................ 291
7.2.14 Replacing the Pump Head of the IC Reaction Solution Pump................... 292
7.2.15 Replacing the Filler of the Optional POC Analysis CO2 Absorber ........... 293
7.2.16 Replacing the Liquid in the B-Type Halogen Scrubber (Option) .............. 294
7.3 Autosampler (ASI-L) Maintenance ......................................................... 295
7.3.1 Rinse Bottle Inspection............................................................................... 295
7.3.2 Sample Catcher Inspection ......................................................................... 295
7.3.3 Replacing the Pump Head of the Rinse Pump............................................ 296
7.4 8-Port Sampler (OCT-L) Maintenance .................................................... 297
7.4.1 Replacing the 8-Port Valve Rotor .............................................................. 297
7.5 TN Unit (TNM-L) Maintenance .............................................................. 299
7.5.1 Replacing the Catalyst in the Ozone Treatment Unit................................. 299
xxii TOC-LCPH/CPN
Table of Contents
7.5.2 Inspecting the Chemiluminescence Detector
and Replacing the Ozone Generator ........................................................... 301
7.5.3 Replacing the NOx Absorber ...................................................................... 303
7.6 Maintenance Menus................................................................................. 304
7.7 Troubleshooting....................................................................................... 311
7.7.1 Error Messages............................................................................................ 311
7.7.2 Troubleshooting .......................................................................................... 318
7.7.2.1 TOC-L.............................................................................................. 318
7.7.2.2 ASI-L ............................................................................................... 323
7.7.2.3 OCT-L, 8-Port Sampler ................................................................... 324
7.7.2.4 Corrective Actions for Poor Reproducibility................................... 325
7.7.2.5 Corrective Action for Combustion Tube Breakage
Inside the Electric Furnace .............................................................. 327
8 Reference Information......................................................................... 329

8.1 Principles of Analysis.............................................................................. 330
8.1.1 Principles of TC (Total Carbon) Analysis .................................................. 330
8.1.2 Principles of IC (Inorganic Carbon) Analysis............................................. 331
8.1.3 Principles of NPOC (Non-Purgeable Organic Carbon) Analysis ............... 332
8.1.4 Principles of POC (Purgeable Organic Carbon) Analysis .......................... 333
8.1.5 Principles of Measuring TOC ..................................................................... 334
8.1.6 Principles of Measuring TN (Total Nitrogen)............................................. 334
8.2 Analysis-Related Technical Information................................................. 335
8.2.1 Peak Area Analysis ..................................................................................... 335
8.2.2 Peak Shape .................................................................................................. 335
8.2.3 Calibration Curves ...................................................................................... 336
8.2.3.1 Types of Calibration Curves ............................................................ 336
8.2.3.2 Shifting of Calibration Curves......................................................... 336
8.2.4 Sparging During Standard Solution Analysis ............................................. 338
8.2.5 Automatic Selection of Optimum Calibration Curve.................................. 338
8.2.6 Automatic Correction for Injection Volume and Dilution Factor............... 340
8.2.7 Multi-Stage Injection .................................................................................. 340
8.2.8 Pharmaceutical Water Testing .................................................................... 341
8.2.8.1 USP (United States Pharmacopeia) and
EP (European Pharmacopoeia) Support .......................................... 341
8.2.8.2 JP (Japanese Pharmacopoeia) Support ............................................ 341
8.3 Specifications........................................................................................... 342
8.3.1 TOC-LCPH/CPN ........................................................................................... 342
8.3.2 ASI-L........................................................................................................... 343
8.3.3 OCT-L 8-Port Sampler................................................................................ 343
8.3.4 TNM-L ........................................................................................................ 343
8.3.5 POC Measurement Kit ................................................................................ 344
8.3.6 Carrier Gas Purifier Kit............................................................................... 344
8.3.7 Manual Injection Kit (Gas Sample Injection Kit) ....................................... 344
8.3.8 B-Type Halogen Scrubber........................................................................... 345
8.3.9 External Sparge Kit ..................................................................................... 345
8.3.10 Recommended PC Specifications ............................................................... 346
TOC-LCPH/CPN xxiii
Table of Contents
8.4 Standard Accessories ............................................................................... 347
8.5 Special Accessories.................................................................................. 349
8.6 Consumable Parts List ............................................................................. 351
8.6.1 Consumable Parts List................................................................................ 351
8.6.2 Recommended Consumable Part Replacement Period .............................. 354
8.7 Maintenance Parts List............................................................................. 355
8.8 Installation................................................................................................ 357
8.8.1 Before Installation ...................................................................................... 357
8.8.2 Installation Site........................................................................................... 357
8.8.2.1 Installation Site Selection................................................................ 357
8.8.2.2 Installation Site Conditions ............................................................. 358
8.8.3 Installation Procedure................................................................................. 359
8.8.3.1 Connecting Power Supply and Ground........................................... 359
8.8.3.2 Changing the Power Supply Voltage .............................................. 360
8.8.3.3 Connecting Gas ............................................................................... 360
8.8.3.4 Installing the Drain Container......................................................... 363
8.8.3.5 Connecting to the PC Using the Provided Cable ............................ 364
8.8.4 Installing the ASI-L.................................................................................... 364
8.8.5 OCT-L Installation ..................................................................................... 370
8.8.6 Installing the TNM-L ................................................................................. 373
8.8.6.1 TNM-L TN Unit Installation........................................................... 373
8.8.6.2 Connecting Ozone Source Air ........................................................ 373
8.8.6.3 Connecting Gas Exhaust Tubing..................................................... 375
8.9 Material Safety Data Sheets..................................................................... 376
8.9.1 Hydrochloric Acid (HCl)............................................................................ 376
8.9.2 Phosphoric Acid ......................................................................................... 379
8.9.3 IC Reagent .................................................................................................. 382
8.9.4 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime .................................. 385
8.9.5 Ceramic Fiber ............................................................................................. 388
8.9.6 Halogen Scrubber ....................................................................................... 390
8.9.7 High Sensitivity Catalyst............................................................................ 391
8.9.8 Normal Sensitivity Catalyst........................................................................ 392
Appendix A Control Charts ....................................................................... 393

A.1 File Menu ................................................................................................. 394
A.1.1 New............................................................................................................. 394
A.1.2 Following Control Chart............................................................................. 398
A.1.3 Open ........................................................................................................... 399
A.1.4 Save ............................................................................................................ 399
A.1.5 Save As....................................................................................................... 399
A.1.6 Print>Data................................................................................................... 399
A.1.7 Print>Graph ................................................................................................ 399
A.1.8 Print Preview>Data/Print Preview>Graph ................................................. 399
A.1.9 Print Setup .................................................................................................. 400
A.1.10 Page Setup .................................................................................................. 400
A.1.11 Exit ............................................................................................................. 402
xxiv TOC-LCPH/CPN
Table of Contents
A.2 Edit Menu ................................................................................................ 403
A.3 View Menu .............................................................................................. 404
A.3.1 Statistics ...................................................................................................... 404
A.3.2 Comparison ................................................................................................. 405
A.3.3 Out of Control Events ................................................................................. 406
A.3.4 Toolbar/Status Bar ...................................................................................... 406
A.4 Options Menu .......................................................................................... 407
A.4.1 Control Chart Options ................................................................................. 407
A.4.2 Font ............................................................................................................. 407
A.4.3 Floating Point Numbering Format .............................................................. 408
A.4.4 ASCII Export Options................................................................................. 409
A.4.5 Enable Exclusion......................................................................................... 409
A.5 Help Menu ............................................................................................... 410
TOC-LCPH/CPN xxv
Table of Contents
xxvi TOC-LCPH/CPN
1
1Overview
This chapter provides an overview of the instrument and operational precautions for its
use.
1.1 Overview
Provides an overview of the TOC-LCPH/TOC-LCPN instrument.
1.2 Operational Precautions
Lists precautions necessary to ensure that the instrument is used correctly.
1.1 Overview
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 JIS1 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))
CAUTION
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.
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 D2575, Standard Methods for
Examination of Water and Waste Water 5310B
2 TOC-LCPH/CPN
Take the following precautions when using this instrument.
CAUTION
• 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.
TOC-L Drain tubing (Tubing

placement should be as
indicated by the solid line.)
Drain container
(Supplied by user.)
Figure 1.1 External Drain Tubing
TOC-LCPH/CPN 3
• 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>
• 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 “ 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 discharged Never turn the lever

to the front of the IC to this position.
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>
• 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 Section 8.9 "Material Safety Data Sheets".
4 TOC-LCPH/CPN
• 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.
• 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.
TOC-LCPH/CPN 5
6 TOC-LCPH/CPN
2
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.
2.2 Autosampler ASI-L (Option)

This section shows the construction of the ASI-L unit using front and rear views
depicted diagonally from the left.
2.3 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.
2.4 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.
2.1.1 Front View
Power switch (with LED)
Indicator
Front door
Indicator
Figure 2.1 Front View
2.1.2 Right Side View
Main power switch
Front door
Figure 2.2 Right Side View
8 TOC-LCPH/CPN
2.1.3 Left Side View
Sampling tubing
Front door
Drain pot IC reagent Hydrochloric Diluent bottle Drain tubing

acid
Figure 2.3 Left Side View
TOC-LCPH/CPN 9
2.1.4 Rear View
AC cord socket
Carrier gas inlet
Dip switches for various settings
PC connection socket
ASI-L/OCT-L connection socket Extension board slot covers
Figure 2.4 Rear View
10 TOC-LCPH/CPN
2.1.5 Front Internal View (Left Diagonal)
Sparge gas flow meter

(option)
Sliding IC sample injector
(H Type only)
Sparge gas flow
adjustment knob (option)
IC reaction vessel Carrier gas pressure

(H Type only) adjustment knob (option)
3-way tap
8-port valve Halogen scrubber
5 mL syringe Humidifier
Cooling tubing unit
Solenoid valve (for IC drainage) Pump (for IC reagent supply)

(H Type only) (H Type only)
Figure 2.5 Front Internal View (Left Diagonal)
2.1.6 Top Internal View (Left Diagonal)
Cooling fan for the

sample injector block
Motor for driving
the slider
Sample injector block
Figure 2.6 Top Internal View (Left Diagonal)
TOC-LCPH/CPN 11
2.1.7 Flow Diagram
Diluent
IC Reaction
Backflow Vessel
IC Reagent
Prevention Trap
Supply Pump
Acid
Solenoid
Valve 3
(To Drain)
Light Source
Sample
Sliding TC
Backflow Sample IC Reagent Phosphoric
Prevention Injector Acid
Valve
CO2 Absorber
NDIR Tandem Cell
(Sample Cell)
Halogen Scrubber
5 mL Syringe
Dehumidifier Membrane Filter Detector
(Electronic Cooler)
Pure Water Trap
TC Combustion
Pressure Sensor PS3 Tube
Proportional Valve 2
Drain Pot
Cooling Tubing
Pressure Proportional Pressure
Solenoid Valve 1 Sensor PS1 Valve 1 Sensor PS2 Humidifier
Carrier Gas
Inlet
Figure 2.7 Flow Diagram (TOC-LCPH)
Diluent IC Reaction
Backflow Vessel
IC Reagent
Prevention Trap Supply Pump
Acid
Solenoid
Valve 3
(To Drain)
Light Source
Sample Chemiluminescence
Sliding TC Phosphoric Detector
IC Reagent
Backflow Sample Acid
Prevention Valve Injector
NDIR Tandem
Cell (Sample
Cell) Ozone
Generator
Halogen Scrubber
5 mL Syringe
Ozone
Membrane Detector
Dehumidifier Treatment
Filter
(Electronic Cooler) Unit
Pure Water Trap

Pressure Sensor PS3 Exhaust
TC Combustion Pressure
Tube Sensor PS5
Drain Pot
Pressure NOx Absorber
Solenoid Pressure Proportional Sensor Regulator
Valve 1 Sensor PS1 Valve 1 Cooling Tubing
Carrier PS2
Gas Inlet Humidifier
Solenoid
Valve
Flow Meter
with Valve Solenoid Carrier
Sample or ASI Valve 6 Gas Inlet
TNM External Sparge Kit
Figure 2.8 Flow Diagram (TOC-LCPH + TNM-L + External Sparge Kit)
12 TOC-LCPH/CPN
Diluent
IC Reaction
Vessel
IC Reagent
Backflow
Supply Pump
Prevention Trap
Acid
Solenoid
Valve 3
(To Drain)
Light Source
Sample
Sliding TC Phosphoric
Backflow Sample Injector IC Reagent Acid
Prevention
Valve
CO2 Absorber
NDIR Tandem
CO2 Absorber
Cell (Sample
Halogen Scrubber Cell)
5 mL Syringe
Dehumidifier Membrane Filter Detector
Oxygen (Electronic Cooler)
Permeation Tubing
N2 Carrier Gas Kit Pure Water Trap
TC Combustion
Tube
Pressure Sensor PS3

Drain Pot
Proportional Valve 2 Cooling Tubing
Pressure Proportional Pressure Humidifier

Solenoid Valve 1
Sensor PS1 Valve 1 Sensor PS2
Carrier Gas Inlet
Figure 2.9 Flow Diagram (TOC-LCPH + N2 Carrier Gas Kit)
IC Reaction
Vessel
Backflow
Diluent IC Reagent
Prevention Trap Supply Pump
4 5 Solenoid Valve 4
Acid
3 P
6
2 Solenoid
Sample or ASI 7 Valve 3
1 8 (To Drain)
Light Source
Phosphoric
Sliding TC IC Reagent
Solenoid Valve 2 CO2 Absorber Acid
Backflow Sample Injector
(For Sparging)
Prevention CO2 Absorber
Valve
NDIR Tandem
Cell (Sample
Halogen Scrubber Cell)
5 mL Syringe
Dehumidifier Detector
Membrane Filter
(Electronic Cooler)
Pure Water Trap
Pressure Sensor PS3 TC Combustion

Tube
Drain Pot
Pressure Proportional Pressure

Humidifier Cooling Tubing
Solenoid Valve 1 Sensor PS1 Valve 1 Sensor PS2
Carrier Gas Inlet
Figure 2.10 Flow Diagram (TOC-LCPH + POC Kit)
TOC-LCPH/CPN 13
Manual IC Gas
Injector
Diluent
IC Reaction
Backflow Vessel
Prevention Trap IC Reagent
Supply Pump
Acid
Solenoid
Manual TC
Valve 3
Gas Injector
(To Drain)
Light Source
Sample
Sliding TC Phosphoric
Backflow IC Reagent
Sample Acid
Prevention
Injector
Valve
CO2 Absorber
NDIR Tandem
Cell (Sample
Cell)
Halogen Scrubber
5 mL Syringe
Detector
Dehumidifier Membrane
(Electronic Cooler) Filter
Pure Water Trap
TC Combustion
Pressure Sensor PS3 Tube
Proportional Valve 2 Drain Pot
Cooling Tubing
Pressure Proportional Pressure Humidifier
Carrier Gas Inlet
Figure 2.11 Flow Diagram (TOC-LCPH + Manual Injection Kit)
Diluent
Acid
Light Source
Sample
Sliding TC
Solenoid Valve 2
Backflow Sample
(For Sparging)
Prevention Injector CO2 Absorber
Valve NDIR Tandem
Cell (Sample
Cell)
Halogen Scrubber
5 mL Syringe
Membrane Filter Detector
Dehumidifier
(Electronic Cooler)
Pure Water Trap
Pressure Sensor PS3

TC Combustion
Tube
Drain Pot
Pressure Proportional Pressure Humidifier Cooling Tubing

Carrier Gas Inlet
Figure 2.12 Flow Diagram (TOC-LCPN)
14 TOC-LCPH/CPN
Diluent
Acid
Light Source
Sliding TC
Backflow Detector
Sample
Solenoid Valve 2 Prevention
Injector
(For Sparging) Valve
NDIR Tandem
Cell (Sample
Ozone
Cell)
Generator
Halogen Scrubber
5 mL Syringe
Membrane Detector Ozone
Dehumidifier Filter Treatment
Pure Water Trap
Pressure Sensor PS3 Exhaust
TC Combustion Pressure
Tube Sensor PS5
Pressure
NOx Absorber
Solenoid Pressure Proportional Sensor Drain Pot Regulator
Cooling Tubing
Valve 1 Sensor PS1 Valve 1 PS2
Carrier
Humidifier
Gas Inlet
Solenoid
Valve
Flow Meter
With Valve Solenoid Carrier Gas Inlet
Sample or ASI Valve 6
External Sparge Kit
Figure 2.13 Flow Diagram (TOC-LCPN + TNM-L + External Sparge Kit)
Solenoid
Valve 4
Diluent
Acid
Light Source
Sample
Solenoid Valve 2 Sliding TC

Backflow Sample
(For Sparging)
Prevention Injector CO2 Absorber
Valve NDIR Tandem
Cell (Sample
Cell)
Halogen Scrubber
5 mL Syringe
Membrane Filter Detector
Dehumidifier
(Electronic Cooler)
Pure Water Trap
Pressure Sensor PS3

TC Combustion
Tube
Drain Pot
Pressure Proportional Pressure Humidifier Cooling Tubing

Carrier Gas Inlet
Figure 2.14 Flow Diagram (TOC-LCPN + POC Kit)
TOC-LCPH/CPN 15
Diluent
Acid
Light Source
Sliding TC
Backflow Detector
Sample
Solenoid Valve 2 Prevention Injector
(For Sparging) Valve
NDIR Tandem
Pure Water Trap
Cell (Sample Ozone
Cell) Generator
Halogen Scrubber
5 mL Syringe
Membrane Detector Ozone
Filter Treatment
Dehumidifier
Exhaust
Pressure Sensor PS3 TC Pressure
L-Shaped Combustion Sensor PS5
Combustion Tube
Tube
NOx Absorber
Drain Pot Regulator
Pressure Cooling Tubing
Solenoid Pressure Proportional Sensor
Valve 1 Sensor PS1 Valve 1 PS2
Humidifier Solenoid
Valve
Carrier
Gas Inlet
Carrier Gas Inlet
Carrier Gas Purification Kit
CO2 Absorber
Figure 2.15 Flow Diagram (TOC-LCPN + TNM-L + Carrier Gas Purification Kit)
16 TOC-LCPH/CPN
2.2.1 Front View (Left Diagonal)
Sparging tubing (option)
Sampling tubing
Door for needle replacement
Power switch
Sample cover
Figure 2.16 Front View (Left Diagonal)
2.2.2 Rear View (Left Diagonal)
Rinse bottle
Stirrer rotation speed
adjustment dial (option)
Drain tubing Tubing to supply rinse water

Connection cable
Figure 2.17 Rear View (Left Diagonal)
TOC-LCPH/CPN 17
2.3.1 Front View (Left Diagonal)
8-port valve
Figure 2.18 Front View (Left Diagonal)
2.3.2 Rear View (Right Diagonal)
Connection cable
Connection cable
(For linking to the OCT-L)
Figure 2.19 Rear View (Right Diagonal)
18 TOC-LCPH/CPN
2.4.1 Front View (Right Diagonal)
TNM-L
TNM-L maintenance door
Figure 2.20 Front View (Right Diagonal)
2.4.2 View Inside the Door on the Right Side
Flow rate adjustment

knob for ozone air
source
Figure 2.21 View Inside the Door on the Right Side
TOC-LCPH/CPN 19
2.4.3 Rear View
Ozone air source inlet
Figure 2.22 Rear View
20 TOC-LCPH/CPN
3
3Preparation 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

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 Section 3.1.1.1 "Catalyst for TOC Analysis" on
page 23. For TOC/TN catalyst filling, follow the procedure in Section 3.1.1.2 "TOC/TN
Catalyst (Option)" on page 25.
CAUTION
Exercise caution when handling the combustion tube to prevent breakage, as it is
made of quartz glass.
Note: 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.
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
Section 3.1.18.2 "TC Blank Check Analysis" on page 64.
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.
22 TOC-LCPH/CPN
3.1.1.1 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.
Note: 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.
3. Fill the TOC standard catalyst to a height of about 100 mm.
Combustion tube
TOC standard catalyst
100 mm
Quartz wool
Platinum mesh
Figure 3.1 Combustion Tube with TOC Standard Catalyst
CAUTION
Take care not to inhale any quartz wool when filling the combustion tube.
TOC-LCPH/CPN 23
¬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.
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.
Combustion tube
TOC high-sensitivity
catalyst
110 mm
Platinum mesh
Figure 3.2 Filling of TOC Combustion Tube with High Sensitivity Catalyst
24 TOC-LCPH/CPN
3.1.1.2 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. 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.
5. Lightly press down on the ceramic fiber using the catalyst filling rod to attain a
thickness of 10 mm.
Note: • 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
Combustion tube
140 mm
Ceramic fiber 10 mm
TOC standard catalyst
Quartz wool
Platinum mesh
Figure 3.3 Filling Combustion Tube with Catalyst for TOC/TN Analysis
TOC-LCPH/CPN 25
CAUTION
Take care not to inhale any quartz wool or ceramic fiber when filling the
combustion tube.
3.1.2 Installing the Cooling Tube Unit (H Type Only)

Install the cooling tube unit to the outlet of the combustion tube.
CAUTION
• 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.
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.
To the pure water trap
Cooling tube unit outlet

(PTFE coupling)
Fastening
screws
Cooling tubing unit
Figure 3.4 Installing the Cooling Tube Unit
26 TOC-LCPH/CPN
3.1.3 Connecting the Combustion Tube

The installation procedure for the combustion tube differs for the H Type and N Type
instruments.
CAUTION
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.
3. Loosen the two knurled screws on the sample injector and remove the sample injector
in the upward direction.
Slider retaining
screw
Slider
Sample injector retaining screws Carrier gas

(two) introduction tubing
Hexagon cap nut
Sample injector
Drain tubing
Figure 3.5 Sample Injector
TOC-LCPH/CPN 27
4. Securely insert the top end of the combustion tube filled with catalyst into the hole on
the bottom of the sample injector.
5. Fit the combustion tube into the hole in the center of the electric furnace and then
insert the bottom end of the combustion tube into the PTFE coupling of the cooling
tubing inlet. At this point, securely connect the drain tubing, which protrudes out of
the sample injector, to the Y-shaped fitting.
Sample injector
Drain tubing
Combustion
tube
Y-shaped fitting
Figure 3.6 Installing the Combustion Tube
6. Secure the sample injector to the instrument body using the knurled screws.
28 TOC-LCPH/CPN
7. Reattach the slider and carrier gas introduction tubing to their original positions.
Sample injector
Drain tubing
Sample injector retaining screws
Figure 3.7 Securing the Sample Injector to the Instrument Body
Note: Do not allow organic substances, such as grease or oil, to contaminate any parts
exposed to gas including the inner surfaces on the tip of the combustion tube as
well as joints. This is especially important for high sensitivity measurement.
8. Connect the bottom of the combustion tube to the PTFE coupling of the cooling
tubing inlet. Carefully tighten the hexagon cap nut while holding the PTFE coupling
in place with your finger.
Combustion tube
Cooling tubing unit
PTFE coupling
(cooling tubing inlet)
Figure 3.8 Connecting the Combustion Tube and Cooling Tubing
TOC-LCPH/CPN 29
Bottom end of the

combustion tube
Hexagon cap nut
PTFE coupling
Cooling tubing inlet
Figure 3.9 Connecting the Bottom End of the Combustion Tube to the PTFE Coupling
CAUTION
The quartz glass combustion tube will break if the hexagon cap nut is
overtightened.
Tightening the PTFE coupling without holding it in place will break the cooling
tubing because it is made of hard glass.
9. In order to prevent heat from escaping from the furnace, use the provided quartz wool
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.
CAUTION
Combustion tube
Electric furnace
Quartz wool
Figure 3.10 Filling With Quartz Wool (Bottom of the Electric Furnace)
30 TOC-LCPH/CPN
Fill with quartz wool Insulator
Figure 3.11 Filling With Quartz Wool (Top of the Electric Furnace)
TOC-LCPH/CPN 31
Installation for the N Type

sample injector.
in the upward direction.
Slider retaining
screw
Slider

Hexagon cap nut
Sample injector
Drain tubing
4. Securely insert the top end of the combustion tube filled with catalyst into the hole on
the bottom of the sample injector.
32 TOC-LCPH/CPN
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.
Sample injector
Drain tubing
Combustion
tube
Y-shaped fitting
Figure 3.13 Installing the Combustion Tube
6. Secure the sample injector to the instrument body using the knurled screws.
TOC-LCPH/CPN 33
7. Reattach the slider and carrier gas introduction tubing to their original positions.
Sample injector
Drain tubing
Sample injector retaining screws
Figure 3.14 Securing the Sample Injector to the Instrument Body
Note: 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.
CAUTION
• The quartz glass combustion tube will break if the compression fitting is over-
tightened.
34 TOC-LCPH/CPN
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.
Cooling tubing PTFE coupling (Connects to the

bottom end of the combustion tube.)
Figure 3.15 Connecting the Combustion Tube and Cooling Tubing
9. In order to prevent heat from escaping from the furnace, use the provided quartz wool
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.
CAUTION
Combustion tube
Electric furnace
Quartz wool
Figure 3.16 Filling With Quartz Wool (Bottom of the Electric Furnace)
TOC-LCPH/CPN 35
Fill with quartz wool Insulator
Figure 3.17 Filling With Quartz Wool (Top of the Electric Furnace)
CAUTION
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 is
measured and is proven to be sufficiently low with respect to the maximum permissible
dust concentration level.
36 TOC-LCPH/CPN
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.
Replace Scrubber When

Discoloration Band Reaches
Gas Flow Direction this Point
Dehumidifier To Sample
Cell Inlet
Halogen Reactant-filled Cylinder
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.
Halogen scrubber
(take note of the
arrow direction)
Figure 3.19 Halogen Scrubber Connection
TOC-LCPH/CPN 37
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.
CAUTION
• 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.
• 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.
3.1.5.1 Syringe Installation
The syringe is installed according to the following procedure.

Note: A system configuration must be created before syringe installation. Refer to
Section 5.1.1 "Creating a New System Configuration" on page 110 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.
Reference: The procedure for opening the Sample Table Editor is described in Section 5.2.1 "Opening
the Sample Table Editor" on page 119.
2. Right-click on the appropriate instrument icon in the Sample Table tab of the file
viewer, and click Connect.
38 TOC-LCPH/CPN
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.
TOC-LCPH/CPN 39
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.
8-port valve
Syringe
Plunger Plunger retaining screw
Plunger holder
Figure 3.20 Installing the Syringe
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.
CAUTION
• 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.
40 TOC-LCPH/CPN
8. Click Finish Replacement. The syringe pump zero point detection operation is
executed automatically.
9. Click Close.
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. 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.
CAUTION
Do not bend drain tubing, as this may prevent drain discharge.
Rubber cap Drain discharge tubing
Cooler drain vessel
Figure 3.21 Filling the Cooler Drain Vessel with Water
TOC-LCPH/CPN 41
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.
Note: Use pure water that contains as little TC as possible when
performing high sensitivity measurement.
Water supply port
Humidifier
Figure 3.22 Filling the Humidifier with Water
42 TOC-LCPH/CPN
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. 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.
Note: Verify that the tip of the intake tubing nearly reaches the bottom of
the container.
Dilution water
intake tubing
Dilution water bottle
Figure 3.23 Preparing Dilution Water
About pure water:

• Use the purest water that can be obtained.
• Refer to Section 3.1.17.1 "Preparation of Standard Solutions" on page 59 for details
on the degree of purity of "pure water".
TOC-LCPH/CPN 43
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.
CAUTION
Hydrochloric acid is a hazardous chemical. Use precautions to avoid contact
when handling this substance. For details, refer to Section 8.9 "Material Safety
Data Sheets" on page 376.
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.
5. Place the cap on the container.
Note: Verify that the tip of the acid intake tubing nearly reaches the
bottom of the container.
Acid intake tubing
Acid container (250 mL capacity)
Figure 3.24 Acid Preparation
44 TOC-LCPH/CPN
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.
Note: The flexible tubing should not be bent.
3. Place the CO2 absorber in the holder on the upper rear of the instrument.
Connect to
the absorber
CO2 absorber
Figure 3.25 Installation of the CO2 Absorber
TOC-LCPH/CPN 45
3.1.11 Adjusting Sparge Gas Flow Rate

The gas flow rate must be adjusted before conducting sparging during measurement.
Adjustment Procedure
46 TOC-LCPH/CPN
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.
Click Open for Ext. Sparge.
4. 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.
Note: Adjust the flow rate to suit the size and shape of the sample
container. A flow rate of about 100 mL/min is appropriate.
TOC-LCPH/CPN 47
Sparge gas flow

adjustment knob
Figure 3.26 Adjusting the Sparge Gas Flow Rate
5. Close the front door of the instrument.

