Shimadzu TOC5000 Manual 2

M393-0085D
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Total Organic Carbon Analyzer
TOC-5000/5050
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PIN 638-90216 \~
Instruction Manual \
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Copyright © Shimadzu Corporation 1991. All rights are reserved, including those to reproduce
this publication or parts thereof in any form without permission in writing from Shimadzu
Corporation.
Information in this publication 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 publication despite the utmost care taken
in its production will be corrected as soon as possible, but not necessarily immediately upon detection.
Table of Contents
1 Introduction 1
2 Inspection 3
3 Installation 5
3.1 Installation site .5
3.1.1 Placement and space requirements .5
3.1.2 Environmental requirements .5
3.2 Unpacking .6
3.3 Power Connection and Grounding .6
3.4 Change of supply voltage .7
3.5 Gas requirements .7
3.6 Gas connection

.8
3.7 Connection of drain tubing .9
4 Instrument preparation
11
4.1 Filling dehumidifier drain vessel
11
4.2 Preparing humidifier
12
4.3 Preparing soda lime scrubber
12
4.4 Filling TC combustion tube with TC catalyst
13
4.4.1 Procedure for regular sensitivity catalyst
13
4.4.2 Procedure for high-sensitivity catalyst
14
4.5 Connecting TC combustion tube
14
4.6 Loading chart paper in printer
16
4.7 Preparing IC reagent reservoir
17
4.8 Preparing IC reaction vessel
17
+.9 Mounting microliter syringe
18
5 Keypad and LCD unit

21
5.1 Key functions
21
5.2 LCD unit 22
6 Screen displays and functions 23
6.1 INITIAL START screen (Normal Start) .23
6.2 INITIAL START screen (ALL RESET Start) .24
6.3 MAIN MENU screen ..... .26
6.4 CALIBRATION/CONDITIONS screen .29
6.5 MEASUREMENT START screen (for Calibration) .32
6.6 DATA PROCESSING STANDARD screen .34
6.7 CALIBRATION CURVE screen . . . . .37
6.8 SAMPLE MEASUREMENT/CONDITIONS screen .39
6.9 MEASUREMENT START screen (at Sample Measurement) .42
6.10 DATA PROCESSING SAMPLE screen .44
6.11 GENERAL CONDITIONS Screen . . .48
6.12 CALIBRATION CURVE FILE LIST screen . 51
6.13 DATA REPORT screen .54
6.14 MONITOR screen .57
6.15 STANDBY OPTIONS screen .59
6.16 MAINTENANCE screen .62
7 Analysis preparation 67
7.1 Supplying carrier gas . .67
7.2 Setting syringe size (GENERAL CONDITIONS screen) .67
7.3 Turning on TC furnace (GENERAL CONDITIONS screen) .67
7.4 Zero point detection of syringe pump (MAINTENANCE screen) .68
7.5 Setting date and time (in MAINTENANCE screen) . . . . .68
7.6 Regeneration of TC catalyst (also in MAINTENANCE screen) .68
7.7 Regeneration of IC solution (MAINTENANCE screen) .69
7.8 Preparation of standard solutions . . . . . .69
7.8.1 Preparation of TC (TOC) standard solution .69
7.8.2 Preparation of IC standard solution .70
7.8.3 Storage of standard solutions .70
8 Analysis 71
8.1 Calibration 71
8.1.1 Preparation for calibration 71
8.1.2 Calibration proced ure 71
8.2 Sample measurement 72
8.2.1 Measurement procedure 72
8.3 High-sensitivity measurement 73
8.3.1 Handling of TC combustion tube with high-sensitivity catalyst 73
8.3.2 Handling of purified water or samples with ultra-low carbon content 74
8.3.3 Dedicated microliter syringe 74
8.3.4 IC removal in high-sensitivity measurement 75
8.3.5 TC Blank Check 75
8.4 Measurement of samples with high IC content 75
8.4.1 Acidification 76
8.4.2 Sparging 76
8.5 Measurement of samples with suspended solids 78
8.6 Measurement of samples containing acid, alkali or salts 78
8.6.1 Chloric acids and salls 79
8.6.2 Non-chloric acids and salls 79
8.6.3 Alkali samples . 80
8.6.4 Samples containing salts 80
9 MAINTENANCE 81
9.1 Daily inspection 81
9.2 Zero adjustment of infrared gas analyzer (NDIR) optical system 82
9.2.1 Adjustment procedure 82
9.2.2 Causes of sudden deviation of baseline position 84
9.2.3 Causes of gradual and chronic deviation of baseline position 84
9.3 Regeneration procedures 85
9.3.1 Regeneration of TC catalyst 85
9.3.2 Regeneration of IC solution . 87
9.3.3 Regeneration of TC catalyst and IC solution . 88
9.4 Maintenance procedures . 88
9.4.1 Replacement of high purity air (in cylinder) . 88
9.4.2 Cleaning/replacement of syringe plunger tip . 88
9.4.3 Cleaning and replacing the sampling needle . 88
9.4.4 Replacing O-rings in sliding TC sample injection block (monthly) . 89
9.4.5 Replacing O-ring between injection block and TC combustion tube . 90
9.4.6 Replacing O-rings in IC reaction vessel sliding sample injection block . 90
9.4.7 Cleaning and replacing sample injection needle . 91
9.4.8 Replacement of soda lime scrubber (annually) . 93
9.4.9 Replacement of halogen scrubber and membrane filter . 93
9.4.10 Supply of IC reagent . 94
9.4.11 Repositioning silicon tube in IC drain pinch valve (once a month) . 94
9.4.12 Replacement of ferrules in TC combustion tube outlet connector . 95
9.4.13 Washing or replacement ofTC combustion tube .95
9.4.14 Washing or replacing TC catalyst . 95
9.4.15 Replacement of high-sensitivity TC catalyst . 96
9.4.16 TC Blank Check . 96
9.5 MECHANICAL CHECK screen . 98
9.6 Consumable parts . 100
10 Principles of operation 101
10.1 Measurement of TC (Total Carbon) 101
10.2 Measurement of IC (Inorganic Carbon) 101
10.3 Measurement of TOC (Total Organic Carbon) 101
10.4 Measurement of NPOC (Non-purgeable Organic Carbon) 102
10.5 Electronic Signal Processing 102
10.6 Peak Area Measurement 102
10.7 Calibration Curve 103
10.7.1 One-point calibration curve 103
10.7.2 Multi-point calibration curve . 104
10.7.3 Shifting to origin . 104
10.7.4 Sparging process in measurement of standard solution . 105
10.8 Quantitative calculation . 106
10.9 Calculation of Mean Value, Standard Deviation and Coefficient of Variation . 106
10.10 Voiding abnormal values/performing additional measurement . 106
10.11 Automatic setting ofrange and injection volume . 107
10.12 Automatic selection of optimum calibration curve . 108
10.13 Automatic change ofrange and injection volume . 111
10.13.1 Automatic change of range . 111
10.13.2 Automatic change of injection volume .111
10.14 Measurement based on carbon equivalent . 112
10.15 Automatic regeneration of IC solution . 114
11 TROUBLESHOOTING 115
11.1 Error Messages . 115
11.2 Troubleshooting . 119
12 Specifications 123
Table of Figures
Figure 2.1 Outside Dimensions of TOC-SOOO . . 5
Figure 3.1 Gas Tubing for TOC-SOOO . . . . . . 9
Figure 4.1 Internal View of TOC-SOOO . . . . . .11
Figure 4.2 Filling TC Combustion Tube with Catalyst . .13
Figure 4.3 Combustion Tube/Swage Union Connection .14
Figure 4.4 TC Sample Injecting Block Assembly .15
Figure 4.S Positioning of 3-Way Cock .17
Figure 4.6 Plunger Holder Assembly . .19
Figure 5.1 TOC-SOOO Keypad . .21
Figure 6.1 INITIAL START Screen (Normal Start) .23
Figure 6.2 INITIAL START Screen (ALL RESET Start) .24
Figure 6.3 MAIN MENU Screen . . . . . . . . . . . . . .26
Figure 6.4 CALIBRATION/CONDITIONS Screen . . . .29
Figure 6.S MEASUREMENT START Screen (for CALIBRATION) .32
Figure 6.6 DATA PROCESSING STANDARD Screen . .34
Figure 6.7 CALIBRATION CURVE Screen . .37
Figure 6.8 SAMPLE MEASUREMENT/CONDITIONS Screen .39
Figure 6.9 MEASUREMENT START Screen (at Sample Measurement) .42
Figure 6.10 DATA PROCESSING SAMPLE Screen .. .44
Figure 6.11 GENERAL CONDITIONS Screen . . . . . .48
Figure 6.12 CALIBRATION CURVE FILE LIST Screen .51
Figure 6.13 DATA REPORT Screen . .54
Figure 6.14 MONITOR Screen . .57
Figure 6.15 STANDBY OPTIONS Screen .59
Figure 6.16 FINISH Screen . .59
Figure 6.17 RUNNING Screen . .59
Figure 6.18 MAINTENANCE Screen .. .62
Figure 9.1 Top Internal View of TOC-5000 .83
Figure 9.2 MAINTENANCE Screen . . . . .85
Figure 9.3 REGENERATION OF TC CATALYST Screen .86
Figure 9.4 Sample Injection Patterns . . . . . . . .91
Figure 9.5 Proper Positioning of Injection Needle .92
Figure 9.6 Halogen Scrubber . . . . . . . . .93
Figure 9.7 MECHANICAL CHECK Screen . . . .98
Figure 10.1 Peak Area Processing Method . . . . .103
Figure 10.2 Shifting Calibration Curve to Origin .104
Table of Tables
Table 2.1 Standard Accessories . . 3

Table 2.2 Optional Accessories , . . 4
Table 4.1 Microliter Syringe and Concentration Range .18
Table 9.1 Consumable Parts List . .100
Table 10.1 Absorption of C02 by Distilled Water . . . .105
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1 Introduction
Thank you for your purchase of the Shimadzu Total Organic Carbon Analyzer
TOC-5000/5050.
The TOC-5000 Analyzer Series measures the levels of total carbon (TC), inorganic
carbon (IC), total organic carbon (TOC) and non-purgeable organic carbon (NPOC)
in water. The measurement system is based on the combustion/non-dispersive infrared
gas analysis method widely employed for TOC measurement.
The advanced design of the TOC-5000/5050 Analyzer enables precision analysis and
convenient operation. However, to ensure trouble-free operation and accurate results,
it is strongly recommended that the operator refer closely to this manual and observe
proper laboratory procedures in preparing standards, samples and other materials.
Strict adherence to periodic maintenance will also playa significant role in ensuring
long-term satisfactory operation.
Note on the TOC·SOSO (Available only in U.S., Canada and Europe)

To enable smooth reading of the manual, all occurrences of the term "TOC-5000"
apply equally to the TOC-5050, except where specifically stated. The TOC-5050 is
recommended only for users not intending to routinely perform ultra-high sensitivity
analysis, i.e., below 300 - 500ppb.
In addition, any descriptions or procedures which do not apply to the TOC-5050 will
be identified with a "shaded" background, as follows:
-1
-2
2 Inspection
The TOC-SOOO shipping container consists of the TOC-SOOO main unit with a box
of standard accessories placed on a wooden pallet. After unpacking the containers,
confirm that all parts and standard accessories listed below are included in the
shipment.
(Note: Refer to Sec. 3.2 for proper unpacking procedure. Also, the packing
materials should be saved for possible transport of the instrument in the future.)
Table 2.1 Standard Accessories
Part Name Part No. Q'ty
Accessory kit (TOC-5000) for U.S. 638-90217-03 or

1
for Europe 638-90217-05
Accessory kit (TOC-5050) for U.S. 638-90217-02 or
for Europe 638-90217-04
[Brea kdown ]
1 Overflow cup 638-14305 1
2 Humidifier 638-52813 1
3 Soda lime scrubber (C02 absorber) 630-00999 1
4 Soda lime container holder 631-26482 1
5 Shaft 631-28177 1
6 Chart paper 630-08913 1
7 Connecting cable 071-60814-01
1
for Europe 071-60814-02
8 Combustion tube 631-41524

2
9 TC catalyst set 638-92069-01 1
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11 IC reagent 630-00710 1
12 IC reagent reservoir 630-02657 1
13 O-ring for adapter 036-11216 1
14 Microliter syringe, 250f,l1 630-02591-04 1
:·~~9[ql~ffit*¥~B§~~~~99~j··;!,§!:~~gft97.·:·
16 Half union, 5304, 1/8 CM4 035-55026-02 1
17 Template for LCD 631-51959 1
18 Plastic tube, 9 mm ID, 12 mm OD 630-00315-09 2m
19 Sparging tube pack 630-00337 1
20 Catalyst filling rod 638-16023 1
21 Cleaning wire, for needle 638-30002 1
22 O-ring (inj. slide) 036-11209 1
23 O-ring (inj. slide, Teflon) 036-11408 1
24 O-rin C port 630-01566 -00 1
-3
Part Name Part No. Q'ty
25 O-ring (IC vessel) 036-11222 1

26 Needle (sample injection) 630-01565 2
27 Plunger tip for 250!!1 630-02546-45 1
)7$.U~,wm«!tPfPt·g;~~eh).·.···)'63ffiU2S~;t4~;;
29 Flanged tube, O.5mm ID, 1.5mm 638-41269 1
OD, 400mm long
30 2N-hydrochloric acid 630-00998 1
31 Silicon grease (for high vacuum) 017-30812-01 1
32 Potassium hydrogen phthalate 25g 630-00635-01 1
33 Sodium carbonate 25g 630-00962-01 1
34 Sodium hydrogen carbonate 25g 630-00963-01 1
Instruction Manual M393-0085 1
Additional items are available as optional accessories, as listed in Table 2.2. These
items must be ordered separately.
Table 2.2 Optional Accessories
Part Name Part No. Remarks
Adsorption type gas purifier 638-52824-02
High purity air cylinder 630-00960

To be supplied by user in U.S.
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Plunger tip (3 pes. in a set) 638-60734-06 For 500ul microliter syringe
Plunger tip (3 pes. in a set) 638-60734-07

For l,OOOul microliter syringe
RS-232C interface (25P) 638-72376

For output to RS-232C
RS-232C interface (9P) 638-72376-01

For output to RS-232C (For IBM PC/AT
and compatible computers)
Optional board mounting kit 638-70292 Required for mounting RS-232C interface
-4
3 Installation
3.1 Installation site
3.1.1 Placement and space requirements
The TOe-5000 should be installed on a sturdy, level surface convenient to a

grounded power source of the appropriate voltage. An installation width of
approximately 1 meter is recommended for convenient operation and
maintenance. If the soda lime container holder is to be mounted (at rear of
instrument), at least 137 mm (5 in.) of space must be allowed beyond the rear
panel of the instrument. If space at the rear is limited, the soda lime may be
placed at the side of the instrument. The outside dimensions are as indicated in
Figure 2.1.
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About 80 mm
Figure 2.1 Outside Dimensions of TOG-5000
3.1.2 Environmental requirements

• Select an installation site which is free from corrosive or organic gas and
dust. For high sensitivity measurement in particular, contaminated
atmosphere may cause erroneous measurement.
• Ambient temperature must be stable. Do not install the instrument where
it will be exposed to direct sunlight, heat from a local heat source, drafts
from an air-conditioner, etc.
• Do not install the equipment where use of fire is prohibited.
• Do not install the instrument in the vicinity of strong magnetic or electric
fields or high frequency waves.
-5 -
3.2 Unpacking
1) After removing the shipping bands, lift off the cardboard container to reveal the
main unit and standard accessories box.
NOTE: Retain all shipping materials for future transport of the instrument.
Lift the TOC-SOOO main unit carefully from the pallet, taking care not to lift using
the door or putting pressure on the LCD screen.
NOTE: Two people should lift the unit.
2) Remove the 2 screws securing the top cover at the rear of the instrument. Then lift
off the top cover and remove the 2 Styrofoam blocks above the furnace.
3) Remove the plastic bag covering the sampling tube assembly which exits through
the door. At the same time, remove the outer Teflon tube covering the sampling
tube during transport. This outer Teflon tube (inner diam. 2mm, outer diam. 3mm)
is fitted over the sampling tube again when sparging is to be performed during
operation (see Sec. 8.4.2).
4) Remove the door fixing screw at the lower left below the door. After opening the
door, the door fixing bracket may be swiveled up to the side by loosening the screw
in the door rear panel, and secured in place by tightening the screw.
Remove one more Styrofoam block situated beneath the furnace, and the three
plastic bags covering the drain tube at lower right, the IC reservoir bottle cap and
the TC combustion tube union.
5) Remove the 2 screws which secure the LCD monitor unit. These are located at
about mid-height in the door rear panel, offset to the right and left. When these are
removed, the LCD unit may be tilted up and down.
3.3 Power Connection and Grounding
This instrument is preset to a specified source voltage before shipment according

to the power supply at the destination. The set voltage is indicated on the label
affixed at the lower right on the rear panel. Confirm that the source voltage to be
used corresponds with that indicated on label before connecting the power cord.
-6
NOTE: The power supply must be stable to ensure reliable operation. Unstable
voltage may adversely affect results in high-sensitivity measurement.
The power cord included in the standard accessories is equipped with a 3P

grounded connector. A 2P adapter connector is also provided with an attached
grounding wire.
NOTE: Complete grounding is essential not only for safety but also to protect
the logic circuit and microcomputer.
The TOC-SOOO is equipped with a thermal breaker instead of a fuse. A power

surge will activate the circuit breaker and cause the power switch to be turned off
automatically. Power may be supplied again by simply turning ON the power
switch. However, if the thermal breaker is frequently activated, preventive
measures should be taken to determine and eliminate the cause of the over-current.
3.4 Change of supply voltage
If the supply voltage is to be changed due to relocation or other reasons, it will be

necessary to change the wiring connection to the supply voltage-adjusting terminal
board and to modify the settings on the main board to conform to the new supply
voltage. In this case, contact your Shimadzu Service Representative.
3.5 Gas requirements
The TOC-SOOO requires air or oxygen as a carrier/combustion gas. The TOC is an

ultra-sensitive measuring device which absolutely requires a high quality
carrier/combustion gas to ensure accurate, reproducible data. The use of gases that
do not meet the specifications will result in poor data quality and, in severe cases,
prevent the instrument from coming to the "READY" condition.
The following minimum gas specifications must be observed:
Regular Sensitivity Catalyst Operation
C02 ~ 1.0ppm
CO :5 l.Oppm
THC* :5 l.Oppm (*total hydrocarbons)
-7
High Sensitivity Catalyst Operation
C02 s l.Oppm
CO s l.Oppm
THC* s O.lppm (*total hydrocarbons)
CAUTION:
To ensure that the carrier gas meets the above specifications, do not rely on
names such as "pure', "ultra-pure", "high purity", etc. A guaranteed analysis,
which most gas suppliers will provide, should be requested.
NOTE: Use of optional adsorption type gas purifier

The use of a 13x molecular sieve and ascarite filter additions with lower quality
gas is not recommended. Rapid deterioration of the purifier may occur depending
upon the levels and types of impurities and the amount of moisture in the gas. A
purifier may, however, be useful in high-sensitvity measurement.
I
~AUTION:
• Under no circumstances may untreated, compressed, atmospheric air be used as a
carrier/combustion gas for the TOC-SOOO.
3.6 Gas connection
Connect a two-stage pressure regulator to the carrier/combustion gas cylinder to

ensure stable gas supply to the instrument at about 8Spsi (6 kg/cm 2) [lOOpsi max.
2
(7 kg/cm max.)]. Clean copper, stainless steel (1/8" 0.0.) or the optional air
piping set may be used between the pressure regulator and the gas inlet at the rear
of the TOC-SOOO (see Fig. 3.1).
A half union connection adapter is provided as standard for connection using 1/8"
metal tubing. Quick-connect half unions for nylon tubing is also available.
Check for gas leakage

Open the gas cylinder valve and use Snoop, Leak-tee, etc. at all tubing and
regulator connections (outside the instrument) to check for gas leakage. All gas
leaks must be eliminated to prevent rapid depletion of carrier/combustion gas in
the cylinder.
·8
Pressure regulator Pressure regulator
(8S - lOOpsi) [2200psi min. (200kglcm 2 )
(6 7kglcm2)
Carrier/combustion gas
Air cylinder
1/8" (00)
tubing
o
00 I TOC-SOOO gas inlet
Figure 3.1 Gas Tubing for TOC-5000
NOTE:
Be sure to monitor the carrier/combustion gas cylinder pressure frequently, and
replace the cylinder when the pressure reaches 200psi to prevent moisture or
residues from passing into the TOC-SOOO.
3.7 Connection of drain tubing
Drainage is collected from the dehumidifier drain vessel, the IC reaction vessel
and from the rinse tubes for TC and IC into a single drain tube at the lower right
inside the instrument. Pass one end of the provided plastic tubing
(pIN 630-00315-09) through the round opening at the lower right side of the
instrument and fit it onto the unused "leg" of the Y-shaped drain collection tube.
Insert the external end of the drain tubing into an appropriate drain container
placed at a level lower than that of the instrument. Since the drainage may contain
acids, a polyethylene container with a capacity of 1 - 2 gallons (5 - 10 liters) is
recommended.
-9
- 10
4 Instrument preparation
Carrier gas_
flow meter
Microliter
syringe Humidifier
Dehumidifier
drain vessel
3-way valve
Figure 4.1 Internal View of TOG-SOOO
4.1 Filling dehumidifier drain vessel
1) Remove the cap of the plastic dehumidifier drain vessel secured by flexible
clasps in the instrument at the lower right (see Fig. 4.1).
2) Add water to the level of drain outlet (upper opening) on the wall of the vessel.
3) Cap the drain vessel and set it in its original position inside the flexible clasps.
- 11
4.2 Preparing humidifier
1) Fill the humidifier vessel (PIN 638-52813; shipped in standard accessories box)
with a .3N NaOH solution to the upper line through port on the side wall. For
high-sensitivity catalyst measurement, use water as low as possible in TC
content to prepare the solution.
2) Fit the reducing union of the Teflon tube labeled "L" (originating at carrier gas
flow meter and passing through opening at upper part of Toe-sooo internal
divider) onto the longer glass tube that extends into the humidifier vessel. Fit
the reducing union of the Teflon tube labeled "S" (from check valve on internal
divider) onto the other glass tube of the humidifier vessel.
3) Set the humidifier inside the flexible clasps mounted on the right side of the
TOC-5000 internal divider.
NOTE: Check the liquid level in the humidifier every 2 -3 weeks and supply
more purified water when necessary. The water level should never fall below
the lower line, nor should it be filled to above the upper line.
4.3 Preparing soda lime scrubber
1) Mount the soda lime scrubber holder (pIN 631-26482; shipped in standard
accessories box) with the 2 screws near the central lower part of the instrument
rear panel. (If there is insufficient space at the rear of the instrumen~ the soda
lime scrubber may be placed alongside the instrument withoUl the holder.)
2) Use a cutter to cut the ends of two tubes in the cap of the soda lime scrubber.
3) Fit the end of the flexible tube labeled "L" (passing through the opening at the
upper part of the rear panel) onto the tube in the soda lime cap which extends
into the container, and the tube labeled" S" ooto the other tube in the cap.
4) Place the soda lime scrubber in the mounted holder, taking care that the flexible
tubes are not pinched.
-12
4.4 Filling TC combustion tube with TC catalyst
Two kinds of catalyst are available for use with the TOC-SOOO, the TC catalyst for
regular sensitivity measurement (PIN 017-42801-01), standard accessory) and TC
catalyst for high-sensitivity measurement (PIN 630-00996-00), standard with
TOC-5000, optional with TOC-5050). Select the appropriate catalyst according to
the intended measurement referring to Sec. 8.3. ~.,
.... , .~
C\:t ,/,' i
Filling of TC Catalyst Filling of High-sensitivity TC Catalyst
D
TC combustion tube
(PIN 631-41524)
TC catalyst
(Alumina spherical support)
I
(PIN 017-42801-01) E High-sensitivity
E T
I
E
oC') E
...... (PIN 630-00996) oC')
..--l
Quartz wool
(PIN 630-00557)
Platinum screens (2) Platinum screens (2)

(PIN 630-00105-01)
Figure 4.2 Filling TC Combustion Tube with Catalyst
4.4.1 Procedure for regular sensitivity catalyst
Fill the TC combustion tube with TC catalyst as shown in Fig. 4.2. One full bottle
(20 grams) of TC catalyst is required for each combustion tube.
NOTE: When filling the tube, be sure that the catalyst is not contaminated with
foreign substances. Contamination of the catalyst may cause high blank values or
abnormal measurement.
- 13
4.4.2 Procedure for high-sensitivity catalyst
Fill the TC combustion tube with the high-sensitivity TC catalyst (pIN

