638-94837 Toc-L Ssm-5000a Um en Labsolutionstoc
638-94837 Toc-L Ssm-5000a Um en Labsolutionstoc
638-94837 Toc-L Ssm-5000a Um en Labsolutionstoc
Apr. 2021
SSM-5000A
User's Manual
For LabSolutions TOC
Read this manual thoroughly before you use the product.
Keep this manual for future reference.
This page is intentionally left blank.
Introduction
Read this Instruction Manual thoroughly before using the product.
Thank you for purchasing this product. This USER'S MANUAL describes how to use
this product in addition to any accessories and options related to this product. Read this
manual thoroughly before using the product and operate the product in accordance with
the instructions in this manual.
IMPORTANT
• If the user or usage location changes, ensure that this Instruction Manual is
always kept together with the product.
• If this manual or a product warning label is lost or damaged, immediately contact
your Shimadzu representative to request a replacement.
• To ensure safe operation, read all Safety Instructions before using the product.
• To ensure safe operation, contact your Shimadzu representative if product
installation, adjustment, or re-installation (after the product is moved) is required.
Notice
• Information in this manual is subject to change without notice and does not represent a commitment on the
part of the vendor.
• Any errors or omissions which may have occurred in this manual despite the utmost care taken in its
production will be corrected as soon as possible, although not necessarily immediately after detection.
• All rights are reserved, including those to reproduce this manual or parts thereof in any form without
permission in writing from Shimadzu Corporation.
• Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States and/or other
countries.
Microsoft®, Windows® XP Operating System is expressed as Windows XP.
Microsoft® Windows 7® Operating System is expressed as Windows 7.
Microsoft® and Windows® are either registered trademarks or trademarks of Microsoft Corporation in the
United States and/or other countries.
• PARAFILM 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.
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.
Convention Description
Reference: Indicates a reference location in the manual where more detailed information can
be found.
ii SSM-5000A
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 solid sample module for total organic carbon analyzer.
Use this instrument ONLY for the intended purpose.
Using this instrument for any other purpose could cause accidents.
Installation Site
Installation
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.
SSM-5000A iii
In an Emergency
In an emergency, turn OFF the power switch on the right side towards the rear of the
SSM-5000A as well as the main power switch on the right side towards the top of the
TOC-L.
Also, when the product is used again, inspect the product and, if necessary, contact
your Shimadzu representative to request servicing.
iv SSM-5000A
Warning Labels and Residual Risks
In order to ensure safety, warning labels are attached in places requiring caution.
If a warning label is lost or damaged, obtain a new label through your Shimadzu
representative and attach it in the correct position. A residual risk indicates a risk that
could not be reduced or eliminated in the process of design and manufacture. Be sure to
thoroughly read and understand the contents in "Description" before using the product.
SSM-5000A v
2
3
vi SSM-5000A
5
SSM-5000A vii
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
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.
viii SSM-5000A
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 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.
SSM-5000A ix
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.
Note: Cobalt oxide may occur after using this product. Handle with care.
To dispose of it, ask an industrial waste disposer in compliance with the local
laws and regulations.
x SSM-5000A
Electromagnetic Compatibility
This instrument complies with European standard EN50011 class A for
electromagnetic emission and EN61326-1 for electromagnetic immunity.
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.
SSM-5000A xi
Contents of this Manual
1 - Overview
This section gives an overview of the instrument and describes precautions to ensure its
safe use.
2 - System Components
This section describes the names and major functions of the various components of the
SSM-5000A.
3 - Operation
This section describes screen displays and procedures for pre-analysis preparation of
the instrument, sample analysis, and calibration curve measurement.
4 - Maintenance
This section describes maintenance, servicing and other important procedures for
operating the instrument. Error messages and troubleshooting procedures are also
described.
5 - Reference Information
This section describes the instrument specifications, accessories, and consumables. The
appropriate installation conditions are explained. Refer to this section when moving the
instrument.
xii SSM-5000A
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 and Residual Risks...................................................................................... v
Warranty ..................................................................................................................................... viii
After-Sales Service and Availability of Replacement Parts ....................................................... ix
After-Sales Service ................................................................................................................ ix
Replacement Parts Availability ............................................................................................. ix
Disposal Precautions................................................................................................................... x
Maintenance, Inspections, and Adjustment ................................................................................ x
Electromagnetic Compatibility ................................................................................................... xi
Contents of this Manual.............................................................................................................. xii
1 1Overview ................................................................................................................... 1
1.1 Overview ........................................................................................................................ 2
1.2 Operational Precautions ................................................................................................. 3
3 3Operation .................................................................................................................. 13
3.1 Analysis Preparations ..................................................................................................... 14
3.1.1 Sample Boats, Measurement Tools, and Quartz-glass Filter Paper ....................... 14
3.1.2 Pulverizing the Sample .......................................................................................... 16
3.1.3 Drying the Sample.................................................................................................. 16
3.1.4 Pretreatment for Removing IC ............................................................................... 17
3.1.5 Loading the Sample Boat ....................................................................................... 18
3.1.5.1 Solid Samples .............................................................................................. 18
3.1.5.2 Liquid Samples ............................................................................................ 18
3.1.5.3 Swab Samples .............................................................................................. 19
3.1.6 Sample Additives ................................................................................................... 20
SSM-5000A xiii
Table of Contents
3.1.7 IC Reaction Acid .................................................................................................... 20
3.1.8 Standards ................................................................................................................ 21
3.1.9 Calibration Curve ................................................................................................... 22
3.1.10 Changing TC Combustion Temperature ................................................................ 23
3.1.11 Relationship Between Carbon Content and Peak Height ....................................... 25
3.2 Start Up........................................................................................................................... 26
3.2.1 Turning on the Power ............................................................................................. 26
3.2.2 Carrier Gas Pressure ............................................................................................... 26
3.2.3 Setting the Carrier Gas Flow Rate.......................................................................... 28
3.3 Measurements Using the TOC-LCSH/CSN ...................................................................... 29
3.3.1 Analysis Parameters ............................................................................................... 29
3.3.1.1 Setting Up the SSM...................................................................................... 29
3.3.1.2 Turning on the SSM Electric Furnace.......................................................... 30
3.3.1.3 Setting the SSM Cell Length........................................................................ 31
3.3.1.4 Setting the Unit of Concentration ................................................................ 31
3.3.2 Calibration Curve Measurement............................................................................. 34
3.3.2.1 Creating Calibration Curves......................................................................... 34
3.3.2.2 Changing Calibration Curve Parameters...................................................... 42
3.3.3 Sample Measurement ............................................................................................. 43
3.3.3.1 Measurement Procedure............................................................................... 44
3.3.4 Stopping Measurement........................................................................................... 51
3.3.5 Deleting Data.......................................................................................................... 52
3.3.6 Ending Measurement.............................................................................................. 53
3.3.7 Referencing Data .................................................................................................... 56
3.3.7.1 Calibration Curve List.................................................................................. 56
3.3.7.2 Data Reports................................................................................................. 62
3.3.8 Screen Displays ...................................................................................................... 63
3.3.8.1 Background Monitor .................................................................................... 63
3.3.8.2 Conditions .................................................................................................... 64
3.3.8.3 "Data Report - Measurement Log" .............................................................. 66
3.3.8.4 "Data Report - Calibration Curves" ............................................................. 67
3.3.8.5 "SSM Calibration - Settings" ....................................................................... 70
3.3.8.6 "SSM Calibration" ....................................................................................... 71
3.3.8.7 "SSM Measurement Settings"...................................................................... 73
3.3.8.8 "SSM Measurement".................................................................................... 74
3.4 Measurement Using the TOC-LCPH/CPN ........................................................................ 76
3.4.1 Instrument Setup Wizard........................................................................................ 76
3.4.1.1 New Instrument Setup.................................................................................. 76
3.4.1.2 Edit the Instrument Setup............................................................................. 78
3.4.2 New Sample Table ................................................................................................. 80
3.4.3 Calibration Curve File ............................................................................................ 83
3.4.4 Method File ............................................................................................................ 87
xiv SSM-5000A
Table of Contents
3.4.5 Control Sample File ............................................................................................... 90
3.4.6 Schedule File.......................................................................................................... 96
3.4.7 Measurement .......................................................................................................... 97
3.4.7.1 Sample Table Preparation............................................................................ 97
3.4.7.2 Connecting to the Instrument....................................................................... 97
3.4.7.3 Starting Measurement .................................................................................. 98
3.4.8 Ending Measurement ............................................................................................. 101
3.4.8.1 Shutdown ..................................................................................................... 102
3.4.8.2 Sleep............................................................................................................. 103
3.4.9 Screen Descriptions................................................................................................ 104
3.4.9.1 Measurement Properties Windows .............................................................. 104
3.4.9.2 Monitor Window.......................................................................................... 116
3.4.9.3 Mechanical Check Window......................................................................... 117
3.4.9.4 Default Measurement Parameters................................................................ 118
3.4.10 Instrument Validation............................................................................................. 119
3.5 Measurement Using the Cell Switching Valve Set (Option) ......................................... 121
3.5.1 High Sensitivity Measurement Using the Cell Switching Valve Set..................... 121
3.5.2 Cell Switching Valve Configuration...................................................................... 122
SSM-5000A xv
Table of Contents
5.5.2.1 Selecting an Installation Site........................................................................ 143
5.5.2.2 Site Conditions ............................................................................................. 144
5.5.3 Electrical Connections............................................................................................ 144
5.5.4 Changing the Power Source Voltage...................................................................... 145
5.5.5 Power Supply and Ground Connection .................................................................. 146
5.5.6 Connecting the Gas Tubing .................................................................................... 147
5.5.6.1 Carrier Gas ................................................................................................... 147
5.5.6.2 Gas Connections........................................................................................... 147
5.5.7 Gas Connections to Cells........................................................................................ 148
5.5.8 Installing the TC Combustion Tube and IC Reaction Tube ................................... 150
5.5.8.1 Filling the TC Combustion Tube with Catalyst ........................................... 150
5.5.8.2 Installing the TC Combustion Tube and IC Reaction Tube......................... 152
5.5.9 Connecting the IC Reaction Acid Dispenser.......................................................... 155
5.5.10 Drain Tubing .......................................................................................................... 156
5.5.11 Supplying Water to the Drain Vessel ..................................................................... 156
xvi SSM-5000A
1
11 Overview
This chapter gives an overview of the instrument and describes the operational
precautions for safe instrument use.
1.1 Overview
This section provides an overview of the instrument.
1.1 Overview
The SSM-5000A is a special accessory for the TOC-L series Total Organic Carbon
Analyzer which combines with the TOC-L to create a TOC Solid Sample Analysis
System capable of analyzing solid samples, such as soil.
This manual describes the operation of the SSM-5000A Solid Sample Module alone
and also the operation of the TOC-L with the SSM-5000A attached. For other
procedures related to the TOC-L, refer to the appropriate USER'S MANUAL.
To ensure that the SSM-5000A is used correctly, be sure to read this USER'S
MANUAL before using the SSM-5000A. The manual should be conveniently stored
for future reference.
CAUTION
Safety may be compromised if the instrument is used in a fashion other than
indicated in this USER'S MANUAL. Pay particular attention to the
CAUTION sections to ensure safe operation of the instrument.
2 SSM-5000A
1.2 Operational Precautions
CAUTION
• When the electric furnace is heating or when it has reached operating
temperature, the internal parts are at high temperature. Due to risk of burn injury,
be sure to wait until the furnace oven cools to room temperature before opening
the cover to perform maintenance related to the combustion tube or catalyst.