6. Click Close for Ext. Sparge and then click OK to close the window.
48 TOC-LCPH/CPN
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)
CAUTION
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.
Note: During analysis, verify that the sample flow is normal. Refer to
Section 7.7.2.4 "Corrective Actions for Poor Reproducibility" on
page 325
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.
¬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.
TOC-LCPH/CPN 49
For TOC-L+ASI-L (TOC-L and ASI-L)

Refer to Section 8.8.4 "Installing the ASI-L" on page 364 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 Section 3.1.18.4 "Analysis of Samples
Containing Suspended Solids" on page 67.
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.
50 TOC-LCPH/CPN
3.1.13 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.
CAUTION
The IC reagent contains corrosive phosphoric acid. Always handle acid with care to prevent
spills and contact with the skin. For details, refer to Section 8.9 "Material Safety Data
Sheets" on page 376.
¬Preparation and Placement of the IC Reagent
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.
¬Replenishing IC Reaction Vessel with IC Reagent

Use the following procedure to replenish the IC reagent.
TOC-LCPH/CPN 51
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
Connection is established with the Sample Table Editor, and the Ready indicator
illuminates.
52 TOC-LCPH/CPN
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.
TOC-LCPH/CPN 53
3.1.14 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.
CO2 absorber for

POC analysis
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.
Note: 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.
6. Install the CO2 absorber for POC analysis in the original position.
54 TOC-LCPH/CPN
CAUTION
• 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.
Cap
Nipple
O-Ring
Lithium hydroxide
Quartz wool
Figure 3.29 Preparing the CO2 Absorber for POC Analysis
3.1.15 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.
3.1.15.1 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.
TOC-LCPH/CPN 55
Note: Make sure there are no kinks in the flexible tubing.
L S
L S
Connect to the absorber
NOx absorber
Figure 3.30 Connecting the NOx Absorber
3.1.16 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
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).
Note: 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.
56 TOC-LCPH/CPN
Preparation Procedure
1. Prepare 0.05 mol/L hydrochloric acid by either diluting 1 mol/L hydrochloric acid
with 40 parts pure water or diluting concentrated hydrochloric acid (12 mol/L) with
240 parts pure water. A concentration accuracy of approximately ±2 % is acceptable.
As a guide, the TOC value of the pure water used for dilution should be less than
0.5 mg/L.
2. Release the clamps that secure the B-type halogen scrubber in place, remove the B-
type halogen scrubber from the instrument, and open the screw cap.
B-type halogen
scrubber
Figure 3.31 Removing the B-Type Halogen Scrubber
TOC-LCPH/CPN 57
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.
Screw cap
0.05 mol/L hydrochloric acid
Stainless mesh for absorption
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.
CAUTION
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 Section 8.9
"Material Safety Data Sheets" on page 376.
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.
58 TOC-LCPH/CPN
3.1.17 Preparation and Storage of Standard Solutions
3.1.17.1 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.
Note: 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.
Note: • 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.
4. Accurately dilute this standard stock solution with zero water to prepare standard
solutions at the required concentrations.
Note: • 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.
TOC-LCPH/CPN 59
• 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

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.
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.
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.
60 TOC-LCPH/CPN
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.
The hydrochloric acid concentration will be about 0.05 M after dilution.
3.1.17.2 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.
Note: 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.
3.1.18 Sample Preparation
3.1.18.1 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.
TOC-LCPH/CPN 61
¬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.
Note: Exercise caution with plastic containers, as elution of TOC-containing
components can occur.
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.
• 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.
62 TOC-LCPH/CPN
¬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.
¬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.
TOC-LCPH/CPN 63
¬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.
3.1.18.2 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.
Note: Practically no blank peaks are generated in the IC measurement. Also, because
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.
Note: Do not enter anything into the Sample Table. The blank check sample will be
inserted automatically upon completion of the blank check setup operation.
Reference: Refer to Section 5.1.1 "Creating a New System Configuration" on page 110 to set up a new
system configuration. Refer to Section 5.3.1 "Creating a Sample Table" on page 125 to
create a Sample Table.
2. Press Connect to establish communication between the Sample Table Editor and the
instrument.
Reference: Refer to Section 5.7.1.1 "Connection" on page 210 to connect the Sample Table Editor to
the Instrument.
64 TOC-LCPH/CPN
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.
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.
TOC-LCPH/CPN 65
• 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.
7. Fill the dilution water bottle to capacity with distilled water, and place it in the
specified position.
Note: 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.
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.
Note: 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.
3.1.18.3 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.
66 TOC-LCPH/CPN
Sparge Sequence
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 Section 3.1.11 "Adjusting Sparge Gas Flow Rate" on page 46 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.
Note: 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.
3.1.18.4 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.
TOC-LCPH/CPN 67
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
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.
3.1.18.5 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.
68 TOC-LCPH/CPN
Acid
Dilution to a concentration of 1000 mg/L or less is desirable for acids. Concentrations up to
5000 mg/L can be used if this level of dilution cannot be attained. Note that there are also
methods to reduce the acidity of hydrochloric acid or sulfuric acid to a more neutral pH of 2
to 3 using potassium hydroxide or sodium hydroxide. This process produces thermally
stable sodium chloride or sodium sulfate, which prevent the generation of acidic gas during
sample combustion. Acid neutralization should be stopped at a pH of about 2 to 3 and TOC
direct analysis (NPOC analysis) should then be performed after sparging to remove any IC.
It is necessary to consider the TOC associated with impurities contained in the alkali
reagents used for neutralization. All salts of nitric acid generate acidic gas under thermal
decomposition; as a result, neutralization is ineffective. When the sample contains
hydrochloric or hypochlorous acid, hydrochloric acid gas is generated from salts that are
readily subject to thermal decomposition, such as ammonium chloride, calcium chloride
and magnesium chloride. The instrument is equipped with a halogen scrubber; however, the
scrubber's main function is absorb hydrochloric acid gas generated by corrosion of the gold
plating on the internal surface of the NDIR cell.
Alkaline samples
When performing TC analysis on alkaline samples, the following problems can arise:
• Rapid decrease in sensitivity and loss of reproducibility
• Rapid degradation of catalyst or wear of the combustion tube
• Likelihood that IC will be high due to absorption of carbon dioxide
For these reasons, the NPOC analysis is suitable for alkaline samples.
In NPOC analysis, dilute hydrochloric acid is added first to adjust the solution to a pH of 2
to 3. This causes a reaction that generates salt. For example, calcium chloride will be
formed as a salt if the sample contains calcium hydroxide as the base. Since it is preferable
for this salt concentration to be low, alkaline samples should be diluted as much as possible.
Salt accumulation
Samples should be diluted as much as possible to reduce the salt concentration and extend
the life of the combustion tube and catalyst. Conducting a large number of analyses on
samples containing salts will allow the salts to accumulate in the combustion tube,
gradually increasing resistance to the flow of carrier gas and resulting in decreased analysis
reproducibility. When decreased reproducibility is observed, perform the combustion tube
maintenance procedure described in Section 7.2.4 "Washing/Replacing the Combustion
Tube and Carrier Gas Purification Tube (Option)" on page 281.
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.
TOC-LCPH/CPN 69
3.1.19 Sample Preparation for Autosampler Measurement
3.1.19.1 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
Vial Type Sample Volume Sample Volume When Sparging ASI-L Vials
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
Note: • Note 1: Sample volume when sample is introduced up to about 17 mm from

the top of the vial.
• Note 2: Sample volume when sample is introduced up to about 10 mm from
the top of the vial.
• Note 3: Sample volume when sample is introduced to about 10 mm from the
bottom of vial cap.
• Note 4: 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 and NPOC+POC analysis cannot be performed.
Note: Wash any new vials using laboratory glassware detergent and then rinse them
thoroughly with water before use.
70 TOC-LCPH/CPN
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.
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 Full Scale
NPOC Analysis TC Analysis TC-IC Analysis
100 µg/L 2 3 1
500 µg/L 4 5 1
1 mg/L 5 6 2
5 mg/L 6 7 3
10 mg/L More than 6 More than 7 More than 3
Table 3.3 40 mL Vials

Maximum Number of Measurements
Calibration Full Scale
NPOC Analysis TC Analysis TC-IC Analysis
100 µg/L 2 3 1
500 µg/L 4 5 1
1 mg/L 5 6 2
5 mg/L 6 7 3
10 mg/L More than 12 More than 17 More than 8
Note: When using a TOC-LCPN, perform measurement using a calibration curve full
scale greater than 1 mg/L.
The target measurement range for three repeated measurements using 9 mL vials is shown
in Table 3.4.
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.
TOC-LCPH/CPN 71
Table 3.4 Maximum Number of Measurements Using 9 mL Vials

Analyte Measurement Range Maximum Number of Measurements
NPOC Range over 0 to 1 mg/L When sparging with the sample injector 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
3.1.19.2 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.
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 marketed
under such names Sealon Film.
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.
Note: 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.
72 TOC-LCPH/CPN
¬Using Caps
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.
Note: Because the seals are perforated during injection, discard the seals
after use.
¬Using Sealing Film

1. Cut the sealing film into approximately 25 mm squares.
2. Place a square of sealing film over the opening of the vial and stretch the film over the
edges of the vial to seal it.
3. Press the edges down so that they wrap around the outside of the vial.
Be careful that
film edges do not
descend below
vial threads.
Figure 3.33 Sealing the Vial
3.1.19.3 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.
TOC-LCPH/CPN 73
TIP » 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.
Note: During analysis, the turntable must be covered. The ASI-L will not
operate if the turntable cover is not detected.
3.1.19.4 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 3.34 "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.
Note: Rinse water will not flow properly if the rinse tube is not inserted correctly, and
measurement values may be adversely affected.
Use the provided tubing

ring-band to adjust the
tubing insertion depth.
Ensure that the tubing
reaches nearly to the
bottom of the rinse bottle.
Figure 3.34 Rinse Tubing Placement
74 TOC-LCPH/CPN
¬Rinse Water Usage

The required volume of rinse water will vary depending on the measurement parameters.
The information in Table 3.5 "Rinse Water Usage Examples" 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.
Table 3.5 Rinse Water Usage Examples

No. of Flow Wash No. of Flow Wash Rinse Remarks
(between vials) (after all meas. Water
completion) Usage
1 1 Approx.1.3 L Analyzing 93 samples with standard model.
Approx.2.3 L Conducting NPOC analysis of 93 samples
with external sparge kit.
2 2 Approx.2.6 L Analyzing 93 samples with standard model.
Approx.3.6 L Conducting NPOC analysis of 93 samples
with external sparge kit.
3.1.19.5 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 Section 3.1.18.1 "High Sensitivity
Analysis" on page 61 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.
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 Section 5.3.2 "Creating a Calibration Curve File" on page 126. 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 Section 5.3.2 "Creating a
Calibration Curve File" on page 126.
TOC-LCPH/CPN 75
• 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.
3.1.19.6 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.
CAUTION
Hydrochloric acid is a hazardous chemical. Exercise caution when handling to
prevent contact and spills. For details, refer to Section 8.9 "Material Safety Data
Sheets" on page 376.
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.
76 TOC-LCPH/CPN
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.
3.1.19.7 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.
CAUTION
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.
3.1.19.8 Stirrer Preparation
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.
Reference: Refer to Section 5.1.2 "Reviewing and Editing a System Configuration" on page 116, to
display the Instrument Properties window.
TOC-LCPH/CPN 77
2. Select the ASI tab.

3. Place a check mark next to Activate Stirrer to enable this option.
4. Click OK.
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.
Note: 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.
78 TOC-LCPH/CPN
Procedure
1. Open the Instrument Properties window associated with the instrument used for
measurement.
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.
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.
TOC-LCPH/CPN 79
3.1.20 OCT-L (8-Port Sampler) Measurement
3.1.20.1 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.
Note: Wash all sample containers with an appropriate laboratory detergent, and rinse
them thoroughly with water before using them for the first time.
3.1.20.2 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
Note: 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.
Note: 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.
80 TOC-LCPH/CPN
3. Press the overlapping portions of the Parafilm around the neck of the opening.
Parafilm
Figure 3.35 Sealing the Container
3.1.20.3 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 Section 3.1.18.1
"High Sensitivity Analysis" on page 61 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.
TOC-LCPH/CPN 81
3.1.21 Starting Up the Instrument
3.1.21.1 Turning on the Power
Turn on power to the instrument to perform measurements.
TIP » Main power switch

mark: ON
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.
TIP » Electric furnace heating and carrier gas supply will not start until the instrument starts up
and communication is established between the instrument and the Sample Table Editor.
The lit states of the power switch and the indicator in the middle of the TOC-L front door
represent the instrument states shown in Table 3.6.
Table 3.6 Relationship Between Power Switch and Indicator Lit States and
Instrument State
Instrument State Indicator in the Middle of Power switch
the Front Door
Ready condition not established Lit orange Lit green
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
82 TOC-LCPH/CPN
Table 3.6 Relationship Between Power Switch and Indicator Lit States and
Instrument State
Instrument State Indicator in the Middle of Power switch
the Front Door
Warning occurred Lit red Lit green
Shutting down Off Flashing orange
Shut down Off Lit orange
Main power switch OFF Off Off
3.1.21.2 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 Section 5.1.1 "Creating a New System Configuration" on page 110 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.
Note: • 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.
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.
Note: 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.
TOC-LCPH/CPN 83
3.1.21.3 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 Section 5.1.1 "Creating a New System Configuration" on page 110 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.
Note: If the carrier gas supply pressure must be set higher than 300 kPa,
never allow the pressure to exceed 600 kPa.
4. Display the Background Monitor window.
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.
Carrier gas pressure

adjustment knob
Figure 3.36 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.
Note: 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.
84 TOC-LCPH/CPN
3.1.21.4 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.
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.
Note: Allow 30 minutes for the furnace to reach the set temperature.
3.1.21.5 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.
Note: Never allow the air supply pressure for ozone to exceed 300 kPa.
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.
TOC-LCPH/CPN 85
86 TOC-LCPH/CPN
4
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.
Step 1 Checks Before Analysis
Step 2 Turning on the Instrument
Step 3 Opening the Sample Table Editor
Step 4 Creating a Sample Table
Step 5 Creating an Analysis Parameters File
• Calibration Curve File
• Method File
Step 6 Editing the Sample Table
Step 7 Entering the Vial Numbers
Step 8 Connecting to the Instrument
Step 9 Conducting Analysis
• Analysis with an ASI-L or OCT-L
• Analysis without an ASI-L or OCT-L
Step 10 Viewing and Outputting Analysis Results
Step 11 Ending Analysis
4.1 Analysis Flow
4.1 Analysis Flow

This section presents a general description of the overall analysis flow.
For more detailed descriptions, refer to the indicated reference destinations.
Step 1 Checks Before Analysis

Perform the following daily inspections before switching on power to the instrument.
• Remaining dilution water: Refer to Section 7.1.1 "Checking Dilution Water" on page
272.
• Remaining acid: Refer to Section 7.1.2 "Checking Acid" on page 272.
• Drain vessel water level: Refer to Section 7.1.3 "Checking Drain Vessel Water Level"
on page 272.
• Humidifier water level: Refer to Section 7.1.4 "Checking Humidifier Water Level" on
page 273.
88 TOC-LCPH/CPN
4.1 Analysis Flow
Step 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.
Main power switch
Power switch
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.
TOC-LCPH/CPN 89
4.1 Analysis Flow
Step 3 Opening the Sample Table Editor

The Sample Table Editor is an application used for analyzing samples from the PC by
performing software operations.
Reference: Refer to Section 5.2.1 "Opening the Sample Table Editor" on page 119.
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.
Reference: Refer to Section 5.1.1 "Creating a New System Configuration" on page 110.
Procedure
1. Start TOC-Control L from the Windows Start menu, and click the Sample Table
Editor button.
The Sample Table Editor application starts up.
TIP » The Sample Table Editor can also be started directly from the Windows Start menu and
from the shortcut icon created on the desktop.
90 TOC-LCPH/CPN
4.1 Analysis Flow
Step 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.
Reference: Refer to Section 5.3.1 "Creating a Sample Table" on page 125.
Procedure
1. Click in the Sample Table tab of the file viewer, or click on

the toolbar.
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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4.1 Analysis Flow
3. Click OK.
A new Sample Table is created, and opened in the Sample Table Editor.
Step 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).
¬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.
Reference: Refer to Section 5.3.2 "Creating a Calibration Curve File" on page 126 for more details.
Procedure
1. Click in the Calibration Curve tab of the file viewer.
92 TOC-LCPH/CPN
4.1 Analysis Flow
The Calibration Curve Wizard (Page 1) System Information page is displayed.
2. Select the System and click Next.

The Calibration Curve Wizard (Page 2) Calibration Curve Type page is displayed.
3. Select Normal and then click Next.
TOC-LCPH/CPN 93
4.1 Analysis Flow
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. Enter a name for the calibration curve file in the File Name field, and click
Next.
The Calibration Curve Wizard (Page 4) Calibration Measurement Parameters page is
displayed.
5. Select the Units, and click Next.
94 TOC-LCPH/CPN
4.1 Analysis Flow
The Calibration Curve Wizard (Page 5) Calibration Points List page is displayed.
6. Click Add.
The Edit Calibration Point Parameters window is displayed.
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4.1 Analysis Flow
7. Enter the calibration point concentration in the Cal. Point Conc. field, and click OK.
8. 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.
9. Click Finish to complete the calibration curve setup.

A calibration curve file is created based on the calibration curve parameters.
96 TOC-LCPH/CPN
4.1 Analysis Flow
¬Method File
The procedure for entering the main parameters of the method file is described below. Only
the basic parameters are described here.
Reference: Refer to Section 5.3.3 "Creating a Method" on page 133 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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4.1 Analysis Flow
3. Select the type of Analysis, enter a method file name in the File Name field, and click
Next. The analysis type "TOC" indicates TOC measurement using TC-IC.
The Method Wizard (Page 3) Calibration Curves page is displayed.
4. Select the calibration curve to use in measurement and then click Next.
The Method Wizard (Page 4) Injection Parameters page is displayed.
98 TOC-LCPH/CPN
4.1 Analysis Flow
5. The default values entered for the settings on this page may be used for conducting
basic analysis. Verify the settings, and click Next.
6. Check the settings and then click Next.

The Method Wizard (Page 6) Pharmaceutical water testing window is displayed.
7. Click Finish to complete the settings.

A method file is created based on these parameters.
TOC-LCPH/CPN 99
4.1 Analysis Flow
Step 6 Editing the Sample Table

Insert the sample measurement parameters into the Sample Table.
Reference: Refer to Section 5.3.6 "Reviewing and Editing a Sample Table" on page 146 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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4.1 Analysis Flow
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 Analysis Flow
Step 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.
Reference: Refer to Section 5.4.6 "Vial Numbers" on page 173 for more details.
Note: 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.
102 TOC-LCPH/CPN
4.1 Analysis Flow
Step 8 Connecting to the Instrument

Communication is established between the Sample Table Editor and the instrument to
enable sample analysis.
Reference: Refer to Section 5.7.1.1 "Connection" on page 210 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.
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 Analysis Flow
Step 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
Reference: Refer to Section 5.7.3 "Analysis with an ASI-L or OCT-L" on page 216 for more details.
Procedure
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.
3. Click Start to begin the analysis sequence.
4. After a peak appears, click to open the Sample window.
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4.1 Analysis Flow
¬Analysis without an ASI-L or OCT-L
Reference: Refer to Section 5.7.4 "Analysis without an ASI-L or OCT-L" on page 218 for more details.
Procedure
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.
Reference: Refer to Section 5.7.4 "Analysis without an ASI-L or OCT-L" on page 218
for more details.
The TOC Measurement window is displayed.
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.
TOC-LCPH/CPN 105
4.1 Analysis Flow
Step 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
Reference: Refer to Section 5.5.1 "Sample Window" on page 184 for more details.
Procedure
1. Click .
The Sample window is displayed. Each of the sample analyses can be reviewed.
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4.1 Analysis Flow
¬Output to a Printer or File
Reference: Refer to Section 5.6 "Sample Table Data Output and Printing" on page 195 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
Step 11 Ending Analysis

This procedure describes the end of analysis and post-analysis instrument settings.
Reference: Refer to Section 5.7.7 "Instrument Shutdown" on page 224 for more details
Procedure
1. Click .
The Shutdown dialog box is displayed.
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.
108 TOC-LCPH/CPN
5
5 Software Operation
This chapter describes the use of the TOC-Control L software to set analysis
parameters and conduct analysis operations.
5.1 System Configuration

Describes the procedures for creating system configurations necessary for
performing analysis.
5.2 Sample Table Editor
Describes the basic operations and screens of the Sample Table Editor
application used for conducting analysis.
5.3 Creating and Editing Files
Describes the procedures used for creating and editing the various files necessary
for conducting analysis.
5.4 Editing a Sample Table
Describes the procedures for entering analysis information into the Sample
Table.
5.5 Reviewing and Editing Measurement Data
Describes the procedures for checking and conducting re-calculation of
previously acquired data.
5.6 Sample Table Data Output and Printing
Describes the procedures for printing analysis results and outputting data.
5.7 Operation and Analysis
Describes the procedures for operating the instrument and conducting analysis.
5.8 Display Options
Describes the procedure for changing the Sample Table display.
5.9 Security Functions
Describes the login procedures such as, using passwords, screen lock release and
other software administration functions.
5.10 Other Functions
Describes supplementary functions.
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. Start the TOC-Control L from the Windows Start menu.
2. Click the H/W Settings button.
Note: When the User window is displayed, log in referring to Section

5.9.1 "Login" on page 244.
The H/W Setting List window is displayed.
3. Click the Create a New Setting button.
110 TOC-LCPH/CPN
The Instrument Setup Wizard - System Information window is displayed.
4. Enter the system information.
Item Description
System Enter a system name using up to 32 single-byte characters. Entry is
mandatory. Use of a name that is already assigned to an existing system
configuration is not permitted.
Instr Serial No. Enter the serial number of the instrument. Entry is mandatory. The serial
number is printed on the plate attached to the lower right side of the
instrument.
User The name of the current user is automatically entered into the User field.
Date of Creation The current date is automatically entered into the Date of Creation field.
Comment Enter additional system information in the Comment text box. The Comment
field is optional and can contain up to 512 characters.
5. Click Next.
The Instrument Setup Wizard - Options window is displayed.
TOC-LCPH/CPN 111
6. Set the TOC instrument type and any options.
Item Description
Model Select the type of TOC instrument you are using.
Options 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 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.
7. Click Next.
The Instrument Setup Wizard - TOC window is displayed.
8. Enter the settings related to TOC measurement.
Item Description
Auto regeneration of IC Selecting this checkbox will cause the instrument to
solution automatically regenerate IC reagent in the following situations.
Normally, this checkbox should be selected.
• When the instrument power is turned on
• Before the initial IC measurement, following a preset
number of injections and preset volume of injected samples
• If peak tailing occurs in IC measurement
TN Power Selecting this checkbox will supply power to the optional TNM-
L. If the TNM-L is installed, ensure that this checkbox is
selected.
This option is only enabled if the TNM-L checkbox was selected
under Options in the Instrument Setup Wizard Options window.
112 TOC-LCPH/CPN
Item Description
Ext. Sparge Valve OPEN Selecting this checkbox in the system configuration for the
added external sparge kit allows sparge gas to continue flowing
while the Sample Table Editor is connected to the instrument.
Enable ready status check Selecting this checkbox enables the instrument's Ready Status
Check function. Normally, this checkbox should be selected.
Stir Suspended Solids Selecting this checkbox agitates the sample extracted with the
syringe of the sample injector with sparge gas immediately
before injecting it into the combustion tube (or IC reaction
vessel).
Carrier Gas Flow Set the carrier gas flow rate. Normally, this should be set to
150 mL/min (default value).
Carrier Gas Select the type of carrier gas to supply to the TOC instrument.
The available types of carrier gas are Air, Oxygen, and Nitrogen.
The optional N2 carrier gas kit is required to use nitrogen gas.
Catalyst Type Select the catalyst type. Click on the box, and select either
Regular, High Sense, or TC/TN.
Tubing Diameter 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 measurements, select Regular. Select Suspended Particle
if the optional Suspended Solids kit will be used.
Cell Length This item sets the detector cell length. Click the box, and select
either Long or Short. Normally, Long is selected.
TC Furnace This item sets the TC furnace temperature. Select 680 for
Regular or 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 Setup Wizard - ASI window is displayed.
TOC-LCPH/CPN 113
10. Enter the ASI-L-related settings.

Item Description
Vial Type Select the vial rack type. Click on the box, and select 9 mL Vial,
24 mL Vial or 40 mL Vial.
Needle Type 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
Wizard.
• Sample: for analysis using only a sample needle
• Sample + Sparge: for analysis using a sample needle and
sparge needle
No. of Flow Wash (between Select the number of times (0 - 10) the outside of the needle will
vials) be washed with dilution water, after each sample analysis.
No. of Flow Wash (after all Select the number of times (0 - 10) the flow line will be washed
meas. completion) with dilution water from the needle to the injection tube, at the
completion of the sample sequence. A single wash is acceptable
for typical samples. Select 3 – 4 washes when analyzing samples
containing acid, alkali or salt.
Needle Rinse (after sampling) 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.
Better results are obtained by not rinsing between samples when
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.
Needle Rinse (after acid Select this item to rinse the sampling needle with dilution water
addition) after each acid addition. If the difference in NPOC content among
the samples is not large, this rinse may be omitted.
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.
114 TOC-LCPH/CPN
13. Click Next.

The Instrument Setup Wizard - Communication window is displayed.
14. Enter the parameters for communication between the PC and the instrument.
Item Description
Com Port 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 TOC-L.
For details on the USB device driver, refer to the "Administrator Manual".
Stop Bits This item is entered automatically and is dependent on the Com Port selection.
Parity This item is entered automatically and is dependent on the Com Port selection.
15. Click Finish.

The system configuration is created and 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.
TOC-LCPH/CPN 115
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.
The Instrument Properties window is used for viewing and editing the system configuration
parameters. This window can be accessed from either the H/W Setting List window or the
Sample Table Editor.
¬Access from the H/W Setting List
Procedure
1. Start TOC-Control L from the Windows Start menu.
2. Click the H/W Settings button.
3. Click the icon of the system configuration to be viewed or edited.

4. Click Open.
The Instrument Properties window is displayed.
5. Click the tabs at the top of the window to view or edit the content as necessary.
TIP » Click Print to open the Print window and enable printing of the Instrument Properties
window settings.
116 TOC-LCPH/CPN
The tabs are described below.

Note: 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.
6. Click OK.
Any changes to the system configuration are saved, and the window closes.
¬Access from the Sample Table Editor
Procedure
Reference: Refer to Section 5.2.1 "Opening the Sample Table Editor" on page 119 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.
Reference: 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.
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".
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5.1.3 Deleting a System Configuration

If an existing system configuration becomes unnecessary, it can be deleted.
Note: A deleted system configuration cannot be restored.
Procedure
2. Click H/W Settings.
3. Select the system configuration icon to be deleted.

4. Click Delete.
A delete confirmation window is displayed.
5. Click Yes.
The system configuration is deleted.
118 TOC-LCPH/CPN
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
2. Click the Sample Table Editor button.
TIP » The Sample Table Editor can be started directly from either the Window Start menu or from
the shortcut icon created on the desktop.

The Sample Table Editor application starts.
5.2.2 Exiting the Sample Table Editor
Procedure
1. Select File – Exit.
The Sample Table Editor closes.
TOC-LCPH/CPN 119
5.2.3 Sample Table Editor Window Components

The Sample Table Editor window consists of the components shown below.
File Viewer Menu Bar Tool Bar Ready Indicator
Output Window Status Bar Status Monitor
Component Description
Menu Bar Many operations can be performed from the menus.
Tool Bar Primary operations can be performed from the icons.
Ready Indicator 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.
: 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.
File Viewer 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 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.
Status Monitor Displays the name, ID, measurement results, etc. associated with the sample in the table.
Status Bar Displays a brief description of selected menu items and the user's name.
Output Window Displays information regarding the instrument operation.
120 TOC-LCPH/CPN
¬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.
Reference: Refer to Section 5.3.1 "Creating a Sample Table" on page 125 for details on creating a
Sample Table.
Note: 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.
Note: The columns displayed vary depending on the display settings. To change the
settings, refer to Section 5.8.1 "Sample Table" on page 234.
Column Description
Type Displays the sample type.
• Standard is displayed for standard solutions.
• 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.
Sample ID Displays the sample ID.
Object ID Displays the object ID. Depending on the software, a unique number 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.
Notes Displays information such as whether the assessment is based on a control sample
or on USP/EP measurement.
Comment Displays any entered comment.
Status Displays the sample status.
• Defined
• Measuring
• Completed
• Aborted
TOC-LCPH/CPN 121
Column Description
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.
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.
Reference: Refer to Section 5.5.1 "Sample Window" on page 184 for details regarding the Sample
Window.
When a sample is selected in the Sample Table, the following information is displayed in
the Sample Window.
Note: The columns displayed vary depending on the sample type and display item
settings. Refer to Section 5.8.2 "Sample Window Display Options" on page 236
to change the settings.
122 TOC-LCPH/CPN
Column Description
Spl. No./Std. No. Displays the sample or standard number.
Spl. No. is used for Unknown and Control samples.
Std. No. is used for calibration curve samples.
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.
Remarks Displays a remark. Remarks consist of the following types.
T: Tailing occurred in the detector output.
H: Saturated signal occurred in the detector output.
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.
Status Displays the injection status.
• Defined
• Measuring
• Completed
• Aborted
Vial Displays the vial number of the sample.
Excluded Displays the exclusion flag (E) for exclusion of the injection. If analysis
parameters were changed due to software settings, R is displayed.
Inj. Vol. Displays the injection volume
Auto Dil. Displays the dilution factor.
Calibr. Curve Displays the name of the calibration curve file referenced to obtain the
calibration curve calculation.
Date / Time Displays the date and time the analysis was conducted.
5.2.6 File Types Used

The types of files created and used in the Sample Table Editor are described below.
¬Sample Table File (*.tlx)

The measurement parameters and results for each sample are recorded in this file.
A file of the same name but with the *.pkt extension records the peaks obtained from
measurement of the corresponding sample.
A template containing the measurement parameters is inserted into the sample table file,
and measurement is conducted.
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¬Calibration Curve File (*.cal)

The calibration curve file is a template file containing the calibration curve generation
parameters.
A file (Example: ABC.cal) 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 (ABC.2007_03_19_11_46_37.cal), is created.
The file containing the calibration curve generation parameters, such as the above-
mentioned ABC.cal, 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 (*.met)

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
measurement is conducted.
¬Control Sample File (*.tpl)

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 (*.tsc, *.txt)

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 text file format schedule file (*.txt) is a text file that contains descriptions of the
sample type, analysis type, and source parameter file for each sample.
The sample table editor can manipulate either the sample format or the text file format.
Schedule files can be exported from the sample table file.
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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.

TIP: The Select H/W Settings window can also be displayed by selecting File – New –
Sample Table.
Enter a comment in the Comment box, as necessary.
3. Click OK.
A new Sample Table is created, and opens inside the Sample Table Editor.
Reference: Refer to Section 5.4 "Editing a Sample Table" on page 160 for the procedure for inserting
information into the Sample Table.
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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.

TIP: The Calibration Curve Wizard (Page 1) System Information page can also be displayed
by selecting File – New – Calibration Curve.
2. Select the system configuration to be used.
Item Description
System Select the system to be used for measurement.
User The name of the User conducting the operation is
automatically entered.
Date of Creation The current date and time are automatically entered.
Comment A comment (using up to 512 single-byte characters)
regarding the system configuration may be entered as
necessary.
3. Click Next.
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The Calibration Curve Wizard (Page 2) Calibration Curve Type page is displayed.
Type settings
4. Enter the type of calibration curve.
Item Description
Type settings • Normal:
Normally, use this option. Selecting the Use dilution
from standard solution checkbox sets the usage of
standard solution automatically prepared inside the
instrument.
• USP/EP Support:
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.

TIP: For information on the zero shift setting, refer to Section 8.2.3.2 "Shifting of
Calibration Curves" on page 336.
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.
Zero Shift Select this item to shift the calibration curve through the
origin.
Multiple Injections If this item is selected, multiple injections are made from a
single aliquot of standard solution. This larger standard
aliquot is drawn in the syringe in one aspiration and is
sufficient to accommodate all of the repeat injections.
File Name Enter the calibration curve file name.
7. Click Next.
The Calibration Curve Wizard (Page 4) Calibration Measurement Parameters page is displayed.
8. 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.
No. of Injections 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 analysis
injections. If, however, the result exceeds the SD Max. and CV Max. limit,
the additional injections are performed for confirmation. The maximum
number of injections includes the analysis injections and the additional
injections.
No. of Washes Select the number of times (1 – 10) the flow line will be washed before the
first injection.
128 TOC-LCPH/CPN
Item Description
SD Max. 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. of Injections
setting has a larger maximum number of injections than the number of
analysis injections.
CV Max. Enter the coefficient of variation (CV) limit (0.0 – 100). This limit is used to
Sparge Gas Flow Enter the sparge gas flow rate (50 – 200). Normally, a flow rate of 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.
9. Click Next.
Calibration point list
10. Enter the advanced parameters for each calibration point.