638-92070-01) as shown in Fig. 4.2. Two cylinders of catalyst are required for
each TC combustion tube. Remove the caps from both ends of the cylinders.
Using the supplied catalyst filling rod, empty the contents of the catalyst container
into the TC combustion tube by pushing catalyst from the opening on one side of
the container into the combustion tube. Add the second cylinder, and then tamp
the catalyst to the proper level (130mm).
NOTE: Whenever the TC combustion tube is filled with new TC catalyst or

high sensitivity TC catalyst, execute the REGENERATION OF TC CATALYST
function in the MAINTENANCE screen once or twice (see Sec. 9.3.1).
4.5 Connecting TC combustion tube
1) Lift off the instrument top cover by removing the two screws on the rear panel.
2) Disconnect the sliding TC sample injecting block assembly above the TC

furnace by removing the 2 knurled thumb screws in the mounting plate. Shift
the disconnected assembly to the left side to gain access to the furnace.
3) Carefully insert the TC combustion tube (narrow tube portion first) into the
center opening in the furnace.
4)
*For the TOC-5050, connect the
tube projecting from the bottom
of the TC furnace to the elbow
connector attached to the Teflon
tubing.
- 14
CAUTIONS: .
.-: .:-:- .;:': -'.;.". . " " ........• " -: -:.:.' -:-:.;". '.:.;-:.~.~.:-:.: ~-: -:.:." ". ." '.". :-:-:-:.:-:-:.:-:.:::::-:.:.;. -,'. -,' .- .
'
~Pr()tecCiiiriei-and outer sudaces the combustion tube lower end, inner surface
of Swage lock fitting, ferrules and other gas contact surfaces from grease, oils
and other organic substances, particularly when high-sensitivity measurement is
conducted.
6) Apply a thin coat of the supplied high vacuum silicon grease on the outer
surface of the combustion tube upper end, and fit the TC port (with O-ring) of
the sliding TC sample injecting block assembly onto the coated upper end of the
combustion tube. Align the sample injecting block assembly and re-mount it
using the screws, but do not fully tighten the screws yet.
drain tube slider sample injection needle
sample injecting block
Figure 4.4 Te Sample Injecting Block

Assembly
.:.; ... :. ..;....... ..' .... ": :-:::.;.;.;:;):-:-:.:.:-: ......
- 15
8) Finally, tighten the screws to securely mount the sample injecting block
assembly (see Fig. 4.4).
NOTE: Take care not to exert downward force on the slider, adversely affecting
the airtightness between the slider and O-ring in the sample injecting block.
4.6 Loading chart paper in printer
1) Open the printer cover on the top of the TOe-SOOo and set a chart paper roll
(with shaft (PIN 631-28177) inserted through roll) in the chart paper holder.
The ends of the shaft should be seated in the lateral slots of the chart paper
holder. The roll must be mounted so that the paper will feed from below the roll.
2) Fold or cut the leading edge of the paper on a slant and guide it forward under
the paper feed roller of the printer. Turn ON the power switch and press the
I FEED I key to feed the paper into the printer until the leading edge emerges from
the printer cutter section.
3) Correct the paper alignment if necessary. Then turn OFF the power switch.
NOTE:
The appearance of a red streak along the edge of the chart paper indicates that
the paper roll is nearly used up. Since a single roll contains 40m of chart paper,
the paper will last about 14 days with a daily paper consumption of 2.Sm.
CAUTION: Do not actuate the printer without properly setting the chart paper.
Operating the printer without chart paper will damage the printer head.
- 16
4.7 Preparing Ie reagent reservoir
1) Set the IC reagent overflow cup on the floor inside the front door of the
instrument, so that the 2 projections on the bottom of the cup fit into the
corresponding holes in the floor.
2) Fill the IC reagent reservoir bottle (pIN 630-02657) with 120 - 130ml of the
provided IC reagent (PIN 630-00710).
3) Carefully apply a small amount of the provided silicon grease to the O-ring on
the adapter inside the cap of the IC reagent reservoir bottle, preventing any
grease from contacting other parts. The IC reagent reservoir bottle adapter is
pre-connected to 2 tubes, a black IC reagent carrier gas tube and a thin plastic
tube leading up to the IC reagent vessel. Confirm that these tubes are snug in
the adapter, and then securely screw the cap on the IC reagent reservoir bOLlle.
The thin plastic tube should reach to the bottom of the IC reagent reservoir
bottle.
4) Place the IC reagent reservoir bottle in the IC reagent overflow cup.
4.8 Preparing Ie reaction vessel

1) Dismount the IC reaction vessel (see Fig. 4.1) by first removing the 2 screws
securing the IC reaction vessel bracket below the vessel. Then, holding the main
body of the vessel, twist the vessel while pulling downward until it comes loose
from the injection block above it. Take care not to apply pressure to the plastic
tubes attached to the vessel
2) Position the 3-way cock as shown in B of
Figure 4.5, and confirm that it is securely
connected to the IC reaction vessel.
3) Fill the vessel with purified water (or
deionized water) up to the drain tube on the
right wall of the vessel.
A B
4) Apply a very thin coat of grease on the
outer surface of the upper part of the

Figure 4.5 Positioning of
vessel, and insert the upper part of the 3-Way Cock
vessel back into the sliding IC sample
injection block.
5) Remount the IC reaction vessel bracket below the vessel and position the 3-way
cock as shown in A of Figure 4.5
-17
4.9 Mounting microliter syringe
<~J•. ~ D:I• •11•. ~r

. :: :
. t)..i.~ .•tilr~tll.l.t.~.?.r.i.•~;.J~.i .iI.1
::.:::::::~::.::
a. •nm
.••. ·:•.•:.Q:i.]
.•.
:.:.:.:-:.:.:-:- "." :.:.:.:...:.:-:.;.:.;.:.:.;.;
U @
•.•
.. •j.
Size Plunger tip Injection TC Concentration IC Concentration

Part No.
(f!l) PIN volume (f!l) range range
250 630-02591-04 630-60734-05 4 - 250 100ppb - 4000ppm 100ppb - 5000ppm
l;;=l;j=_=i=II~:·I=III:·
• • ~.Qq • • :19il~g~~I • · ·• :§~IQ11~ip~: • ·.;'·:::.::~::B'ga;,·.: • • . ::::.::.:.:.·~m~PID:.:I~*~.:.: • • • · • •·• ·.:• .••j·.,_p@m~~~ • • :.·• • • ·

Table 4.1 Microliter Syringe and Concentration Range
NOTE: The TOC-SOOO employs a Type C (threaded) fitting on the syringe.

Only this type of syringe fitting may be used.
Procedure
1) Washing: The syringe must be washed thoroughly before mounting. To wash

the syringe, pump the plunger 10 - 20 times with the end of the syringe
immersed in acid (such as the provided 2N HCl) or in quality soap or detergent
for laboratory glassware. Then rinse the syringe thoroughly using running water
and finally purified water (or deionized water, or reverse osmosis water).
2) Confirm that the instrument is OFF. Lower the plunger holder assembly (see
Fig. 4.6) manually to its lowest position. Remove the plunger holder assembly
from the injector by unscrewing the black knob.
3) Unscrew the plunger holder cap (used to secure the plunger head in the plunger
holder). Pass the microliter syringe plunger through the plunger holder cap
(from the threaded side). Replace the plunger holder cap onto the plunger
holder assembly.
4) Working the plunger, draw purified water into the microliter syringe,
confirming the absence of bubbles in the syringe near the plunger tip.
-18
Sparging
connector
Sampling tube
Microliter
syringe
Plunger holder
assembly
Figure 4.6 Plunger Holder Assembly
5) Reposition the plunger holder assembly onto the injector assembly. Do not
tighten the black knob yet.
6) Manually raise the assembly until the microliter syringe can be screwed to the
4-port valve. Hand-tighten the syringe fitting to secure the syringe. Do not
over-tighten. Take care not to lower the plunger causing air to enter the syringe.
NOTE: At this time, confirm that the plunger holder assembly is properly
aligned. If necessary, re-align the plunger holder assembly, and re-tighten the
black securing knob.
7) Pass the end of the sampling tube through the opening in the front door and
close the front door. Place a beaker of purified water on the sample platform
mounted on the front door and immerse the end of the sampling lube in the
purified water.
8) Turn the TOe-5000 on using the power switch on the lower righl side of lhe
instrument.
- 19
NOTE:
If leakage is ever noticed at the line connections of the 4-port valve, the cause
may be a severely clogged injection needle or tubing leading to the needle.
Check the condition of the injection needle, referring to Sec. 9.4.7, and clean or
replace the injection needle as required. DO NOT USE A TOOL TO
TIGHTEN THE CONNECTIONS AT THE 4-PORT VALVE IN CASE OF
LEAKAGE. This will damage the 4-port valve, requiring replacement. These
connectors must be hand-tightened only.
·20
r 5 Keypad and LCD unit
ENTER
Figure 5.1 TOC-5000 Keypad
r
5.1 Key functions
1) ISTART/STOP I key
The ISTART/STOP I key is used to start and stop measurement.
2) F1 - F6 keys
The "function keys" are used to perform functions indicated at the bottom of
the LCD screen, with the functions varying from screen to screen. When a
function key is indicated in this manual, it will be shown as the function
designation (as named on the LCD screen) enclosed in a double box.
For example, "press the NU key" requires the operator to press the
appropriate function key (Fl - F6) corresponding to the designation at the
bottom of the LCD screen.
NOTE: A function key template (PIN 631-51959) is provided to facilitate

identification of the appropriate function key number. This template should be
affixed to the TOC unit below the LCD screen when the instrument is turned ON
so that the keys on the template correspond to those shown on the screen.
- 21
3) []] OJ EJ Bkeys
The "cursor keys" are used to move the screen cursor to a desired position, so
that parameters may be selected, inserted or changed
4) [Q] - [}] keys

The "numeric keys" are used to input numeric values. They can also be used to
bring the cursor directly to a menu item instead of using the cursor keys, and to
select among parameters for setting conditions.
5) I ENTER I key
The I ENTER I key is used to validate an entry or a selected condition.
NOTE: When entering values, it is necessary to press I ENTER I to validate each

entry. After keying in a value, use of the cursor keys will move the cursor in the
indicated direction, however, the keyed-in entry will not become valid.
6) ICE!key
The ICE I key is used to clear or delete a key entry which has not yet been
validated using the I ENTER I key.
7) I FEED I key
The IFEED I key is used to feed the chart paper through the printer. Chart paper
continues to be fed as long as the I FEED I key is depressed.
5.2 LCD unit
The LCD unit employs a high contrast backlit screen with 640 x 400 dots. The
unit itself may be rotated vertically about 10° for adjustment of the viewing angle.
Contrast and brightness adjustment

Contrast and brighness of the image are adjusted for optimum viewing before
shipment, however, these may be adjusted via the 2 adjustment screws recessed in
the 2 small holes at the right of the LCD unit. The upper screw adjusts the
brightness of the backlight, while the lower screw adjusts the image contrast.
NOTE: Operation under extreme ambient temperatures may cause deterioration

of the image display, but this is remedied with return to normal ambient
temperature.
Protect the plastic-coated LCD screen from damage by preventing contact with
organic solvents and sharp-pointed objects.
- 22
6 Screen displays and functions
The TOC-SOOO operation is controlled through the various screens on the LCD.
These screens and their associated functions will be introduced in this chapter.
In general, functions are carried out using the keys on the keypad as described in
the previous chapter. All items listed in the various screens may be selected for
their respective functions, except those function keys which display "*,, before
their indicated function. These functions are "locked out" while the * is displayed.
6.1 INITIAL START screen (Normal Start)
INITIAL 8TART 06(JUN)-22-1989 2l: 26 6
2 1 - - + - - - - - - - - - - - TOC-5000
~_ _- - - - - - - - VERSION 2.00
3
r INITlALIZING
4 TC FURNACE OFF
Copr.1989 Shimadzu Corporation

IND
Figure 6.1 INITIAL START Screen (Normal Start)
When the instrument is turned on using the power switch alone, the screen
appears as shown above. In this case, all previously stored calibration files, date
and time settings and syringe zero point remain valid.
- 23
6.2 INITIAL START screen (ALL RESET Start)
INITIAL START 00(**)-00-0000 00: 00

RAM OK
ROM OK
TOC-SooO
VERSION 2.00
8 1 - + - - - - - - - - - - - - - - ALL RESET
TC FURN ACE OFF
FIND SYRINGE ZERO POINT ON "MAINTENA~CE" DfSPLAY (#8)
9 \---1-------{
LSF:T DATF: & TIMF: ON "MAINTENANCE" DISPLAY (#8)
Copr. 1989 Shimadzu Corporation

11-:1
Figure 6.2 INITIAL START Screen (ALL RESET Start)
When the instrument Power Switch is turned ON while the I ENTER I key is
depressed or if there is an abnormality detected in the RAM memory, lhe
TOC-5000 slarts up in the ALL RESET mode. In this case, all previously stored
calibration files, date and lime settings and syringe zero point are deleted from
memory (RAM) and must be reset.
1) Screen item descriptions
1. Screen title "INITIAL START" is displayed.
2. Instrument model name is displayed.
3. Version number of ROM is displayed.
4. The syringe pump and other mechanical components move to their

"home positions". During this process, the message "INITIALIZING" is
displayed, and when the entire process is completed, lhe message
"INITIALIZED" is displayed.
5. The READY message indicates that the temperature of the TC

furnace and electric dehumidifier, and the position, fluctuation and noise
- 24
r
conditions of the baseline have all met the preset conditions for
measurement (warm-up is completed). "WARMING UP" is displayed
during the period prior to the display of "READY",
If the TC furnace is not turned on, "TC FURNACE OFF" is displayed.
6. Date and hour are displayed. When the operation starts in the ALL
RESET mode, all displayed digits are 0 (zero).
7. Results of the RAM and ROM check are displayed. If an error

is found, either RAM ERROR or ROM ERROR is displayed, and other
messages are cleared form the screen.
8. Indicates ALL RESET condition, (reset has been performed).
9. Messages:
FIND SYRINGE ZERO POINT ON "MAINTENANCE" DISPLAY (#8)
SET DATE & TIME ON "MAINTENANCE" DISPLAY (#8)
Select MAINTENANCE on the MAIN MENU screen. Carry out zero
point detection of the microliter syringe and set the date and time as
described in Sec. 7.4, 7.5.
r
2) Operations
Purpose Key Operation Function

Proceed to next Press I NEXT II Proceeds to MAIN MENU. Carry out any
step. operations indicated in ALL RESET screen.
3) NOTE
When the instrument is turned ON, the date and time it was last turned OFF are
printed oul along with the current date and time.
- 25
6.3 MAIN MENU screen
MAIN MENU <GENERAL CONDlTIONS~
l--f--[!] CALIBRATION TC CATALYST : NOR!vlAL SENS
1-=-1--- 2 SAMPLE MEASUREMENT SYR SIZE ; 25Dtll
~I--- 3 GENERAL CONDITIONS NO OF WASHES: 4

9
~-f--- 4 CALIBRATION CURVE FILE LIST UNIT : ppm
;--1--- 5 DATA REPORT AUTO RANGE ; ON
~-f--- 6 MONITOR
AUTO Ie REGF:N: ON
~I--- 7 flTANDBY OPTIONS AUTO PRINT : 01")0'
~-f--- 8 MAINTJ::NANCE TC FURN ACE ; OFF
RUZZER : USED
MOVE CURSOR TO ITEM OR I:\,PUT ITEMl: THEN PRESS [ENTER1----t-.. IO
-daMume
Figure 6.3 MAIN MENU Screen
Almost all operation procedures are initiated from the MAIN MENU screen.
1. CALIBRATION: Select to begin procedure for creating calibration

curve(s).
2. SAMPLE MEASUREMENT: Select to begin sample measurement

procedure.
3. GENERAL CONDITIONS: Select to set general conditions for
measurement.
4. CALIBRATION CURVE FILE LIST: Displays list of stored
calibration curves.
5. DATA REPORT: Displays up to 99 consecutive sample measurement

results.
6. MONITOR: Displays instrument range, real time analog signal of

NDIR, temperatures of TC furnace and electronic dehumidifier, and
- 26
r gives information on baseline conditions (i.e. position, fluctuation and
noise).
. 7. STANDBY OPTIONS: Used to specify manual shut-down of operation

or programmed restart from "RUNNING" standby state.
8. MAINTENANCE: Enables selecting various functions and operations
associated with maintenance and service of the instrument.
9. GENERAL CONDITIONS: Current General Condition settings are
displayed for monitoring. Confirm that they are set appropriately.
(SYR SIZE not listed for the TOC-SOSO)
10. Messages
MOVE CURSOR TO ITEM OR INPUT ITEM#

THEN PRESS [ENTER]
An item may be designated by either moving the cursor to the item
using the cursor keys or by inputting the item number via the numeric
keys. The operation is then initiated by pressing the IENTER I key.
When the instrument is turned on in the ALL RESET mode (see Sec.
6.2) the following messages are displayed.
FIND SYRINGE ZERO POINT ON "MAINTENANCE" DISPLAY (#8)

SET DATE & TIME ON "MAINTENANCE" DISPLAY (#8)
Select MAINTENANCE (#8) and carry out zero point detection of the
microliter syringe, and set the date and time as described in Sec. 7.2,
7.3.
2) Operations
When operation is started normally
Select an item. Press IENTER Iafter Proceeds to screen indicated by item

specifying item with cursor selected.
keys or numeric key.
Return to INITIAL Press IIRETIJRN II. Returns to INITIAL START screen.

START screen.
- 27
When operation is started in ALL RESET mode
Go to GENERAL Press IENTER Iafter Proceeds to GENERAL CONDITIONS

CONDITIONS specifying #3 with cursor screen. Return to MAIN MENU after setting
screen. keys or inputting [}] . conditions appropriately.
Go to Press IENTER Iafter Proceeds to MAINTENANCE screen. Carry

MAINTENANCE specifying #8 with cursor out zero point detection of syringe pump and
screen. keys or inputting [I] . set date and time.
Select an item Press IENTER Iafter Proceeds to screen indicated by item

specifying item with cursor selected.
keys or numeric key.
Return to INITIAL Press Ii RETURN II· Returns to INITIAL START screen.

START screen
3) NOTES and CAUTIONS
1. NOTE:
Items #1 CALIBRATION and #2 SAMPLE MEASUREMENT cannot
be designated when operation is started in the ALL RESET mode
(number in # column is not displayed). These operations can be
executed only after setting the microliter syringe size in the GENERAL
CONDITIONS screen and performing zero point detection in the
MAINTENANCE screen.
2. CAUTION:
Be absolutely certain that the settings for TC catalyst and/or microliter
syringe size correspond to those items actually used in the instrument.
A discrepancy will not only prevent accurate measurement but may
cause error messages to be displayed or cause damage to the TC
combustion tube and other nearby parts when the instrument is in use.
- 28
r 6.4 CALffiRATION/CONDITIONS screen
CALIBRAT10N I CONDlTIOl\S <( GENERAL CONDITIONS ~
CAL CURVE F# , 6(SEl:: CAL FILE STATUS) TC CATALYST:NORMALSENS

}-=----1I--TYPE I (l ~TC 2~JC) SYR SI7.E : 250td
Itlt STO CONC :IIOO,olppm NO OF WASHES: 4
2nd STD CONC : - p p m UNIT :lJlJm 9
3rd STO CONC : _ppm AUTO RANGE :ON
lh STO CONC : . . - ppm AUTO IC REGEN: ON
HANGE : x5 (xl x5 x30) AUTO PRI:-.JT :OFF
>-=-_~INJ VOL 20ttl (8-100)

TC FURNACE :ON
\----J----t~0 OF INJECTS: I (1-10) BUZZEH :USED
,-=,-_t-MAX NO OF INJ: 1 (1-10)
SD <( CALlRRATION FILE STATUS~
CV ~I:PROTECT #10: FREE
SPARGE TIME: Omin(O-20) #2: PHOTECT '11: FREE
8 '3: PROTECT ~12: FREE
#4: PROTECT #I:! : FREE 10
#5: STORED #14: FREE
#6: FREE #15: FREE
17: FREE #16: FREE
#8: FREE #11: FREE
#9: FREE #Ill: FREE
1"Dt;' Bbi'''ZIIN'' IjBIOI
Figure 6.4 CALIBRATION/CONDITIONS Screen

r
This screen, which appears when item #1 CALIBRAnON is selected in the
MAIN MENU screen, allows setting of the conditions to be used in creating
calibration curves for standard solutions. Currently set general conditions and
stored calibration curve files are also displayed for monitoring.
1. CAL CURVE F#:

This is used to designate a calibration curve file number. When the
screen first appears, the number of the first available "FREE" file will
be pre-selected to allow creation of a new calibration curve. However,
any FREE number may be selected to create a new curve. Selection of
a stored curve is carried out by moving the cursor to
CAL CURVE F#, inputting the number of the appropriate calibration
curve file and pressing IENTER I .
Up to 18 calibration curves may be stored and listed for display. When

a "STORED" file number is selected, all of the other settings in this
screen may be modified directly, but if a "PROTECT" file is selected,
r none of the settings may be changed unless the PROTECT status is
- 29
removed in the CALIBRATION CURVE FILE LIST screen (see Sec.
6.12) accessed from the MAIN MENU.
2. TYPE: Designate TC or Ie. TC calibration curve should be used for

NPOC measurement.
3. STD CONC: This sets the standard solution concentration(s). Up to

four concentrations may be set for corresponding standard solutions
(4-point calibration). The setting range for concentration depends on the
microliter syringe used, according to the values listed in Table 4.1. (P18)
4. RANGE: This sets the NDIR range. A suggested value (and possible
settings) will be displayed automatically as soon as the value is entered
for SID CONC, described above.
5. INJ VOL: This sets the injection volume. A suggested value (and
setting range) will be displayed automatically as soon as the value is
entered for STD CONC, described above. These will be based on the
settings made for the microliter syringe and TC catalyst in the
GENERAL CONDITIONS screen.
6. NO OF INJECTS: This sets the number of repeat measurements to be

carried for a single standard solution.
7. MAX NO OF INJ: The maximum number of injections is
automatically set to the same value as that entered for NO OF
INJECTS, described above.
Setting a higher value will allow additional injections to be performed

should the initial injections generate abnormal results (tailing, outliers,
etc.). Furthermore, when a higher value is set, suggested values for SD
(standard deviation) as an area count and CV (coefficient of variation)
will be displayed. These values may be changed if desired. Additional
injections will then be performed if these parameters are not met. The
TOC-SOOO will then select the most appropriate values for the
averagmg.
8. SPARGE TIME: This sets the sparging time when spargmg is to be
performed on standard solutions.
9. GENERAL CONDITIONS: Current General Condition settings are

displayed. Confirm that they are set appropriately. (SYR SIZE does not
appear on the TOe-5050)
- 30
r 10. CALIBRATION FILE STATUS: This is a listing of the 18 storage
files and their status, identified by number. The "STORED" status
refers to a calibration curve which may be recalled and modified. The
"PROTECT" status refers to a calibration curve which may be recalled,
but may not be modified unless the PROTECT status is removed in
the CALIBRATION CURVE FILE LIST screen accessed from the
MAIN MENU.
11. Messages
*GENERAL CONDITION MISMATCH TC CAT (or SYR SIZE,

UNIT, NO OF WASHES)
The General Condition settings do not correspond with the calibration
settings. Modify the settings ill the GENERAL CONDITIONS screen or
in CALIBRATION/CONDITIONS screen so that they correspond
appropriately.
*CONCENTRATION IS TOO HIGH

The concentration set for the standard solution exceeds the instrument
range. Change the setting appropriately.
2) Operations

Set conditions. Press IENTER Iafter Sets all calibration conditions. Values are
inputting value with suggested for NDIR range and injection
numeric key. volume on basis of concentration value set.
Print Press I PRINT II· Prints out calibration/ conditions.
Proceed to next
step.
Press II NEXT i. Proceeds to MEASUREMENT START
screen.
Return to MAIN Press i MAIN MENU II. Returns to MAIN MENU screen.
MENU screen.
3) NOTES and CAUTIONS
1. It is necessary to press IENTER I after inputting each value In order to

validate the new value.
- 31
6.5 MEASUREMENT START screen (for Calibration)
MEASUREMENT START
SET 1st STANDARD VESSEL