• The SSM-5000A is capable of measuring solids, suspensions, and solutions. The
solid sample can have many attributes that affect the result, such as shape,
matrix, and water content. The efficiency of the carbon combustion oxidation
reaction (TC analysis) and carbonate acidification reaction (IC analysis) may
vary with the sample type. The TC or IC recovery rate of some samples may be
low. IC analysis of some samples may be difficult due to insufficient mixing with
the phosphoric acid added for acidification, or because of solidification due to a
reaction with the phosphoric acid. Determine the optimal parameters before
starting sample analysis. Particle size, dryness, sample weight, carrier gas flow
rate, whether the sample boat is covered, selection of additives, and types of
standards used for calibration are examples of the parameters that need to be
predetermined.
• If a sample contains highly volatile TOC components, before measuring place
the sample boat in the sample port then cover it immediately. This precaution
may not entirely prevent a low bias due to loss of volatile components during
sampling, weighing, or analysis.
• Never analyze explosive samples. Explosions could injure people nearby and
damage the instrument.
• Never analyze samples that emit toxic substances during combustion, such as
samples containing mercury or arsenic.
• Do not directly analyze seawater or water with a salt content equivalent to
seawater. Dilute these samples to lower the salt concentration before analysis. If
analyzed directly, substances emitted during TC combustion or IC reaction may
hinder the analysis or damage the interior of the detector.
• When using the TOC Solid Sample Analysis System, carrier gas must flow
through both the 200mm and 1.0mm cells of the tandem NDIR. Even when a
liquid sample is analyzed using the TOC-L only, the SSM-5000A carrier gas
must flow through the 1.0mm cell as purge gas. To minimize the SSM-5000A
carrier gas consumption, the gas flow rate may be decreased to 20mL/min. When
using the SSM-5000A, the carrier gas flow rate on the TOC-L side automatically
decreases to 20mL/min.
SSM-5000A 3
1.2 Operational Precautions
• Since the gas flow lines of the TC and IC sample ports are connected in series,
ensure that both ports are fully closed during analysis. However, always open the
IC sample port cover (raising it a few millimeters is sufficient) when performing
high sensitivity measurement using the optional cell switching valve set (see the
chapter that explains the cell switching valve set) to prevent water in the drain
pot from being sucked up into the drain separator as the IC furnace heats up or
cools down.
• Clean the instrument with a damp cloth; do not use chemicals.
• Keep samples and chemicals away from the PC and printer.
• Avoid injury by contacting your Shimadzu representative to perform any repairs
to the interior of the instrument.
• Never disassemble or modify the instrument beyond the range of maintenance
described in the Instruction Manual. Safety may be compromised.
• This instrument does not have a flameproof construction. Do not use it in a
dangerous area.
• Utilize a 100 to 115VAC power supply (100V series) or a 220 to 240VAC power
supply (200V series).
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.
Note: Cobalt oxide may occur after using this product. Handle with care.
To dispose of it, ask an industrial waste disposer in compliance with the local
laws and regulations.
4 SSM-5000A
2
22 System Components
This chapter describes the names and major functions of the various components of the
SSM-5000A.
6 SSM-5000A
2.2 Top View
SSM-5000A 7
2.3 Right View
8 SSM-5000A
2.4 Rear View
SSM-5000A 9
2.5 Flow Diagram
10 SSM-5000A
2.5 Flow Diagram
Diluent
IC Reaction
Backflow Vessel
IC Reagent
Prevention Trap Supply Pump
Acid
Solenoid
ASI Valve 3 Light
(To Drain) Source
Sample
Backflow IC Reagent Phosphoric
Prevention Sliding TC Acid
Valve Sample Injector
NDIR Tandem
Cell (Sample
CO2 Absorber
Cell)
Halogen Scrubber
5 mL Syringe
Detector
Dehumidifier Membrane Filter
(Electronic Cooler)
TC Combustion
Pressure Sensor PS3 Tube
Regulator
Carrier Gas
Inlet
Gas Outlet
Pressure
Gauge
High Purity Air Oxygen
Pressure
Adjustment Mass Flow
Valve Controller
Sample Boat
Sample Poat Cover TC Combustion Tube
TC Furnace (900 C) Flow Meter
Sample Boat
Push Rod
Cooling Coil on
Condensation Coil the Rear Panel
Drain Separator
Oxidation
Catalyst
Acid
Dispenser
IC Reaction Tube
IC Furnace (250 C)
Drain Pot
Drain Tubing
SSM-5000A 11
2.5 Flow Diagram
2.5.3 Flow Diagram for TOC-L + SSM-5000A + Cell Switching Valve Set
Substitute the TOC-LCSH/CPH section of this flow diagram with the TOC-LCSN/CPN (refer
to the TOC-L USER'S MANUAL) when the TOC-LCSN/CPN is connected to the
SSM-5000A.
Diluent IC Reaction
Backflow Vessel
Acid
4 5 IC Reagent
3 Drain Prevention Trap Supply Pump
6 Light Source Sub-trap
2 P
ASI 7
1 8 Solenoid
Sample Backflow Sliding TC Valve 3 NDIR Tandem Cell
Prevention Sample (To Drain) (Sample Cell)
Valve Injector Mist Trap
Phosphoric
IC Reagent
Acid
Detector CO2 Absorber
Halogen Scrubber
5 mL Syringe Drain
Container
Dehumidifier Membrane
(Electronic Filter
Pure Water Trap Cooler)
Pressure
Adjustment Mass Flow
Sample Boat Valve Controller
Pressure Dryer
TC Reaction Tube Gauge
M M
Drain Separator
Acid
Dispenser Flow Meter
Delay Tubing
IC Furnace (250 C)
SSM-5000A
Figure 2.7 • Flow Diagram for TOC-LCSH/CPH + SSM-5000A + Cell Switching Valve Set
12 SSM-5000A
3
33 Operation
This chapter describes the analysis preparations, parameter entry procedures and
operation procedures for calibration curve generation and sample analysis.
3.2 Start Up
This section describes the procedure for starting up the instrument.
Preparation
Heat the sample boats in a furnace to oxidize any carbon content. Use an electric
furnace of the type normally used in a laboratory.
Note: Tweezers are supplied to handle sample boats. Heat the tip of the tweezers
that contacts the sample boat to red hot in the furnace or with gas burner to
oxidize any attached carbon.
1. Cut off a suitable amount of ceramic fiber for a single analysis (approx. 40 to
60mg).
2. Shape the ceramic fiber to about 35mm long x 10mm wide.
3. Heat the ceramic fiber, as described for the sample boat.
4. Use the heat-treated tweezers to insert the heat-treated ceramic fiber into a
clean container or case for storage.
14 SSM-5000A
3.1 Analysis Preparations
Note: The stand used to hold sample boats during analysis should be
made of an inorganic material, such as ceramic, glass, or metal,
with a surface free from contamination.
Handling
Using a new sample boat for each sample is recommended. However, a sample boat
may be reused if the sample analyzed does not contaminate, modify, or degrade the
sample boat material. Do not reuse the quartz-glass filter paper.
1. Remove as much of the sample remaining in the used sample boat as possible.
Use a brush or the tip of a scraper to scrape off pieces adhering to the bottom of
the sample boat.
2. Soak the boat in approximately 2M sulfuric acid or hydrochloric acid for about
10 minutes.
3. Wash under running tap water for several minutes.
4. Rinse the tap water off the boat with de-ionized or distilled water. Dry the boat.
5. Bake the dried sample boat in a furnace at approximately 900°C for 20
minutes.
Note: • Evaluate whether a sample boat can be reused by running a blank test
(an analysis with no sample in the boat) to determine the amount of
residual carbon.
• For some samples, it may not be possible to reuse the sample boat
even after performing the above treatment procedure. In these cases,
use a more appropriate method to remove the residual material from
the sample boat or use a new sample boat.
Ceramic Fiber
Ceramic fiber can be reused in cases where a pure product, such as glucose, is
measured as the standard.
Although ceramic fiber can be treated according to the above method to remove any
contamination, the use of new ceramic fiber is recommended because it is relatively
inexpensive.
SSM-5000A 15
3.1 Analysis Preparations
Sampling Technique
1. Remove any foreign matter that is not the subject of the analysis from the
sample material.
2. Select portions of the sample from several locations. Thoroughly pulverize and
mix these portions in a pulverizer or mortar.
3. After pulverizing the sample, pass it through a sieve with a suitable mesh size.
4. Repeatedly pulverize any pieces that do not pass through the sieve. Reduce the
sample using conical quartering or a riffle sampler.
5. Repeat steps 3 and 4 to obtain a final sample that will pass through a 200-mesh
sieve.
TIP » The combustion-oxidation reaction (TC analysis) and the carbonate acidification
reaction (IC analysis) are more efficient when the sample particles are smaller in size.
Note: Volatile organic components contained in a sample may be lost during drying.
16 SSM-5000A
3.1 Analysis Preparations
Note: Use a volatile acid, such as hydrochloric acid, for pretreatment. Non-volatile
acid may remain in the sample and hinder TC analysis or damage the
detector. Include a step to remove the excess hydrochloric acid at the end of
the pretreatment.
SSM-5000A 17
3.1 Analysis Preparations
Loading Procedure
1. Weigh the sample.
Note: • Reduce the effects of poor distribution, which commonly occur with
solid samples.
• Reduce the weighing error.
• Reduce the impact of external contamination, by choosing a sample
amount that will produce a result close to the upper limit of the
instrument (about 30mg C).
IC Analysis of Carbonates
Adding phosphoric acid to a carbonate during IC analysis will cause a violent reaction
that may allow part of the sample to scatter outside the sample boat. Pre-moisten this type
of sample with a small amount of water.
The following two sampling methods are available for liquid samples:
1) Weighing the sample with a balance
2) Measuring the volume of the sample with a microsyringe or pipette
18 SSM-5000A
3.1 Analysis Preparations
Note: The maximum measurable mass of a liquid sample is 0.5g for TC and 0.3g
for IC.
For TC analysis of a liquid sample, the sample can be impregnated into ceramic fiber
placed on the bottom of the sample boat. Ceramic fiber is not used for IC analyses.
Pipette, Microsyringe, etc.
Solid Sample
Water Sample
Sampling methods for cleaning validation differs depending on the equipment being
swab tested. Use the optimal method for the type of equipment being tested.
Sampling Method
TOC Measurement
SSM-5000A 19
3.1 Analysis Preparations
Note: To ensure that all of the CO2 generated will be carried by the carrier gas, the
total volume of dilute phosphoric acid and sample must not exceed 0.5mL.
Reference: See Section "3.1.4 Pretreatment for Removing IC" on page 17.
CAUTION
Phosphoric acid is highly corrosive. Use care to avoid touching or spilling it
during handling. See the "Material Safety Data Sheet (SDS)" section in the
TOC-L USER'S MANUAL for details.
20 SSM-5000A
3.1 Analysis Preparations
3.1.8 Standards
The SSM-5000A uses different types of standards depending on the sample type. Some
of the typical standards are listed below.
1) Government standards that are available from various associations or
councils, such as the Marine Sediment Reference Materials available from
the National Research Council of Canada.
2) Reagents with known compositions and purity, such as glucose and
acetanilide for TC analysis, and sodium carbonate and calcium carbonate for
IC analysis.
3) Standard solutions obtained by adjusting the reagents in item 2 to desired
concentrations.
4) Synthetic standards that are prepared by adding the reagents in item 2 or
standard solutions in item 3 to actual samples with a known carbon content
or with the carbon removed.
The standards used in preparing calibration curves should ideally be of the same type as
the sample. If a standard substance described in item 1 is suitable, it should be used. If
the carbon content in a sample is known, a pure reagent as in item 2 may be used. A
variety of organic reagents are also available commercially for organic element
analysis.
