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TOCN-4110 - Instruction - Manual PDF
TOCN-4110 - Instruction - Manual PDF
TOCN-4110 - Instruction - Manual PDF
TOCN-4110 Series
INSTRUCTION MANUAL
SHIMADZU CORPORATION
ANALYTICAL & MEASURING
INSTRUMENTS DIVISION
KYOTO, JAPAN
TOCN-4110
Copyright Shimadzu Corporation 2003. All rights reserved, including those to reproduce this publication or
parts thereof in any form without permission in writing from Shimadzu Corporation.
Read and understand this manual before operation. Save this manual.
Information in this publication is subject to change without notice and does not represent a guarantee on the part
of the vendor.
Any errors or omissions which may have occurred in this publication despite the utmost care taken in its produc-
tion will be corrected as soon as possible, but not necessarily immediately upon detection. We appreciate notifica-
tion of any errors or omissions.
Shimadzu does not have any responsibility for errors or injuries resulting from following the instructions in this
manual.
TOCN-4110
Table of Contents
1 Introduction.............................................................................................. 1
1.1 Precautions.................................................................................................. 3
1.1.1 Operational Precautions ...................................................................... 3
1.1.2 Maintenance Precautions..................................................................... 4
1.2 Specifications............................................................................................... 5
1.2.1 TOCN-4110......................................................................................... 5
1.2.2 TOC-4110............................................................................................ 7
1.2.3 TN-4110 .............................................................................................. 9
2 Installation .............................................................................................. 11
2.1 Parts Inspection.......................................................................................... 11
2.2 Selecting an Installation Site ..................................................................... 14
2.3 Power Connection and Grounding ............................................................ 15
2.4 Drain Tubing Connections......................................................................... 16
2.5 Gas Connection.......................................................................................... 17
2.5.1 Carrier Gas Connection ..................................................................... 17
2.5.2 Exhaust Tubing ............................................................................... 17
2.6 Sample Delivery Lines .............................................................................. 18
2.7 Connecting Input/Output Terminals.......................................................... 19
2.7.1 Contact Output .................................................................................. 19
2.7.2 Contact Input ..................................................................................... 20
2.7.3 Analog Output ................................................................................... 21
TOCN-4110 iii
Table of Contents
3.4 Quantitation................................................................................................ 36
3.5 Auto-setting of Measurement Conditions.................................................. 36
3.6 Auto-modification of Measurement Conditions ........................................ 37
3.7 Operation Panel.......................................................................................... 38
4 Preparations........................................................................................... 39
4.1 Filling the Combustion Tube with Catalyst ............................................... 39
4.1.1 Catalyst for TOC/TN Analysis ........................................................ 40
4.1.2 Catalyst for TOC Analysis .............................................................. 41
4.2 Connecting the Combustion Tube ............................................................. 42
4.3 Filling the Carrier Gas Purification Tubes with Catalyst........................... 44
4.4 Connecting the Carrier Gas Purification Tube........................................... 44
4.5 Filling and Connecting the POC Combustion Tube ................................ 45
4.6 Sample Pretreatment/Injection System Syringe......................................... 45
4.7 IC Removal Acid ....................................................................................... 47
4.8 Dilution Water ........................................................................................... 48
4.9 CO2 (Soda Lime) Absorbers and Ozone Treatment Tube ......................... 49
4.9.1 CO2 Absorber for Carrier Gas Purification ....................................... 49
4.9.2 CO2 Absorber for the Optical System Purge ................................... 50
4.9.3 CO2 Absorber for Sparge (Option) .................................................. 50
4.9.4 CO2 Absorbers for Short Cell Purge (Option) ................................. 50
4.9.5 Ozone Treatment Tube .................................................................... 51
4.9.6 CO2 Absorbers for POC Measurement (Option) ............................. 52
4.9.7 NOx Absorber .................................................................................. 53
4.10 Humidifier (Option) ................................................................................. 54
4.11 Dehumidifier Drain Vessel Water ............................................................. 54
4.12 Printer and Recorder Chart Paper (Option) ............................................... 55
4.12.1 Printer Chart Paper ............................................................................ 55
4.12.2 Recorder Chart Paper......................................................................... 55
4.13 Standard Solution Preparation ................................................................... 56
4.13.1 About Pure Water (Zero Water) ........................................................ 56
4.13.2 TC Standard Solution Preparation ................................................... 57
4.13.3 TN Standard Solution Preparation ................................................... 57
4.13.4 IC Standard Solution Preparation (Option) ..................................... 58
4.13.5 POC Standard Solution Preparation (Option) ................................. 58
4.13.6 TC/TN Mixed Standard Solution Preparation .................................. 58
4.13.7 Filling the Standard Solution Bottle .................................................. 58
4.14 Zero Correction of the Sample Injection Volume...................................... 59
iv TOCN-4110
Table of Contents
5 Measurement .......................................................................................... 61
5.1 TC Catalyst Selection .............................................................................. 61
5.2 Carrier and Sparge Gas Flow Rate Adjustment......................................... 62
5.3 Operation Procedures ................................................................................ 63
5.3.1 On-line Measurement ........................................................................ 64
5.3.2 Off-line Measurement ....................................................................... 69
5.4 Screen Displays, Functions and Operations .............................................. 72
5.4.1 INITIAL Screen ................................................................................ 73
5.4.2 MENU Screen ................................................................................... 74
5.4.3 GENERAL CONDITIONS Screen ................................................... 76
5.4.4 CALIBRATION/CONDITIONS Screen .......................................... 78
5.4.5 CAL CURVE Screen ........................................................................ 82
5.4.6 SMPL MEAS/CONDITIONS (1) Screen ......................................... 83
5.4.7 SMPL MEAS/CONDITIONS (2)-SCHEDULE Screen ................... 86
5.4.8 SMPL MEAS/CONDITIONS (3)-AUTO CAL,CAT REG Screen.. 88
5.4.9 SMPL MEAS/CONDITIONS (4)-ANALOG OUTPUT Screen ...... 90
5.4.10 SMPL MEAS/CONDITIONS (5)-ALARM Screen ......................... 92
5.4.11 ON-LINE MEAS START Screen ..................................................... 95
5.4.12 ON-LINE MEAS START-PAUSE SETTING Screen ..................... 97
5.4.13 ON-LINE MEASURING Screen ...................................................... 99
5.4.14 PEAK PROFILE Screen ................................................................. 101
5.4.15 OFF-LINE MEAS COND (1) Screen ............................................. 103
5.4.16 OFF-LINE MEAS COND(2)-SELECT Screen .............................. 104
5.4.17 OFF-LINE MEAS COND (2)-SPECIFIC Screen........................... 106
5.4.18 OFF-LINE MEAS COND (3) Screen ............................................. 108
5.4.19 OFF-LINE MEASURING Screen .................................................. 110
5.4.20 CALIBRATION START Screen .................................................... 112
5.4.21 CALIBRATION CURVE MEASURING Screen........................... 113
5.4.22 MAINTENANCE Screen................................................................ 114
5.4.23 COUNTER (1) Screen .................................................................... 116
5.4.24 COUNTER (2) Screen .................................................................... 117
5.4.25 SERVICE Screen ............................................................................ 119
5.4.26 MONITOR(C) Screen ..................................................................... 123
5.4.27 MONITOR(N) Screen..................................................................... 124
5.4.28 TREND GRAPH Screen ................................................................. 126
5.4.29 CALIBRATION DATA Screen...................................................... 127
5.4.30 OUTPUT TERMINAL STATUS Screens ...................................... 128
TOCN-4110 v
Table of Contents
5.5 Measuring Samples Containing Suspended Substances .......................... 132
5.6 Handling Samples Containing Acid, Alkali and Salts ............................. 132
5.6.1 Acids and Salts ................................................................................ 133
5.6.2 Alkali Samples................................................................................. 133
5.6.3 Salt Deposits .................................................................................... 134
5.6.4 Dilution Function............................................................................. 134
5.7 Shutting Down the Instrument ................................................................ 135
vi TOCN-4110
Table of Contents
7 Special Accessories............................................................................... 157
7.1 Flow Line Switching Modules ................................................................ 158
7.1.1 Sampling Pipe Set ........................................................................... 158
7.1.2 Suspended Particle Flow Line Switcher.......................................... 159
7.2 Standard Solution Switching Set (2-port and 6-port) .............................. 161
7.3 DF and AD/DF Options ......................................................................... 162
7.4 Recorder................................................................................................... 165
7.5 Printer (Thermal) ..................................................................................... 165
10 Appendix............................................................................................... 191
TOCN-4110 vii
Table of Contents
viii TOCN-4110
1
1Introduction
Thank you for purchasing one of Shimadzu's on-line analyzers.
• TOCN-4110 Total Organic Carbon - Total Nitrogen Analyzer
• TOC-4110 Total Organic Carbon Analyzer
• TN-4110 Total Nitrogen Analyzer
This instruction manual has been written for the TOCN-4110. The following icons are
used throughout the manual in the section headers to indicate the portions of the
manual that are relevant to the specified instruments.
• TOCN : TOCN-4110
• TOC: TOC-4110
• TN : TN-4110
The TOCN-4110 measures both total organic carbon (TOC) and total nitrogen (TN) in
water. TOC measurement is based on the combustion oxidation and nondispersive
infrared detection, while TN measurement is based on the combustion oxidation and
chemiluminescence detection.
Read this manual and keep it with the instrument for future reference.
Note: DO NOT operate this instrument before understanding the CAUTION, NOTE
and WARNING statements in this manual.
Notation Conventions
The following notation conventions are used in this manual.
Convention Description
Indicates the possibility of personal injury or
equipment damage.
CAUTION
Specification Differences
The instrument specifications are different and dependant on the optional attachment(s)
used.
The standard TOCN-4110 and TOC-4110 models are designed to measure Total
Carbon (TC) and Nonpurgeable Organic Carbon (NPOC). However, the options listed
below allow these instruments to perform additional analyses.
This Instruction Manual includes descriptions of the various optional functions. Use
your instrument according to its configuration.
Option Measurement Function
Standard Specification NPOC, TC
With DF option NPOC, TOC (TC - IC), TC, IC
With AD/DF option NPOC, TOC (TC - IC), TOC (POC + NPOC), TC, IC,
POC
When the DF or AD/DF option is included with the TOCN(P)-4110 (enclosure type),
TN and IC cannot be measured during the same analysis.
Refer to Section 3.1.1 through Section 3.1.6, for an explanation of the above terms.
2 TOCN-4110
1.1 Precautions
1.1.1 Operational Precautions
1.1 Precautions
Note: Only authorized Shimadzu service engineers should perform repairs to internal
components of the instrument, as such repairs may pose a danger to the user.
Do not make modifications to this instrument that are not described in this
documentation, as user safety may be jeopardized.
WARNING
This instrument is not explosion proof.
This instrument may be an ignition source.
The appropriate power supply MUST be used. Contact your Shimadzu
representative for the specific power requirements for instruments sold
in your country.
TOCN-4110 3
1.1 Precautions
1.1.2 Maintenance Precautions
1) Do not heat the furnace without a combustion tube. If the furnace must
be heated without a combustion tube, first remove the white plastic
injection port parts to prevent deformation from the radiant heat of the
furnace.
2) Before shutting down the instrument, turn OFF the ozone generator at
least 3 minutes before switching OFF the instrument power. This
allows sufficient time for any residual ozone to be eliminated from the
ozone gas tubing.
3) The furnace operates at either 680°C or 720°C. Cool the furnace
before performing maintenance on the combustion tube. It is
STRONGLY recommended that appropriate protective gloves be worn
unless the furnace is at room temperature.
4) The ozone generator operates at high voltage (6000V). Use care to
avoid electrical shocks.
5) The POC option uses a CO2 absorber filled with lithium hydroxide
(LiOH) anhydride to remove CO2 from the purgeable organic carbon
(POC) measurement flow line. Lithium hydroxide anhydride can be
dangerous. Use extreme care when filling or replacing the LiOH
container. Dispose of the LiOH according to your local regulations.
Refer to Section 9.1 “Material Safety Data Sheets” for precautions for
handling lithium hydroxide anhydride.
6) Hand tighten the fittings to the 8-port sampling valve or 6-port
standards valve. Over tightening the fittings may deform the valve
body and cause leaks or instrument damage.
7) Shut down the instrument completely before performing maintenance
on the syringe drive parts of the Sample Pretreatment/Injection
System. Drive components may suddenly start moving or liquid may
be expelled from detached tubing when the instrument power is not
completely OFF.
8) Sample is supplied to port #2 of the 8-port sampling valve even when
the instrument is not running. Before disconnecting the sample tubing,
ensure that all sample flow is stopped to prevent leakage, spraying or
spilling of liquids that might be hazardous to the operator and/or the
instrument.
Note: Do not use solvents or other chemicals to clean the surface of the instrument.
Instead, wipe the surface with a water-dampened cloth.
4 TOCN-4110
1.2 Specifications
1.2.1 TOCN-4110
1.2 Specifications
1.2.1 TOCN-4110
TOCN-4110 5
1.2 Specifications
1.2.1 TOCN-4110
Alarms*2 Level: Select from High, Ext. high, Low and Ext. low.
Instrument trouble: Warning1, Warning2 and Fatal Error.
Event Signals*2 Ready, Measuring, Calibrating, Regeneration, Pausing, Standby
(TOC/TN), Data Output, Sample Measurement Completed,
Flow Line Identification, Power OFF, etc.
Input Signals Calibration Start, Sample Measurement Start, Measurement
Stop, Alarm Reset
Carrier Gas Pressurized air or oxygen, free of mist, oil, water or particulate
Supply Pressure: 250-300kPa (36-43psi).
Sample Conditions Require flow rate: 1-3 L/min with the sample pipe set
10 L/min with the suspended particle flow line switcher
Temperature: 1-40°C (34-104°F)
Other: Suspensions and slurries may require use of optional suspended
particle flow line switcher. On-board straining (#50 mesh)
requires tap water connection at a pressure of more than 300kPa
(43psi) for rinsing.
Power Supply AC 110, 115, 120, 220, 230 or 240V as ordered, 7A, 50-60 Hz.
Ambient Temperature 0-40°C (32-104°F)
Construction Indoor wall mounting (optional stand available)
Weight Approximately 70kg (154lbs.) main unit only
*1)Analysis time depends on the measurement conditions and sample matrix (this is an example of the
typical measurement conditions).
*2)Contact signal, rating: 1A, 30VDC, noninductive.
6 TOCN-4110
1.2 Specifications
1.2.2 TOC-4110
1.2.2 TOC-4110
TOCN-4110 7
1.2 Specifications
1.2.2 TOC-4110
Sample Conditions Require flow rate: 1-3 L/min with the sample pipe set
10 L/min with the suspended particle flow line switcher
operation
Temperature: 1-40°C (34-104°F)
Other: Suspensions and slurries may require use of optional suspended
particle flow line switcher. On-board straining (#50 mesh)
requires tap water connection at a pressure of more than 300kPa
(43psi) for rinsing.
Power Supply AC 110, 115, 120, 220, 230 or 240V as ordered, 7A, 50-60 Hz.
Ambient Temperature 0-40°C (32-104°F)
Construction Indoor wall mounting (optional stand available)
Weight Approximately 70kg (main unit only)
*1)Analysis time depends on the measurement conditions and sample matrix (this is an example of the
typical measurement conditions).
*2)Contact signal, rating: 1A, 30VDC, noninductive.
8 TOCN-4110
1.2 Specifications
1.2.3 TN-4110
1.2.3 TN-4110
TOCN-4110 9
1.2 Specifications
1.2.3 TN-4110
Sample Conditions Require flow rate: 1-3 L/min with the sample pipe set
10 L/min with the suspended particle flow line switcher
operation
Temperature: 1-40°C (34-104°F)
Other: Suspensions and slurries may require use of optional
suspended particle flow line switcher. On-board straining
(#50 mesh) requires tap water connection at a pressure of
more than 300kPa (43psi) for rinsing.
Power Supply AC 110, 115, 120, 220, 230 or 240V as ordered, 7A, 50-60
Hz.
Ambient Temperature 0-40°C (32-104°F)
Construction Indoor wall mounting (optional stand available)
Weight Approximately 70kg (main unit only)
*1)Analysis time depends on the measurement conditions and sample matrix (this is an example of the
typical measurement conditions).
*2)Contact signal, rating: 1A, 30VDC, noninductive.
10 TOCN-4110
2
2Installation
2.1 Parts Inspection
After opening the shipping container, verify that all of the items listed in Table 2.1
“Standard Accessories” are present in your shipment.
Table 2.1 Standard Accessories
Qty Qty Qty
Part Name Part Number TOCN TOC TN Comment
Accessories Set, TOCN 638-92160-11 1 For TOCN-4110
Accessories Set, TOC 638-92160-13 1 For TOC-4110
Accessories Set, TN 638-92160-15 1 For TN-4110
Included items
1 CO2 absorber 630-00999 3 2 2 Section 4.9,Section 6.3
2 Platinum catalyst, (33g) 638-60116 1 1 1 Section 4.1,Section 4.3
3 Combustion tube 638-41323 1 1 1 Section 4.1
4 L-shaped combustion tube 631-41564 1 1 1 Section 4.3, Section 4.4
5 Quartz wool, (1g) 630-00557 1 1 1 Section 4.1.1,Section 4.3
6 Ceramic fiber 638-60074 1 1 Section 4.1.1
7 Platinum screen, (2 pc) 630-00105-01 1 1 1 Section 4.1
8 Silicon grease, (high vacuum) 017-30812-01 1 1 1 Section 4.2
9 Metallic screen for B-type halogen scrubber 630-60069 1 1 Section 6.8
10 Potassium hydrogen phthalate, (25g) 630-00635-01 1 1 Section 4.13.2
11 Potassium nitrate, (25g) 017-40533-01 1 1 Section 4.13.3
12 Container, 2L (for acid) 638-52444 1 1 1 Section 4.7
13 Container, 500mL (for standard solution) 638-52445 1 1 1 Section 4.13.6
14 Container, 10L (for diluent) 638-52446 1 1 1 Section 4.8
15 Syringe, (5mL) 638-59231 1 1 1 Section 4.6
16 Syringe body retaining screw 631-02330 1 1 1 Section 4.6
17 Syringe holder 631-86046 1 1 1 Section 4.6
18 Catalyst filling rod 638-16023 1 1 Section 4.1
19 Ozone deactivator 638-65233-01 1 1 Section 4.9, Section 6.3.5
20 Key 037-20286-05 2 2 2 For door
21 Bolt, M12x30 (SS) 022-07228 4 4 4 To wall mount instrument
22 Nut, M12 (SS) 023-04074 4 4 4 To wall mount instrument
23 Spring washer, M12 (SS) 023-77085 4 4 4 To wall mount instrument
24 Key wrench 631-78001 1 1 1 Section 6.3.9
25 Hex wrench, (2.5) 086-03819 1 1 1 Section 6.3.8
26 Connecting cord Section 2.3
(UL, CSA) 071-60814-08 1 1 1
(Europe) 071-60814-02 1 1 1
27 Instruction Manual 638-94257 1 1 1
2.1 Parts Inspection
The special accessories listed in Table 2.2 “Special Accessories” are available as
options.
Table 2.2 Special Accessories
12 TOCN-4110
2.1 Parts Inspection
The parts listed in Table 2.3 “Maintenance Parts” are consumable parts or parts that
have a relatively short service life. It is recommended that they be kept on hand to
avoid unnecessary instrument downtime.
