Beruflich Dokumente
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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
3.2 Unpacking .6
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
7 Analysis preparation 67
8 Analysis 71
8.1 Calibration 71
8.4.1 Acidification 76
8.4.2 Sparging 76
9 MAINTENANCE 81
10.9 Calculation of Mean Value, Standard Deviation and Coefficient of Variation . 106
11 TROUBLESHOOTING 115
12 Specifications 123
Table of Figures
Table of Tables
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.
In addition, any descriptions or procedures which do not apply to the TOC-5050 will
be identified with a "shaded" background, as follows:
-1
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-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.)
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
Additional items are available as optional accessories, as listed in Table 2.2. These
items must be ordered separately.
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-4
3 Installation
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-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.
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.
-6
NOTE: The power supply must be stable to ensure reliable operation. Unstable
voltage may adversely affect results in high-sensitivity measurement.
NOTE: Complete grounding is essential not only for safety but also to protect
the logic circuit and microcomputer.
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
I
~AUTION:
• Under no circumstances may untreated, compressed, atmospheric air be used as a
carrier/combustion gas for the TOC-SOOO.
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.
·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
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.
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
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- 10
4 Instrument preparation
Carrier gas_
flow meter
Microliter
syringe Humidifier
Dehumidifier
drain vessel
3-way valve
1) Remove the cap of the plastic dehumidifier drain vessel secured by flexible
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.
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
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)
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
1) Lift off the instrument top cover by removing the two screws on the rear panel.
3) Carefully insert the TC combustion tube (narrow tube portion first) into the
center opening in the furnace.
4)
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.
- 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.
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
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.
A B
4) Apply a very thin coat of grease on the
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
l;;=l;j=_=i=II~:·I=III:·
Procedure
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
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
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.
- 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
5) I ENTER I key
The I ENTER I key is used to validate an entry or a selected condition.
6) ICE!key
The ICE I key is used to clear or delete a key entry which has not yet been
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.
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.
- 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.
2 1 - - + - - - - - - - - - - - TOC-5000
~_ _- - - - - - - - VERSION 2.00
3
r INITlALIZING
4 TC FURNACE OFF
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)
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)
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.
- 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",
6. Date and hour are displayed. When the operation starts in the ALL
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
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
~-f--- 6 MONITOR
AUTO Ie REGF:N: ON
RUZZER : USED
-daMume
Almost all operation procedures are initiated from the MAIN MENU screen.
measurement.
calibration curves.
- 26
r gives information on baseline conditions (i.e. position, fluctuation and
noise).
10. Messages
When the instrument is turned on in the ALL RESET mode (see Sec.
6.2) the following messages are displayed.
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
- 27
When operation is started in ALL RESET mode
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
- 29
removed in the CALIBRATION CURVE FILE LIST screen (see Sec.
6.12) accessed from the MAIN MENU.
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.
- 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
2) Operations
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.
- 31
6.5 MEASUREMENT START screen (for Calibration)
MEASUREMENT START
PRESS [START] -
-8""'D
This screen appears when the [I NEXT II key is pressed in the CALIBRATION/
CONDITIONS screen.
1) Messages
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.
- 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
r
3) NOTES
Use the sparging tube when SPARGE TIME has been set.
·33·
6.6 DATA PROCESSING STANDARD screen
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
This screen appears when the ISTART/STOP I key is pressed to initiate measurement
- 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
2) Operations
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.
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.
- 35
Purpose Key Operation Function
Print IlpRINT!
I~:IJOWing function
t
keys activated)
IIALL PRINT II Entire screen printed out
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.
3) NOTES
- 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
AREA
[ DATA]
S'l'D CONC AHEA #lNJ SD CV
SO.Oppm 27841 3 115 0.41%
TC [ppm] SO.O
PHINT
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.
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
2) Operations
Shift curve through PressOJ and then Shifts calibration curve vertically to pass
origin IENTERI through origin (see Sec. 10.7.3).
Print screen Press I PRINT II· Prints out all data with calibration curve.