Note: Avoid using organic reagents that cause violent combustion. These reagents
tend to scatter the sample and increase the likelihood of incomplete
combustion.
When samples contain alkaline earths or metals, residual material in the sample boat
after combustion will make reusing the sample boat or ceramic fiber difficult without
treatment. The potassium hydrogen phthalate used as a TOC-L standard solution
contains potassium, which leaves a potassium residue in the bottom of the sample boat.
As a result, it would be easier to use glucose instead of potassium hydrogen phthalate
with the SSM-5000A.
SSM-5000A 21
3.1 Analysis Preparations
TC Measurement
It is possible to measure only the peaks related to the sample because the sample peak
appears after the blank peak is complete.
1. Allow carrier gas to flow at a rate of 500mL/min for 1.5 to 2 minutes after
closing the sample port cover.
Note: If the sample contains volatile organic matter, heat from the TC
furnace on the sample boat may cause the organic matter to
evaporate into the carrier gas.
Note: In some cases, the TOC-L Ready lamp may go out 60 to 90 seconds after
closing the sample port cover. This occurs because the blank peak is
evaluated as a baseline disturbance. The Ready lamp illuminates again when
the blank peak ends about 2 minutes after closing the sample port cover. After
the Ready lamp has illuminated again, insert the sample boat into the furnace
and start measurement.
22 SSM-5000A
3.1 Analysis Preparations
IC Analysis
Immediately after the acid is injected into the sample, CO2 is generated from the
reaction with IC in the sample, thereby reducing measurement accuracy.
1. Allow carrier gas to flow at a rate of 500mL/min for 1.5 to 2 minutes after
closing the sample port cover.
2. Inject the acid and immediately insert the sample into the furnace. Start
measurement.
Note: In some cases, the TOC-L Ready lamp may go out 60 to 90 seconds after
closing the sample port cover. This occurs because the blank peak is
evaluated as a baseline disturbance. The Ready lamp illuminates again when
the blank peak ends about 2 minutes after closing the sample port cover. After
the Ready lamp has illuminated again, insert the sample boat into the furnace
and start measurement.
CAUTION
Verify that the TC and IC furnaces have cooled to room temperature before
removing the rear cover to change the temperature setting.
SSM-5000A 23
3.1 Analysis Preparations
1. Remove the rear cover of the SSM-5000A while the TC furnace and IC furnace
are cold.
Note: Two temperature controllers are located on the right side of the
SSM-5000A. The left temperature controller regulates the TC
furnace and the controller on the right regulates the IC furnace.
The procedure below applies to the TC temperature controller
(left).
Reference: See Section "5.5.8.2 Installing the TC Combustion Tube and IC Reaction Tube" on page
152.
5. Press switch until both the "SP" and "AL" indicators are no longer
illuminated and the LED displays the actual furnace temperature.
6. Return the PROTECTION switch to the up position.
7. Replace the SSM-5000A rear cover.
LED Display
"SP"/"AL"
Indicators
PROTECT
Switch
24 SSM-5000A
3.1 Analysis Preparations
Note: The relationship below was obtained from the measurement of glucose. The
relationship may vary depending on the physical and chemical states of the
sample.
SSM-5000A 25
3.2 Start Up
3.2 Start Up
Turn on the power to the TOC-L and SSM-5000A before starting measurement.
1. On the TOC-L, turn on the main power switch on the left side towards the top left
of the instrument.
2. Turn on the power switch on the left side of the SSM-5000A.
1. Set the SSM-5000A carrier gas supply pressure to 200 to 300kPa (44PSI).
26 SSM-5000A
3.2 Start Up
2. Open the flow controller on the SSM-5000A and adjust the carrier gas pressure
to 200 kPa (29PSI) using the carrier gas adjustment knob.
Regulator Valve
Note: The SSM-5000A carrier gas supply pressure must be set to 200
to 300kPa (44PSI).
SSM-5000A 27
3.2 Start Up
Note: Tandem NDIR cells are used for SSM-5000A measurements and carrier gas
must flow to both of these cells. Carrier gas must always be supplied to both
the TOC-L and the SSM-5000A. The flow rate of carrier gas for the unused
cell can be decreased below the prescribed value in order to reduce gas
consumption.
Regulator Valve
Note: Do not change the carrier gas flow rate during analysis. The
peak area changes in an inversely proportional relationship to
the carrier gas flow rate and changing the flow rate may cause
measurement errors.
28 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
This section describes the procedures used to perform measurements with the
SSM-5000A when it is connected to the TOC-LCSH/CSN.
2. Press the arrow keys to move the cursor to the SSM - SSM Measurement item.
3. Turn SSM Measurement ON or OFF.
SSM-5000A 29
3.3 Measurements Using the TOC-LCSH/CSN
This section describes how to turn on the power to the SSM electric furnace.
Turn on the TC furnace for TC measurement or the IC furnace for IC measurement.
TIP » It is possible to turn the TC and IC Furnaces ON even when the SSM measurement item
is set to OFF.
The SSM Measurement item must be set to OFF to analyze samples using the TOC-L.
Procedure
2. Press the arrow keys to move the cursor to the appropriate item.
• SSM-TC Furnace item for TC analysis
• SSM-IC Furnace item for IC analysis
3. Turn the electric furnace ON or OFF.
Note: It takes 40 to 50 minutes for the furnace temperature to stabilize after the
furnace power is turned on. Follow the procedures in Section "3.3.6 Ending
Measurement" on page 53 to turn the power off.
30 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
This section describes how to select which NDIR detector cell will be used for
measurement.
The SSM cell length can be set to "Short" or "Long". "Short" is the default setting for
SSM cell length.
Note: Set the SSM cell length to "Long" when using the long cell to perform
measurement with the cell switching valve set (option).
Procedure
2. Press the arrow keys to move the cursor to the SSM Cell Length item.
3. Press the [Enter] key to select "Short".
4. Press the F1 [Return] key.
The display returns to the "Initial Display".
This section describes how to set the unit of concentration for sample measurement.
The concentration units are set independently for the standards used to create
calibration curves and for sample measurements.
Procedure
SSM-5000A 31
3.3 Measurements Using the TOC-LCSH/CSN
3. Press the arrow keys to move the cursor to the appropriate item:
• Output-Unit-Solid Smpl (Cal) item to set the concentration units for creating
calibration curves
• Output-Unit-Solid Sample item to set the concentration units for sample
analysis
4. Press the [Enter] key to display the concentration units.
TIP » Press the [Enter] key to interrupt the settings and return to step 3.
32 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
5. Press the keys to select the required units from the following options.
Options for Output-Unit-Solid Smpl (Cal):
• g/L
• mg/L
• µg/L
• ppm
• ppb
• %
Options for Output-Unit-Solid Sample:
• g/L
• mg/L
• µg/L
• ppm
• ppb
• %
• g
• mg
• µg
6. Press the [Enter] key to enter the selected units.
7. Press the F1 [Return] key.
The display returns to the "Initial Display".
SSM-5000A 33
3.3 Measurements Using the TOC-LCSH/CSN
The method for creating calibration curves can be broken down into the following five
steps:
Step 1 Set the Measurement Mode
Step 2 Set the Calibration Curve Measurement Parameters
Step 3 Load the Standard
Step 4 Press the [Start] Key
Step 5 End Measurement
34 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Procedure
1. Press F2 [SSM-TC].
The parameter box for TC analysis is displayed as the default. The currently
saved calibration curves are displayed at the top of the screen.
TIP » Press the F1 [Return to Settings] key to return to the "Setting" screen to repeat entry of
the calibration curve parameters. Press the [Cal] key to quit without making the
calibration curve measurements. Then press the F6 [Yes] key to quit and return to the
"Initial Display" or the F1 [No] key to cancel the quit command.
SSM-5000A 35
3.3 Measurements Using the TOC-LCSH/CSN
(3) Density
Density is entered for liquid standards that do not have mg/mL designated as the
concentration unit.
TIP » See Section "3.3.1.4 Setting the Unit of Concentration" on page 31.
36 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
(4) Concentration
1. Press the key to move the cursor to the Concentration (Conc) item.
Reference: See Section "3.3.1.4 Setting the Unit of Concentration" on page 31.
(5) Amount
SSM-5000A 37
3.3 Measurements Using the TOC-LCSH/CSN
3. Set the parameters for the second point in the same way as parameters for the
first point were set.
4. Repeat steps 2 and 3 to set the parameters for the third and subsequent points in
the calibration curve.
Note: If the F6 [Delete Point] key is pressed while the parameter box
for the first point (point 1) is selected by the cursor, this
parameter box is not deleted but the display reverts to the default
display.
TIP » Press the F1 [Return to Settings] key to return to the "Setting" screen to repeat entry of
the calibration curve parameters. Press the [Cal] key to quit without making the
calibration curve measurements. Then press the F6 [Yes] key to quit and return to the
"Initial Display" or the F1 [No] key to cancel the quit command.
38 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Procedure
• If the standard is a solid, a dialog box prompts the operator to enter the weight
of the standard in mg.
• If the standard is a liquid, a dialog box prompts the operator to enter the
volume of the standard in µL.
2. Weigh the standard into the sample boat.
Enter the amount of the standard in the sample boat and press the [Enter] key.
3. Press the [Enter] key again.
A dialog box instructs the operator to load the *** mg/L Standard Set Sample
and press the START button.
*** Represents the standard concentration entered in the "SSM Calibration Settings"
screen.
TIP » Press the F1 [Return to Settings] key to return to the "Setting" screen to repeat entry of
the calibration curve parameters. Press the [Cal] key to quit without making the
calibration curve measurements. Then press the F6 [Yes] key to quit and return to the
"Initial Display" or the F1 [No] key to cancel the quit command.
SSM-5000A 39
3.3 Measurements Using the TOC-LCSH/CSN
Reference: The parameters used to create the calibration curve can be changed on the "SSM
Calibration" screen during the calibration curve measurement or on the "SSM Calibration
Setting" screen after calibration curve measurement is complete. See Section "3.3.2.2
Changing Calibration Curve Parameters" on page 42.
Procedure
1. Verify that the Ready lamp is illuminated and the [Start] key is flashing.
2. Press the [Start] key.
A dialog box prompts the operator to move the standard to the MEASURING
position.
The graph scale (vertical axis) is automatically displayed. The range can be changed
between 10 and 1000mV with the F3 [Zoom In] and F4 [Zoom Out] keys. The scale
changes by 10mV each time the F3 and F4 key is pressed in the 10-100mV range and
by 100mV each time the key is pressed in the 100-1000mV range.
40 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
2. Return the sample boat push rod knob to the SAMPLE CHANGE position.
3. Proceed to the next step.
• Press the F1 [Add Injection] key for additional measurements of the same
standard. Steps 3 "Load the Standard" and 4 "Press the [Start] Key" are
repeated.
• Press the F2 [Remeasure Point] key to delete the data and repeat the
measurement. Then press the F6 [Yes] key to repeat steps 3 "Load the
Standard" and 4 "Press the [Start] Key".
• Operation proceeds to step 5 "End Measurement" when measurement is
complete.
• Press the F6 [Go to Next Cal. Point] key to proceed to the measurement of the
next concentration (for multi-point calibration curve). Steps 3 "Load the
Standard" and 4 "Press the [Start] Key" are repeated.
Reference: See Section "3.3.5 Deleting Data" on page 52 before deleting any measured data.
Procedure
SSM-5000A 41
3.3 Measurements Using the TOC-LCSH/CSN
The following three calibration curve parameters can be changed during or after
calibration curve measurement:
(1) Protection
Select whether the stored calibration curve data is protected. Protected calibration
curve data cannot be deleted.