Table 2.3 Maintenance Parts
Replacement
Part Name Part Number Comment Interval*
Combustion tube 638-41323 Combustion tube 6 months
L-shaped combustion tube 631-41564 For carrier gas purification and POC option 1 year
Platinum catalyst, 33g 638-60116 Replacement catalyst 2-6 months
High sensitivity catalyst 630-00996 Replacement high sensitivity catalyst TOCN 2-6 months
TOC
Quartz wool, 1g 630-00557
Ceramic fiber 638-60074 TOCN TN
Printer paper 630-08913-01 Printer (option), 10 pcs
Recorder chart paper 080-82564-51 Recorder (option), 5 pcs
Ink pad (6 impacts) 080-82564-55 Recorder (option)
O-ring, Viton, 4D P10A 036-11209-84 Injection port slider, 5 pcs 3-6 months
O-ring, Teflon, P10 036-11408-84 Injection port slider, 5 pcs 3-6 months
O-ring, TC, AS568A-116 630-01566 Combustion tube, 1 pc 1 year
Flared tube 638-41337-03 For off-line measurement
Syringe, (5mL) 638-59231
Plunger tip, (5mL) 638-59161-01 3-4 months
Halogen scrubber 630-00992 3-6 months
Stainless steel net 613-60069 For halogen scrubber type B 6 months
Ball filter (10pc) 630-00681-01 For halogen scrubber type B
CO2 absorber (soda lime) 630-00999 For gas purification 2 months
For NDIR purge (option) TOCN TOC 3 months
For sparge (option) TOCN TOC
For short cell purge (option) TOCN TOC
For NOx absorber TOCN TN
Potassium hydrogen phthalate, (500g) 630-00635-02 For TOC standard solution TOCN TOC
Potassium nitrate, (500g) 017-40533-02 For TN standard solution TOCN TN
Sodium carbonate, (500g) 630-00962 For IC standard solution (option) TOCN TOC
Sodium hydrogen carbonate, (500g) 630-00963 For IC standard solution (option) TOCN TOC
Lithium hydroxide anhydride, (250g) 638-60110-22 For POC measurement (option) TOCN TOC 2 months
Hydrochloric acid, reagent grade 638-58144 For IC removal 2 months
(500mL)
Rotor, 8-port valve 631-56032 For 8-port valve
Stator, 8-port valve 631-56033 For 8-port valve
Packing, Teflon 631-43820-02 For 8-port valve
Sheet, PET 631-80402 For 8-port valve
Flared tubing, 1.6x0.5x250 638-41269-02 For injection
Sample tubing, 1.6x1.0x150 638-41337-05 For sampling
Packing 631-43818 For Chemiluminescence detector TOCN TN
O-ring, 4DP26 036-11228 For ozone generator TOCN TN
Ozone treatment catalyst 638-65232 300g, for ozone deactivator TOCN TN
Polypropylene cotton 630-00325 100g, for ozone deactivator TOCN TN
Viton tubing set 638-42015 For Chemiluminescence detector exhaust TOCN
TN
Consumable parts set, TOCN 638-92176 1 year
Consumable parts set, TOC 638-92176-01 1 year
Consumable parts set, TN 638-92176-02 1 year
* Replacement intervals are suggestions. Actual maintenance requirements will depend
on the sample matrix and measurement frequency.
TOCN-4110 13
2.2 Selecting an Installation Site
WARNING
Internal parts of this instrument operate at high temperatures. Do not
install this instrument where open flames are prohibited.
CAUTION
Flammable substances may be generated if the sample contains
volatile organic materials.
CAUTION
Internal parts of the instrument become very hot. Position the
instrument at least 20cm from the wall for ventilation.
Note: Avoid setting up the instrument near equipment that generates strong magnetic
fields, electrical fields or high frequency waves.
14 TOCN-4110
2.3 Power Connection and Grounding
AC - Hot
FG - Ground
ACC - Neutra
Connect the instrument to a stable power supply with the appropriate voltage (±10
volts) and a supply current capacity of more than 10A. A stable voltage supply is
required for high sensitivity measurement. Voltages outside the allowable range may
result in abnormal operation or damage to the unit. Contact your Shimadzu
representative for the specific power requirements for instruments sold in your country.
Since this instrument is set for both 50 and 60 Hz, a power supply with either of these
frequencies is acceptable.
Complete grounding is important for safety as well as to prevent external noise from
affecting the logic circuits and computer components. The analyzer needs to be
grounded to less than 100 Ω. Refer to power equipment technical standards for details.
The power supply switch in this instrument incorporates thermal breakers instead of
fuses. The switch turns off automatically when there is a surge in the current. If the
thermal breaker becomes tripped, the power may be turned back ON again with the
switch. In the event of repeated breaker trips, locate the problem and take remedial
measures.
WARNING
The instrument should be individually grounded. Avoid connecting the
ground to water pipes, gas pipes or the lightning rod.
TOCN-4110 15
2.4 Drain Tubing Connections
Drain outlet
CAUTION
Drainage occurs by gravity. Resistance to flow in the drain tubing may
result in insufficient drainage and flooding inside the instrument.
Verify that the external drain tubing remains below the drainage
discharge port.
CAUTION
The drain liquid may be acidic. Use caution when handling the drain
liquid.
Note: Locate the drain near the instrument to accommodate the constant flow from
the Flow Line Switcher.
16 TOCN-4110
2.5 Gas Connection
2.5.1 Carrier Gas Connection
Connect the compressed air (or oxygen) supply tubing that will serve as the carrier gas,
sparge gas and ozone source. See Figure 2.2 “Drain / Gas Connection.”
Gas supply: Compressed air or oxygen that is free of dust, oil and water.
Pressure: 250-300kPa (36-43psi)
Gas supply ¼" Male NPT
connector:
This instrument utilizes a gas purifier to remove CO2 from the carrier gas through
catalyst-assisted combustion. Since the purifier has limited capabilities, the supply of
compressed air should adhere to the following conditions:
TOCN-4110 17
2.6 Sample Delivery Lines
2.5.2 Exhaust Tubing
CAUTION
The sample overflow pipe MUST remain open to the atmosphere to
prevent damage to the internal components of the instrument during
sample influent pressure surges. If necessary, an extension pipe
(P/N 631-41593-01) is provided to protect against spills.
18 TOCN-4110
2.7 Connecting Input/Output Terminals
2.7.1 Contact Output
This instrument allows output of event signals, instrument alarms (see Section 5.4.30
“OUTPUT TERMINAL STATUS Screens,”) and concentration value alarms (see
Section 5.4.10 “SMPL MEAS/CONDITIONS (5)-ALARM Screen.”) The signal
input/output terminal board located inside the door on the right side of the instrument is
illustrated in Figure 2.3.
The standard configuration of the instrument supports use of contact output terminals
1-12. Connection of the optional relay board provides added support for output
terminals 13-28. The contact point capacity is 1A, DC30V (noninductive load).
For details on terminal number vs. the various event signals and alarms, refer to
Section 5.4.30 “OUTPUT TERMINAL STATUS Screens” and Section 5.4.10
“SMPL MEAS/CONDITIONS (5)-ALARM Screen.”
Note: Contact output signals are entered in the SMPL MEAS/CONDITIONS (5)-
ALARM screen. The assigned terminal numbers on the OUTPUT
TERMINAL STATUS screen do not include the alarm limits. Contact your
Shimadzu representative for further information on resetting the terminal
assignments.
Refer to Figure 2.5 through Figure 2.9 for the contact output timing charts.
TOCN-4110 19
2.7 Connecting Input/Output Terminals
2.7.2 Contact Input
The following input contacts can be utilized for remote-control. Refer to the diagram
below to set the position on the terminal board.
Contact
Description
Input Number
1 Remote start for sampling flow line 1
2 Remote start for sampling flow line 2
3 Remote start for sampling flow line 3
4 Remote start for sampling flow line 4
5 Remote start for sampling flow line 5
6 Remote start for sampling flow line 6
9 Remote start for calibration
10 Remote stop
11 Remote start for on-line measurement program
12 Alarm reset
13 NC
Over 200msec
Open
Close
Note: Contact input signals are accepted after the contact point is closed for more
than 200msec. Except for the “Alarm Reset” signal, at least a 200msec interval
is required between one contact input signal and the next.
Measurement from a particular flow line is continuous while the corresponding remote
start terminal (No. 1 - No. 6) is closed. When the terminal is opened, measurement
stops after the current measurement. Measurement conditions are listed according to
CONDITION NO on the ON LINE MEAS START screen.
Note: Remote start may be activated from the INITIAL screen. The INITIAL screen
shows the VERSION number and is the one displayed before the MENU
screen.
Note: When more than one remote start terminal is closed at the same time, the
terminal with the lowest number is used. Remote start terminals that are closed
continuously stop other actions from occurring.
When the remote start calibration terminal is closed for a period of more than 200msec,
all of the calibration curves entered in the calibration curve conditions of the
CALIBRATION/ CONDITIONS screen are generated. This includes the calibration
curves specified by CONDITION NO on the ON-LINE MEAS START screen.
20 TOCN-4110
2.7 Connecting Input/Output Terminals
2.7.3 Analog Output
When the remote stop terminal is closed, the operation in progress at that moment stops
and the display reverts to the INITIAL screen.
Note: The remote stop terminal may be activated even when the INITIAL screen is
not displayed.
When the remote start on-line measurement program terminal is closed for a period of
200 msec or more, measurement (including automatic calibration) is made according to
the settings specified by CONDITIONS NO on the ON-LINE MEAS START screen.
TOCN-4110 21
22
Measurement Pause
Measurement Regeneration Wait Measurement Pause Calibration Measurement
Stream1 Stream2 Stream1 Stream2 Stream1 Stream2 Stream1 Stream2
TOCN-4110
Peak
1a 1b 2a 2b 1c 1d 2c 2d 1e 1f 2e
2.7.3 Analog Output
2f 1g 1h 2g 2h
Analog output 1 1a 1b 1c 1e 1g
1d 1f 1h
(hold on)
(hold off)
1a 1b 1c 1e 1g
1d 1f 1h
Analog output 2
2.7 Connecting Input/Output Terminals
2a 2b 2c 2d 2e 2g
(hold on) 2f 2h
Data output
Sample measuring
Contact output
Calibrating
Regeneration
Figure 2.5 Contact Output and Analog Output during On-line Measurement (Two Streams)
On-line meas.
2.7 Connecting Input/Output Terminals
2.7.3 Analog Output
Stream 1 Stream 2
Measurement Measurement
Peak
Contact input 1
Analog output 1
(hold on)
Data output
Sample measuring
Standby (TOC/TN)
Figure 2.6 Contact Output and Analog Output in Remote Start (Single Stream) Operation
Peak
Off-line meas.
Sample measuring
TOCN-4110 23
2.7 Connecting Input/Output Terminals
2.7.3 Analog Output
Calibration
Peak
Calibration
contact input
Off-line meas.
Calibrating
Standby (TOC/TN)
Figure 2.8 Contact Output during Off-line Calibration (Including Remote Calibration)
Off-line measuring
Regeneration
24 TOCN-4110
3
3Operating Principles
3.1 Measurement Principles
The combustion tube is filled with catalyst and heated to 680°C (or 720°C). Carrier gas
(purified air or oxygen) is supplied to this tube at the rate of 150mLmL/min.
When the sample is introduced into the combustion tube, the TC component in the
sample is combusted/oxidized to form carbon dioxide. The carrier gas, with the
combustion product (CO2) flows to the dehumidifier where it is cooled and dried. It
then passes through a halogen scrubber into the sample cell of the nondispersive
infrared (NDIR) detector, where the CO2 is detected. The NDIR outputs an analog
detection signal that generates a peak. The area of this peak is calculated by a data
processor.
The peak area is proportional to the TC concentration in the sample. A calibration
curve is generated by the external standard method, to express the relationship between
the peak area and the TC concentration. The sample TC concentration is determined
from the calculated peak area.
Acidify the sample (pH 2-3) by adding hydrochloric acid to convert IC to carbon
dioxide. Sparging the sample with carrier gas removes the CO2 and carries it to 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 IC.
3.1 Measurement Principles
3.1.3 NPOC (Nonpurgeable Organic Carbon) Measurement
POC is the measurement of the organic component of TOC that is volatilized during
sample sparging for NPOC measurement. The sparge gas passes through the CO2
absorber (LiOH) for POC to eliminate the CO2 from the IC in the sample. The gas then
passes through the POC combustion tube to be oxidized. The resulting CO2 is detected
in the NDIR. Data processing is conducted the same way as for TC measurement. See
Section 3.1.1 “TC (Total Carbon) Measurement.”
POC is not precisely defined. The extent to which an organic compound is volatilized
during sparging, depends on the type of organic, the gas/liquid contact with the sparge
gas, the ambient temperature and the vapor pressure of the component. Since the
organic component in the aqueous solution is the target of measurement, organic
compounds that are highly soluble in water are not easily volatilized by sparging. For
example, only a small percentage of methanol present in a sample is volatilized.
The CO2 converted from inorganic carbon compounds during acidification and
sparging is removed as the sample passes through a CO2 absorber (LiOH). This strong
base may also absorb POC components that are acidic, such as esters.
Therefore, the POC measurement results obtained using this technique are not
absolute. The user should take all of the above factors into consideration when
analyzing for POC using this instrument.
26 TOCN-4110
3.1 Measurement Principles
3.1.5 Choosing a TOC Measurement Method
As in TC analysis, the sample is injected into the combustion tube (720°C), where the
TN content of the sample is converted into nitrogen monoxide (NO). Nitrogen gas is
not converted to NO. The carrier gas, along with the NO, is cooled dehumidified and
exposed to ozone (O3) to convert the NO to NO2 whwew it enters the
chemiluminescent gas analyzer and is detected. The signal from the chemiluminescent
(CLM) detector is converted to a peak, enabling measurement of the TN concentration
in the sample.
The type of nitrogen bond in the sample greatly affects the TN detection rate. A
detection rate of nearly 100% is usually observed for nitrogen in nitrate, nitrite,
ammonia and organic radicals; however, for some organic groups such as hydrazines,
pyrozolones and azide compounds, the detection rate can vary between 10 and 60%.
TOCN-4110 27
3.2 Measurement Operations
3.2.1 Carrier Gas Purification
The amount of impurities in the carrier gas must be extremely small for this instrument
to accurately measure the amount of carbon in a sample. Consequently, this instrument
incorporates a carrier gas purification function.
Compressed air supplied to this instrument passes through the furnace and is heated in
a platinum catalyst-filled L-shaped combustion tube. Organic impurities in the carrier
gas are completely oxidized to CO2 gas that is removed by the CO2 absorber to
produce a clean carrier gas. Compressed air used with this function must meet
instrument grade standards. Cylinders of high purity air or a TOC air generator may
also be used to supply the carrier gas.
3.2.2 Sampling
Water flows continuously through the overflow pipe at the upper left exterior of this
instrument and is sampled through the Sample Pretreatment/Injection System. The
constant sample volume is 3mL. If sample is to be diluted, the necessary amount of
sample is drawn into the syringe and dilution water is added to create a total sample
volume of 3mL.
In the calibration operation, the standard solution is drawn from a standard solution
bottle inside the instrument. The dilution function is available during the calibration
operation.
28 TOCN-4110
3.2 Measurement Operations
3.2.2 Sampling
TOCN-4110 29
3.2 Measurement Operations
3.2.2 Sampling
30 TOCN-4110
3.2 Measurement Operations
3.2.2 Sampling
TOCN-4110 31
3.2 Measurement Operations
3.2.3 Pretreatment (Dilution, Acidification, Sparging)
If a sample is to be diluted, the sample and dilution water are drawn into the syringe as
described in Section 3.2.2 “Sampling.” The syringe plunger descends to a point below
the sparge gas inlet in the sidewall of the syringe, allowing sparge gas to be introduced.
The 8-port valve of the Sample Pretreatment/Injection System is opened to exhaust the
sparge gas. The sample and dilution water are mixed by the sparge gas.
When performing NPOC measurement, the sample and dilution water, if required, are
drawn into the syringe. A fixed amount of acid is drawn from the acid bottle inside the
instrument. Sparging is conducted as described above to remove the IC component and
mix the sample.
In TC, NPOC and TN measurement, a fixed volume of sample in the syringe is injected
into the combustion tube.
Before injecting the sample, the inside of the sample injection tubing (between the
Sample Pretreatment/Injection System and the injection slider) is rinsed with water
from the dilution bottle. As dilution water is being drawn back into the syringe, carrier
gas from the combustion tube is drawn into the sample injection tube. This clean gas
contains no CO2. The sample is then drawn into the syringe and injected. The actual
amount of the sample injected into the combustion tube is equal to the amount of the
sample delivered from the syringe minus the internal volume of the sample injection
tubing. It is necessary to determine the internal volume of the sample injection tubing
(see Section 4.14 “Zero Correction of the Sample Injection Volume”) to determine the
actual amount of sample injected into the TC combustion tube,
In IC measurement, the sparge gas goes directly from the syringe to the NDIR detector.
In IC measurement using the TOC1 measurement method (TC-IC), the sample
remaining in the syringe after IC measurement is then subjected to TC measurement.
In POC measurement using the TOC2 measurement method (POC+NPOC), the sparge
gas is conducted to the POC combustion tube after passing through the CO2 absorber
(LiOH). The sample remaining in the syringe after POC measurement is then subjected
to NPOC measurement.
32 TOCN-4110
3.2 Measurement Operations
3.2.5 Peak Area Measurement
The software automatically detects the start and end points of a peak that is generated
from the NDIR or CLM detector and calculates the peak area. The start and end points
are determined on the basis of slope. When the slope exceeds a preset value, it is
detected as a peak start and conversely, when the slope value decreases below a preset
value, it is detected as the peak end. If the sample volume is large, as in TC
measurement, multiple peaks may be generated. In these cases, only the end point of
the last peak is detected. The total area of two or more peaks is calculated. Baseline
correction is performed to obtain the correct peak area when a peak is generated on a
fluctuating baseline.
3.2.6 Washing
After measurement, flow line washing may be performed as programmed by the user.
Since this function is performed after each injection, the measurement cycle time
becomes longer.
Flow line washing is performed by introducing dilution water and sparge gas into the
sample tubing connected to the Sample Pretreatment/Injection System.
TOCN-4110 33
3.3 Calibration Curve
3.3.1 Calibration Curve
The NDIR output signal is linear throughout the instrument range. The output
relationship does not deviate from a linear curve.
1-point or 2-point calibration curves may be used. A 1-point calibration curve passing
through the origin is sufficient from a practical standpoint for IC or TC calibrations
greater than 100ppm.
The TN output signal from the chemical luminescence gas analyzer is linear within the
specified concentration range of the instrument. 1-point or 2-point calibration curves
may be used. The 1-point calibration curve uses a single intercept through the origin,
while a 2-point calibration curve has both a blank and a standard and can be shifted
through the origin.
A 2-point calibration curve should be used for standard solutions less than 10ppm. The
TC contained in the standard preparation water cannot be ignored in these standards
with respect to the standard solution concentration. Refer to Section 3.3.2 “Shifting to
Origin” for details. Up to nine separate calibration curves may be used.
This function is used when the amount of TC contained in the standard preparation
water used cannot be ignored with respect to the standard solution concentration. The
calibration curve is corrected for the amount of TC in the standard preparation water.
For example, when water containing nmg/L of TC is used to prepare a 10ppm standard
solution (actually 10 + nppm), the calibration curve will appear as shown in Figure 3.4
by the solid line. However, if this curve is used as is, the measured sample will always
show a value nppm less than the true value. Shifting the curve so that it passes through
the origin, as shown by the broken line in Figure 3.4, corrects the curve to compensate
for the nppm TC contained in the standard preparation water.
When there is a system blank, the measured value will be greater by the amount of the
system blank. In most cases, the error due to the TC associated with the standard
preparation water is larger than the system blank. Therefore, Shifting to Origin results
in more accurate measurement values.
In Figure 3.4 “Shifting the Calibration Curve to Origin,” the solid line represents the
actual curve and the broken line is the shifted curve.