INSERT SAMPLI:'-lG TUBE
PRESS [START] -
-8""'D
Figure 6.5 MEASUREMENT START Screen (for CALIBRATION)
This screen appears when the [I NEXT II key is pressed in the CALIBRATION/
CONDITIONS screen.
1) Messages
SET 1st STANDARD VESSEL
INSERT SAMPLING TUBE
PRESS START
Place the vessel containing the 1st standard solution on the sample
platform, insert the sipper and press the ISTART/STOP I key to initiate
measurement.
STANDARD CONC OF PREVIOUS DISPLAY IS NOT YET SET

Set concentration value(s) for standard solution(s) in CALIBRATION/
CONDITIONS screen.
FIND SYRINGE ZERO POINT DETECTION ON

MAINTENANCE SCREEN (#8)
Select MAINTENANCE (#8) from MAIN MENU and carry out zero
point detection of the microliter syringe.
- 32
r *GO TO "MONITOR" DISPLAY (#6) TO SEE READY STATE
This appears if the ISTART/STOP I key is pressed when the instrument
has not yet attained the READY state. When the READY state
conditions are satisfied, the instrument will automatically continue with
the specified analysis.
2) Operations
Start measurement Press ISTART/STOP I Starts measurement.
Return to At start of calibration for Returns to CALIBRATION/CONDITIONS

CALIBRATION/ 1st standard solution, screen
CONDITIONS press II STD CO ND JI·
screen
At start of calibration for
2nd - 4th standard solution:
II 1st START II Returns to MEASUREMENT START
~ screen for 1st standard solution.
IISTDCOND~ Returns to CALIBRATION/CONDITIONS
screen
r
3) NOTES
Use the sparging tube when SPARGE TIME has been set.
·33·
6.6 DATA PROCESSING STANDARD screen
DATA pnOCESSING 1st STANDARD CAL FILE # 1

0{
1 TC. 80.0ppro. I~J VOL 25/Ll. RANGE "5
f- NO OF INJECTS 3/ 3(max5), SPARGE TIME 0 min
I:'JJ#AREA
ill
'1:7727
2 COMPLETED 2 '1:7958
3 '1:7839
100%
MN 2784J
o SD 115
2 CV 0.41 %
INJ#I 3
5\--1---- PRESS [START] FOR REINJECTION. IF NECESSARY
",c. @l1.IUII. lEi_tiM MIII18 'emINW'NII
Figure 6.6 DATA PROCESSING STANDARD Screen
This screen appears when the ISTART/STOP I key is pressed to initiate measurement
of a standard solution in the MEASUREMENT START screen during calibration.
The progress of the measurement sequence is displayed in real time.
1. The measurement conditions set in the CALIBRATION/CONDITIONS
screen are displayed. The NO OF INJECfS (measurement repetitions) is
updated after each injection during the measurement sequence.
2. The progress of the measurement sequence is displayed as follows:
SPARGING XX min to end: Displayed when SPARGE TIME is set
WASHING : Washing of the microliter syringe with sample
SAMPLING : Aliquot of standard is drawn for injection
INJECfING : Injection of stwldard
MEASURING: Peak detection and area measurement
WAITING: 1) Standby due to unsatisfied measurement conditions
(READY STATE SENS)

2) Displayed when ISTART/STOP I key is depressed during
SPARGING, WASHING, or SAMPLING
COMPLETED: Measurement sequence completed
(continued)
- 34
MEASURING/WASHING: Washing for next injection starts during
peak processing
3. The peak is displayed with time (min) as the horizontal axis. When the
measurement repetitions are completed, the sequence is ended and the
time axis is marked.
4. Injection No. (INJ#) and peak area (AREA) are displayed. The mean
value (MN), standard deviation (SD) and coefficient of variation (CV)
are calculated on the basis of the peak area data.
5. Message
PRESS [START] FOR REINJECTION, IF NECESSARY

Press ISTART/STOP I if additional measurement is desired. When
REINJECTION is carried out, time is not displayed.
2) Operations
Purpose Operation Function
Delete/retrieve Bring cursor to appropriate "-" displayed at deleted lNJ#, and MN, SD
measured value. lNJ# and press IENTER I. and CV values are recalculated.
Additional meas Press ISTART/STOP I Additional measurement is performed and

urement when COMPLETED is dis measurement value is displayed with "+" at
played. right of INJ#.
Change conditions Press II STD COND II and Changeable parameters include NO OF IN-
during measure- change value(s) in JECTS, MAX NO OF INJ, SD, CV. STD
ment. CALIBRATION/ CONDI- CONC may be set if not yet set and if value
TlONS screen, then press will be less than those already sel.
[I RETURN lito return to this
screen.
Interrupt ISTART/STOP I WAITING is displayed. During WASHING

measurement or SAMPLING, standby state is entered
(Following function after syringe moves to zero point or just
keys activated) after sample sipping is completed. During
MEASURING, peak processing executed
without entering standby state.
~ IIESCAPEII Returns to MEASUREMENT START

screen. Data is lost. (See NOTE 3 next page)
f-- TINUEII Standby cancelled, measurement continues.
Available only during "MEASURING", this

1_[1 PEAK STOP ij terminates measurement of peak area and
displays incomplete results up that point.
- 35
Magnify plot Zooms in on 25% of the plot by height

II EXP SCALE I]
display (0 - 25% F.S.)
1
II STD SCALE II Scale returned to normal (0 - 100% F.S.)
Print IlpRINT!
I~:IJOWing function
t
keys activated)
IIALL PRINT II Entire screen printed out
Data only printed out (without plot)

IDATA PRINT!
- II PEAK PRINTI] Peak only printed out
~ NO PRINT ~ Print cancelled
Return to MAIN Press 11 MAIN MENU II· Returns to MAIN MENU screen. (Only
MENU screen. GENERAL CONDITIONS, MONITOR
items available). To proceed, return to
DATA PROCESSING STANDARD screen.
Proceed to next Press [I NEXT II after Proceeds to CALIBRATION CURVE

step. "COMPLETED" displayed. screen or when standards remain, returns to
MEASUREMENT START screen.
3) NOTES
1. If a record of results is required, be sure to designate printout In

advance (in the GENERAL CONDITIONS screen) or in this screen by
selecting I PRINT II before using I~!I or I END I~ It is not possible to
return to the current screen after proceeding to the next step.
3. To interrupt measurement of the 2nd - 4th standard solution in

generating a multiple point calibration curve, perform as follows:
Press ISTART/STOP I to bring up MEASUREMENT START screen for
2nd - 4th standard solution.
Press [115t SID I] to bring up MEASUREMENT START screen for
1st standard solution
Press II STD COND II to bring up CALIBRATION/CONDITIONS screen.
Note that all measured data for generating the calibration curve is lost.
- 36
r 6.7 CALIBRATION CURVE screen
CALIBRATIO:--J CURVE # I
TC l-POINT SHIFT TO ORIGIN: [2] (l=YES. 2=NO) 2
FILE NOT PROTECTED PROTECT : 2 (l=YES, 2=NO)
3
r CONDITIONSl I
~784l , - - - - - - - - - -.....
TC CATALYST : NORMAL SE1\S '
INJ VOL/SYR SIZE: 25/250ul
RANGE : x5 4
SP ARG E TIJI,1E : a min
NO OF WASHES : 4
PEAK DATE : OG(JUN)-22-1989
AREA
[ DATA]
S'l'D CONC AHEA #lNJ SD CV
SO.Oppm 27841 3 115 0.41%
TC [ppm] SO.O
PHINT
Figure 6.7 CALIBRATION CURVE Screen
i
This screen appears when the NEXT II key is pressed in the DATA PROCESSING
STANDARD screen after all of the standard solutions have been measured. Here,
creation of the calibration curve is carried out on the basis of the measurement
values obtained in the pATA PROCESSING STANDARD screen.
1. The calibration curve, created on the basis of 1 - 4 measurement

values, is displayed here along with the file number.
2. If YES is designated, the calibration curve is shifted down vertically so

that it passes through the anglO.
3. If YES is designated, the calibration curve is stored as a "PROTECT"

file (see Sec. 6.4) 1), and the file status displayed at the upper left
changes to "FILE PROTECTED".
4. The relevant condition settings are displayed.
r 5. The measurement results for each standard solution are listed, including
the values of mean area count, # of replicates, SO, and CV).
- 37
6. Message
*FAILED CALIBRATION NO CAL CURVE WAS MADE

If the measurement values of a standard solution produce a calibration
curve of abnormal slope, the calibration curve will not be created.
Verify that the appropriate standard solution is being used, or that the
solution was not erroneously prepared.
2) Operations
Shift curve through PressOJ and then Shifts calibration curve vertically to pass
origin IENTERI through origin (see Sec. 10.7.3).
"PROTECT" file PressOJ and then A PROTECTed calibration curve cannot be

IENTER I modified unless its status is changed, but it
will be deleted if the instrument is started in
the ALL RESET mode.
Remove measure II,

Press II VOID move cur The designated measurement value is
ment value from sor to value to be removed, removed from consideration in creating
calibration curve.
Dr~l~~then calibration curve. A "-" will appear next to
the removed value.
IfVOID E .
Reinstate voided II,

Press II VOID move The value removed using the VOID function
measurement value. cursor to value to be will be reinstated in the calibration curve ca]
I
reinstated, press ENTER l culation.
then !IVOID EXIT~.
Proceed to next step
• Create another Press [ISTANDARDII . Returns to CALIBRATION/CONDITIONS
calibration curve screen.
• End calibration Press I MAIN MENU II· Returns to MAIN MENU screen.
curve creation
Print screen Press I PRINT II· Prints out all data with calibration curve.
3) NOTE
is used to cancel unwanted measurement values for the

II VOID II
multi-point calibration curve. An error in standard solution preparation
or in setting of concentration value in the CALIBRATION/
CONDITIONS screen, etc. could cause a measurement value to be
offset linearly from the other points in a calibration curve. Such a
measurement value may be removed from the calibration curve
following the procedure outlined in the Operations description above.
Upon completion of the procedure, a new calibration curve is created
on the basis of the remaining measurement values.
- 38
6.8 SAMPLE MEASUREMENT/CONDITIONS screen
SAMPLE MEASUHEMENT 1 CONDITIONS <{CALIBRATION CUHVE FILE LIST}>

FI TYP HIGH CONC INJ/SYRu.l RG CAT
SAMPLE# : 1 TC 80.0 ppm 25/250 5NOHM
TC IC NPOC 2 TC 400.0 ppm 30/250 30NORM 11
2 3 TC 20.0 ppm 20/250 1NORM
1st CAL CURVE# 1 **[!!) 4 TC 240.0 ppm 11/250 5NORM
2nd CAL CURVE# 2 5 TC 240.0 ppm 11/250 5 NORMNE
3rd CAL CURVE# 3
**
** **
RANGE(XI )(5 )(30) 5 0
**o
_ ~ __- INJ VOL u.l 25 50 50
SPARGE TIME min -- I
NO' OF WASHES 4 1
DlL FACTOR 1 1
NO OF INJECTS 3 1
MAX NO OF INJ 4 1
10 SD 100
CV % I. a
MUMi IMMII·liMl. PHiNT
Figure 6.8 SAMPLE MEASUREMENT/CONDITIONS Screen
This screen appears when item #2 SAMPLE MEASUREMENT is selected in the

MAIN MENU screen, usually after the calibration procedure is completed.
1. SAMPLE#
This is for setting the sample number for the current analysis. The
number displayed when the screen appears is the next available number
in the DATA REPORT screen. If the number entered corresponds to
one already associated with data, the new measurement data will
overwrite the previous data at that sample number. A number up to
"120" may be entered.
2. TC, IC, NPOC

These are the types of measurement for which each of the following
conditions may be seL
3. CAL CURVE#
Up to three calibration curves may be designated for each of the three
types of measurement (fC, IC, NPOC). Measurement is first per.formed
using the first (1st) calibration curve. If this curve does not provide
- 39
appropriate results, either the second or third curve will be selected and
the analysis will be performed again. Measurement may be performed
without designating a calibration curve, however, the peak area value
will be displayed without a concentration value.
4. RANGE
This refers to the NDIR range, and is set automatically in accordance
with the range setting of the selected calibration curve. This setting
may not be changed. However, if measurement is to be carried out
without designating a calibration curve, the range may be set optionally.
5. INJ VOL
The injection volume is also set automatically according to the corre
sponding setting of the selected calibration curve. This may be changed,
unless two or more calibration curves are designated. When the
injection volume setting is changed, the measurement value displayed IS
the corrected value ( Refer to NOTE regarding "w" on next page).
6. SPARGE TIME
This is used for setting the sparging time for NPOC measurement. It
can only be set for NPOC measurement.
7. NO OF WASHES
This refers to the number of times the microliter syringe is washed
with sample, and is also set automatically in accordance with the
setting used to create the calibration curve selected. The value may be
changed and measurement can be carried out even if the value is
different from that set in the GENERAL CONDITIONS screen. (Refer
to NOTE regarding "W" on next page.)
8. DIL FACTOR
This allows setting of a dilution factor for a sample which has been
diluted. When a dilution factor is set (set "2" for a dilution factor of
two), the value for concentration displayed in the DATA PROCESSING
SAMPLE screen is corrected by the set dilution factor.
9. NO OF INJECTS
This sets the number of repetitive measurements to be carried out for
each sample. A value from 1 - 10 may be set, and is not related to
the number of injections used to prepare the selected calibration curve.
10. MAX NO OF INJ

The maximum number of injections is automatically set to the same as
that entered for NO OF INJECTS. Setting a higher value will cause
- 40
r replacement of any abnormal results or tailing peaks obtained in the
mitial series of injections with normal results obtained through
additional injections. When a higher value is set, suggested values for
SD (standard deviation) as an area count and CV (coefficient of
variation) will be displayed. These values may be changed as desired.
11. «CALIBRATION CURVE FILE LIST»

The main conditions associated with the stored calibration curve files
are displayed here. "NEW" displayed at the right of one of the files
denotes that it is the latest calibration curve to be stored.
NOTE: The designation "W" (warning) displayed just to the right of a set value
(lNJ VOL, NO OF WASHES) denotes a discrepancy between that value and the
corresponding value set in the calibration curve selected.
2) Operations

set sample meas Input appropriate numeri· Sets sample measurement conditions.
urement conditions cal value for each item and Refer to:
press I ENTER I key. Sec. 10.12 Automatic selection of optimum
calibration curve
Sec. 10.14 Quantitation by carbon equivalen
Sec. 10.10 Automatic measurement for
replacement of abnormal values
Print settings. Press Prints out measurement condition settings.
Proceed to next i
Press NEXT ~ . Proceeds to MEASUREMENT START
screen.
step.
Return to MAIN
MENU screen.
i
Press MAIN MENU il· Returns to MAIN MENU screen.
3) NOTES:
1. When measurement is performed on the basis of "carbon equivalent"

(see Sec. 10.14), only the "1st CAL CURVE" may be set.
2. When "FLOW" is set for the SPARGE GAS FLOW item in the
MAINTENANCE screen, SPARGE TIME is set to 0 in this screen.
Sparge gas will flow continuously.
3. To change the calibration file entry, press ICE I and enter a new number.
·41
6.9 MEASUREMENT START screen (at Sample Measurement)
MEASUREMENT START
NON-STOP MODE=ITJ (l=ON 2 = O F F } - - - - - - - t - - - {
SET SAMPLE VESSEL

lNS~R'l' SJ\MPLII\G TUH~ \-----------+---( 2
PRESS [START)
S~,,1PL COND
Figure 6.9 MEASUREMENT START Screen (at Sample Measurement)
This screen appears when the I NEXT II key is pressed in the SAMPLE
MEASUREMENT/CONDITIONS screen.
1. NON-STOP MODE
When more than one type of measurement is selected in the SAMPLE
MEASUREMENT/CONDITIONS screen, using the NON-STOP MODE
causes measurement to continue from one type of measurement to the
next (for example, continuous TC and IC measurement in TOC
analysis), starting from the left-most measurement setting. If it is not
used, operation will stop in the DATA PROCESSING SAMPLE screen
after completion of each type of measurement. To continue
measurement in this case, it is necessary to press the II NEXT !I key.
- 42
2) Messages and operations
SET SAJJPLE VESSEL
INSERT SAJJPLING TUBE
PRESS [START]
Place the vessel containing the sample on the sample platform, insert
the sipper and press the ISTART/STOP I key to initiate measurement.
RANGE VALUE OF PREVIOUS DISPLAY IS NOT YET SET

Set RANGE value in the SAMPLE MEASUREMENT/ CONDITIONS
screen.
FIND SYRINGE ZERO POINT DETECTION ON

MAINTENANCE DISPLAY (#8)
Select MAINTENANCE (#8) from MAIN MENU and carry out zero
point detection of the microliter syringe.
*GO TO "MONITOR" DISPLAY (#6) TO SEE READY STATE

This appears if the ISTART/STOP I key is pressed when the instrument
has not yet attained the READY state. When the READY state
conditions are satisfied, the instrument will automatically continue with
the specified analysis.
3) Operations
Set NON-STOP IT] IENTER I Perform continuous analysis from one type
mode. of measurement to another when mulliple
types of measurement are set for a sample.
Start measurement Press ISTART/STOP I Starts measurement.
Return to SAMPLE Press I SMPL COND II· Returns to SAMPLE MEASURE

MEASUREMENT/ MENT/CONDITIONS screen
CONDITIONS
screen.
4) NOTE
Use the sparging tube when SPARGE TIME has been set.
- 43
6.10 DATA PROCESSING SAMPLE screen
,----------\ 4
DATA PROCESSING SAMPLE SAMPLE# 1 INJ# AREA ppm RMK 5

Te, INJ VOL 30( 25 ltd. RANGE x30 ( 5) 1-67077 192.7 H
NO OF INJECTS 4/ 3(max 4), SPARGE TIME Omin (2) 23252 334. 4 C02
COMPLETED 3 23261 334, 5
~l-I-------------
4 23241 334.2
lOQ%I"""Ir------------------,
MN 23251 334.41
o '- '- SD 10 0.1441
a [min] ! CV 0.04 %
2 4 COR CONC OIL 334.41[x 1.0]
INJ#l 3 COR CONC INJ 334.41[X 1.0]
PRESS [START) FOR REINJECTION, IF NECESSARY
6 H----;:;;;;;;;;:;;._ _nnII.-_
'~IDt:t -D1QII GMI;M'IlNu IMIBIh1M* MUUlD! '''%'I4\'lm~1II
Figure 6.10 DATA PROCESSING SAMPLE Screen
This screen appears when the ISTART/STOP I key is pressed to initiate measurement
of a sample in the MEASUREMENT START screen. The progress of the
measurement sequence is displayed in real time.
1. The measurement conditions set m the SAMPLE MEASUREMENT/
CONDITIONS screen are displayed. When the INJ VOL or RANGE
setting is changed due to the AUTO RANGING AND INJ VOL
function (which was selected in the GENERAL CONDITIONS screen
[see Sec. 6.11]), the initial setting is displayed in parentheses ( ). The
NO OF INJECTS (measurement repetitions) is updated after each
injection during the measurement sequence.
2. The progress of the measurement sequence is displayed here as follows:
SPARGING XX min to end: When SPARGE TIME is set
WASHING : Washing of the microliter syringe with sample
SAMPLING : Aliquot of sample is drawn for injection
INJECTING Injection of sample
MEASURING: Peak detection and area measurement
(continued)
- 44
WAITING: 1) Standby due to unsatisfied measurement condirwns
(READY STATE SENS)
2) Displayed when ISTART/STOP I key is depressed during
SPARGING, WASHING, or SAMPLING
COMPLETED: Measurement sequence completed
MEASURING/WASHING: Washing for next injection starts during
peak processing
3. The peak is displayed with time (min) as the horizontal axis. When the
measurement repetitions are completed, the sequence is ended and the
time axis is marked.
4. Injection number (lNJ#), peak area (AREA) and concentration are

displayed. The mean value (MN), standard deviation (SO) and
coefficient of variation (CV) are calculated using the peak area data.
When OIL FACfOR has been set, the corrected concentration value IS
displayed at the COR CONC OIL item. When the injection volume
used for creating the calibration curve differs from that for sample
measurement, the corrected concentration (multiplied by ratio of
calibration curve injection volume to sample measurement injection
volume) is displayed at the COR CONC INJ item.
5. REMARKS (RMK)
Supplementary information IS provided as follows:
RMK
* * * * * *
Changed range, injection volume or calibration

curve number (Ex. R30 = range 30, 0100 = 100fll,
COS = CAL CURVE F#S)
H : Peak height is beyond range of full scale.
T Peak is not el uted by the end of the

measurement procedure.
6. Messages
PRESS [START] FOR REINJECTION, IF NECESSARY
Press ISTART/STOP I if additional measurement is desired. When
REINJECTION is carried Ollt, time is not displayed.
- 45
GO TO "MONITOR" DISPLAY (#8) TO SEE READY STATE
This message appears when the instrument is in the standby state due
to unsatisfied READY conditions. Select the MONITOR screen to review
the "READY" conditions (see Sec. 6.14). In most cases, the READY
conditions will be satisfied within 10 minutes ("OK" will be displayed
at the relevant condition(s)), and measurement may be carried out.
2) Operations
Purpose Operation Function

Delete/retrieve Bring cursor to appropriate "-" wiJ] appear to the right of the INJ#, and
measured value. lNJ# and press I ENTER I. MN, SD and CV values are recalculated.
Additional meas Press 1START/STOP I Additional measurement is performed and

urement when COMPLETED is dis measurement value is displayed with "+" at
played. right of INJ#.
Change conditions Press II SMPL COND ~ Changeable parameters include NO OF IN

during measure and change value(s) in JECTS, MAX NO OF INJ, SO, CY.
ment. SAMPLE MEASURE The STD CONC may be set if not yet set
MENT/CONDITIONS and if value will be less than those already
screen, then press set.
IIRETURN!1 to return to
this screen.
Interrupt WAITING is displayed (standby state).
measurement ~TART/STOpl During WASHING or SAMPLING, the
standby state is entered after syringe moves
to zero point or just after sample Sipping is
Following function completed. During MEASURING, peak
keys activated) processing is executed without entering the
standby state.
f- Returns to MEASUREMENT START

!!ESCAPEII
screen. Measurement values are lost.
f- !ICONTINUEij Standby cancelled, measurement continues.
Available only during "MEASURING", this
' - II PEAK STOP II terminates measurement of peak area and
displays incom plete results up thal point.
Magnify plot
display
!EXP SCALE II Zooms in on 25% of the plot by height
(0 25% F.S.)
m0CALEII Scale returned to normal (0 100% F.S.)
- 46
Print II PRINT I]
(Following function
keys activated)
f-- ~ALL PRINTI] Entire screen printed out
I- I~A PRINTII Data only printed out (without plot)

I- !IPEAK PRINT~ Peak only printed out
L.-- Ir -NO PRINT I] Print cancelled
Return to MAIN Press ~ MAIN MENU II· Returns to MAIN MENU screen. (Only
items #3 - #6 will be available). To proceed,
MENU screen.
return to DATA PROCESSING SAMPLE
screen.
Proceed to next
step.
1) Continue Press II NEXT ~ . Carries out measurement(s) for other types
measurement of measurement (i.e. IC if set, after comple
tion ofTC)
Proceeds to SAMPLE MEASUREMENT/
CONDITIONS screen (after completing
specified measurements of current sample).
SAMPLE # is updated by 1 to indicate
completed measurement of previous sample.
r
2) End Press II END ~ Changes to MAIN MENU. Select #5 DATA
measurement REPORT to print out data.
NOTE:
If a record of results is required, be sure to designate printout in advance (in the
GENERAL CONDITIONS screen) or in this screen before using I NEXT ~ or
I END II· It is not possible to return to the current screen after proceeding to the
next step.
- 47
6.11 GENERAL CONDITIONS Screen
GENERAL CONDlTIONS
TC CATALYST(TC CAT) : IT] (I=NOflMAI. SENS 2=H[(iH S~NS)

r-------IL SYRINGE SlZE, /Ll(SYR SIZE) : 1 (1=250 2=500 3=1000 4=2500)
r -_ _. NUMBER 01" WASIlES : 4 (0-9, NORMAL 4)
r - - - 1 - UNIT OF CONC(UNIT) : 1 (I=ppm 2=ppb 3=m~/1 4=tLg / 1 5=NO UNIT)
r---I- AllTO flAN(;JNU A'JIJ lNJ VOL: 1 (1=01\ 2=OFF)
} - - - t - AUTO REGENERATION OF IC SOLUTION: I (l=ON 2=OFF)
\ - - - t - AUTO I'H1NTOUT : 3 (l=DATA ONLY 2=DATA & PEAK PLOT a=OFf)
\ - - - - - 1 r TC FCRNACE ON/OFF : 2 (l=ON 2=OFF)
BUZZER : 1 (l=USED 2=NOT USED)
M"'O_':allu 11110
Figure 6.11 GENERAL CONDITIONS Screen
This screen appears when item #3 GENERAL CONDITIONS is selected in the