(2) Curve Type
Select whether calibration curves with 3 or more points are created using
regression lines by the method of least squares (Least Squares) or using the
polygonal method linking consecutive points with straight lines (Pt to Pt).
(3) Curve Shift
Select whether the calibration curve is parallel shifted to pass through the origin.
Procedure
• Protection: OFF
• Curve Type: Least Squares
• Curve Shift: none
42 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
TIP » Press the [Measure Sample] key to interrupt the settings and return to the "Initial
Display" screen.
SSM-5000A 43
3.3 Measurements Using the TOC-LCSH/CSN
The method for measuring samples can be divided into the following five steps:
Step 1 Set the Measurement Mode
Step 2 Set the Measurement Parameters
Step 3 Load the Sample
Step 4 Press the [Start] Key
Step 5 End Measurement
Procedure
TIP » Press the function key corresponding to the measurement mode to hide the parameter
box for that measurement mode.
44 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
SSM-5000A 45
3.3 Measurements Using the TOC-LCSH/CSN
1. Press the key to move the cursor to the Calibration Curve (Calib.) item.
A list of TC analysis calibration curves is displayed at the top of the screen.
2. Select the calibration curve to be used by one of the following two methods:
• Select it from the "SSM Measurement Settings" screen.
• Select it from the calibration curve display.
46 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
2. Press the keys to select the calibration curve from the list at the top of the
screen.
3. Press the F6 [Select] key.
The display reverts to the "SSM Measurement Settings" screen. The
concentration and injection amount that correspond to the selected calibration
curve are displayed.
Note: • For single mode measurement: Proceed to step 3 "Load the Sample".
• For multiple mode measurement: Repeat the procedure from step 1
"Set the Measurement Mode".
Procedure
1. Press the [Next] key.
SSM-5000A 47
3.3 Measurements Using the TOC-LCSH/CSN
• If the sample is a solid, a dialog box prompts the operator to enter the weight of
the sample in mg.
• If the sample is a liquid, a dialog box prompts the operator to enter the volume
of the sample in µL.
2. Measure the sample into the sample boat.
Enter the amount of the sample in the sample boat and press the [Enter] key.
3. Press the [Enter] key again.
A dialog box instructs the operator to load the sample and press the [Start]
button.
4. Open the sample port cover.
5. Place the sample boat (with sample) on the sample boat holder.
6. Close the sample port cover completely.
When the instrument is in standby, the Ready lamp is illuminated and the
[Start] key flashes.
TIP » Press the F1 [Return] key to return to the "Setting" screen to repeat the sample
measurement settings. Press the [Measure Sample] key to quit without making the
sample measurement and return to the "Initial Display".
48 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Procedure
1. Verify that the Ready lamp is illuminated and the [Start] key is flashing.
2. Press the [Start] key.
A dialog box prompts the operator to move the sample to the MEASURING
position.
The graph scale (vertical axis) is automatically displayed. The range can be changed
between 10 and 1000mV with the F3 [Zoom In] and F4 [Zoom Out] keys. The scale
changes by 10mV each time the F3 and F4 key is pressed in the 10-100mV range and
by 100mV each time the key is pressed in the 100-1000mV range.
SSM-5000A 49
3.3 Measurements Using the TOC-LCSH/CSN
2. Return the sample boat push rod knob to the SAMPLE CHANGE position.
3. Proceed to the next step.
• Press the F1 [Add Injection] key for additional measurements of the same
sample. Steps 3 "Load the Sample" and 4 "Press the [Start] Key" are repeated.
• Operation proceeds to step 5 "End Measurement" when measurement is
complete.
• Press the F6 [Next Measurement] key to proceed to the measurement of the
next mode (for multiple mode measurement). Steps 3 "Load the Sample" and 4
"Press the [Start] Key" are repeated.
Procedure
1. Press the F6 [Exit] key to return to the "Initial Display" and save the
measurement results in the data report.
50 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Procedure
4. Return the sample boat push rod knob to the SAMPLE CHANGE position.
A dialog box is displayed verifying whether to end measurement.
5. Press the F6 [Exit Measurement] key.
The display returns to the "Initial Display".
SSM-5000A 51
3.3 Measurements Using the TOC-LCSH/CSN
Note: Data cannot be deleted after measurements are complete and the "Measuring"
screen has been closed.
Deleting Data
1. Verify that measurements are complete and the measurement results are
displayed in the list at the right of the screen.
2. Press the keys to select the data to be deleted.
3. Press the [CE] key.
The data is deleted. "Exc" is displayed before "Inj#". The mean area, SD, and
CV% values show at the top of the screen are updated.
52 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Procedure
1. Press the F1 [Standby Option] key in the "Initial Display".
The "Standby Option - Sleep" screen is displayed.
SSM-5000A 53
3.3 Measurements Using the TOC-LCSH/CSN
TIP » Press the F1 [Cancel] key to cancel turning off the power and return to the "Initial
Display".
54 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Sleep
Set the time and date for the next measurement session. The TOC-L stays in an inactive
state until then.
About 1 hour before the preset date and time, the TOC-L prepares for measurement.
The power is turned on, the carrier gas flow is started and the electric furnace
temperature rises.
The furnace power and carrier gas can be turned off during the inactive period.
Power to the SSM-5000A electric furnaces are controlled by the TOC-L. The carrier
gas for the SSM-5000A is turned ON and OFF manually. If the SSM-5000A is going to
be turned ON automatically by the Sleep function, the carrier gas flow rate to the
SSM-5000A must remain ON during the inactive period.
Procedure
2. Enter the desired date and time of the next instrument startup.
TIP » The date and time can be set between the present and December 31, 2099. Press the
key to move the cursor to the right and the key to move the cursor to the left. The
cursor moves in the sequence: month, day, year, hour, minute. Press the [Enter] key to
confirm each numerical value.
3. Press the key to move the cursor to the unit to be set, then press the [Enter]
key to toggle the setting ON or OFF.
Note: • The term "Furnace" refers to the SSM-TC furnace, SSM-IC furnace,
and TOC-L furnace.
• The carrier gas ON/OFF setting affects only the TOC-L carrier gas
setting. Turn the SSM-5000A carrier gas ON and OFF manually.
TIP » Press the F1 [Return] key to cancel turning off the power.
SSM-5000A 55
3.3 Measurements Using the TOC-LCSH/CSN
Procedure
56 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Note: Press the F3 [IC] key to list the IC analysis calibration curves.
Procedure
1. Press the F6 [Data Report] key in the "Initial Display".
The "Data Report - Measurement Log" screen is displayed.
SSM-5000A 57
3.3 Measurements Using the TOC-LCSH/CSN
Note: Press the F3 [IC] key to list the IC analysis calibration curves.
58 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Procedure
SSM-5000A 59
3.3 Measurements Using the TOC-LCSH/CSN
Note: Press the F3 [IC] key to list the IC analysis calibration curves.
60 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
SSM-5000A 61
3.3 Measurements Using the TOC-LCSH/CSN
Referencing Data
Deleting Data
1. Specify and highlight the data for deletion using the up and down arrow keys
( ) and then press the [Enter] key to select the data. Alternatively, press the
F5 [All Select/All Clear] key to select all the data on the currently displayed
page. Note that the selection can be cleared by pressing the F5 [All Select/All
Clear] key when all the displayed data is selected. Data selection can be
performed across multiple pages.
2. Press the F4 [All Select/All Clear] key.
The message "YES to delete?" is displayed.
62 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Press the F3 key in the "Initial Display" to display the "Background Monitor" screen.
3
4
5
6
2
9
10
SSM-5000A 63
3.3 Measurements Using the TOC-LCSH/CSN
Function Keys
Key Function
F1 [Return] Returns to the "Initial Display".
F3 [Zoom In] Enlarges the baseline full scale to 20mV.
3.3.8.2 Conditions
This section describes only the items related to the SSM-5000A on the "Conditions"
screen.
The "Conditions" screen comprises two screens: "Unit Management" and
"Measurement Conditions (Meas. Cond.)".
Item Description
SSM Measurement Turns SSM-5000A measurement ON or OFF.
SSM-TC Furnace Turns the SSM-5000A TC furnace ON or OFF.
SSM-IC Furnace Turns the SSM-5000A IC furnace ON or OFF.
Cell Length Set to "Long" or "Short" to designate whether the long
or short tandem NDIR detector cell is used for
SSM-5000A measurements. The "Short" is the default
setting for the SSM-5000A.
64 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Item Description
Unit-Liquid Sample Set the unit to use when measuring liquid samples with the
SSM-5000A
Unit-Solid Smpl (Cal) Set the unit to use when performing calibration curve measurement
using standard solid samples with the SSM-5000A
Unit-Solid Sample Set the unit to use when measuring solid samples with the
SSM-5000A
SSM-5000A 65
3.3 Measurements Using the TOC-LCSH/CSN
This section describes the "Data Report - Measurement Log" screen, which shows the
results history of previously conducted measurements. Each measurement type item is
displayed on a single line. Up to 200 measurement results can be saved. Up to 25
measurement results can be displayed on each page.
1 2 3 4 5 6 7 8 9
Item Description
(1) Sample Name Name of the measured sample.
(2) V# 0 is displayed for SSM measurements.
(3) Date & Time Date and time of the measurement.
(4) Type Measurement type.
(5) Conc. Concentration analysis value.
(6) SD SD of measurement results.
(7) CV% CV% of measurement results.
(8) TOC TOC concentration calculated as TOC = TC-IC. Displayed in the IC
position when TC and IC measurements are made.
(9) Page number Current page number is displayed before the slash (/) and the total
number of pages is displayed after the slash. To switch pages, move
the cursor to the bottom of the page and press the key or move the
cursor to the top of the page and press the key.
66 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Function Keys
Key Function
F1 [Return] Returns the display to the "Initial Display" screen.
F2 [Data Save] Outputs the selected data to a USB memory device.
F3 [Data Search] Opens the "Data Search" screen.
F4 [Clear Select] Deletes the selected data.
F5 [All Select/All Clear] Selects or deselects all of the displayed data.
F6 [Cal. Curves List] Opens the "Data Report - Calibration Curves" screen.
2 3 4 5 6
8
10
11
12
14 15 16 13
SSM-5000A 67
3.3 Measurements Using the TOC-LCSH/CSN
2 3 4 5 6
8
10
11
12
14 15 16 13
68 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Item Description
(9) Point display Displays the measurement results at each measurement
point on the selected calibration curve.
• #: The number of each calibration point.
• Conc.: The standard concentration at the point.
• Amount: The amount of the standard.
• µgC: Carbon amount determined from carbon
concentration and the weight or volume of the
standard.
• Area: Area value for the measurement result at each
point.
• #: Number of measurement repetitions.
2 Indicates the correlation coefficient (R2) of the selected
(10) R
calibration curve. Displayed for a least squares method
curve with at least three points.
(11) Cell Indicates the length of the NDIR detector cell that was
used.
(12) Density Indicates the density of the standard.
(13) Date Indicates the date of the last revision.
(14) Protect Indicates the protection status of the calibration curve:
• OFF: not protected
• ON: protected
(15) Curve Type Indicates the method by which the curve was created:
• Least squares: method of least squares
• Pt to Pt: polygonal method
(16) Shift Indicates whether the calibration curve is parallel shifted
to pass through the origin (0 concentration point):
• none: not shifted to origin
• Origin: shifted to origin
Function Keys
Reference mode
Key Function
F1 [Return] Returns to the "Data Report - Measurement Log" screen.
F2 [TC], F3 [IC] Switches the calibration curve measurement type.
F6 [Edit] Enables editing mode for the selected calibration curve.