34 TOCN-4110
3.3 Calibration Curve
3.3.3 Sparging for Standard Measurement
Peak
area
0 10
(n) (10+n)
TC Concentration (ppm)
The TC standard solution is sparged with carrier gas before generating a TC or NPOC
calibration curve. This function is effective for low concentration standards that might
be affected by dissolved CO2 in the standard solution. Sparging removes the dissolved
CO2. The amount of dissolved CO2 in the standard preparation water is affected by the
standard solution preparation method, the method of storage and the concentration of
CO2 in the surrounding atmosphere. Even if the concentration of the dissolved CO2 in
the standard preparation water is low, further dissolution is possible by contact with air
during the standard preparation. Table 3.1 indicates the relationship between CO2 in
the air and the amount dissolved in water.
This method is appropriate when the TOC in the sample water is low and/or the
dissolved CO2 is so high that it cannot be ignored.
The Shift to Origin function is not used when the sparging function is used on the
calibration standard. It is not necessary to sparge the standard if the Shift to Origin
function is to be used.
Note: Never sparge IC standard solutions. Sparging decreases the IC concentration.
Table 3.1 Relationship Between CO2 in Air and in Distilled Water (ppm)
CO2 in Air (Vol%) Temperature (°C)
0 5 10 15 20 25 30
0.030 1.00 0.83 0.79 0.59 0.51 0.44 0.38
0.033 1.10 0.91 0.76 0.65 0.56 0.48 0.42
0.044 1.47 1.22 1.02 0.87 0.74 0.64 0.56
The CO2 amounts in the above table can be used to calculate the IC amount using the
following formula:
CO2 (ppm) × 0.27 = IC (ppm)
TOCN-4110 35
3.4 Quantitation
3.3.3 Sparging for Standard Measurement
3.4 Quantitation
The sample measurement value is derived from a comparison of the measured sample
peak area to the previously generated calibration curve.
If repeat measurements are conducted, an average value (MN), standard deviation
SD% and coefficient of variation CV% are calculated and displayed on the screen. The
standard deviation and coefficient of variation are used to verify the degree of
reproducibility in repeat measurements.
36 TOCN-4110
3.6 Auto-modification of Measurement Conditions
3.3.3 Sparging for Standard Measurement
TOCN-4110 37
3.7 Operation Panel
3.3.3 Sparging for Standard Measurement
38 TOCN-4110
4
4Preparations
4.1 Filling the Combustion Tube with Catalyst
The type of catalyst used with this instrument differs depending on the type of analysis
performed. To measure both TOC and TN, fill the combustion tube as described in
Section 4.1.1 “Catalyst for TOC/TN Analysis.” To measure only TOC, follow the
directions described in Section 4.1.2 “Catalyst for TOC Analysis.” Be careful not to
contaminate the catalyst or allow foreign matter to mix with the catalyst when filling
the combustion tube. Contamination could cause high blank values or abnormal values.
CAUTION
The combustion tube is made of quartz glass. Use care when handling to
avoid breakage.
Note: New catalyst may result in large blank peaks. Repeated injections of acidified
water or sample will gradually diminish and stabilize the blank peaks.
Measurement fluctuation that could result in significant errors, will result if
analyses are conducted while the blank peaks are still large.
To stabilize the blank peaks to the smallest possible values. Performing repeated
injections of acidified water. Distilled or ion exchange water is acidified to a pH 2-3.
Normally, one hundred 100µL injections are performed with the detector sensitivity set
to “H”. Record the peak areas to verify stabilization of blank peaks. Determination of
the appropriate blank values depends on the quality of the water (concentration of TC
due to impurities) and the expected range of TC concentrations. Blank peaks
corresponding to 1ppm have little effect on measurement values of 100ppm samples.
However, for sample concentrations in the vicinity of 10ppm. Blank peaks must be
stabilized to 0.5ppm or less.
Blank peaks are small and stable in TN analysis, even when new catalyst is used.
Prepare the catalyst for measurement by making ten 100mL injections of distilled
water or ion exchange water with the detector sensitivity set to “H”. The blank peaks
should remain small and pose no problems for analysis.
The electric furnace temperature needs to be changed depending on the type of catalyst
used. An authorized service engineer must perform this change. Contact your
Shimadzu representative if these changes are necessary for your application.
4.1 Filling the Combustion Tube with Catalyst
4.1.1 Catalyst for TOC/TN Analysis
The TOC/TN catalyst is used for both TC and TN analyses. The furnace temperature is
set to 720°C for this catalyst. If the IC component exceeds 10ppm, the TC-IC method
yields an unacceptably low detection rate. Use the NPOC method for TOC analysis in
these situations.
If TN measurement will not be conducted, the catalyst described in Section 4.1.2
“Catalyst for TOC Analysis” is recommended. This catalyst requires a lower furnace
temperature, which increases the service life of both the catalyst and combustion tube.
Combustion tube
140mm
10mm
Ceramic fiber
Platinum catalyst
(alumina spherical
support)
Figure 4.1 Filling the Combustion Tube with Catalyst for TOC/TN Measurement
40 TOCN-4110
4.1 Filling the Combustion Tube with Catalyst
4.1.2 Catalyst for TOC Analysis
Two types of catalyst are available for measuring TOC. These catalysts are the regular
TC catalyst and the high sensitivity catalyst. Do not use either of these for TN
measurement. The furnace temperature is set to 680°C when using these catalysts.
The regular TC catalyst is most commonly used. This catalyst is applicable for the
(TC-IC) method and for the NPOC method of TOC analysis. Fill the combustion tube
with catalyst as described in Figure 4.2. The high sensitivity catalyst option is used to
measure samples with TC concentrations of 1ppm or less. Blank peaks may be larger
with the regular TC catalyst and can interfere with analysis in this range. The high
sensitivity catalyst has insignificant blank values. The high sensitivity catalyst is
mainly used for trace TOC analysis of pure water (less than 1ppm). If the IC
concentration in the sample exceeds 5ppm with the high sensitivity catalyst, the
detection rate is low with the (TC-IC) method. It is recommended that the NPOC
method of measurement be used in these applications. Fill the combustion tube
according to Figure 4.2. Two containers of high sensitivity catalyst are required to fill
the combustion tube. Align the openings of the combustion tube and cylindrical
catalyst container. Use the catalyst-filling rod to push the catalyst into the combustion
tube.
Filling with regular Filling with high
TC catalyst sensitivity catalyst
Platinum Platinum
screens (2) screens (2)
Figure 4.2 Filling the Combustion Tube with Catalyst for TOC Measurement
TOCN-4110 41
4.2 Connecting the Combustion Tube
4.1.2 Catalyst for TOC Analysis
CAUTION
The furnace and combustion tube are VERY HOT. Allow the
combustion tube and catalyst to cool to room temperature before
handling. It is STRONGLY recommended that appropriate protective
gloves be worn if the furnace has not been allowed to cool.
Procedure
1. Insert the catalyst-filled combustion tube, narrow end down, into the 22mm
diameter furnace opening.
CAUTION
The hole at the bottom of the furnace is large enough to allow the
combustion tube to drop completely through the furnace.
2. Apply a very thin layer of high vacuum silicon grease to the outside of the
upper end of the combustion tube (where the O-ring contacts). Firmly insert
the upper end of the combustion tube into the injection port assembly.
Note: Use only a very small amount of silicon grease. Use special care to
ensure that the grease does not contact the inside of the combustion
tube.
3. Refer to Figure 4.5 to connect the scrubber and PTFE union to the bottom of
the combustion tube.
4. Turn the knurled thumbscrews clockwise to secure the sample injection port.
Ensure that there is no up/down movement of the slider at the drive gear
connection. Movement at this connection will adversely affect the seal
between the slider and the Teflon sample injector block O-ring.
5. Stuff quartz wool (P/N 630-00557) into the space at the bottom of furnace to
surround the neck of the combustion tube.
42 TOCN-4110
4.2 Connecting the Combustion Tube
4.1.2 Catalyst for TOC Analysis
Combustion
tube
Furnace
Quartz wool
Furnace
Scrubber
Scrubber
To dehumidifier
TOCN-4110 43
4.3 Filling the Carrier Gas Purification Tubes with Catalyst
4.1.2 Catalyst for TOC Analysis
Bottom of
Carrier gas purifier tube L-shaped
combustion tube
Swage lock
fitting
Platinum catalyst
(alumina spherical support)
Quartz wool
Teflon tubing
Figure 4.6 Filling L-shaped Combustion Tube Figure 4.7 Attaching Installation Fitting to L-
with Catalyst shaped Combustion Tube
CAUTION
Hand-tighten only. Do not use a wrench or tools to tighten. Over
tightening may cause the quartz glass tube to shatter. Wear gloves to
protect hands.
CAUTION
Ensure that the tubing is securely inserted into the fittings. Hot gasses
may be expelled if the tubing becomes detached from the fittings.
44 TOCN-4110
4.5 Filling and Connecting the POC Combustion Tube
4.1.2 Catalyst for TOC Analysis
CAUTION
Hand-tighten only. Do not use a wrench or tools to tighten. Over
tightening may cause the quartz glass tube to shatter. Wear gloves to
protect hands.
WARNING
Installing or changing the syringe can be dangerous because acids are
used in this instrument.
CAUTION
To avoid injury, keep hands away from the Sample
Pretreatment/Injection System while it is in motion.
Note: The syringe barrel is made of glass; use care when handling to avoid breakage.
TOCN-4110 45
4.6 Sample Pretreatment/Injection System Syringe
4.1.2 Catalyst for TOC Analysis
Procedure
Syringe
Holder
Barrel
Surface C
Section A-A
Plunger Sleeve
Plunger Spacer
retaining
screw Sparge gas
Syringe supply port
Figure 4.8 Installing the Syringe Holder Figure 4.9 Syringe Assembly
2. Remove the protective cap from the bottom port of the 8-port valve and attach
the syringe.
CAUTION
Tighten the syringe by hand only: DO NOT USE TOOLS. Over
tightening may cause deformation of the 8-port valve and result in
leakage.
3. Place the syringe holder clip over the barrel of the syringe and rotate it until the
support touches surface C. Refer to Figure 4.8 “Installing the Syringe Holder.”
4. Press [UP] (F1) to raise the plunger holder as far as possible. At this position,
use the plunger retaining screw to secure the plunger to the plunger holder.
Hand-tighten only; do not use tools. Refer to Figure 4.9 “Syringe Assembly”
to connect the sparge gas tubing to the syringe.
46 TOCN-4110
4.7 IC Removal Acid
4.1.2 Catalyst for TOC Analysis
CAUTION
Hydrochloric acid is a corrosive chemical. Refer to the MSDS in
Section 9.1 “Material Safety Data Sheets.”
Pour the IC removal acid into the provided 2-liter bottle and cap the bottle. Place the
bottle on the platform indicated in Figure 4.10 and insert the delivery tube (PTFE tube,
outer diameter 1.6mm) through the hole in the cap until it reaches the bottom of the
bottle.
Figure 4.10 Placement of Humidifier, Acid Bottle and Standard Solution Bottle
TOCN-4110 47
4.8 Dilution Water
4.1.2 Catalyst for TOC Analysis
Dilution water
delivery tube
Tube guide
Dilution water
bottle
Dilution water
bottle support
M6 bolts
48 TOCN-4110
4.9 CO2 (Soda Lime) Absorbers and Ozone Treatment Tube
4.9.1 CO2 Absorber for Carrier Gas Purification
1. Cut off the ends of the two tubes on the cap of the CO2 absorber.
2. Open the door of the instrument and locate two Teflon tubes near the platform
labeled “CO2 Absorber1.” One tube is equipped with a membrane filter and
Viton connector and the other only a Viton connector. Connect the tube labeled
“L1” to the CO2 absorber tube labeled “L.” Connect the tube labeled “S1” to
the CO2 absorber tube labeled “S.” This CO2 absorber is used for carrier gas
purification.
3. Once the CO2 absorber is connected to the tubing, place it on the platform
labeled “CO2 Absorber 1.”
TOCN-4110 49
4.9 CO2 (Soda Lime) Absorbers and Ozone Treatment Tube
4.9.2 CO2 Absorber for the Optical System Purge
4.9.2 CO2 Absorber for the Optical System Purge TOCN TOC
1. Cut off the ends of the two tubes on the cap of the CO2 absorber.
2. Locate the two Teflon tubes near the platform labeled “CO2 Absorber2.” One
tube is equipped with a membrane filter and Viton connector and the other
only a Viton connector. Connect the tubes labeled “L2” and “S2” to the tubes
on the CO2 absorber labeled “L” and “S,” respectively.
3. Once the CO2 absorber is connected to the tubing, place it on the platform
labeled “CO2 Absorber 2.”
Install this CO2 absorber if the instrument is equipped with the DF option or the
AD/DF option.
1. Cut off the ends of the two tubes on the cap of the CO2 absorber.
2. Locate two blue tubes near the platform labeled “CO2 Absorber 3.” One tube is
equipped with a membrane filter and Viton connector and the other only a
Viton connector. Connect to the tubes labeled L3 and S3 to the tubes on the
CO2 absorber labeled “L” and “S,” respectively.
3. Once the CO2 absorber is connected to the tubing, place it on the platform
labeled “CO2 Absorber 3.”
4.9.4 CO2 Absorbers for Short Cell Purge (Option) TOCN TOC
Install this CO2 absorber if the instrument is equipped with the DF option or the
AD/DF option.
1. Cut off the ends of the two tubes on the cap of the CO2 absorber.
2. Locate the two Teflon tubes near platform labeled “CO2 Absorber 4.” Both
tubes are equipped with a Viton connector. These are connected to the tubes
labeled “L4” and “S4” to the tubes on the CO2 absorber labeled “L” and “S,”
respectively.
3. Once the CO2 absorber is connected to the tubing, place it on the platform
labeled “CO2 Absorber 4.”
50 TOCN-4110
4.9 CO2 (Soda Lime) Absorbers and Ozone Treatment Tube
4.9.5 Ozone Treatment Tube
1. Remove the gas inlet and outlet caps from the ozone treatment tube.
2. Insert the ozone treatment tube between the heat shield and the furnace. The
gas inlet end of the ozone treatment tube is placed to the top, as shown in
Figure 4.13.
3. Connect the Viton tubing on the right side of the furnace to the inlet end of the
ozone treatment tube and secure it with the supplied hose clamp.
4. Connect the Viton exhaust tubing located below the furnace to the outlet end of
the ozone treatment tube and secure it with the supplied hose clamp.
Gas inlet
TOCN-4110 51
4.9 CO2 (Soda Lime) Absorbers and Ozone Treatment Tube
4.9.6 CO2 Absorbers for POC Measurement (Option)
Fill the CO2 absorber for POC measurement with lithium hydroxide anhydride crystals
using the following procedure.
WARNING
The lithium hydroxide anhydride fine powder crystals are strongly
alkaline and corrosive. Review the MSDS in Section 9.1 “Material
Safety Data Sheets” before handling.
Procedure
Cap
Nipple
O-ring
CAUTION:
Do not tightly pack the quartz wool CO2 absorber container
or the lithium hydroxide anhydride. for POC measurement
WARNING
The CO2 absorber for POC measurement is made of glass. Handle
with care. Wear gloves to prevent hand injuries.
2. Install the CO2 absorber for POC measurement using the clamp shown in
Figure 4.15 and connect the tubing.
52 TOCN-4110
4.9 CO2 (Soda Lime) Absorbers and Ozone Treatment Tube
4.9.7 NOx Absorber
Note: When lithium hydroxide anhydride is exposed to air, CO2 in the atmosphere is
quickly absorbed. Such exposure decreases the service life of the material.
Minimize handling and connect the tubing to the filled container immediately.
Furnace
Clamp
The Soda Lime CO2 absorber is used as the NOx absorber. Connect the NOx absorber
as follows.
Procedure
1. Cut off the ends of the two tubes on the cap of the CO2 absorber.
2. Locate the two Viton tubes below the furnace. Both tubes are equipped with
Viton connectors. Connect the tubes labeled “L5” and “S5” to the tubes on the
CO2 absorber labeled “L” and “S,” respectively.
3. Once the CO2 absorber is connected to the tubing, place it below the furnace.
TOCN-4110 53
4.10 Humidifier (Option)
4.9.7 NOx Absorber
Fill the humidifier container with pure water through the supply opening to the upper
level indicator. Three pellets of NaOH may be added to help maintain the water quality.
Wrap the glass threads one time with Teflon tape and replace the cap.
Place the humidifier as indicated in Figure 4.10 “Placement of Humidifier, Acid Bottle
and Standard Solution Bottle” and secure it with the mounting clip.
Connect the Teflon tube labeled “L” to the longer glass tube of the humidifier and the
Teflon tube labeled “S” to the shorter glass tube of the humidifier.
Note: DO NOT reverse these connections.
CAUTION
There should be no water in either glass tube. The long tube MUST be
above the water level.
54 TOCN-4110
4.12 Printer and Recorder Chart Paper (Option)
4.12.1 Printer Chart Paper
Procedure
1. Place the chart paper on the chart paper roller. Place the roller in the chart
paper holder.
2. Fold the leading edge of the chart paper diagonally and manually feed the
paper into the chart paper feed slot. Verify that the Shimadzu Corporation
name is visible as it is fed through the printer slot. Switch on the power and
then press the (FEED) key to feed the paper through the printer. This is a
thermal printer. If the paper is mounted incorrectly, printing will not occur.
Note: Do not print unless there is paper in the printer. Printing without paper may
damage the print head.
Procedure
1. Pull out the chart paper supply bin and insert well-loosened paper with the
printing side of the chart paper facing up.
2. With the chart paper retainer pulled down, pull out the chart paper. Align the
chart paper sprocket holes with the drum feed pins and pull out 2-3 sections of
chart paper so that it folds correctly in the collector stand.
3. Return the chart paper retainer and holder to their original positions.
TOCN-4110 55
4.13 Standard Solution Preparation
4.13.1 About Pure Water (Zero Water)
Pure or zero water refers to a standard solution with zero concentration of TC, IC or
TN or the water used to prepare these standard solutions. The water stored in the
dilution water container is used for sample dilution and should be pure water. Water
that is in theory absolutely free of carbon (TC) or nitrogen (TN) is used as zero water. It
is difficult, in practice, to obtain this type of water. Even ultra-pure water obtained
using a high-performance membrane technique or water that has been repeatedly
distilled will have a TC content of about 10ppb. This value is measured directly after
manufacture and increases when the water is stored in a container. Carbon dioxide is
contained in the atmosphere at 300-500mg/L. The CO2 content is higher in a room
with many people or where combustion equipment is used. This carbon dioxide
dissolves in the water and is present as IC. The dissolved amount is generally about
0.2mg/L, but is dependent on the water temperature and carbon dioxide content of the
air in contact with the water. Refer to Table 3.1 “Relationship Between CO2 in Air and
in Distilled Water (ppm)” page 35. Instruments that prevent contact with air are not
incorporated in water up-take, retention or storage during common distillation and
purification of water. For this reason, IC is present in most distilled or purified water.
There are cases where the TC content in distilled water commercially available in
plastic or glass containers is 1ppm.
The purity of water required for zero water varies depending on the analysis range.
There would be no problems using commercially available purified water for a sample
containing more than 200ppm carbon. The quality of the zero water should be
considered along with the analysis range. In low-level applications, a direct delivery
system from a water purification system may be necessary.
56 TOCN-4110
4.13 Standard Solution Preparation
4.13.2 TC Standard Solution Preparation
Accurately weigh 7.219g of reagent grade potassium nitrate into a 1-liter volumetric
flask. Dissolve in and dilute to volume with zero water. This stock solution has a
concentration of 1000mg/L (1000mgN/L) = 1000ppmN. Prepare working standards
following the procedure in Section 4.13.2 “TC Standard Solution Preparation.”