MAIN MENU. It is used mainly for setting various conditions which do not need
to be changed frequently,
1. TC CATALYST
This indicates the type of TC catalyst. For measurement using the
regular catalyst, select "NORMAL SENS" and for the high-sensitivity
catalyst, select "HIGH SENS".
3. NUMBER OF WASHES
This sets the number of times the microliter syringe will be washed
with sample between samples. The instrument will always perform one
wash between injections of a given sample.
- 48
r 4. UNIT OF CONC
This sets the unit to be used for concentration.
5. AUTO RANGING AND INJ VOL

This specifies whether or not "Automatic change of range and injection
volume" function will be functional (see Sec. 10.13).
6. AUTO REGENERATION OF IC SOLUTION

When ON is selected, IC reagent is automatically pumped from the IC
reagent reservoir up to the IC reaction vessel in order to acidify the
water in the IC reaction vessel (see Sec. 10.15).
7. AUTO PRINTOUT
This selects the format which will be printed when proceeding from the
DATA PROCESSING/CALIBRATION screen or the DATA
PROCESSING/SAMPLE screen. If set to "DATA ONLY", only the
numerical data will be printed out, and if set to "DATA & PEAK
PLOT", both the data and the plot will automatically be printed out
when II NEXT II or II END :1 is pressed. When OFF is selected, no automatic
printing will be performed. The print function selected in this screen
will be performed whenever II NEXT II or ~ END II is pressed (while in a
data processing screen) even if the user has already selected the print
function key in the screen.
8 TC FURNACE ON/OFF
This setting turns the TC furnace either ON or OFF.
9. BUZZER
If this is set to "USED", the buzzer will sound whenever a key is
pressed. If set to "NOT USED", the buzzer will sound only when the
instrument meets all of the "READY" conditions (see Sec. 6.14) and
whenever an analysis is completed.
- 49
2) Operations

Set conditions. I I
Press ENTER after Sets all GENERAL CONDITIONS.
inputting appropriate
numeric value
Return to MAIN Press I MAIN MENU :1· Returns to MAIN MENU screen.
MENU screen.
Print settings. Press I PRINT II· Prints out all general conditions related to
analysis.
CAUTION:
The TC CATALYST and/or SYRINGE SIZE settings must be in accordance
with those actually mounted in the instrument. A wrong setting will not only
have an adverse effect on analysis data, but may also result in damage to
components.
- 50
6.12 CALIBRATION CURVE FILE LIST screen
CALIBRATION CURVE FILE LIST

F# TYPE HlGH C.'ONC P'l' INJJ::>YR;1 1 HANG}; GATALYST SP #WASH DATE
rn TC 80.0 ppm 1 25/250 x 5 NORMAL Omin 4 06(JUN)-22-1989
PROTECT
II
2 TC 400.0 ppm 2 30/2fiO x 30 NORMAL Omin 4 06(JUN)-22-1989
PHOTEC'1'
~ TC 20.0 ppm I 20/2fiO x 1 NORMAL Omin 4 06~JlJN)-22-1989
P O'l'ECT 12
4 TC 240.0 ppm 1 8/250 )( 5 },lORMAL 0 min 4 06~JUN)-22-1989
P OTECT
5 TC 240.0 ppm 2 8/250 )( 5 },lORMAL 0 min 2 06kJUN)-'22-1989
N W
7}--t---------------------J
8}--t--------------------
9}--t------------------------'
lO}--t---------' PRESS [ENTER) TO SEE CURVE - - - - - - - - - t - - i I3
"61""'4'lu M'''i MIM ALL' '!.I'AF< 1'1·11'1'1
Figure 6.12 CALIBRATION CURVE FILE LIST Screen
This screen appears when item #4 CALIBRATION CURVE FILE LIST is

selected in the MAIN MENU. It displays pertinent information on all of the
calibration files currently stored in memory, and allows deletion of selected file(s).
1. F# (file number)
This specifies the number of the calibration file. The cursor may be
moved to the desired number (#1 - 18) in order to select the file for
further viewing.
2. TYPE
Either TC (TC calibration curve) or IC (IC calibration curve) is
indicated for each file.
3. IDGH CONC
This displays the highest concentration of the standard solution used 10
creating the calibration curve.
4. PT
This Indicates the number of points used to create the calibration curve.
·51 •
5. INJ/SYR
This indicates the injection volume and the size of the microliter
syringe used in creating the calibration curve.
6. RANGE
The range for measurement IS displayed.
7. CATALYST
The type of TC catalyst used (NORMAL or HIGH SENS) IS displayed.
8. SP (sparge time, min)

This indicates sparging time III minutes.
9. #WASH
The number of times the microliter syringe is washed with sample prior
to injection is displayed.
10. NEW
The last calibration file stored will always be indicated by "NEW".
11. DATE
This indicates the year, month and day when the calibration curve was
created.
12. PROTECT
This indicates that the data IS protected (PROTECT status) see Sec. 6.4)
1).
13. Message
PRESS [ENTER] TO SEE CURVE

To view the stored data of a particular calibration curve) move the
cursor to the F# corresponding to that calibration curve) and press
IENTER I .
- 52
2) Operations
View calibration Move cursor to appropriate Displays CALIBRATION CURVE screen.

curve data F# and press IENTER I.
O1ange PROTECT Move cursor to appropriate O1anges PROTECT status.

status F# and press 1ENTER I.
Then change status (see
Sec. 6.7)
Delete calibration Move cursor to appropriate The designated file is deleted and the file
curve data F# and press: status is denoted as "FREE".
I CLEAR FILE II
~
~ALL CLEAR~ Deletes all calibration curve files except
~ those with PROTECT status.
1\ ALL CLEAR II
Return to MAIN Press [I MAIN MENU I] . Returns to MAIN MENU screen.
MENU screen.
Print screen Press [I PRINT II· Prints out the entire contents of the screen.
contents
3) NOTES
1. Cancellation of the protected status of a calibration file can only be

executed in CALIBRATION CURVE screen.
2. After Ii CLEAR FILE 11 or II ALL CLEAR II is pressed, the CLEAR operation

may still be cancelled by pressing IINO CLEAR~.
3. A file that is cleared cannot be retrieved.
- 53
6.13 DATA REPORT screen
DATA REPORT PAGEl 07 (J UL)-05-1989 13: 47
SPL# TC RMK IC RMK Toe

1 14.23pprn 1**** 8.820 ppm 2 **** fi.412pprr
2 11. 13ppm 1**** 8.114 ppm 2RV*I 3.022 ppm
3 12.lOpprn 1**** 9.457 ppm 2 **"'* 2.647 ppm
2 4 7!J.4~ppm 4~. 51 ppm 4 **** 35.91 ppm
::3****
5 98.35 ppm 5**** 41. 32 ppm 6 **** 57.02 ppm
6 50. 32ppm 5**** 26.14 ppm 6 **** 24.17 ppm
7 111.lppm riR'h* 55.53 ppm 6 **** 55.58 ppm
MAIN MENI' * NEXT PAl :E * HACK PAnl· Pl<lNT DATA ('I.I·:AR
Figure 6.13 DATA REPORT Screen
This screen appears when #5 DATA REPORT is selected in the MAIN MENU
screen. The measured sample concentration along with various analysis conditions
are displayed for each of the samples.
1. The page number of the current page is displayed. Up to 15 pages of

sample data may be stored with a maximum of 120 sample files.
2. Analysis results are displayed in the order in which the samples were
analyzed, i.e. in the order of the displayed sample number (SPL#).
3. The RMK (remark) column is used to display additional information, as

indicated on the following page.
- 54
RMK
* * * * *
Indicates whether or not measurement value is
corrected by injection volume factor (if sample
injection volume was different than that used in
calibration curve).[I: Corrected, *: Not corrected]
, - - - - Indicates whether or not measurement value is

corrected by dilution factor.
[D: Corrected *: Not corrected]
L- Indicates whether or not automatic injection

volume change was carried out.
[V: Changed *: Not changed]
Indicates whether or not automatic range selection

was carried out.
[R: Auto-ranging *: No Auto-ranging]
, - - - - - - - Indicates calibration curve number used

(CAL CURVE#)
2) Operations
View next page Press IINEXT PAGEII Displays next page of data.
View previous page Press \@ACKPAGEII Displays previous page of data.
Delete data IIDATA CLEARI\
(Following function
keys become available)
_ IIDATA CLEAR~ All data in DATA REPORT is deleted.

- ~ NO CLEAR I] Data deletion is cancelled.
Print screen Press II PRINT ~ . Prints out entire screen contents.
contents
Return to MAIN Press I MAIN MENU II· Returns to MAIN MENU screen.
MENU screen.
- 55·
3) NOTE
It is suggested that the entire DATA REPORT be printed at the end of the
measurement day and that the DATA REPORT screens be cleared. If a new
measurement day is started without deleting the data report, the sample number
will be the next free number, or old data might be overwritten if the data report
file is full. Confusion of data may occur, since sample numbers. (SPL#) and
measurement items (TC, IC, NPOC, etc.) which are not used in the new
measurement will retain old data, and is therefore mixed with new data.
- 56
6.14 MONITOR screen
MONITOR 06(JUN)-22-1989 19: 48
- RANGE: x3Q
+100%~--------------~
TC FURN ACE TEMP: 1- r-G)

679'C OKJ
DEHUMIDIFIER TEMP: 1J f4\
1.I'C OKJI'-V
0'"-------
BASEUNE POSITION : OK
I3ASELINE FLUCTUATION ~
:OK ~
-100% L -_ _...l..-_ _- ' -_ _----'-_ _- - '_ _- - - - '
BASELINE NOISE : OK
a [min] 5 10 15 20 25
'1'4""10111 latJID
Figure 6.14 MONITOR Screen
This screen appears when #6 MONITOR is selected in the MAIN MENU screen.
It allows monitoring of the current conditions which determine whether or not the
instrument is in the READY state for carrying out measurement.
1. This indicates the currently selected range for the NDIR.
2. The baseline is displayed.
3. The TC furnace temperature is indicated along with its READY status

(OK: READY; NG (NO GOOD): NOT READY).
4. The dehumidifier temperature is indicated along with its READY status.
5. The READY status is indicated for the baseline conditions of position,

fluctuation and noise.
- 57
2) Operations
Print screen. Press IPRINTII. Prints out entire screen contents.
Return to MAIN Press ~ MAIN MENU II. Returns to MAIN MENU screen.
MENU screen.
3) NOTES
1. The RANGE setting may be changed via the RANGE SET item tn the
MAINTENANCE screen (see Sec. 6.16).
2. NG is displayed for the BASELINE POSITION when baseline deviates

from 0% by ±100% for the range setling xl, by ±50% for x5, and by
±10% for x30. To correcl the baseline position, it is necessary to carry
out zero adjustment of the NDIR optical component (see Sec. 9.2).
Since the baseline may fluctuate while the TC furnace is heating up or
immediately after a catalyst Change, wait until the baseline stabilizes
before carrying out zero adjustment.
·58·
6.15 STANDBY OPTIONS screen
ST ANDBY OPTIONS
--1---__
- FINISH OR RUNNING: rn (l=FINISH 2=RUNNING)
5r _
1 PRESS [STANDRY] TO DO IT
a"w,_ 6.1'QOOIII)OI
Figure 6.15 STANDBY OPTIONS Screen
This screen appears when #7 STANDBY OPTIONS is selected in the MAIN

MENU screen. It is used to specify complete manual shut-down (FINISH) of
instrument operation or programmed restart (RUNNING) to end the standby state.
3'1A~DBY omONS STA~I)8Y 0PI10~S
FI~ISH 0 .. P..UNNI~G, IiI·flNISH I'RU~~ING)
AumSTAHTmlf: :o;{JU~)-U-I""":1ll -----I-~4.
WA:-: II /.lJ~ TO TURN IoIAlN S~1TC1! oFr
l.()H'T nlHN "tAl:-l SYllTCtI uff'
------ Fig. 6.16 FINISH Screen

lIIaIIIIIlmIIIIllIII
Fig. 6.17 RUNNING Screen

_
- 59
1. This enables selection of FINISH (to manually shut down instrument

operation) or RUNNING (to specify a defined standby state and restart
time). When FINISH is selecled, lhe TC furnace and carrier gas are
turned off, while the ventilating and cooling fans remain on to protect
the TC injection port and electronic components from heat damage. The
unit will display a wait time, and count down the time until it is safe
to manually tum off the fans. When RUNNING is selected, the
following STANDBY condition items are displayed (see Fig. 6.17).
2. TC FURNACE
This specifies whether the TC furnace IS to remain ON or to be turned
OFF unlil restart of the instrument
3. CARRIER GAS
This specifies whelher the carrier gas flow IS to remam ON or OFF
until restart of the instrument
4. AUTO START TIME

This specifies the date and time when measurement will begin again.
The TC furnace and/or carrier gas will be turned ON automatically (if
they had been turned OFF) one hour before the set AUTO START
TIME to allow for proper stabilization prior to measurement
5. Messages
PRESS [STANDBY] TO EXECUTE

Press IISTANDBylj to execute the designated operation (either
FINISH or RUNNING).
DON'T TURN MAIN SWITCH OFF

Do not turn OFF the power switch. (This is to enable automatic
start-up of the instrument when RUNNING is selected.)
WAIT 30MIN TO TURN MAIN SWITCH OFF

Wait 30 minutes before turning OFF the power switch. (This allows
minimum cool-down when FINISH is selected.) When the displayed
remaining time reads 0 (zero), minimum cool-down is completed and it
is safe to turn OFF of the power supply (see Fig. 6.16).
WAIT A MOMENT
There is a pause in instrument operation when either of the shut-down
options is canceled by pressing the II ESCAPE I] key.
- 60
2) Operations
Execute [TI - IENTER I FlNISH is executed, with only TC furnace

FINlSH or RUN 1 and carrier gas being turned off. Waiting
NING time is displayed to indicate when power
iSTANDBYij
switch may be safely turned off.
W -IENTERI RUNNlNG is executed on basis of set

1 conditions. When conditions specify that TC
Set RUNNING conditions furnace and/or carrier gas be turned off, the
via [TIor W -I ENTER I specified item(s) will be turned on one hour
before the set AUTO START TIME.
1
IISTANDBYI]
Cancel executed Press IIESCAPEI] Cancels either of the executed shut-down

STANDBY option. options (FINISH or RUNNING).
Tum off LCD Press I SCREEN OFFII Turns off LCD screen (to conserve LCD
display monitor 1 componenLs during the RUNNING standby
I
(press any key Ito turn period).
LCD on again)
Return to MAIN Press II MAIN MENU II· Returns to MAIN MENU screen.
MENU screen.
3) NOTES
1. Whenever the instrument is to be turned offk the use of the FINISH

function is advised in order to prolong the life of the TC injection port
and electronic components. However, in an emergency, the instrument
may be turned off immediately via the power switch.
2. When using the RUNNING function, the NDIR, electronic dehumidifier,

ventilating fan, cooling fan and CPU remain activated.
3. When using the RUNNING function, the TC furnace temperature will

start rising and carrier gas will start flowing one hour before the set
AUTO START TIME in order to allow for stabilization of the TC
furnace.
4. The RUNNING function is preferred if the instrument will not be out

of service for a prolonged period. The FINISH function provides a
minimum cooling period, and whenever possible, a longer cooling time
prior to fan shutdown is recommended.
- 61
6.16 MAINTENANCE screen
MAINTENANCE
FOR OPERATION
l--~---- 0 DATE & TIME
ZERO POINT DETECTION OF SAMPLE SYRIKGE PUMP
REGENERATION OF TC CATALYST
REGENERATION OF IC SOLUTION
REGENERATION OF TC CATALYST & IC SOLUTION
SPARGE GAS FLOW
TC BLANK CHECK
FOR SERVICE
} - + - - - - - KEYBOARD CHECK
PRINTER CHECK
MECHANICAL CHECK
READY STATE SENS
RS-~3~C !IF CHECK
RANGE SET
gr.ijIIII'IOIU
Figure 6.18 MAINTENANCE Screen
This screen appears when #8 MAINTENANCE is selected in the MAIN MENU

screen. Various set-up and routine maintenance functions are performed via this
screen, in addition to service-related functions.
1) "FOR OPERATION" screen item descriptions
1. DATE & TIME SET

This sets the year, month, day, hour and minute.
2. ZERO POINT DETECTION OF SAMPLE SYRINGE PUMP

This automatically zeroes lhe syringe so that accurate measurement of
the sample aliquot is possible.
3. REGENERATION OF TC CATALYST
This item is selected to regenerate the TC catalyst with 2N-hydrochloric
acid (see Sec. 9.3.1).
4. REGENERATION OF Ie SOLUTION
This item is selected to pump IC reagent from the IC reagent reservoir
up to the IC reaction vessel to acidify the liquid in lhe IC reaction
vessel (see Sec. 9.3.2, 10.15).
- 62
5. REGENERATION OF TC CATALYST & IC SOLUTION
This item is selected to carry out regeneration of the TC catalyst and
IC solution at the same time.
6. SPARGE GAS FLOW

This opens or closes the solenoid valve which controls the flow of
sparge gas.
2) "FOR SERVICE" screen item descriptions
1. KEYBOARD CHECK
This item is used to check the operation of the keys. When a key is
pressed, its function will be indicated on the screen if the key is
functional. To exit the KEYBOARD CHECK mode, press I ENTER lance
to confirm the "ENTER" function and once again to exit the check
mode.
2. PRINTER CHECK
This item initiates a test pattern printout. Press IENTER I again to stop
the test printout.
3. MECHANICAL CHECK
This item brings up a special screen which allows the operator to
check the operation of various mechanical components. For further
details of the MECHANICAL CHECK screen and its functions, refer to
Sec. 9.5.
4. READY STATE SENS

This item toggles between deactivating/activating of the READY
STATE sensor. When the sensor is deactivated ("INACTIVE" is
displayed), the instrument may be operated even though the READY
conditions are not yet satisfied. (NOTE: Data obtained when the
READY STATE sensor is deactivated may not be reliable.)
5. RS·232C IfF CHECK

This item will display the OPEN/CLOSED status of the RS-232C port.
(OPEN : communication circuit not complete; CLOSED :
communication possible)
- 63
6. RANGE SET
This item allows the NDIR range for the MONITOR function to be
changed without affecting a calibration curve or an analysis.
2. Operations
Set date and time Move cursor to DATE & If the system is staned using ALL RESET,
TIME and press IENTER ~ set all date and time items as described. Nor
Input month (2 digits), day mally, the date and time need not be entered
(2 digits), year (4 digits), again even if the power switch is turned off.
hour (2 digits), minutes (2
digits), pressing I ENTER 1
after each.
Carry out zero Zero point detection of the syringe is carried

point detection out automatically (see Sec. 7.4).
Regenerate TC Move cursor to appropriate Regeneration of TC catalyst is carried out

catalyst I
item and press ENTER I. automatically (see Sec. 9.3.1).
Regenerate IC solu Move cursor to appropriate Regeneration of IC solution is carried out

tion item and press 1ENTER I. automatically (see Sec. 9.3.2).
Open or close Move cursor to SPARGE When "FLOW" is displayed, the sparge gas
sparge gas valve. GAS FLOW item and press solenoid valve is open and gas is flowing.
IENTERI. The flow rate is adjusted via the sparge gas
("FLOW" is displayed, pressure controller (normal flow rate:
valve is open) 150mllmin). THE VALVE REMAINS
Move cursor to same item OPEN EVEN AFTER MOVING TO
I
and press ENTER I. ANOTHER SCREEN UNLESS IT IS
(Noth.ing is displayed, CLOSED BY USER (see Sec. 8.4.2).
valve is closed)
. . . . . /y</
l:!,i~J~~\i~ll
/Y\HI \f[}llliPf~ri~press ... . ..•... ...>:::::J".<' « •.•
·•I~A:R'tfSt:6PI;··
Check key Move cursor to appropriate Confirms normal functioning of keys. Press
functions item and press ENTERI I. IENTER Itwice to exit check mode.
Then press each key in turn.
Check printer Move cursor to appropriate Initiates test pattern printout if printer is
I
item and press ENTER I. normal. Press IENTER Iagain to stop.
Check operation of Move cursor to MECHANI Allows manual operation of the various in
various instrument CAL CHECK item and strument components (see Sec. 9.5).
components. I I.
press ENTER Press keys
corresponding to
appropriate component
(Continued)
- 64
r
Purpose Key 0 peration Function
Perform operations Move cursor to appropriate Allows operation regardless of the READY
by overriding item and press 1ENTER I· STATE status. Data obtained in this meas
READY STATE urement mode should not be considered
sensor reliable.
Check status of Move cursor to appropriate Indicates whether communication mayor

RS-232C port item and press 1ENTER I. may not be conducted through RS-232C port.
Set NDIR range Move cursor to appropriate Sets NDIR range for the MONITOR
item and press IENTER I. function.
Then input range.
Return to MAIN Press I MAIN MENU II· Returns to MAIN MENU screen.
MENU
3) NOTE
Zero point detection of the microliter syringe must be performed whenever the
instrument is turned on using ALL RESET, or whenever the microliter
syringe is changed.
- 65
-66
7 Analysis preparation
7.1 Supplying carrier gas

1) Confirm that the carrier gas pressure controller knob (inside front door) is
turned all the way counter-clockwise to the closed position. Open the valve of
2
the carrier gas cylinder to supply gas at a rate of 85 - lOOpsi (6 kg/cm ).
2) Tum ON the power switch. Turn the carrier gas pressure controller knob
2
(inside front door) clockwise so that the gauge reads 4 - 5kg/cm .
3) Tum the carrier gas mass flow controller clockwise to adjust the flow to about
150ml/min.
7.3 Turning on TC furnace (GENERAL CONDITIONS screen)
Move the cursor down to the "TC FURNACE ON/OFF item. Then press [I] to
select the ON option, and press IENTER I to turn the TC furnace on.
NOTE: Confirm that carrier gas is supplied before turning on the furnace to
prevent "lifting up" of the high-sensitivity catalyst in the combustion tube.
- 67
At this time, set all of the other items in the GENERAL CONDITIONS screen
referring to Sec. 6.11. Then press the [I MAIN MENU II function key to return to the
MAlN MENU screen. Verify all of the General Condition settings in the MAIN
MENU display.
7.4 Zero point detection of syringe pump (MAINTENANCE screen)
It is necessary to perform automatic zero point detection of the syringe pump

whenever the syringe is changed. Select MAINTENANCE in the MAIN MENU
to bring up the MAlNTENANCE screen (see Sec. 6.16). First place a
water-filled vessel on the sample platform and insert the sampling tube. Bring
the cursor down to the second item "ZERO POINT DETECfION OF SAMPLE
SYRINGE PUMP", and press the IENTER I key to initiate the operation. The zero
point detection will take about two minutes.
7.5 Setting date and time (in MAINTENANCE screen)
While in the MAlNTENANCE screen, use the m cursor key to bring the cursor
up to the first item "DATE & TIME", and press the IENTER I key. Use the
numeric keys to first set the month (using 2 digits, i.e. "09" for September,
etc.). Then press IENTER I to validate the entry and bring the cursor to the next
setting value (day). Use 2 digits to set the day, press the IENTER I key to validate.
Proceed to the year and time settings using the same procedures. Note that the
time setting is based on the 24 hour system (i.e. 2:00PM is set as 14:00).
7.6 Regeneration of TC catalyst (also in MAINTENANCE screen)
Whenever the TC catalyst is changed, the area counts drop or become variable,
or the unit has not been used for some time, it is advisable to regenerate the TC
catalyst.
1) Replace the inner sealing cap on the provided 2N-hydrochloric acid bottle with
the supplied inner cap having a small hole. Place the bottle on the sample
platform and insert the sampling tube (exiting through the opening in the closed
front door) through the hole in the cap into the bottle of HCr.
NOTE: Do not use any other acid other than dilute HCI (refer to Sec. 9.3.1
"Regeneration of TC catalyst" under Maintenance.)
2) Select the MAINTENANCE screen. Bring the cursor to the item