Editing mode
Key Function
F1 [Cancel] Returns to the reference mode without making the
changes.
F2 [Protect ON/OFF] Use this to turn the protection function ON or OFF.
F3 [Cal. Curve Type] Use this to select least squares display or Pt to Pt.
F4 [Zero Shift Status] Select none or Origin.
F6 [OK] Returns to the reference mode after making the changes.
SSM-5000A 69
3.3 Measurements Using the TOC-LCSH/CSN
Press the [Cal] key in the "Initial Display" to display the "SSM Calibration - Settings"
screen.
1
2
4
3 5
6 8
7
9
10
Item Description
(1) Screen title "SSM Calibration - Settings".
(2) Calibration curve Displays information on previously set calibration
information curves for the selected measurement type.
• SSM-TC, SSM-IC: calibration curve type.
• #: calibration curve number.
• Concentration: Maximum concentration of the
standard used to create the calibration curve.
• Amount: Amount of the standard used to create the
calibration curve.
• Status: Status of the calibration curve.
"S": Calibration curve is being used for sample
measurement.
"P": Calibration curve is protected.
(3) Calib. # Calibration curve number (0 to 9). Enter a previously set
calibration curve number to display setting details for
that calibration curve.
(4) Amount Unit Select whether the standard amount is entered as a mass
or a volume.
(5) Cell Length Displays which NDIR detector cell type is used.
(6) Density Enter the density of a liquid standard.
(7) [***.***] Defines the setting range of the item currently selected
by the cursor.
70 SSM-5000A
3.3 Measurements Using the TOC-LCSH/CSN
Item Description
(8) POINT 1 to 10 Displays the point number. To add a calibration curve
point, move the cursor to the solid box below the point
number and press the right arrow key. To delete a
calibration curve point, move the cursor to the solid box
below the point number and press the F6 (Delete Point)
key.
(9) Conc. Enter the carbon concentration of the standard.
(10) Amount Enter the amount of the standard, as either a mass or
volume.
Function Keys
Key Function
F2 [SSM-TC] Selects the SSM-TC calibration curve type.
F3 [SSM-IC] Selects the SSM-IC calibration curve type.
F6 [Delete Point] Deletes the selected calibration point.
Other Keys
Key Function
[Cal] Returns to the "Initial Display".
[Next] Starts calibration curve measurement.
Press the [Next] key in the "SSM Calibration - Settings" screen to display the "SSM
Calibration" screen.
1
2
5
6
7
8 9 10
SSM-5000A 71
3.3 Measurements Using the TOC-LCSH/CSN
Item Description
(1) Screen title "SSM Calibration".
(2) Calib. # Number of the calibration curve.
(3) Conc, Mean Area, Displays the concentration and measurement results for
SD, CV% each point.
(4) Peak graph Displays a graph of the detector output during peak
detection.
(5) Cnv Area Area of nth measurement x (mass or volume of first
measured sample/mass or volume of nth measured sample).
SD and CV values in item are calculated using the
converted area.
(6) Remark The following remark symbols are displayed.
• "T": Detector output tailing.
• "H": Detector output out of range.
• "F": Electric furnace temperature out of range.
• "P": Incorrect sample boat position during
measurement.
• "B": Unstable baseline during measurement.
(7) Date & Time Displays the current date and time.
(8) Protect Indicates the protection status of the calibration curve.
• OFF: not protected.
• ON: protected.
(9) Curve Type Indicates the method by which the curve was created.
• Least squares: method of least squares.
• Pt to Pt: polygonal method.
(10) Shift Indicates whether the calibration curve is parallel shifted to
pass through the origin (0 concentration point).
• none: Not shifted to origin.
• Origin: Shifted to origin (standard concentration 0 =
area 0).
Function Keys
Key Function
F1 [Add Injection] Makes an additional measurement for the current point.
F2 [Remeasure Point] Repeats the measurement for the current point.
F3 [Zoom In] Enlarges the peak graph scale.
F4 [Zoom Out] Reduces the peak graph scale.
F5 [Browse Cal. Curves] Displays a graph of the carbon amount and area of the
calibration curve.
F6 [Exit Cal. Measurement] Ends calibration curve measurement.
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To start sample measurement, press the [Measure Sample] key in the "Initial Display".
The "SSM Measurement Settings" screen is displayed.
1 5
2 6
3
4
Item Description
(1) Sample Name Enter the sample name here.
(2) [***.***] Displays the setting range of the item currently selected
by the cursor.
(3) Calib. Enter the number of the calibration curve to use for the
measurement. Align the cursor with a measurement type
in the calibration curve box to display the available
calibration curves in the calibration curve list at the top
of the screen. Enter the number of the desired calibration
curve. The measurement range of each calibration curve
is displayed to the right of the calibration curve number.
Measurement is possible using a calibration curve in the
list for which measurements are incomplete (calibration
curve number is highlighted) but only the area result is
displayed; the concentration is output as zero. The F1
key is displayed as [Calibration Curve] when the cursor
is in the calibration curve box.
(4) Density Enter the density of a liquid sample.
(5) Cell Length Displays which NDIR detector cell type is used.
(6) Amount Unit Sets whether the sample amount is entered as a mass or a
volume. Press the [Select] key to toggle the setting.
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Function Keys
Key Function
F1 [Calibration Curve] Opens the "Calibration Curve" screen. Except for the
names of the function keys, this screen is identical to the
"Data Report - Calibration Curves" screen. Select a
calibration curve by pressing the cursor arrow keys to
display detailed information for that calibration curve.
Press the F6 [Select] function key in the "Calibration
Curve" screen to select that calibration curve and enter it
into the calibration curve box on the "SSM
Measurement Settings" screen. Press the F1 [Cancel]
key to return to the "SSM Measurement Settings" screen
without entering the calibration curve number.
F2 [SSM-TC], F3 [SSM-IC] Selects the measurement type. Press the function key for
the required measurement type to display the parameter
box for that type and to select that measurement type for
subsequent use. Press the same function key again to
hide the parameter box and cancel the selection. The
actual measurement is conducted left to right using each
chosen measurement type.
1
2
3
4
5
6
7
10
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Item Description
(1) Sample Name Displays the name of the currently measured sample.
(2) Area Displays the mean area for multiple injections.
(3) Conc. Displays the mean concentration for multiple injections.
(4) SD Standard deviation of the concentration values.
(5) CV% Coefficient of variance of the concentration values.
(6) TOC Conc. The TOC value is automatically calculated if both TC
and IC measurement types are selected.
(7) CNV Displayed below a converted measurement item set on
the "Conditions - Meas. Cond." screen. The character
string "CNV" can also be changed to any other character
string on the "Conditions - Meas. Cond." screen.
(8) Graph Displays the peak waveform being measured.
(9) Remark The following remark symbols are displayed:
• "T": Detector output tailing
• "H": Detector output out of range
• "F": Electric furnace temperature out of range
• "P": Incorrect sample boat position during
measurement
• "B": Unstable baseline during measurement
(10) Date & Time Displays the current date and time.
Function Keys
Key Function
F1 [Add Injection] Makes an additional measurement.
F3 [Zoom In] Enlarges the peak graph scale.
F4 [Zoom Out] Reduces the peak graph scale.
F6 [Exit Measurement] Ends measurement.
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This section describes the procedures used to perform measurements with the
SSM-5000A when it is connected to the TOC-LCPH/CPN.
76 SSM-5000A
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6. Click Next.
The Instrument Setup Wizard TOC dialog box is displayed.
7. Set [Cell Length] to [Short]. Set the other items appropriately for your
conditions of use. Enter the rest of the parameters according to the TOC-L
system.
8. Click Next.
The Instrument Setup Wizard SSM dialog box is displayed.
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3.4 Measurement Using the TOC-LCPH/CPN
Procedure
1. Launch LabSolutions Manager from the Windows Start menu and click (TOC
icon) in the Instruments tab.
The Sample Table Editor application starts up.
2. In the menu bar, select Options and click Hardware List.
78 SSM-5000A
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3.4 Measurement Using the TOC-LCPH/CPN
Procedure
1. Open the Sample Table Editor.
2. Click in the tool bar, or click in the Sample Table tab of
the file viewer.
TIP » The Select H/W Settings dialog box can also be opened by selecting File - New -
Sample Table.
3. Select the SSM-5000A configured system from the System drop down list.
Enter a comment as appropriate in the Comment field.
4. Click OK.
A new Sample Table is created, and displayed in the Sample Table Editor.
5. Use the following procedure to enter the parameters in the Sample Table.
Reference: For a more detailed explanation of these operations, refer to "5.4 Editing a Sample Table" in
the TOC-LCPH/CPN manual.
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Insert samples by dragging calibration curves and method files into the sample
table.
Drag the appropriate files from the file viewer.
Calibration curve files are used to generate a calibration curve. Method files
are used to measure an unknown sample.
Insert multiple samples using the same measurement parameters by copying and
pasting.
Select the inserted sample, right-click on the left-most cell of the row, and
select Copy.
Right-click on the left-most cell of the row into which the sample is to be
inserted, and select Paste.
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3.4 Measurement Using the TOC-LCPH/CPN
Insert multiple samples with the same measurement parameters collectively using
the Sample Group Wizard.
Right-click on the left-most cell of a row, and click Insert – Multiple Samples.
Enter the sample measurement parameters using the Sample Group Wizard,
and insert the samples into the table.
Reference: Refer to Section"5.4.4 Inserting Multiple Samples with the Same Measurement Parameters" of
the TOC-LCPH/CPN manual for a detailed description of the Sample Group Wizard.
Reference: Refer to Section "3.4.6 Schedule File" on page 96 for a description of the procedure to create a
schedule file.
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Procedure
1. Display the Calibration Curve tab in the file viewer, and click .
TIP » The Calibration Curve Wizard can also be opened by selecting File – New –
Calibration Curve.
2. Select the SSM-5000A configured system to be used from the System drop
down list.
3. Click Next.
The Calibration Curve Wizard (Page 3) Analysis Information page is
displayed.
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3.4 Measurement Using the TOC-LCPH/CPN
5. Click Next.
The Calibration Curve Wizard (Page 4) Calibration Point Parameter page is
displayed.
84 SSM-5000A
3.4 Measurement Using the TOC-LCPH/CPN
7. Click Next.
The Calibration Curve Wizard (Page 5) Calibration Points List window is
displayed.
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3.4 Measurement Using the TOC-LCPH/CPN
8. Verify each of the parameters and change them as necessary. Click the Add
button to enter a new calibration curve point. To change a calibration point,
select the relevant row and click the Edit button.
9. Click Next.
The Calibration Curve Wizard (Page 6) Additional Settings window is
displayed.
10. Enter the peak integration parameters or use the default settings. Enter the error
judgment parameters, as necessary.
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Procedure
1. Click in the Method tab of the file view list pane.
TIP: The Method Wizard can also be opened by selecting File – New – Sample Table.
2. Select the SSM-5000A configured system to be used from the System drop
down list
3. Click Next.
The Method Wizard (Page 2) SSM Analysis Information page is displayed.
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3.4 Measurement Using the TOC-LCPH/CPN
5. Click Next.
The Method Wizard (Page 3) SSM Parameters page is displayed.
88 SSM-5000A
3.4 Measurement Using the TOC-LCPH/CPN
7. Click Next.
The Method Wizard (Page 5) Peak Time Parameters page is displayed.
8. Enter the peak integration time parameters as necessary or use the default
settings.
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3.4 Measurement Using the TOC-LCPH/CPN
9. Click Finish.
The Method Wizard closes, and the method file is saved.
Procedure
2. Select the SSM-5000A configured system to be used from the System drop
down list.