TOCN-4110 57
4.13 Standard Solution Preparation
4.13.4 IC Standard Solution Preparation (Option)
Accurately weigh 3.50g of reagent grade sodium hydrogen carbonate that was
previously dried for 2 hours in a silica gel desiccator and 4.41g of sodium carbonate
previously dried for 1 hour at 280-290°C and cooled in a desiccator in a 1-liter
volumetric flask. Dissolve in and dilute to volume with zero water. This solution has a
concentration of 1000mgC/L=1000ppmC. Except for the addition of the diluted
hydrochloric acid, prepare working standards following the procedure in
Section 4.13.2 “TC Standard Solution Preparation.” Do not add the hydrochloric acid
to the IC standard solution.
Note: IC standard solutions are also used as standards for POC measurement. Stock
and standard solutions should be sealed tightly and stored at 4°C.
The IC standards are used for POC analysis. Refer to Section 4.13.4 “IC Standard
Solution Preparation (Option).” Because of the stability of the carbonates and
bicarbonates, solvents such as benzene and chloroform may be used as standard
solutions. However, the solubility of these organic solvents is extremely low as
compared to water, making it difficult to prepare standard solutions of the required
concentrations. The concentrations of these prepared standards are not very stable, so
handling them is somewhat difficult.
Do not add any acid to the POC standard solution.
A mixed TC/TN standard solution may be used when TC (or NPOC) and TN are
analyzed simultaneously. If the optional standard solution switching set is not installed
it is necessary to use a mixed standard, because in this configuration only one standard
bottle may be used.
TC/TN mixed standard solution is prepared by mixing the respective standard
materials, according to the description in Section 4.13.2 “TC Standard Solution
Preparation” and Section 4.13.3 “TN Standard Solution Preparation.” Add diluted
hydrochloric acid to the standard solution as described in these preparations.
Pour the standard solution into the provided standard solution bottle (500mL
polyethylene container), cap and label. Place the bottle on the stand in the position
indicated in Figure 4.10 “Placement of Humidifier, Acid Bottle and Standard Solution
Bottle” page 47. Insert the standard solution delivery tube (Teflon tube, outer diameter
1.6mm) through the opening in the center of the cap, until it reaches the bottom of the
container.
58 TOCN-4110
4.14 Zero Correction of the Sample Injection Volume
4.13.7 Filling the Standard Solution Bottle
Procedure
2. Fill the dilution water bottle with pure water and press the (START / STOP)
key. This initializes the Sample Pretreatment/Injection System.
3. Detach the slider from the injection port by pulling forward on the slider. It is
not necessary to detach the sample injection tube from the slider.
5. When the surface of the dilution water is aligned with the end of the sample
injection tubing, press the (ENTER) key. The internal volume of the sample
injection tubing is entered into the instrument and the display returns to the
MAINTENANCE screen. The internal volume value is preserved even if an
ALL RESET is performed.
CAUTION
To avoid injury, keep hands away from the Sample
Pretreatment/Injection System while it is in motion.
TOCN-4110 59
4.14 Zero Correction of the Sample Injection Volume
4.13.7 Filling the Standard Solution Bottle
60 TOCN-4110
5
5Measurement
Two types of TC catalysts may be used with this instrument, Regular TC catalyst and
High Sensitivity catalyst.
Regular TC catalyst is typically used for higherppm analyses. The High Sensitivity TC
catalyst has a lower blank value and should be used when analyzing samples having a
TOC content of 1ppm or less.
High Sensitivity catalyst is used in low/ultra-low level analyses. There is a 5ppm IC
concentration limitation when using the High Sensitivity catalyst. High IC
concentrations physically damage the catalyst bed by causing the quartz wool fibers to
become brittle. There are no limitations with respect to TOC. Although the High
Sensitivity catalyst bed may be used for the entire analysis range, it costs more than the
Regular TC catalyst.
Note: The High Sensitivity catalyst cannot be restored for reuse by washing, as is
possible with the Regular catalyst.
5.2 Carrier and Sparge Gas Flow Rate Adjustment
Adjust the carrier gas flow rate meter to 150mL/min. by turning the carrier gas flow
adjustment knob. The combustion tube must be installed, the dehumidifier drain vessel
filled and all other flow lines completely plumbed before this adjustment can be
performed.
Select the SPRG GAS VALV item in the SERVICE, MECHANICAL CHECK screen.
Refer to Figure 5.32 “MECHANICAL CHECK Screen” page 120 to supply the sparge
gas. Adjust the flow rate using the sparge gas adjustment knob until the carrier/sparge
gas flow meter reads in the range of 50-150mL/min. The greater the sparge gas flow
rate, the faster the IC is eliminated from the sample. Set the flow rate based on the
characteristics of the sample. Adjust the sparge gas flow rate to a point where the IC is
completely removed from the sample during the allocated sparge time.
CAUTION
Do not allow the supply pressure of carrier gas to this instrument to
exceed 300kPa (43psi). Do not set the carrier gas internal pressure
gauge to greater than 200kPa (28psi). Excessive pressure may damage
the instrument components.
62 TOCN-4110
5.3 Operation Procedures
TOCN-4110 63
5.3 Operation Procedures
5.3.1 On-line Measurement
1. Supply carrier gas from the supply source to the instrument at a pressure of
approximately 250-300kPa (38-45psi).
Normal Start All Reset Start
2. Switch the power ON, then 2-1. While pressing the (ENTER)
switch the furnace ON. key, switch the power ON;
release the (ENTER) key and
switch the furnace ON.
4. Open the door and enter items (1) - (4) as shown below.
(1) Carrier gas pressure 200kPa
(2) Carrier gas flow rate 150mL/min. (adjust as necessary)
(3) Sparge gas flow rate 50-150mL/min.
(4) Ozone air source gas flow rate 0.5 L/min. (TOCN, TN)
64 TOCN-4110
5.3 Operation Procedures
5.3.1 On-line Measurement
CAUTION
Enter the type of catalyst actually being used
in the instrument.
TOCN-4110 65
5.3 Operation Procedures
5.3.1 On-line Measurement
66 TOCN-4110
5.3 Operation Procedures
5.3.1 On-line Measurement
TOCN-4110 67
5.3 Operation Procedures
5.3.1 On-line Measurement
14. Use the following procedure to shut down the instrument. Refer to Section 5.7
“Shutting Down the Instrument.”
1) Turn the ozone generator switch OFF.
2) Turn the furnace switch OFF.
3) After waiting 30 minutes, turn the power switch OFF.
4) Shut off the carrier gas supply at the source.
Note: Turn the furnace OFF at LEAST 30 minutes before switching off the
instrument power. This allows sufficient time for cooling and prevents damage
to the injection port and catalyst bed.
Note: Turn the ozone generator OFF at LEAST 3 minutes before switching off the
instrument power. This allows sufficient time for any residual ozone to be
eliminated from the ozone gas tubing.
Before shutting down the instrument for an extended period of time, fill the sampling
line (sampling pipe or pretreatment module) with clean water and use this water to
perform several measurements to rinse the flow lines.
68 TOCN-4110
5.3 Operation Procedures
5.3.2 Off-line Measurement
TOCN-4110 69
5.3 Operation Procedures
5.3.2 Off-line Measurement
70 TOCN-4110
5.3 Operation Procedures
5.3.2 Off-line Measurement
15. The display remains on the MEASURING(C) or (N) screen after sample
measurement is complete. After printing the results with the optional printer,
press [RETURN] (F1) to return to the MENU screen.
TOCN-4110 71
5.4 Screen Displays, Functions and Operations
5.3.2 Off-line Measurement
ON-LINE OFF-LINE
CALIBRATION
MEAS MEAS MENU
START
START COND(1)
PAUSE CALIBRATION
SETTING CURVE GENERAL CONDITIONS
MEASURING
ON-LINE
MEASURING CALIBRATION/CONDITIONS CAL CURVE
SAMPLE
OFF-LINE OFF-LINE MEASUREMENT (2) (3)
MEAS MEAS /CONDITIONS (1)
COND (2) COND (2)
-SELECT -SPECIFIC
(5) (4)
VALVE DRYING
OFF-LINE
MEASURING
SERVICE MECHANICAL CHECK
MONITOR(C) MONITOR(N)
TREND GRAPH
72 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.1 INITIAL Screen
Display
1) This screen displays the results of the RAM check. If an error occurs,
ERROR is displayed in the upper left corner and the function keys will
not operate. In this instance, it is necessary to perform an ALL RESET
as described in item 3) below.
2) The ROM version number is displayed in the center of the screen.
3) The ALL RESET start is performed when the power is switched on
with the (ENTER) key pressed. ALL RESET is displayed below the
version number.
CAUTION
When starting up using the ALL RESET function, all settings except
for the calibration curve conditions and part of the data will be deleted.
TOCN-4110 73
5.4 Screen Displays, Functions and Operations
5.4.2 MENU Screen
Functions
This is the first screen to appear when the power is switched ON. This screen
displays the model name, ROM version number and the result of the RAM
check.
This screen provides access to and from the ON-LINE MEAS START, OFF-
LINE MEAS COND (1), CALIBRATION START and MENU screens.
Operation
Press the function keys (F1) - (F4) to proceed to the desired screen.
Note: If the overflow pipe set two streams (option) is installed, [OFF-LINE] (F2) is
not displayed.
Function Keys
Key Function
RETURN Returns to the INITIAL screen.
74 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.2 MENU Screen
Display
The following items are listed on the screen.
1) GENERAL CONDITIONS
Displays the screens where the general measurement parameters are
entered.
2) SAMPLE MEASUREMENT/CONDITIONS
Displays the screen where the sample measurement parameters are
entered.
3) CALIBRATION/CONDITIONS
Displays the screens where the calibration curve parameters are entered.
4) MAINTENANCE
Displays the screens used for performing instrument maintenance.
5) SERVICE
Displays the screens used for verifying normal operation of the instrument
functions.
6) MONITOR
Displays the screens used for monitoring the operational status of the
instrument.
7) TREND GRAPH
Displays the measurement results using a trend graph.
8) CAL DATA RECORD
Displays the recorded CALIBRATION DATA screen.
9) OUTPUT TERMINAL STATUS
Displays the screen used for setting output terminal conditions.
Functions
This menu screen is used to access screens that are used to set measurement
conditions, check various functions and view stored information.
Operations
Use the cursor keys ↑↓ to highlight the desired menu item, then press the
(ENTER) key.
Press [RETURN] (F1) to return to the INITIAL screen.
TOCN-4110 75
5.4 Screen Displays, Functions and Operations
5.4.3 GENERAL CONDITIONS Screen
Function Keys
Key Function
NEXT Validates the settings in this screen and returns to the
MENU screen.
MENU Cancels changes made in this screen and returns to the
MENU screen.
Display
The following items are listed on the screen.
1) VALVE SELF-PROT INT
This fixed time interval is how often the 8-port valve will rotate during
prolonged idle periods. A 6-hour time interval is typically appropriate.
This function is used when the instrument is to be left idle for a prolonged
period (one week or more). After an extended idle period, the 8-port valve
of the Sample Pretreatment/Injection System may not rotate smoothly
when restarted. With this function, the valve will automatically operate as
long as power to the instrument is maintained throughout the idle period.
This function keeps the valve in good working condition. Dilution water is
pumped through the valve to the drain one time during each rotation. Refer
to Section 5.4.22 “MAINTENANCE Screen” for details on the procedure
for shutting down the power to the instrument during an idle period.
2) SAMPLING TIME
This item is displayed when an optional Flow Line Switcher is installed on
the instrument. This function is used to set the amount of time given to
draw the sample from the sampling point. The optimum value is dependent
upon the sample water flow rate. Conduct an actual measurement to
determine the optimal setting for this function.
76 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.3 GENERAL CONDITIONS Screen
TOCN-4110 77
5.4 Screen Displays, Functions and Operations
5.4.4 CALIBRATION/CONDITIONS Screen
Function Keys
Key Function
NEXT Validates settings made in this screen and returns to
MAIN MENU screen.
MENU Cancels settings made in this screen and returns to the
MAIN MENU screen.
CAL CURVE Used to view or delete the calibration curve.
HELP Displays the HELP menu.
78 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.4 CALIBRATION/CONDITIONS Screen
Display
This screen consists of two pages. The page number for the screen is indicated
in the upper right corner as 1/2 or 2/2. Move to page 2 by pressing the cursor
down key when the cursor is in calibration curve #5 of page 1. Move back to
page 1 by pressing the cursor up key when the cursor is in the top row of
page 2.
The following items are listed on the screen under the menu name. These items
are used for calibration curve generation.
1) C# (Calibration curve number)
*
Displays the calibration curve number. An “ ” to the left of the calibration
curve number signifies that the curve has already been generated.
2) TYP (Measurement type)
Designates the measurement type [TC, IC, POC, TN]. The available
settings depend upon the installed options. When using a 2-point
calibration curve, enter settings for the high standard on the first TYP row
and the settings for the zero standard on the second TYP row.
3) B# (Bottle number)
Indicates the standard solution bottle number to be used. Set this value to 0
to use dilution water as the zero standard solution.
4) STD (Standard)
Enter the concentration of the standard solution stored in the bottle number
set under B#.
5) DIL (Dilutin factor)
Enter the dilution factor (1-20) for the standard solution.
6) DS (Detector sensitivity)
Displays the detector (NDIR/CLM) sensitivity. This value is automatically
entered based on the values in the STD and DL columns. The user may
change this value.When “TC” or “IC” is entered in the TYP column, the
values are automatically chosen from “H”, “M” and “L.”When “TN,” is
entered in the TYP column, the values are automatically chosen from “H”,
“MH” “ML” and “L.” No setting made in the DS column for the zero
standard of a 2-point calibration curve.
7) INJV (Injection volume)
The standard solution injection volume (µL) is entered automatically
based on the values in the STD and DL columns. The user may change this
value.
8) RP (Standard repitions)
Enter the number of standard solution measurements repetitions to be
performed to obtain one data point.
9) MX (Maximum number of injections)
Enter the maximum number of measurements. The automatic outlier
function is enabled when this value is higher than the value in the RP
column. The standard deviation (SD) and coefficient of variation (CV)
values entered in the GENERAL CONDITIONS screen are used as the
criteria for determining whether additional measurements will be
performed. The instrument averages the number of measurements set in
the RP column that best meet the SD and CV criteria and disregards any
outliers.
TOCN-4110 79
5.4 Screen Displays, Functions and Operations
5.4.4 CALIBRATION/CONDITIONS Screen
Functions
This screen is used for setting the calibration curves generation conditions.
The optimum detector sensitivity and injection volume are automatically
entered based on the concentration of the standard to be used and the dilution
factor. The user may change these values.
Operations
Use the cursor keys to highlight the calibration curve parameter to be set.
Press the (SEL) key to change the values for the TYP, DS and ZS items. Press
the (ENTER) key to confirm the desired value.
Use the number keys to enter the desired value for the other items. Press the
(ENTER) key to confirm the newly entered value.
Note: Once generated, calibration curve data will be deleted if the values for TYP,
STD, DL, DS, INJV or SP are changed and the [NEXT] (F1) key is pressed.
Note: Calibration curve items on this page may be automatically entered based on
the parameters entered in the SMPL MEAS/CONDITIONS (1) screen. If this
is the case, they cannot be modified or deleted in the CALIBRATION/
CONDITIONS screen.
80 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.4 CALIBRATION/CONDITIONS Screen
In the normal mode, pressing [MENU] (F2) displays the MENU screen.
Pressing [CAL CURVE] (F3) in the normal mode, changes the function keys
to [CAL CURVE] (F1), [DELETE] (F2) and [RETURN] (F4).
In this mode, pressing [CAL CURVE] (F1) displays the CAL CURVE screen
with the calibration curve highlighted. Pressing [DELETE] (F2) in this mode
changes the function keys to [DELETE] (F1) and [RETURN] (F4).
In this mode, pressing [DELETE] (F1) deletes the currently highlighted
calibration curve and the function keys return to those described in the normal
mode.
At any point, pressing [RETURN] (F4) cancels calibration curve deletion.
Calibration curves set for use in the SMPL MEAS/CONDITIONS (1) screen
cannot be modified or deleted in this screen until the settings in the SMPL
MEAS/CONDITIONS (1) screen are canceled.
Press [NEXT] (F1) to validate the settings in this screen and return to the
MENU screen. Press [MENU] (F2) to cancel any changes made in this screen
and return to the MENU screen.
This screen displays a description for each item in the REGISTER
CALIBRATION CURVE screen. Pressing [BACK] (F4), returns to the
REGISTER CALIBRATION CURVE screen.
TOCN-4110 81
5.4 Screen Displays, Functions and Operations
5.4.5 CAL CURVE Screen
Function Keys
Key Function
RETURN Return to the CALIBRATION/CONDITIONS screen.
Display
1) CAL CURVE # indicates the file number of the displayed calibration
curve.
2) TYPE, DIL FACTOR, DETEC SENS, INJEC VOL, SPRG TIME and
SET ORIGIN are the parameters used to generate the displayed
calibration curve. Refer to the description of the CALIBRATION/
CONDITIONS screen in Section 5.4.4 “CALIBRATION/
CONDITIONS Screen” for details on setting each of these parameters.
3) CONC, #INJ, AREA, SD and CV% are the standard solution
measurement data obtained during calibration curve generation.
4) The graphic display of the calibration curve is located on the right side
of the screen.
Functions
This screen is used to display calibration curve data stored in a previously
generated calibration curve file.
This screen is for reference purposes only. None of the displayed settings may
be changed.
Operations
Press [RETURN] (F1) to return to the CALIBRATION/CONDITIONS screen.
82 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.6 SMPL MEAS/CONDITIONS (1) Screen
Function Keys
Key Function
NEXT Displays the SMPL MEAS/CONDITIONS (2) screen.
MENU Returns to the MENU screen.
HELP Displays the Help menu.
Display
“CONDITION NO.” is the measurement conditions storage number. A
maximum of three separate and distinct sets of measurement conditions may
be stored.
This screen consists of two pages. The page number for the screen is indicated
in the upper right corner as 1/2 or 2/2. Move to page 2 by pressing the cursor
down key when the cursor is in the lowest row of page 1. Move back to page 1
by pressing the cursor up key when the cursor is in the uppermost row of page
2.
TOCN-4110 83
5.4 Screen Displays, Functions and Operations
5.4.6 SMPL MEAS/CONDITIONS (1) Screen
3 types of measurement may be entered for each flow line. The following
combinations of measurement types are NOT available.
IC with any other TYPE
TC with NPOC
TOC1 with TC, NPOC or TOC2
TOC2 with TC or NPOC
3) C# (Calibration curve number)
Displays the calibration curve number (1-9).
4) RANGE
Sets the measurement range. Once a C# value is entered in the previous
column, the full-scale value from that calibration curve is automatically
displayed. The user may modify this value. Place the cursor in the RANGE
column and press (SEL) to successively change the RANGE values. The
DL values change with each RANGE change to match the values specified
in the calibration curve. The DL value is an integer from 1-20 and the
RANGE value is calculated so the product of the RANGE value and DL
value are constant. The combination of RANGE value and the DL values
cannot exceed 20000. If TOC1 or TOC2 are selected as the measurement
type, the RANGE value for the second measurement type (IC in the case
of TOC1, NPOC in the case of TOC2) is automatically calculated so the
DL value is equal to the first measurement type (TC in the case of TOC1,
POC in the case of TOC2). The DL value for the first measurement item
always takes precedence.
5) DL (Dilution factor)
Indicates the dilution factor used to dilute the sample. When a value is set
for C#, the value entered in the calibration curve conditions is
automatically entered and displayed. This may be modified as necessary.
Refer to the description under RANGE to change this value.
6) DS (Detector sensitivity)
Indicates the detector (NDIR/CLM) sensitivity. When a value is set for C#,
a corresponding value is automatically displayed. This value cannot be
modified.
7) INJV (Injection volume)
Indicates the sample injection volume. When a value is set for C#, a
corresponding value is automatically displayed. This setting cannot be
modified.
84 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.6 SMPL MEAS/CONDITIONS (1) Screen
Functions
This screen is used to enter the sample measurement conditions. The sample
measurement conditions cannot be changed because they must match the
measurement conditions used in calibration curve generation.