Depending on the settings, some items may not be displayed.
Item Description
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.
Edit Opens the Edit Calibration Point Parameters dialog box to allow
editing of the selected calibration point.
Add Opens the Edit Calibration Point Parameters dialog box to add a new
calibration point.
Delete Deletes the selected calibration point.
Delete All Deletes all of the calibration points in the Calibration point list.
11. 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.
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• When not using the dilution of stock solution function
Item Description
Calibration Point No. Displays the calibration point number that corresponds to the number in
Calibration Curve Wizard (Page 5) Calibration Points List.
Cal. Point Conc. Enter the calibration point concentration.
No. of Injections 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. If, however, the result exceeds the SD Max. and CV Max. limit,
the additional injections are performed for confirmation. The maximum
number of injections includes the analysis injections and the additional
injections.
SD Max. Enter the standard deviation (SD) limit (0.0 – 9999). This limit is used to
• When using the dilution of stock solution function
Item Description
Calibration Point No. Displays the calibration point number that corresponds to the
number in Calibration Curve Wizard (Page 5) Calibration Points
List.
Standard Solution Conc. Enter the standard solution concentration.
Cal. Point Conc. Enter the calibration point (concentration) for calibration.
130 TOC-LCPH/CPN
Item Description
Auto. Dilution Displays the automatic dilution factor calculated from Auto.
Dilution / Standard Solution Conc.
No. of Injections 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 analysis injections. If, however, the result
exceeds the SD Max. and CV Max. limit, the additional injections
are performed for confirmation. The maximum number of
injections includes the analysis injections and the additional
injections.
SD Max. 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. of Injections setting has a larger maximum number of
injections than the number of analysis injections.
CV Max. 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 No. of Injections setting has a larger maximum number of
injections than the number of analysis injections.
Note: 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

TC, NPOC Normally: 30,000 mg/L
If using Dilution from Standard Solution*: 2,500 mg/L
IC Using TOC-LCPH: 35,000 mg/L
Using TOC-LCPN: 3,000 mg/L
If using Dilution from Standard Solution*: 3,000 mg/L
TN Normally: 4,000 mg/L
If using Dilution from Standard Solution*: 200 mg/L
POC 500 mg/L
Manual injection TC 20,000 mg/L
Manual injection IC Using TOC-LCPH: 20,000 mg/L
* If the Dilution from Standard Solution item is selected in the Calibration Curve Wizard
(Page 2) Calibration Curve Type page.
12. Click OK.

13. Click Next.
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The Calibration Curve Wizard (Page 6) Additional Settings page is displayed.
14. Enter the remaining parameters.
Item Description
Use default settings If this item is selected, the software default values are used for peak
detection and the Min. integration time and Max. integration items
are disabled.
Min. integration time Enter the minimum time the instrument signal will continue to be
detected.
Max. integration Enter the maximum time the instrument signal will be detected when
no peak is found.
Correlation Coeff. Check If this item is selected, the calibration curve error judgment is based
on the correlation coefficient. When this item is selected, Failure
Action (1st time), Failure Action (2nd time) and Lower limit items
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.
Failure Action (1st time) Select the process to be conducted if an error occurs.
Continue: Records the error in the Sample Table, and allows analysis
to continue.
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.
Failure Action (2nd time) Select the process to be conducted if a second error occurs.
Continue: Records the error in the Sample Table, and allows analysis
to continue.
Stop: Records the error in the Sample Table, and stops analysis.
Lower Limit Enter the minimum correlation coefficient value. If the calculated
correlation coefficient is less than the value entered, an error is
assessed.
15. 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.
TIP: 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
necessary.
3. Click Next.
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The Method Wizard (Page 2) Analysis Information page is displayed.
4. Enter the basic method information.
Item Description
Analysis Select the analysis type from the list. "TOC" indicates TOC
measurement using TC-IC.
Manual Dilution Enter the sample preparation dilution factor if the sample
was diluted manually. The entered value will be used in the
concentration calculation. The default value is 1.
No. of Determinations Enter the number of times each sample is to be injected. If
the multiple injections item is selected one aliquot will be
drawn into the syringe and all of the required injections are
made from this aliquot.
File Name Enter a method file name.
5. Click Next.
134 TOC-LCPH/CPN
The Method Wizard (Page 3) Calibration Curves page is displayed.
6. 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.
Reference: Refer to Section 8.2.5 "Automatic Selection of Optimum Calibration

Curve" on page 338 for more details.
Item Description
Analysis Displays the analysis type selected in the Method Wizard
(Page 2) Analysis Information page. "TOC" indicates TOC
Calibration Curve 1, Click to locate the calibration curve folder, and
Calibration Curve 2, select the file using the Open dialog box.
Calibration Curve 3
7. Click Next.
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The Method Wizard (Page 4) Injection Parameters page is displayed.
8. Set the advanced analysis parameters.

Depending on the Analysis type setting, some items may not be displayed.
Item Description
Analysis Displays the analysis type selected in the Method Wizard (Page 2) Analysis
Information page. "TOC" indicates TOC measurement using TC-IC.
Injection Volume The injection volume is automatically entered.
Expected Conc. Range Enter the expected concentration value if one is known. This item is not required. A
range value is automatically entered based on the calibration curve selected on
Method Wizard (Page 2) Calibration Curves.
No. of Injections 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 analysis injections. If, however,
the result exceeds the SD Max. and CV Max. limit, the additional injections are
performed for confirmation. The maximum number of injections includes the
analysis injections and the additional injections.
SD Max. 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. of Injections setting has a
larger maximum number of injections than the number of analysis injections.
CV Max. 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 No. of Injections setting has a
No. of Washes Enter the number of times (1 – 10) the flow line will be washed before the first
analysis injection.
Auto Dilution Enter the sample dilution factor.
Sparge Time Enter the sparging time (0 – 20).
Multiple Injections If this item is selected, multiple injections are made from a single sample aliquot.
This larger aliquot is drawn in the syringe in one aspiration and is sufficient to
accommodate all of the repeat injections.
Use blank check area If selected, the blank analysis value is subtracted from the analysis result.
136 TOC-LCPH/CPN
Item Description
Auto. correction of inj. If selected, the instrument will automatically adjust the injection volume and
vol. and dilution dilution factor and conduct re-analysis when the measurement result exceeds the
calibration curve range.
9. Click Next.
The Method Wizard (Page 5) Peak Time Parameters page is displayed.
10. Enter the peak detection parameters.
Item Description
Analysis Displays the analysis type selected in the Method Wizard (Page 2) Analysis
Information page. "TOC" indicates TOC measurement using TC-IC.
detection and the Min. integration time and Max. integration items are
disabled.
Min. integration time Enter the minimum time the instrument signal will continue to be detected.
Max. integration Enter the maximum time the instrument signal will be detected when no
peak is found.
11. Click Next.

Note: 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.
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12. Click Next.

The Method Wizard (Page 6) Pharmaceutical water testing window is displayed.
13. Configure the settings related to the acceptance of measurement values when using
pharmaceutical water control. (Refer to Section 8.2.8 "Pharmaceutical Water Testing"
on page 341.)
Item Description
Testing method settings • 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
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.
14. Click Finish.

The method file is saved.
138 TOC-LCPH/CPN
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.
TIP: The Control Sample Wizard (Page 1) System Information page can also be displayed
by selecting File – New – Control Sample.
2. Select the system to be used.
Item Description
necessary.
3. Click Next.
TOC-LCPH/CPN 139
The Control Sample Wizard (Page 2) Control Sample Type page is displayed.
Control sample types
4. Select the Control Sample type.
Item Description
Control sample types • Control Sample
Specifies use of a typical control sample.
• Control Chart Sample
Select this option to add the control sample to a defined
control chart. Click to locate the folder where
the control chart file is stored, and select the file using
the Open dialog box.
Save the data in a control Enter a file name that will become the name of the control
sample template sample file.
5. Click Next.
The Control Sample Wizard (Page 3) Parameter Source page is displayed.
Parameter sources
140 TOC-LCPH/CPN
6. Select the source file type to be used for creating the control sample.
Item Description
Parameter sources • 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 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 Select this item to skip the remaining Wizard pages. A
and use measurement Finish button is displayed at the bottom of the page. Click it
parameters from the source to save the control sample file.
Note: 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.
7. Click Next.
The Control Sample Wizard (Page 4) Analysis Parameters page is displayed.
8. Enter the basic control sample information.
Item Description
Analysis Click the box, and select the analysis type from the list.
Calibration Curve 1 Click to locate the calibration curve folder, and
select the appropriate file using the Open dialog box.
TOC-LCPH/CPN 141
9. Click Next.
The Control Sample Wizard (Page 5) Injection Parameters page is displayed.
10. Enter the advanced analysis parameters.

Depending on the Analysis setting, some items may not be displayed.
Item Description
Analysis Displays the analysis type selected in Control Sample Wizard (Page 4)
Analysis Parameters.
Expected Conc. Range Enter the expected concentration value if one is known. Input is not mandatory.
analysis injections and the right box indicates the maximum number of
injections. If, however, the result exceeds the SD Max. and CV Max. limit, the
additional injections are performed for confirmation. The maximum number of
injections includes the analysis injections and the additional injections.
SD Max. 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. of Injections setting
has a larger maximum number of injections than the number of analysis
injections.
setting has a larger maximum number of injections than the number of analysis
injections.
analysis injection.
Multiple Injections If this item is selected, multiple injections are made from a single aliquot. This
larger aliquot is drawn in the syringe in one aspiration and is sufficient to
142 TOC-LCPH/CPN
Item Description
Use area retrieved from If selected, the blank analysis value is subtracted from the analysis result.
the blank check
11. Click Next.

The Control Sample Wizard (Page 6) Peak Time Parameters page is displayed.
Item Description
Analysis Displays the analysis type that was selected for Analysis Type in
the Control Sample Wizard (Page 4) Analysis Type page.
Use default settings If this item is selected, the software default values are used for
peak detection and the Min. integration time and Max. integration
items are disabled.
detected.
Max. integration Enter the maximum time the instrument signal will be detected
when no peak is found.
13. Click Next.
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The Control Sample Wizard (Page 7) Control Checking page is displayed.
Evaluation type
14. Enter the control sample evaluation parameters.
Item Description
Evaluation type • 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)
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.
Low Lmt. Enter the lower limits for the selected control sample evaluation procedure.
Up. Lmt. Enter the upper limits for the selected control sample evaluation procedure.
Ignore Zero Shift of Cal. Select this item to ensure that the concentration calculation is conducted while
Curve in Conc. ignoring the calibration curve shift to origin setting.
Calculation
Action when the failure Select the action to be taken the first time a control sample exceeds the control
event occurs the first time 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.
• Stop (whole sample run)
Records the failure in the Sample Table, and stops the analysis.
• 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.
144 TOC-LCPH/CPN
Item Description
Action when the failure Select the action to be taken if a control sample exceeds the control limits when
event occurs the second during repeat analysis as specified for the 1st failure action. Click the box, and select
time the appropriate action from the following options:
• Continue (notify)
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.
15. 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.
Note: 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.
Procedure
1. Click in the Schedule tab of the file viewer.
TIP » The Select H/W Settings window can also be displayed by selecting File – New – Schedule.
TOC-LCPH/CPN 145
Enter a comment in the Comment box, as necessary.
3. Click OK.
A new schedule is created, and opens in the Sample Table Editor.
Note: • Enter information in the schedule in the same manner as in the Sample
Table. For details, refer to Section 5.4 "Editing a Sample Table" on page
160.
• A sample file can export a schedule file with the same content. For
details, refer to Section 5.6.7 "Exporting a Schedule File" on page 208.
¬Creating a Schedule File in Text Format
A schedule file can be saved in text format so that it can be edited in a text editor. For
details on creating a text format schedule file, refer to Section 5.6.7 "Exporting a Schedule
File" on page 208.
5.3.6 Reviewing and Editing a Sample Table

For details on opening an existing Sample Table and entering information, refer to Section
5.4 "Editing a Sample Table" on page 160, and Section 5.5 "Reviewing and Editing
Measurement Data" on page 184.
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.
Reference: The parameters in the Calibration Curve Properties window were entered when the
calibration curve was generated. For details regarding these items, refer to Section 5.3.2
"Creating a Calibration Curve File".
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.
TIP » 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.
2. Review and edit the items by clicking on the desired tabs.
Note: Some items cannot be edited.
146 TOC-LCPH/CPN
• The Common tab is described below.
Item Description
System Displays the system used for analysis and cannot be edited.
User Displays the name of the user who created the file and cannot be 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.
Print Opens the Print dialog box. Make the necessary print settings, and 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.
Status Displays the measurement status of the calibration curve. If
Measured is displayed, most of the Calibration Curve
Properties can be edited.
• Defined: not measured
• Completed: measured
• Aborted: measurement cancelled in progress
Units Displays the concentration unit.
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.
Calibration Curve File Displays the file name and directory folder. This item
cannot be edited.
148 TOC-LCPH/CPN
• The Analysis tab is described below.
Item Description
No. Washes Displays the number of times (1 – 10) the flow line will be washed
before the first analysis injection.
Acid Add Displays the percentage of acid to be added to the sample.
detection and the Min. integration time and Max. integration items
are disabled.
detected.
Max. integration Enter the maximum time the instrument signal will be detected
when no peak is found.
Correlation Coeff. Check If this item is selected, the calibration curve error judgment is based
on the correlation coefficient. When this item is selected, Failure
Action (1st time), Failure Action (2nd time) and Lower limit items
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.
Failure Action (1st time) Displays the process to be conducted if an error occurs.
• Continue
Records the error in the Sample Table, and allows analysis to
continue.
• 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.
Failure Action (2nd time) Displays the process to be conducted if a second error occurs.
• Continue
Records the error in the Sample Table, and allows analysis to
continue.
• Stop
Records the error in the Sample Table, and stops analysis.
Lower Limit Enter the minimum correlation coefficient value. If the calculated
correlation coefficient is less than the value entered, an error is
assessed.
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• The Data tab is described below.
Calibration points list
Item Description
Auto Dilution Displays the automatic dilution factor.
Inj. Volume Displays the calculated injection volume.
Calibration points list Displays the information associated with each calibration
point.
Edit Displays the Edit Calibration Point Parameters dialog box
to allow editing of the selected calibration point parameters.
Add Displays the Edit Calibration Point Parameters dialog box
to allow 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 Exclude the selected calibration point from the analysis
results. This function is enabled only if the Status in the
Parameter tab is Completed.
150 TOC-LCPH/CPN
• The Graph tab is displayed below.
Item Description
Slope / Intercept / r^2/r Displays the slope, y-intercept and coefficient of
determination and correlation coefficient values.
• The History tab is displayed below.
Item Description
Ascii export Displays the Save As dialog box. A history of the changes
made to the calibration curve file can be exported as an
ASCII format text file.
3. After reviewing and editing the calibration curve properties, click OK.
The changes are saved, and the window closes.
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5.3.8 Reviewing and Editing a Method

An existing method can be reviewed and edited by opening the Sample/Method Properties
window.
Reference: The parameters in the Sample/Method Properties window were entered when the method
was created. For details regarding these items, refer to Section 5.3.3 "Creating a Method"
on page 133.
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.
2. Review and edit the items by clicking on the desired tabs.
• The Common tab is described below.
Item Description
System Displays the system used for analysis and cannot be edited.
User Displays the name of the user who created the file and
cannot be 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.
Print Opens the Print dialog box. Make the necessary print
settings, and then print the contents of the Sample/Method
Properties window.
152 TOC-LCPH/CPN
• The Parameters tab is described below.
Item Description
Analysis Displays the type of analysis. "TOC" indicates TOC
Status Displays the measurement status of the method file.
Manual Dilution Displays the dilution factor that was entered when the
method was created.
No. of Determinations Displays the number of injections for each sample.
Pharmaceutical water testing 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.
• 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.
Current Method Displays the method file name and storage location. This
item cannot be edited.
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• The TC tab is described below.

Depending on the analysis type, five different tabs may be displayed.
• TC
• IC
• NPOC
• POC
• TN
Note: Depending on the type of tab, some items may not be displayed.
Item Description
Units Displays the concentration unit.
No. of Inj. Displays 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.
No. of Wash Displays the number of flow line washes.
SD Max. Displays the standard deviation (SD) limit (0.0 – 9999).
used to assess the analysis result.
CV Max. Displays the coefficient of variation (CV) limit (0.0 – 100)
used to assess the analysis result.
Acid Add Displays the percentage of acid added to the sample.
Sparge Gas Flow Enter the sparge gas flow rate (50 – 200). Normally, a flow
rate of 80 to 100 mL/min is appropriate.
Sparge Time Displays the sparge time.
Use default settings Displays whether or not the software default values will be
used for the peak detection time.
Min. integration time Displays the time allowed for signal detection from the
instrument to continue.
Max. integration Displays the time at which signal detection from the
instrument will stop.
Multiple Injections If this item is selected, multiple injections are made from a
single aliquot of standard solution. This larger standard
aliquot is drawn in the syringe in one aspiration and is
sufficient to accommodate all of the repeat injections.
Auto. correction of inj. vol Displays the setting for automatic re-injection of the
and dilution sample.
154 TOC-LCPH/CPN
Item Description
Auto Dilution Displays the automatic dilution factor.
Inj. Volume Displays the injection volume.
Expected Conc. Range Displays the expected concentration.
Use area retrieved from the If selected, the bank analysis value is subtracted from the
blank check analysis result.
Calibration Curve 1, Displays the file names of the calibration curves
Calibration Curve 2, incorporated in the method, and the folders where they are
Calibration Curve 3 stored.
• The History tab is described below.
Item Description
Ascii export Displays the Save As dialog box. A history of the changes
made to the method file can be exported as an ASCII format
text file.
3. After viewing and editing the method properties, click OK.

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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.
Reference: 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 Section
5.3.4 "Creating a Control Sample File" on page 139.
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.
2. Click on the Control Parameters tab view and edit the control sample parameters.
TIP: Click the Sample Table row where the control sample is inserted, and click View –
Measurement Parameters to display the Sample/Method Properties window.
• The Control Parameters tab is described below.
Check sample evaluation type Sample type
Reference: For details regarding tabs other than the Control Parameters tab, refer to Section 5.3.8
"Reviewing and Editing a Method".
Item Description
Control Sample / Control The selected radio button indicates the type of control
Chart Sample sample used in measurement.
Control Checking Type Selected radio buttons indicate the type of control sample
evaluation that will be conducted.
Original Concentration Displays the concentration of the original control sample.
156 TOC-LCPH/CPN
Item Description
Spiked Concentration Displays the concentration of the of the spiked control
sample.
Max. Dev. Displays the upper limit of the allowed concentration
deviation in 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 Cal. If selected, this item allows the calibration curve shift to the
Curve in Conc. Calculation zero point to be ignored when calculating the concentration.
Action when the failure event Read-only display of the measures to be taken if the control
occurs the first time / Action sample exceeds any of the limit values.
when the failure event occurs
the second time
3. After checking and editing the Control Parameters, click OK.

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
Section 5.4 "Editing a Sample Table" on page 160, and Section 5.5 "Reviewing and Editing
Measurement Data" on page 184.
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: Section 5.3.7 "Reviewing and Editing a Calibration Curve".
• Method: Section 5.3.8 "Reviewing and Editing a Method".
• Control Sample: Section 5.3.9 "Reviewing and Editing a Control Sample".
TOC-LCPH/CPN 157
5.3.11.1 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.
5.3.11.2 From the Tool Bar
Procedure
1. Click in the tool bar.
158 TOC-LCPH/CPN
The Open dialog box is displayed.
2. Select the type of file you wish to open.

3. Select the desired file, and click Open.
The file opens.
5.3.11.3 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)
• All Cal. Curve Files (calibration curve file and calibration curve analysis results)
• Method
• Control Sample
• Schedule
3. Select the desired file, and click Open.
The file opens.
TOC-LCPH/CPN 159
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.
Note: 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.

Note: If the row above the insertion position is empty, the row is filled
with the new content.
160 TOC-LCPH/CPN
¬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.

TIP: 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.
TOC-LCPH/CPN 161
5.4.2 Inserting a Sample

The sample is inserted into the sample table by dragging the method file from the file
viewer.
Note: Method files are displayed as Unknown when they are inserted into the sample
table.
TIP » Unknown samples can also be added to the sample table by clicking a calibration curve file
from the file viewer and while pressing the SHIFT key, dragging the calibration curve into
the sample table.
Procedure
1. Display the Method tab of the file viewer.
2. Select the file, and drag it into position in the sample table.

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

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.
162 TOC-LCPH/CPN
2. Click Insert – Sample.
The Sample Wizard (Page 1) Parameter Source page is displayed.

TIP: The Sample Wizard (Page 1) Parameter Source page can also be displayed by
selecting Insert – Sample from the menu bar.
3. Select the sample parameter source file.
Parameter source
Item Description
Create the sample by using • Method
parameters from: Analysis parameters are from an existing method file. Click
to display the Open dialog box, and select the method file to use.
Analysis parameters are from an existing calibration curve file. 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 Select this item to skip the remaining Wizard pages. A Finish button is
and use measurement displayed at the bottom of the page. Click it to save the control sample
parameters from the source file.
TOC-LCPH/CPN 163
4. Click Next.
The Sample Wizard (Page 2) Analysis Information page is displayed.
5. Set the basic sample information.
Item Description
Analysis Select the analysis type from the list.
No. of Determinations Enter the number of times each sample is to be injected.
6. Click Next.
The Sample Wizard (Page 3) Calibration Curve page is displayed.
164 TOC-LCPH/CPN
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
Analysis Displays the type of analysis selected in Sample Wizard (Page 2)
Analysis Information.
Calibration Curve 1, Displays the calibration curves files incorporated with the sample,
Calibration Curve 2, and their location. Click and select the calibration curve
Calibration Curve 3 file from the Open dialog box.
8. Click Next.
The Sample Wizard (Page 4) Injection Parameters page is displayed.
9. Enter the advanced analysis conditions.

Depending on the Analysis type, some items may not be displayed.
Item Description
Analysis Displays the analysis type selected in Sample Wizard (Page 2) Analysis
Information.
Expected Conc. Range Enter the expected concentration value if one is known. This item is not required.
A range value is automatically entered based on the calibration curve selected on
Method Wizard (Page 3) Calibration Curves.
analysis injections and the right box indicates the maximum number of injections.
The result is calculated using the mean value of the analysis injections. If,
however, the result exceeds the SD Max. and CV Max. limit, the additional
injections are performed for confirmation. The maximum number of injections
includes the analysis injections and the additional injections.
SD Max. 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. of Injections setting has a
CV Max. 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 No. of Injections setting has a
TOC-LCPH/CPN 165
Item Description
analysis injection.
Multiple Injections If this item is selected, multiple injections are made from a single aliquot. This
larger aliquot is drawn in the syringe in one aspiration and is sufficient to
Use blank check area If selected, the blank analysis value is subtracted from the analysis result.
Auto. correction of inj. If selected, the instrument will automatically adjust the injection volume and
vol and dilution dilution factor and conduct re-analysis when the measurement result exceeds the
calibration curve range.
10. Click Next.

The Sample Wizard (Page 5) Peak Time Parameters page is displayed.
Item Description
Analysis Displays the analysis type selected in Sample Wizard (Page 2) Analysis
Information.
detection and the Min. integration time and Max. integration items are
disabled.
Min. integration time Enter the minimum time the instrument signal will continue to be detected.
Max. integration Enter the maximum time the instrument signal will be detected when no
peak is found.
12. Click Finish.

The sample is inserted into the sample table.
166 TOC-LCPH/CPN
5.4.3 Inserting a Control Sample

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.

Note: If there is an empty row above the insertion position, it is filled with
the new content.
Procedure
1. Right-click in the left cell of the row where the control sample will be inserted.
2. Click Insert – Control Sample.

TIP: The Open dialog box can also be displayed by selecting Insert – Control Sample from
the menu bar.
TOC-LCPH/CPN 167
3. Select the control sample to be inserted, and click Open.

The selected control sample is inserted into the sample table.
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.
2. Select Insert – Multiple Samples.
TIP: 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.
Parameter source
168 TOC-LCPH/CPN
3. Select the parameter source file.
Item Description
Parameter source • Method
The analysis parameters of an existing method file are
used to create the samples. Click to display the
Open dialog box, and select the method file to use.
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.
5. Enter the necessary parameters.
Item Description
No. of Samples Enter the number of samples (1 – 100) to be inserted in the
group.
Start Vial 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.
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 / Sample ID Enter the sample name and sample ID using up to 64 single-
byte characters.
Index Start Select this option to append the sample names and Sample
IDs with sequential numbers. Enter a desired starting
number in the field at right.
Insert Cal. Curves / Control Select this option to insert calibration curves and control
Samples samples along with the samples.
TOC-LCPH/CPN 169
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.
7. This dialog box is used for setting the calibration curves to be inserted.
Calibration Curve list
Item Description
At the beginning of the Select this item to insert a calibration curve before the
sample group sample analysis.
Always, after "number" of Select this item to insert a calibration curve after every
samples fixed number of samples. Enter that number in the box.
Calibration Curves Displays the information related to the added calibration
curves. Up to 3 separate calibration curves may be added.
Add Displays the Open dialog box. Select the calibration curve
and click Open to add the calibration curve to the
calibration curve list.
Delete Deletes a selected calibration curve.
8. Click Next.
170 TOC-LCPH/CPN
The Sample Group Wizard (Page 4) Calibration Curve Check page is displayed.
Control Sample selection
9. Select the control samples to be inserted with the calibration curves.
Item Description
Control Sample selection Select the control sample to be attached to the calibration curve. Click
to display the Open dialog box, and select the control sample.
These parameters can be entered for each calibration curve selected in Sample
Group Wizard (Page 3) Calibration Curves. This parameter is disabled if a
calibration curve was not selected.
10. Click Next.

The Sample Group Wizard (Page 5) Controls page is displayed.
Control Templates list
11. Select the control samples to be inserted.
TOC-LCPH/CPN 171
Item Description
At the beginning of the Select this item to insert a control sample before sample measurement.
sample group
Always, after "number" Select this item to insert a control sample after every fixed number of samples.
Samples Enter that number in the box.
At the end of the sample Select this item to insert a control sample at the and of the sample measurements.
group
Control Templates Displays the information related to the added control samples. Up to three
separate Control Samples may be added.
Add Displays the Open dialog box. Select the control sample and click Open to add the
control sample to the control sample list.
Delete Deletes a selected control sample.
12. Click Finish.

The group of samples are inserted into the sample table.
5.4.5 Inserting a Schedule

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.

Note: If there is an empty row above the insertion position, it is filled with
the new content.
172 TOC-LCPH/CPN
¬From the Menu
Procedure
1. Select the row of the sample table where the schedule content is to be added.
Note: The schedule content will be inserted above the selected row.
2. Select File – Import Schedule File in the menu bar.

3. Select the schedule file, and click Open.
The schedule content is inserted into the sample table.
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.
Note: If the system does not contain an ASI-L, this item is not displayed.
Procedure
1. Open a completed sample table and click .
TIP: The Vial Settings dialog box can also be displayed by selecting View – Vial Settings
from the menu bar.
TOC-LCPH/CPN 173
The Vial Settings dialog box is displayed.
Table Vial arrangement
Enter the sample vial numbers.

This diagram represents using the ASI-L to analyze samples in 24 mL vials.
Item Description
Table 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. Refer
to "Entering Vial Numbers" on page 175 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.
Vial arrangement 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.
The arrangement drawing differs depending on the ASI-L type and
connection condition. Refer to "Vial Arrangement Drawing Types"
on page 176.
Vial Move the mouse pointer over a vial icon and click to display the
vial's number.
is displayed if the total injection volume exceeds the vial
capacity.
Required Displays the amount of sample required for the vial displayed in the
above Vial field.
Off-Line Select a cell in the Vial, Ex.1, Ex. 2, or Ex. 3 columns, and enter a
"0" to conduct sampling from the sampling tube on the left side of
the instrument.
2. After all of the parameters are entered, click OK.

The vial numbers are entered into the sample table and the window closes.
174 TOC-LCPH/CPN
¬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.
2. Position the cursor precisely over the lower right corner of the selected cell until "+"
is displayed.
3. 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.
TIP: Dragging while holding down the Ctrl key, will enter numbers identical to that in the
original cell.
TOC-LCPH/CPN 175
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
These images are dependant on the number of vials and vial type.
176 TOC-LCPH/CPN
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.
TOC-LCPH/CPN 177
1. Select a cell and enter the desired text.
2. Position the cursor over the lower right corner of the selected cell until "+" is
displayed.
3. 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.
TIP: Dragging while holding down the Ctrl key, will enter numbers identical to that in the
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 Section 5.3.7 "Reviewing
and Editing a Calibration Curve" on page 146.
• Unknown
Displays the Sample / Method Properties window. Refer to Section 5.3.8 "Reviewing
and Editing a Method" on page 152.
• Control
Displays the Control Sample Properties window. Refer to Section 5.3.9 "Reviewing and
Editing a Control Sample" on page 156.
178 TOC-LCPH/CPN
Using Double-Click
Procedure
1. Double-click on the left cell of the sample row.
The Properties window of the sample is displayed.
TIP: 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.
TOC-LCPH/CPN 179
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 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.
180 TOC-LCPH/CPN
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.
Note: 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.
¬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.
Note: 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.

3. Select the row where the data is to be pasted.
Note: 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.
TOC-LCPH/CPN 181
4. Click Edit – Paste.
The data is pasted into the selected row.
5.4.9 Deleting a Sample

Rows in the sample table can be deleted.
Note: 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.
182 TOC-LCPH/CPN
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.
TOC-LCPH/CPN 183
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.
5.5.1.1 Opening the Sample Window
Procedure
1. Click .
The Sample Window is displayed.
TIP » The Sample Window can also be displayed by selecting View – Sample Window.
Graph Format Graph Area Sample Selection
Sample Information List
Injection Table
TIP » 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.
184 TOC-LCPH/CPN
Item Description
Graph Format Set the graph format to Current Peak, All Peaks, or Cal. Curve.
•
Displays the peak profile of the selected injection in the table.
•
Displays all the injection peaks in the table.
•
Displays the calibration curve peak. This is not enabled
during analysis.
Sample Selection Select the sample (row) for display from the sample table.
• Sample number/Row number: Select a sample to display.
• : Display the first sample.
• : 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
List peak profile for that sample in the graph area.
Injection Table If the sample was analyzed by more than one analysis method,
several tabs are displayed at the bottom of the 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.
2. To close the Sample Window, click again.