3. Click Next.
The Control Sample Wizard (Page 2) Control Sample Type page is displayed.
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3.4 Measurement Using the TOC-LCPH/CPN
5. Enter an appropriate file name in the "Save the data in a control sample
template" field.
6. Click Next.
The Control Sample Wizard (Page 3) Parameter Source page is displayed.
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3.4 Measurement Using the TOC-LCPH/CPN
8. Click Next.
The Control Sample Wizard (Page 4) Analysis Parameters page is displayed.
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94 SSM-5000A
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3.4 Measurement Using the TOC-LCPH/CPN
Procedure
1. Click in the Schedule tab of the file viewer.
TIP: The Select H/W Settings dialog box can also be opened by selecting File – New –
Schedule.
2. Select the SSM-5000A configured system to be used from the System drop
down list.
Enter a comment in the Comment entry field, as necessary.
3. Click OK.
A new schedule is created and opened in the Sample Table Editor.
The measurement parameters and sample sequence is entered into the schedule
in the same manner as for the sample table. For details, refer to Section "3.4.2
New Sample Table" on page 80.
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3.4 Measurement Using the TOC-LCPH/CPN
3.4.7 Measurement
The following procedure describes connecting the PC and the TOC-L. For these
purposes, the term "connect" refers to the establishment of communication between the
TOC-Control L software and the TOC-L main unit.
Connection
The Sample Table Editor will connect to the instrument and the ready state of
the instrument will be shown at the right end of the toolbar.
The connected instrument icon in the Sample Table tab of the file viewer, also
illuminates.
Note: After connection is complete and the power is turned on to the SSM-5000A
electric furnaces, it takes about 40 to 50 minutes for the temperature to
stabilize.
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3.4 Measurement Using the TOC-LCPH/CPN
TIP: Measurement can also be started by selecting Instrument – Start Measurement while
the instrument is properly connected.
2. Click Start.
4. Open the sample port cover, and place the sample boat and sample on the
sample boat transfer plate.
5. Securely close the sample port cover.
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3.4 Measurement Using the TOC-LCPH/CPN
6. Click Start.
Note: If the carbon content of the standard is 3.0mg or less, wait 1.5 - 2 minutes
after the cover is closed before clicking Start to avoid inclusion of an
atmospheric CO2 peak.
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3.4 Measurement Using the TOC-LCPH/CPN
CAUTION
After TC measurement, the sample boat transfer rod must be allowed to cool.
Always move the sample boat transfer knob to the Cooling position and
allow it to cool before moving it to the Change position. The instrument may
be damaged if the sample boat transfer rod is moved directly to the Change
position.
10. Examine the measurement results, and set further processing steps as
appropriate.
• Repeat
Click the Repeat button to repeat the sample from step 2.
• Next
Click the Next button to measure the next sample by repeating the procedure
from step 2.
• Stop
Click the Stop button to end the measurement process.
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3.4 Measurement Using the TOC-LCPH/CPN
Note: IC reaction acid may occasionally overflow from the sample boat and
accumulate on the bottom of the IC sample boat transfer plate. During sample
boat replacement, inspect and clean the sample boat transfer plate using a
cotton swab or the cotton-tipped applicator.
TIP: To reject the measurement data, select the data to be excluded, and click the Exclude
button.
Note:
• Turn the power to the SSM-5000A TC furnace off at least 30 minutes before
turning off the power to the instrument. If the instrument is switched off
without allowing the TC furnace to cool, the cooling fan for the TC furnace
stops operating, causing accelerated wear of the O-rings due to the high
temperature inside the furnace. This procedure does not apply in emergency
situations.
• If the SSM-5000A is to remain idle for an extended period, flush any
remaining phosphoric acid in the IC reagent tubing, or replace the phosphoric
acid with water. If phosphoric acid is allowed to remain in the tubing,
particulates may form and obstruct the tubing.
• Use a cotton swab or cotton-tipped applicator, etc. to remove any acid or other
corrosive substances that may have contacted the swage lock fittings or any of
the TC and IC sample port parts, such as the sample boat holder and sample
boat push rod. Wash the affected surfaces with water if they have been in
contact with any especially corrosive substances.
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3.4 Measurement Using the TOC-LCPH/CPN
3.4.8.1 Shutdown
This section describes the procedure for switching off power to the instrument.
Shutdown Procedure
1. Click .
TIP: The Shutdown window can also be displayed by selecting Instrument – Shutdown.
Note: If the power to the electric furnace of the TOC-LCPH/CPN is turned OFF, the
furnace temperature decreases and then the carrier gas flow stops. After 30
minutes, the TOC-L power is automatically turned OFF (although the main
power remains on).
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3.4 Measurement Using the TOC-LCPH/CPN
3.4.8.2 Sleep
This function allows the instrument to enter a standby state where the furnace is off and
the carrier gas flow has been stopped. Approximately one hour before a predetermined
time, the instrument automatically turns the flow of the carrier gas back on and turns
the power on to the furnace. The instrument returns to a state of readiness at the
predetermined time.
Sleep Procedure
1. Click .
TIP: The Shutdown window can also be displayed by selecting Instrument – Shutdown.
2. Select Sleep.
3. If any units should remain on during the sleep state, click Extra Settings and
select the corresponding checkbox for each unit.
Note: The carrier gas ON/OFF setting refers to the carrier gas supply to the TOC-L.
The carrier gas supply to the SSM-5000A must be turned ON/OFF manually.
4. Enter the date and time for the instrument restart in the Auto Restart Time
fields.
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3.4 Measurement Using the TOC-LCPH/CPN
5. Click OK.
The specified units will be turned off automatically. Approximately one hour
prior to the set time, the power to each of those units will turn on automatically,
allowing measurement to start at the set time.
TIP: Click End Sleep mode to release the instrument from the sleep state.
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Common Tab
The Common tab displays basic information related to the calibration curve.
Item Description
System This is a read-only field displaying the system used to measure the calibration
curve.
User This is a read-only field displaying the name of the user who generated the
calibration curve file.
Date of Creation This is a read-only field displaying the date and time the calibration curve file
was created.
Comment A text comment related to the system settings may be entered in this field.
This field handles up to 512 alphanumeric characters.
Print This opens the Print dialog box. Make any necessary changes, and click the
Print button to print the contents of the Calibration Curve Properties window.
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3.4 Measurement Using the TOC-LCPH/CPN
Parameter Tab
The Parameter tab displays the measurement parameter settings.
Item Description
Analysis Displays the type of measurement.
Status Displays the condition of the calibration curve file. After the calibration
curve has been Completed, many of calibration curve properties items
cannot be edited.
• Defined: Unmeasured state
• Completed: Measurement completed
• Aborted: Measurement cancelled state
Sample Name Displays the sample name.
Sample ID Displays the sample ID.
No. of Cal. Points A read-only display of the number of points in the calibration curve.
Calculation Displays the calculation method.
Method
Zero Shift Displays the shift to zero point setting.
Calibration Curve A read-only display of the file name and directory path for the calibration
File curve file.
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Analysis Tab
The Analysis tab displays additional analysis parameter settings.
Item Description
Density Displays the density of a liquid sample.
Volume or Weight Selected radio button indicates the type of calculation that is used.
Use default settings If this item is checked, the default software settings are used for
peak detection time.
Min. integration time Displays the minimum time the instrument signal will continue to
be detected.
Max. integration time Displays the maximum time the instrument signal will be detection
when no peak is detected.
Correlation Coeff. Check If this item is checked, the calibration curve error judgment is
based on the correlation coefficient.
Failure Action (1st time) / Displays the processing conducted if errors occur.
Failure Action (2nd time)
Lower Limit Displays the lower correlation coefficient limit.
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3.4 Measurement Using the TOC-LCPH/CPN
Data Tab
The Data tab displays information related to each of the calibration points used to
generate the calibration curve.
Item Description
No. Displays the calibration point number.
Conc. Displays the concentration of the calibration point.
Mean CNV Displays the average of the conversion values.
No. of Inj. Displays the number of injections.
Excluded "E" is displayed if the calibration point has been excluded as a data
value.
Weight Displays the weight of the standard sample.
Volume Displays the volume of the standard sample.
Abs. C (ug) Displays the carbon amount determined from the weight or volume
and carbon concentration of the standard sample.
SD Displays the standard deviation value.
CV Displays the coefficient of variation value.
Edit This button opens the Edit Calibration Point Parameters dialog
box. The selected calibration point parameters can be edited.
Add This button opens the Edit Calibration Point Parameters dialog
box. A new calibration point can be added.
Delete This button deletes the selected calibration point.
Delete All This button deletes all of the calibration points.
Exclude This button excludes the selected calibration point from the
calculations.
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3.4 Measurement Using the TOC-LCPH/CPN
Graph Tab
The Graph tab displays the calibration curve graph.
Item Description
Slope/Intercept/r^2/r Displays the slope, y-intercept and coefficient of determination and
correlation coefficient values.
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3.4 Measurement Using the TOC-LCPH/CPN
History Tab
The History tab displays the change history associated with the calibration curve file.
Item Description
ASCII export Click this button to open the Save As dialog box. The history of the
changes made to the calibration curve file can be exported as a text
file in ASCII format.
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Common Tab
The Common tab displays basic information related to the method or control sample.
Item Description
System Read-only field that displays the system used to measure the
calibration curve.
User Read-only field that displays the name of the user who generated
the calibration curve.
Date of Creation Read-only field that displays the date and time the calibration
curve was generated.
Comment A text comment related to the system settings may be entered in
this field. This field handles up to 512 alphanumeric characters.
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3.4 Measurement Using the TOC-LCPH/CPN
Parameter Tab
The Parameter tab displays the measurement parameter settings.
Item Description
Analysis Displays the type of measurement.
Manual Dilution Displays the preparation dilution factor.
Sample Name Displays the sample name.
Sample ID Displays the sample ID.
No. of Determinations Displays the number of times sample analysis is conducted.
Use Weight or Use Volume Select Use Weight for solid samples and Use Volume for liquid
samples.
Density Displays the sample density when the sample is a liquid.
Current Method Displays the method file name or control sample file name.
112 SSM-5000A
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3.4 Measurement Using the TOC-LCPH/CPN
History Tab
The History tab displays the change history associated with the file.
Item Description
ASCII export Click this button to open the Save As dialog box. The history of the
changes made to the calibration curve file can be exported as a text
file in ASCII format.
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Item Description
Control Sample / Control Chart The selected radio button indicates the selected control sample
Sample type.
Recovery / Mean Value The selected radio buttons indicate the type of control sample
(Concentration) / Blind Value check that will be conducted.
(Area) / Spanwidth (Conc.)
Spiked Select this item to calculate the Recovery % of the original
control sample to a spiked control sample.
Original Concentration Displays the concentration of the original control sample.
Spiked Concentrations 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. Curve Select this item to ignore the calibration curve shift to the zero
in Conc. Calculation point when calculating the concentration.
Action when the failure event Displays the measures to be taken if the control sample exceeds
occurs the first time / Action any of the limit values.
when the failure event occurs
the second time
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3.4 Measurement Using the TOC-LCPH/CPN
The Monitor window displays the current instrument condition. To display the Monitor
window, click .
There may be multiple tabs in the Monitor window. To check the condition of the
SSM-5000A, select the SSM tab.
SSM Tab
TIP: The Background Monitor window can also be displayed by selecting Instrument –
Monitor.
Item Description
SSM Power / SSM-TC These display the status of the SSM power, TC furnace and the IC
Furnace / SSM-IC Furnace furnace. For each, the Ready state is indicated with and the Not
Ready state with .
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.
The cursors in the left bar displays the position of the Y axis.