3) NOTE
- 38
6.8 SAMPLE MEASUREMENT/CONDITIONS screen
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.
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.
- 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.
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
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:
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
PRESS [START)
S~,,1PL COND
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
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.
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.
4) NOTE
Use the sparging tube when SPARGE TIME has been set.
- 43
6.10 DATA PROCESSING SAMPLE screen
,----------\ 4
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
This screen appears when the ISTART/STOP I key is pressed to initiate 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.
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
* * * * * *
6. Messages
PRESS [START] FOR REINJECTION, IF NECESSARY
- 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
- 46
Purpose Key Operation Function
Print II PRINT I]
(Following function
keys activated)
f-- ~ALL PRINTI] Entire screen printed out
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
M"'O_':allu 11110
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.
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
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
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
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
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.
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
- 52
2) Operations
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
- 53
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.
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#).
- 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]
2) Operations
View next page Press IINEXT PAGEII Displays next page of data.
(Following function
keys become available)
- 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
- RANGE: x3Q
+100%~--------------~
I3ASELINE FLUCTUATION ~
:OK ~
-100% L -_ _...l..-_ _- ' -_ _----'-_ _- - '_ _- - - - '
BASELINE NOISE : OK
a [min] 5 10 15 20 25
'1'4""10111 latJID
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.
- 57
2) Operations
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).
·58·
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
- 59
1) Screen item descriptions
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
5. Messages
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
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
- 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
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.
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.
- 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.
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.
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
This page intentionally left blank.
-66
7 Analysis preparation
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.
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.
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).
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.)
- 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.
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.
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.
- 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.
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
water.
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.
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.
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.
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.
-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).
-74
8.3.4 IC removal in high-sensitivity measurement
:.:;:::: :':
::
NOTE:
Sparging should not be applied to samples containing volatile organic carbon
substances which may be lost during sparging.
-75
8.4.1 Acidification
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
-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.
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
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
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
piece of Teflon tube into the end of the black Viton tube.
-77
8.5 Measurement of samples with suspended solids
The following special factors must be taken into consideration when
• 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.
CAUTION:
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.
- 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.
-79
TOC analysis in a sample containing acid may also be carried out as follows:
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.)
NOTE:
Exceeding pH 11 in untreated samples may cause catalyst poisoning.
- 80
9 MAINTENANCE
- 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.
Pinch off the tubes at the soda lime scrubber, and confirm bubbling in the
dehumidifier drain vessel.
- 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
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.
- 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.
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
- 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.
accessory) with the provided inner cap having a hole, and place the
WMeta.
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:
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.
- 87
9.3.3 Regeneration of TC catalyst and IC solution
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.
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.
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.
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.
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.
NOTE:
needle to confirm that the needle is clear and allows a vertical stream of sample
- 89
4) Remount the sliding injection block following the reverse procedure as
that described in 1) and 2) above.
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.
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
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
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
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.
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.
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).
Replacement procedure
- 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.
CAUTION:
Replace the entire halogen scrubber. DO NOT attempt to refill the original
container with new internal absorbant. Dispose of the expended halogen scrubber
amino diphenylmethane.
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:::~::::::::~:~:~~:\::::;:~:~~:::~::::::::::::
WARNING:
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
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.
- 96·
- 97
9.5 MECHANICAL CHECK screen
~~~~dbdb
@@
~~~~
OFF OFF OFF FF
~~5J
6 11 2
@@BUSY
@@J DDDD
SIZE
DDI@ I
END
(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".
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.
-100
r 10 Principles of operation
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 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.
·101
10.4 Measurement of NPOC (Non-purgeable Organic Carbon)
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.
-102
Peak area processing for Peak area processing for
fluctuating baseline multiple peaks
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").
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
/
/
/
Peak
/
Area
/
/
/
/
/
/
/
01£------------1-
o 10
(a) (10 + a)
TC Concentration, mg/l
-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.
~:!:.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
-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.