The Sample Window closes.
5.5.1.2 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.
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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.
Cancel Click this to return the graph display to the default parameters, and
close the dialog box.
¬Full Scale
Use the following procedure to adjust the graph scale to enlarge the largest peak to full
scale.
Procedure
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
2. Select Auto Adjust.
3. Click X Axis, Y Axis or X,Y Axis, as appropriate.
The display range is adjusted automatically.
186 TOC-LCPH/CPN
¬Default
If the graph display has been changed, it can be returned to the default range with the
following procedure.
Procedure
2. Select Scale - Default.
The display range returns to the default parameters.
TIP: Double-clicking anywhere on the graph will also return to the default display
parameters.
5.5.1.3 Copy to Clipboard
The graph can be copied to the clipboard. The copied graph can then be used by pasting it
into another software application.
Procedure
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 Section 5.3.7 "Reviewing and
Editing a Calibration Curve" on page 146.
• Unknown
Displays Sample / Method Properties window. Refer to Section 5.3.8 "Reviewing and
Editing a Method" on page 152.
• Control
Displays Control Sample Properties window. Refer to Section 5.3.9 "Reviewing and
Editing a Control Sample" on page 156.
TOC-LCPH/CPN 187
¬Using Double-Click
Procedure
1. Double-click on the left cell of the sample row.
The properties window of the sample is displayed.
TIP: 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.
2. Click .
The properties window is displayed.
188 TOC-LCPH/CPN
¬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.
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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.
2. Click View Cal. Curve.
The Calibration Curve Properties window is displayed. refer to Section 5.3.7

"Reviewing and Editing a Calibration Curve" on page 146 for details regarding the
Calibration Curve Properties window.
190 TOC-LCPH/CPN
5.5.4 Editing the Calibration Curve

The calibration curve file associated with the unknown sample or control sample can be
edited.
Procedure
1. Select the sample table row that is associated with the calibration curve you wish to
view.
TIP » 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.

3. Confirm or change the calibration curve.
Tab
Item Description
Tab Select a tab to view the calibration curve for each tab.
The number of tabs displayed depends on the Analysis Type. In the
above example, the Analysis Type is TC.
Cal. Curve for Conc. Calculation Select this item to change the calibration curve. Click to
display the Open dialog box, and select the new calibration curve file.
Note: If the check mark is omitted, the new calibration curve will not be
reflected in the concentration calculation.
4. Click OK.
The changes are saved, and the dialog box closes.
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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.
2. Click Exclude to remove the result from the calculation.
An exclusion confirmation box is displayed

TIP: The exclusion confirmation box can also be displayed by selecting the relevant row,
and clicking Edit – Exclude/Include Injections.
3. Click Yes.
The selected injection result is excluded.
Remove the exclusion by performing the procedure again.
192 TOC-LCPH/CPN
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.
¬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.
TIP: 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.
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
1. Select the sample that you wish to clear. To select a sample, click the left cell of the
sample row.
TIP: 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.
key and clicking on the samples to be added.
2. Select Edit – Clear Measured Data – Highlighted.
The clear confirmation box is displayed.

3. Click Yes.
The selected analysis results are cleared.
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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.

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
Print settings
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Item Description
Print system information Select this option to print the selected items in the sample report.
Items selected in the frame below are not printed unless this item is
selected.
Preview Press this button to display a preview of the sample report. Refer to
Section 5.6.3.2 "Sample Report Preview" on page 200.
Select All All items in the frame are selected.
Select None All items in the frame are deselected.
Default Default system items are selected.
• Calibrations tab
• Samples tab
196 TOC-LCPH/CPN
3. Click the Graph tab to change the peak profile print options.
Graph scale settings
Item Description
Black & White Select this item to print the report in black and white.
Chart scale settings Enter the scale of the peak profile. The X axis and Y axis values are
entered separately.
• Auto: Allows the software to set suitable scale values.
• Manual: The scale is the value in the box relative to the zero point.
Preview Press this button to display a preview of the sample report. Refer to
Default Select this item to reset all of the Graph tab items to the default values.
4. Select the Miscellaneous tab to review the remaining parameters.
Header
parameters
Margin parameters Report font settings
Item Description
Margin parameters Enter the print margins in these boxes.
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Item Description
Header parameters 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 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.
Footer / Page No. Select this item to print a page number at the bottom of each sample report page.
Page Break / After Select this item to print information for each sample on a separate page of the
every sample report.
Report Font Settings • Set the font used for column headings in sample reports.
• Set the font used for the information contained in sample reports.
Preview Click this button to display a preview of the sample report before printing. Refer to
5. Click OK.
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.
198 TOC-LCPH/CPN
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.
5.6.3.1 Sample Table Preview
Procedure
1. Click .
2. Select Sample Table.
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The print preview is displayed.
TIP: The preview can also be displayed by selecting File – Print Preview – Sample Table.
3. Examine the preview.
Item Description
Print Displays the Print dialog box. If there are no problems with the preview, make the
necessary settings and print the report.
Next Page Displays the next page of the report. This button is disabled when viewing the last page
of the report.
Prev Page Displays the previous page of the report. This button is disabled when viewing the first
page of the report.
Two Page Displays two pages, side by side on 1 screen. When in the Two Page view, this button is
displayed as One Page, and returns the display to one page per screen.
Zoom In Increases the magnification of the displayed page. There are three levels of Zoom In.
Zoom Out Decreases the magnification of the displayed page. There are three levels of Zoom Out.
Close Closes the print preview window.
5.6.3.2 Sample Report Preview
¬All
Procedure
1. Click .
200 TOC-LCPH/CPN
2. Select Sample Report – All.
The preview is displayed.
TIP » The preview can also be displayed by selecting File – Print Preview – Sample Report - All.
3. Check the displayed Preview.
Reference: The operations available while displaying this are the same as those described in Section
5.6.3.1 "Sample Table Preview" on page 199.
¬Highlighted
Procedure
1. Select the samples to be previewed from the sample table.
TIP » 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.
key and clicking on them.
TOC-LCPH/CPN 201
2. Click .
3. Select Sample Report – Highlighted.
The print preview is displayed.
TIP » 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.
• Sample Report (Highlighted)
Prints the selected content of the sample table in a detailed report format.
5.6.4.1 Sample Table
Procedure
1. 1. Click .
Reference: The contents of a sample report can be selected prior to printing. Refer to Section 5.6.1
"Selecting Content to Print" on page 195.
202 TOC-LCPH/CPN
2. Select Sample Table.

TIP: The sample table can also be printed by selecting File – Print – Sample Table.
The Print dialog box is displayed.

3. Make any necessary changes and print the sample table.
5.6.4.2 Sample Report

¬All
Procedure
1. Click .
2. Select Sample Report - All.

TIP: The entire sample report can also be printed by selecting File – Print – Sample Report
- All.
3. Make any necessary changes and print the sample report.
¬Highlighted
Procedure
1. Select all of the samples to be included in the report.
TIP: 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.
TOC-LCPH/CPN 203
2. Click .
3. Select Sample Report - Highlighted.

4. Make any necessary changes and print the sample report selections.
TIP: The sample report selections can also be printed by selecting File – Print – Sample
Report - Highlighted.
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.
Reference: Refer to Section 5.6.6 "Exporting to ASCII Format" on page 207 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.
204 TOC-LCPH/CPN
Operating Procedure
1. Click File – Ascii Export Setting and then Normal or Detail.
The ASCII Export Options dialog box is displayed.

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
Output settings
Item Description
Export header information Select this option to export the selected items. The items
selected in the frame below are not exported unless this
item is selected.
Select All Selects all items in the frame.
Select None Deselects all items in the frame.
Default Selects only the software default items.
TOC-LCPH/CPN 205
• System tab
• Data tab
3. Click the Misc. tab to enter the other export option parameters such as the separator
type and whether to use quotation marks.
206 TOC-LCPH/CPN
Item Description
Separator Select the character that will separate items in the text file.
This character separates the items that reside in adjacent
sample table cells. Select from among Tabulator, Comma,
Semicolon, and Space.
Export strings in quotation Select this item to enclose text strings inside quotation
marks marks in the export text file. When selected, numerical data
may be read as text. This may prevent calculations with this
data. If a spreadsheet or other software is used to process
the output data, ensure this item is NOT selected.
4. Click OK.
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.
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.
TOC-LCPH/CPN 207
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.
2. Select either Sample Table Format or ASCII Text Format.

The Save As dialog box is displayed.
3. Enter the file name and destination path, and click Save.
The file is saved.
Reference: Refer to Section 5.4.5 "Inserting a Schedule" on page 172 for details on inserting an
existing schedule file into a sample table.
208 TOC-LCPH/CPN
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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5.7.1 Instrument Connection and Disconnection
5.7.1.1 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.
2. Click .
TIP: Connection is also possible by selecting Instrument – Connect.
The sample table editor connects to the instrument and the ready state of the
instrument is shown at the right end of the toolbar.
210 TOC-LCPH/CPN
The icon of the connected instrument in the Sample Table tab of the file viewer also
illuminates.
¬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.
TOC-LCPH/CPN 211
5.7.1.2 Disconnection
¬With an Open Sample Table
Procedure
1. While connected, click .
The Disconnect box is displayed.
TIP: 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.
212 TOC-LCPH/CPN
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 .
Reference: Refer to Section 5.7.1.1 "Connection" on page 210 to connect the instrument.
The Background Monitor window is displayed. Click the tabs to select the various
content pages.
TIP: The Background Monitor window can also be displayed by clicking Instrument –
Background Monitor while connected to the instrument.
• The following screenshot shows the TOC tab.
Graph
TOC-LCPH/CPN 213
Item Description
NDIR Indicates the analysis status. indicates a Ready status and indicates
a Not Ready status for Baseline Pos., Baseline Fluc., and Baseline Noise.
Temp. Displays the current temperature for the Furnace, Dehumidifier, and NDIR.
Supply Gas Displays the current supply pressure of the carrier gas.
Pressure
Carrier Gas Displays the current flow rate of the carrier gas.
Flow
Sparge Gas Displays the current flow rate of the sparge gas.
Flow
X1 to X50 Enlarges the Y axis scale to 50 times that of the default value. Note that the
X axis scale does not change.
Graph Displays the signal intensity from the time the Background Monitor
window is opened. The display is updated every second.
• The following screenshot shows the TN tab. This tab is displayed when
configuring settings for TN analysis.
Graph
Item Description
TN Reactor Displays the current TN reactor temperature.
Ozone Gas Displays the current supply pressure of the gas for TN ozone.
Chemiluminescence Indicates the analysis status. indicates a Ready status and
indicates a Not Ready status for Baseline Pos., Baseline Fluc., and
Baseline Noise.
X1 to X50 Enlarges the Y axis scale to 50 times that of the default value. Note
that the X axis scale does not change.
Graph Displays the signal intensity from the time the Monitor window is
opened. The display is updated every second.
214 TOC-LCPH/CPN
• The following screenshot shows the ASI tab. This tab is displayed when
configuring settings to use the ASI-L.
Graph
Item Description
ASI Power / ASI Indicates the analysis status. indicates a Ready status and
Cover indicates a Not Ready status for ASI Power and ASI Cover.
X1 to X50 Enlarges the Y axis scale to 50 times that of the default value. Note
that the X axis scale does not change.
Graph Displays the signal intensity from the time the Background Monitor
window is opened. The display is updated every second.
3. To close the Background Monitor window, click the . The window closes.
¬Not from an Open Sample Table
Procedure
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.
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5.7.3 Analysis with an ASI-L or OCT-L
Procedure
1. Open the sample table to be used and place the samples in the ASI-L accordingly.
3. Click .

4. 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.
216 TOC-LCPH/CPN
TIP: Analysis can also be started by selecting Instrument – Start Measurement after
connection is established.
5. Select the processing that will take place after analysis is complete.
TIP: To return to the sample table, click Cancel to close the Measurement Start window.
Item Description
Keep running After analysis, the system maintains the current status.
Shut down instrument After analysis, the instrument is turned off.
Sleep After analysis, the instrument enters the sleep state. The instrument
restarts automatically at the specified time. Enter the date and time for the
instrument to restart in the Auto Restart boxes.
Extra Settings If the Sleep option is selected, set the units to leave running while the
instrument is sleeping. Select the units to remain on even during the sleep
state.
6. Click Start.
Analysis starts. When measurement is complete, the results are displayed in the
sample table, and analysis ends.
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5.7.4 Analysis without an ASI-L or OCT-L
5.7.4.1 Single Sample Analysis
Procedure
1. Open the sample table to be used for analysis, and place the sample in the instrument.
3. Click .
The Meas Mode dialog box is displayed.
4. Select Normal or Non-stop Mode.
Item Description
Single Measurement stops after a single sample measurement and the
Measurement 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
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 All samples in the sample table are measured without stopping.
Measurement
5. Click OK.
218 TOC-LCPH/CPN
The TOC Measurement window is displayed.
6. Click Start.
The Analysis starts.
TIP: To return to the sample table, click Stop to close the TOC Measurement window.
7. The results are displayed in the TOC Measurement window after the measurement is
complete.
8. Examine the results, and select the type of processing to be conducted.
Result display list
Item Description
Results display list Displays the analysis results for each injection.
Exclude Select an injection result in the list and click the Exclude
button.
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.
TOC-LCPH/CPN 219
5.7.4.2 Continuous Analysis
Procedure
1. Open the sample table to be used for analysis, and place the sample in the instrument.
3. Click .
The Meas Mode dialog box is displayed.
4. Click Batch Measurement.
5. Click OK.
220 TOC-LCPH/CPN
6. Select the processing that will take place after analysis is complete.
TIP: To return to the sample table, click Cancel to close the Measurement Start window.
Item Description
Keep running After analysis, the system maintains the current status.
Shut down instrument After analysis, the instrument is turned off.
Sleep After analysis, the instrument enters the sleep state. The
instrument restarts automatically at the specified time. Enter
the date and time for the instrument to restart in the Auto
Restart boxes.
Extra Settings If the Sleep option is selected, set the units to leave running
while 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.
5.7.5 Stopping Analysis
5.7.5.1 Peak Stop
This option interrupts processing of the current injection, and analysis proceeds to the next
injection measurement.
TIP » 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.
TOC-LCPH/CPN 221
5.7.5.2 Stop (after current sample is completed)
This option stops analysis after all of the scheduled injections of the current sample have
been analyzed.
TIP » This option can also be accessed by clicking Instrument – Stop – Stop (after current sample
is completed).
Procedure
1. Click while analysis is in progress, and then select Stop (after current
sample is completed).
All analysis stops after the current sample analysis is complete.
5.7.5.3 Stop (stop all processes immediately)
This option immediately interrupts the current analysis.
TIP » This option can also be accessed by clicking Instrument – Stop – Stop (stop all processes
immediately).
Procedure
1. Click while analysis is in progress, and then select Stop (stop all
processes immediately).
The analysis stops.
222 TOC-LCPH/CPN
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
2. Click to cancel the Edit Mode and restart analysis.
The restart analysis confirmation window is displayed.
TIP » The Edit Mode can also be cancelled by selecting Instrument – Edit Mode.
3. Click OK.
The Edit Mode is cancelled, and analysis continues.
TOC-LCPH/CPN 223
5.7.7 Instrument Shutdown
5.7.7.1 Shutdown
Instrument shutdown processing takes place. The connection to the device is released when
the instrument is shut down, and thus the sample table editor can be closed and the PC can
be turned off.
Procedure
2. Click
TIP » The Shutdown dialog box can also be displayed by selecting Instrument – Shutdown.
3. Select Shut down instrument.
224 TOC-LCPH/CPN
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).
TIP » The instrument can be restarted by holding down the power switch for three seconds during
a shutdown (while the power switch's LED is flashing orange) before the power to the
instrument is switched off.
Procedure
2. Right-click on the instrument icon in the Sample Table tab of the file viewer, and
select Shutdown.
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5.7.7.2 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.
Procedure
2. Click
TIP » The Shutdown dialog box can also be displayed by selecting Instrument – Shutdown.
3. Select Sleep.
226 TOC-LCPH/CPN
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.
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.
TIP » The instrument can be brought out of the Sleep state by clicking End Sleep mode.
Procedure
2. Right-click on the instrument icon in the Sample Table tab of the file viewer, and
select Shutdown.

Note: 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.
TOC-LCPH/CPN 227
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.

2. Click the System drop down menu and select the system configuration to use.
Next, click the Table Type drop down menu and select Validation.
Note: Note that validation cannot be performed if the SSM-5000A or manual

injection kit options are set in the selected system configuration.
228 TOC-LCPH/CPN
3. 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.
TOC-LCPH/CPN 229
¬Preliminary Measurement
Execute a preliminary measurement by measuring blank water in order to stabilize the
instrument before performing validation or between measurements of each validation item.
The settings related to preliminary measurement can be changed by clicking the Settings
button.
Setting Description
Analysis Select the measurement type.
Number of samples Set the number of samples to measure.
Default Return the settings to their default state.
¬Sensitivity
The instrument's sensitivity can be verified by measuring blank water and a 30 mg/L
sample and calculating the difference between the two resulting peak areas. The settings
related to this measurement can be changed by clicking the Settings button to open the
following window.
Setting Description
230 TOC-LCPH/CPN
The sensitivity index is calculated in the following manner and output to the Notes 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.
¬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
Span Set the span concentration. An intermediate concentration point is automatically
determined based on this value.
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 following value is output to the Notes column in the sample table as the repeatability
index.
A 2-point calibration curve derived from the zero point and span point measurement
results. The repeatability index is the CV value of the concentration calculated using the
intermediate point based on this calibration curve.
A linearity of less than ± 2.0 % and a repeatability of less than 1.5 % is acceptable.
TOC-LCPH/CPN 231
¬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.
Span Set the span concentration. When the Verify CV value of target conc. is selected, the
concentration of Target is automatically calculated to be 1/10th of Span.
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.
232 TOC-LCPH/CPN
5.7.9 Maintenance Operations

Refer to Chapter 7 "Maintenance" on page 271 for specific maintenance procedures on the
various instrument components. Refer to Section 7.6 "Maintenance Menus" on page 304
for descriptions of the Maintenance menus.
TOC-LCPH/CPN 233
5.8 Display Options
5.8 Display Options
5.8.1 Sample Table

The display options for the Sample Table, such as row height, can be changed using the
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.

2. Click the tabs to switch the displayed page, and make any necessary changes to the
display parameters.
• General tab
Item Description
Columns to freeze Enter the number of columns (0 – 14) to be displayed counting from the left. This
number of columns will always be displayed even when scrolling horizontally.
234 TOC-LCPH/CPN
5.8 Display Options
Item Description
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 the Reference Source
"Origin" File column.
Wrap text Select this item to allow the text in a cell to flow to the next line without being truncated.
Bold characters for Select this item to display the column header using bold text.
column headers
Default This button selects the default settings for all of the items on this tab.
• Display Items Tab
Display Items
Item Description
Display Items The selected items are displayed as column headers in the sample table
and schedule.
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.

TOC-LCPH/CPN 235
5.8 Display Options
5.8.2 Sample Window Display Options

Display options for the Sample window, such as row height, can be changed using the
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
Columns to freeze Enter the number of columns (0 – 15) to be displayed counting from 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 Cal. Select this item to display the full filename and path for the file in the Cal.
Curve Curve column.
236 TOC-LCPH/CPN
5.8 Display Options
Item Description
Wrap text Select this item to allow the text in a cell to flow to the next line without
being truncated.
Bold characters for Select this item to display the column header using bold text.
column header
Auto fit to viewable area Select this item to ensure that when the Sample Window is opened it does
not overlay the Sample Table.
• Initial height: Enter an integer (100 – 1000) to set the initial height of the
Sample Window.
• Display Items tab
Display Items
TOC-LCPH/CPN 237
5.8 Display Options
• Graph tab
Chart scale settings
Item Description
Chart scale settings Use these items to set the X axis and Y axis scales.
• Auto: The appropriate scale is determined by the software.
• Manual: The scale is set to range from the zero point to the value
entered in the box.
Show Crosshair Select this item to display the cursor point crosshairs.
3. After all of the settings are complete, click OK. The changes are saved, and the
window is closed.
238 TOC-LCPH/CPN
5.8 Display Options
5.8.3 File Viewer Display Options

Display options for the File Viewer, such as tab position, can be changed using the
Procedure
1. Click Options – Display Settings – File View.
The File View dialog box is displayed.
Tabs to be displayed
Tab position
2. Select the tabs that will be displayed.
Item Description
Select File Types to Select each tab to be displayed in the File Viewer. The
Sample Table tab is always displayed.
Tab Position Select whether to display the tabs at the top of the File
Viewer or the bottom.
3. Click OK after the settings are complete.

The changes are saved, and the window is closed.
TOC-LCPH/CPN 239
5.8 Display Options
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.
Font setting
2. Select the font to be used.
Item Description
Font The currently selected font is displayed in the dialog box.
Click to display the Font dialog box and select the
desired font.
240 TOC-LCPH/CPN
5.8 Display Options
Change the font setting and click OK to validate the change and close the dialog box.
Item Description
Font Select the font to be used. The available fonts vary according to the fonts installed.
Font style Select the font style to be used. The available font styles vary according to the fonts
installed.
Size Select the font size to be used. The available font sizes vary according to the fonts
installed.
Script Select the character set and language to be used. The available character sets vary
according to the fonts installed.
3. Make any necessary changes and click OK.

4. Click OK in the Output Window dialog box.
The changes are saved, and the dialog box is closed.
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.
TOC-LCPH/CPN 241
5.8 Display Options
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
Font Select the font to be used. The available fonts vary
Font style Select the font style to be used. The available font styles
vary according to the fonts installed.
Size Select the font size to be used. The available font sizes vary
Script Select the character set and language to be used. The
available character sets vary according to the fonts installed.
3. After the font settings are complete, click OK.

242 TOC-LCPH/CPN
5.8 Display Options
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.
Common
number settings
Percent value
settings
2. Enter the number of decimal places to be displayed.
Item Description
Common Floating Point • Number of significant digits
Numbers Select this item to set the total number of digits to be
displayed. Enter that number in the box.
• 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.
Percent Values • Number of significant digits
displayed. Enter that number in the box.
• Number of digits after the decimal point
displayed after the decimal point. Enter that number in
the box.
3. After completing the settings, click OK.

TOC-LCPH/CPN 243
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.
Procedure
1. Click Tools – Screen Lock.
244 TOC-LCPH/CPN
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.

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.
2. Click OK.
The lock is released, and the window closes.
TOC-LCPH/CPN 245
5.9.4 Recording the Operation History

Depending on the System Policy settings, the Operation History records all operations each
time the Sample Table is saved, or whenever a properties window is closed after changes
were made.
Comments may be added to the Operation History to record various operations such as
catalyst replacement, that are not automatically recorded by the software.
Note: This function is only available to users who have Add Event Logs authority.
Procedure
2. Click the Administration tab.
3. Click the Add a Log Event button.

Note: When the User dialog box is displayed, log in according to Section
246 TOC-LCPH/CPN
The Add a Log Event dialog box is displayed.
4. Select the history category from Administration, General Operation, Create/Edit Data,
H/W Settings, Maintenance, or Error.
5. Enter a comment as necessary.
6. 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 complete descriptions of all the security functions, refer to the
TOC-LCPH/CPN Administrator Manual.
TOC-LCPH/CPN 247

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.
Note: 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
No. of Injections 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 analysis injections. If, however, the result
exceeds the SD Max. and CV Max. limit, the additional injections are performed for
confirmation. The maximum number of injections includes the analysis injections and
the additional injections.
No. of Washes Select the number of times (1 – 10) the flow line will be washed before the first
injection.
248 TOC-LCPH/CPN
Item Description
Max SD 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. of Injections setting has a larger
maximum number of injections than the number of analysis injections.
Max CV 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 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.

5.10.2 Data Storage Folders

This option determines the destination folders for saving the sample table files, method
files, calibration curve files, control sample files and schedule files.
The files saved in these default destination folders are displayed in the file viewer.
Procedure
1. Click Options – Select Data Folders.
The Select Data Folders window is displayed.
2. Click to locate the desired file location.
TOC-LCPH/CPN 249
The Folder window is displayed.
Folder tree
3. Select the appropriate destination folder from the tree structure.

Select a different drive if necessary. Click the Network button to select a folder on the
network.
4. Click OK.
The Select Data Folders window is once again displayed.
5. After all the necessary folders have been selected, click OK.
250 TOC-LCPH/CPN
5.10.3 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.

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.
3. Click OK.
This sets the conversion formula, closes the window, and displays the conversion
result in the Result column in the sample table.
TOC-LCPH/CPN 251
5.10.4 Searching for Files

File searches can be conducted based on the following procedure.
Procedure
1. Click Tools – Find Files.
The File Search dialog box is displayed.
Results display
2. Use this window to specify the search parameters.
Item Description
File Type Select this item to search by file type, then select the file type in the drop-down box.
Folder name Select this item to isolate the file search to an individual folder. Click to display
the Browse for Folder dialog box, and select the folder to be searched.
Select the Auto Folder Select to automatically determine the folder type based on the
File Type setting.
Select the Search sub-folder item to extend the search to the sub-folders of the set
folder.
User name Select this item to allow narrowing of the search based on the user name associated
with the target file(s). Enter the relevant user name in the box to the right.
252 TOC-LCPH/CPN
Item Description
Date of Creation Select this item to narrow the search based on the date the file was created. Select
either the Date or Period radio button.
• Date
Enter the beginning date in the first box and the end date in the second box.
• Period
Select from Last Week, This Week, Last Month or This Month.
Keyword Select this item to narrow the search based on a specific character string. Enter the
keyword in the box to the right.
The keyword search examines the following character strings according to file type.
Schedule files (*.txt): File names and character strings included in file are searched.
Files other than schedule files (*.txt): File names, sample names, sample IDs and
comments included in the file are searched.
Results display Search results are displayed. Click on a file name to display a summary of the file in a
tooltip.
Double-click on a file name to open the file.
Find Executes the search based on the search parameters.
Stop Stops the search. This function is only enabled while the search is in progress.
3. After the target files are located, click Close.

The dialog box closes.
5.10.5 File Organization

Files, such as, Sample table files, Calibration curve files, Method files, Control template
files, Schedule files (*.tsc) and Schedule files (*.txt) can be organized by moving them to
folders based on creation date or time period.
Procedure
1. Close all of the files currently open in the sample table editor and select Tools –
Organize Files.
TOC-LCPH/CPN 253
The File Organization wizard (Page 1)- Select the Files to be organized is displayed.
Files to be organized Current storage location
2. Select the files to be organized and the current storage folder.
Item Description
Files to be organized Select the files to be organized.
Current storage location Click to display the Folder window, and select the
current storage folder of the respective files.
3. After the selections are complete, click Next.

The File Organization wizard (Page 2)-Select output folders is displayed.
Output destination folders
254 TOC-LCPH/CPN
4. Enter the file output folders.
Item Description
Output destination folders The output destination folders are automatically entered
based on the parameters in the File Organization Wizard
(Page 1)-Select the Files to be organized page. The output
folders are renamed by appending "Bkup (creation date)" to
the respective source folder names.
To specify a different folder, click to display the
Folder window, and select an output destination folder as
desired.
5. Click Next when the settings are complete.

The File organize wizard (Page 3)- Conditions for the operation is displayed.
Move process settings Creation date settings
6. Enter the organization parameters.
Item Description
Date of Creation Select this item to organize files based on a specific time period in which the files
were created. Select either the Date or Period radio button.
• Date: Enter the beginning date in the first box and the end date in the second box.
• Period: Select from Last Week, This Week, Last Month or This Month.
Exclude Cal. Curve Select this item to exclude calibration curve parameter files from those being
Setting Files organized.
Exclude the Latest Select this item to exclude the most recent calibration curve data files from those
Cal. Curve Data being organized.
Operations Select the operation that will be used to move files from the source folder to the
output destination folder.
• Move Files: The files are moved and the original files no longer remain in the
source folder.
• Copy Files: The files are copied and the original files remain in the source folder.
7. Click Finish when the settings are complete.