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3.4 Measurement Using the TOC-LCPH/CPN
SSM Tab
Item Description
SSM Power Selected when power is ON.
Sample Change Position Selected when TC sample boat transfer knob is in the Sample
(TC) Change position.
Measurement Position (TC) Selected when TC sample boat transfer knob is in the Measuring
position.
Sample Change Position Selected when IC sample boat transfer knob is in the Sample
(IC) Change position.
Measurement Position (IC) Selected when IC sample boat transfer knob is in the Measuring
position.
SSM TC Furnace Ready Selected when the TC furnace temperature is in the Ready state.
SSM IC Furnace Ready Selected when the IC furnace temperature is in the Ready state.
AUX This is an auxiliary signal terminal setting. This is disabled as it is
not used.
SSM TC Furnace Control Select this item to turn ON the power to the TC furnace.
SSM IC Furnace Control Select this item to turn ON the power to the IC furnace.
Cooling Fan Control Select this item to turn ON the power to the cooling fan in front of
the TC furnace.
AUX 1 – AUX 5 These are auxiliary signal terminal settings. These are disabled
even if they are selected.
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This section describes the procedure for setting the default measurement parameters.
The settings defined in this operation are used when generating a calibration curve and
and creating a method.
The default values for use with the SSM-5000A consist of two settings, the unit of
concentration and the number of injections.
Procedure
1. Click Options – Default Measurement Parameters.
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Procedure
1. Click New on the Sample Table tab in the file viewer or New on the tool bar.
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3. Click OK.
The Validation Settings window is displayed.
120 SSM-5000A
3.5 Measurement Using the Cell Switching Valve Set (Option)
3.5.1 High Sensitivity Measurement Using the Cell Switching Valve Set
The addition of the cell switching valve to the SSM-5000A and TOC-L improves the
TC measurement sensitivity for solid samples in two steps of approximately 6 times
(for specification [A]) and approximately 100 times (for specification [B]).
Table 3.1 • Cell Switching Valve Functionality and Measurement Performance Specifications
Specification Cell Switching Valve Measurement Remarks
Functionality Performance
(TC Measurement
Only)
Specification Bypasses the IC measurement Full scale: 300 gC Carrier gas is oxygen gas of greater
[A] stream and carrier gas flow Detection limit: 5 gC than 99.9 % purity.
stabilizer in the SSM-5000A. Sample water content within 0.4 g
Specification In addition to specification [A], the Full scale: 25 gC Carrier gas is high purity oxygen
[B] SSM-5000A connects to the NDIR Detection limit: 0.3 gC (CO, CO2, and HC all less than
long cell of the TOC-L. 1 ppm).
Sample water content within 0.4 g
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Table 3.2 • Cell Switching Valve Functionality and Measurement Performance Specifications
Specification NDIR Cell IC Other Configuration NDIR Carrier
Switching Measurement Cell Gas Flow
Valve Stream Bypass Settings Rate
Configuration Valve
(Valve on the Configuration
Upper Rear of (Valve on the
the TOC-L) Upper Rear of
the
SSM-5000A)
Standard S N - SHORT 500 mL/min
specification
Specification S H • Remove the rubber tubing SHORT 400 mL/min
[A] that connects the two nipples
on the upper rear of the
SSM-5000A and install a
PTFE tubing with a rubber
joint from the left nipple to
the NDIR cell switching
valve on the upper rear of the
TOC-L. (see Figure 3.6)
• Open the IC sample port
cover (raise it a few
millimeters).
Specification L H In addition to specification [A], LONG 400 mL/min
[B] perform the following:
• Remove both the PTFE
tubing and rubber joint
connected to the inlet (with
an "L" label) of the CO2
absorber for optical system
purge gas purification on the
TOC-L, and in their place,
connect the plastic tubing
with the "L" label attached to
it, which is protruding out of
the rear panel of the TOC-L.
(See Figure 3.7)
122 SSM-5000A
3.5 Measurement Using the Cell Switching Valve Set (Option)
The IC measurement stream is sealed up for both specification [A] and specification
[B]. Always open the IC sample port cover (raising it a few millimeters is sufficient) to
prevent water in the drain pot from being sucked up into the drain separator as the IC
furnace heats up or cools down.
The mist trap and sub-trap included in this option are installed to prevent IC reagent or
IC reagent mist within the IC reaction vessel of the TOC-L from flowing into the NDIR
short cell when using specification [B]. Insert the drain tubing of the mist trap into a
suitable container. Although the tap below the mist trap should be closed during
measurement, check at least once a day to verify whether IC reagent has accumulated
in the drain, and if so, open the tap to discharge any reagent. Discharge any reagent in
the drain before running the instrument for an extended period of time, particularly
when the instrument will be left unattended, such as over night.
Standard Specification
Rubber Tubing
IC Measurement Stream
Bypass Valve
Stream Change
To the TOC-L
Switch to "H"
Figure 3.6 • Method to Bypass the IC Measurement Stream (Specification [A] and Specification [B])
SSM-5000A 123
3.5 Measurement Using the Cell Switching Valve Set (Option)
From SSM-5000A
Figure 3.7 • Connection Changes for the CO2 Absorber for Optical System Purge Gas
Purification (Specification [B])
CAUTION
The cell switching valve knobs each click into place at the "S" and "L"
positions and "N" and "H" positions. When the knobs are oriented at any
other position (and move freely without clicking), the corresponding valve
blocks the flow of carrier gas. Do not leave the knobs oriented in this free
state for long in order to prevent damage to stream components.
124 SSM-5000A
4
4 Maintenance
Maintenance and service are extremely important to ensure proper instrument
operation and to obtain stable, accurate measurement.
4.1 Inspection
This section describes the parts and components requiring inspection and
replacement and describes the inspection and replacement procedures.
4.2 Troubleshooting
This section describes the error messages displayed by the SSM-5000A and the
appropriate troubleshooting procedures.
4.1 Inspection
4.1 Inspection
CAUTION
To avoid burn injuries, wait for the TC combustion tube and TC catalyst to
cool to room temperature before starting maintenance work.
The electric furnace temperature is indicated in the SSM-5000A display
window.
TC Combustion Tube
When the inside surface of the combustion tube reacts with salts contained in the
samples, it devitrifies, or becomes crystalline in texture and turns white. The tube can
continue to be used in this condition until it breaks or cracks, causing gas leaks.
Measurement of samples containing components that erode the quartz tube when
burned (such as fluorine or alkaline components), combined with the high TC furnace
temperature up to 900°C, can shorten the service life of the TC combustion tube.
TC Catalyst
It is time to replace the TC catalyst when the following phenomena occur:
• Measured values (peak area values) for a standard sample are lower than previous
values obtained using the same measurement parameters.
• Measurement repeatability accuracy deteriorates.
When such phenomena occur, first check that the gas flow line is not leaking. If no
leaking is discovered, replace the TC catalyst.
The efficiency of combustion oxidation of a solid sample varies considerably according
to the sample type and organic content. When evaluating the performance of the TC
catalyst, use a standard of the same type and characteristics as the actual samples.
Measuring various amounts of the sample and checking for a linear proportionality
relationship is a method of inspecting the oxidation catalyst using the actual sample.
Use a sample with evenly distributed carbon for this method to reduce errors during
sampling.
Generally, when performance of an oxidation catalyst deteriorates, the effects are larger
at higher carbon content levels, such that the linear proportionality relationship is no
longer maintained.
Note: Cobalt oxide may occur after using this product. Handle with care.
To dispose of it, ask an industrial waste disposer in compliance with the local
laws and regulations.
126 SSM-5000A
4.1 Inspection
SSM-5000A 127
4.1 Inspection
If the water level in the drain vessel drops, the float continuously seals the ring,
preventing discharge of carrier gas or drain water.
Note: Supply enough water to the drain vessel to ensure the float is separated from
the ring, as drain water cannot be discharged if the water level is too low.
The supply of drain water to the drain vessel during SSM-5000A measurement is
less than during TOC-L measurement. Therefore, it is easy for the water level in
the drain vessel to drop. Check the drain vessel water level before starting
measurements.
O-Ring PTFE P6(A)
Sample Port Block
O-Ring 4D(B)
O-Ring Installation Adapter Installation Screws
(Hex Screws)
Sample Boat
Push Rod
128 SSM-5000A
4.1 Inspection
Drain Separator
Drain Vessel
Float
Ring
Reference: See Section "5.5.8.2 Installing the TC Combustion Tube and IC Reaction Tube" on page
152.
Replacing O-Rings Between the Sample Port Block and Sample Boat Push Rod
Note: Turn off the SSM-5000A power before replacing the O-rings.
SSM-5000A 129
4.1 Inspection
3. Push the sample boat push rod knob about 4 to 5cm into the furnace from the
SAMPLE CHANGE position.
4. Open the sample port cover, and fit the O-ring removing adapter over the
sample boat push rod through the sample port opening.
O-Ring Removal
Adapter Place Over the
Sample Boat Sample
Push Rod Boat
Push
Rod
Sample Boat
Push Rod
O-Ring Installation
Adapter
Pull Out
Phillips Screw
130 SSM-5000A
4.1 Inspection
Note: Any foreign matter that is stuck to the surface of the sample boat
push rod prevents the rod from sliding smoothly and may cause
gas leaks due to accelerated wear or scratching of the PTFE
O-rings.
If foreign matter is found on the surface of the sample boat push rod, clean
it off or use a soft cloth to polish the surface of the rod.
If foreign matter is stuck to the part of the rod that enters the furnace and
cannot be easily wiped off, wash it in approximately 1M hydrochloric acid
or polish with polishing powder. Using polishing powder may reduce the
diameter of the sample boat push rod, causing more frequent gas leaks.
TIP » The surface of the TC sample boat push rod may become discolored due to the formation of
an oxide film on the portion that is inserted into the furnace. This film does not interfere
with analysis unless the surface of the sample boat push rod becomes roughened.
9. Reverse the procedure for removing the O-rings to put two new O-rings and
the O-ring installation adapter on the sample boat push rod. Tighten the
Phillips screw on the back of the sample boat push rod knob.
10. Holding the knurled part of the O-ring installation adapter, turn it clockwise to
screw it into the sample port block until the sample boat push rod resists
movement.
11. Verify that no gas leaks from the PTFE O-rings.
Reference: See Section "4.1.2 Checking for Gas Leaks" on page 127.
12. Apply a light coat of silicone grease (supplied with TOC-L) to the sample boat
push rod on the IC side, so that it moves smoothly and easily.
Note: • The IC sample boat push rod must be moved gently to avoid spilling the IC
reaction acid out of the sample boat.
• Never use grease on the TC sample boat push rod. The grease will burn when
the sample boat is moved into the TC furnace, generating CO2 and creating a
high margin of error in the measured values.
SSM-5000A 131
4.2 Troubleshooting
4.2 Troubleshooting
The following messages may be displayed in the center of the TOC-L screen. Take the
appropriate remedial action as described in the table below.
132 SSM-5000A
4.2 Troubleshooting
The following messages may be displayed in the center of the TOC-L screen. The red
warning indicator simultaneously flashes. These messages indicate that a fatal error
occurred and operation cannot continue.
SSM-5000A 133
4.2 Troubleshooting
The following messages are displayed when an error is detected during parameter entry
or operation. Use the remedial measures listed in the table below to alleviate the
situation.
The following messages indicate that an error has occurred that prevents measurement
operations from continuing. Take appropriate measures as indicated in the table.
134 SSM-5000A
4.2 Troubleshooting
Is the SSM-5000A NO
power indicator LED
illuminated?
Power cord is unplugged or
Power is not turned ON.
YES
Remedy the cause if the
no-fuse breaker in the power
Is the supply switch has been tripped.