Note: In sample measurement, the number of washes performed on the
syringe is always set to 1 and the sampling volume is always set to
3mL.
Operations
Use the cursor keys to highlight the measurement condition item to be
modified.
For the CONDITION NO, TYPE and RANGE items, press the (SEL) key to
change the values. Press the (ENTER) key to confirm the value.
Use the number keys to enter values for the other items and press the (ENTER)
key to confirm the new values.
Press [NEXT] (F1) to validate the settings in this screen and proceed to the
SMPL MEAS/CONDITIONS (2) screen.
Press [MENU] (F2) to cancel any changes made in this screen and return to the
MENU screen.
Press [HELP] (F4) to display a screen describing the settings found in this
screen.
TOCN-4110 85
5.4 Screen Displays, Functions and Operations
5.4.7 SMPL MEAS/CONDITIONS (2)-SCHEDULE Screen
Function Keys
Key Function
NEXT Displays the SMPL MEAS/CONDITIONS (3) screen.
MENU Returns to the MENU screen.
Display
This screen displays the online sample measurement schedule. Each row of the
schedule may contain scheduling for only 1 flow line. Measurement is
performed in sequential row order. Up to 24 rows can be entered into the
schedule table.
The schedule table page number is indicated in the upper right corner of the
screen. Only 8 rows are displayed on each page of the schedule table. Use the
cursor down key to move from the last row of a page to the first row of the next
page. Likewise, use the cursor up key to move from the top row of one page to
the last row of the page before it.
1) INTERVAL
Selects the type of measurement interval (EVEN, NOT SET, ZERO).
EVEN The entered number of repeat measurements is equally spaced
over the measurement interval time cycle so the entire set is
conducted within the PERIOD/min.
NOT SET The entered number of repeat measurements is continuously
conducted within the PERIOD/min. If the measurements are
completed before the PERIOD/min has elapsed, measurement is
paused until the total PERIOD/min time is reached.
Measurement continues on the next row of the schedule table.
ZERO: The MAX number of repeat measurements is continuously
conducted within the PERIOD/min. A specific clock time is used
to establish the sample measurement timing for functions such as
calibration and catalyst regeneration.
86 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.7 SMPL MEAS/CONDITIONS (2)-SCHEDULE Screen
2) S# (Stream number)
The sample stream number is entered in this column. The number of
available sampling streams is dependent on the instrument model and the
sampling accessories that are installed on the instrument. Up to 3 sampling
streams are available (6 streams for TOC-4110 or TN-4110) if either the
sample flow line set (option) or the solid sample flow line switcher
(options) is installed.
The S# (stream number) must be entered before any other parameters can
be entered in the schedule table row.
3) PERIOD/min (Measurement time)
Enter the total measurement time for a schedule table row. The maximum
time is 1440 minutes for each row. When S# (stream number) is entered, a
default minimum value for TYP is automatically displayed.
4) TYP. (Typical measurement time)
This value is the typical time required for one measurement. The TYP
value is based on the sampling stream number and is calculated
automatically. The value displayed in the TYP column as a reference.
5) NO OF INJECT (Number of injections)
Enter the number of repeat measurements to be conducted within the time
specified in PERIOD/min. This value must be less than or equivalent to
the value displayed in the MAX column. If ZERO was selected for the
INTERVAL type, a value cannot be entered in this column.
6) MAX
The maximum numbers of repeat measurements, which can be
accommodated within the PERIOD/min, is automatically calculated and
displayed in this column for reference.
Functions
This screen displays the sample online measurement schedule table. Each row
of the schedule table is specific for an individual sampling stream.
Measurement is performed in sequential row order. The schedule table can
accommodate up to 24 rows.
Operations
Press the (SEL) key to change the values for the INTERVAL items. Press the
(ENTER) key to confirm the INTERVAL value.
Use the number keys to enter values for the other items and press the (ENTER)
key to confirm the new entry.
Press [NEXT] (F1) to validate all the changes made in this screen and continue
to the SMPL MEAS/CONDITIONS (3) screen.
Press [MENU] (F2) to cancel any changes made in this screen and return to the
MENU screen.
TOCN-4110 87
5.4 Screen Displays, Functions and Operations
5.4.8 SMPL MEAS/CONDITIONS (3)-AUTO CAL,CAT REG Screen
Function Keys
Key Function
NEXT Displays the SMPL MEAS/CONDITIONS (4) screen.
MENU Returns to the MENU screen.
Display
1) CALIBRATION TYPE
Select either RE-CAL or CHECK.
RE-CAL: This selection directs the instrument to generate a new
calibration curve at the indicated calibration time.
CHECK: This selection directs the instrument to verify the current
calibration curve at the indicated calibration time. The standard
solution is measured and if the result is within the specified
TOLERANCE of the previous calibration curve, the check
ends and calibration is not conducted. If the result exceeds the
TOLERANCE, a new calibration curve is generated.
TOLERANCE: This value is the range used for comparing the standard
measurement value with the previous calibration curve data.
Enter a value from 1-99%. The TOLERANCE value can only
be entered if CHECK is selected for the CALIBRATION
TYPE.
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5.4 Screen Displays, Functions and Operations
5.4.8 SMPL MEAS/CONDITIONS (3)-AUTO CAL,CAT REG Screen
Functions
This screen is used to enter the automatic calibration timing parameters.
The CALIBRATION TYPE setting is common to all calibration curves. The
automatic calibration mode is set in this screen. Settings related to the timing
for automatic calibration are made in the SMPL MEAS/CONDITIONS (3)
screen.
Operations
Use the cursor keys to highlight the desired item and make them as described
below.
Press the (SEL) key to change the values for the CALIBRATION TYPE and
CHECK items. Press the (ENTER) key to confirm the value.
Use the number keys to enter values for the other items and press the (ENTER)
key to confirm the new entry.
Press [NEXT] (F1) to validate all changes made in this screen and continue to
the SMPL MEAS/CONDITIONS (4) screen.
Press [MENU] (F2) to cancel any changes made in this screen and return to the
MENU screen.
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5.4 Screen Displays, Functions and Operations
5.4.9 SMPL MEAS/CONDITIONS (4)-ANALOG OUTPUT Screen
Function Keys
Key Function
NEXT Displays the SMPL MEAS/CONDITIONS (5) screen.
MENU Returns to the MENU screen.
Display
The following analog output conditions are entered on this screen.
1) CN (Output terminal)
Displays the output terminal number.
2) R# (Recorder pen number)
Displays the recorder pen number if the recorder (option) is installed.
3) S# (Stream number)
Enter the sample stream number associated with the output terminal.
4) TYPE
Enter the type of measurement associated with the output terminal and
related stream (S#) setting.
5) RANGE
Enter the full-scale range for the associated output terminal.
6) HOLD
Select whether the previous measurement value is maintained during
measurement of the next sample stream.
7) a (Conversion output constant)
Enter the coefficient for the conversion output constant.
8) +bx (Primary coefficient)
Enter the primary coefficient for the conversion output.
90 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.9 SMPL MEAS/CONDITIONS (4)-ANALOG OUTPUT Screen
Functions
This screen is to enter the analog output conditions and recording conditions
for sample measurement. For details on output terminals, refer to the
TERMINAL TABLE screen in Section 5.4.14 “PEAK PROFILE Screen.”
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Press the (SEL) key to change the value for the HOLD item. Press the
(ENTER) key to confirm the value.
Use the number keys to enter values for the other items and press the (ENTER)
key to confirm the new entry.
Press [NEXT] (F1) to validate all changes made in this screen and continue to
the SMPL MEAS/CONDITIONS (5) screen.
Press [MENU] (F2) to cancel any changes made in this screen and return to the
MENU screen.
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5.4 Screen Displays, Functions and Operations
5.4.10 SMPL MEAS/CONDITIONS (5)-ALARM Screen
Function Keys
Key Function
NEXT Displays the MENU screen.
MENU Returns to the MENU screen.
TERMINAL Displays the TERMINAL TABLE screen.
Display
This screen is composed of multiple pages. Each page is dedicated to a single
stream. Depending on the instrument model, 3-6 pages are available. Press
[NEXT S#] (F3) to display the next page.
1) MARGIN TO RESET
After an alarm is triggered, the alarm may be automatically turned off if
the next measurement value is within the normal range. The alarm is a
light on the upper right of the keyboard. This feature is based on how far
within the normal range the next measurement value falls. The MARGIN
TO RESET item determines the degree to which the next measurement
value must fall within the normal range to turn off the alarm.
Once the alarm has been triggered, it cannot be reset unless the next
measurement is below the specified value by n%. For example, MARGIN
TO RESET is 10% and the alarm upper limit is 10000, an alarm is
triggered when the measurement value exceeds 10000. The alarm is not
reset unless the measurement value is less than 9000 or [10000-
(10000×0.1)].
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5.4 Screen Displays, Functions and Operations
5.4.10 SMPL MEAS/CONDITIONS (5)-ALARM Screen
Functions
This screen is used to set the conditions that will trigger an alarm during
sample measurement.
Refer to the description of the TERMINAL TABLE screen for details on the
output terminals.
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Press the (SEL) key to change the value for the TYPE, HOLD and FORM
items Press the (ENTER) key to confirm the value.
Use the number keys to enter values for the other items and press the (ENTER)
key to confirm the new entry.
Press [NEXT] (F1) to validate all changes made in this screen and return to the
MENU screen.
Press [MENU] (F2) to cancel any changes made in this screen and return to the
MENU screen.
Press [TERMINAL] (F4) to display the TERMINAL TABLE screen.
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5.4 Screen Displays, Functions and Operations
5.4.10 SMPL MEAS/CONDITIONS (5)-ALARM Screen
Function Keys
Key Function
RETURN Returns to the previous screen.
Display
The TERMINAL TABLE is displayed on this screen. Highlighted terminal
numbers have already been selected.
Function
This screen displays the contact terminals that have been selected.
Operation
This screen is used for reference only. Contact terminals status cannot be
changed in this screen.
Press [RETURN] (F4) to return previously displayed screen.
94 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.11 ON-LINE MEAS START Screen
Function Keys
Key Function
RETURN Displays the INITIAL screen.
PAUSE Displays the ON-LINE MEAS START-PAUSE
SETTING screen.
Display
1) CONDITION NO
Select the sample measurement condition number set in the SMPL MEAS/
CONDITIONS screen. The numbers displayed inside the parentheses
represents condition numbers that have associated settings made in the
SMPL MEAS/CONDITIONS screen.
2) STARTING TIME
Enter the measurement start time.
3) INITIAL CAL
Determines if a calibration curve will be generated prior to starting
measurement. This setting is based on the measurement schedule in the
SMPL MEAS/CONDITIONS screen. Initial calibration takes precedence
if the measurement schedule has been set using TIME settings. If the
scheduled time of any block overlaps with the initial calibration, initial
calibration is performed first.
4) AUTO PRINTOUT
Determines if measurement results will be automatically output to the
printer (option).
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5.4 Screen Displays, Functions and Operations
5.4.11 ON-LINE MEAS START Screen
Functions
This screen is used to start on-line measurement.
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Use the number keys to enter values for CONDITION NO. and STARTING
TIME. Press the (ENTER) key to confirm the value.
Use the (SEL) key to enter values for the other items and press the (ENTER)
key to confirm the new entry.
Use the number keys to enter the Starting Time. Enter the Hours and then the
Minutes using the 24 hours time system and press (ENTER) key. If the
(START/STOP) key is pressed without entering a time and leaving the field as
it is (**:**), measurement is started immediately.
Press (START/STOP) key, in this screen, to start on-line measurement.
Press [PAUSE] (F4) to display the ON-LINE MEAS START-PAUSE
SETTING screen.
Press [RETURN] (F1) to return to the INITIAL screen.
96 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.12 ON-LINE MEAS START-PAUSE SETTING Screen
Function Keys
Key Function
RETURN Returns to the INITIAL screen.
NXT MON Displays the calendar for the next month.
PRE MON Displays the calendar for the previous month.
CANCEL Displays different function keys for the ON-LINE
MEAS START-PAUSE SETTING screen.
Display
1) PAUSE PERIOD
Enter a pause period (24-hour clock mode) using the actual clock time.
Note: The PAUSE PERIOD takes precedence over any INTERVAL settings
made in the SMPL MEAS/CONDITIONS screen.
Pause start Measurement takes precedence. However, new
time: measurement will not start during a pause period.
Pause end time: Pause takes precedence.
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5.4 Screen Displays, Functions and Operations
5.4.12 ON-LINE MEAS START-PAUSE SETTING Screen
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Use the number keys to enter values for PAUSE PERIOD and press the
(ENTER) key to confirm the value.
Use the (SEL) key to enter values for the other items except for those in the
PAUSE calendar and press the (ENTER) key to confirm the new entry.
To enter the PAUSE calendar, position the cursor at the PAUSE PERIOD item
and press the down cursor key. Conversely, to move out of the calendar,
position the cursor in the top row of the calendar and then press the up cursor
key.
To enter settings in the PAUSE SCHEDULE, select the desired date and press
the (ENTER) key. The selected date is highlighted. Press the (ENTER) key
again to delete the date setting. The maximum pause length is 60 days.
Press [NXT MON] (F2) or [PRE MON] (F3) to display the calendars for the
next month or previous month, respectively.
Press [CANCEL] (F4) to cancel all PAUSE PERIOD settings. The function
keys change to the following when [CANCEL] (F4) is pressed.
(F1) (F2) (F3) (F4)
Normal mode [RETURN] [NXT MON] [PRE MON] [CANCEL]
Cancel mode [CANCEL ALL] [STOP CANCEL]
98 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.13 ON-LINE MEASURING Screen
Function Keys
Key Function
RETURN Displays the INITIAL screen.
KEY LOCK Disables all key functions on the operation panel.
PEAK(C) Displays the PEAK(C) PROFILE screen.
PEAK(N) Displays the PEAK(N) PROFILE screen.
Display
1) The current sample stream number (S#:) is displayed in the top half of
this screen.
2) The current measurement type (TC, IC, NPOC or TN) and the
measurement results are displayed in extra large characters in the top
half of this screen.
3) The operation status is displayed in the upper right corner of the
screen. One of the following items is displayed in the operation status
field; it changes as the measurement operation progresses.
INITIALIZING SPARGING WASHING SAMPLING
INJECTING MEASURING DRAINING PEAK END
HOMOGENIZING PAUSING WAITING COMPLETED
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5.4 Screen Displays, Functions and Operations
5.4.13 ON-LINE MEASURING Screen
Functions
Measurement status and results are displayed on this screen during on-line
measurement.
Operations
Press [KEY LOCK] (F2) to disable all key functions except for (F2). Press
[LOCK OFF] (F2) to cancel the KEY LOCK mode.
When [RETURN] (F1), [PEAK(C)] (F3) and [PEAK(N)] (F4) are pressed, the
display returns to the INITAL screen and then displays the PEAK (C) or PEAK
(N) screen, respectively. The measurement peaks can be viewed in the PEAK
(C) and PEAK (N) screens. Press [RETURN] (F4) to return to the ON-LINE
MEASURING screen.
Even during measurement it is possible to move to other screens from the
INITIAL SCREEN, however, settings cannot be changed in any of those
screens. Return to the INITIAL screen by pressing the (CLR) key.
100 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.14 PEAK PROFILE Screen
Function Keys
Key Function
RETURN Returns to the ON-LINE MEASURING or OFF-LINE
MEASURING screen.
25% FS Enlarges the peak display by decreasing the displayed
vertical axis.
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5.4 Screen Displays, Functions and Operations
5.4.14 PEAK PROFILE Screen
Display
1) Depending on the measurement type, the TC, IC, NPOC or POC peak
is displayed on the PEAK(C) screen. If the measurement type is TOC1
or TOC2, the screen is divided into two parts: with TC or POC is
displayed on the left and IC or NPOC on the right. Figure 5.18
“PEAK(C) PROFILE Screen” is an example of TOC2 type
measurement.
2) For TN measurement, the TN peak is displayed on the PEAK(N)
screen.
3) The measurement status is displayed in the upper right corner of the
screen.
Functions
The peak profile is displayed in this screen during measurement. Information
regarding the sample characteristics and instrument status may be inferred by
studying the peak profile. ON-LINE and OFF-LINE measurement screen
contents are similar.
Operations
Press [25% FS] (F3) to enlarge the displayed peak by reducing the amount of
scale that is displayed. Press [100%FS] (F3) to return to full scale.
Press [RETURN] (F1) to return to the ON-LINE MEASURING or OFF-LINE
MEASURING screen displayed prior to entering this screen.
102 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.15 OFF-LINE MEAS COND (1) Screen
Function Keys
Key Function
RETURN Returns to the INITIAL screen.
Display
1) SELECT FROM SMPL MEAS COND (1-3)
This function is valid only if one or more sets of on-line measurement
parameters are entered. Select the appropriate set of measurement
conditions from the existing on-line measurement conditions.
2) SET SPECIFIC MEAS CONDITION
Select this to manually enter the measurement parameters.
Functions
Select from two methods of setting measurement conditions depending on
whether the measurement conditions have been previously entered.
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Press the cursor up or down keys to move the cursor to the appropriate
measurement condition setting mode.
Select the SELECT FROM SMPL MEAS COND (1-3) and press the
[ENTER] key to display the OFF-LINE MEAS COND (2)-SELECT screen.
Select SET SPECIFIC MEAS CONDITION and press the [ENTER] key to
display the OFF-LINE MEAS COND(2)-SPECIFIC screen.
Press [RETURN] (F1) to cancel any changes made in this screen and return to
the INITIAL screen.
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5.4 Screen Displays, Functions and Operations
5.4.16 OFF-LINE MEAS COND(2)-SELECT Screen
Function Keys
Key Function
NEXT Validates the settings made in this screen.
RETURN Returns to the INITIAL screen.
Display
1) SAMPLE #
Enter the sample identification number.
2) CONDITION NO
Select which set of on-line measurement conditions will be used for
sample measurement.
3) S# (Sample stream)
Enter the sample stream number.
4) NUMBER OF INJECTION
Enter the number of repeat measurements to be performed.
5) MAX NUMBER OF INJ
Enter the maximum number of injections that can be performed when the
automatic outlier function is enabled.
6) SD, CV%
Enter the SD (standard deviation) and CV (coefficient of variation) limits
that will be used to determine if additional measurements will be
conducted when the automatic outlier function is enabled. The SD and CV
of the measured results are compared to these values. If both the SD and
CV measured values are greater than the limits set here, additional
measurements are conducted.
104 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.16 OFF-LINE MEAS COND(2)-SELECT Screen
Functions
The measurement conditions used in off-line sample measurement are entered
in this screen. The sample measurement conditions are the same as those used
to generate the calibration curve.
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Use the (SEL) key to enter a value for TYPE and press the (ENTER) key to
confirm the value.
Use the to number keys enter values for the other items and press the (ENTER)
key to confirm the new entry.
Enter the parameters n this screen and press [NEXT] (F1). The message “Set
sample vessel. Press [START] key.” is displayed. The (F1) key changes to
[RETURN].
Press the (START/STOP) key to initiate off-line measurement.
Press [RETURN] (F1) to retain the settings made in this screen and return to
the INITIAL screen.
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5.4 Screen Displays, Functions and Operations
5.4.17 OFF-LINE MEAS COND (2)-SPECIFIC Screen
Function Keys
Key Function
NEXT Displays the OFF-LINE MEAS COND (3) screen.
RETURN Cancels all changes made in this screen and returns to
the OFF-LINE MEAS COND(1) screen.
Display
1) SAMPLE #
Enter the sample identification number.
2) TYPE
Enter the measurement type. TC, IC, NPOC, POC, TOC1 (TC-IC), TOC2
(POC+NPOC) and TN may be available depending on the options
installed on the instrument. For TOC1 or TOC2, two rows of settings are
allocated for TC and IC or POC and NPOC, respectively.