The files are organized based on these settings.
TOC-LCPH/CPN 255
5.10.6 Online Manual

This documentation can be displayed and viewed on the PC screen.
Note: The online manual is in PDF format. The Adobe Reader is required to display
this manual. Select your operating system and language in the [Extra] - [Adobe
Reader] folder on the Acrobat Reader installation disc and execute the
corresponding setup file to install the software. For information on the operations
used in conjunction with the online manual, refer to the Adobe Reader instruction
manual and Help function.
5.10.6.1 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-LCPH/CPN.
TIP » 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.
256 TOC-LCPH/CPN
5.10.6.2 Displaying the Online Manual
The online manual is displayed using the following procedure.
Procedure
1. Click Help – Online Manual.
The online manual is displayed.
5.10.7 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.
TOC-LCPH/CPN 257
258 TOC-LCPH/CPN
6
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.
6.2 Gas Sample Analysis
This section describes the measurement of gas 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
6.1.1.1 Installation
Procedure
1. Remove the knurled thumbscrew that secures the slider then remove the TC/TN
injector slider.
Slider
Knurled thumbscrew
Figure 6.1 Removing the Slider
2. Install the TC/TN block provided in the kit.
TC/TN block
Figure 6.2 Installing the TC/TN Block
260 TOC-LCPH/CPN
3. Remove the slider of the IC injector in the same manner and install the IC block
provided with the manual injection kit.
IC block
Figure 6.3 Installing the IC Block
Note: When installing the block, be sure that it is properly aligned with
the injection port.
6.1.1.2 System Configuration
Select Manual Injection Kit in the Instrument Setup Wizard Options page during initial
system configuration.
Reference: Refer to Section 5.1.1 "Creating a New System Configuration" on page 110 for information
on creating a system configuration.
Note: The sample injector syringe will not operate when the Manual Injection Kit item
is selected.
TOC-LCPH/CPN 261
6.1.2 Measurement
6.1.2.1 Calibration Curve Measurement
Use the following procedure to perform calibration curve measurement.
Reference: Refer to Section 5.3.2 "Creating a Calibration Curve File" on page 126 for details on
generating a calibration curve.
Refer to Section 5.3.1 "Creating a Sample Table" on page 125 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 Section 6.1.1.2 "System Configuration"
on page 261.
• 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.
2. Create a Sample Table.
• System
on page 261.
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.
Note: 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.
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.
Note: 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.
262 TOC-LCPH/CPN
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.
6.1.2.2 Sample Measurement
Use the following procedure to perform sample measurement.
Reference: Refer to Section 5.3.3 "Creating a Method" on page 133 for details on creating a method.
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 Section 6.1.1.2 "System Configuration" on page
261.
• Calibration Curve 1
This item is found on the Method Wizard (Page 3) Calibration Curve page. Select
the calibration curve file created in Section 6.1.2.1 "Calibration Curve
Measurement"
This item is found on the Method Wizard (Page 4) Analysis Parameters page.
• The other parameters may be set as appropriate.
• System
on page 261.
3. Drag the created method from the file viewer into the Sample Table.
6. Draw an appropriate amount of sample into the syringe.
syringe for analysis.
Set.
8. Verify that the instrument status is READY and click Set.
TOC-LCPH/CPN 263
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.
264 TOC-LCPH/CPN
6.1.4 Manual Injection Kit Maintenance
6.1.4.1 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.
CAUTION
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.
6.1.4.2 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.
Table 6.1 • Gas-Tight Syringes (Option)

Part Name P/N Capacity
Gas-tight syringe set 25 uL S638-60733-02 25 uL*
Gas-tight syringe set 50 uL -03 50 uL*
Gas-tight syringe 1 mL S046-00026-02 1 mL
Gas-tight syringe set 5 mL -03 5 mL
* Set comprises one replacement gas-tight syringe needle and one plunger.
TOC-LCPH/CPN 265
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
CAUTION
• 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
6.2.2.1 Installation of the Manual Injection Kit
Install the manual injection kit by referring to Section 6.1 "Manual Injection Measurement
(H Type Only)" on page 260 and then create a system configuration.
266 TOC-LCPH/CPN
6.2.3 Measurement
6.2.3.1 Calibration Curve
Use the following procedure to perform calibration curve measurement.
Procedure
1. Prepare a standard gas sample with a known carbon concentration.
Note: 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
Select the system configuration created in Section 5.1.1 "Creating a New System
Configuration" on page 110.
This item is found on the Calibration Curve Wizard (Page 4) Plot Settings page.
• Enter the other parameters as appropriate.
Reference: Refer to Section 5.3.2 "Creating a Calibration Curve File" on page 126 for details on
generating a calibration curve.
sample table.
• System
4. Drag the created calibration curve from the file viewer into the Sample Table.
7. Draw an appropriate amount of sample into the gas-tight syringe.
gas-tight syringe for analysis.
Set.
TOC-LCPH/CPN 267
6.2.3.2 Sample Measurement
Use the following procedure to perform sample measurement.
Reference: Refer to Section 5.3.3 "Creating a Method" on page 133 for details on creating a method.
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 Section 5.1.1 "Creating a New System
• Calibration Curve 1
This item is found on the Method Wizard (Page 3) Calibration Curve page. Select
the calibration curve file created in Section 6.2.3.1 "Calibration Curve" on page
267
This item is found on the Method Wizard (Page 4) Analysis Parameters page.
• The other parameters may be set as appropriate.
• System
3. Drag the created method from the file viewer into the Sample Table.
6. Draw an appropriate amount of sample into the gas-tight syringe.
268 TOC-LCPH/CPN
gas-tight syringe for analysis.
Set.
6.2.4 Manual Injection Kit Maintenance
6.2.4.1 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
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.
CAUTION
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.
TOC-LCPH/CPN 269
6.2.4.2 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.
Table 6.2 • Gas-Tight Syringes (Option)

Part Name P/N Capacity
Gas-tight syringe set 25 uL S638-60733-02 25 uL*
Gas-tight syringe 1 mL S046-00026-02 1 mL
* Set comprises one replacement gas-tight syringe needle and one plunger.
Table 6.3 • Relationship Between Appropriate Peak Height and (CO2) Gas
Concentration / Injection Volume *
Gas Concentration (CO2) Gas Injection Volume
TC 100 ppm 10 mL
1000 ppm 1 mL
1% 500 uL
10 % 300 uL
100 % 30 uL
IC 100 ppm 6 uL
1000 ppm 600 uL
1% 300 uL
10 % 200 uL
100 % 20 uL
* The values listed in this table should be regarded as reference values only as slight
differences in data may occur between individual instruments.
270 TOC-LCPH/CPN
7
7Maintenance
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.
7.2 Periodic Inspections
Describes periodic inspection procedures for the TOC-L.
7.3 Autosampler (ASI-L) Maintenance
Describes periodic inspection procedures for the ASI-L.
7.4 8-Port Sampler (OCT-L) Maintenance
Describes periodic inspection procedures for the OCT-L.
7.5 TN Unit (TNM-L) Maintenance
Describes periodic inspection procedures for the TNM-L.
7.6 Maintenance Menus
Describes maintenance menu functions controlled by the TOC-Control L
software.
7.7 Troubleshooting
Describes the error messages and troubleshooting procedures.
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 Section 3.1.8 "Preparation of Dilution Water" on page 43.
7.1.2 Checking Acid

Verify that the acid volume is adequate for analysis. If necessary, replenish the acid as
described in Section 3.1.9 "Acid Preparation" on page 44. Any container such as a small-
mouth glass 1 liter bottle can be used.
7.1.3 Checking Drain Vessel Water Level

Rubber cap Drain discharge tubing
Cooler drain vessel
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).
Reference: Refer to Section 3.1.6 "Water Supply to the Cooler Drain Vessel" on page 41 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.
272 TOC-LCPH/CPN
7.1.4 Checking Humidifier Water Level
Water supply port
Humidifier
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.
TOC-LCPH/CPN 273
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.
CAUTION
The ability to absorb halogen stops if the amount of liquid in the B-type halogen
for absorption.
274 TOC-LCPH/CPN
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 Section 7.2.2
"Washing or Replacing Catalyst" on page 277.
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.
Reference: Refer to Section 5.7.1.1 "Connection" on page 210 for the procedure for connecting to the
Instrument.
TOC-LCPH/CPN 275
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.
TIP » 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.
4. After the process is complete, click Close.
The window closes.
CAUTION
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.
276 TOC-LCPH/CPN
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 Section 7.2.1 "Catalyst Regeneration" on page 275.
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 Section 3.1.3 "Connecting the
Combustion Tube" on page 27.
CAUTION
• Combustion tubes are made of quartz glass. Always wear protective leather
• Do not use wrenches or other such tools. Doing so could break the combustion
tube and cause injury.
Removal Procedure
sample injector.
Slider retaining
screw
Slider

Hexagon cap nut
Sample injector
Drain tubing
TOC-LCPH/CPN 277
3. Loosen the hexagon cap nut on the PTFE coupling located on the cooling tubing inlet
at the bottom end of the combustion tube.
together with the combustion tube in the upward direction.
Sample injector
Drain tubing
Combustion
tube
Y-shaped fitting
Figure 7.4 Removing the Combustion Tube
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.
278 TOC-LCPH/CPN
CAUTION
• 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 Section 3.1.1 "Catalyst Filling" on page 22.
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.
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.
TOC-LCPH/CPN 279
Removing the Carrier Gas Purification Tube (Option)
CAUTION
Allow the electric furnace to cool to room temperature for at least six hours after
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 Section 3.1.3 "Connecting the Combustion Tube" on page 27.
3. Extract the carrier gas purification tube from the electric oven by pulling upward.
Replacing Catalyst
CAUTION
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.
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.
Note: 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.
280 TOC-LCPH/CPN
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 Section 7.2.2 "Washing or Replacing
Catalyst" on page 277.
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.
Reference: For details on replacing the CO2 absorbers, refer to Section 3.1.10 "Installation of the CO2
Absorber" on page 45.
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".
TOC-LCPH/CPN 281
1. Unclip the upper and lower clips that secure the halogen scrubber.
2. Disconnect the Viton connectors and remove the halogen scrubber. Release the white
plastic clamp that secures the Viton connector while twisting it in the vertical
direction.
3. Remove the film at both ends of the new halogen scrubber and connect it to the Viton
connectors.
4. Secure the halogen scrubber with the two clips in its original position.
Replace scrubber when

discoloration band reaches
Gas flow direction this point
Dehumidifier To sample
cell inlet
Halogen Reactant-filled cylinder
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.
Halogen scrubber
(take note of the
arrow direction)
Figure 7.6 Halogen Scrubber Replacement
282 TOC-LCPH/CPN
7.2.8 Syringe Replacement

Use the procedure below to replace the syringe.
CAUTION
• 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.
Reference: Refer to Section 5.7.1.1 "Connection" on page 210 for the connection procedure.
configuration icon, and click Maintenance – Change Syringe.
TOC-LCPH/CPN 283
The Syringe Change window is displayed.
TIP » 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.
8-port valve
Syringe
Plunger Plunger retaining screw
Plunger holder
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.
284 TOC-LCPH/CPN
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.
CAUTION
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.
TOC-LCPH/CPN 285
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.
1. Remove the syringe referring to Section 7.2.8 "Syringe Replacement" on page 283.
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.
Plunger tip
Plunger tip seat
Figure 7.9 Installing the New Plunger Tip (cross-section)
Note: • 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.
286 TOC-LCPH/CPN
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)
White O-ring
Top
Rounded
side
Bottom
Black O-ring
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.
CAUTION
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.
TOC-LCPH/CPN 287
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.
CAUTION
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.
2. Remove the nut using the provided wrench.
Rotor drive
component
mark
Interrupt plate
8-port valve
Wrench
Figure 7.11 Removing the Nut
288 TOC-LCPH/CPN
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.
Retaining nut
Wrench
Figure 7.12 Removing the Retaining Nut
5. Remove the spring-equipped rod.

6. Grasp the rotor with pliers and pull it out.
Rotor
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.
Note: Perform the syringe pump zero detection procedure before analysis.
Refer to Section 7.6 "Maintenance Menus" on page 304.
TOC-LCPH/CPN 289
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
CAUTION
The carrier gas pressure applied to the carrier gas purifier CO2 absorber is
approximately 200 kPa. It is dangerous to perform this maintenance procedure
under these conditions. Before replacing the soda lime, lower the carrier gas
pressure in the instrument to normal as follows:
• Turn the supply valve of carrier gas source OFF.
• Switch OFF the instrument.
Procedure
1. Remove the elbow joints on the CO2 absorber for carrier gas purification, which is
located in the holder on top of the instrument.
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.
CAUTION
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.
CAUTION
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.
290 TOC-LCPH/CPN
6. Using the elbow joints, connect the carrier gas purifier CO2 absorber to the two tubes
exiting the back of the instrument as follows:
• 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"
CAUTION
Only tighten the nuts on the elbow joints by hand. Do not use tools.
7. Place the CO2 absorber for carrier gas purification in the holder on top of the
instrument.
Used soda lime should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the
material contains soda lime.
CAUTION
Soda lime is a corrosive chemical substance. Be careful not to touch it with bare
hands. For details, refer to Section 8.9 "Material Safety Data Sheets" on page
376.
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
Section 3.1.13 "IC Analysis Preparations" on page 51.
CAUTION
The IC reaction solution is acidic. Use care not to spill or touch the fluid when
handling it. For details, refer to Section 8.9 "Material Safety Data Sheets" on
page 376.
TOC-LCPH/CPN 291
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.
CAUTION
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 Section 8.9
Use the following procedure to replace the rubber tubing of the pump head.
1. Grasp the front and rear stops of the pump head by hand. Pull the white pump head
from the black pump body.
2. Disconnect both of the yellow rubber tubes on the left side of the pump head from the
PTFE tubing.
3. Connect the new rubber tubing to the PTFE tubing of the pump head.
4. Replace the pump head by following the above procedure in reverse.
IC reagent
delivery pump
Pump head
Figure 7.14 Replacing the Pump Head of the IC Reaction Solution Pump
292 TOC-LCPH/CPN
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,
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 Section 3.1.14 "Preparation for POC analysis
(When Using the Optional POC Kit)" on page 54.
CAUTION
• 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.
TOC-LCPH/CPN 293
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.
CAUTION
The ability to absorb halogen stops if the amount of liquid in the B-type halogen
for absorption.
294 TOC-LCPH/CPN
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.
Rinse tubing
Rinse bottle
Figure 7.15 Rinse Bottle Inspection
7.3.2 Sample Catcher Inspection

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.
CAUTION
Corrosion of the instrument may occur if spilled sample is allowed to remain in
the sample catcher. Keep the sample catcher clean.
TOC-LCPH/CPN 295
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.
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. Grasp the latch on the pump head by hand and pull the white pump head from the
black pump body.
3. On the left side of the pump head, disconnect both of the yellow rubber tubing from
the PTFE tubing.
4. Connect the new rubber pump head tubing to the PTFE tubing.
5. Replace the pump head by following the above procedure in reverse and then replace
the pump access cover.
Pump head
Latch
Rubber tubing
Figure 7.16 Replacing the Pump Head of the Rinse Pump
296 TOC-LCPH/CPN
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.
CAUTION
Switch OFF the power before replacing to the 8-port valve rotor.
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.
Note: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.
Cover
Nut
8-port valve
Wrench
Figure 7.17 Removing the Nut
TOC-LCPH/CPN 297
4. Remove the 8-port valve by pulling it downward.

5. Loosen the retaining nut using the provided wrench.
Retaining nut
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.
7. Note the orientation of the rotor hole position. Grasp the rotor with forceps, and
remove by pulling upwards.
Rotor
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.
298 TOC-LCPH/CPN
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 Section 5.7.7 "Instrument Shutdown" on page 224.
CAUTION
The interior of the ozone treatment unit is heated to 50°C. Perform maintenance
only after cooling for at least two hours.
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.
Ozone treatment
unit (right side of
Ozone exhaust tubing the electric furnace)
Figure 7.20 Removing the Ozone Treatment Unit
TOC-LCPH/CPN 299
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.)
Gas inlet
About 2 cm
Polypropylene
packing material
Catalyst
Wiring bands
Fluoro rubber plug
Gas outlet
Ozone treatment unit Filling with catalyst
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.
CAUTION
The ozone exhaust tubing must be replaced with a new one each time the
catalyst is replaced.
5. Return the ozone treatment unit to its original position in the instrument and reconnect
the tubing to each end of the unit.
CAUTION
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.
300 TOC-LCPH/CPN
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 8000 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.
Reference: Refer to Section 5.7.1.1 "Connection" on page 210 for the connection procedure.
configuration icon, and click Maintenance – History.
The Maintenance History Dlg window is displayed.
TOC-LCPH/CPN 301
TIP » The Maintenance History Dlg window can also be displayed by selecting Instrument –
Maintenance – History.
3. Examine the number in the Current field for Ozone Generator.
CAUTION
If the ozone generator is used after 8000 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.
302 TOC-LCPH/CPN
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 Section 7.2.6 "Replacing the CO2 Absorber" on page 281), 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.
Reference: Refer to Section 3.1.15.1 "Installation of the NOx Absorber" on page 55 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.
TOC-LCPH/CPN 303
This section describes the Maintenance operations used to conduct instrument maintenance
and checking instrument operation.
Note: The Sample Table editor must be connected to the instrument to access the
Maintenance menu. Refer to Section 5.7.1.1 "Connection" on page 210 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.
304 TOC-LCPH/CPN
¬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 Section 7.2.1 "Catalyst
Regeneration" on page 275.
¬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 Section 3.1.13 "IC Analysis
Preparations" on page 51.
TOC-LCPH/CPN 305
¬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.
306 TOC-LCPH/CPN
¬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
Syringe Pump Click the buttons to move the syringe pump to the Zero, Home and
Sparge positions.
Click the Reset button to move the plunger to the highest position.
Solenoid Valves Use the Open and Close buttons to open and close the following
(Combustion and Option) solenoid valves.
• IC Drain
• Carrier gas
• Sparge Gas
• POC
Port Select Click a numbered button to open the flow line between the syringe
and the injection port. The numbered buttons correspond to the port
numbers of the 8-port valve.
Acid Pump Click Open to turn the IC reagent delivery pump on, and Close to
turn it off.
TC Inj. Port Click Drain or Meas to move the TC slider to the drain or injection
position.
IC Inj. Port Click Drain or Meas to move the IC slider to the drain or injection
position.
TOC-LCPH/CPN 307
ASI/8 Port Sampler Tab

The enabled items will vary depending on the optional accessories connected.
Item Function
Rinse Click On and Off to start and stop the ASI-L flow line rinsing operation.
Move Tray Click the left and right buttons to move the ASI-L vial rack left and right. Click
Reset to return the rack to the home position.
Arm Click the up and down buttons to move the arm up and down. Click Reset to
return the arm to the home position.
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.
Vial Position Enter a vial position number, and then click the Move button to move the arm to
the specified position.
Magnetic Stirrer Click On and Off to start and stop the magnetic stirrer operation.
¬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.
308 TOC-LCPH/CPN
¬Change Syringe
This function is used when installing and replacing a syringe. For details of the procedure,
refer to Section 3.1.5 "Installing the Syringe" on page 38, or Section 7.2.8 "Syringe
Replacement" on page 283.
¬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 Section 3.1.18.2 "TC Blank Check Analysis" on page 64.
¬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 and last replacement date for the
CO2 absorber).
• 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
TOC-LCPH/CPN 309
TIP » 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.
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.
¬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.
310 TOC-LCPH/CPN
7.7 Troubleshooting
7.7 Troubleshooting
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
ERROR: Find zero point Failed to detect the syringe zero point. Switch off power to the instrument. Switch
on the power again, operate the instrument,
and verify whether the same error occurs
again.
ERROR: No vial rack Operation cannot continue because the vial Mount the vial rack in the turntable and
rack is not mounted in the turntable. execute the operation again.
ERROR: Rack type Measurement cannot be performed because Verify the type of vial rack mounted in the
mismatch the vial rack specified in the settings differs instrument.
from the detected vial rack.
ERROR: Battery The battery voltage has depleted. Switch off power to the instrument. Contact
replacement your Shimadzu representative as this
problem requires servicing.
ERROR: No Acid The volume of hydrochloric acid used has Replenish the hydrochloric acid in the acid
exceeded the threshold value set in the vessel and then reset the Total Acid Vol
Maintenance History window. counter in the Maintenance History window.
ERROR: Sample volume The volume of sample injected into the Regenerate or replace the catalyst, replace
count combustion tube has exceeded the threshold the combustion tube, and then reset the Total
value set in the Maintenance History TC Inj Vol counter in the Maintenance
window. History window.
ERROR: Move syringe The number of syringe strokes has exceeded Replace the plunger tip and then reset the
count the threshold value set in the Maintenance Syringe Strokes counter in the Maintenance
History window. History window.
ERROR: TC furnace The temperature of the TC furnace is too low Wait for the electric furnace to rise to the set
temperature during to regenerate catalyst. temperature before executing catalyst
regeneration regeneration.
ERROR: ASI cover open The ASI needle cover or sample cover is Close the ASI needle cover or sample cover.
open.
ERROR: IC acid pump The operation time of the IC pump has Replace the IC pump tube and then reset the
exceeded the threshold value set in the IC Unit Pump (hour) counter in the
Maintenance History window. Maintenance History window.
TOC-LCPH/CPN 311
7.7 Troubleshooting

ERROR: ASI rinse pump The operation time of the ASI pump has Replace the ASI pump tube and then reset
exceeded the threshold value set in the the ASI Rinse Pump (hour) counter in the
Maintenance History window. Maintenance History window.
WARNING: 8port valve The number of operations of the 8-port valve Replace the 8-port valve rotor and then reset
rotor operation has exceeded the value set in the the 8Port Valve Operation (no.) counter in
Maintenance History window. the Maintenance History window.
WARNING: Ozonizer The operation time of the ozone generator Replace the ozone generator and then reset
operation time has exceeded the value set in the the Ozonizer Operation Time (hour) counter
Maintenance History window. in the Maintenance History window.
WARNING: CO2 absorber The CO2 absorber has exceeded its expiry Replace the CO2 absorber and then reset the
date. date for CO2 Absorber, replaced on in the
Maintenance History window.
WARNING: ASI stirrer The operation time of stirrer motor 1 has Replace stirrer motor 1 and then reset the
motor 1 exceeded the value set in the Maintenance ASI Stirrer(1) Operation (hour) counter in
History window. the Maintenance History window.
WARNING: OCT(1) 8port The number of operations of the OCT-L (1) Replace the OCT-L (1) 8-port valve and then
valve operation 8-port valve has exceeded the value set in the reset the OCT-L(1) 8 Port Valve Operation
Maintenance History window. (no.) counter in the Maintenance History
window.
WARNING: OCT(2) 8port The number of operations of the OCT-L (2) Replace the OCT-L (2) 8-port valve and then
valve operation 8-port valve has exceeded the value set in the reset the OCT-L(2) 8 Port Valve Operation
Maintenance History window. (no.) counter in the Maintenance History
window.
312 TOC-LCPH/CPN
7.7 Troubleshooting

WARNING: TOC-L carrier The carrier gas pressure is too low. Check the condition of the carrier gas supply.
gas pres low
ERROR: ASI vial cover If the vial cover opened state is not Before starting measurement based on a
sensor recognized although measurement has been schedule, open the vial cover once and check
conducted for more than 200 vials, the that an error message is displayed, to ensure
sensor may be faulty. This error may also that the sensor is working correctly.
occur due to false recognition when vials are If the sensor is not working correctly, contact
changed while the power is off. your Shimadzu representative as this
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.
Table 7.2 • Fatal Error Messages

ERROR: Flash ROM An error occurred while writing to memory. Switch off power to the instrument. Contact
your Shimadzu representative as this
ERROR: Furnace overheat The electric furnace overheated. With the power on, wait approximately 20
minutes for the temperature of the electric
furnace to decrease and then switch off the
instrument. Switch on the power again,
operate the instrument, and verify whether
the same error occurs again.
ERROR: Furnace error The temperature of the electric furnace does Switch off power to the instrument. Switch
not rise. on the power again, operate the instrument,
again.
ERROR: Carrier gas flow The carrier gas flow rate does not reach the Check the condition of the carrier gas supply.
control error ! set value.
ERROR: Syringe pump The syringe is not operating normally due to Switch off power to the instrument and
clogging of the tubing connected to the 8- remove any foreign particles from the
port valve. tubing. Switch on the power again, operate
the instrument, and verify whether the same
error occurs again.
ERROR: Syringe pulse A problem occurred during syringe Switch off power to the instrument. Switch
count operation. on the power again, operate the instrument,
again.
TOC-LCPH/CPN 313
7.7 Troubleshooting

ERROR: 8Port valve A problem occurred during 8-port valve Switch off power to the instrument. Remove
position operation. the rotor from the 8-port valve, remove any
particles found in the valve, and wash the
valve.
ERROR: 8Port valve pulse The 8-port valve is not operating normally Switch off power to the instrument. Remove
count due to clogging inside the sample injector 8- the rotor from the 8-port valve, remove any
port valve. particles found in the valve, and wash the
valve.
ERROR: TC slider position The TC slider is not operating normally due Switch off power to the instrument and
to particles trapped between its moving remove any particles. Switch on power again
parts. after removing the cause of the error.
ERROR: IC slider position The IC slider is not operating normally due Switch off power to the instrument and
to particles trapped between its moving remove any particles. Switch on power again
parts. after removing the cause of the error.
ERROR: Zero detection A problem occurred during syringe Switch off power to the instrument. Switch
operation. on the power again, operate the instrument,
again.
ERROR: ASI arm vertical The ASI arm is not operating normally in the Switch off power on the TOC-L main unit.
position vertical direction. Switch on the power again, operate the
ERROR: ASI arm vertical The ASI arm is not operating normally in the instrument, and verify whether the same
pulse count vertical direction. error occurs again.
Since the problem is unrelated to the TOC-L
ERROR: ASI arm The ASI arm is not operating normally in the
main unit, disconnect the ASI-L from the
horizontal position horizontal direction.
main unit, and perform operations using the
ERROR: ASI arm The ASI arm is not operating normally in the TOC-L main unit alone until normal
horizontal pulse count horizontal direction. operation of the ASI-L is restored.
ERROR: ASI tray position The ASI turntable is not operating normally. Switch off power to the instrument. Switch
again.
ERROR: ASI tray pulse The rotation direction of the ASI turntable Switch off power on the TOC-L main unit.
count could not be detected. Either the rack is not Make sure the rack is properly seated on the
properly seated in the turntable or some ASI-L turntable and remove any objects that
object may be blocking a position detection may be blocking the position detection notch
notch on the periphery of the rack. on the periphery of the rack. After
eliminating the cause of the problem, close
the ASI-L cover and switch on power to the
instrument again.
ERROR: SSM_TC sample The photocouplers (two locations) for Switch off power to the instrument. Contact
boat position detecting the position of the TC sample boat your Shimadzu representative as this
are not operating correctly. (Both problem requires servicing.
photocouplers are detecting that light is
blocked.)
314 TOC-LCPH/CPN
7.7 Troubleshooting

ERROR: SSM-IC sample The photocouplers (two locations) for Switch off power to the instrument. Contact
boat position detecting the position of the IC sample boat your Shimadzu representative as this
are not operating correctly. (Both problem requires servicing.
photocouplers are detecting that light is
blocked.)
ERROR: 8Port Sampler1 - The OCT-L (1) 8-port valve is not operating Switch off power to the instrument. Remove
8Port Valve Position normally due to clogging inside the valve. the rotor from the OCT-L (1) 8-port valve
and either remove any particles found in the
valve or wash the valve.
ERROR: Dehumidifier fan The fan on the electronic cooler has stopped. Switch off power to the instrument. Switch
stopped ! on the power again, operate the instrument,
again.
ERROR: ASI emergency The ASI encountered an emergency stop. Switch off power to the instrument. Switch
again.
ERROR: Main fan stopped ! The instrument fan has stopped. Switch off power to the instrument. Switch
again.
ERROR: TC Furnace power The power supply to the electric furnace is Switch off power to the instrument. Switch
error! not operating normally. on the power again, operate the instrument,
again.
ERROR: Dehumidifier The temperature controller of the cooler is Switch off power to the instrument. Switch
temperature error ! not operating normally. on the power again, operate the instrument,
again.
ERROR: TOC detector The temperature controller of the TOC Switch off power to the instrument. Switch
temperature error ! detector is not operating normally. on the power again, operate the instrument,
again.
TOC-LCPH/CPN 315
7.7 Troubleshooting

ERROR: TOC detector The motor drive of the TOC detector is not Switch off power to the instrument. Switch
motor error ! operating normally. on the power again, operate the instrument,
again.
ERROR: TOC detector A memory error occurred inside the TOC Switch off power to the instrument. Switch
memory error ! detector. on the power again, operate the instrument,
again.
ERROR: TOC detector The TOC detector is not connected properly. Switch off power to the instrument. Switch
connection error ! on the power again, operate the instrument,
again.
ERROR: TN detector The temperature controller of the TN Switch off power to the instrument. Switch
temperature error ! detector is not operating normally. on the power again, operate the instrument,
again.
ERROR: TN detector A memory error occurred inside the TN Switch off power to the instrument. Switch
memory error ! detector. on the power again, operate the instrument,
again.
ERROR: TN detector The TN detector is not connected properly. Switch off power to the instrument. Switch
connection error ! on the power again, operate the instrument,
again.
ERROR: TN detector fan The TN detector fan has stopped. Switch off power to the instrument. Switch
again.
ERROR: Ozone pressure An error occurred in the pressure sensor for Switch off power to the instrument. Switch
sensor error ! the ozone stream of the TN detector. on the power again, operate the instrument,
again.
ERROR: Sparge gas line An error occurred related to the sparge gas Switch off power to the instrument. Switch
stream. There is a possibility that the stream on the power again, operate the instrument,
line is clogged. and verify whether the same error occurs
again.
ERROR: Pressure sensor 1 An error occurred in the pressure sensor for Switch off power to the instrument. Switch
error ! supplying gas. on the power again, operate the instrument,
again.
error ! detecting the carrier gas flow rate. on the power again, operate the instrument,
again.
316 TOC-LCPH/CPN
7.7 Troubleshooting

error ! detecting the sparge gas flow rate. on the power again, operate the instrument,
again.
ERROR: 8 port valve retry A problem occurred during 8-port valve Switch off power to the instrument. Remove
operation. the rotor from the 8-port valve, remove any
particles found in the valve, and wash the
valve.
ERROR: CF Card The instrument main unit's data storage Switch off power to the instrument. Contact
device is not operating normally. your Shimadzu representative as this
ERROR: Protocol The protocol version of the firmware does Check the protocol version of the firmware
mismatched. Please check not match that of the PC software. and PC software. The PC software must be
the software version. upgraded.
Firmware is old, so update is Firmware is old, so update is required. Switch off power to the instrument. Contact
required. your Shimadzu representative as this
TOC-LCPH/CPN 317
7.7 Troubleshooting
7.7.2 Troubleshooting
7.7.2.1 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.
Does carrier
gas flow normally NO
to the analysis
cell?
Carrier gas leak.
YES Repair the leak.
Is dehumidifier
within the specified NO
temperature?
The dehumidifier temperature
setting is bad.
YES Contact your Shimadzu
representative.
The infrared gas
analyzer is bad.
Contact your Shimadzu
representative.
318 TOC-LCPH/CPN
7.7 Troubleshooting
(4) The baseline is unstable.
Is carrier gas
NO
flowing normally?
Carrier gas leak.