SSM-5000A
power cable correctly NO
connected between the
SSM-5000A and
the TOC-L?
Improper connection of the
connector cable.
YES
Connect the cable properly.
Electrical system is defective.
SSM-5000A 135
4.2 Troubleshooting
Is the
temperature for
the SSM-TC furnace or NO
SSM-IC furnace set to ON
in the "Conditions"
screen? Improper screen settings.
Is the overheat
protection thermostat NO
normal? (Button pops
out when
activated.) Furnace is overheating.
136 SSM-5000A
4.2 Troubleshooting
Is the
carrier gas
supplied correctly to the NO
TOC-L and SSM- 5000A?
Are the gas tubing
connections
correct? Defective tubing connections.
Is gas escape NO
from the drain vessel
correctly prevented?
No water, or gas leak in the
drain vessel.
YES Add water to the drain vessel
or stop the gas leak.
Is the sample NO
port cover fully closed?
Is acid correctly NO
injected into the IC
sample boat?
Defective acid injection.
Is the sample
boat loaded in the NO
correct position for the
TC (or IC)
furnace? Incorrect sample boat position.
SSM-5000A 137
4.2 Troubleshooting
Is carrier gas
flowing properly and NO
without leaks?
Gas leak.
Is the amount of NO
acid injected for IC analysis
appropriate?
Too much or too little
acid injected.
YES 1.) Add a suitable amount of
acid to decompose the IC.
2) If the total amount of acid
and sample is too large,
Is the sample
boat loaded in the reduce the amounts.
NO
correct position for the
TC (or IC)
furnace? Incorrect sample boat position.
YES Load the sample boat in the
correct position.
TOC-L is defective.
Contact your Shimadzu
representative.
138 SSM-5000A
5
5 Reference Information
This chapter presents technical information, such as the specifications, accessories, and
installation procedures in the event that the instrument is moved.
5.1 Specifications
The SSM-5000A specifications are listed here.
5.5 Installation
This section describes the site conditions and installation procedures for the
SSM-5000A.
5.1 Specifications
5.1 Specifications
140 SSM-5000A
5.2 Accessories List
SSM-5000A 141
5.3 Special Accessories List
142 SSM-5000A
5.5 Installation
5.5 Installation
Verify Shipment
Confirm that all of the items listed in Section "5.2 Accessories List" on page 141 are
included.
290
Figure 5.1 • TOC-L + SSM-5000A External Dimensions (Example: Units in mm for TOC-LCSH)
CAUTION
• Internal parts reach very high temperatures and could cause a fire hazard. For
safety and ease of maintenance, leave a space of at least 200mm between walls
and the left, right, and rear of the instrument. In order to prevent any interference
during operation, be aware that the power switch is located on the right side of
the SSM-5000A.
• Lift the SSM-5000A at the bottom of each side of the instrument and lift it by the
base plate. Do not lift it by the front access door, as this may cause instrument
damage.
SSM-5000A 143
5.5 Installation
CAUTION
Avoid locations where flames are prohibited. Some internal parts reach very
high temperatures and could cause a fire hazard.
Due to the possibility of analysis error, avoid the following types of sites:
• Areas near heat sources
• Areas next to windows receiving direct sunlight
• Areas in direct exposure to air expelled from an air conditioner
• Areas near equipment generating strong magnetic fields, electric fields, or high
frequencies
CAUTION
Before proceeding with these operations, verify that the power to the TOC-L
and the SSM-5000A is OFF.
144 SSM-5000A
5.5 Installation
1. On the provided digital I/O board, set 1 to ON and 2 to OFF for "SW1".
2. Remove the screws from the right cover plate of the option board installation
rack located on the rear panel of the TOC-L.
3. Insert the supplied digital I/O board into the option board installation rack.
1. Identify the "TOC" and "SSM" indications on the ends of the provided
connection cable and connect the cable between the TOC-L and the
SSM-5000A, matching the indications with the appropriate unit.
Option Board Installation Rack
Driver Board
SSM-5000A 145
5.5 Installation
CAUTION
The instrument may not function correctly if the supply voltage does not
meet or exceeds the 100 to 115VAC or 220 to 240VAC ranges.
Unstable voltage supply may impede high-sensitivity measurements.
Use a power supply installed with an earth leakage circuit breaker.
Note: This instrument can function at a 50Hz or 60Hz power supply frequency. Use
only Shimadzu-specified or the supplied power cable. Do not use unspecified
power cables.
Ground Connection
The supplied power cable contains three leads, including a ground lead. The attached
plug is a grounded, 3-pin plug.
The live (AC) and ground (ACC) pins of the plug are arranged as shown in "Figure 5.3
• Electrical Plug" on page 146. Connect it to a socket with the same configuration.
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: 100W or less) is recommended.
• Perform grounding separately and avoid contact with water supply pipes, gas
pipes, and lightning rods.
146 SSM-5000A
5.5 Installation
Connection Procedure
1. Connect the oxygen gas cylinder to the gas inlet (GAS INLET) on the back of
the SSM-5000A (Supply pressure of 200 to 300kPa).
TIP » Use of the air tubing set, available as a special accessory, is recommended. The air
tubing set contains nylon tubing and connectors (2 x half-unions).
TIP » Connect the nylon tubing to the half-union by pushing the tubing into the half-union. To
disconnect the tubing, pull it out while firmly pressing the blue ring with a flathead
screwdriver.
2. Guide the PTFE tubing from the gas outlet (GAS OUTLET) on the
SSM-5000A rear panel through the grommet in the upper part of the TOC-L
rear panel.
SSM-5000A 147
5.5 Installation
3. Connect the PTFE tubing to the inlet on the short cell of the TOC-L NDIR
optical system tandem cell using the supplied tapered elbow joint (6 - 4mm
ID).
To TC Sample Port
Pressure
Regulator Mass Flow Controller Flowmeter
148 SSM-5000A
5.5 Installation
Connect the provided PTFE tubing (3mm O.D, 2mm I.D.) between the long cell gas
outlet and the CO2 absorber gas inlet.
From SSM-5000A
Detector
SSM-5000A 149
5.5 Installation
CAUTION
• To avoid burn injuries, allow the TC combustion tube and TC catalyst to cool to
room temperature before performing maintenance. The electric furnace
temperature is indicated in the SSM-5000A display window.
• The TC combustion tube is made of quartz glass and the IC reaction tube is made
of hardened glass. Handle with care to avoid breaking and to prevent injury from
broken glass.
• Inhaling quartz wool may cause health impairment. Handle with care. For details,
refer to the "Safety Data Sheet (SDS)" of the TOC-L Series User’s Manual.
The TC combustion tube is filled with the catalyst, as shown in "Figure 5.6 • Filling the
TC Combustion Tube with Catalyst" on page 151.
Procedure
TIP » To prevent clustering of either type of catalyst, rotate the TC combustion tube while
filling it with the catalyst mixture.
4. Fold the catalyst support screens as shown in "Figure 5.6 • Filling the TC
Combustion Tube with Catalyst" on page 151, and insert them into the TC
combustion tube.
5. Push the catalyst support screens into place with the catalyst filling rod
supplied as a TOC-L accessory.
TIP » Use the catalyst packing rod to pack the catalyst in a manner that creates some
resistance between the inside of the combustion tube and the outside of the mesh. This
prevents the mixed catalyst from crumbling and falling through the mesh and possibly
flowing upstream toward the detector.
150 SSM-5000A
5.5 Installation
Fold Lines
Catalyst Support
Screen (upstream)
Fold Around
the Periphery
Catalyst Support
Screen (downstream)
SSM-5000A 151
5.5 Installation
CAUTION
• To avoid burn injuries, allow the TC combustion tube and TC catalyst to cool to
room temperature before performing maintenance. The electric furnace
temperature is indicated in the SSM-5000A display window.
• Do not use wrenches or other tools as they may break the combustion tube and
cause injuries.
152 SSM-5000A
5.5 Installation
1. Remove the screws (4 knurled, 2 Phillips) then lift out the sample boat moving
units.
2. Place the white PTFE O-ring P35 onto the TC combustion tube or IC reaction
tube. Place the sample port adapter over the white O-ring as shown in "Figure
5.8 • Installing the O-Ring" on page 153. Gently insert the tapered end of the
combustion or reaction tube into the appropriate furnace.
TC Combustion Tube or IC Reaction Tube
Note: Pull the sample boat push rod knob forward to attach the two
Phillips screws to the front.
5. Align the flange of the combustion or reaction tube and push the tube in while
securing the sample port adapter to the sample port block.
Sample Port Block O-Ring 4D P35
TC Combustion Tube or
IC Reaction Tube
SSM-5000A 153
5.5 Installation
TC Combustion Tube
Clearance of 1-2mm
L-shaped Swage Lock Union
Glass L-Pipe
Figure 5.10 • Connecting the TC Combustion Tube to the Swage Lock Union
Procedure
1. Loosen the screws that hold the rear access panel to the TC furnace in place.
Lift up to remove the rear access panel.
2. Insert the tip of the combustion tube into the swage lock union. Lightly
hand-tighten the box nut.
Note: With the box nut slightly tightened but the small diameter part of
the tube still able to slide, slide the tip of the tube to create a
clearance of 1 to 2mm from the contact face of the union.
3. Hand-tighten the box nut.
Sufficient sealing is obtained if the swage lock union does not move when pulled
upward.
CAUTION
• Avoid using wrenches to tighten the box nut. The TC combustion tube is made of
quartz glass, which will break if the box nut is over-tightened.
• The tip of the TC combustion tube may chip if the box nut is tightened with the
tip of the tube touching the contact face of the union.
• Use only the supplied PTFE front and rear ferrules. Never use metal or other
ferrules.
• Protect the inner and outer surfaces of the TC combustion tube tip, inner surface
of the swage lock fitting, ferrules and other gas contact surfaces from grease, oils
or other organic substances.
154 SSM-5000A
5.5 Installation
Procedure
1. Remove the PTFE elbow from the outlet of the acid dispenser.
2. Locate the acid injection tubing which is attached to the SSM-5000A IC
sample port cover. Fully insert the free end into the tubing adapter (located in
the SSM assessors packet).
3. Firmly push the tubing adapter into the acid dispenser outlet.
Acid Injection Tubing
(2mm OD)
Acid Dispenser
IC Sample
Port Cover
Acid
Dispenser
Outlet
TIP » The threads on the neck of the glass container for phosphoric acid match those on the
acid dispenser. This allows the acid dispenser to be attached directly to the glass
phosphoric acid container.
6. Replace the water in the acid dispenser with the phosphoric acid. See Section
"3.1.7 IC Reaction Acid" on page 20 for details on the phosphoric acid
concentration.
7. Operate the acid dispenser to purge the water from the tubing with the
phosphoric acid.
SSM-5000A 155
5.5 Installation
CAUTION
• Phosphoric acid is highly corrosive. Use care to avoid touching or spilling it
during handling. See the Material Safety Data Sheet (SDS) section in the TOC-L
USER'S MANUAL for details.
• If phosphoric acid spills on any sliding parts, wipe it off immediately using a
damp cloth.
Note: The IC sample port cover should always remain in the closed
position, except during sample transfer. Corrosion may occur if
the sample port cover is left open and acid leaks onto the sliding
mechanism of the sample port cover. Keep an empty sample
boat in the IC sample port when it is not in use to catch any acid
that may leak from the acid dispenser.
Reference: For details about the drain tubing see the "Connecting the Drain Tubing" section in the
TOC-L USER'S MANUAL.
CAUTION
The drain liquid may contain acid or other corrosive substances. Use care to
avoid touching or spilling the drain liquid.
156 SSM-5000A