3) CAL CURVE #
Enter the calibration curve number to be used for sample measurement.
This setting determines which previously generated and stored calibration
curve is loaded and used for the measurement.
4) DETECTOR SENS
Displays the detector sensitivity. The user cannot change this value.
5) INJECTION VOL
Indicates the injection volume. This value cannot be changed on this
screen.
6) FULL SCALE
Indicates the full scale at calibration. This value cannot be changed on this
screen.
106 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.17 OFF-LINE MEAS COND (2)-SPECIFIC Screen
7) DILUTION FACTOR
Displays the dilution factor that will be used if the sample is to be diluted.
The appropriate dilution factor is automatically displayed once the
calibration curve is specified. This value cannot be changed. If the
measurement TYPE is TOC1 or TOC2, the dilution factor used for IC or
NPOC is the same as that used for TC or POC.
8) ACID VOLUME
Enter the volume of acid that will be added to the sample to pre-treat for IC
removal.
9) SPARGE TIME
Enter the sparge time used for IC removal.
Functions
This screen, together with the OFF-LINE MEAS COND (3) screen, is used to
enter the off-line sample measurement conditions.
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Enter numeric values for the desired and press the (ENTER) key to confirm the
entries.
Use the (SEL) key to enter a value for TYPE and press the (ENTER) key to
confirm the value.
Press [NEXT] (F1) to validate the changes made in this screen and display to
the OFF-LINE MEAS COND (3) screen.
Press [RETURN] (F2) to cancel all changes made in this screen and return to
the OFF-LINE MES COND (1) screen.
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5.4 Screen Displays, Functions and Operations
5.4.18 OFF-LINE MEAS COND (3) Screen
Function Keys
Key Function
NEXT Validates the changes made in this screen.
RETURN Cancels all changes made in this screen and returns to
the OFF-LINE MEAS COND (1) screen.
Display
1) NUMBER OF INJECTION
Enter the number of repeat measurements to be performed.
2) MAX NUMBER OF INJ
Enter the maximum number of injections that can be performed when the
automatic outlier function is enabled.
3) SD, CV%
Enter the SD (standard deviation) and CV (coefficient of variation) limits
that will be used to determine if additional measurements will be
conducted when the automatic outlier function is enabled. The SD and CV
of the measured results are compared to these values. If both the SD and
CV measured values are greater than the limits set here, additional
measurements are conducted.
108 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.18 OFF-LINE MEAS COND (3) Screen
Functions
This screen, together with OFF-LINE MEAS COND (2)-SPECIFIC screen, is
used to set the conditions for off-line sample measurement.
Operations
Use the cursor keys to highlight the desired item and make the changes as
follows.
Enter numeric values for the desired and press the (ENTER) key to confirm the
entries.
Press [RETURN] (F2) to cancel all changes made in this screen and return to
the OFF-LINE MEAS COND (1) screen.
Enter the parameters in this screen and press [NEXT] (F1). The message “Set
sample vessel. Press [START] key.” is displayed. The (F1) key changes to
[RETURN].
Press the (START/STOP) key to initiate off-line measurement.
Press [RETURN] (F1) to retain the changes made in this screen and return to
the INITIAL screen.
TOCN-4110 109
5.4 Screen Displays, Functions and Operations
5.4.19 OFF-LINE MEASURING Screen
Function Keys
Key Function
KEY LOCK Disables the key functions.
RETURN Returns to the INITIAL screen.
PEAK(C) Displays the PEAK (C) PROFILE screen.
PEAK(N) Displays the PEAK (N) PROFILE screen.
110 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.19 OFF-LINE MEASURING Screen
Display
1) The current measurement type is displayed on the second line of this
screen. Measurement results are displayed on the screen for TC, IC,
NPOC or TN. If the measurement type is TOC1 or TOC2, the TC and
IC values or POC and NPOC values, are displayed on the left and right
sides of the screen, respectively. Figure 5.18 “PEAK(C) PROFILE
Screen” page 101 is an example of TOC2-type measurement.
2) Injection number (#), peak area (AREA), concentration (CONC) and
remark (RMK) are displayed in the measurement sequence. Mean
(MN), standard deviation (SD) and coefficient of variation (CV) are
calculated and displayed for the peak area and concentration. These
values are calculated and displayed in the lower right portion of the
screen for TOC1 or TOC2.
Remarks may include the following.
T: The peak was over the time limit (tailing).
S: The peak start was not detected normally.
H: The peak exceeded the full scale (high).
F: The range change was conducted, but the peak exceeded even the
maximum range.
B: More than F, the peak far was exceeded the maximum range.
R*: The range was changed. Range value is displayed in the “*”
position.
D**: The dilution factor was changed. Dilution value is displayed
Functions
The status of the measurement operation and the measurement results are
displayed on this screen during off-line measurement.
Operations
Press [KEY LOCK] (F2) to disable all function keys, except (F2). Press
[LOCK OFF] (F2) to cancel the [KEY LOCK] mode.
Press [RETURN] (F1) or [PEAK(C)] (F4) to display the INITIAL screen or
the PEAK(C) PROFILE screen, respectively. The measurement peak is
displayed in the PEAK PROFILE screen.
Press [MEAS N] (F3) to display the MEASURING(N) screen and press
[PEEK(N)] (F4) to display the PEEK(N) PROFILE screen.
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5.4 Screen Displays, Functions and Operations
5.4.20 CALIBRATION START Screen
Function Keys
Key Function
RETURN Returns to the INITIAL screen.
Display
CAL CURVE #
Select the file number for the calibration curve to be generated. Conditions
have been entered in the CALIBRATION/CONDITIONS screen for the
calibration curve numbers in the parentheses.
Functions
Calibration curve generation is initiated in this screen. The selected calibration
curves are generated in numerical order.
Operations
Use the left/right cursor keys to highlight the number of the calibration curve
to be generated and press the (ENTER) key to set the number (*). Press the
(ENTER) key again to delete the number. Calibration curves of any displayed
number may be selected. Multiple calibration curves may be selected.
Press the (START/STOP) key to start generating the selected calibration
curves.
Press [RETURN] (F1) to return to the INITIAL screen.
112 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.21 CALIBRATION CURVE MEASURING Screen
Function Keys
Key Function
RETURN Returns to the INITIAL screen.
KEY LOCK Disable all function keys.
25% FS Enlarges the display to 25% of full scale.
Display
1) The peak profile is displayed on the left side of the screen. Press
[25% FS] (F3) to enlarge the peak display by reducing the displayed
vertical axis. Press [100% FS] (F3) to return to full scale.
2) CAL CURVE # displays the calibration curve number of the
calibration curve being generated. The letter L signifies the low
concentration standard of a 2-point calibration curve and H signifies
the high concentration standard.
3) The operation status is displayed in the upper right corner of the
screen. One of the following status messages is displayed as the
measurement operation progresses.
INITIALIZING SPARGING WASHING SAMPLING
INJECTING MEASURING DRAINING PEAK END
PAUSING WAITING
4) Injection number (#), peak area (AREA) and remark (RMK) are
displayed in the measurement sequence. Mean (MN), standard
deviation (SD) and coefficient of variation (CV) are calculated and
displayed for the peak area. Remarks may include the following.
T: The peak was over the time limit (tailing).
TOCN-4110 113
5.4 Screen Displays, Functions and Operations
5.4.22 MAINTENANCE Screen
Functions
This screen allows the user to monitor the standard solution measurement
status and to view the results of calibration curve generation.
Operations
Press [KEY LOCK] (F2) to disable all function keys, except (F2). Press
[LOCK OFF] (F2) to cancel the [KEY LOCK] mode.
Press [25% FS] (F3) to enlarge the peak display by reducing the displayed
vertical axis. Press [100%FS] (F3) to return to full scale.
Press [RETURN] (F1) to return to the INITIAL screen.
During measurement, it is possible to go to other screens from the INITIAL
SCREEN. Parameters cannot be changed in any of these screens. Press (CLR)
key to return to this screen.
Function Keys
Key Function
NEXT Displays the COUNTER (1) screen.
MENU Returns to the MENU screen.
Display
1) DATE & TIME
Enter the current date and time.
114 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.22 MAINTENANCE Screen
Functions
Various maintenance-related operations are performed from this screen.
Operations
Use the cursor keys to highlight the desired maintenance item and then press
the (ENTER) key.
Use the number keys to enter the appropriate values for DATE & TIME and
press the (ENTER) key to confirm the values.
Use the cursor keys to select FOR ZERO POINT DETECTION OF SYRINGE
or REGENERATION OF CATALYST. Press the (ENTER) key to perform
these operations automatically. This screen is redisplayed when operation is
complete. Refer to Section 6.2 for details on REGENERATION OF
CATALYST.
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5.4 Screen Displays, Functions and Operations
5.4.23 COUNTER (1) Screen
Function Keys
Key Function
NEXT Displays the COUNTER (2) screen.
MENU Returns to the MENU screen
RESET Resets the counter to zero for the selected item.
Display
1) TOTAL NO OF INJ
This item counts and displays the total number of sample injections made.
2) TOTAL INJ VOL
This item calculates and displays the total volume (µL) of sample injected
into the combustion tube.
3) TOTAL NO OF SYR MOVE
This item displays the total number of times the syringe pump has
operated.
4) RUNNING TIME (min)
This item calculates and displays the total amount of time (minutes) power
has been supplied to the instrument.
5) MEASURING TIME (min)
This item calculates and displays the total analysis time (minutes).
Functions
This screen displays information related to instrument maintenance intervals.
Operations
Use the cursor keys to select the desired item. Press [RESET] (F4) to reset that
counter to zero.
Press [NEXT] (F1) or [MENU] (F2) to display the COUNTER (2) screen or
MENU screen, respectively.
116 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.24 COUNTER (2) Screen
Function Keys
Key Function
MENU Return to the MENU screen.
CLEAR Clear the counter and date for the selected item
Display
1) AMNT OF STD 1 - 6
Displays the remaining solution volume in each standard bottle. Preset
values for the remaining amount of solution are used to generate a
warning. The date of solution preparation may be entered for recording
and management purposes. Standard bottles 2-6 are available as an
additional option.
2) AMNT OF WATER
Displays the remaining volume of dilution water in the dilution water
bottle on the exterior right side of the instrument.
3) AMNT OF ACID
Displays the remaining volume of IC removal acid stored in the acid bottle
inside the instrument.
Note: For example, using a 1-liter bottle, enter 800mL as the reset value
rather than 1000mL. This way, even if the Remaining Volume warning
is generated, there is still 200mL remaining. This prevents aborting the
measurement due to interruption of the liquid flow.
TOCN-4110 117
5.4 Screen Displays, Functions and Operations
5.4.24 COUNTER (2) Screen
Functions
Similar to the COUNTER (1) screen, this screen displays information related
to instrument maintenance such as, the amounts of standard solution, diluent
and acid.
A threshold value may be entered for each item except for chart paper. This
value serves as a warning for the remaining amount of the respective solution.
Operations
Use the cursor keys to highlight the desired item. Use the number keys to enter
an appropriate value and press the (ENTER) key to confirm the value.
Some degree of error is associated with calculating the remaining volume of
solution or amount of chart paper. Consider this degree of error when
determining the warning values.
Use the cursor keys to highlight the desired item and press [CLEAR] (F4) to
clear the value for that item.
Press [MENU] (F2) to return to the MENU screen.
An alarm is triggered when the counter value exceeds the warning value.
While measurement continues, press the (ALARM) key to display the screen
that will indicate which preset value has been exceeded. While in the ALARM
screen, press [RETURN] (F1) to return to the previous screen.
To remove an alarm or set up a new solution, use the cursor to select the
desired item and press the ENTER key. This resets the counter value to zero.
Next, press ALARM and then press [Clear] (F4) to extinguish the ALARM
lamp.
Note: All measurement operations continue uninterrupted during this
sequence.
118 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.25 SERVICE Screen
Function Keys
Key Function
MENU Returns to the MENU screen.
Display
1) KEYBOARD CHECK
Use this item to check the operation of each key on the keyboard panel.
2) PRINTER CHECK
Use this item to test the printer (option) operation.
3) ANALOG OUTPUT CHECK
Use this item to test the operation of the analog outputs.
4) CONTACT INPUT CHECK
Use this item to test the operation of the contact inputs.
5) CONTACT OUTPUT CHECK
Use this item to test the operation of the contact outputs.
6) SAMPLE INJECTION CHECK
Use this item to check the sample stream and make any necessary
adjustments. Refer to Section 6.1.4 “Inspecting the Sample Injection
Stream.”
7) MECHANICAL CHECK
Use this item to test the operation of the 8-port sampling and solenoid
valves.
8) RS-422 I/F CHECK
Use this item to test the operation of the RS-422 communication function.
Functions
This screen is used to test the mechanical operation of the keyboard, valves,
printer (option) and various output/input functions.
TOCN-4110 119
5.4 Screen Displays, Functions and Operations
5.4.25 SERVICE Screen
Operations
Use the up and down cursor keys to highlight the appropriate test item. Press
the (ENTER) key to initiate the corresponding test. Test mode operations are
described below.
Test Mode Function
KEYBOARD CHECK The key that is pressed is displayed on the screen.
PRINTER CHECK A test pattern is printed. This mode exits automatically when
complete. [RETURN] (F4) is not displayed.
ANALOG OUTPUT Press [ZERO] (F1) or [SPAN] (F2) to output a signal to all 7
CHECK circuits of analog output terminals simultaneously. The signal
(0-1V, 0-16mA or 4-20mA) is based on the internal circuit
settings, which are specified at the time of purchase. Press
[ZERO] (F1) to output 0V, 0mA or 4mA and press [SPAN]
(F2) to output 1V, 16mA or 20mA for each terminal.
CONTACT OUTPUT Simultaneously output a signal to all 12 circuits (28 with
CHECK optional system) of contact output terminals. Press [ON] (F1)
to close the contact; [OFF] (F2) to open the contact.
CONTACT INPUT The terminal number of the terminal receiving input is
CHECK displayed on the screen. There are 16 input terminals.
RS-422 I/F CHECK The results (OK or NG) are displayed at the completion of this
automatic test.
SAMPLE INJECTION Diluent is drawn into the syringe. Three 200µL aliquots are
CHECK expelled to the slide injector. This mode exits automatically
when complete. Refer to Section 6.1.4 “Inspecting the Sample
Injection Stream” for details on sample injection adjustment.
MECHANICAL Highlight and press the [ENTER] key to display the
CHECK MECHANICAL CHECK screen, shown in Figure 5.32.
120 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.25 SERVICE Screen
Display
Use the cursor keys to highlight an item and press the (ENTER) key to
perform the operations described below.
1) 8-PORT VALVE
Each time the (ENTER) key is pressed the flow changes to the next port.
Port No. 1 → Port No. 2 →... → Port No. 8 → Port No. 1…
2) SYRINGE PUMP
Each time the (ENTER) key is pressed, the pump performs one full stroke
and draws 3mL of liquid from port No. 5 (diluent flow line) and air from
port No. 6. The pump discharges its contents through port No. 8 (waste
flow line).
3) INJECTION SLIDER
Each time the (ENTER) key is pressed, the sample injector slider moves to
cover the combustion tube or over the drain tube.
4) CARIR GAS VALVE (Carrier gas valve)
Each time the (ENTER) key is pressed, the valve opens or closes.
5) SPRG GAS VALVE (Sparge gas valve)
Each time the (ENTER) key is pressed, the valve opens or closes.
6) TEMP CONTRL FAN (Temperature control fan)
Each time the (ENTER) key is pressed; the exhaust fan inside the upper
door of the instrument starts or stops running.
7) S-CEL LINE VALVE (Short cell flow line valve)
This item is only available if the DF or AD/DF option is installed. The
following valves are checked one at a time with every (ENTER) key
operation.
• The solenoid valve opens for the IC measurement flow line.
• The solenoid valve opens for the short cell purge.
• The solenoid valve opens for POC measurement if the AD/DF option
is installed.
This sequence repeats as the (Enter) key is continually pressed. When one
solenoid valve is open, all other solenoid valves are closed.
8) STD SOLN SEL (Standard solution selection)
This item is only available if the Standard Solution Switching set is
installed.
• 6-Port Standard Solution Switching Set
Each time the (ENTER) key is pressed; the flow changes to the next
port in the 6-port standard switcher.
Port No. 1 → Port No. 2 →... → Port No. 6 → Port No. 1...
• 2-Port Standard Solution Switching Set
Each time the (ENTER) key is pressed, the solenoid valve switches
between flow lines 1 and 2.
TOCN-4110 121
5.4 Screen Displays, Functions and Operations
5.4.25 SERVICE Screen
122 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.26 MONITOR(C) Screen
Display
1) The baseline trend is displayed in the box on the left side of the screen.
2) The furnace temperature and READY status (OK or NG -no good) is
displayed on the right side of the screen in the first line.
3) The dehumidifier temperature and READY status is displayed on the
right side of the screen in the second line.
4) The baseline position, fluctuation and noise are displayed with their
respective READY status on the right side of the screen in lines 3-6.
5) The NDIR detector sensitivity is displayed on the right side of the
screen in line 7.
Functions
This screen displays the following items.
• furnace temperature and status
• dehumidifier temperature and status
• baseline parameters and status
• detector (NDIR) sensitivity
Operations
This screen is used for monitoring purposes and to change the NDIR detector
sensitivity. Each time [CHANGE] (F3) is pressed; the detector sensitivity is
changed from Low to Medium to High, in that sequence.
Press [MENU] (F2) to return to the MENU screen.
Press [MONIT (N)] (F3) to display the MONITOR (N) screen.
TOCN-4110 123
5.4 Screen Displays, Functions and Operations
5.4.27 MONITOR(N) Screen
Function Keys
Key Function
MENU Returns to the MENU screen.
CHANGE Changes the detector sensitivity (L, ML, MH, H).
MONIT(C) Displays the MONITOR (C) screen.
Display
1) The baseline trend is displayed in the box on the left side of the screen.
2) The furnace temperature and READY status (OK or NG-no good) is
displayed on the right side of the screen in the first line.
3) The dehumidifier temperature and READY status is displayed on the
right side of the screen in the second line.
4) The CLM reactor temperature and READY status is displayed on the
right side of the screen in the third line.
5) The baseline position, fluctuation and noise and their respective
READY status is displayed on the right side of the screen in lines 4-7.
6) The CLM detector sensitivity is displayed on the right side of the
screen in line 8.
Functions
This screen displays the following items.
• furnace temperature and status
• dehumidifier temperature and status.
• CLM reactor status
• baseline parameters and status
124 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.27 MONITOR(N) Screen
Operations
This screen is used for monitoring purposes and to change the CLM detector
sensitivity. Each time [CHANGE] (F3) is pressed; the detector sensitivity is
changed from Low to Medium Low to Medium High to High, in that sequence.
Press [MENU] (F2) to return to the MENU screen.
Press [MONIT (C)] (F3) to display the MONITOR (C) screen.
TOCN-4110 125
5.4 Screen Displays, Functions and Operations
5.4.28 TREND GRAPH Screen
Display
1) The sample stream number (SAMPLE #) and measurement type to be
displayed in line 2.
2) Measurement values from the previous 12 hours are displayed on this
screen view the measurement trends.
3) The current date and time are displayed on the top right portion of the
screen.
4) The current page associated with this screen is displayed (under the
date and time). The screen consists of four pages (48 hours).
5) The horizontal axis of the trend graph displays the time.
6) The vertical axis displays concentration and can be displayed up to
120% of full scale.
Functions
A maximum of the previous 48 hours of measurement values may be displayed
for each sample stream.
Operations
Press the (SEL) key to select the sample stream number and press the
(ENTER) key to confirm the value. The corresponding stream trend graph is
displayed on the screen.
Proceed to the second page by pressing [PREV 12H] (F3) on the first page.
Conversely, press [NEXT 12H] (F4) to return to the first page.