YES
Repair the leak.
Was
the catalyst NO
replaced?
Accumulated obstructing
substance.
YES
Replace the catalyst.
Is the
dehumidifier NO
operating
normally?
The dehumidifier is bad.
YES
representative.
Are
external
conditions (vibration, NO
temperature, power
voltage)
normal? External conditions are
adverse.
YES
Eliminate the adverse
condition.
The infrared gas analyzer
is bad.
representative.
TOC-LCPH/CPN 319
7.7 Troubleshooting
(5) Poor reproducibility with standard solution.
Is the NO
standard solution
normal?
Bad standard solution.
YES Prepare new standard

solution.
Is the
sample injected NO
normally from injection
tube?
Poor injection condition.
YES Adjust injector. (Refer to Section 7.7.2.4 "Corrective

Actions for Poor Reproducibility")
Do
bubbles remain
in syringe? (especially YES
in dilution
analysis)
Poor injection volume
repeatability.
NO Eliminate bubbles. (Refer to Section 7.7.2.4

"Corrective Actions for Poor Reproducibility")
Was plunger tip NO

replaced recently?
Backlash of plunger tip.
YES Replace plunger tip. (Refer to Section 7.2.8 "Syringe

Replacement")
Does
carrier gas YES
sometimes leak from
the drain
bottle?
Low water level.
NO Replenish the water. (Refer to Section 7.1.3

"Checking Drain Vessel Water Level")
Does the
poor reproducibility IC
occur in the
TC or IC
circuit? IC reaction solution has
deteriorated.
TC Regenerate the IC reaction solution. (Refer to

Section 7.6 "Maintenance Menus")
Was the NO
TC catalyst
regenerated?
Insufficient regeneration of
theTC catalyst .
YES Regenerate the TC catalyst. (Refer to Section 7.6
"Maintenance Menus")
TC catalyst deteriorated.
Replace the TC catalyst.
320 TOC-LCPH/CPN
7.7 Troubleshooting
(6) No peaks appear after sample injection.
Is
sample
injected into TC
NO
combustion tube or IC
reaction vessel?
(confirm
visually) Poor injection.
YES Correct the injection

condition.
Is carrier gas
always flowing from YES
the drain
bottle?
Is the
level of the water NO
normal in the
drain bottle?
Low water level.
YES Replenish water.
Was membrane filter NO

replaced?
Clogged membrane filter.
YES Replace the membrane filter.
Bad infrared gas analyzer. Large resistance downstream

of dehumidifier.
representative. Contact your Shimadzu
representative.
Reference
The following procedure can be used to check whether carrier gas is flowing to the infrared
gas analyzer. However, this procedure cannot determine the existence of minute gas leaks.
Note that checks using this procedure cannot be performed when the TNM-L is connected
to the instrument.
Procedure
1. Block the carrier gas flow by firmly folding over the flexible tubing labeled with an
"L" that is connected to the CO2 absorber, which is located in the holder on top of the
instrument.
2. If carrier gas bubbles out from the bottom of the drain tubing inside the drain
container, which is located on the left side of the instrument, this means that carrier
gas is flowing to the infrared gas analyzer.
For the H Type instrument, whether carrier gas is flowing to the IC reaction vessel can
be determined by visually checking for bubbling of IC reagent in the IC reaction
vessel.
TOC-LCPH/CPN 321
7.7 Troubleshooting
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.
322 TOC-LCPH/CPN
7.7 Troubleshooting
7.7.2.2 ASI-L
(1) The ASI-L does not operate.
Is the connection NO
cable connected
properly?
Incorrectly connected cable
YES Properly connect the cables.
Bad electrical system

representative.
(2) Rinse water is not delivered from the rinse port.
Is there
sufficient NO
rinse water in rinse
water bottle?
Insufficient rinse water
YES Replenish the rinse water.
Is the
rinse tubing NO
properly inserted into
the rinse water
bottle? The rinse tubing is not properly
inserted into rinse water bottle.
YES
Properly insert the tubing into
the rinse water bottle.
The rinse pump is bad.

representative.
TOC-LCPH/CPN 323
7.7 Troubleshooting
(3) Reproducibility is poor.
Is there
any material YES
adhering to the
sample
needle? Deteriorated reproducibility
due to contaminants
NO Remove the obstruction from
the opening at the tip of the
sample needle.
Is there
a leak at the
connection of sample YES
needle and ASI
sample
tubing? Air is drawn in at the
connection.
NO
Properly reconnect the tubing.
Poor reproducibility caused
by the TOC-L
Refer to Troubleshooting
7.7.2.1 TOC-L, item (5).
7.7.2.3 OCT-L, 8-Port Sampler
(1) OCT-L does not operate.
Is the connection NO
cable connected
properly?
Incorrectly connected cable
YES Connect the cables properly.
Electrical system is defective.

representative.
324 TOC-LCPH/CPN
7.7 Troubleshooting
(2) Reproducibility is poor.
Is any foreign
material adhering to YES
the sample tubing?
Deteriorated reproducibility
due to contaminants
NO Eliminate blockage at the tip
of the sample tubing.
Is the leakage
present at the 8-port valve YES
and sample tubing
connection? Connection is leaking.
NO Connect the tubing properly.
Poor reproducibility caused

by the TOC-L
Refer to Troubleshooting
7.7.2.1 TOC-L, item (5).
7.7.2.4 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.
Unacceptable Unacceptable
Appropriate (oblique spray) (scattered spray)
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.
TOC-LCPH/CPN 325
7.7 Troubleshooting
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.
Tube
Bushing
Packing (spacer,
washer, gasket)
Approximately
2 - 2.5mm
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.
Note: 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.
326 TOC-LCPH/CPN
7.7 Troubleshooting
7.7.2.5 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" (Section
3.1.3), 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.
CAUTION
Allow the electric furnace to cool to room temperature for at least six hours after
Combustion tubes are made of quartz glass. Always wear protective leather
TOC-LCPH/CPN 327
7.7 Troubleshooting
328 TOC-LCPH/CPN
8
8Reference 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.
8.2 Analysis-Related Technical Information
This section summarizes technical information related to analysis, including
peak area analysis and calibration curve selection.
8.3 Specifications
This section lists specifications for the TOC-LCPH/CPN main unit, ASI-L, TNM-
L and the various optional kits.
8.4 Standard Accessories
The standard accessories are listed in this section.
8.5 Special Accessories
The optional accessories are listed in this section.
8.6 Consumable Parts List
The consumable parts are listed in this section.
8.7 Maintenance Parts List
The maintenance parts are listed in this section.
8.8 Installation
The installation site requirements and installation procedures for future
relocation of the instrument are described here.
8.9 Material Safety Data Sheets
Material Safety Data Sheets are included for hydrochloric acid, phosphoric acid,
IC regent, the CO2 absorber, and ceramic fiber.
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.
330 TOC-LCPH/CPN
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.
TOC-LCPH/CPN 331
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)
Organic Substance Pre-Sparging Conc. Post-Sparging Conc. Residual Rate
(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
332 TOC-LCPH/CPN
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.
TOC-LCPH/CPN 333
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 10ppm for
TOC/TN catalyst and 5ppm 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.
POC+NPOC Method
The POC+NPOC method should be used when the amount of POC present in the sample
cannot be disregarded.
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.
Note: 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.
334 TOC-LCPH/CPN
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.
Note: • 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
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.
TOC-LCPH/CPN 335
8.2.3 Calibration Curves
8.2.3.1 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
Section 8.2.3.2 "Shifting of Calibration Curves" on page 336.
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
8.2.3.2 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.
336 TOC-LCPH/CPN
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 Figure 8.2 "Shifting of Calibration Curve" on
page 337. 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 Figure 8.2 "Shifting of Calibration Curve" on
page 337, 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.
Peak Area Value
0 TC Concentration (mg/L) 10
(0.5) (10+0.5)
Figure 8.2 Shifting of Calibration Curve
TOC-LCPH/CPN 337
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.
Note: 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 0 5 10 15 20 25 30
(vol%)
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) x 0.27
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.
338 TOC-LCPH/CPN
The automatic selection process occurs on a measurement-by-measurement basis.

Measurement values are always calculated first using Calibration Curve 1. The TOC-
Control 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 →
(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 →
(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 →
Note: 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.
TOC-LCPH/CPN 339
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 calibration curves, automatic correction
function for injection volume, or automatic correction function for dilution
factor.
340 TOC-LCPH/CPN
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.
8.2.8.1 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.
8.2.8.2 JP (Japanese Pharmacopoeia) Support
A recovery rate test and pharmaceutical water test are defined in the JP standards.
TOC-LCPH/CPN 341
8.3 Specifications
8.3 Specifications
8.3.1 TOC-LCPH/CPN
Analyte TC, IC, TOC (TC-IC), NPOC

Measurement principle 680°C catalytically-aided combustion oxidation/non-dispersive
infrared detection (NDIR)
Measuring range TC: 0 - 30000 mg/L
IC:
TOC-LCPH: 0 - 35000 mg/L
TOC-LCPN: 0 - 3000 mg/L
Detection limits TC:
TOC-LCPH: 4 µg/L
TOC-LCPN: TC: 50 µg/L
IC: 4 µg/L
Measurement time TC: Approx. 3 min
IC:
TOC-LCPH: Approx. 3 min
TOC-LCPN: Approx. 4 min
Repeatability TOC-LCPH:
TC, IC, NPOC CV 1.5 % or ±4 μg/L max.
(Option: TN: CV 3.0 % or ±5 μg/L max.)
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
Sample injection volume TC:
• TOC-LCPH: 10 to 2000 μL (variable)
• TOC-LCPN: 10 to 150 μL (variable)
IC:
Sample dilution function Dilution within syringe, dilution factor 2 - 50 times
Pretreatment for IC Automatic acid addition and sparging
Carrier gas High purity air (from cylinder)
High purity nitrogen (with addition of the N2 carrier gas kit)
Pressurized air (with addition of the carrier gas purification kit (only
applicable to the TOC-LCPN))
Carrier gas pressure Approx. 200 ± 10 kPa (300 to 600 kPa when using the carrier gas
regulator option)
Carrier gas flow rate TOC-LCPH: 150 mL/min (230 to 250 mL/min when sparging)
TOC-LCPN: 230 mL/min
Ambient temperature 5 - 35°C
342 TOC-LCPH/CPN
8.3 Specifications
Power requirements AC 100-120V ±10% or AC 220-240V ±10%, 600 VA, 50/60 Hz

Fuse 10 A LAG × 2
Approximate dimensions (W) 340 x (D) 660 x (H) 480 mm (excluding projections)
Weight Approx. 35 kg
8.3.2 ASI-L
Sample containers 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),
100 vials, 100 septum-equipped caps
40 mL vial rack: 40 mL (External diameter 27 x Height 9 mm),
72 vials, 72 septum-equipped caps
Vial rack capacity 9 mL vial rack: 93 vials
24 mL vial rack: 93 vials
40 mL vial rack: 68 vials
Sample pretreatment • Acid addition and sparging possible for NPOC analysis (with
addition of the external sparge kit)
• Needle rinse possible
• Stirring with magnetic stirrer (with addition of the magnetic stirrer,
excluding 9 mL vials)
Weight Approx. 14 kg
8.3.3 OCT-L 8-Port Sampler
No. of sample containers 8 containers

accommodated 16 containers (using 2 OCT-L units)
Ambient temperature 10 - 35° C
External dimensions Approx. (W) 245 x (D) 245 x (H) 440 mm (excluding protruding
parts)
Weight Approx. 3.5 kg
8.3.4 TNM-L
Analyte TN (total nitrogen)

Measurement principle Thermal decomposition / NO detection (chemiluminescence
method)
Measuring range 0 - 10000 mg/L
TOC-LCPH/CPN 343
8.3 Specifications
Detection limit • TOC-LCPH: 5 μg/L

• TOC-LCPN: 20 μg/L
Measurement time Approx. 4 min
Repeatability Higher value of within CV3 % or ± 5 μg/L
Sample injection volume • TOC-LCPH: 10 to 300 μL (variable)
Weight Approx. 6 kg
8.3.5 POC Measurement Kit
Analyte POC (volatile organic carbon)

Measurement method Sparging / CO2 removal / 680 °C combustion oxidation / non-
dispersive infrared detection (NDIR)
CO2 removal method Absorption via lithium hydroxide, removal
Measuring range 0 - 500 mg/L
Detection limit 4 μg/L
Measurement time Approx. 4 min
Repeatability CV within 1.5%
8.3.6 Carrier Gas Purifier Kit
Gas purification method Combustion oxidation / CO2 removal

Carrier gas supply Pressurized air or oxygen (free of dust, oil mist, water droplets, etc.)
Carrier gas supply pressure 200 ± 10 kPa
8.3.7 Manual Injection Kit (Gas Sample Injection Kit)
Analyte 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 gases aside from
carbon dioxide are also measured as TOC)
Measurement of IC, TOC and carbon dioxide is possible with the TOC-LCPH
Measurement principle 680°C catalytically-aided combustion oxidation/non-dispersive infrared
detection (NDIR)
Measuring range Liquid sample:
TC: 0 - 20000 mg/L
IC: 0 - 20000 mg/L
Gas sample:
6 ppm - 100% CO2
344 TOC-LCPH/CPN
8.3 Specifications
Sample injection volume Liquid sample: 1 - 150 µL

Gas sample: 20 µL - 10 mL
Measuring time Liquid sample:
TC: Approx. 3 min
IC: Approx. 3 min
Gas sample: 2 - 4 min
Repeatability Liquid sample: CV within 2% (CV is within 3% when sample concentration
is 8000 mg/L or greater)
Gas sample: CV within 2%
Sample introduction Manual injection using microsyringe
8.3.8 B-Type Halogen Scrubber
Detection limit TC: 60 μg/L

IC: 4 μg/L
TN: 30 μg/L
Sample injection volume TC: 10 to 150 μL
IC:
Repeatability CV within 3 %
8.3.9 External Sparge Kit
Flow rate adjustment 0 to 300 mL/min

range
TOC-LCPH/CPN 345
8.3 Specifications
8.3.10 Recommended PC Specifications
Machine type IBM-PC/AT or compatible

OS Windows XP Professional (32bit),
Windows 7 Professional (32bit),
Windows 7 Professional (64bit)
CPU 1.5 GHz or faster (Windows XP)
2 GHz or faster (Windows 7 (32bit))
2.5 GHz or faster (Windows 7 (64bit))
Memory 1 GB or greater (Windows XP)
2 GB or greater (Windows 7 (32bit))
4 GB or greater (Windows 7 (64bit))
Hard drive 40 GB or greater
Monitor resolution 1024 x 768 pixels or greater
Other DVD drive
USB port
346 TOC-LCPH/CPN
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
S071-60821-08 Power cord set (100-127V) 1 1
S071-60814-06 Power cord set (220-240V) 1 1
S638-59296-01 Plunger tip 1 1
S638-59296 Syringe 1 1
S072-60359-01 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
S088-52859-54 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
S638-94602 English USER'S MANUAL 1 1
S638-94605 English TOC-LCPH/CPN 1 1
Administrator Manual
Table 8.4 • Standard Accessories List 2 (ASI-L Autosampler)

Part Number Part Name 9 mL 24mL 40mL
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
TOC-LCPH/CPN 347
Table 8.5 • Standard Accessories List 3 (OCT-L 8-Port Sampler)

Part Number Part Name OCT-L OCT-L Details
(1) (2)
S638-56251-01 8-port valve rotor 1 1 Rotor (for replacement maintenance)
S638-42106-01 Flared tubing set C 1* 8 sample tubes, 1 tube for connection to
main unit.**
S638-42106-02 Flared tubing set C2 1* 8 sample tubes, 1 tube for connection to
main unit. ***
S638-74492-01 Connection cable 1 Cable for connection to the main unit
S638-74476-02 Second unit 1 Cable for connecting OCT-L (1) to OCT-
connection cable L (2)
* Flanged tubing in C and C2 sets have an inner diameter of 1.0 mm.

** Connect this tubing to the common (COM) port of the OCT-L (1) and port 2 on the TOC-
L unit.
*** Connect this tubing to the common (COM) port of the OCT-L (2) and port 1 on the TOC-
L unit.
348 TOC-LCPH/CPN
Table 8.6 • Special Accessories List

Part Number Part Name Comment
S638-93195 Auto Sampler ASI-L Two models: dedicated 24 mL vial model
and common 9 mL/40 mL vial model
S638-92306-03 ASI Accessories (9 mL)
S638-53044-06 9 mL vial rack set for ASI 9 mL vial rack + 9 mL vial set
S638-53044-04 24 mL vial rack set for ASI 24 mL vial rack + set of 24 mL vials,
caps and septums
S638-53044-05 40 mL vial rack set for ASI 40 mL vial rack + set of 40 mL vials,
caps and septums
S638-67099-01 Stirrer (for 24 mL vials) Autosampler for 24 mL vials
S638-67100-01 Stirrer (for 40 mL vials) Autosampler for 40 mL vials
S046-00617-02 Stirring bar (for 24 mL vials) 1 stirring bar for 24 mL vials, 1 is
required for sample measurement
S046-00617-03 Stirring bar (for 40 mL vials) 1 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.
S038-00158-11 40 mL ASI vial 72 pcs.
Includes caps and septums
S638-20074-01 Cap (for 24 mL vials) 100 pcs.
S038-00165-61 Septum (for 24 mL vials) 100 pcs.
S638-93196-01 8-Port sampler OCT-L (first unit)
S638-93196-11 8-Port sampler OCT-L (second For expanding to a second unit
unit)
S638-91108 TN unit TNM-L For AC 100-127V
S638-93102 SSM-5000A Solid Sample
Module for Total Organic Carbon
Analyzer
S638-56239 Cell switching valve set Option for SSM-5000A
S638-42101-01, 02 POC measurement kit "-01" is for N Type, "-02" is for H Type
S638-41447 Carrier gas purifier kit
S638-77183 External sparge kit Only when using TOC-L
S638-77183-01 External sparge kit (with ASI-L) When using ASI-L Autosampler
S638-93149-03 Manual injection kit
S638-41586 Suspended solids kit (when used Only when using TOC-L
with TOC-L alone)
TOC-LCPH/CPN 349
Table 8.6 • Special Accessories List

S638-93151-04 Suspended Solids Kit (when ASI- When using ASI-L Autosampler
L is used)
S638-42054-02 Nitrogen currier gas kit Enables use of high purify nitrogen gas
with less than 1 ppm each of CO, CO2
and HC as carrier gas.
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
S638-93176-01,-02 Combustion tube kit for high salt "-01" is for N Type, "-02" is for H Type
samples
S630-08585-05 Cylinder pressure regulator User can provide this item.
S638-41204 Air supply tubing set (with 20 User can provide this item.
meters of tubing)
S638-52344 Drain bottle (for ASI)
S638-56255 Carrier gas regulator Use this regulator when the pressure
from the carrier gas supply source cannot
be stably maintained at 200 ± 10 kPa.
350 TOC-LCPH/CPN
8.6.1 Consumable Parts List
Table 8.7 • Consumable Parts List 1 (TOC-LCPH)

S638-41323 Combustion tube, in case
S638-60116 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
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.
S042-00405-11 IC reaction solution supply pump head
S046-00044-12 Membrane filter
S638-56251-01 8-port valve rotor Type name: Plug, XT24-197-1-4
S638-59296-01 Plunger tip
S638-92206-04 TOC-LCPH consumable parts set Refer to “Table 8.9 • TOC-LCPH, CPN
Consumable Parts Set Breakdown” for
an itemized list
Table 8.8 • Consumable Parts List 2 (TOC-LCPN)

S638-41323 Combustion tube, in case
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.
TOC-LCPH/CPN 351
Table 8.8 • Consumable Parts List 2 (TOC-LCPN)

S046-00044-12 Membrane filter
S638-56251-01 8-port valve rotor
S638-59296-01 Plunger tip
S638-92206-05 TOC-LCPH consumable parts Refer to “Table 8.9 • TOC-LCPH, CPN
set Consumable Parts Set Breakdown” for
contents
Table 8.9 • TOC-LCPH, CPN Consumable Parts Set Breakdown

Part No. Description Qty Remark
TOC-LCPH TOC-LCPN
S638-41323 Combustion tube (in case) 2 2
S638-60116 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.
S042-00405-11 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)

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.
S038-00165-61 Septum 24 mL, 100 pcs.
S038-00165-50 Septum 40 mL, 100 pcs.
S638-20074-01 Cap 24 mL, 100 pcs.
S038-00165-40 Cap 40 mL, 200 pcs.
S042-00405-11 Rinse pump head
352 TOC-LCPH/CPN
Table 8.11 • Consumable Parts List 4 (8-Port Sampler OCT-L)

S638-56251-01 8-Port valve rotor
Table 8.12 • Consumable Parts List 5 (TNM-L TN Unit)

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)

S630-00556 CO2 absorber, absorbent 500 g included
Table 8.14 • Consumable Parts List 7 (B-Type Halogen Scrubber)

S631-60069 Stainless mesh for absorption
TOC-LCPH/CPN 353
8.6.2 Recommended Consumable Part Replacement Period

Table 8.15 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

S638-41323 Combustion tube (case included) 6 months
S638-60116 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
S638-59213-01 Plunger tip 6 months
354 TOC-LCPH/CPN
Table 8.16 • Maintenance Parts List 1 (TOC-LCPH/CPN)

S638-56251 8-port valve
S638-59296 Syringe
S638-42119-01 Tube 1 For port number 1 on the 8-port valve
S638-42029-07 Tube set (sampling) For port number 2 on the 8-port valve
(for ASI connection)
Table 8.17 • Maintenance Parts List 2 (ASI-L Autosampler)

S638-41472-01 Water sampling needle The sparging needle is identical to this
part.
S638-41450-01 Needle for suspended solids For use with 24 mL and 40 mL vials and
kit the suspended solids kit, 0.8 mm, 1
included
S638-42029-07 Tube set 1 tube, retainer, and tube seal for both
sampling and sparging
S638-42029-04 Tube set (sampling for the 1 sampling tube for the suspended solids
suspended solids kit) kit, with retainer and tube seal
S638-67095-01 Motor (for 24 mL vials) For stirrer 24 mL vials
S638-67095-02 Motor (for 40 mL vials) For stirrer 40 mL vials
S638-67099-01 Stirrer (for 24 mL vials) For autosampler 24 mL vials
S638-67100-01 Stirrer (for 40 mL vials) For autosampler 40 mL vials
Table 8.18 • Maintenance Parts List 3 (OCT-L 8-Port Sampler)

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
TOC-LCPH/CPN 355
Table 8.19 • Maintenance Parts List 4 (Manual Injection Kit)

S630-02621 Open / Close valve, TC
injection port
S638-60733-01 Microsyringe, MANU10 10 µL
356 TOC-LCPH/CPN
8.8 Installation
8.8 Installation
8.8.1 Before Installation
Parts Inspection
Confirm that all of the components listed in Section 8.4 "Standard Accessories" on page
347 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.
8.8.2.1 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" on page 357. 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.
TOC-L
main
unit
TOC-L
main
unit
PC
Figure 8.3 External Dimensions of Instrument with ASI-L
TOC-LCPH/CPN 357
8.8 Installation
TOC-L
main
unit
TOC-L
main
unit
PC
Figure 8.4 External Dimensions of the Instrument with the OCT-L 8-Port Sampler
and TNM-L TN Unit (Units: mm)
CAUTION
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.
8.8.2.2 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.
Note: Contamination in the atmosphere will cause analysis errors, especially for high
sensitivity analyses.
• A strong, level bench, free of vibration and shock.
• A location with a stable ambient temperature.
• A location with access to a completely grounded, stable power supply.
358 TOC-LCPH/CPN
8.8 Installation
CAUTION
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
8.8.3.1 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.
CAUTION
The instrument may not operate properly if the power supply voltage exceeds
the range of AC100-127V ±10% or AC 220-240V ±10%. Unstable voltage may
cause problems during high sensitivity analysis.
Note: The instrument is compatible with both 50 Hz and 60 Hz power supplies and can
be used with either frequency.
¬Grounding
The included power cord is a three-conductor cable including a ground wire, and a 2P plug
(with ground) at the end.
The voltage terminals (AC) and ground terminal (ACC) on the power plug of this
instrument are arranged as shown in Figure 8.5 "Power Plug" on page 359. Connect them
so that they match the power outlet being used.
Voltage terminal (AC) Ground terminal (ACC)
Ground terminal (G)

(Be sure to ground completely.)
Figure 8.5 Power Plug
TOC-LCPH/CPN 359
8.8 Installation
CAUTION
• 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: 100Ω or less) is recommended.
• Perform grounding separately and avoid contact with water supply pipes, gas
pipes, and lightning rods.
8.8.3.2 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.
8.8.3.3 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)
¬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.
Note: If the carrier gas contains excessive impurities, analysis accuracy is diminished
and good results will not be obtained.
360 TOC-LCPH/CPN
8.8 Installation
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
the SLP5D-2SV oilless and silent air compressor (P/N S638-59203) and AW30-02BG-
N filter regulator (P/N S040-82112-43) as options.
• There are cases where the organic gas concentration is too high to be removed
completely by the gas purifier. Analysis accuracy is poor in atmospheres containing
high concentrations of volatile gases from exposed organic solvents and gasoline, or
high concentrations of automobile and diesel engine exhaust. If the possibility of the
presence of these kinds of gases cannot be avoided, use a filter to remove organic
particles and/or gases.
¬Using Gas Cylinder High Purity Nitrogen or Instrumentation High Purity Nitrogen
High purity nitrogen gas must be guaranteed to contain less than 1 ppm of each of the
following impurities: carbon dioxide, carbon monoxide, and hydrocarbons.
Install a pressure regulator on the cylinder and supply gas to the gas connection inlet on the
instrument at 200 ± 10 kPa.
These specifications limit the upper measurement concentration to 100 mg/L for TC and
NPOC. For sample measurements that exceed this concentration, measurement is possible
using the automatic dilution function if the concentration of the sample is less than
100 mg/L after dilution. Also note that TN measurement cannot be performed using the
TNM-L with these specifications.
Note: Excessive impurities in the carrier gas will diminish analysis accuracy and
prevent the acquisition of sound measurement results.
TOC-LCPH/CPN 361
8.8 Installation
¬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.
Note: 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
Half union
Nylon tubing
Figure 8.6 Gas Tubing Connection
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.
Note: 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.
362 TOC-LCPH/CPN
8.8 Installation
CAUTION
• 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.
8.8.3.4 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.
TOC-L
Drain discharge tubing (Avoid
installing the tubing as shown
by the dotted line.)
Drain container (Prepare a

suitable drain container.)
Figure 8.7 How to Lead the Drain Tubing from the Instrument to the Drain Container
TOC-LCPH/CPN 363
8.8 Installation
CAUTION
• 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.
8.8.3.5 Connecting to the PC Using the Provided Cable
This section describes how to connect the TOC-L and PC using the provided USB cable.
1. Insert one plug on the provided USB cable into the USB terminal on the rear of the
TOC-L. (Refer to Section 2.1.4 "Rear View" on page 10)
2. Insert the other plug on the cable into the USB connector on the PC.
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.
Figure 8.8 Installing the ASI-L
Note: 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.
364 TOC-LCPH/CPN
8.8 Installation
¬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.
CAUTION
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.
¬Connecting Cables
The TOC-L and ASI-L are connected using cables, as described below.
CAUTION
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.
Connection cable
Figure 8.9 Connecting the Cables (TOC-L to ASI-L)
TOC-LCPH/CPN 365
8.8 Installation
¬Connecting the Sample Tubing and Sparge Tubing (External Sparge Kit)
The procedure for connecting the ASI-L sample tubing and sparge tubing for the External
Sparge Kit is as follows.
Procedure
1. Attach the bush on the end of the water sampling tubing to port number 2 on the 8-
port valve of the sample injector on the TOC-L.
2. If using the external sparge kit, attach the sparging tubing for ASI-L.
Sparging tubing for ASI-L

Sparging tubing if not using the ASI-L

ASI-L sparging
needle
Figure 8.10 Attaching the Sparging Tubing for ASI-L
¬Installing the Needle

This section describes how to install the ASI-L needle. There are two types of needle: water
sampling needle and sparging needle (for use with the external sparge kit). The needle with
a single slot is the water sampling needle and the needle with two slots is the sparging
needle.
CAUTION
Verify that the TOC-L is switched OFF before performing the following
procedure.
366 TOC-LCPH/CPN
8.8 Installation
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.
Needle holder Needle retaining

retaining screw bracket
Needle holder
Needle cover Water sampling needle
Sparging needle
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.
Note: There are two openings; the left opening is for the sample tubing
and the right opening is for the sparge tubing.
Retaining bracket
Needle holder
Sample needle
Figure 8.12 Installing the Needle
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.
TOC-LCPH/CPN 367
8.8 Installation
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.
Note: 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.
Turntable
Figure 8.13 Installing the Turntable
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.
Note: There is a magnet at the left rear of the cover. Verify that the cover
and ASI-L are in contact at the magnet.
368 TOC-LCPH/CPN
8.8 Installation
¬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 Section 8.8.3.4 "Installing the Drain Container" on
page 363. Such a container of sufficient capacity can be used in conjunction with the
drain container for TOC-L.
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.
CAUTION
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.
TOC-LCPH/CPN 369
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.
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”.
TIP » 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.
CAUTION
Confirm that the power to the TOC-L main unit is switched OFF before
performing this 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 and then reattach the
cover to its original position.
370 TOC-LCPH/CPN
8.8 Installation
4. Connect the other end of the OCT-L cable to the OCT-L connector on the rear of the
TOC-L main unit.
Cover
Connection cable
Figure 8.15 Cable Connections (TOC-L and OCT-L)
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).
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).
Connection cable
Figure 8.16 Connecting Two OCT-L Units
TOC-LCPH/CPN 371
8.8 Installation
3. Remove the port number label from the OCT-L (2) unit and replace it with the port
number label provided with the unit.
Note: 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.
¬Connecting the Water Sampling Tubing

Connect the water sampling tubing according to the procedure described below.
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)).
Water sampling
Water sampling
tubing
tubing
COM port
Figure 8.17 COM Port and Water Sampling Tubing Connections
Note: 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
372 TOC-LCPH/CPN
8.8 Installation
8.8.6 Installing the TNM-L
8.8.6.1 TNM-L TN Unit Installation
A technician from Shimadzu or designated by Shimadzu will install this unit.
8.8.6.2 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 S638-59203) and AW30-02BG-N
filter regulator (P/N S040-82112-43) 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.
Note: If there are excessive contaminants in the carrier gas, measurement results will be
adversely affected due to low measurement reproducibility, etc.
TOC-LCPH/CPN 373
8.8 Installation
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.
Note: 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.
¬Gas Tubing Connections

The special accessory Air Supply Tubing Set includes nylon tubing and connectors (two (2)
half unions).
Half union
Nylon tubing
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.
374 TOC-LCPH/CPN
8.8 Installation
2. Connect the nylon tubing (4 mm O.D., 2.5 mm I.D.) between the gas supply source
and the instrument.
Note: 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.
CAUTION
• 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.
¬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.
8.8.6.3 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.
CAUTION
• 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.
Note: Expose the exhaust gas tubing to atmospheric pressure to reduce resistance.
TOC-LCPH/CPN 375
8.9.1 Hydrochloric Acid (HCl)

Shimadzu Scientific Instruments, Inc. Revised Date: 2008/06/12
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
SECTION I IDENTIFICATION OF THE SUBSTANCE OR MIXTURE

PRODUCT IDENTIFIER : Hydrochloric Acid
SECTION II HAZARDS IDENTIFICATION
GHS CLASSIFICATION : Skin corrosion/irritation: Category 1A
Serious eye damage/eye irritation: Category 1
Acute toxicity-Oral: Category 4
Acute toxicity-Inhalation: Category 1
Sensitization-Respiratory: Category 1
Specific target organ systemic toxicity Single exposure: Category 1
Specific target organ systemic toxicity Repeated exposure: Category 1
Hazardous to the aquatic environment -Acute hazard: Category 1
HAZARD SYMBOL :
DANGER
HAZARD STATEMENTS : Causes severe skin burns and eye damage
Causes serious eye damage
Harmful if swallowed
Fatal if inhaled
May cause allergy or asthma symptoms or breathing difficulties if inhaled.
Causes damage to organs
Causes damage to organs through prolonged or repeated exposure
Very toxic to aquatic life
PRECAUTIONARY STATEMENTS : <Prevention>
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
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.
<Resoponse>
Collect spillage.
Get medical attention/advice if you feel unwell.
If experiencing respiratory symptoms call a 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.
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.
<Storage>
Store container tightly closed in well-ventilated place -if product is as volatile as to generate hazardous atmosphere.
Store locked up.
<Disposal>
Dispose of contents/container to a located point (in accordance with local/regional/national/international regulation).
376 TOC-LCPH/CPN
SECTION III COMPOSITION/INFORMATION ON INGREDIENTS