"REGENERATION OF TC CATALYST", press [ENTER I to select, and then
press the I START/STOP I key to initiate the procedure. Regeneration takes 5 - 7
minutes to complete, depending on the microliter syringe used. (The progress
- 68
may be monitored on the LCD, which displays "REGENERATING" along with
the remaining time.) To interrupt the process at any time, press the E
function key.
7.7 Regeneration of IC solution (MAINTENANCE screen)
Regeneration of IC solution refers to the acidification of the liquid in the IC

reaction vessel by pumping IC reagent from the IC reagent reservoir up to the IC
reaction vessel.
1) Select the MAINTENANCE screen. Bring the cursor to the item
"REGENERATION OF IC SOLUTION", press IENTER I to select. Press the
I START/STOP I key to initiate the procedure.
2) The IC reaction vessel drain valve will open for 3 to 20 seconds (depending on
the microliter syringe used). After the valve is closed, two pulses of pressurized
air will be sent to the IC reagent reservoir bottle, thereby forcing IC reagent up
to IC reaction vessel.
At this time, confirm that IC reagent flows all the way up through the
Teflon tube to IC reaction vessel. If IC reagent does not flow into the vessel,
stopping partway in the tube, wait for the operation to end and then repeat the
procedure again. (TIle progress of the operation may be monitored on the LCD,
which displays "REGENERATING" along with the remaining time.)
If IC reagent does not rise in the tube at all or rises and then drops, check for
and eliminate gas leaks at fittings of the IC reagent reservoir.
7.8 Preparation of standard solutions
7.8.1 Preparation of TC (TOC) standard solution
1) Stock solution
Accurately measure 2.125g of dried reagent grade potassium hydrogen
phthalate. Dissolve it in purified water in a I-liter volumetric flask and bring the
solution to volume. This stock solution contains 1,000mgll of carbon (l,OOOmg
C/I), equivalent to 1,OOOppm C. Store the solution (see Sec. 7.8.3 below) as a
stock solution for makeup of varying concentrations of TC standard solutions.
NOTE: Depending on measurement requirements, the concentration of the

standard stock solution need not always be 1,OOOppm C. It may be, for example,
3,OOOppm C.
- 69
2) Standard solution
To prepare a standard solution, dilute an appropriate aliquot of the stock
solution (using a Class A pipette) in a 100ml volumetric flask with purified
water. For example, 10ml of stock solution diluted to 100ml will result in a
100ppm standard solution.
7.8.2 Preparation of Ie standard solution
1) Stock solution
Accurately measure 3.50g of reagent grade sodium hydrogen carbonate and
4.41g of sodium carbonate (which has been dried). Dissolve these in purified
water in a l-liter volumetric flask and bring the solution to volume. The
resultant stock solution contains 1,OOOmg C/l, equivalent to 1,OOOppm C.
2) Standard solution
To prepare a standard solution, dilute an appropriate aliquot of the stock
solution (using a Class A pipette) in a 100ml volumetric flask with purified
water.
7.8.3 Storage of standard solutions
Store stock solutions in clean, airtight glass bottles placed in a dark, cool place
(4°C is recommended). The storing period for TC stock/standard solution is
limited (stock solution of 1,OOOppm C keeps about two months; diluted standard
solution of lOOppm C, about a week if stored airtight in a refrigerator).
Airtight storage is critical, particularly for the IC stock solution in which the
concentration is easily affected due to the absorption of C02 in the atmosphere.
NOTE:
When measurement reproducibility has deteriorated or sensitivity has changed,
prepare new stock solutions. Any turbidity or foreign matter in stock/standard
solutions is an indication of possible deterioration or contamination. New
stock/standard solutions must be prepared.
-70
r 8 Analysis
The analysis procedure includes the creation of calibration curves and sample
measurement.
8.1 Calibration
In the TOC-SOOO, the output signal of the NDIR is linearized for all ranges.
A I-point calibration is adequate for measurement, however, calibration using
up to 4 points is possible.
8.1.1 Preparation for calibration
1) Monitor READY status

Prior to performing calibration measurement, confirm that the READY
lamp on the key pad is on, indicating that the instrument READY
conditions are satisfied. This normally takes about 40 - 50 minutes
from the time the instrument and the TC furnace are turned on. It is
advised to select #6 MONITOR in the MAIN MENU screen to confirm
that the baseline position is zeroed to ensure accurate measurement.
Perform baseline position adjustment as described in Sec. 9.2.
2) Verify GENERAL CONDITIONS

In the MAIN MENU screen, review the current General Condition
settings to confirm that they reflect the actual conditions of the
instrument and the various setting options available to the operator. To
modify the settings, select the GENERAL CONDITIONS item in the
MAIN MENU screen and make the appropriate changes referring to
Sec.6.11 .
8.1.2 Calibration procedure
1) Select item #1, "CALIBRATION" in the MAIN MENU to bring up the

CALIBRATION/CONDITIONS screen. Set all the conditions as
described in Sec. 6.4, and then press !L@xT II to bring up the
MEASUREMENT START screen for calibration (see Sec. 6.5).
2) Place the indicated standard vessel on the sample platform and insert
the sampling needle into the vessel. Press ISTART/STOP I to bring up the
DATA PROCESSING STANDARD screen (see Sec. 6.6) and begin
measurement. After measurement (with set number of injections
performed automatically), press I NEXT II to proceed to the measurement
of the next standard solution (if set), or to bring up the
CALIBRATION CURVE screen.
- 71
NOTE: It is not possible to return to the current DATA PROCESSING
STANDARD screen once it is exited. Therefore, if AUTO PRINTOUT was not
specified in the GENERAL CONDITIONS screen, printout should be specified
before pressing ~ NEXT ~ if a record is required.
3) The calibration curve created in the calibration curve screen may by

processed in various ways (see Sec. 6.7) and printed out. Exiting this
screen will cause the calibration curve to be stored and to be protected
if the PROTECT status is selected.
8.2 Sample measurement
The same instrument preparations used for measurement in calibration are

used in sample measurement. (Refer to Sec. 8.1.1 for details.)
NOTE: Selecting TC CATALYST (lUGH SENS or NORMAL SENS)

Measurement with high-sensitivity catalyst should be specified in the GENERAL
CONDITIONS screen if the TC concentration in the sample is in the range of
Sppb - 500ppb (.Sppm). If high- sensitivity catalyst is used, refer to Sec. 8.3.
8.2.1 Measurement procedure
1) Select item #2, "SAMPLE MEASUREMENT" in the MAIN MENU to

bring up the SAMPLE MEASUREMENT/CONDITIONS screen. Set the
conditions as described in Sec. 6.8, and press I[NEXT] to bring up the
MEASUREMENT START screen for sample measurement (see Sec. 6.9).
NOTE: Specifying calibration curve

When specifying the calibration curve(s) in the SAMPLE MEASUREMENT
/CONDITIONS screen, select a curve with a standard high value which is greater
than the estimated concentration of the sample.
2) Place the sample vessel on the sample platform and insert the sampling
needle. If using a large sample vessel, place it on the table beside the
instrument and remove the sample platform. If the sample tube is not
long enough, replace it with the flanged tube (638-4'269). Press
!START/STOP! to bring up the DATA PROCESSING SAMPLE screen
(see Sec. 6.10) and begin measurement. After measurement (with set
-72
r number of injections performed automaticaLLy), press [I NEXT II to proceed
with another type of measurement for the same sample (for example,
IC, after completion of TC measurement), or to return to the SAMPLE
MEASUREMENT/CONDITIONS screen to analyze another sample.
3) When there are no more samples to analyze, press II END ~ to return to

the MAIN MENU. For a comprehensive report on all of the stored
analyses, select item #5 DATA REPORT in the MAIN MENU screen.
8.3 High-sensitivity measurement
Measurement using high-sensitivity catalyst should be performed when the

sample concentration is in the range of 4ppb - 500ppb (50 - 500ppb for
the TOe-5050), or when differentiation between minute changes on
concentration are necessary. While the high-sensitivity catalyst will measure
over the entire instrument range, it is advisable from an economic standpoint
to use the regular sensitivity catalyst except when high-sensitivity
measurement must be performed.
This catalyst will accept injection volumes of up to 20001-l1. It will provide

high oxidation performance even with the large injection volumes, and
produces negligibly small blank peaks. Use of this catalyst is restricted to
samples containing <5ppm IC and/or <5% free acid content. The cayalyst is
a quartz wool support impregnated with platinum and will therefore become
brittle, and may collapse when subjected to higher IC or acid content. The
catalyst efficiency is not affected, however, until a complete collapse occurs.
Since carbon is present everywhere in the environment, special precautions

and procedures must be observed to prevent contamination of standard
solutions, samples and glassware used in sample handling.
NOTE:
Before turning ON the TC furnace, confirm that carrier gas is supplied to prevent
"lifting up" of the high-sensitivity catalyst in the combustion tube.
8.3.1 Handling of TC combustion tube with high-sensitivity catalyst
1) Use a TC combustion tube containing high-sensitivity catalyst only for

high-sensitivity measurement.
2) If the concentration of the sample measured far exceeds the range

typically measured, subsequent high-sensitivity measurement using that
-73
TC combustion tube may be adversely affected. To restore the high
sensitivity catalyst, perform repeated injections using purified "zero"
water or, for TOC-SOOO users, run the TC Blank Check program to
clean the catalyst (see Sec. 9.4.16).
3) When storing a TC combustion tube contammg high-sensitivity catalyst,

seal both ends of the combustion tube using Parafilm to prevent
contamination.
8.3.2 Handling of purified water or samples with ultra-low carbon content
1) Purified water or samples with ultra-low carbon content should be
analyzed immediately after being sampled, if possible.
2) If analysis cannot be performed immediately after sampling, store the

samples in a dark place at low temperature (4DC), and perform
measurement as soon as possible.
3) The storage container for ultra-low carbon content sample should:

• Be glass rather than plastic to minimize contamination
• Be thoroughly cleaned in advance using an acid wash, multiple rinses and heat
treatment
• Have a capacity of 500 ~ 1000ml at least
• Be filled to the brim with ultra-low carbon content sample
• Be sealed airtight using a ground glass stopper or Teflon-lined cap
4) When analysis is performed, the sample container should:
• Be glass
• Be thoroughly cleaned
• Have a capacity of 500 ~ 1000ml at least
• Be sealed from the environment using a paraffin film after inserting the
sampling needle
8.3.3 Dedicated microliter syringe
To minimize the possibility of contamination when performing

high-sensitivity measurement, it is advisable to use a micro-liter synnge
specially dedicated for that purpose.
-74
8.3.4 IC removal in high-sensitivity measurement
Since the high-sensitivity catalyst should not be subjected to >5ppm IC,

sparging of the sample is usually required in high-sensitivity
measurement. .When sparging is to be performed for removal of the IC
component (see Sec. 8.4.2) prior to high-sensitivity measurement, use
approximately 50 - 100mi of sample in a glass container, leaving a
small amount of space at the top of the container to avoid overflow
due to sparging.
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8.4 Measurement of samples with high IC content
When TOC is determined by subtracting the IC from the TC content in

samples with a higher IC content than TOe, significant error in TOC
determination may be expected due to inherent errors of the TC - IC
method. Accordingly, for such samples it is advised to measure the
TOC directly via the TC measurement procedure (NPOC measurement)
after first removing the Ie component through pretreatment of the
sample using an acidification and sparging procedure.
Pretreatment of the sample is carried out to remove the IC component,

consisting primarily of dissolved C02 and carbon in the form of
carbonate in water.
NOTE:
Sparging should not be applied to samples containing volatile organic carbon
substances which may be lost during sparging.
-75
8.4.1 Acidification
Introduce a small amount of 2N-hydrochloric acid into the sample

container to reduce the pH to between 2 and 3. All of the carbonates
will be converted to C02 by the following types of reactions.
Na2C03 + 2HCl -- C02 + 2NaCI + H20

NaHC03 + HCI -- C02 + NaCI + H20
The C02 may then be eliminated by sparging the sample with

C02-free air.
NOTE:
The TOC-SOOO is protected against the corrosive effects of HCl. Avoid using
sulfuric acid or phosphoric acid for acidification of the sample, if possible.
8.4.2 Sparging
The TOC-SOOO features a sparging function which enables manual

control over sparging or automatic inclusion of a sparging step in the
NPOC measurement sequence. The procedures are as follows.
Automatic sparging in measurement
1) Adjust the sparge gas flow rate.

First open the front door of the instrument and turn the SPARGE GAS
pressure control knob counter-clockwise a few turns. Then select item
#8 MAINTENANCE in the MAIN MENU to bring up the
MAINTENANCE screen (see Sec. 6.16). Move the cursor down to
"SPARGE GAS FLOW", and press IENTER I to open the sparge gas
solenoid valve. Gradually turn the SPARGE GAS pressure control knob
clockwise to adjust the sparge gas flow rate to 150 - 200mllmin. With
the cursor at the SPARGE GAS FLOW item, press IENTER I again to
close the sparge gas solenoid valve.
2) Connect the sparging tube.

Fit the sparging tube (PIN 630-00337) over the sampling tube and
needle and push the end into the sparge tube connector (see Fig. 4.6).
If necessary, widen the angle of the bend in the sparging tube to
facihtate fitting it over the sampling tube and needle. Cutting the end
of the sparging tube at an angle will ease its insertion into the
sampling tube connector.
-76
The length of the connected sparging tube should be such that 12mm
of the sampling needle tip is exposed.
3) Place the sample container on the sample platform and insert the
sampling tube with the covering sparge tube.
4) Select #2 SAMPLE MEASUREMENT in the MAlN MENU to bring

up the SAMPLE MEASUREMENT/CONDITIONS screen. Set the
appropriate time (min) for sparging at the SPARGE TIME item.
NOTE:
The appropriate sparge time will vary with the shape of the sample container,
volume of sample and sparge gas flow rate. Typically, 4 - 6min is adequate.
Various trial times might be used for sparging to ascertain the most appropriate
SPARGE TIME setting prior to actual sample measurement.
The sample will now be automatically sparged for the set time when
measurement is started, and the measurement sequence will continue
normally when sparging is completed. When multiple injections are
specified, the sparge gas will flow continuously except during sipping
of the sample in order to prevent re-dissolving of C02 into the sample
from the atmosphere
Sparging independent of measurement
1) Open the front door and detach the Teflon gas tube with black Viton
end from the side of the sparge tube connector. Pass the tube through
the hole in the side of the instrument and lengthen it by inserting a
piece of Teflon tube into the end of the black Viton tube.
2) Select #8 MAINTENANCE in the MAIN MENU. Move the cursor

down to "SPARGE GAS FLOW", and press IENTER I to open the
sparge gas solenoid valve. Adjust the flow rate to 150 - 200ml/min via
the SPARGE GAS pressure control knob.
Sparging may thus be performed independent of measurement. This function

allows a reduction in the time required to perform multiple NPOC analyses
by enabling sparging of sample while the preceding sample is being analyzed.
-77
8.5 Measurement of samples with suspended solids
The following special factors must be taken into consideration when
performing analysis of samples containing suspended solids.
• The suspended solids must be small enough to pass through the needles.
• The suspended solids must be uniformly distributed in order to obtain
satisfactory repeatability.
Use of a homogenizer may adequately address the above restnctlons,
depending on the nature of the suspended solids and the type of
homogenizer used. An ultrasonic homogenizer, more powerful than the high
speed agitator type, will be more effective in homogenizing large suspended
solids. Sludgy type suspended solids are more easily homogenized than those
that are fibrous. Some suspended solids cannot be homogenized. Generally,
it is advisable to use only the supernatant of samples which contain
sediment which will not remain suspended.
Depending on the application, the sample is often filtered prior to

measurement in order to eliminate irrelevant substances or life forms from
the analysis. In these cases, it is important to select a filter which will not
contaminate the sample with organic substances or fibers.
CAUTION:
Do not perform measurement without the sampling needle to prevent large
particles from entering the tubing and obstructing the injection needle.
NOTE:
If the small holes in the sampling needle become clogged, the plunger driving
motor will not run normally. "ERROR! SYRINGE PUMP" will be displayed and
lhe operation stops. Turn OFF the instrument. Use the provided needle cleaning
wire (PIN 638-30002) or a sonicating bath to clear the holes in the needle, and
then turn ON the instrument.
8.6 Measurement of samples containing acid, alkali or salts
The TOe-SOOo will perform measurement of samples containing acid, alkali

or salts. In all of these cases, however, consideration should be paid to
increased consumption of associated instrument parts in addition to
interference of the NDIR detector. These types of components begin to show
adverse affects when they are present in concentrations above 1000ppm.
Such interferences will be more noticeable in the data at range xl.
- 78·
In general, the most effective way of handling measurement of samples with
r such high concentrations of these components is to dilute the sample
whenever possible.
8.6.1 Chloric acids and salts
When a sample containing chloric acids or salts is injected into the TC

combustion tube, chlorine (C12) is generated. Hydrochloric acid,
hypochlorite and such salts as ammonium chloride, calcium chloride and
magnesium chloride that are easily decomposed by heat can generate
considerable quantities of chlorine. The generated chlorine is removed
by the halogen scrubber. The halogen scrubber also protects against
similar compounds containing fluorine and bromine ions.
Hydrogen chloride and other gaseous or misty components are also

generated from the sample. Most of these are eliminated at the IC
reaction vessel. However, if these components are contained in very
high concentrations, they may not be completely removed. In this
situation, it is recommended to dilute the sample to reduce the
concentration of the salts to below 3% and the acids to below 1%.
8.6.2 Non·chloric acids and salts
Samples containing inorganic acids such as sulfuric acid, llltnc acid or

their salts, though producing components which are less corrosive and
interfering than those of chloric acids and salts, cannot be removed vIa
the halogen scrubber. For this reason, it is recommended that the
sample be moderately diluted whenever possible.
Since acids and salts themselves generate components which interfere

with the NDIR detector, possibly causing their own blank peaks, it is
necessary to use a high purity reagent containing the same
concentrations of acid(s) and salt(s) as those in the sample. If a
reproducible blank peak is created, determine the validity of the sample
peak value after subtracting the obtained blank peak value.
In most cases, a blank peak will generate a positive error in TOC

measurement. Since a blank peak may grow larger with repeated
measurement, it is important to deal with it directly. Correction of the
blank peak may be carried out via 2-point calibration using CD a
blank solution containing the blank component alone and @ a standard
solution to which the blank component has been added.
r
-79
TOC analysis in a sample containing acid may also be carried out as follows:
1) Assuming a sample containing sulfuric acid, reduce the acidity of the

sample (to pH 2 - 3) with potassium hydroxide or sodium hydroxide
to generate thermally stable potassium sulfate or sodium sulfate.
2) Sparge the acidified sample to remove the IC, and then measure the
TOC directly. (This procedure is inappropriate for samples with nitric
acid due to the thermal instability of all the salts of nitric acid.)
8.6.3 Alkali samples
Alkali samples may be analyzed, but measurement of untreated alkali

samples will lead to increased deterioration of the combustion tube and
catalyst as well as reduced sensitivity and reproducibility. Due to
buffering action, it is difficult to predict the maximum pH of of
analysis sample, however, in general, a pH in the vicinity of 11 may
be considered maximum.
NOTE:
Exceeding pH 11 in untreated samples may cause catalyst poisoning.
It is recommended that such alkali samples be acidified to pH 2 - 3

using hydrochloric acid, and then sparged to remove the Ie. When
sample acidification is undesirable, it is strongly recommended to
alternate measurement of alkali samples with acid samples or acidified
water.
8.6.4 Samples containing salts
Frequent analysis of high-salt samples will eventually lead to the

accumulation of these salts in the combustion tube to the point of
restricting the flow of carrier/combustion gas and adversely affecting
reproducibility. When this occurs, maintenance of the combustion tube
(see Sec. 9.4.13) is required to restore the instrument performance.
- 80
9 MAINTENANCE
Periodic inspection and maintenance are essential for assuring normal

operation and stable, accurate measurement in the TOC-5000. The frequency
of conducting inspection and maintenance procedures, as well as the
replacement rate for consumable parts, will vary depending upon the work
schedule of the instrument, the number of samples analyzed, the quality of
samples (particularly levels of salt concentration) and the sample injection
volume. The recommendations offered in this chapter are approximate
figures based on a typical manual operation work schedule of eight
hours/day and five days/week, with daily measurement of about 25 samples
having a salt content not higher than 500ppm.
9.1 Daily inspection
The following inspection procedure should be carried out before starting

measurement each day.
1) ConfIrm cylinder gas pressure and gas flow.

Confirm that the cylinder gas pressure is a lease 200psi and the carrier gas flow
meter indicates 150ml/min.
2) Inspect dehumidifIer drain vessel water level.

Confirm that the water level in the dehumidifier drain vessel reaches to the
overflow port on the drain vessel side wall. If necessary, add water. Then verify
that carrier gas is not bubbling from the dehumidifier drain tube into the drain
vessel. Such bubbling indicates possible clogging of the membrane filter or
halogen scrubber. For inspection of the membrane filter and halogen scrubber,
refer to Sec. 9.4.9.
3) Inspect humidifier water level.