Press [MENU] (F2) to return to the MENU screen.
126 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.29 CALIBRATION DATA Screen
Display
1) The calibration curve number (CAL CURVE #) associated with the displayed
data is displayed under the screen title.
2) The data history of the calibration curve is displayed on line 3 of the screen.
Data for one calibration curve is displayed on each screen, in chronological
order. When the amount of data exceeds 11 rows, the oldest data is deleted
and the newest data is appended. Two points of data are displayed for a 2-
point calibration curve using two rows (a maximum of five calibrations per
screen may be displayed).
Example of Data Display
04/07 17:40 26804 2/3 1.73% -0.00/+0.00%
Coefficient of variation
# of injections measured /
maximum # of injections
Time
Date
3) The measurement type, concentration of the standard solution and
dilution factor are displayed in the upper right portion of the screen.
TOCN-4110 127
5.4 Screen Displays, Functions and Operations
5.4.30 OUTPUT TERMINAL STATUS Screens
Functions
This screen displays the data history of the calibration curves, which may be
useful in evaluating the instrument operation.
Operations
Press [MENU] (F2) to return to the MENU screen.
128 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.30 OUTPUT TERMINAL STATUS Screens
Function Keys
Key Function
NEXT Proceeds to page 2/3, 3/3.
MENU Returns to the MENU screen.
RETURN Returns to page 2/3, 1/3.
Display
1) The contact output signals are listed on the left side of the screen.
WARNING 1 Signals a relatively minor problem. Instrument
operation continues. The following events
correspond to this problem.
(1) Interruption of the standard solution 1 (-6.)
(2) Acid interruption.
(3) Diluent interruption.
(4) Catalyst regeneration failed.
WARNING 2 Signals that measurement cannot be conducted
because a calibration curve has not been generated.
The following events correspond to this problem.
(1) Initial calibration error.
(2) Calibration curve not generated.
When WARNING 2 is generated because of one of
the above events, pressing any key will restore
instrument operation.
FATAL ERROR Signals a more serious problem. The Instrument is
shut down and all keyboard function is disabled. The
following events correspond to this problem.
(1) EEPROM write error.
(2) Furnace overheating.
(3) Furnace temperature detection thermocouple
wire is broken.
(4) Furnace temperature detection thermocouple
short circuited.
(5) Syringe movement error.
(6) 8-port rotary valve error.
(7) Slider movement error.
(8) 6-port rotary valve (option) error.
READY Indicates that the instrument is ready to start an
analysis. Displayed only if all MONITOR screen
parameters are OK and the instrument is not currently
performing an analysis.
ON-LINE MEAS. Indicates that the instrument is in the on-line
measurement mode. This output is active during
measurement pause intervals.
EXTERNAL Indicates that the current measurement uses the
OPERATION MEAS. specific stream remote start function. This output is
active from input of the “Remote Start, Channel 1-6”
signal until measurement in that stream is complete.
TOCN-4110 129
5.4 Screen Displays, Functions and Operations
5.4.30 OUTPUT TERMINAL STATUS Screens
2) Enter the contact output terminal number under the TERM column.
Refer to the description for the TERMINAL TABLE screen for the
terminal status.
130 TOCN-4110
5.4 Screen Displays, Functions and Operations
5.4.30 OUTPUT TERMINAL STATUS Screens
Functions
This screen is used to assign event output signals to a signal terminal.
Operations
Press [NEXT] (F1) in page 1/3 or 2/3, to display the next page. Press
[RETURN] (F3) in page 2/2 or 3/3, to return to the previous page.
Press [MENU] (F2) to return to the MENU screen.
TOCN-4110 131
5.5 Measuring Samples Containing Suspended Substances
5.4.30 OUTPUT TERMINAL STATUS Screens
132 TOCN-4110
5.6 Handling Samples Containing Acid, Alkali and Salts
5.6.1 Acids and Salts
Strongly corrosive Cl2 or Br2 gas attacks the internal surfaces of the measurement cell
if samples containing chlorine or bromine acids or salts are injected into the TC
combustion tube. Chlorine is produced not only from hydrochloric and hypochlorous
acid, but also by heating ammonium chloride, calcium chloride, magnesium chloride,
etc. The halogen scrubber removes most of this chlorine.
The halogen scrubber and the scrubber connected to the bottom of the TC combustion
tube absorb and eliminate most of the chlorine, hydrogen chloride and other gaseous or
mist substances. The sample moves through the scrubbers at a flow rate of 150mL/min.
If the sample contains these substances in very high concentrations, the scrubbers are
overwhelmed and cannot completely remove the halogens as they pass. It is highly
recommended that whenever possible these types of samples are diluted.
Interfering components and corrosive substances are produced when measuring
samples containing sulfuric acid, nitric acid or other inorganic acids or salts. The
halogen scrubber has little effect in counteracting these substances. Avoid these acids
whenever possible.
If required, use 2N hydrochloric acid for adjusting the sample pH. HCl is an EPA
approved acid.
Reduced sensitivity and poor reproducibility quickly result when measuring alkali
samples. Deterioration of the catalyst and combustion tube also result from these types
of samples. Alkali samples readily absorb atmospheric CO2 and are likely to produce
high IC concentrations. Using the NPOC method for TOC analysis is recommended.
When the alkaline samples are analyzed for TN, acidify the samples by adding diluted
hydrochloric acid. Refer to the ACV item in Section 5.4.6 “SMPL MEAS/
CONDITIONS (1) Screen.” A large amount of acid is required to acidify these
samples. Use pH test paper or a pH meter to verify a pH range of 2-3. Enter the amount
of acid to be added using the automatic acid addition function to achieve the proper pH
range.
TOCN-4110 133
5.6 Handling Samples Containing Acid, Alkali and Salts
5.6.3 Salt Deposits
134 TOCN-4110
5.7 Shutting Down the Instrument
5.6.4 Dilution Function
Procedure
WARNING
When stopping instrument operation, turn the furnace power OFF at
least 30 minutes before turning OFF the instrument power. This allows
for adequate cooling of the furnace and prevents damage to injection
port parts or electronic components.
WARNING
When shutting down the instrument, turn the ozone generator OFF at
least 3 minutes before turning off the instrument power. This allows
sufficient time for any residual ozone to be eliminated from the ozone
gas tubing.
If the instrument is to remain idle for a prolonged period (one week or more), execute
the VALVE DRYING function in the MAINTENANCE screen before switching OFF
the instrument power. Refer to Section 5.4.22 “MAINTENANCE Screen.” This
ensures that the 8-port valve of the Sample Pretreatment/Injection System will rotate
smoothly upon restart.
If the power will remain ON during the idle period, it may be preferable to use the
VALVE SELF-PROT INT function in the GENERAL CONDITIONS screen. This
function sets a fixed time interval at which the Sample Pretreatment/Injection System
8-port valve automatically operates. See Section 5.4.3 “GENERAL CONDITIONS
Screen.”
TOCN-4110 135
5.7 Shutting Down the Instrument
5.6.4 Dilution Function
136 TOCN-4110
6
6Inspection and Maintenance
6.1 Inspection
Periodically inspect each of the containers to verify that there is a sufficient quantity of
the appropriate liquids and solutions in the various containers. Refer to Section 5.4.24
“COUNTER (2) Screen,” to set the warning levels.
Periodically inspect the humidifier to verify that there is a sufficient amount of water. If
necessary, replenish with pure water through the supply port. Fill to the upper indicator
line.
WARNING
Do not overfill. Do not immerse the glass tube into water.
Verify that the water level in the drain vessel is within 10mm of the overflow tube on
the side of the container. If necessary, add water to the appropriate level.
With the carrier gas flowing at 150mL/min, verify that gas is not leaking into the drain
vessel from the drain tube. If gas is leaking and the water level in the drain vessel is
normal, the membrane filter or halogen scrubber may be clogged. However, directly
after sample injection, bubbles exiting the drain tube are a normal pressure release.
6.1 Inspection
6.1.4 Inspecting the Sample Injection Stream
When reinserting the sample injection tubing into the slider, do not allow the tip of the
tubing to extend beyond the bottom of the slider. If the tip is lower than the bottom of
the slider, it may scratch the O-ring and result in a gas leak. The tip of the tubing must
extend into the depression on the bottom of the slider for the sample to be properly
injected.
WARNING
To avoid injury, keep hands away from the Sample Pretreatment/
Injection System while it is operating.
138 TOCN-4110
6.2 Catalyst Regeneration
6.1.5 Inspecting the Printer and Recorder Chart Paper (Option)
Inorganic substances in the samples accumulate on the catalyst bed as salts or oxidized
substances. Measurement sensitivity and reproducibility decline as the quantity of
these substances become excessive. Verify performance by measuring standard
solutions. Regenerating the catalyst may restore performance. Regeneration is
performed automatically through the MAINTENANCE screen. Refer to
Section 5.4.22 “MAINTENANCE Screen” for more details.
Measurement of standard or zero water on a new catalyst bed or one that has not been
used for a long period sometimes results in high blank peaks with a decreasing trend. In
these cases it is appropriate to perform the catalyst regeneration procedure to activate
or reactivate the catalyst bed.
IC removal acid is used in the regeneration process.
If performance is not restored after performing the catalyst regeneration procedure, it
may be necessary to wash or replace the catalyst. Refer to Section 6.3.1 “Washing or
Replacing Catalyst” for more information.
Note: Catalyst regeneration is only necessary for TC measurement. In NPOC
measurement, the sample injected into the combustion tube is already acidic,
so catalyst regeneration is unnecessary.
TOCN-4110 139
6.3 Maintenance
6.3.1 Washing or Replacing Catalyst
6.3 Maintenance
CAUTION
The furnace operates at 680°C (or 720°C). Cool the furnace prior to
performing maintenance on the combustion tube, catalyst, etc. If the
furnace has not cooled to room temperature, it is STRONGLY
recommended that appropriate protective gloves be worn.
WARNING
The catalyst beads MUST be completely cooled prior to washing.
As the washed catalyst is heated in the furnace, large amounts of steam are generated.
Heat the combustion tube and catalyst carefully with the exit of the combustion tube
open until the steam dissipates.
If washing the catalyst does not restore performance, it is necessary to replace the
catalyst. A single bottle of platinum catalyst will fill the combustion tube. The
platinum screens (2 pc.) and the combustion tube may be reused after washing with
hydrochloric acid (concentrated hydrochloric acid diluted two times with water),
rinsing with water and then drying. Fill the combustion tube following the directions
given in Section 4.1 “Filling the Combustion Tube with Catalyst.”
Washing will not restore high sensitivity catalyst. When regeneration does not restore
acceptable measurement sensitivity and reproducibility, it is necessary to replace the
high sensitivity catalyst. Clean the platinum screens and combustion tube with
hydrochloric acid. Two tubes of platinum catalyst are required to fill the combustion
tube one time. Fill the combustion tube following the directions given in Section 4.1
“Filling the Combustion Tube with Catalyst.”
140 TOCN-4110
6.3 Maintenance
6.3.2 Washing or Replacing the TC and L-shaped Combustion Tube
The combustion tube may be used until it breaks or starts leaking due to cracks.
Reaction with salts in the sample may cause devitrification or whitening of the internal
surface. This does not impact performance. When the catalyst is washed or replaced,
the combustion tube may be reused after washing it with hydrochloric acid and drying
it.
L-shaped combustion tube (for carrier gas purification and/or POC measurement) may
be used until it breaks or starts leaking due to cracks.
CAUTION
The furnace operates at 680°C (or 720°C). Cool the furnace prior to
performing maintenance on the combustion tube, catalyst, etc. If the
furnace has not cooled to room temperature, it is STRONGLY
recommended that appropriate protective gloves be worn.
The CO2 absorber is used for the cleaning carrier gas, NDIR optical system purge gas,
sparge gas, for POC measurement and for the NOx absorber. Replace the entire
container.
The CO2 absorber used for the cleaning carrier gas and as the NOx absorber must be
replaced at least every 2 months. The replacement interval depends largely on the
operation conditions. It is not necessary to use a new CO2 absorber as the NOx
absorber. Used CO2 absorbers can be used efficiently as the NOx absorber, because the
CO2 absorber that is saturated with CO2 still has the capability to absorb NOx. To
reduce operation cost, used CO2 absorbers should be used for the NOx absorber.
Note: The carrier gas CO2 absorber and the NOx absorber MUST be replaced every
2 months.
TOCN-4110 141
6.3 Maintenance
6.3.4 Replacing Halogen Scrubber
Dehumidifier To sample
cell inlet
The ozone treatment tube decomposes the ozone generated by the ozone generator. It is
positioned to the right and in front of the furnace. The catalyst inside the ozone
treatment tube must be replaced periodically.
Before performing maintenance on the ozone treatment tube, stop instrument operation
according to the procedure described in Section 5.7 “Shutting Down the Instrument.”
CAUTION
The furnace heats the ozone treatment tube. Allow it to cool
sufficiently before performing maintenance.
142 TOCN-4110
6.3 Maintenance
6.3.5 Replacing the Ozone Treatment Catalyst
Procedure
2. Remove the larger rubber stopper. Remove the used catalyst and
polypropylene fiber plug.
3. Press a small amount of new polypropylene fiber into the bottom of the vessel
to plug it. Introduce fresh catalyst into the vessel to about 2cm from the neck of
the vessel. Approximately 150g of catalyst is required. Cover the catalyst with
a small amount of new polypropylene fiber and replace the rubber stopper.
CAUTION
The Viton tubing MUST be replaced each time the ozone treatment
catalyst is replaced.
5. Place the ozone treatment tube back in the original position (with the larger
diameter opening at the bottom) and reconnect the tubing.
The used catalyst contains manganese dioxide. Follow all local and federal
laws regarding the disposal of the used catalyst. Label the disposal container
appropriately.
About 2 cm
Gas inlet
Ozone Ozone
treatment treatment
tube catalyst
Gas outlet
TOCN-4110 143
6.3 Maintenance
6.3.6 Replacing Syringe Plunger Tip
The plunger tip is made of fluorine resin. Over time the plunger tip wears with use.
Eventually, gaps develop between the plunger tip and glass syringe barrel, resulting in
leaks. Once a leak occurs, bubbles form near the plunger tip as sample is drawn in or
sample leaks from the bottom of the barrel as it is injected. Use the provided
replacement plunger tip if necessary.
Note: Keep a spare plunger tip on hand at all times.
1. Using a sharp cutter, knife, etc., make cuts into the bottom of the plunger tip at
two or three locations, as shown in Figure 6.4.
2. Grasp the plunger tip using pliers, etc. and pull the plunger tip out of the
plunger. Remove the O-rings from the tip of the plunger. These O-rings must
not be reused.
Small cuts at
2-3 locations
Do not scratch the periphery of the plunger tip, as leaks will result. Use only plunger
tips specified by Shimadzu as use of other plunger tips may result in reduced
performance.
144 TOCN-4110
6.3 Maintenance
6.3.7 Cleaning the Sparge Tubing
Sparge gas
Wire
Figure 6.6 Cleaning the Sparge Tubing
Sparging to remove IC from the sample is performed inside the syringe. During
sparging bubbles are formed as shown in Figure 6.6. After extended use, it is possible
for the sparge gas tubing to become partially clogged and reduce the sparge gas flow
rate.
If this occurs, remove the intermediate connector from the sparge tubing and the
knurled thumbscrew from the syringe. Pass a piece of wire 0.2-0.3mm in diameter
through the sparge tubing to remove any blockage.
Two types of O-rings are used between the sample injector slider and the injection
block. If a gas leak occurs at this location, replace both O-rings. The upper, white O-
ring is Teflon (P/N 036-11408) and the lower, black O-ring is Viton (P/N 036-11209).
Apply a small amount of silicon grease (P/N 017-30812-01) to the black Viton O-ring.
Note: DO NOT apply grease to the Teflon O-ring.
A Teflon coated O-ring, AS-568A-116 (P/N 630-01566), is used between the injector
block and TC combustion tube. Replace this O-ring if gas leak occurs at this location.
Do not scratch any O-ring or O-ring seat.
TOCN-4110 145
6.3 Maintenance
6.3.9 Replacing 8-port Valve Rotor and Stator
The rotor and stator in the 8-port valve of the Sample Pretreatment/Injector System are
ceramic. These items typically require no maintenance. However, in applications
where minute granular particles are present in the sample, scratching of the rotor and
stator sliding surfaces can occur. These scratches could result in sample leaks,
inclusion of bubbles when suctioning or the delivery of sample to the wrong port. It
may be necessary to replace the rotor and stator if these types of problems occur.
Use the following procedure to replace the 8-port valve rotor and stator.
CAUTION
Sample pressure is applied to Port #2 of the 8-port valve (also to Port
#1 when the optional Sample Flow Line Addition Set is installed).
Ensure that the sample supply is shut off and that an appropriate
container is on hand to collect any liquid remaining in the sample
overflow pipe.
4. Using the provided hex wrench, remove the three hex head screws indicated in
Figure 6.7.
146 TOCN-4110
6.3 Maintenance
6.3.9 Replacing 8-port Valve Rotor and Stator
(top view)
8-port valve
body
(front view)
5. Detach the rotor drive component shown in Figure 6.7 by lifting it upward.
CAUTION
The white rotor may come off with the rotor holder in the bottom of
the rotor drive component. DO NOT DROP the rotor while
performing this procedure.
6. Detach the 8-port valve rotor if it did not come off in Step #5. Do not use
excessive force. The rotor can be removed along with the stator by continuing
the procedure.
7. As shown in Figure 6.8, remove the stator retaining screw with the provided
hex wrench.
TOCN-4110 147
6.3 Maintenance
6.3.9 Replacing 8-port Valve Rotor and Stator
Key wrench
(top view)
Stator retaining
screw
Seal
Stator
8. Fit the hex wrench into the hex slots on top of the stator and turn counter
clockwise.
9. Use forceps to lift out the white ceramic stator. If the rotor was not removed in
Steps #5 or #6, remove it along with the stator.
10. Insert the new stator into the 8-port valve. Align the holes at the bottom of the
stator with the two notches inside the 8-port valve. Place the clear thin plastic
seal into the depression on the top surface of the stator.
11. Insert the stator retaining screw, reversing the procedure for removal.
12. Insert a new rotor in the rotor holder at the bottom of the rotor drive
component.
Note: Refer to Figure 6.9 to ensure proper orientation of the groove in the
rotor (10 o'clock) and the notch on the rotor holder.
Rotor holder
Rotor
Notch at bottom of rotor
(sliding surface) Note: Align the holes at the
top of the rotor with the two
Rotor drive component pins inside the rotor holder.
Figure 6.9 Installing the Rotor (view from the bottom of the rotor drive component)
148 TOCN-4110
6.3 Maintenance
6.3.10 Special Handling for the 8-Port Valve
Before switching OFF the power, if the instrument is to remain idle for a prolonged
period (one week or more), it is necessary to perform one of the operations described in
Section 5.7 “Shutting Down the Instrument” or Section 5.4.3 “GENERAL
CONDITIONS Screen.” Even when the instrument is shut down properly, the rotor and
stator may stick.
Use the following procedure to free the 8-port valve.
Procedure
1. Switch OFF the power. Using the provided hex wrench, loosen the coupling
screw.
Rotation hole
2. Insert a 2.5 hex wrench or 3mm diameter metal rod into the rotation hole
shown in Figure 6.10 “Freeing the 8-port Valve.” Turn the 8-port valve back
and forth until it moves freely.
CAUTION
This procedure requires the use of some force to start the rotation. Use
care to avoid pinching fingers in the mechanism during the operation.
3. After rotating the 8-port valve several times, return it to its original position on
the shaft and retighten the coupling screw. One side of the shaft is flat. Adjust
the 8-port valve so that the coupling screw contacts this flat surface.
WARNING
Major problems will result from the misalignment of the ports of the
8-port valve. Ensure that the orientation is correct.