CHEMILCAL IDENTITY : Hydrochloric acid (36 %)
SYNONYMS : Muriatic acid
FORMULA : HCl
MOLECULAR WEIGHT : 36.46
CAS NUMBER : 7647-01-0
TSCA INVENTORY : Listed
EINECS No. : 231-595-7
EC INDEX NUMBER : 017-002-00-2
SECTION IV FIRST AID MEASURES
GENERAL ADVICE : Wash off immediately with soap and plenty of water. In the case of respirable dust and/or fumes, use self-contained
breathing apparatus and dust impervious protective suit. Use personal protective equipment.
INHALATION : Move victim to fresh air. If breathing is difficult, give oxygen. If breathing has stopped, administer artificial respiration.
Maintain normal body temperature with a blanket. If irritation persists, transport to a hospital immediately.
SKIN CONTACT : Remove contaminated clothes and shoes, rinse skin with plenty of water or shower. Use soap to help assure removal. If
irritation persists, transport to a hospital immediately.
EYE CONTACT : Remove any contact lenses at once. Flush eyes well with flooding amounts of running water for at least 15 minutes.
Assure adequate flushing by separating the eyelids with sterile fingers. If irritation persists, transport to a hospital
immediately.
INGESTION : Rinse mouth, give plenty of water to dilute the substance. Never give anything by mouth to an unconscious person.
Transport to a hospital immediately.
SECTION V FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA : Carbon dioxide, dry chemical powder, foam, water
FIRE & EXPLOSION HAZARDS : Toxic and irritating fumes or smoke may be emitted. Explosive hydrogen gas is released upon contact with common
metals.
SPECIAL PROTECTIVE EQUIPMENT FOR FIREFIGHTERS :
Firemen should wear normal protective equipment (full bunker gear) and positive-pressure self-contained breathing
apparatus.
SECTION VI ACCIDENTAL RELEASE MEASURES
PERSONAL PRECAUTIONS : Remove ignition sources and ventilate the area. In case of insufficient ventilation, wear suitable respiratory equipment.
Avoid contact with skin and eyes.
ENVIRONMENTAL PRECAUTIONS :
Prevent spills from entering sewers, watercourses or low areas.
METHODS FOR CLEANING UP : Do not touch spilled material without suitable protection (See section 8). Take up spilled material with ashes or other
incombustible absorbents and dilute it with plenty of water and neutralize with soda ash. After material is completely
picked up, wash 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.
SECTION VII HANDLING AND STORAGE
PRECAUTION FOR SAFE HANDLING :
Avoid contact with eyes, skin and clothing. Avoid prolonged or repeated exposure. Handle material with suitable
protection.
CONDITIONS FOR SAFE STORAGE :
Store away from sunlight in well-ventilated dry place at room temperature. Keep container tightly closed.
INCOMPATIBILITIES : Strong oxidizers, alkalis, amines, metals
SECTION VIII EXPOSURE CONTROLS/PERSONAL PROTECTION
ENGINEERING MEASURES : Use exhaust ventilation to keep airborne concentrations below exposure limits. Use only with adequate ventilation.
VENTILATION : Local Exhaust ; Necessary, Mechanical (General) ; Necessary
Special; Closed system is recommended.
INDIVIDUAL PROTECTION MEASURES ;
Respiratory protection : NIOSH/MSHA or European Standard EN149 approved respirator
Hand protection : Impervious gloves
Eye protection : Safety glasses (goggles)
Skin protection : Protective clothing
CONTROL PARAMETER : as Hydrogen chloride
OSHA Final Limits : Ceiling = 5 ppm, 7 mg/m3; STEL = 2 ppm
ACGIH TLV(s) : Ceiling = 5 ppm, 7.5 mg/m3
SECTION IX PHYSICAL AND CHEMICAL PROPERTIES
APPEARANCE : Colorless clear liquid
ODOUR : Irritating odor
pH : Not available
FREEZING POINT : -46.2 °C = -51.2 °F (31.24 %)
INITIAL BOILING POINT : 108.58 °C = 227.44 °F
FLASH POINT : Not available
FLAMMABILITY (solid, gas) :-----
EXPLOSIVE LIMITS : Not available
VAPOR PRESSURE : Not available
VAPOR DENSITY : 1.3 (air = 1)
RELATIVE DENSITY : 1.180 (35.39 %)
SOLUBILITY IN ; WATER : Miscible
ETHANOL, ETHL ETHER : Miscible
PARTITION COEFFICIENT : 0.25
DECOMPOSITION TEMPERATURE : Not available
TOC-LCPH/CPN 377
SECTION X STABILITY AND REACTIVITY

CHEMICAL STABILITY : Will not occur.
CONDITIONS TO AVOID : Sunlight, heat
INCOMPATIBILE MATERIALS : Strong oxidizers, alkalis, amines, metals
HAZARDOUS DECOMPOSITION PRODUCTS :
Hydrogen chloride gas may be formed.
SECTION XI TOXICOLOGICAL INFORMATION
as Hydrogen chloride;
ACUTE TOXICITY (oral/dermal/inhalation) :
LDLo (orl,woman): 420 μL/kg (JJTOEX 9,351,1996)
LC50 (ihl,rat): 7004 mg/m3/30M (VCVN5* -, 383, 1989)
TCLo (ihl,human): 50 mg/m3 (VCVN5* -, 383, 1989)
SKIN CORROSION/IRRITATION : Skin; human; 4 %/24H; Mild (BJDEAZ 68,192,1988)
EYE DAMAGE/EYE IRRITATION : Eye; rabbit, rinsed; 5 mg/30S; Mild (TXCYAC 23,281,1982)
RESPIRATORY OR SKIN SENSITIZATION :
Not available
GERM CELL MUTAGENICITY : Cytogenetic analysis; hamster; ovary; 8 mmol/L (MUREAV 225,55,1989)
DNA repair; E.coli; 25 μg/well (ENMUDM 3, 429, 1981)
TOXIC TO REPRODUCTION : TCLo (ihl,rat): 450 mg/m3/1H (female 1D pre): Effects on Embryo or Fetus - fetotoxicity (AKGIAO 53 (6), 69,1977)
STOST-SINGLE EXPOSURE : Not available
STOST-REPEATED EXPOSURE : Not available
ASPIRATION TOXICITY : Not available
CARCINOGENICITY : Not available
ADDITIONAL INFORMATION ; NTP : Not listed
IARC : Not Classifiable as to Carcinogenicity to Humans (Group 3)
OSHA : Not listed
ACGIH : Not listed
EPA GENETOX PROGRAM 1988, Negative: Cell transform.-SA7/SHE
SECTION XII ECOLOGICAL INFORMATION
ECOTOXICITY : LC50 (starfish): 100 to 330 ppm (as Hydrogen chloride)
PERSISTENCE AND DEGRADABILITY :
Not available
BIOACCUMULATION POTENTIAL : Not available
MOBILITY IN SOIL : Not available
OTHER ADVERSE EFFECTS : WGK; 1
SECTION XIII DISPOSAL CONSIDERATION (INCLUDING CONTAINER)
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 drain with plenty of water. Any
disposal practice must be in compliance with country, local, state, and federal laws and regulations (contact country, local
or state environmental agency for specific rules).
SECTION XIV TRANSPORT INFORMATION
IATA : UN NUMBER : UN1789
UN PROPER SHIPPING NAME : Hydrochloric acid
CLASS or DIVISION : Corrosives. (Class 8)
PACKING GROUP : PG II
MARINE POLLUTANT : Yes
DOT (Department of Transportation) : IDENTIFICATION NUMBER : UN1789
PROPER SHIPPING NAME : Hydrochloric acid
HAZARD CLASS : Corrosive material (Class 8)
SECTION XV REGULATORY INFORMATION
US REGULATIONS ; CAA/112 1990 Amend., CAA/122(r) Acci. Release Pre. Subst., CERCLA Haz. Subst., DOT Haz. Mat., DOT Haz. Sub.
and Rep. Quant., Mass. Subst. List , New Jers. RTK Haz. Subst. List , Penn. Haz. Subst. List
EPA : CERCLA RQ= 5000 lb
EPCRA TPQ= Not listed
EPA FIFRA 1998 STATUS OF PESTICIDES: Red Completed
OSHA : TQ= Not listed
SECTION XVI OTHER INFORMATION INCLUDING INFORMATION ON PREPARATION AND REVISION
OF THE SDS
No specific notes
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.
378 TOC-LCPH/CPN
8.9.2 Phosphoric Acid

Tel: 1(800) 477-1227

PRODUCT IDENTIFIER : Phosphoric Acid
GHS CLASSIFICATION : Skin corrosion/irritation: Category 1A
Serious eye damage/eye irritation: Category 1
Acute toxicity-Oral: Category 4
Acute toxicity-Dermal: Category 5
Specific target organ systemic toxicity Single exposure: Category 3 <the respiratory tract irritation>
HAZARD SYMBOL :
DANGER
Causes serious eye damage
Harmful if swallowed
May be harmful in contact with skin
May cause respiratory irritation; or May cause drowsiness and dizziness <the respiratory tract irritation>
PRECAUTIONARY STATEMENTS : Do not eat, drink or smoke when using this product.
Get medical attention/advice if you feel unwell.
rinsing.
IF ON SKIN: Gently wash with plenty of soap and water.
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 CLASSIFICATIONS: according to EC Directives
SYMBOL : C
HAZARD STATEMENTS, including R-phrase :
R34 Causes burns.
CHEMILCAL IDENTITY : Phosphoric acid (min.85.0 %)
SYNONYMS : Orthophosphoric acid, Hydrogen phosphate ; Phosphoric Acid, Ortho
FORMULA : H3PO4
MOLECULAR WEIGHT : 98.00
TSCA INVENTORY : Listed
EINECS No. : 231-633-2
EC INDEX NUMBER : 015-011-00-6
INHALATION : Move victim to fresh air. If breathing is difficult, give oxygen. If irritation persists, consult a physician.
immediately.
INGESTION : Rinse mouth, give plenty of water to dilute the substance. Never give anything by mouth to an unconscious person.
EXTINGUISHING MEDIA : Carbon dioxide, dry chemical powder, foam, water
FIRE & EXPLOSION HAZARDS : Toxic, irritating fumes or smoke may be emitted. Explosive hydrogen gas is released upon contact with common metals.
apparatus.
Avoid contact with skin and eyes.
ENVIRONMENTAL PRECAUTIONS :Prevent spills from entering sewers, watercourses or low areas.
METHODS FOR CLEANING UP : Do not touch spilled material without suitable protection (See section 8). Take up spilled material with ashes or other
incombustible absorbents and dilute it with plenty of water and neutralize with soda ash. After material is completely
picked up, wash 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.
TOC-LCPH/CPN 379

protection. This material is hygroscopic.
INCOMPATIBILITIES : Oxidizers, alkalis, metals
Respiratory protection : Use a NIOSH/MSHA or European Standard EN149 approved respirator
CONTROL PARAMETER : OSHA Final Limits : TWA = 1 mg/m3
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 POINT : 213 °C = 415 °F
FLAMMABILITY (solid, gas) : -----
VAPOR PRESSURE : 4.0 Pa (at 20 °C = 68 °F)
VAPOR DENSITY : 3.4 (Air = 1)
SPECIFIC GRAVITY : 1.685
SOLUBILITY IN ; WATER : Freely soluble (670 g/100 mL at 25 °C = 77 °F)
ETHANOL : Freely soluble
PARTITION COEFFICIENT : Not available
CHEMICAL STABILITY : May occur. Violent polymerization can occur with epoxides, azo compounds, and polymerizable compounds.
CONDITIONS TO AVOID : Sunlight, heat, moisture
INCOMPATIBILE MATERIALS : Oxidizers, alkalis, metals
Phosphorous oxide may be formed.
LD50 (orl, rat) : 1.25 gm/kg (RTECS)
LD50 (orl, mouse) : 1.25 gm/kg (RTECS)
LC50 (ihl, rat) : 25.5 mg/m3 (RTECS)
LD50 (orl, rat) : 1530 mg/kg (IUCLID, 2000) (HSDB, 2006)
LD50 (skin, rabbit) : 2740 mg/kg (IUCLID, 2000) (HSDB, 2006)
SKIN CORROSION/IRRITATION : Skin; rabbit; 595 mg/24H; Severe (RTECS)
Skin; rabbit; 75-85 %/24H; Irritation (IUCLID, 2000)
EYE DAMAGE/EYE IRRITATION : Eye; rabbit; 119 mg; Severe (RTECS)
Not available
GERM CELL MUTAGENICITY : Not available
TOXIC TO REPRODUCTION : Not available
STOST-SINGLE EXPOSURE : Human; mist, irritation of the upper respiratory tract (ACGIH 7th, 2001)
IARC : Not listed
OSHA : Not listed
ACGIH : Not listed
EPA GENETOX PROGRAM 1988, Negative: Cell transform.-SA7/SHE
380 TOC-LCPH/CPN

ECOTOXICITY : Not available
Not available
OTHER ADVERSE EFFECTS : WGK; 1
package them for hazardous-waste disposal. Flush the aqueous solutions down the drain with plenty of water.
Any disposal practice must be in compliance with country, local, state, and federal laws and regulations (contact country,
local or state environmental agency for specific rules).
After contents are completely removed, dispose of its container at hazadous or special waste collection point. (in
accordance with local/regional/ national/international regulation).
UN PROPER SHIPPING NAME : Phosphoric acid
PACKING GROUP : PG III
MARINE POLLUTANT : No
PROPER SHIPPING NAME : Phosphoric acid
US REGULATIONS ;
as Phosphoric acid; CWA/311 Haz., NIOSH Recommend. Subst., CERCLA Haz. Subst., SARA III/313 Tox. Chem., DOT Haz. Mat., DOT
Haz. Sub. and Rep. Quant., Mass. Subst. List , New Jers. RTK Haz. Subst. List , Penn. Haz. Subst. List , Canad. WHMIS
IDL 1 % conc.
EPA : CERCLA RQ= 1000 lb
EPCRA SECTION 313 de minimis concentration is 1.0 %.
FIFRA 1988 PESTICIDE SUBJECT TO REGISTRATION OR RE-REGISTRATION
FIFRA 1998 ; RED Completed
NFPA : HR= health-2, flam.-0, react.-0
EU REGULATIONS: according to EC Directives
SYMBOL : C
HAZARD STATEMENTS, including R-phrase :
R34 Causes burns.
ADDITIONAL HAZARD STATEMENTS :
Harmful if inhaled and ingested. React with most metals to form flammable hydrogen gas.
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
OF THE SDS
No specific notes
TOC-LCPH/CPN 381
8.9.3 IC Reagent
Tel: 1(800) 477-1227
SECTION I PRODUCT AND COMPANY INFORMATION

PRODUCT NAME : IC reagent
COMPANY NAME : Shimadzu Corporation
ADDRESS : 1, Nishinokyo-Kuwabara-cho, Nakagyo-ku, Kyoto, Japan
DEPARTMENT : Analytical and Measuring Instruments Department, Environmental Business Unit
TELEPHONE NUMBER : 075-823-1207
FAX NUMBER : 075-823-4614
EMERGENCY CONTACT NUMBER :075-823-1207, Analytical and Measuring Instruments Department, Environmental Business Unit
SECTION II COMPOSITION/INFORMATION ON INGREDIENTS
SINGLE PRODUCT OR COMPOUND CLASSIFICATION :
Single product
CHEMICAL OR GENERIC NAME : Phosphoric acid
CONTENT : Phosphoric acid, 25% aqueous solution
CHEMICAL PROPERTIES (CHEMICAL FORMULA)
H3PO4
OFFICIAL GAZETTE REFERENCE NUMBER (CSCL/ISHL) :
1-422
CAS NO. : 7664-38-2
HAZARDOUS COMPONENTS : Phosphoric acid
SECTION III SUMMARY OF HAZARDOUS PROPERTIES
PRIMARY HAZARDOUS PROPERTY :
Corrosive to skin.
HAZARDS : 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.
In a mist or vapor state, causes irritation to the eyes, skin, mucous membrane, respiratory tract, and lungs.
Oral ingestion may cause nausea, vomiting, abdominal pain, and bloody diarrhea.
ENVIRONMENTAL IMPACT : Hazardous to aquatic organisms due to strong acidity.
PHYSICAL AND CHEMICAL HAZARDS :
Contact with alkaline substances generates heat.
Reacts with many types of metals to produce hydrogen gas that mixes with air to form a flammable and explosive gas.
CLASSIFICATION NAME : Corrosive substance
INHALATION : 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 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.
SKIN CONTACT : 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 the affected area without specific instruction from a
physician.
If the appearance of the skin changes or irritation and pain persist, transport to a hospital immediately.
EYE CONTACT : 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 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.
INGESTION : 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 taken immediately, give large amounts of water.
NEVER induce vomiting as this may have the opposite effect of damaging the stomach wall due to the corrosive nature of
the material. Never give anything by mouth to an unconscious person.
PROTECTION FOR THE GIVER OF FIRST AID:
The person who provides first aid should wear protective equipment including protective eyewear and protective gloves to
avoid contact with the hazardous substance.
SECTION IV FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA : This product does not ignite on its own.
Use a suitable extinguishing media for the other materials caused to ignite by this product.
SPECIFIC EXTINGUISHING METHOD :
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 location if fire breaks out.
If the container cannot be transferred to 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.
SPECIFIC HAZARDS : The molecules that comprise this substance contain phosphorus. Avoid inhaling any smoke produced due to contact with
fire as it contains irritants, toxic fumes and gas.
PROTECTION FOR FIREFIGHTERS :
Always wear suitable protective equipment due to the strong acidity of the liquid.
Perform firefighting from an up wind position as mush as possible. Wear protective equipment that covers the eyes, nose,
and mouth to prevent exposure and inhalation of smoke that contains toxic gas.
382 TOC-LCPH/CPN
SECTION V ACCIDENTAL RELEASE MEASURES

PERSONAL PRECAUTIONS : 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 not perform any work down wind
from the 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.
ENVIRONMENTAL PRECAUTIONS :Take measures to prevent the discharge of this product into rivers that will adversely affect the environment.
When this substance is diluted with large amounts of water, do not allow the discharge of contaminated water into the
environment without suitable treatment. Do not discharge spilled material directly into rivers or the sewage system.
CLEANUP METHOD : SMALL SPILLS : Clear away any spilled material after soaking it up with dry sand or earth. Alternatively, dilute the
spilled material with water, neutralize it with lime hydrate or soda ash, and then wash the material
away with a large amount of water.
LARGE SPILLS : 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.
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.
SECTION VI HANDLING AND STORAGE
HANDLING : TECHNICAL MEASURES :
• 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.
• Prevent the generation of mist and vapor as much as possible and keep the work 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.
• 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 compounds, and metal powder at removed 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.
PRECAUTIONS : If there is a risk that mist or vapor may be generated, handle the material
within local ventilation or at a location with general ventilation equipment.
PRECAUTIONS FOR SAFE HANDLING : Avoid contact with alkaline substances due to the material's strongly acidity.
As this liquid reacts with metals, select a suitable material for handling.
As this material will cause metals such as iron to rust, relevant facilities
require anti-rust treatment.
STORAGE CONDITIONS FOR SAFE 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.
• Install drainage prevention facilities to 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.
SAFE CONTAINERS AND PACKAGING MATERIAL :
Due to a strong corrosive reaction with metals, select a suitable material to handle this liquid.
Cast iron containers cannot be used.
Resin-based materials such as polyethylene, PTFE, and FRP as well as glass are resistant to this liquid.
SECTION VII EXPOSURE CONTROL AND PERSONAL PROTECTION
FACILITY MEASURES : In handling locations that generate mist or vapor, seal the generation source or use local ventilation equipment.
Install facilities for emergency eye and body washing near the area of handling and clearly indicate the position of such
facilities.
CONTROL CONCENTRATION : Not set.
ACCEPTABLE CONCENTRATION : Japan Society for Occupational Health 1 mg/m3
ACGIH1mg/m3 (TLV-TWA) 3 mg/m3 (TLV-STEL)
*) TWA : Time-weighted average value,
STEL : Short-term exposure limit
PROTECTIVE EQUIPMENT RESPIRATORY PROTECTION : Gas mask for acidic gases
HAND PROTECTION : Protective gloves (impervious and acid resistant)
EYE PROTECTION : Protective eyewear (normal glasses with side protection, goggles)
SKIN PROTECTION : Protective clothing (long-sleeved work clothes), protective shoes, apron
TOC-LCPH/CPN 383
SECTION VIII PHYSICAL AND CHEMICAL PROPERTIES

PHYSICAL PROPERTIES SHAPE : Viscous liquid
COLOR : Clear and colorless
ODOR : Odorless
pH : Strongly acidic
FLASH POINT : Nonflammable.
DENSITY (SPECIFIC GRAVITY) : 1.15 g/cm3 (20 °C)
SOLUBILITY SOLUBILITY WITH RESPECT TO SOLVENT: Freely mixes with water.
Soluble in ethyl alcohol.
SECTION IX STABILITY AND REACTIVITY
CHEMICAL STABILITY : Stable under normal handling conditions.
CHEMICAL REACTIVITY : 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 to the point of decomposition.
While a comparatively weak acid as an aqueous solution, it will react with iron, aluminum, and zinc to produce hydrogen
and generate each type of salt.
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 AVOID : Direct sunlight, heat
INCOMPATIBLE MATERIALS : Metals, alkaline substances
Phosphorus oxide, hydrogen gas
SECTION X TOXICOLOGICAL INFORMATION
ACUTE TOXICITY : Oral ingestion may cause nausea, vomiting, abdominal pain, and bloody diarrhea.
Rat, oral LD50 1,530 mg/kg
Rabbit, skin LD50 2,740 mg/kg
Human, inhalation TCL0 100 mg/m3
LOCAL EFFECTS IRRITATION (SKIN, EYES) : Contact with the eyes causes irritation and may cause conjunctival
hyperemia, corneal impairment, and iritis.
Contact with the skin and mucous membrane causes itching and pain
and may cause soreness and inflammation.
In a mist or vapor state, causes irritation to the eyes, skin, mucous
membrane, respiratory tract, and lungs.
CHRONIC AND LONG-TERM TOXICITY : Repeated inhalation of mist or vapor may cause bronchitis.
CARCINOGENICITY : Not included on IARC and NTP lists.
MUTAGENICITY : Not available
TERATOGENICITY : Not available
REPRODUCTIVE TOXICITY : Not available
SECTION XI ENVIRONMENTAL INFORMATION
MOBILITY : From its physicochemical properties, this material has the potential to move into atmospheric, aquatic, and soil
environments.
RESIDUAL/RESOLVABILITY : Not available
ECOTOXICITY TOXICITY TO FISH : Hazardous to aquatic organisms.
LD50 over 96 hours is 100-10 mg/L.
The fatal dose for fish is 135 mg/L.
SECTION XII DISPOSAL CONSIDERATIONS
RESIDUAL WASTE : 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.
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.
Always wear protective equipment suitable to the task at hand.
Protective equipment : Protective eyewear or face shield, impervious protective gloves, protective shoes, protective
clothing (impervious, long-sleeved work 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.
CONTAINER : Dispose of containers after completely removing their contents.
SECTION XIII TRANSPORTATION INFORMATION
UN CLASSIFICATION : Class 8 (Corrosives), PG III
UN NUMBER : 1805
SPECIFIC SAFETY MEASURES AND CONDITIONS FOR TRANSPORTATION :
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 light-shielding cloth to avoid exposure to
direct sunlight. Prevent containers from becoming wet with rain.
Carefully handle containers to prevent 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.
384 TOC-LCPH/CPN
8.9.4 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime

Tel: 1(800) 477-1227

PRODUCT IDENTIFIER : Soda Lime
GHS CLASSIFICATION : Skin corrosion/irritation: Category 1B
HAZARD SYMBOL :
DANGER
PRECAUTIONARY STATEMENTS : <Prevention>
Wear protective gloves and eye/face protection.
Do not breathe dust
<Response>
IF ON SKIN (or hair): Remove/Take off immediately all contaminated clothing. Rinse skin with water/shower.
rinsing.
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.
<Disposal>
Dispose of contents/container to a located point.
EU CLASSIFICATION: according to Directive 67/548/EEC.
SYMBOL : C
R-phrase : R34 Causes burns.
S-phrase : S26 In case of contact with eyes, rinse immediately with plenty of water and seek medical advice.
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.
CHEMILCAL IDENTITY : Soda lime
FORMULA : -----
MOLECULAR WEIGHT : -----
TSCA INVENTORY : Not listed (See Section 15)
EINECS No. : Not listed
EC INDEX NUMBER : Not listed
INHALATION : Move victim to fresh air. If breathing is difficult, give oxygen. If breathing has stopped, administer artificial respiration.
Maintain normal body temperature with a blanket. If irritation persists, transport to a hospital immediately.
immediately.
INGESTION : Rinse mouth, give plenty of water to dilute the substance. Do not induce vomiting. Never give anything by mouth to an
unconscious person. Transport to a hospital immediately.
EXTINGUISHING MEDIA : Not combustible. Use extinguisnig media appropriate to the surrounding fire.
FIRE & EXPLOSION HAZARDS : Toxic and irritating dust, fumes or smoke may be emitted.
apparatus.
Avoid raising dust and avoid contact with skin and eyes.
ENVIRONMENTAL PRECAUTIONS : Prevent spills from entering sewers, watercourses or low areas.
METHODS FOR CLEANING UP : Do not touch spilled material without suitable protection (See section 8). After material is completely picked up, wash 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.
TOC-LCPH/CPN 385

protection.
This material is hygroscopic.
INCOMPATIBILITIES : Strong acids
Respiratory protection : NIOSH/MSHA approved respirator
CONTROL PARAMETER : OSHA Final Limits : None established
ACGIH TLV(s) : None established
APPEARANCE : White - slightly brown, shot
ODOUR : Odorless
pH : Not available
MELTING POINT : Not available
INITIAL BOILING POINT : Not available
FLAMMABILITY (solid, gas) : Not available
VAPOR PRESSURE : Not available
SPECIFIC GRAVITY : 2.1
SOLUBILITY IN ; WATER : Practically insoluble
PARTITION COEFFICIENT : Not available
CHEMICAL STABILITY : Stable under recommended storage conditions.
CONDITIONS TO AVOID : Sunlight, heat, moisture
INCOMPATIBILE MATERIALS : Strong acids
Not available
Not available
TOXICITY DATA : Harmful if inhaled and ingested.
SKIN CORROSION/IRRITATION : May be harmful if absorbed through skin. Causese skin burns.
EYE DAMAGE/EYE IRRITATION : Causes burns.
Not available
GERM CELL MUTAGENICITY : Not available
TOXIC TO REPRODUCTION : Not available
STOST-SINGLE EXPOSURE : Not available
IARC : Not listed
OSHA : Not listed
ACGIH : Not listed
ECOTOXICITY : Not available
Not available
OTHER ADVERSE EFFECTS : Not available
package them for hazardous-waste disposal. Flush the aqueous solutions down the drain with plenty of water.
Any disposal practice must be in compliance with country, local, state, and federal laws and regulations (contact country,
local or state environmental agency for specific rules).
After contents are completely removed, dispose of its container in accordance with local/regional/national/international
regulation.
386 TOC-LCPH/CPN

UN PROPER SHIPPING NAME : Corrosive solid, basic, inorganic, n.o.s. (Soda lime)
PACKING GROUP : PG III
MARINE POLLUTANT : No
PROPER SHIPPING NAME : Corrosive solid, basic, inorganic, n.o.s.
US REGULATIONS ; New Jers. RTK Haz. Subst. List
EPA : CERCLA RQ= Not listed
EPCRA TPQ= Not listed
NFPA : HR= health-2, flam.-0, react.-1
HMIS : HR= health-2, flam.-0, react.-1
TSCA : Use of this product must be restricted to research or analysis for the development of a product in accordance
with the Act.
OF THE SDS
No specific notes
TOC-LCPH/CPN 387
8.9.5 Ceramic Fiber

Shimadzu Scientific Instruments, Inc. Revised Date: 2005/04
Tel: 1(800) 477-1227
SECTION I PRODUCT IDENTIFICATION
Refractory ceramic fiber
Alternative names: Polycrystalline alumino-silicate fiber, ceramic fiber
Trade Name: FIBERMAX
Product: Bulk fiber
Chemical composition: Al2O3 72-97, SiO2 3-28
SECTION II HAZARDOUS INGREDIENTS / IDENTITY INFORMATION
INGREDIENT % HAZARD DATA TLV-TWA REMARK S
3
Alumina Ceramic Fiber 100 0.2 f/cm Counting fibers;
[CAS# 675106-31-7] [Notice of Intended Changes on ACGIH] Longer ≥ 5 μm
Diameter about 3 μm Diameter < 3 μm
Length/Diameter ≥ 3
Hazard Data Source: ACGIH Threshold Limit Values for 2002

SECTION III PHYSICAL/CHEMICAL CHARACTERISTICS
Boiling Point: No data Solubility in Water: N/A
Melting Point: No data Appearance: White, loose wool
Evaporation Rate: N/A Odor: No odor-
Density (kg/m3): - Service Temperature (°C): 1,300 - 1,700
SECTION IV FIRE AND EXPLOSION HAZARD DATA
Flash Point (Method used): This product is not flammable. Special Fire and Fighting Procedures: None
Explosion Point (Method used): N/A Unusual Fire and Explosion Hazards: None
Extinguishing Media: N/A
SECTION V REACTIVITY DATA
Stability: Stable Hazardous Decomposition or By-products: None
Incompatibility (Materials to avoid): None Conditions to Avoid: None
SECTION VI HEALTH HAZARD DATA
Acute Hazard: Skin Contact: May cause irritation.
Eye Contact: May cause irritation, inflammation and rash.
Chronic Hazard: Repeated, prolonged or excessive inhalation of fiber may cause respiratory disease.
At this time there are no known published reports demonstrating negative health outcomes of workers exposed to ceramic fiber.
Other Precautions on Health Hazard:
1. Perform periodic medical examination by X-ray of the lung function of the workers who handle this product.
2. Perform periodic monitoring of individual exposure of workers who handle this product to check if exposure level is in compliance
with TLV.
3. Record details of operation and arrange training/education of workers.
4. Workers should wash hand and rinse mouth after use.
Emergency and First Aid Procedures:
Inhalation: First aid procedure is not necessary for respiratory tract. May cause cough, phlegm, etc., in case continue to inhale more
than acceptable level as described below. Get medical attention in such case.
Ingestion: Ingestion is unlikely. If ingested, drink sufficient water and vomit and get medical attention.
Skin Contact: Flush with water or slightly warm water and wash with soap. Get medical attention if pain and inflammation.
Eye Contact: Flush eyes with water for a least 15 minutes. Abrasive action may cause damage to the outer surface of the eye. Get
medical attention if irritating.
Carcinogenicity (Refractory Ceramic Fiber):
NTP: B2 - Reasonably anticipated to be a carcinogen
IARC Monographs: 2B - Possibly carcinogenic to humans
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.
1. There is a report that increase of lung tumor has been observed in rats exposed to the inhalation of 8.4 mg/m3 of Alumina Silicate
Ceramic Fiber (RCF) into lung for twelve months.
2. There is a report that pleural sarcoma has been frequently observed in rats exposed to the dose of ceramic fiber into pleural cavity,
especially be diameter less than 0.25 mm and length more than 8 μm (8 μm exclusive).
3. There is a report that pleural interstitial fibrosis has been observed in 3 rats out of 36 rats exposed to one dose of 20 mg RCF into
pleura.
4. 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 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.
5. There is a report that tumor has been observed in 2.6-14.5% of rats exposed to the inhalation of RCF 3-30 mg/m3 with kaolin as raw
materials for 24 months (6 hours per day, 5 days per week).
388 TOC-LCPH/CPN
SECTION VII PRECAUTION FOR SAFE HANDLING AND USE

Step to be taken in case material is released or spilled:
Use vacuum suction with HEPA filters to clean up spilled material suppressing generations of airborne dust. Wear air purifying respirator
or mask when clean up.
Precaution on waste disposal:
Disposal of this waste material must be by plastic bag with minimum 0.05mm thickness to prevent generations of airborne dust.
The transportation, storage, treatment and disposal of this waste material must be conducted in compliance with all applicable local
regulations.
Precaution on transportation:
Avoid generations of airborne dust by breakage of package during transportation. Repair broken part of package by adhesive tape and
also arrange new packing in case of breakage.
Refer "Step to be taken in case material is released or spilled" in this MSDS for treatment of spilled material.
SECTION VIII CONTROL MEASURES