Confirm that the humidifier water level is between the two line markings. The
volume between the upper and lower lines is about 25ml, which will be
sufficient for about three weeks of operation. When the water level drops below
the lower line, add purified water through the supply port.
4) Inspect IC reaction vessel/IC reagent reservoir (if IC measurement is

performed).
Confirm that the IC reaction vessel liquid level is within about 10mm above or
below the drain tube on the vessel side wall. When the water level is too low,
carry out the "REGENERATION OF IC SOLUTION" procedure (see
Sec. 9.3.2). Confirm that there is IC reagent in the reservoir bottle. The reservoir
bottle should contain between 50 - 130ml of the IC reagent.
- 81 •
5) Inspect microliter syringe.
The syringe should be clean and should operate smoothly. Confirm smooth
operation using the SYRINGE UP/DOWN functions in the MECHANICAL
CHECK screen (see Sec. 9.5) accessed from the MAINTENANCE MENU.
6) Perform "Leak Test".
Pinch off the tubes at the soda lime scrubber, and confirm bubbling in the
dehumidifier drain vessel.
7) Wash tubing (at end of day)

At the end of the measurement day, it is necessary to wash the tubing from the
sampling needle to the sample injection needle(s). This is done via the
MECHANICAL CHECK screen (see Sec. 9.5), using purified water in the
sample vessel. Press the lliell
key (and trEJl
key if Ie channel has been used)
under the "WASHING" indication (Item #21, #22 in Fig. 9.6).
WARNlNG:Failure to perform this procedure may lead to clogging of the tubing

and 4-port valve, which may lead to unnecesary down-time. This procedure is
critical in high salt matrices.
9.2 Zero adjustment of infrared gas analyzer (NDIR) optical system
9.2.1 Adjustment procedure
To ensure accurate peak area measurement irrespective of a drifting baseline,

an auto zero correction function is continuously applied to the baseline
signal, except during actual peak measurement. If, for some reason, the
baseline exceeds the auto zero correction range, "NG" will be displayed at
the BASELINE POSITION item in the MONITOR screen, and the READY
lamp on the key pad will be OFF, indicating that measurement is not
currently possible (WAITING state). In this situation, zero adjustment of the
NDIR optical system may be necessary, but only after confirming that:
• Carrier gas is flowing from the gas cylinder
• There is no internal gas leak on basis of leak test (see Sec. 9.1, 6, above)
• Instrument is up to measurement temperature (OK in MONITOR screen)
After confirming the above, perform zero adjustment of the NDIR optical
system as follows:
- 82
1) If the current NDIR range (in MONITOR screen) is not set to x30,
r change to the MAINTENANCE screen (select MAINTENANCE in MAIN
MENU) and set the NDIR range to x30 (see Sec. 6.16). Then change
back to the MONITOR screen to monitor the baseline adjustment.
Membrane ~~===~~
filter
NDIR Halogen
adjustment scrubber
screw
TC injection
block assembly
Figure 9.1 Top Internal View of TOC-5000
2) An adjustment screw is visible through one of two adjustment holes

labeled OPTICAL ZERO toward the rear of the instrument top cover.
Tum the adjustment screw in steps while monitoring the baseline on
the MONITOR screen. The baseline is shifted to the positive or
negative direction by turning the screw clockwise or counter-clockwise,
respectively. Continue the adjustment until the baseline is at the 0%
position.
NOTE: Since the baseline display response is somewhat delayed, rotate the screw
slowly in small increments while monitoring the adjustment.
3) Set the range to x5 by using the maintenance screen and adjust the
baseline to the 0% position.
(continued)
- 83
4) Set the range to xl and repeat the procedure.
NOTE:
The baseline position should be set at 0% at range xl even if measurement will
be performed at higher ranges.
NOTE:
Very rarely, when the baseline is shifted drastically in the negative direction, it
may be noticed that rotation of the adjustment screw in the arrow-marked
direction will cause the baseline to move further in the negative direction. If such
a response is noted, continue rotating the adjustment screw in the arrow-marked
direction until the baseline signal reaches the negative limit and then returns in
the positive direction.
9.2.2 Causes of sudden deviation of baseline position
In addition to the three conditions mentioned to be disqualified before

performing the baseline zero adjustment, sudden deviation of the baseline
position may be caused by any of the following:
• Contamination of carrier gas
• Contamination of TC catalyst occurring during TC catalyst replacement, etc.
• Contamination of humidifier liquid
• Contamination of IC reagent
• Contamination of O-rings during their replacement
• Contamination of the halogen scrubber
• Contamination of the membrane filter
• Contamination of the soda lime scrubber
9.2.3 Causes of gradual and chronic deviation of baseline position

• If a 13x molecular sieve is being used to further purify the carrier gas, the
replacement of the sieve may be required.
• When zero adjustment of optical system is required frequently (and
particularly when the baseline tends to drift in the positive direction),
replacement of the halogen scrubber or the soda lime scrubber may be
required.
- 84·
• If the humidifier water has not been changed recently, it may require
r replacement.
• The TC catalyst may have deteriorated to the point that is needs regeneration or
replacement.
9.3 Regeneration procedures

When measurement senSItivity or reproducibility decreases, it may
be necessary to regenerate the TC catalyst or IC solution. This regeneration
can be conducted automatically on the MAINTENANCE screen.
MAiNTENANCE
FOR OPERATION
'1' o DATE & TIME
0~ ZERO POiNT DETECTION OF SAMPLE SYRII\GE PUMP
f3' REGENERATION OF TC CATALYST
4'::../ REGENERATION OF IC SOLUTION
~® REGENERATION OF TC CATALYST & IC SOLUTION
SPARGE GAS FLOW
6/ G) TC BLANK CHECK
FOR SERVICE
(7\
0 KEYBOARD CHECK
0~
2(;\ PRINTER CHECK
MECHANICAL CHECK
READY STATE SENS
4~® RS-:l3:1C IfF CHECK
RANGE SET
6
1I'4111mlOllii
Figure 9.2 MAINTENANCE Screen
9.3.1 Regeneration of TC catalyst
As samples are measured, various inorganic substances contained in the

samples will remain in the form of salts or oxides on the surface of the TC
catalyst or high-sensitivity TC catalyst. Accumulation of such residues may
lead to deterioration in measurement sensitivity or repeatability. (A standard
solution should be measured to evaluate the measuring performance.)
Deterioration in performance is obvious particularly after measuring alkaline
samples or samples with high IC content. In these cases, satisfactory
performance may often be restored with the injection of dilute hydrochloric
acid into the catalyst (regeneration of catalyst).
- 85
When a standard solution or purified water is measured repeatedly with new
catalyst or with catalyst which has has been stored for a long time,
measurement values tend to be higher than usual at first and then decrease
gradually. Injection of dilute hydrochloric acid in this situation may be
effective in restoring measurement accuracy.
Regenerating the catalyst is carried out from the MAINTENANCE screen

using the following procedure, which is the same for TC catalyst as well as
high-sensitive TC catalyst.
1) Replace the inner cap of the 2N-hydrochloric acid bottle (standard
accessory) with the provided inner cap having a hole, and place the
bottle on the sample platform.
2) Move the cursor to REGENERATION OF TC CATALYST item and

press IENTER I. The REGENERATION OF TC CATALYST screen will
appear, as shown in Fig. 9.3).
REGENERATION OF' TC CATALYST
PUT SAMPLE TUBE IN ca. 2N-HCI SOLUTION. THEN PRESS [START]
WMeta.
Figure 9.3 REGENERATION OF TC CATALYST Screen
3) Following the prompt, insert the sampling tube through the hole in the
inner cap into 2N-hydrochloric acid bottle, and then press
I START/STOP I. The operation, which takes 5 - 7 minutes, will be
carried out automatically and the time remaining will be updated
continuously on the screen.
- 86
NOTE:
The regeneration operation may be interrupted at any time by pressing IIESCAPElj.
If satisfactory performance of the instrument is not restored by the

regeneration process, it may be necessary to wash or replace the TC catalyst
(see Sec. 9.4.14)
CAUTION:
Use only dilute hydrochloric acid for regeneration of TC catalyst or
high-sensitivity TC catalyst. Do not use phosphoric acid, which will generate
abnormally high peaks and/or lead to fluctuating peak values, requiring
replacement of the TC catalyst to restore normal peak values.
9.3.2 Regeneration of IC solution
This procedure is carried out only in cases of IC channel measurement (see

Sec. 10.2) or when TOC is being measured by subtraction (see Sec. 10.3).
With repetitive sample measurement, the acidity of the IC solution in the IC

reaction vessel is gradually reduced through reaction with IC components in
the samples and through dilution with sample. When the acidity decreases,
the IC solution gradually loses its ability to react sufficiently with the IC
components. (A tailing peak will be evident and peak area will show lower
than normal values.) When the tailing peak is pronounced, a "T" will
appear at the right of the peak area value, jlli!i~.~.!iQ!L!..h_~_ne~ssity_t?_a~d
JC r.eagent to the IC solution in the J~ ..re~~J:iC2..~ ~~s~l: If "AUTO
REGENERATION OF IC SOLUTION" has been set to ON in the
GENERAL CONDITIONS screen, the regeneration procedure is performed
automatically after a fixed interval based on the number of injections
performed and the injection volumes (see Sec. 10.15). If "AUTO
REGENERATION OF IC SOLUTION" has been set to OFF, the message
of "GO TO "MAINTENANCE" DISPLAY (#8) TIlEN REGENERATE IC
SOLUTION" will appear on the screen when it is time to regenerate the IC
solution. When this prompt appears, change to MAINTENANCE screen,
move the cursor to "REGENERATION OF IC SOLUTION" and press
1ENTER I. IC reagent will automatically be pumped up to the IC reaction
vessel.
- 87
9.3.3 Regeneration of TC catalyst and IC solution
The dual operation of regenerating TC catalyst and lC solution may be

performed in one sequence. Move the cursor to REGENERATION OF TC
CATALYST AND IC SOLUTION in the MAINTENANCE MENU and
press IENTER I . The entire operation takes 8 about minutes to complete.
9.4 Maintenance procedures
9.4.1 Replacement of high purity air (in cylinder)
2
A type A 200 lb (47 liters, 120kg/cm ) cylinder of carrier gas will last
about three months if gas flow is reduced when the unit is not in use. Be
sure to change the cylinder before the carrier gas is completely consumed
(when the pressure reaches 200psi) to prevent impurities from being
introduced into the system. Before connecting a new cylinder, clean the
connection port so that dust will not enter the instrument after connection of
cylinder. It is recommended to keep at least one spare cylinder in stock.
9.4.2 Cleaning/replacement of syringe plunger tip
Clean the syringe and plunger tip as necessary with laboratory cleanser.
Rinse thoroughly with water-acid-water. The syringe plunger tip (made of
fluorocarbon polymers) will gradually wear down with use, leaving a gap
between the tip and the inner surface of the syringe barrel and cause
leakage. This will be evident with the formation of bubbles around plunger
tip when sample is sucked, or as sample leaks from the bottom part of
barrel when sample is injected. If this occurs, it is necessary to replace the
plunger tip with a new one (use only specified plunger tip). The old
plunger tip may be removed from from the plunger end by pulling on it
forcefully. Place the new plunger tip on a flat sturdy surface with the
insertion hole face up, and insert plunger end into this hole, pushing from
above. Take care not to scratch or damage the plunger tip surface to
prevent any leakage.
9.4.3 Cleaning and replacing the sampling needle
The sampling needle prevents large particles and other foreign substances
from being sucked into the system. However, if the holes in the body of
the needle become clogged, the plunger driving motor will labor during the
suction stroke, causing the message "ERROR!! SYRINGE PUMP" to be
displayed and the instrument to shut down automatically. (This same
response occurs during the injection stroke if the sample injection needle
becomes clogged) When the holes in the sampling needle become clogged,
- 88
clear them of any foreign matter using the supplied cleaning wire or by
r sanification, and turn ON the power switch again to resume measurement.
CAUTION:
When inserting a new or cleaned sampling needle into the end of the sampling
tube, be sure that the end of the needle with the holes around the shaft protrudes
from the tube. If the closed end is inserted first, the syringe pump cannot pump
and the instrument will cease operation.
9.4.4 Replacing O-rings in sliding TC sample injection blocly)

(Quarterly, or monthly with ASI or CSM)
Excessive wear of the a-rings in the sliding injection block will cause
leakage of carrier gas. The a-rings are of two different types (upper white
O-ring, Teflon [PIN 036-11408J and lower reddish brown or black O-ring,
[PIN 036-11209]), placed one over the other in the upper groove of the
lower fixed part of the injection block. The Teflon O-rings should be
replaced on schedule or when gas is found to be leaking from this area.
Procedure: (Take care not to scratch the O-rings.)
1) Remove the top cover of the instrument (see Fig. 9.1).
2) Remove the sliding injection block by first pushing it towards the back
as far as it will go and lifting its rear end until the transverse
mounting screw is clear of the notch in the drive arm. Then push the
sliding injection block a little more towards the rear until it is free of
the lower fixed part of the injection block.
3) Remove the Teflon a-ring and replace it if the upper surface is

flattened. Inspect the lower reddish brown or black a-ring for pliability
and replace it if appears worn or has lost its pliability. Dress the
reddish brown or black a-ring with a small amount of silicon grease
before seating it in the groove and then place the new white a-ring on
top of it.
NOTE:
At this time, it is convenient to inspect the condition of the sample injection
needle to confirm that the needle is clear and allows a vertical stream of sample
during injection (see Sec. 9.4.7 below).
- 89
4) Remount the sliding injection block following the reverse procedure as
that described in 1) and 2) above.
9.4.5 Replacing O-ring between injection block and TC combustion tube

(biannually)
There is another O-ring (Teflon-coated O-ring, [PIN 630-01566]), seated

between the fixed part of the sliding injection block and the TC combustion
tube which should be replaced every 6 months. The O-ring is replaced as
follows. (Take care not to scratch the O-rings.)
1) Lift off the instrument top cover by removing the two screws on the
rear panel (see Fig. 9.1).
2) Disconnect the entire sliding sample injection block assembly above the
TC furnace by removing the 2 knurled screws in the mounting plate
and carefully working the assembly upward until it separates from the
combustion tube.
3) Carefully remove the O-ring from its seat accessed from the bottom of
the injection block, and insert a new one in its place.
4) Apply a thin coat of the supplied high vacuum silicon gel on the outer
surface of the combustion tube upper end, and fit the TC port (with
new O-ring) of the sliding sample injection block onto the coated upper
end of the combustion tube.
5) Align the sample injecting block assembly and re-mount it USlng the
two knurled screws.
9.4.6 Replacing O-rings in IC reaction vessel sliding sample injection

block (Quarterly, or monthly with ASI, CSM if IC channel is used)
This procedure is identical to that for the sliding TC sample injection block
(see Sec. 9.4.4 above), except that access is from the open front door.
O-rings in IC reaction vessel sliding sample injection block need not be
changed if measurement via the IC channel is not being pedormed.
There is also an O-ring (pIN 036-11222) in the joint between the injecting
block and IC reaction vessel which should be changed every six months.
This procedure is identical to that for the O-ring between the injection block
and TC combustion tube (see Sec. 9.4.4 above), except that the injection
block assembly is dismounted by removing the two Phillips head screws
from the front of the injection block.
- 90
9.4.7 Cleaning and replacing sample injection needle
Reproducibility is greatly influenced by the manner in which sample is

injected through the TC or IC sample injection needle. Ideally, sample
should be injected as a vertical stream without splashing onto the TC
catalyst or into the IC reaction vessel, as shown in the left-hand example of
Fig. 9.4. The injection pattern is easily monitored by removing the sliding
injection block from its assembly and performing injection in the
MECHANICAL CHECK mode (see Sec. 9.5).
Good Bad Ugly
Figure 9.4 Sample Injection Patterns
If a problem in reproducibility is traced to a poor sample injection pattern

(monitored when the injection block is removed for changing of O-rings,
etc.), the needle should be cleaned or replaced as follows.
Disconnecting needle from injection block

To remove the needle from the injection block, first remove the injection
block as described in Sec. 9.4.4 above, then unscrew the needle fixing nut
in the injection block and pull out the needle and its Viton bushing.
Cleaning needle
Pass the provided cleaning wire through the needle. To remove any residual
foreign matter, place the needle in a sonicating bath for 10 - 15 minutes. If
the obstructing matter cannot be dislodged, replace the injection needle with
a new one.
Remounting needle
Insert the cleaned or new needle with its 2 Viton bushings into the proper
side of the sliding injection block so that the needle end passes into the
concave area on the under-surface of the block (see Fig. 9.5). Fix the
needle in place by screwing down the fixing nut. Confirm that the tip of
the needle does not protrude beyond the sliding surface of the injection
- 91
block. If it does protrude too far, withdraw the needle slightly so that the
needle end emerges through the insertion hole but does not reach the sliding
surface.
CAUTION:
Protrusion of the needle end beyond the sliding surface will damage the O-ring
when sliding, ruining the seal and causing gas leakage.
Sample injection needle
Injection needle gasket

Sliding block
About lmm :b~~~~~~~---_.J
Figure 9.5 Proper Positioning of Injection Needle
With repeated insertion and removal of the injection needle into and from
the Teflon tubing, stretching of the tube will gradually occur and will
eventually cause sample leakage during injection. If this occurs, cut away 5
- 10 mm of the tube end prior to insertion of the needle. Confirm that the
remaining tube length is sufficient to accommodate smooth movement of the
sliding injection block. If the tube is too short, replace it with a new
section of tube (PIN 638-41269).
WARNING:
Be sure that the TC injection block assembly is dismounted and shifted well to
the side of a hot TC furnace while the combustion tube is not mounted. The heat
from the furnace will defonn the injection block.
NOTE:
A severely clogged injection needle will cause leakage at the 4-port valve. If
leakage is noticed at the line connections of the 4-port valve, a clogged injection
needle is likely the cause. If this is confirmed, clean or replace the injection
needle. DO NOT USE A TOOL TO TIGHTEN THE CONNECTIONS AT
THE 4-PORT VALVE IN CASE OF LEAKAGE. This will damage the 4-port
valve, requiring replacement.
- 92
9.4.8 Replacement of soda lime scrubber (annually)
r
The soda lime scrubber (PIN 630-00999) should be replaced once a year.
9.4.9 Replacement of halogen scrubber and membrane nIter (annually or

as needed)
Quartz wool
packing Halogen reactant
I
,.....".---- I
---l-. --"
Membrane
!.ilter ---
c[]1- I
L_ "
Gas flow direction
[IP-i
_J1
Scrubber
~ in! et
1
Replace scrubber before
blue zone reaches here.
Figure 9.6 Halogen Scrubber
The halogen scrubber (located inside the instrument at the upper part of the
rear panel; see Fig. 9.1) absorbs halogens (eI2, Bf2, F2) generated from the
measurement of samples containing common acids and salts (HCI, NaBr,
HCI02, HF, etc.). These halogens must be removed from the flow path to
prevent corrosion of the gold reflective surface on the interior of the optics
in the measurement cell. The halogen scrubber will turn blue (or green) as
it is consumed, the blue zone gradually extending from the inlet toward the
outlet side as absorbed halogen is accumulated. Replace the halogen scrubber
(pIN 630-00992) at least once a year or before the blue zone reaches the
point indicated in Figure 9.6. Temporary baseline fluctuation may occur
immediately after replacement of the halogen scrubber, however, it should
stabilize within about an hour. (Discoloration of the halogen scrubber to a
pale brown may be ignored).
It is recommended that the membrane filter (pIN 638-58088-00), connected

at the oullet side of the halogen scrubber, be replaced al the same time as
halogen scrubber.
Replacement procedure
1) Remove the top cover of the TOC-SOOO.
- 93
2) Open the two bands which secure the halogen scrubber to the rear
panel. Pull off the black Viton reducing unions at each end of the
scrubber. At this. time, also disconnect the membrane filter.
3) Connect a new membrane filter (white end downline), confirming that

the wire clamp secures the small end of the Viton reducing union over
the green end of the membrane filter.
4) Connect a new halogen scrubber so that the arrow mark on the

scrubber points toward the NDIR (toward the downline membrane
filter). Make sure that all connections are secure.
CAUTION:
Replace the entire halogen scrubber. DO NOT attempt to refill the original
container with new internal absorbant. Dispose of the expended halogen scrubber
as plastic waste. The halogen scrubber contains light sensitive p, pi-tetraethyl d:
amino diphenylmethane.
9.4.10 Supply of IC reagent
Check the volume of IC reagent occasionally. If it is depleted, bring the

reservoir of IC reagent up to a volume of 120 - 130m\.
9.4.11 Repositioning silicon tube in IC drain pinch valve (once a month)
The silicon tube connected to the overflow port of the IC reaction vessel
passes down through lhe pinch valve (see Fig. 4.1) to empty into the drain
lube. The silicon tube remains pinched off for prolonged periods, except
occasionally, when the pinch valve opens to allow drainage of IC reaction
solution. Mter a while, the pinched part of the silicon tube becomes
deformed, losing its ability to open up when the pinch valve is opened.
When this happens, the IC drainage cannot be discharged, causing sample
and IC reaction solution to overflow into the dehumidifier.
Periodically shift the portion of the silicon tube in the pinch valve after
manually opening the pinch valve. This is accomplished by setting the
"IC-O" item to ON in the MECHANICAL CHECK screen, accessed from
the MAINTENANCE screen (see Sec. 9.5). When repositioning the tube no
longer alleviates the tube deformation, replace the silicon tube (PIN
630-00344).
- 94
:-:.:-;.>::;.:.:.:.::::::::::::::::::::::::::\~?:::::::::::::':::::::::::':': :-::::;.;.;.:.............
::::::{::::::{::»:{;::>})~:::::::::::::::::::::::::::::::::: .....:.:.:.:...:.:.:.:.:.:.:.:.:...:.:...:.:.:-:.:-:.;.:.;.:.;.:.:.....:.:.:... :.;.:.:::::.:::;::::::::::;:;:;:;;:;::::::=;::::::>:::\{::;:;::: .: .: .: .:1.: .:.:.:.:.:.:.:.~:.·~.: .:·.:j.: ".:.:.':,:.:.:.: ~:.~..·.~:. .:·.;·.:,: .:·.:.:·.'.:.:.:.Y:.:;.:1:]::::::[l~l:::~::::::::~:~:~~:\::::;:~:~~:::~::::::::::::
9.4.13 Washing or replacement of TC combustion tube
The TC combustion tube may be used until it is broken or cracked, which

will result in gas leakage. With prolonged use, the tube will become white,
losing transparency due to reaction with salts in the samples. Even then, the
combustion tube may be used as long as it does not leak gas. When
washing or replacing the catalyst, also wash the combustion tube interior
using 4 - 6N hydrochloric acid solution, and then rinse it in water and dry.
WARNING:
Wait until the TC furnace temperature has decreased sufficiently before
attempting to remove or mount the TC combustion tube (Turn OFF the TC
fUrnace on the GENERAL CONDITION screen.)
Also, be sure that the TC injection block assembly is dismounted and shifted well
to the side of a hot TC furnace while the combustion tube is not mounted. The
heat from the furnace will deform the injection block.
9.4.14 Washing or replacing TC catalyst
If measurement sensitivity or reproducibility is not be restored after

performing the TC regeneration operation (see Sec. 9.3.1), then the TC
catalyst may require washing or replacement.
Washing TC catalyst
If large amounts of salt have accumulated in the TC catalyst due Lo
measurement of samples with high salt content, wash catalyst as follows:
1) Place the catalyst with the platinum screens in a 250ml beaker, and
wash it in purified water to remove all of the salt adhering to the
catalyst.
- 95
2) Neutralize any alkali and reactivate the catalyst by washing with 2N
hydrochloric acid. The catalyst must then be completely dried in a
drying oven at 100°e.
3) When the TC combustion tube is filled with the restored TC catalyst

(see Sec. 4.4) and mounted in the instrument, a large amount of hot
steam may be generated for a while as the TC furnace heats up. For
this reason, leave the tube disconnected at the bottom of the
combustion tube outlet until all of the steam has escaped.
The TC catalyst may be restored to satisfactory condition several times

using this washing procedure. When the performance is not restored by
washing, replace the TC catalyst (pIN 017-42801-01) and the quartz wool
(PIN 603-00557). The platinum screens (PIN 630-00105-01) may be used
indefinitely. One bottle of TC catalyst contains one replacement batch of
catalyst, while a bag of quartz wool contains several replacement batches.
Pack the TC combustion tube with regular sensitivity catalyst referring to
Sec. 4.4.1. It is suggested that a spare TC catalyst be kept on hand.
9.4.15 Replacement of high-sensitivity TC catalyst
Unlike the TC catalyst, the high-sensitivity TC catalyst is not restored to its

original condition by washing. Therefore, if regeneration does not restore
satisfactory measurement sensitivity and reproducibility, replace the
high-sensitivity TC catalyst and clean the platinum screens and combustion
tube with hydrochloric acid. It is recommended that a spare high-sensitivity
TC catalyst (PIN 630-00996) be kept on hand. The two tubes of
high-sensitivity catalyst contain one replacement batch. Pack the TC
combustion tube with high-sensitivity catalyst referring to Sec. 4.4.2.
- 96·
- 97
9.5 MECHANICAL CHECK screen
I SYR PUMP I I INJ PORT I I WASHING I

r--- SOLENOID VALVES ~
IC-D CAR SPRG ACID
~~~~dbdb
@@
~~~~
OFF OFF OFF FF
~~5J
6 11 2
@@BUSY
@@J DDDD
SIZE
DDI@ I
END
@ SYRINGE SIZE, Ill: 4 (1 = 250 2 = 500 3 = 1000 4 = 25(0)
Figure 9.7 MECHANICAL CHECK Screen
This screen appears when "MECHANICAL CHECK" is selected in the

MAINTENANCE screen. The keys indicated in the screen correspond to the
keys on the keypad. Various functions may be carried out manually by
pressing the appropriate keys while in the MECHANICAL CHECK screen,
as outlined below.
Key Indication Function

1 UP Moves microliter syringe plunger up.
2 DOWN Moves microliter syringe plunger down.
3 TC Moves TC sliding injection block with needle (alternates direction).
4 IC Moves IC sliding injection block with needle (alternates direction).
5 on Opens drain discharging pinch valve of IC reaction vessel.
6 off Closes drain discharging pinch valve of IC reaction vessel.
7 on Opens solenoid valve for carrier gas.
8 off Closes solenoid valve for carrier gas.
9 on Opens solenoid valve for sparge gas.
10 off Closes solenoid valve for

_ sparge
___ gas._ _ _ _ _ _ _ _ _ _ _ _ _ _--J
(Continued)
- 98
Key Indication Function
11 on Changes solenoid valve position for IC reagent (acid) gas feed to "feed".
12 off Changes solenoid valve position for IC reagent (acid) gas feed to "stop feed".
13 Lamp Power lamp
14 BUSY When lamp is on, indicates some operation is in progress.
17 IC Opens line between microliter syringe and IC injection port.
18 AUX Opens line between microliter syringe and AUX port.
19 SAMP Opens line between microliter syringe and sampling tube.
20 TC Opens line between microliter syringe and TC injection port.
21 TC Washes microliter syringe and TC injection needle twice.

22 IC Washes microliter syringe and IC injection needle twice.
23 END Ends the mechanical check session and returns to MAINTENANCE MENU.
- 99
9.6 Consumable parts
The following table contains a list of parts and materials that are consumed
and need to be replaced or replenished periodically.
Table 9.1 Consumable Parts List
Part Name Part No. Remarks
TC combustion tube 631-41524

Platinum catalyst, 20g 017-42801-01 Replacement catalyst
High sensitivity TC catalyst 630-00996-00 Replacement catalyst
Chart paper 630-08913-01 For printer, package of 10 rolls
O-ring (inj. slide) 036-11009-84 5 pes included
O-ring (inj. slide, Teflon) 036-11408-84 5 pes included
O-ring (fC port) 630-01566 1 pc included
O-ring (IC vessel) 036-11222-84 5 pes included
Gasket for injection needle 631-43404-84 5 pes included
Needle, injection 630-01565 Needle for sample injection
Needle, sampling 630-02655 Needle for sampling
Microliter syringe, 250 f.l.l 630-02591-04
MItt-qHtersyfipge>~$Oqt+l: < • ·i;3bi 0259V07.<:< . ·········' ': .
~.· .Jl ·g .f~ ~.:p~fr(:~..•e~.•.· '.~ ·.•·n.• .• ·.•.•~.·•.