-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.
were set, the instrument could not be used to analyze samples with
concentrations that are low with respect to the measuring range. To enable
measuring range, injection volume, and the condition of the instrument, input
-107
vaLues). As these are only suggested values, they may be changed as
required.
curve (CAL#2), which is smaller than that of CAL#l, then the second
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.
CAL#l, while the other calibration curve has a higher concentration than
-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.
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.
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.
- 110
10.13 Automatic change of range and injection volume
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).
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.)
- 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.
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.
(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.
- 114
11 TROUBLESHOOTING
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).
- 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.
- 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.
-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.
- 118
set SPARGE TIME to zero or cancel the FLOW setting for the
SPARGE GAS item on the MAINTENANCE screen.
• 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.
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·
NO
Eliminate leakage.
NO
-120
4) Baseline is not stable.
NO
NO
Accuml,llation of
NO
Defective dehumidifier
Contact service representative.
NO
Defective NDIR
Disturbance exists.
-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
NO
Defective injection
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
:.·.~~§~~A~~w~t6-i$&TJf$i~~14~~lg~flBgi)·•
Sample injection volume
t~~?(:}::::>::<:· ........... '." '.'." ".' .:.".:.:.",: :::;.. >::>::::::::::::<:'~:::;:;::::< .
- 123
This page intentionally left blank.
-124
Index
carbonates, 101
3-way cock, 17
81 - 82, 84, 88, 101 - 102, 105,
coefficient of variation
acidification
SeeCV
IC reagent, 49, 62, 69
concentration
NPOC, 75, 80, 102
101-103,106,111 - 112
ascarite filter, 8
113, 120
114, 117
108
115, 118
buzzer, 49
calibration curve
drain tube, 9, 17, 81 - 82, 94, 117
displaying, 53
E
calibration curve file
deleting, 53
list, 41
114
-125
F K
F.S., 107
keys
ferrule, 14 ~ 15, 95
cursor, 22, 27
ilow meter
carrier gas, 11 ~ 12
L
sparge gas, 11
leakage
full scale
LCD unit, 22
G M
grounding, 6 ~ 7
H matrix, 112
mean value
H, 45,109
SeeMN
94, 101
See also "scrubber", "halogen
high-sensitivity measurement, 73
microliter syringe
85, 101,
size, 18
molecular sieve, 8, 84
I
IC reaction vessel, 11,17,62,69,
N
79,81,87,90,94,101,114
IC solution
101 ~ 103, 120 ~ 121
117
sample injection, 15, 82, 88 - 89,
123
NPOC, 1,30,39 - 40, 56, 76, 77,
.. 126
RMK, 45, 54 - 55, 111
o ROM, 24 - 25,118
110,112
s
origin, 37 - 38, 104,
salt, 78 "" 80, 85, 93, 95
platinum screen, 95 - 96
ALL RESET (INITIAL), 24
pressure
71, 104, 114
regulator, 8
29,31,34,36,71,105,107,
53, 72
DATA PROCESSING SAMPLE,
PT,51
40,42,44,72,113
DATA PROCESSING
STANDAR6, 34, 37,71 -72
30 - 31,36,40,44,47, 48
49, 65, 67 - 68, 72, 87, 106,
64, 107
39,41, 47, 49, 53 - 55,57
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
requirements
82,94,98
gas, 7 - 8
MONITOR, 46, 57,64,82 - 83,
installation site, 5
117, 119 - 120
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SAMPLE MEASUREMENT!
TC furnace, 48 - 49,58, 60 - 61,
76,106,108,116 -117
temperature, 57,25 - 26,61, 71, 92,
STANDBY OPTIONS, 59
95,116
scrubber
temperature, 74, 82
soda lime
116
See scrubber
thermal breaker, 7
ultra-low, 74
ultra-pure, 8, 97
standard deviation
SeeSD
stock solution, 69 - 70
v
STORED, 29, 31
synnge
volatile organic carbon, 75, 102
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
96 - 97
TC catalyst
replacing, 13 - 14
washing, 95
116,118
TC combustion tube
connecting, 14
filling, 13
washing, 95
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