Suppressive procedure: Restrict and separate areas where this product is used.
Close up tight and/or install/provide proper general and/or local ventilation at the places where dust concentrations exceeds TLV. Inspect
regularly such ventilation to maintain initial functions.
Respiratory Protection (Specify Type):
Respiratory protection must be selected/used according to airborne concentrations as described below.
Respiratory protection must be checked for fitness to face and also arranged proper maintenance on filter in case use Half-Face air
purifying respirator.
Concentration (8-hours TWA) Minimum Acceptable Respirator Type
0.1- 1 f/cm3 Disposable dust respirator.
1- 5 f/cm3 Half-Face, air-purifying respirator equipped with high-efficiency particulate air (HEPA) filter cartridges.
5-25 f/cm3 Full-Face, air purifying respirator with high-efficiency particulate air (HEPA) filter cartridges or
powered air-purifying respirator equipped with HEPA filter cartridges.
3
Greater than 25f/cm Full-Face, positive pressure supplied air respirator.
Eye Protection: Wear proper eye protection such as chemical goggles, safety glasses with side seal.
Other Protective Clothing or Equipment:
Wear gloves and long-sleeve work clothes to prevent skin irritation as necessary. Remove materials from area of contact of clothes by
vacuum suction with HEPA filter or adhesive tape avoiding generations of airborne dust.
Recommended workers who may be sensitive to a fiber not to engage in handling this product.
SECTION IX SPECIAL PRECAUTIONS
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, laws, regulations, etc.
NOTICE: The information presented herein is based on 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 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.
TOC-LCPH/CPN 389
8.9.6 Halogen Scrubber
Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date
MATERIAL SAFETY DATA SHEET
CAT. NO. 630-0092-00 CAS NO. 07740-50-8
NAME: Halogen Scrubber OTHER NAME: Copper Wool
PRODUCT USE: This product is for specific use with TOC instruments.
SECTION II PRODUCT USE
For use specifically with the Shimadzu TOC 500, TOC 5,000, and TOC 4,000 instruments. Consult the appropriate instrument manual for proper use.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
1083°C 2595°C N/A N/A N/A N/A N/A Reddish Solid Malleable N/A
Metal
SECTION IV HAZARDS IDENTIFICATION
Dust, mist or fumes may cause eye and skin irritation. Avoid contact.
SECTION V TOXICITY DATA
RAT/MOUSE LD50 RTECS# OSHA PEL ACGIH TLV-TWA
N/A GL5325000 N/A N/A
Exposure to large amounts can cause gastrointestinal disturbances, nausea, vomiting, headaches, or dizziness.
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes. in case of skin contact, immediately wash skin with soap and
copious amounts of water. if ingested and subject is conscious, immediately give large amounts of water. get medical attention.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: Appropriate to surrounding fire. Possible formation of toxic copper fumes. Use appropriate respiratory support.
SECTION IX ACCIDENTAL RELEASE MEASURES
N/A
INCOMPATIBILITIES: Strong acids, active halogens such as chlorine, fluorine, iodine, and bromine. ammonia.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
390 TOC-LCPH/CPN
8.9.7 High Sensitivity Catalyst

Tel: 1(800) 477-1227 Date
CAT. NO. 630-00996-00 CAS NO. N/A
NAME: High Sensitivity TC Catalyst OTHER NAME: Platinum on Quartz Wool
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
N/A N/A N/A N/A N/A N/A N/A Grey Fibrous Solid N/A
FLAMMABLE: Possible sensitizer. Keep away from sources of ignition - NO SMOKING. Take precautionary measures against static
discharges. Keep container tightly closed and in a well-ventilated place.
ACUTE EFFECTS: May be harmful by inhalation or ingestion. May cause eye irritation. May cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. Prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
EXPOSURE CAN CAUSE: Coughing, chest pains, difficulty in breathing. To the best of our knowledge, the chemical, physical, and toxicological
properties have not been thoroughly investigated.
SEE SECTION 5.
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 not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided
person is conscious. Call a physician. Remove and wash contaminated clothing promptly.
EXTINGUISHING MEDIA: CARBON dioxide, dry chemical powder or appropriate foam.
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves.
Sweep up, place in a bag and hold for waste disposal. Ventilate area and wash spill site after material pickup is complete.
INCOMPATIBILITIES: Strong oxidizing agents, organic materials.
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:Nature of decomposition products not known. Hazardous polymerization will not occur.
TOC-LCPH/CPN 391
8.9.8 Normal Sensitivity Catalyst

Tel: 1(800) 477-1227 Date
CAT. NO. 017-42801-01 CAS NO. 7440-06-4(Platinum) and 1344-28-1(Alumina)
NAME: Regular Sensitivity Catalyst OTHER NAME: Platinum on 1/8" Alumina Pellets
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
N/A N/A N/A N/A N/A N/A N/A Grey Solid Pellets N/A
FLAMMABLE: Possible sensitizer. keep away from sources of ignition - no smoking. Take precautionary measures against static discharges.
Keep container tightly closed and in a well-ventilated place. Harmful by inhalation. Irritating to respiratory system.
TARGET ORGAN(S): Lungs, bones, do not breathe dust. In case of insufficient ventilation, wear suitable respiratory equipment. Wear suitable
protective clothing.
ACUTE EFFECTS: May be harmful by inhalation or ingestion. May cause eye irritation. may cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
EXPOSURE CAN CAUSE: Coughing, chest pains, difficulty in breathing, gastrointestinal disturbances.
CHRONIC EFFECTS: Prolonged exposure can cause damage to the lungs and bones. TO the best of our knowledge, the chemical, physical, and
toxicological properties have not been thoroughly investigated.
TARGET ORGAN DATA: Lungs, thorax or respiration (tumors) tumorigenic (neoplastic by RTECS criteria) tumorigenic (equivocal tumorigenic agent by
RTECS criteria) tumorigenic (tumors at site of application) only selected registry of toxic effects of chemical substances
(RTECS) data is presented here. see actual entry in RTECS.
OSHA PEL: 8H TWA 5MG/ME respirable fraction; 8h TWA 10MG/M3 total dust
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 artificial respiration. If breathing is difficult, give oxygen. If 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 MEDIA: Carbon dioxide, dry chemical powder or appropriate foam.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS: Material may have an exothermic reaction above 200 c with halocarbon vapors and may produce toxic
hydrochloric acid and phosgene.
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Sweep up, place in a bag and hold for waste dis-
posal. Ventilate area and wash spill site after material pickup is complete.
Stability: Stable.
Incompatibilities: Strong acids, strong bases, chlorine trifluoride, ethylene oxide, halocarbons, oxygen difluoride, sodium nitrate, vinyl acetate,
strong oxidizing agents, organic materials. Protect from moisture. Hazardous combustion or decomposition products. Nature of
decomposition products not known. Hazardous polymerization will not occur.
392 TOC-LCPH/CPN
Appendix A
Appendix A Control Charts
The Control Charts software monitors precision and accuracy of a defined data set. The
software supports five types of Control Charts:
•Mean Value Control Charts
•Recovery Control Charts
•Blind Value Control Charts
•Spanwidth Control Charts
•User Defined Control Charts
The Mean Value Control Chart checks the accuracy of an analytical method on an
instrument. Control value drifts may indicate a change in system performance.
The Recovery Control Chart tests an analytical method for matrix influences and provides a
restrictive control of accuracy by testing proportional system errors. Using certified
standards will test the accuracy of the system as well as the recovery rate.
The Blind Value Control Chart is a special form of the Mean Value Control Chart used for
quality assurance of the instrument and variable elements. Unlike the Mean Value Control
Chart, the control value is the information value (absorbance, peak height, peak area)
received from the analysis.
The Spanwidth Control Chart tests the precision of an analytical method and monitors the
accuracy under actual conditions (Drift Control). For this type of Control Chart, there are
several existing models for calculating the control and warning limits.
Each type of control chart can be used to create charts for different working range and
analysis methods. For each control chart, a file is created which contains general
information about the type, data structure and other global data.
A.1 File Menu
Figure A.1 File Menu
A.1.1 New
The New function is used to define new control charts and displays the Control Chart
Wizard. Follow the Control Chart Wizard process to enter a new control chart. The file
extension *.cc is used for all control charts.
Note: Control Chart parameters can be changed at a later time by selecting
Options>Control chart options from the main menu bar.
Control Chart Wizard System Information Window

The first page of the Control Chart Wizard is used to enter basic system information and is
similar to the System Information pages in the Method and Sample Wizards. Refer to
Section 5.4.2 "Inserting a Sample" and Section 5.3.3 "Creating a Method".
Figure A.2 Control Chart Wizard: System Information Window
394 TOC-LCPH/CPN
Control Chart Wizard Control Chart Type Window
Select the type of control chart to be created and select the analysis type from the drop
down list.
Figure A.3 Control Chart Wizard: Control Chart Type Window
Control Chart Wizard Control Chart Parameters Window

Enter the control chart parameter values and limits as described below.
Figure A.4 Control Chart Wizard: Control Chart Parameters Window
Setting Item Description

Automatic calculation of the Select to enable automatic calculation of the control chart
control chart limits limits. The upper and lower warning and control limits are
calculated after the control samples for the preparation period
are added to the control chart.
No. of samples in the pre- Enter the number of samples in the preparation period. The
period default value is 12. This option is disabled if the Automatic
calculation of the control chart limits option is not selected.
No. of samples in the control Enter the number of samples in the control period. The
period default value is 50.
TOC-LCPH/CPN 395
Working range Enter the upper and lower limits of the working range. Match
the range with the concentration of samples used for control
tracking and the concentration range of the selected
calibration curve. Use the drop-down list to select the units.
Rated Value Enter the rated value of the working range. This option is
enabled if the Automatic calculation of the control chart
limits option is not selected.
Control Limits Enter the upper and lower control limits. This option is
Warning Limits Enter the upper and lower warning limits. This option is
Exclusion Limits Enter the upper and lower exclusion limits.
Control Chart Wizard Recovery Control Chart Parameter Window

This window is only displayed if the Recovery Control Chart is selected in the Control
Chart Wizard, and Automatic calculation of the control chart limits is not selected.
Figure A.5 Control Chart Wizard: Recovery Control Chart Parameter Window

Use of certified standard Select this option to use a certified sample as a control
sample.
Fixed theoretical Select this option if the standard has a fixed concentration.
concentration Enter the concentration in the text box.
Use of real sample Select this option if the control sample is a real sample.
Fixed concentration of the Select this option if the spiked component has a fixed
spiked component. concentration. Enter the concentration in the text box.
396 TOC-LCPH/CPN
Control Chart Wizard Spanwidth Control Chart Options Window
This window is only displayed if the Spanwidth Control Chart is selected in the Control
Chart Wizard.
Figure A.6 Control Chart Wizard: Spanwidth Control Chart Options Window

No. of inj. per sample Enter the number of injections for a sample used in the
control chart. The default value is 3, and the range is 3-25.
Refuse control samples with Select this option to exclude from the control chart samples
different inj. no whose number of injections differs from those specified in
the No. of inj. per sample field.
TOC-LCPH/CPN 397
Control Chart Wizard History Window
The Control Chart Wizard History function is identical to other history functions in the
TOC-Control V system. Refer to Section 5.3.3 "Creating a Method" for more details about
the History function. The History window provides information on all control chart
changes when enabled.
Figure A.7 Control Chart Wizard: History Window

Enable history log Select this option to enable the History Log, which is used to
monitor all modifications to the control charts. Once the
History Log is enabled, it cannot be turned off.
Operator has to comment on Select this option to require the user to enter comments or
all modifications obtain approval for modifications to the control charts.
A.1.2 Following Control Chart

Select the Following Control Chart menu item to create a Following Control Chart. It is
recommended that a new control chart be created after 50 samples have been entered in the
control period. The new control chart uses the calculated standard deviation from the
control period as the new control chart limits. Control chart options are:
File Name Displays the name of the currently active control chart.
Save the current control chart Enter a new file name in this field to save the currently active
as control chart to a new location or with a new file name. A
confirmation message is displayed to confirm the operation.
Create Select this option to create the Following Control Chart. The
new limits are calculated from the samples of the control
period stored in the previous control chart.
Parameter Select this option to display the parameters of the newly
created Following Control Chart. This function can also be
accessed using the Options>Control Chart Options command
in the main window.
398 TOC-LCPH/CPN
A.1.3 Open
The Open command is used to open files. Select a *.cc file to open a control chart file.
A.1.4 Save
The Save command saves the current control chart.
A.1.5 Save As
Use the Save As command to save files for the first time, or to save a file using a new file
name. Files can be saved as file types *.cc or *.txt (ASCII format).
A.1.6 Print>Data
Use the Print>Data command to print data in spreadsheet format. For more information on
the Print function, refer to Section 5.6.4.1 "Sample Table".
A.1.7 Print>Graph
Use the Print>Graph command to print data in graphical format. For more information on
the Print function, refer to Section 5.6.4.1 "Sample Table".
A.1.8 Print Preview>Data/Print Preview>Graph

Use the Print Preview>Data function to display a preview of the data to be printed. Use the
Print Preview>Graph function to display a preview of the graph to be printed. For more
information on the Print Preview function, refer to Section 5.6.3.1 "Sample Table Preview".
TOC-LCPH/CPN 399
A.1.9 Print Setup
Use the Print Setup command to select the printing parameters.
Figure A.8 Print Setup Dialog Box
The print options available vary based on the printer installed. Select the paper size and
source from the drop-down lists, and select Portrait or Landscape to change the orientation
of the printed file. Select OK to save the selections, or Cancel to close the dialog box
without saving changes.
A.1.10 Page Setup

Use the Page Setup command to select items to be printed and to select options for printing
format, such as margins, headers, and footers.
Figure A.9 Page Setup Window: Data Tab
The Page Setup window consists of several tabs. Use the OK button to save changes and
exit the Page Setup window. Click the Cancel button to exit the Page Setup window without
saving changes. Click the Apply button to update the parameters without closing the Page
Setup window.
Note: On each tab in the Page Setup window, certain items are checked (selected) by
default. To deselect these options, click the item.
400 TOC-LCPH/CPN
Data Tab
The Data tab displays a list of items that can be selected for printing. Select the desired
items and click the OK button.
Grid Tab
Figure A.10 Page Setup Window: Grid Tab
The Grid tab displays a list of format items for the report.
Option Description
Row Headers Prints row headers in the table.
Column Headers Prints column headers in the table.
Print Frame Prints a frame around the table.
Vertical Lines Prints vertical lines in the table.
Horizontal Lines Prints horizontal lines in the table.
Only Black and White Prints only in 2 colors, without gray backgrounds or other
colors.
First Rows, then Columns Prints rows first, followed by columns, when more than one
page is printed
First Columns, then Rows Prints columns first, followed by rows, when more than one
page is printed.
Vertical Prints the table on the vertical center of the page.
Horizontal Prints the table on the horizontal center of the page.
TOC-LCPH/CPN 401
Miscellaneous Tab
Figure A.11 Page Setup Window: Miscellaneous Tab
The Miscellaneous tab displays a list of format items for the report, as described below.
Margins Use the spin controls to enter the page margins (in mm).
Footer, Page No. Select this option to print the page number in the footer of
each page.
Header Organization: Select this option and enter the name of the
organization in the text box to print the organization name in
the page header.
Logo: Select this option to print a bitmap in the page header.
Use the Browse button to select the bitmap file.
Date/Time: Select this option to print the current system date
and time in the page header.
Operator: Select this option to print the current user name in
the page header.
A.1.11 Exit
Select Exit to close the Control Chart application.
402 TOC-LCPH/CPN
A.2 Edit Menu
Figure A.12 Edit Menu
Copy
Use the Copy command to copy the selected range from the data table to the clipboard.
Recalculate
Use the Recalculate command to recalculate the limits of the control chart. This function
should be performed after one or more control samples have been excluded or added to the
control chart.
Exclude
Use the Exclude command to exclude a selected range of control samples from the control
chart calculations. When Exclude is selected, the Exclude dialog box is displayed. Enter a
comment describing the reason for excluding the sample. The Exclude function is only
available when one or more control samples are selected. A dialog box displays a message
requesting confirmation that the sample be excluded. Select Yes to confirm and recalculate
the control limits, or No to abort recalculation.
TOC-LCPH/CPN 403
A.3 View Menu
Figure A.13 View Menu
A.3.1 Statistics
The Statistics command displays the Statistics window.
Figure A.14 Statistics Window

Type Displays the type of control chart.
No. of samples (pre-period) Displays the number of samples in the preparation period.
This value was entered in the Control Chart Wizard.
Total no. of samples Displays the total number of samples in the control chart.
Excluded samples are not included in the total number.
Control limits Displays the control limits.
Data from the control period Displays the Average Control Value, which is the mean value
of the samples in the control period. Also displays the
calculated standard deviation and coefficient of variation.
404 TOC-LCPH/CPN
A.3.2 Comparison
After a control chart is completed, the results from the control period must be compared
with the results from the preparation period. For control charts without a preparation
period, the current values must be compared with the results of the preparation period or the
control period from the previous control chart. The View>Comparison command displays
the Comparison between control charts window.
Figure A.15 Comparison Between Control Charts Window

Previous control chart Displays the file name of the previous control chart, if
applicable.
Mean value t-test Displays the results of the T-test in the text box beneath the
Item and Value lists. The T-table value and the calculated test
value are also displayed in the Item and Value list. The test
value is calculated based on the mean values and variances
obtained from the control and preparation period. The T-test
result shows whether the long term deviation of the control
samples is significant.
F-test Displays the results of the F-test in the text box beneath the
Item and Value list. The F-table value and the calculated test
value are also displayed in the Item and Value list.
TOC-LCPH/CPN 405
A.3.3 Out of Control Events
The Out of Control Events window displays a list of all out of control events.
Figure A.16 Out of Control Events Window
Spl. No.
Displays the sample number for which the out of control event occurred.
Event
Describes the out of control event.
A.3.4 Toolbar/Status Bar

The View>Toolbar and View>Status Bar commands show and hide the Toolbar and Status
Bar, respectively.
406 TOC-LCPH/CPN
A.4 Options Menu
Figure A.17 Options Menu
A.4.1 Control Chart Options

Use the Control Chart Options command to view and edit the control chart parameters
entered in the various pages of the Control Chart Wizard. Refer to Section A.1.1 "New".
Note: Some options within the Control Chart Options tabs (such as control chart type or
sample concentrations) may be disabled if the control chart contains data. The
disabled parameters are options that cannot be modified once data is entered.
A.4.2 Font
The Font command opens the standard Font dialog box. Refer to Section 5.8.6 "Display
Font" for detailed information about font options.
TOC-LCPH/CPN 407
A.4.3 Floating Point Numbering Format
The Floating Point Numbering Format command is used to select display options for
numeric results in the control charts. These options apply only to the manner in which
numbers are displayed; internal data retain their original values.
Figure A.18 Floating Point Format Window
Common Floating Point Numbers

Number of significant digits Select this option to display common floating point numbers
using a specified number of significant digits. Use the spin
control to set the number of significant digits. The default
value is 4.
Number of digits after the Select this option to display common floating point numbers
decimal point using a specified number of digits after the decimal point.
Use the spin control to set the number of digits after the
decimal point. The default value is 2.
Percent Values
Number of significant digits Select this option to display percent values using a specified
number of significant digits. Use the spin control to set the
number of significant digits. The default value is 4.
Number of digits after the Select this option to display percent values using a specified
decimal point number of digits after the decimal point. Use the spin control
to set the number of digits after the decimal point. The default
value is 2.
408 TOC-LCPH/CPN
A.4.4 ASCII Export Options
The ASCII Export Options function is used to export control chart data to an ASCII-
formatted file.
Figure A.19 ASCII Export Options Dialog Box

Header Select this option to export control chart file header.
Data Select this option to export control chart data.
Limits Select this option to export control chart limits.
Separator Select the type of separator to be used between items in the
ASCII file.
Export strings in quotation Select this option to add quotation marks to all exported
marks strings.
To export a file, create or open a control chart. Select the desired options from the ASCII
Export Options dialog box, and select OK. The File>Save As dialog box is displayed. Enter
a file name for the ASCII file and select the *.txt file type.
A.4.5 Enable Exclusion

Use the Enable Exclusion command to exclude a selected range of control samples from
the control chart calculations. When the Enable Exclusion command is executed, the
Exclude dialog box is displayed. Enter a comment describing the reason for excluding the
sample. This option is only available when one or more control samples are selected. A
dialog box displays a message requesting confirmation that the sample be excluded. Select
Yes to confirm and recalculate the control limits, or No to abort the process.
TOC-LCPH/CPN 409
A.5 Help Menu
About ContrCharts...
Use the About command to view copyright and version information.
410 TOC-LCPH/CPN
Index
Numerics
8-port sampler .................. See OCT-L (8-port sampler)
A
Accessories ASI-L (autosampler)
Special..............................................................349 External views....................................................17
Standard ...........................................................347 Filling with sample ............................................ 72
Acid Initialization ..................................................... 308
Inspection .........................................................272 Inoperable ........................................................ 323
Preparation .........................................................44 Installation ....................................................... 364
Adjusting and storing standard solution.....................59 Measurement.....................................70, 173, 216
Adjusting the sparge gas flow rate.............................46 Needle replacement.......................................... 366
Placing vials in the vial rack ..............................73
Preparing the stirrer ...........................................77
Rinse bottle inspection.....................................295
Rinse pump head replacement .........................296
Sample catcher inspection ............................... 295
Specifications................................................... 343
Autosampler..........................See ASI-L (Autosampler)
B
Background monitor ................................................213 B-type halogen scrubber
Blank check analysis..................................................64 Inspecting the internal liquid ........................... 274
Preparation ......................................................... 56
Replacing the internal liquid............................294
C
Calibration curve Checking the calibration curve
Creation............................................................126 for calculating concentration ................................... 190
Inserting into the sample table .........................160 Checking the water level in the drain container ...... 272
Reviewing and editing .....................................146 Clearing measurement results..................................194
Carrier gas CO2 absorber
Flow rate settings ........................................ 83, 84 Installation ......................................................... 45
Pressure settings.......................................... 83, 84 Replacing ................................................ 281, 290
Carrier gas purification tube Combustion tube
Replacing the CO2 absorber Connection ......................................................... 27
for carrier gas purification................................290 Removal ...........................................................277
Washing/replacement.............................. 279, 281 Washing/replacement.......................................281
Catalyst Consumable parts..................................................... 351
Filling .................................................................22 Control sample
Regenerating ....................................................275 Creation............................................................ 139
Washing and replacing catalyst........................277 Inserting into the sample table .........................167
Changing the calibration curve Reviewing and editing .....................................156
for calculating concentration....................................191 Copy......................................................................... 180
Creating a new file.........................126, 133, 139, 145
D
Data storage..............................................................249 Dilution water
Decimal point display ..............................................243 Checking .......................................................... 272
Default analysis parameters .....................................248 Preparing............................................................ 43
Displaying peaks......................................................184
Displaying software version information ................ 257
TOC-LCPH/CPN 411
Index
E
Editing measurement conditions ............................. 187 Excluding injection results ...................................... 192
Editing mode............................................................ 223 Exporting to ASCII format...................................... 207
Error messages......................................................... 311
F
File viewer Flow diagram............................................................. 12
Displaying and hiding interface items ............. 241 Font settings ....................................................240, 242
Position ............................................................ 119
Settings for displaying files ............................. 239
H
Halogen scrubber High sensitivity measurement ...................... 61, 75, 81
MSDS .............................................................. 390 Humidifier .........................................................42, 273
High sensitivity catalyst, MSDS.............................. 391
I
Inserting a sample .................................................... 162 Instrument....................................................See TOC-L
Inspection Instrument connection
Daily ................................................................ 272 Connecting...............................................103, 210
Periodic ............................................................ 275 Disconnecting .................................................. 210
Installation ................................................................. 45
L
Login........................................................................ 244
M
Maintenance............................................................. 271 Measurement principles .......................................... 330
Maintenance history ................................................ 309 Measuring gas samples............................................ 266
Maintenance parts list .............................................. 355 Menu bar.................................................................. 119
Manual injection measurement................................ 260 Method
Material Safety Data Sheets .................................... 376 Creation ........................................................... 133
Measurement Inserting into the sample table......................... 168
Changing to editing mode Reviewing and editing..................................... 152
during measurement ........................................ 223 Monitor .................................................................... 213
Manual injection measurement........................ 260 MSDS ...................................................................... 376
Measuring gas samples .................................... 266 halogen scrubber.............................................. 390
Stopping measurement .................................... 221 high sensitivity catalyst ................................... 391
With ASI-L or OCT-L ..................................... 216 normal sensitivity catalyst ............................... 392
Without ASI-L or OCT-L................................ 218
N
Normal sensitivity catalyst, MSDS ......................... 392
O
OCT-L (8-port sampler) Online manual
8-Port valve rotor replacement ........................ 297 Displaying the online manual.......................... 256
External views ................................................... 18 Selecting the online manual to display............ 256
Initialization..................................................... 308 Operation history log............................................... 246
Inoperable ........................................................ 324 Operational checks .................................................. 307
Installation ....................................................... 370 Organizing files ....................................................... 253
Specifications................................................... 343
412 TOC-LCPH/CPN
Index
Output window
Displaying and hiding interface items .............241
Position.............................................................119
Setting the display font ....................................240
P
Page settings.............................................................195 Print
Peak Stop..................................................................221 Previewing a sample report before printing.....200
Preparing for IC measurement ...................................51 Previewing the sample table before printing ...199
Preparing for POC measurement ...............................54 Sample report................................................... 203
Preparing the suspended solids kit .............................49 Sample table..................................................... 202
Selecting content to print ................................. 195
Setup ................................................................ 198
Printer settings .........................................................198
R
Ready indicator ........................................................119 Replacing O-rings
Recalculating measurement results..........................193 (on the sliding sample injector) ............................... 287
Regenerating IC reagent...........................................305 Replacing the CO2 absorber filling agent
Regenerating TC catalyst .........................................275 for POC measurement.............................................. 293
Releasing the time out lock......................................245 Replacing the halogen scrubber............................... 281
Removing bubbles from streams..............................306 Replacing the pump head
on the IC reagent delivery pump..............................292
S
Sample table Searching for files....................................................252
Copy .................................................................180 Setting the number of decimal places ...................... 243
Creation............................................................125 Setting warning values.............................................309
Cut....................................................................180 Settings for exporting to ASCII format ...................204
Deleting sample................................................182 Shutdown ................................................................. 224
Display options ................................................234 Sleep......................................................................... 226
Displaying file information..............................183 Sparge processing ........................................... 332, 338
Editing measurement conditions......................177 Sparging ..................................................................... 66
Insert sample ....................................................162 Specifications...........................................................342
Paste .................................................................180 Status bar
Reviewing and editing .....................................146 Displaying and hiding interface items ............. 241
Sample Table Editor Position ............................................................ 119
Exiting..............................................................108 Status monitor .......................................................... 119
General flow of analysis ....................................88 Stirrer ......................................................................... 77
Lock .................................................................244 Syringe pump
Start ..................................................................119 Replacing the 8-port valve rotor ...................... 288
Sample window Replacing the plunger tip................................. 286
Display .............................................................184 Zero point detection .........................................305
Display options ................................................236 System configuration
Graph display ...................................................185 Creation............................................................ 110
Schedule Deleting............................................................ 118
Creation............................................................145 Reviewing and editing .....................................116
Loading schedules into the sample table..........172
Reviewing and editing .....................................157
TOC-LCPH/CPN 413
Index
T
Technical information..................................... 330, 335 TOC-L
TN analysis preparation............................................. 55 External views and configuration diagrams ........ 8
TNM-L (TN unit) Flow diagram..................................................... 12
External views ................................................... 19 Installation ....................................................... 357
Installation ....................................................... 373 Maintenance parts............................................ 271
NOx absorber............................................ 55, 303 Specifications .................................................. 342
Replacing the catalyst Tool bar
in the ozone treatment unit .............................. 299 Displaying and hiding interface items............. 241
Specifications................................................... 343 Position ............................................................ 119
Chemiluminescence detector replacement ...... 301 Troubleshooting....................................................... 311
Ozone generator replacement .......................... 301 Turning ON the power supply
Electric furnace..........................................85, 110
Main unit ........................................................... 89
V
Vial
Setting the vial number.................................... 173
Types ................................................................. 70
W
Washing streams...................................................... 306 Water supply
Supplying water to the cooler
drain container ...........................................41, 272
Supplying water to the humidifier.............42, 273
Z
Zero point detection................................................. 305
414 TOC-LCPH/CPN

Toc-L CP

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TOTAL ORGANIC CARBON ANALYZER

Also, keep this manual for future reference.

© 2011-2012 Shimadzu Corporation. All rights reserved.

Precautionary Conventions Used in this Manual

The following precautionary conventions are used in this manual.

CAUTION Indicates a potentially hazardous situation which, if not avoided, may

Note: Emphasizes additional information that is provided to ensure the proper

Other Conventions Used in this Manual

Instrument Model Names

TIP » Indicates a particular technique, alternative means of operation, or useful advice.

This instrument is a total organic carbon analyzer.

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

To ensure safe operation, contact your Shimadzu representative if product installation,

Emergency Stop Procedure

During a Power Outage

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

High Temperature Warning

Replacement Parts Availability

Maintenance, Inspections, and Adjustment

Action for Environment (WEEE)

To all users of Shimadzu equipment in the European Union:

Contact Shimadzu service representative when the

EN55011 Emissions (Electromagnetic Interference)

EN61326-1 Immunity (Electromagnetic Susceptibility)

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

EMC Directive 2004 / 108 / EC

Chapter 2 System Description

Chapter 3 Preparation for Measurement

Chapter 4 Analysis Procedure

Chapter 5 Software Operations

Chapter 6 Analysis with Special Options

Chapter 8 Reference Information

3 Preparation for Measurement.............................................................. 21

4 Analysis Procedure ............................................................................... 87

5 Software Operation.............................................................................. 109

6 Analysis with Special Options............................................................. 259

8 Reference Information......................................................................... 329

Appendix A Control Charts ....................................................................... 393

This page is intentionally left blank.

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

1.2 Operational Precautions

Take the following precautions when using this instrument.

TOC-L Drain tubing (Tubing

Figure 1.1 External Drain Tubing

Carrier gas is discharged Never turn the lever

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

This page is intentionally left blank.

2.1 TOC-LCPH/CPN Construction

2.2 Autosampler ASI-L (Option)

2.3 8-Port Sampler OCT-L (Option)

2.4 TN Unit TNM-L (Option)

2.1 TOC-LCPH/CPN Construction

2.1.1 Front View

Power switch (with LED)

Figure 2.1 Front View

2.1.2 Right Side View

Main power switch

Figure 2.2 Right Side View

2.1.3 Left Side View

Drain pot IC reagent Hydrochloric Diluent bottle Drain tubing

Figure 2.3 Left Side View

2.1.4 Rear View