.·•. .•:. .ev.ri
.• .• .·.r.s.••••• p;.:.·.• . .•.•.•.·.• •.•.•l. . s. • . et.· ·.·.•).·•. i.· ••.•••. ·;..•.••·.••. ·.~·.~· .·:I.~.·~..:. 9.~.'.t.:.'!.!"·M€lg;rr~~fio~l~!W1iq;i~t:1~~r·
ll.'..•. ·•.1.• • . .• •. J.9.:.
• •·...g9f#~qqH]m18i()J Ittt:~y~ipg~> . ..:</
Plunger tip (3 pcs. in a set) 638-60734-05 For 250 ul microliter syringe
Halogen scrubber 630-00992
Silicon rubber tube, 3mm ID, 630-00344 For IC drain pinch valve (1 m)
5mmOD
Soda lime scrubber 630-00999 For purifying purge gas for NDIR optical
system
IC reagent 630-00710
-100
r 10 Principles of operation
10.1 Measurement of TC (Total Carbon)

The TC combustion tube is filled with TC catalyst and heated to 680°C.
Carrier gas (purified air or oxygen) is supplied into this tube after the flow
rate is adjusted to 150mllmin by pressure and mass flow controllers and
moistened by a humidifier.
When sample is introduced into the TC combustion tube via the sample
injector, the TC component in the sample (comprising TOC, [total organic
carbon] and IC [inorganic carbon]) is combusted/oxidized to form C02.
The carrier gas with the combustion product (C02) from the TC combustion
tube flows through the IC reaction vessel and is cooled and dried by a
dehumidifier. It then passes through a halogen scrubber into the sample cell
of the non-dispersive infrared gas analyzer (NDIR), where the C02 is
detected. The NDIR outputs a detection signal (analog signal) which
generates a peak, the area of which is calculated by a data processor.
The peak area is proportional to the TC concentration in the sample. If a

calibration curve expressing the relationship between the peak area and the
TC concentration is obtained using a TC standard solution, the TC
concentration of the sample may be determined from the calculated peak
area. This is an external standard method of calibration.
10.2 Measurement of IC (Inorganic Carbon)
The sample is introduced via sample injector into the IC reaction vessel
(containing IC reagent), through which carrier gas is flowing in the form of
tiny bubbles. Only the IC component in the sample is decomposed to form
C02, which is detected upon reaching the NDIR. The concentration of IC is
determined in the same way as that of the TC. Carbon in the form of
carbonates and hydrogen carbonates may be measured as Ie. The IC reagent
is a solution of phosphoric acid.
10.3 Measurement of TOC (Total Organic Carbon)
The TOC concentration may be determined by subtracting the IC

concentration, obtained as described in Sec. 10.2, from the TC concentration,
obtained as described in Sec. 10.1.
·101
10.4 Measurement of NPOC (Non-purgeable Organic Carbon)
The TOC concentration may be determined directly, using another procedure.

In this case, the sample is acidified beforehand, and then sparged
automatically with purified gas to remove the entire IC component. The
sample is then analyzed to obtain the TC concentration, as described in
Sec. 10.1 above. This method is referred to as the NPOC method.
NPOC (non-purgeable organic carbon) specifically refers to non-volatile

organic carbon which is not eliminated by evaporation during the sparging
process. (Volatile organic compounds, such as organic solvent which are not
readily soluble in water, are eliminated from a sample at room temperature
via sparging. The organic carbon which is evaporated during sparging is
referred to as poe [purgeable organic carbon].) NPOC is identical to the
TOC obtained using the acidify and sparging process described in the
TOC-related standard methods, and referred to in water quality-related test
methods of such organizations as AWWA, ASTM, etc.
10.5 Electronic Signal Processing
The amplifier of the NDIR generates an analog signal corresponding to the

C02 concentration in the carrier gas. The signal is converted by a VIF
converter to a pulse frequency proportional to the input signal. This pulse
signal, insulated by a photocoupler, is read by the CPU, which detects the
peaks, measures the peak area and outputs the result to the LCD and/or
printer.
10.6 Peak Area Measurement
The CPU detects the starting and ending points of peaks generated by
sample injection and calculates the peak area automatically. Detection of
peaks is performed on the basis of the peak gradient (slope of tangent at
every point). When a positive peak gradient exceeds a specified value, the
CPU identifies this as a peak starting point. The peak ending point is
identified when the negative peak gradient becomes smaller than a specified
value.
When a large amount of sample is injected for TC measurement, two peaks

are generated, which are either overlapping or close to each other. In this
situation, the CPU detects the ending point of the latter peak only, and
outputs the total area of the two peaks to the printer. Automatic baseline
correction enables accurate peak area calculation for peaks with a fluctuating
baseline (see Fig. 10.1).
-102
Peak area processing for Peak area processing for
fluctuating baseline multiple peaks
Figure 10.1 Peak Area Processing Method
On detecting a peak ending point, the peak area is displayed on the LCD.
Sometimes, the CPU cannot detect a peak ending point within a specified
period of time (about 4.5 minutes for TC and 3.5 minutes for IC after
sample injection) after detection of the peak starting point. In this case, the
area of the peak generated by the specified time is displayed with a letter T
at the right of the value. If the starting point of a peak is not detected
within 1.5 minutes from the sample injection, the sample will be judged to
have no peaks, and a "0" will be assigned as the peak area.
The peak detection process is displayed in the DATA PROCESSING screen
continuously from the point of sample injection ("INJECTING" is displayed)
until the calculated peak area is displayed (at the end of "MEASURING").
10.7 Calibration Curve
The TOC-SOOO provides the following functions 10 generating calibration

curves.
10.7.1 One-point calibration curve
The output signal of the NDIR is linearized for all ranges. Regardless of
whether TC measurement or IC measurement is performed, the
concentration-output characteristic will not be deviated from linearity. This
constant linearity, therefore, ensures that calibration based on a one- or
two-point calibration curve will be satisfactory for accurate measurement in
most cases. For example, the one point calibration method is quite sufficient
for developing an IC calibration curve or TC calibration curve with
relatively high concentration (lOOmgll or higher) which passes through the
origin. When only one standard solution is specified in the CALIBRATION/
r CONDITIONS screen, the generated one point calibration curve will pass
through the zero origin point.
-103
10.7.2 Multi-point calibration curve
For even more reliable measurement, a multi-point calibration curve may be

created, based on up to four points. Calibration using three or four points
will generate a polygonal calibration curve.
10.7.3 Shifting to origin
The "shift-to-origin" function available in the CALIBRATION CURVE

screen causes a parallel shift of a "non-zeroed" calibration curve so that it
will pass through the zero origin point. This function is useful when the TC
content in the water used for preparing the standard solution is too large to
ignore with respect to the concentration of the standard solution
concentration (or normaLLy when a calibration curve is created for a
standard solution with a concentration no higher than 1 Omg/(). Referring to
Fig. 10.2, if a two-point calibration curve is created using a standard
solution with a TC content of 10 mg/l (actually 10 + amgll), which was
prepared using water containing amgll of TC, the calibration curve generated
will be as indicated by the solid line. Sample measurement using this
calibration curve would always provide results amgll lower than the actual
value. Using the shift-to-origin function to shift the calibration curve so that
it passes through the zero origin point (indicated by dotted line) corrects for
the calibration curve deviation due to the am gil of TC contained in the
water used for preparing the standard solution.
/
/
/
Peak
/
Area
/
/
/
/
/
/
/
01£------------1-
o 10
(a) (10 + a)
TC Concentration, mg/l
Figure 10.2 Shifting Calibration Curve to Origin
-104
10.7.4 Sparging process in measurement of standard solution
r
One of the TC calibration curve conditions which may be set in the
CALIBRATION/CONDITIONS screen is "SPARGE TIME". If a value other
than a is assigned for this parameter, and the sparge tube is appropriately
connected, the standard solution will be sparged with carrier gas at the start
of the measurement sequence for the set period of time. This function is
used when the TC concentration in the standard solution is so low that the
carbon content of the dissolved C02 in the standard solution is enough to
influence the measurement results. The sparging process will eliminate all of
the dissolved C02 in the standard solution.
The concentration of the dissolved C02 in the water used for preparing the
standard solution will be dependent upon the degree to which the water has
been exposed to the atmosphere in the water purification process, during
storage and even during the preparation of the standard solution. Table 10.1
gives an indication of the amount of C02 which is absorbed by distilled
water under different conditions of atmospheric C02 and temperature.
The key factors in determining whether or not sparging should be performed

are the concentration of the standard solution and that of the TOC contained
as an impurity in the water. Sparging is indicated even when the amount of
TOC in the water is negligible if the amount of dissolved C02 is great
enough to significantly influence the concentration of the standard solution.
Table 10.1 Absorption of C02 by Distilled Water
~:!:.emperature(0C)
0 5 15 20 25 30
(VO]~
10
Atmosphere
0.030 1.00 0.83 0.79 0.59 0.51 0.44 0.38
0.033 1.10 0.91 0.76 0.65 0.56 0.48 0.42
0.044 1.47 1.22 1.02 U.87 0.74 0.64 0.56
C02 (mg/I) x 0.27 =C (mg/l)
NOTE: Do not sparge an IC standard solution as this will decrease the Ie

concentration.
-105
10.8 Quantitative calculation
The sample concentration is determined using a quantitative calculation based
on comparison of the measured peak area with that of a calibration curve
developed beforehand. The concentration may be expressed in ppm, ppb,
mg/l or f-lg/l, according to that set in the GENERAL CONDITIONS screen.
10.9 Calculation of Mean Value, Standard Deviation and Coefficient of

Variation
If two or more injections are used in the analysis of a standard solution or
sample, the mean value (MN), standard deviation (SD) and coefficient of
variation (CV) are calculated and displayed on the screen. The SD and CV
values are used to check the reproducibility (fluctuation of measured values
in an identical sample) of the analysis. The maximum number of sample
injections allowed at the initial setting is 10. However, since three more
injections may be added, up to 13 injections per analysis are possible.
10.10 Voiding abnormal values/performing additional measurement by use

\ of SD/CV functions
When multiple injections are used in the analysis of a standard solution or
sample, abnormal values may be detected. If there is a large fluctuation
(with large SD and CV), additional measurement may be conducted
automatically to replace these abnormal values. The procedure is as follows:
1) When setting conditions in the CALIBRATION/CONDITIONS or

SAMPLE MEASUREMENT/CONDITIONS screen tsee Sec 6.4, 6.8), input
a larger value for the item "MAX NO OF INJ" (maximum number of
sample injections) than for "NO OF INJ" (number of sample injections).
This difference between the two settings is the number of additional
measurements to be performed if necessary.
2) Suggested values for SO and CV will be displayed automatically. These

may be modified as appropriate for the specific application.
3) If either the SD or CV of the measured values obtained after n number

of injections is smaller than the set SO or CV setting, the mean value of
the measured values is employed. If both exceed their respective settings,
an additional measurement is conducted, and the SO is calculated for all
combinations of n measured values selected from n + I measured values
to identify a combination for which SO becomes minimum. The selected
combination will then undergo the same comparison with the set SO and
CV. If either the SO or CV is smaller than the SO or CV setting, the
mean value of this combination is used as the measured value. If both
exceed their respective settings, another measurement is conducted. The
above process will be repeated to obtain an adequate mean value until the
-106
number of sample injections reaches the set maximum number of sample
r injections. If none of the measured SD or CV values are smaller than the
corresponding set value, without further measurement, the mean value of a
combination of n measured values providing the smallest SD will be
employed as the measurement value.
Reproducibility is normally judged on the basis of the CV value alone. In
the TOC-SOOO, both SD and CV are used to evaluate reproducibility. When
the carbon content of a sample is small with respect to the measuring
range, the resultant measurement tends to show a large CV. If CV alone
were set, the instrument could not be used to analyze samples with
concentrations that are low with respect to the measuring range. To enable
analysis in this situation, it would be necessary to set a higher CV for a
sample whose concentration is appropriate for the set measuring range.
In contrast, if SD is included as a criterion, it is possible to set CV at an
adequate value for a sample of appropriate concentration. Furthermore, even
when the sample concentration is extremely low, the number of injections
need not be increased unnecessarily.
Since reproducibility may vary depending upon the carbon content,
measuring range, injection volume, and the condition of the instrument, input
r appropriate values for SD and CV depending on the specific application.
10.11 Automatic setting of range and injection volume
When the concentration of a standard solution has been set in the

CALIBRATION/CONDITIONS screen, the instrument will display suggested
suitable values for RANGE and INJ VOL (injection volume). The instrument
will choose from the possible range/injection volume combinations which
will result in a peak height of 50 - 90% F.S. (full scale). Specifically, the
instrument will select a combination with the smallest possible injection
volume that will allow sufficient reproducibility: Injection volume should be
as small as possible to prolong the life of the TC catalyst and IC reagent.
For a standard solution concentration of TC 200ppm (250 microliter syringe
is used), the peak is fairly consistent at about 70 - 90% F.S. when
measurement is conducted at range xl with an injection volume of 3fAI,
range xS with 13fAl and range x30 with 80fAl (although peak height tends to
decrease somewhat with increasing injection volume). However, since 3fAi is
smaller than the minimum possible injection volume, the instrument will
select range x5 with injection volume 13fAl (as the smaller of the selectable
-107
vaLues). As these are only suggested values, they may be changed as
required.
A larger Injection volume may be desirable to offset an increased CV value

due to deflected or splashed sample during injection (caused by foreign
matter in injection needLe, etc.) In the above example, this situation might
warrant the selection of range x30 with an injection volume of 80~1. If the
suggested values are to be changed, the new values should be as close as
possible in volume-to-range ratio as that of the suggested values.
10.12 Automatic selection of optimum calibration curve
If more than one calibration curve is specified when setting measurement

conditions in the SAMPLE MEASUREMENT/CONDITIONS screen, the
"automatic selection of optimum calibration curve" function will become
operative. This function works as follows:
1) Measurement is initially conducted using the first calibration curve (1st
CAL CURVE abbreviated as CAL#1 here.)
2) If the sample concentration (SAMP) is smaller than the standard high

concentration (hereinafter referred to simpLy as concentration) of the first
calibration curve and larger than the concentrations of the other calibration
curves (CAL others), the first calibration curve (CAL#l) is used.
CAL#1 > SAMP > CAL others - CAL#1 is used.
3) If two calibration curves are designated, and the sample measurement
value (SAMP) is smaller than the concentration of the second calibration
curve (CAL#2), which is smaller than that of CAL#l, then the second
calibration curve (CAL#2) is used.
CAL#1 > CAL#2 > SAMP - CAL#2 is used.
If three calibration curves are designated, the function works as

follows:
CAL#1 > CAL other 1 > SAMP > CAL other 2 - "CAL other 1" is used.
CAL#1 > CAL other 1 > CAL other 2 > SAMP - "CAL other 2" is used.
4) If the sample concentration (SAMP) is larger than the concentration of
CAL#l, while the other calibration curve has a higher concentration than
than CAL#l, the function works as follows:
-108
1. When the sample concentration is displayed with an appended "H"
(indicating that peak height exceeds the full scale range of the first
calibration curve), the other calibration curve is used.
CAL other> SAMP H > CAL#1 -- "CAL other" is used.
2. When the sample concentration is not marked with an H, the

instrument compares the ratio of the measured concentration to that of
the first calibration curve (CAL#1) with the ratio of the measured
concentration to that of the other calibration curve (CAL other) to
determine the appropriate calibration curve. In most cases, the first
calibration curve is selected for the following reason: Since the NDIR
is linear for any range setting, and a concentration within the full scale
range will not far exceed the concentration of the first calibration curve
(CAL#1), use of an extended CAL#1 will efficiently provide a
quantitative value at least as accurate as if another calibration curve
were used. Therefore:
CAL other> SANIP > CAL#1 -- In most cases, CAL#1 is used.
3. If the sample concentration is larger than that of the other calibration

curve, the other calibration curve is used.
SAMP > CAL other> CAL#1 -- "CAL other" is used.
5) If the sample concentration is larger than that of the first calibration curve
(CAL#1) and the other two calibration curves have higher concentrations
than CAL#l, measurement will be conducted with the calibration curve of
lower concentration, followed by the procedure described in 4) above.
CAL other 1 > SAMP > CAL other 2 > CAL#1
-- In most cases, "CAL other 2" is used.
SAMP > CAL other 1 > CAL other 2 > CAL#1
-- "CAL other 1" is used.
The following points should also be noted with regard to the automatic
selection of the optimum calibration curve.
The procedures described above are valid for both one-point and
multi-point calibration curves.
• In the case of multiple injections, when the first peak is within the full
scale while succeeding peaks exceed this scale, the instrument will
ignore the fact that the succeeding peaks were over scale and continue
operation on the basis of the first injection. The excess peak height
- 109
beyond the full scale range is considered too small to affect the
measurement.
• The TC catalyst type (NORMAL SENS or HIGH SENS) and the

microliter syringe size used in creating the 1st through 3rd calibration
curves must be the same as those set in the GENERAL CONDITIONS
screen.
Different units may be used for the concentrations of the calibration
curves, providing these units are of the same grouping (i.e. a
combination of ppm and ppb, or mg/l and IJ-g!l). Thus, a calibration
curve developed using "ppm" is compatible with one using "ppb" but
not with one using "mg!l". The unit of concentration need not conform
to that set in the GENERAL CONDITIONS screen.
• For measurements in a wide concentration range, it is recommended to
set the concentration ratio between two calibration curves using a factor
of 5 - 10.
Considering that measurement is always started with the 1st calibration
curve, a calibration curve which is most often used should be specified
as the first calibration curve. The priority of the 2nd or 3rd calibration
curve depends on their standard high concentrations and the
concentration of the sample.
Automatic selection of the optimum calibration curve cannot be used In
measurement based on carbon equivalent (see Sec. 10.14).
- 110
10.13 Automatic change of range and injection volume
One of the conditions which may be specified in the GENERAL

CONDITIONS screen is "AUTO RANGING AND INJ VOL". If this is set
to ON, the range and injection volume may be changed from their original
settings during sample measurement as described in the following paragraphs.
10.13.1 Automatic change of range
If the initially set range is inappropriate for sample measurement, first the
range will be changed. Specifically, if at the first sample injection the peak
height exceeds the full scale (H is displayed in RMK column of
measurement result), the range is changed automatically to that for a higher
concentration, and measurement is conducted again. Thus, an initial range
setting of xl, would be changed to x5 or x30. If the initial setting is
already at the maximum of x30, the range setting is left as it is and the
instrument proceeds to modify the injection volume setting, as described in
Sec. 10.13.2.
• If measurement is possible within the full scale of the new range
setting, the sample is injected the specified number of times, and the
new range setting is displayed in the RMK column. The determined
concentration is displayed after being corrected by a ratio of the new
r range setting to the initial one. For example, if xl is changed to x5,
the peak area measured with the x5 range is applied to the calibration
curve created with the xl range to obtain the concentration, and the
concentration multiplied by five is displayed.
10.13.2 Automatic change of injection volume
In cases where the peak height exceeds the full scale even at the maximum
x30 range, the initial injection volume setting is automatically changed by a
factor of 1/2, 1/5 or 1/2.5. The factor employed is based on the degree to
which the peak height exceeds the full scale. When applying a factor of 1/2
or 1/5 to the initial setting does not result in an integer, the fraction is
rounded off to an integer. Thus, 17.5~1 will be rounded off to 18~1 in
applying a factor of 1/2 to 35~1. The measurement result with the new
injection volume setting is corrected by a ratio of the new setting to the
initial, and the new injection volume setting is displayed in the RMK
column.
The following points should be considered III applying the automatic change
of range and injection volume function.
The ratios used in range change and IllJection volume change contain an
error factor of several percent. This error may become particularly
- 111
significant when the change ratio is large, injection volume is small (for
example, from 8",,1 to 4",,1), or when both range and injection volume
are changed. For this reason, to enable accurate measurement of samples
with a wide range of concentrations, it is recommended to utilize the
"automatic selection of optimum calibration curve" function, described in
Sec. 10.12.
• The "automatic change of range and injection volume" function and
"automatic selection of optimum calibration curve" function (see Sec.
10.12) may be utilized in combination. In this case, if automatic
selection of the optimum calibration curve is not adequate to allow
measurement, automatic changing of range and injection volume are
initiated.
• The "automatic change of range and injection volume" function will not
work reversely to enlarge small peaks (i.e., to obtain a lower instrument
range setting or increased injection volume).
10.14 Measurement based on carbon equivalent
Normal measurement, relying on comparison with calibration curves, uses

concentration in the quantitative calculation. In this case, the injection
volume used in sample measurement must be the same as that used in
developing the calibration curves.
It is also possible to obtain a measurement value by comparing the carbon

content, since the peak area is proportional to the amount of carbon in a
sample, and coexisting components such as water have a relatively small
influence (matrix effect) on the peak area. The carbon content is obtained as
a product of concentration and injection volume. For instance, the amount of
carbon in 10",,1 of sample with 100 mg/l TC is:
100 mg/l x 10",,1 x 10-6 (1/",,1) =1 x 10-3 mg
And that in 50",,1 of sample with 20 mg/l TC is:
20 mg/l x 50",,1 x 10-6 (II",,!) = 1 x 10-3 mg
Since the two samples contain an equivalent amount of carbon, their peaks
have almost the same area. (Actual measurement may contain an error up
to a maximum of 10% due to unavoidable error in injection volume and
influence due to matrix effect.)
The carbon equivalent measurement method may be useful for such

applications as analysis of trace quantities of TOC in pure water. Normally,
when preparing a standard solution, the TC pre-existing in the water to be
- 112
used in preparing the solution in addition to carbon contamination occurring
during the preparation procedure will affect the TC content in the standard
solution. Thus, a standard solution with an intended 1mg/1 of TC may
actually contain a much greater concentration of TC, resulting in a
significant measurement error. Using the carbon equivalent measurement
method, as described below, this effect is minimized, since the standard
solutions used will have TC concentrations 10 times that normally required.
Procedure (This is an example. Syringe sizes and standard concentrations may be

altered to suit specific applications. The TOC·5050 may use only the 250f!1
syringe. The procedure, however, is the same.)
1) Use high sensitivity TC catalyst and, for example, a SOOf!1 microliter

syringe.
NOTE:
The larger the capacity of the microliter syringe, the smaller will be the stroke,
with a greater degree of error between the setting ratio of the sample injection
volume to that of the standard solution and the corresponding ratio in the actual
injection. Therefore, it is recommended to select as small a syringe as possible to
enable the largest possible stroke. For injection of SOf!1 of standard solution and
SOOf.t1 of sample, a SOOf!1 microliter syringe will introduce less error than a
2,SOOf!1 syringe due to its larger stroke.
2) Prepare a standard solution with a TC concentration 10mgil. Specify "10

(mg/l)" for the "1st SID CONC" in the CALIBRATION/CONDITIONS
screen. Then create a one-point calibration curve following the normal
procedure.
3) When performing sample measurement, specify the obtained calibration

curve for the "1st CAL CURVE #" in the SAMPLE MEASUREMENT/
CONDITIONS screen. Also change the displayed injection volume (INJ
VOL) from S3f!1 to SOOf!I, and then perform measurement as usual.
(4) The DATA PROCESSING SAMPLE screen will display the measurement
value obtained by comparing the concentration to 10mg/1 TC, and the
value corrected using the sample injection volume ratio (500f!1/53f-l1 = 9.43
times) at "COR CONC INJ", at the lower right of part of the screen.
Even using this measurement method, the water used to prepare a standard
solution with a TC concentration of 10mg/l may contain too much carbon
to allow accurate measurement. To carry out correction in this case,
generate a two-point calibration curve using Omg/l for the water used in
- 113
preparation of the 10mg/l standard solution. Then use the "SHIFT TO
ORIGIN" function in the CALIBRATION CURVE screen.
NOTE:
When performing measurement using the carbon equivalent method, it is
important that the sample injection volume be no greater than ten times that used
for measurement of the standard solution to mimimize the error inherent in this
method.
10.15 Automatic regeneration of Ie solution

IC solution in the IC reaction vessel, which is acidified with IC reagent,
converts IC components in the sample into C02. However, the acid
concentration in the IC solution gradually decreases due to reaction with IC
and dilution by the injected sample, eventually losing its ability to fully
convert all of the IC into C02. (Since the sample injected into the TC
combustion tube is also drained in to the IC reaction vessel, it also
contributes to the decreased acidity of the IC reaction solution.
Setting the AUTO REGENERATION OF IC SOLUTION to ON in the

GENERAL CONDITIONS screen maintains the appropriate pH of the IC
reaction solution by automatically pumping IC reagent from the IC reagent
reservoir up to the IC reaction vessel in the following circumstances.
• Prior to the initial IC measurement after instrument is turned ON
• Prior to the initial IC measurement following a preset number of
injections and preset volume of injected samples
If tailing peak occurs ("Til is indicated at measurement value) III IC
measurement
- 114
11 TROUBLESHOOTING
11.1 Error Messages
The various error messages described below will be displayed on the screen in
response to an erroneous setting or operation or instrument abnormality. They are
listed in alphabetical order.
NOTE:
If an error occurs requiring the instrument to be turned OFF and then ON again
to restore normal function, the date and time of the error will be printed out (ex.
STOP 06 (JUN)-22-1990).
• CONCENTRATION IS TOO HIGH

This message appears on the CALIBRATION/CONDITIONS screen
when the setting for the concentration of the standard solution is too
high. Measurement may be continued, but the generated peak may
exceed the full scale. Specify a lower concentration or,
~f;:llj~mgHp.~:ro~9f91~~i[§yt~ng~m:·~ggB:·:g~§QQl!~··!iB!~£~.··m;w~lh··~;
sm~lIet:Ufi.~J@:: ::%\:::;<:::::.::.:::/::~::..:: .<:\)::~:: . ««::\:< ..
...... ,' ;.: :.:.:.:.:.:.:.:-:.: -.;.;;.;.;-:.;.:...;.... . ;.;.: ; ; ::::;:{{{{:::~:: }~<{:::r::~~~ ::::~r:r~<tttt:~::{ tt~\\: ;;:::::::::::: :.:.:::::::::/:::~~:::!:~:r~~:r}r . ::~:~:;:~:~::: ~:;:;:;::/::~:~:::::~:~::. -..
• ERROR!! SELECT VALVE DEFECT

This message appears when the 4-port valve position IS not properly
detected. Contact your service representative.
• ERROR!! SYRINGE H.P. DEFECT

This message appears when the syringe pump home pOSItIon (H.P.)
cannot be detected. Contact your service representative.
• ERROR!! SYRINGE PUMP

When syringe pump operation is abnormal due to foreign substances
clogging the sampling needle or injection needle or other reason, this
message appears. Tum OFF the instrument, clean the needle, and turn
ON the instrument again. If the syringe pump operation has been
restored by the above procedure, perform automatic zero point detection
for the syringe pump on the MAINTENANCE screen prior to resuming
measurement.
- 115
• ERROR!! TC FURNACE OVER HEAT (Reversed display)
This message appears when the TC furnace temperature increases above
780°C. If this message appears, the power supply to the TC furnace is
automatically shut off. The message will not be cleared even after the
TC furnace temperature drops below 780°C. Specific service-related
counter-measures are required. Contact your service representative.
• ERROR!! THERMOCOUPLE DISCONNECIED (Reversed display)

This message appears when the TC furnace temperature-detecting
thermocouple wire is broken. Power is not supplied to the TC furnace
while the thermocouple wire is broken. Contact your service
representative.
• ERROR!! THERMOCOUPLE SHORTED (Reversed display)

This message appears when the TC furnace temperature does not nse to
100° C within 10 minutes from the time the TC furnace is turned on
in the GENERAL CONDITIONS screen. It is an indication of a short
circuit in the thermocouple, discontinued power supply to the TC
furnace or other electrical problem. Contact your service representative.
• FIND SYRINGE ZERO POINT ON "MAINTENANCE" DISPLAY (#8)

This message appears when zero point detection of syringe pump is
necessary. Execute zero point detection on the MAINTENANCE screen
after first confirming that the size of microliter syringe mounted is the
same as that specified on GENERAL CONDITIONS screen.
• GENERAL CONDITION MISMATCH

1) If "NO UNIT" is currently specified in the GENERAL CONDITIONS
screen, this message appears on the CALIBRATION/CONDITIONS
screen if a FREE calibration curve No. is used and the NEXT key is
- 116
pressed without setting the range or injection volume. Set the range
and injection volume or, unless there is special reason for using "NO
UNIT", designate a unit in the GENERAL CONDITIONS screen.
2) This message appears when NEXT is pressed in the SAMPLE

MEASUREMENT/CONDITIONS screen if. after a calibration curve No.
is specified, it is cleared on the CAL CURVE FILE LIST screen
without clearing the calibration curve No. in the SAMPLE
MEASUREMENT/CONDITIONS screen. Return to the SAMPLE
MEASUREMENT/CONDITIONS screen and delete the calibration curve
No. which was cleared (or made FREE) in the CAL CURVE FILE
LIST screen.
• GENERAL CONDITION MISMATCH TC CAT (or SYR SIZE, UNIT,

NO OF WASHES or INJ VOL)
This message appears on the CALIBRATION/CONDITIONS screen, or
on the SAMPLE MEASUREMENT/ CONDITIONS screen when a
calibration curve No. is input and one of the conditions (in GENERAL
CONDITIONS screen) of the calibration curve does not conform to the
current setting with respect to the kind of TC catalyst (TC CAT),
microliter syringe size (SYR SIZE), unit (UNIT) or number of washes
(NO OF WASHES). (On the SAMPLE MEASUREMENT/ CONDITIONS
screen, the settings that must conform are the kind of TC catalyst,
microliter syringe size and injection volume.) Select a calibration curve
having general measurement conditions that coincide with the currently
set general conditions .
• GO TO "MAINTENANCE" DISPLAY (#8) THEN REGENERATE IC

SOLUTION
This message appears if AUTO REGENERATION OF IC SOLUTION
is set to OFF on the GENERAL CONDITIONS screen, and a T mark
appears at a peak in IC measurement. It indicates insufficient acid
content in the IC solution. Bring up the MAINTENANCE screen and
execute REGENERATION OF IC SOLUTION (IC reagent is pumped
into the IC solution).
• GO TO "MONITOR" DISPLAY (#6) TO SEE READY STATE

This message appears on the DATA PROCESSING screen after
SAMPLING (before INJECTING), if any conditions required to place
the instrument in the READY state are unsatisfied. Bring up the
MONITOR screen and check the READY conditions. An "NG"
indication for BASE LINE FLUCTUATION or BASE LINE NOISE
will, in most cases, change to "OK" within 10 - 15 minutes, when
-117
the instrument stabilizes. If the BASE LINE POSITION is indicated
NG, pinch or bend the tube leading to the soda lime scrubber at the
rear of unit, and check that carrier gas is bubbling out of the drain
tube end in the drain pot. (Bubbles confirm the absence of significant
gas leakage in the flow line to the measuring cell of the NDIR.) Then
adjust the baseline zero point, referring to Sec. 9.2.1. If the temperature
of the TC furnace or dehumidifier is inadequate after allowing
suffucient stabilization time, contact your service representative.
• MAXIMUM CONCENTRATION IS THE SAME AS OTHER

This message appears on the SAMPLE MEASUREMENT/
CONDITIONS screen when attempting to specify a calibration curve at
CAL CURVE# with the same high concentration value of a curve
already specified. Specify a calibration curve with a different high
concentration value.
• RAM ERROR, ROM ERROR (Reversed display)

This message appears when an error is detected during the initialization
RAM and ROM check. If the same message appears when the
instrument is started in the ALL RESET mode, contact your service
representative.
• SET DATE & TIME ON "MAINTENANCE" DISPLAY (#8)

This message appears when the date and time (year, month, day, hour
and minute) have not been set. Set these on the MAINTENANCE
screen.
• SPARGE GAS FLOW IS SET ON "MAINTENANCE" DISPLAY (#8)

This message appears upon return to the CALIBRATION/CONDITIONS
screen when a value other than zero has been set for SPARGE TIME
on the CALIBRATION/CONDITIONS screen followed by setting
"FLOW" for the SPARGE GAS item on the MAINTENANCE screen.
When SPARGE GAS is set to FLOW, a SPARGE TIME cannot be set
since the sparge gas solenoid valve already open. To clear the message,
- 118
set SPARGE TIME to zero or cancel the FLOW setting for the
SPARGE GAS item on the MAINTENANCE screen.
• TURN MAIN SWITCH OFF THEN TURN IT ON AGAIN

This message appears after the occurrence of a momentary power
outage. Tum OFF the instrument and then tum it ON again.
• UNIT MISMATCH
This message appears on the SAMPLE MEASUREMENT/
CONDITIONS screen when attempting to specify two or more
calibration curve Nos. having different units (i.e., units of a different
grouping; mg! and g! are of the same group, as are ppm and ppb).
Set calibration curves with units of the same group.
11.2 Troubleshooting
This section covers problems that can be checked relatively easily. When the
cause cannot be identified using the following procedures or when replacement of
parts is required, contact your service representative.
I) Error message appears. - Refer to Section 11.1 above.
2) READY lamp does not light. - Bring up the MONITOR screen and identify
the unsatisfied condition which is preventing the instrument from attaining the
READY state.
·119·
3) The baseline remains beyond the auto zero correction range.

(liNG" (no good) indicated for BASELINE POSITION on MONITOR screen)
NO
Carrier gas is leaking.
Eliminate leakage.
NO
Contact service representative.
Deviation of NDIR zero point

Note:
If zero point of NDIR cannot be adjusted,
there may be a defect in the optical
Adjust zero point (Sec. 9.2.1).
component (such as contamination of the
sample cell inner surface), the carrier gas
may be contaminated, or other component
in the flow path may be contaminated.
-120
4) Baseline is not stable.
NO
Carrier gas is leaking.

Eliminate leakage.
NO
Accuml,llation of
Replace Ie catalyst (Sec. 4.4)
NO
Defective dehumidifier
NO
Defective NDIR
Disturbance exists.

Eliminate disturbance.
-121
5) Standard solution provides poor repeatability.
YES
Note: H is printed out
when peak exceeds full
scale.
YES
Note: T is printed out when
Insufficient gas flow rate
peak is not completely eluted
by the end of measurement
Adjust gas flow rate properly.
procedure (tailing peak).
NO
Defective standard solution

Prepare l'Jew sta(ldard
solUtion ~Sec. 7.8).
NO
Defective injection
Wash or replace injection
needle. Sec. 9.4.7)
YES
Inaccurate injection volume
Eliminate bubbles (Sec. 4.9)
YES
Note: Bubbling at the
Water level is low. time of sample injection is
AeJd water to normal.
ralse water level Carrier gas leakage at any
other Lime is abnormal.
IC
NO
Deteriorated TC catalyst
-122
12 Specifications
Types of measurement TC, IC, TOC (IC - IC), NPOC*

Method Combustion/non-dispersive infrared gas analysis
Combustion temperature 680°C
Range 4ppb - 4000ppm (4ppb - 5000ppm for IC)
Analysis time Normally 2 - 3min for TC or IC (maximum 4.5min for TC, 3.5min for
IC)
Repeatability s2000ppm (s2500ppm for IC): Standard deviation within 1% of full
scale range
2000 - 4oo0ppm (2500 - 5000ppm for IC): Standard deviation within
2% of full scale range
Sample introduction Introduction with automatic injector
method
:.·.~~§~~A~~w~t6-i$&TJf$i~~14~~lg~flBgi)·•
Sample injection volume
t~~?(:}::::>::<:· ........... '." '.'." ".' .:.".:.:.",: :::;.. >::>::::::::::::<:'~:::;:;::::< .
Pretreatment method for Automatic sparging

IC
Carrier gas High purity air (filled in a cylinder)
Pressure: Approx. 85psi (6kglcml (max. 7kglcml
Flow rate: 150ml/min (300ml/min including sparging gas)
CPU functions
Signal processing Linearization, baseline correction, peak detection/area calculation
Data processing Concentration calculation by 1- - 4-point calibration curve methods,
automatic selection of optimum calibration curve from 3 calibration
curves, storing of up to 18 calibration curves, automatic deletion of ab
normal values and automatic additional measurement and calculation to
replace deleted values, SD/CV calcuJation, and repeated measurement
with automatic change in range and sample injection volume
Control Sample injector movements, TC furnace temperature, and on/off of car
rier gas and sparge gas
Others Automatic selection of optimum measurement conditions, main-
tenance/check functions, abnormality detection, and timer setting for re
start
Display LCD (white liquid crystal with baCklight)
640 x 400 dots, 88 characters x 22 Jines
Printer 240 dots for graphic, 40 characters/line, chart width 110mm, thermal
printer
Ambient temperature 5 - 35°C
Power requirements AC 100, 110, 115, 120, 220, 230 or 240V as ordered, ±1O%, 5A (normal
power consumption: about 330VA, SO/60Hz
External dimensions About 480W x 520D x 480H (mm) (excluding protrusions)
Weight About 46kg
*NPOC (Non-Purgeable Organic Carbon): TOC measured after sparging
- 123
-124
Index
carbonates, 101
carrier gas, 8, 11 - 12, 60 - 61,67,
3-way cock, 17
81 - 82, 84, 88, 101 - 102, 105,
4-port valve, 11, 19, 92, 115

117, 120 - 123
See also "requirements"
chart paper, 16,22, 100
A cleaning wire, 78,89, 91
CLEAR, 22, 53, 55
abnormal value(s), 106
coefficient of variation
acidification
SeeCV
IC reagent, 49, 62, 69
concentration
NPOC, 75, 80, 102
sample, 40, 45, 49, 54, 69 -70,
alkali, 78 - 80, 85, 96
72 - 73, 78 - 80, 97, 101
area, 30, 34 - 35,37,40,44 - 45,
102, 105 - 112
101-103,106,111 - 112
standard, 30 - 32, 38, 51, 103
ascarite filter, 8
105, 107 - 110, 113, 115
AUTO RANGING, 44, 49, 111
contamination, 13, 73 - 74, 84,97,
AUTO REGENERATION, 49, 87,
113, 120
114, 117
contrast (LCD unit), 22
COR CONC, 45, 113
B CV, 30, 35, 37, 41, 45, 97, 106
108
baseline, 25, 57 - 58, 71, 82 - 84,
93, 102, 117, 120
brightness (LCD unit), 22

D
bubbles, 18,82,88,101,122
dat~ 23, 25,27, 52,60, 62,64, 68,
bubbl ing, 82, 117
115, 118
buzzer, 49
dehumidifier, 25 - 26, 57,61,94,
101, 118, 120 - 121
c dehumidifier drain, 9, 11,81 - 82
dilution factor, 40, 55
calibration curve
drain tube, 9, 17, 81 - 82, 94, 117
auto-selection of, 108 - 110
creating, 29 - 31, 103 -104
displaying, 53
E
calibration curve file
error messages, 115
deleting, 53
list, 41
carbon equivalent, 41, 110, 112
114
-125
F K
F.S., 107
keys
ferrule, 14 ~ 15, 95
cursor, 22, 27
How, 60 ~ 61,67,69, 80 ~ 82,88,

numeric, 22, 27,
101, 120 ~ 122
ilow meter
carrier gas, 11 ~ 12
L
sparge gas, 11
leakage
fluctuation, 25, 27, 57 ~ 58, 93, 102,
at 4-port valve, 20, 92
FREE, 29, 116 ~ 117

gas, 8,69, 82,92, 95,117,122
full scale
LCD unit, 22
See F.S. linearity, 71, 103, 109
G M
grounding, 6 ~ 7
mass flow controller

carrier gas, 11
H matrix, 112
mean value
H, 45,109
SeeMN
halogen scrubber, 79, 81, 84, 93 ~

membrane filter, 81, 84, 93 ~ 94
94, 101
See also "scrubber", "halogen
See also scrubber

scrubber"
high-sensitivity measurement, 73
microliter syringe
humidifier, 11 - 12, 81 - 82, 84

mounting, 18
85, 101,
size, 18
MN, 35, 45, 97, 106
molecular sieve, 8, 84
I
IC reaction vessel, 11,17,62,69,
N
79,81,87,90,94,101,114
IC reagent reservoir, 11, 17,49, 62,

NDIR, 26, 30, 40, 57 ~ 58, 61,
69,81 - 82, 114

64 - 65, 71, 78, 79, 82 ~ 83,
IC solution
101 ~ 103, 120 ~ 121
regeneration, 49, 62, 69, 87, 114,

needle
117
sample injection, 15, 82, 88 - 89,
injection block, 11, 17, 89 ~ 92, 95

91- 92
injection volume, 30, 40, 45, 49, 52,

sampling, 78,82, 88 ~ 89, 115
55, 107 ~ 108, 111 - 112, 114,117,

NON-STOP MODE, 42 - 43
123
NPOC, 1,30,39 - 40, 56, 76, 77,
inorganic carbon, 1, 75, 101

102, 105, 123
.. 126
RMK, 45, 54 - 55, 111
o ROM, 24 - 25,118
O-ring(s), 15 - 17, 84, 89 ~ 92
optimum calibration curve, 108 ""
110,112
s
origin, 37 - 38, 104,
salt, 78 "" 80, 85, 93, 95
overflow cup, 11, 17

sample injection needle
See needle
p sampling needle
See needle
pinch valve, 11, 94
screen
platinum screen, 95 - 96
ALL RESET (INITIAL), 24
plunger (syringe), 18"" 19, 67, 88

CALIBRATION CURVE, 37, 53,
pressure
71, 104, 114
controller, carrier gas flow, 11

CALIBRATION CURVE FILE
controller, sparge gas, 11

LIST, 30 - 31, 51
gauge, carrier gas, 11

CALIBRATION/CONDITIONS,
regulator, 8
29,31,34,36,71,105,107,
PROTECT, 29, 31, 37 - 38, 52

113, 115 - 118
53, 72
DATA PROCESSING SAMPLE,
PT,51
40,42,44,72,113
DATA PROCESSING
STANDAR6, 34, 37,71 -72
Q DATA REPORT, 39, 54, 56
GENERAL CONDITIONS, 28,
quartz wool, 73, 96
30 - 31,36,40,44,47, 48
49, 65, 67 - 68, 72, 87, 106,
R 110 - 111, 114, 116 - 118
INITIAL START, 23 - 24, 27 - 28,
RAM, 24 - 25, 118

67
RANGE, 30, 40, 43, 51 - 52, 58,

MAIN MENU, 25 - 26, 29,31,36,
64, 107
39,41, 47, 49, 53 - 55,57
READY, 7, 25, 33 - 34,43,45

59, 61 - 62, 67 - 68, 71, 73
46,57,63,65,71,82,117,119
MAINTENANCE, 14,28,41,58,
REMARKS
62,68 - 69, 76, 83, R5 - 87,
See RMK
94, 97 - 98, 115 - 11R
repeatability
MEASUREMENT START
See reproducibility
calibration, 32 - 33, 34, 36, 71
rL:producibiJity, 70, 75, 80, 85, 91,

sample, 42 - 43, 44, 72
95 - 96, 106 ~ 107

MECHANICAL CHECK, 63, 65,
requirements
82,94,98
gas, 7 - 8
MONITOR, 46, 57,64,82 - 83,
installation site, 5
117, 119 - 120
-127·
SAMPLE MEASUREMENT!
TC furnace, 48 - 49,58, 60 - 61,
CONDITIONS, 39, 42, 72,

67,71,90,92,95,118
76,106,108,116 -117
temperature, 57,25 - 26,61, 71, 92,
STANDBY OPTIONS, 59
95,116
scrubber
temperature, 74, 82
halogen, 79,81,84,93 - 94, 101

ambient, 5, 121, 123
soda lime, 5, 12,82,84, 93, 100, 117

dehumidifier, 117 - 118, 120, 121
SD, 30, 35, 37, 41, 45, 97, 106 - 107

furnace, 25 - 26, 57,61, 71,92, 95,
soda lime
116
See scrubber
thermal breaker, 7
solids, suspended, 78, 88

total carbon, 101
sparge connector, 19, 76 - 77

total organic carbon, 1, 101
sparge gas flow, 41, 63 - 64, 76

77,118
SPARGE TIME, 30, 33 - 34, 40 u

41,43 - 44, 52, 77, 105, 118
ultra-low, 74
sparging, 30, 74, 75 - 77, 102, 105
ultra-pure, 8, 97
sparging tube, 6, 33, 43, 76, 105
ultra-pure water trap, 11, 97
standard deviation
SeeSD
stock solution, 69 - 70
v
STORED, 29, 31
synnge
volatile organic carbon, 75, 102
See microliter syringe
w
T
W, 40 - 41
T (tailing peak), 30, 41, 45, 87, 114,
WAIT, 34,45, 60, 82
122
wash, 31, 34 - 35, 40 - 41,44 - 45,
tailing (peak)
48,52,82,117
See T
catalyst, 87, 95
TC Blank Check, 63 - 64,75,

glassware, etc., 18, 74
96 - 97
TC catalyst
regeneration of, 14, 62 - 63, 68,

z
85 - 86,88
zero point (syringe), 23 - 25,27
replacing, 13 - 14
28, 32, 43, 62, 64 - 65, 68, 115,
washing, 95
116,118
TC combustion tube
connecting, 14
filling, 13
washing, 95
-128

Shimadzu TOC5000 Manual 2

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Shimadzu TOC5000 Manual 2

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M393-0085D

Total Organic Carbon Analyzer

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3.1.1 Placement and space requirements .5

3.1.2 Environmental requirements .5

3.3 Power Connection and Grounding .6

3.4 Change of supply voltage .7

3.5 Gas requirements .7

3.6 Gas connection

5 Keypad and LCD unit

6 Screen displays and functions 23

6.1 INITIAL START screen (Normal Start) .23

6.2 INITIAL START screen (ALL RESET Start) .24

6.3 MAIN MENU screen ..... .26

6.4 CALIBRATION/CONDITIONS screen .29

6.5 MEASUREMENT START screen (for Calibration) .32

6.6 DATA PROCESSING STANDARD screen .34

6.7 CALIBRATION CURVE screen . . . . .37

6.8 SAMPLE MEASUREMENT/CONDITIONS screen .39

6.9 MEASUREMENT START screen (at Sample Measurement) .42

6.10 DATA PROCESSING SAMPLE screen .44

6.11 GENERAL CONDITIONS Screen . . .48

6.12 CALIBRATION CURVE FILE LIST screen . 51

6.13 DATA REPORT screen .54

6.14 MONITOR screen .57

6.15 STANDBY OPTIONS screen .59

6.16 MAINTENANCE screen .62

7.1 Supplying carrier gas . .67

7.2 Setting syringe size (GENERAL CONDITIONS screen) .67

7.3 Turning on TC furnace (GENERAL CONDITIONS screen) .67

7.4 Zero point detection of syringe pump (MAINTENANCE screen) .68

7.5 Setting date and time (in MAINTENANCE screen) . . . . .68

7.6 Regeneration of TC catalyst (also in MAINTENANCE screen) .68

7.7 Regeneration of IC solution (MAINTENANCE screen) .69

7.8 Preparation of standard solutions . . . . . .69

7.8.1 Preparation of TC (TOC) standard solution .69

7.8.2 Preparation of IC standard solution .70

7.8.3 Storage of standard solutions .70

8.1.1 Preparation for calibration 71

8.1.2 Calibration proced ure 71

8.2 Sample measurement 72

8.2.1 Measurement procedure 72

8.3 High-sensitivity measurement 73

8.3.1 Handling of TC combustion tube with high-sensitivity catalyst 73

8.3.2 Handling of purified water or samples with ultra-low carbon content 74

8.3.3 Dedicated microliter syringe 74

8.3.4 IC removal in high-sensitivity measurement 75

8.3.5 TC Blank Check 75

8.4 Measurement of samples with high IC content 75

8.5 Measurement of samples with suspended solids 78

8.6 Measurement of samples containing acid, alkali or salts 78

8.6.1 Chloric acids and salls 79

8.6.2 Non-chloric acids and salls 79

8.6.3 Alkali samples . 80

8.6.4 Samples containing salts 80

9.1 Daily inspection 81

9.2 Zero adjustment of infrared gas analyzer (NDIR) optical system 82

9.2.1 Adjustment procedure 82

9.2.2 Causes of sudden deviation of baseline position 84

9.2.3 Causes of gradual and chronic deviation of baseline position 84

9.3 Regeneration procedures 85

9.3.1 Regeneration of TC catalyst 85

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