TOCN-4110 149
6.4 Zero Adjustment of the (NDIR) Optical System
6.3.10 Special Handling for the 8-Port Valve
Auto zero correction is normally performed on the baseline signal to obtain accurate
peak area measurement even if the baseline is drifting. The time interval between the
beginning and end of peak measurement is excluded from the auto zero procedure. If
the baseline exceeds the auto correction range, NG is displayed in the baseline position
of the READY conditions in the Monitor screen and the READY lamp will not light. In
this case, the instrument is in the wait state and measurement cannot be performed.
Perform zero adjustment of the NDIR optical system using the following procedure.
Procedure
2. The NDIR detector is located at the top of the instrument. Push the SW1
switch to the TEST position.
3. While observing the baseline position in the MONITOR (C) screen, adjust the
zero adjustment potentiometers VR1 and VR2 so that the baseline is near 0%.
If the baseline does not adjust sufficiently by turning one potentiometer, use
both. Turning the potentiometer clockwise moves the baseline in the 'plus'
direction. Turn the potentiometer slowly since the display has a short response
time.
If this optical zero adjustment must be performed frequently (especially if drift is in the
plus direction), the interior of the NDIR cell may be contaminated or corroded. If this
is the case, replace the halogen scrubber and perform appropriate pretreatment
procedures when measuring samples with high acid or salt concentrations. Continuing
to use the NDIR cell in that condition may require replacement of the cell.
150 TOCN-4110
6.5 Chemiluminescence Detector
6.3.10 Special Handling for the 8-Port Valve
Procedure
1. Disconnect the tubing from the reactor, then detach the reactor by removing
the 4 screws.
Reactor
Remove
the screws
Detector Gasket
Disconnect
the tubing
2. Remove the gasket and examine it for dirt or scratches. If dirt or scratches are
observed, replace the gasket.
3. Examine the window. If it is dirty, gently wipe the window with a lint-free
tissue or cloth to clean it.
4. Place the gasket between the reactor and the detector window, so that the flat
surface is against the window. Tighten the 4 screws uniformly to secure the
assembly.
TOCN-4110 151
6.6 Ozone Generator
6.3.10 Special Handling for the 8-Port Valve
When a message appears on the screen indicating that use of the ozone generator has
exceeded 8000 hours, contact your Shimadzu representative to request replacement of
the ozone generator.
CAUTION
If the ozone generator is used after it has been operating for 8000
hours, ozone may begin to leak from the unit. Replace the unit with a
new ozone generator.
WARNING
The lithium hydroxide anhydride fine powder crystals are corrosive
(strongly alkali). Review the MSDS in Section 9.1 “Material Safety
Data Sheets” before handling.
152 TOCN-4110
6.8 B-type Halogen Scrubber
6.3.10 Special Handling for the 8-Port Valve
Effect
Samples that contain high concentrations of halogens such as chlorine, bromine, iodine
and fluorine, may cause corrosion of the inside of the measuring cell. During the
combustion process these types of samples produce various acids such as hydrogen
chloride and other halogens. These acids are exported from the combustion tube to the
measuring cell and because of their superior oxidation capability may corrode the gold
plating.
0.05 mol/L hydrochloric acid is used In the B-type halogen scrubber. After the
combustion process the sample gas is passed through the hydrochloric acid which
dissolves the iron and chromium components of the stainless steel net to produce iron
chlorides (FeCl2) and chromium chlorides (CrCl2). Because of their superior reduction
capability, the iron and chromium chlorides absorb the chlorine, bromine, iodine, etc.
from the sample gas.
The B-type halogen scrubber has a better absorption efficiency and larger absorption
capacity than the standard halogen scrubber.
Accessories
Description Quantity
Stainless steel net 4 pcs (Only one piece is used at a time.)
Maintenance
Replace the solution in the B- type halogen scrubber every three months with fresh
0.05M hydrochloric acid. The stainless steel net is effective until it is completely
dissolved. Regular examination of the stainless steel net is recommended. Each net is
expected to last for more than six months.
Part Numbers
Description Part Number
Stainless steel net 631-60069
Hydrochloric acid Adjust and use reagent grade hydrochloric acid.
TOCN-4110 153
6.9 Multi-Stream Suspended Solids Pretreatment Unit (Option)
6.3.10 Special Handling for the 8-Port Valve
Screws (2 locations)
Butterfly Screws
(3 locations)
154 TOCN-4110
6.10 Single Stream Suspended Solids Pretreatment Unit (Option)
6.3.10 Special Handling for the 8-Port Valve
Motor
Strainer Nozzle
Clamp
Sampling unit
Sample homogenizer
Pinch valves
TOCN-4110 155
6.11 Backwash Strainer Sample Pretreatment Unit (Option)
6.3.10 Special Handling for the 8-Port Valve
Butterfly nut
Packing
Strainer
156 TOCN-4110
7
7Special Accessories
Table 2.2 “Special Accessories” displays a list of the various options that may be added
to this instrument to modify the instrument function. Except for high sensitivity
catalyst, special accessories are installed by authorized service engineers. This
instruction manual is limited to descriptions of the functional changes provided with
the addition of the most common special accessories.
7.1 Flow Line Switching Modules
7.1.1 Sampling Pipe Set
This option is appropriate for clean water samples, such a tap water, which contains no
suspended particles, slime, etc. The sample pipe set is available in either a 1- or 2-flow
line configuration. A 1-flow line type configuration may be upgraded to the 2-flow line
type by obtaining the sample flow line addition set.
With the 1-flow line switching option, the sample enters the sampling tube mounted
near the top of the left-side panel (overflow type), then passes through the T connector
and is introduced into the number 2 port of the internal 8-port valve through the flared
tube.
With the 2-flow line switching option, the second flow line is connected to the number
1 port of the 8-port valve, as indicated in Figure 7.1. For that reason, off-line
measurement is not possible with this configuration.
Sample 1
Sample 2
Sampling Sampling
tube 1 tube 2 Dilution water
To slide injector
To drain
Acid Standard
solution
To drain
Gas purifier Sparge
Carrier gas inlet flow rate solenoid Syringe
controller
Carrier gas
158 TOCN-4110
7.1 Flow Line Switching Modules
7.1.2 Suspended Particle Flow Line Switcher
This option is designed for particulated and/or slimy sample streams that could cause
clogging of the sample flow lines.
The sample flow path with this option installed is shown in Figure 7.2 “Suspended
Particle Flow Line Switcher.” An external sampling system or “sample thief” performs
the flow line switching. Only the sample of the selected flow line is introduced into the
pretreatment unit. The sample pretreatment unit consists of 2 cylindrical vessels.
Sample flows from the sample thief through a #50 mesh stainless-steel screen to
eliminate very large particles into the inner cylinder of the homogenizer. A mixer at the
bottom reduces the size of many types of particulates and ensures sample homogeneity
prior to measurement. Sample is delivered from this module to the Sample
Pretreatment/Injector System measurement. Excess sample is discharged from the
module through the drain solenoid valve. Wash water is forcefully sprayed upward
through the spinning stainless steel screen and mixing blade. This effectively washes
the screen and sample vessel.
Since the sampling tube and stainless steel mesh are washed with each sampling
sequence, this system does not clog easily. If however, the samples contain high
concentrations of viscous or fibrous particles or suspended solids that have a tendency
to adhere, it may become necessary to disassemble and clean the sampling unit.
Tap water must be supplied as the wash water for the Suspended Particle Flow Line
Switcher. Since water must be constantly supplied the line between the water source
and the instrument water inlet must be capable of withstanding the continuous tap
water pressure of the facility. The user supplies this line. Once the tap water line is
connected, while the source water is OFF, adjust the pressure regulator on the
instrument to 150kPa (1.5kg/cm2). With the water flowing, decrease this pressure to
50-100kPa (0.5-1.0 kg/cm2).
Note: When the typical sample matrix contains excessive quantities of suspended
particles or large amounts of viscous or fibrous particles, some type of sample
filtering may be required before the sample enters the instrument.
TOCN-4110 159
7.1 Flow Line Switching Modules
7.1.2 Suspended Particle Flow Line Switcher
Sample 3
Sample 2
Sample 1
Sampler 1
Sampler 2
Sampler 3
Dilution water
To slide injector
Acid Standard
solution
To drain
To drain
160 TOCN-4110
7.2 Standard Solution Switching Set (2-port and 6-port)
7.1.2 Suspended Particle Flow Line Switcher
NC COM To IC removal
acid bottle To dilution water bottle
NO
To drain outlet
1 2
Standard solution
bottle number
To off-line Syringe
sampling
Figure 7.3 Flow Line Diagram with Installed Standard Solution Switching Set (2-port)
To IC removal
acid bottle To dilution water bottle
1 2 3 4 5 6 To drain outlet
Standard solution bottle number
To off-line sampling
Syringe
Figure 7.4 Flow Line Diagram with Installed Standard Solution Switching Set (6-port)
TOCN-4110 161
7.3 DF and AD/DF Options
7.1.2 Suspended Particle Flow Line Switcher
The standard configurations of the TOCN-4110 and TOC-4110 allow for NPOC and
TC measurement, however, with the addition of these options, the specified
measurement options are modified as listed in Table 7.1 “Options and Associated
Specification Changes.”
The flow line configurations associated with the respective options are as shown in
Figure 7.5 and Figure 7.6.
162 TOCN-4110
7.3 DF and AD/DF Options
7.1.2 Suspended Particle Flow Line Switcher
TOCN-4110 163
7.3 DF and AD/DF Options
7.1.2 Suspended Particle Flow Line Switcher
Figure 7.6 Flow Line Diagram with Installed AD/DF Option (TOCN-4110).
164 TOCN-4110
7.4 Recorder
7.1.2 Suspended Particle Flow Line Switcher
7.4 Recorder
This is a 6-pen recorder that may be installed in the TOCN-4110, TOC-4110 and TN-
4110. In the default configuration, recording is limited to one item (pen No. 1). When
the recorder board set option (P/N 638-72497-16 or -17) is installed, this recorder can
record up to 6 items.
Enter the recording parameters in the SMPL MEAS/CONDITIONS (4) screen.
Parameters are entered for each pen and include sample flow line (S), measurement
type (TYPE), degree of full scale (RANGE), recorder pen number (1-6) and whether to
hold output (HOLD).
TOCN-4110 165
7.5 Printer (Thermal)
7.1.2 Suspended Particle Flow Line Switcher
166 TOCN-4110
8
8Troubleshooting
If one of the above abnormal conditions is not the cause, contact your
Shimadzu service representative.
8.1 Error Messages
168 TOCN-4110
8.1 Error Messages
TOCN-4110 169
8.2 Troubleshooting
8.2 Troubleshooting
This section describes procedures taken by the user in response to instrument operation
problems. Contact your Shimadzu service representative if, after following the
described procedures, the cause of the problem is not clarified or it becomes necessary
to replace a part.
[1] Error message is displayed → Refer to Section 8.1 “Error Messages.”
[2] READY lamp does not light → Change to the MONITOR screen to determine
which READY condition is not satisfied.
[3] The baseline of NDIR remains over the auto zero range. → TOCN TOC
(Baseline position is NG.)
Yes
Yes
Yes
NDIR breakdown
Perform zero adjustment.( Section 6.4)
Note: If zero adjustment cannot be performed for the NDIR detector, the optical
system may be contaminated. Contact your Shimadzu service representative.
170 TOCN-4110
8.2 Troubleshooting
[4] The baseline of CLM remains over the auto zero range. (Baseline position is NG.)
Yes
TOCN-4110 171
8.2 Troubleshooting
No There is an accumulation of
Did you replace the catalyst? impeding substances.
Replace the catalyst. ( Section 6.3.1
or Section 6.3.2)
Yes
Yes
Yes
172 TOCN-4110
8.2 Troubleshooting
Yes
Yes
Yes
TOCN-4110 173
8.2 Troubleshooting
No
No
Yes
No
174 TOCN-4110
8.2 Troubleshooting
Yes
Note: “T” is printed when peak is not complete at end of the measurement time. The
maximum measurement interval is set internally and cannot be changed.
Note: If bubbles are seen in the drain vessel during injection, this is normal. It is
abnormal to have bubbles appear at other times.
TOCN-4110 175
8.2 Troubleshooting
Yes
No
Is the tubing clogged? Check the tubing.
Yes
No
Is the tubing detached? Check the tubing connections.
Yes
No
Is the syringe loose? Check the syringe.
Yes
Yes
NDIR breakdown
Contact your Shimadzu representative.
176 TOCN-4110
9
9Reference Materials
Operation of this instrument involves the use of hydrochloric acid (HCl), potassium
hydrogen phthalate (KHP), sodium carbonate (Na2CO), sodium bicarbonate
(NaHCO3), platinum catalyst, soda lime and a halogen scrubber. Lithium hydroxide
anhydride (LiOH) is also used with some of the optional accessories. It is necessary to
use caution when handling these substances. The characteristics and handling
precautions are described in the Material Safety Data Sheets (MSDS) that follow.
This information is based on the information found in the available literature. It is by
no means comprehensive in scope.
9.1 Material Safety Data Sheets
9.1.1 High Sensitivity Catalyst
178 TOCN-4110
9.1 Material Safety Data Sheets
9.1.2 Hydrochloric Acid (HCl)
TOCN-4110 179
9.1 Material Safety Data Sheets
9.1.3 Lithium Hydroxide (monohydrate)
180 TOCN-4110
9.1 Material Safety Data Sheets
9.1.4 Normal Sensitivity Catalyst
ACUTE EFFECTS: May be harmful by inhalation or ingestion. May cause eye irritation. may cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
EXPOSURE CAN CAUSE: Coughing, chest pains, difficulty in breathing, gastrointestinal disturbances.
CHRONIC EFFECTS: Prolonged exposure can cause damage to the lungs and bones. TO the best of our knowledge, the chemical, physical and
toxicological properties have not been thoroughly investigated.
TARGET ORGAN DATA: Lungs, thorax or respiration (tumors) tumorigenic (neoplastic by RTECS criteria) tumorigenic (equivocal tumorigenic agent by
RTECS criteria) tumorigenic (tumors at site of application) only selected registry of toxic effects of chemical substances
(RTECS) data is presented here. see actual entry in RTECS.
SECTION VI HEALTH HAZARD DATA
OSHA PEL: 8H TWA 5MG/ME respirable fraction; 8h TWA 10MG/M3 total dust
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. If inhaled,
remove to fresh air. If not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided person is
conscious. Call a physician. Remove and wash contaminated clothing promptly. In case of skin contact, immediately wash skin with soap and copious amounts of
water.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: Carbon dioxide, dry chemical powder or appropriate foam.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS: Material may have an exothermic reaction above 200 c with halocarbon vapors and may produce toxic
hydrochloric acid and phosgene.
SECTION IX ACCIDENTAL RELEASE MEASURES
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Sweep up, place in a bag and hold for waste dis-
posal. Ventilate area and wash spill site after material pickup is complete.
SECTION X STABILITY AND REACTIVITY
Stability: Stable.
Incompatibilities: Strong acids, strong bases, chlorine trifluoride, ethylene oxide, halocarbons, oxygen difluoride, sodium nitrate, vinyl acetate,
strong oxidizing agents,organic materials. Protect from moisture. Hazardous combustion or decomposition products. Nature of
decomposition products not known. Hazardous polymerization will not occur.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
TOCN-4110 181
9.1 Material Safety Data Sheets
9.1.5 Ozone Treatment Catalyst
ACUTE EFFECTS: May be harmful by inhalation or ingestion. May cause eye irritation. may cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
EXPOSURE CAN CAUSE: Coughing, chest pains, difficulty in breathing, gastrointestinal disturbances.
CHRONIC EFFECTS: Prolonged exposure can cause damage to the lungs and bones. TO the best of our knowledge, the chemical, physical and
toxicological properties have not been thoroughly investigated.
TARGET ORGAN DATA: Lungs, thorax or respiration (tumors) tumorigenic (neoplastic by RTECS criteria) tumorigenic (equivocal tumorigenic agent by
RTECS criteria) tumorigenic (tumors at site of application) only selected registry of toxic effects of chemical substances
(RTECS) data is presented here. see actual entry in RTECS.
SECTION VI HEALTH HAZARD DATA
OSHA PEL: 8H TWA 5MG/ME respirable fraction; 8h TWA 10MG/M3 total dust
SECTION VII FIRST-AID MEASURES
When attached to skin: wash thoroughly the effected portion with a plenty of water and soap.
When entered into eye: Wash the eye with a plenty of clean water for at least 15 minutes and receive medical treatment by an eye doctor if any
abnormality remains.
When swallowed: Gargle with water and drink much water and vomit it thoroughly and then receive medical treatment.
In case of contact: Immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated
clothing and shoes. Wash contaminated clothing before reuse. Discard contaminated shoes. Assure adequate flushing of the eyes by separating
eyelids with fingers. If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. If
swallowed, wash out mouth with water provided person is conscious. CALL A PHYSICIAN. Only selected registry of toxic effects of
chemical substances (RTECS) data is presented here. See actual entry in RTECS for complete information.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: Carbon dioxide, dry chemical powder or appropriate foam.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS: Material may have an exothermic reaction above 200 c with halocarbon vapors and may produce toxic
hydrochloric acid and phosgene.
SECTION IX ACCIDENTAL RELEASE MEASURES
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Sweep up, place in a bag and hold for waste dis-
posal. Ventilate area and wash spill site after material pickup is complete.
SECTION X STABILITY AND REACTIVITY
Stability: Stable under ordinary handling conditions.
Incompatibilities: Strong acids, strong bases, chlorine trifluoride, ethylene oxide, halocarbons, oxygen difluoride, sodium nitrate, vinyl acetate,
strong oxidizing agents,organic materials. Protect from moisture. Hazardous combustion or decomposition products. Nature of
decomposition products not known. Hazardous polymerization will not occur.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
182 TOCN-4110
9.1 Material Safety Data Sheets
9.1.6 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime
TOCN-4110 183
9.1 Material Safety Data Sheets
9.1.6 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime
184 TOCN-4110
9.1 Material Safety Data Sheets
9.1.6 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime
TOCN-4110 185
9.1 Material Safety Data Sheets
9.1.6 CO2 Absorber, Ca(OH)2, KOH, NaOH: Soda Lime
186 TOCN-4110
9.1 Material Safety Data Sheets
9.1.10 Sodium Persulfate
TOCN-4110 187
9.1 Material Safety Data Sheets
9.1.10 Sodium Persulfate
188 TOCN-4110
9.1 Material Safety Data Sheets
9.1.10 Sodium Persulfate
TOCN-4110 189
9.1 Material Safety Data Sheets
9.1.10 Sodium Persulfate
190 TOCN-4110
10
10Appendix
Copy the Maintenance Check Sheet on the next page and use it for maintenance
control. Place it in the holder on the inner wall of the front door.
Maintenance Check Sheet
Parts (P/N) Date Date Date
CO2 absorber for NDIR optical system purge {TOCN /TOC-4110} (630-00999)
Ozone deactivator catalyst {with Viton tubing, TOCN/TN-4110} (638-65232 with 638-
42015)
Packing (631-43818)
192 TOCN-4110
Index
Numerics
8-Port valve
rotor replacement..................................146
special handling ....................................149
A
Accessories ACID ADD FOR TC CAL ............................ 77
special ............................................ 12, 157 ACID VOLUME.......................................... 107
standard...................................................11 ACV ............................................................... 85
Acid ................................................................47 AD/DF option .............................................. 162
bottle installation ....................................47 Alkali samples.............................................. 133
hydrochloric (HCl), MSDS ..................179 Analog output................................................. 21
in sample...............................................133 AUTO PRINTOUT........................................ 95
inspection..............................................137 AUTO RE-MEAS(DIL)................................. 77
B
B# ...................................................................79 Basic samples............................................... 133
Backwash strainer.........................................156
C
C# ............................................................ 79, 84 CATALYST MISMATCH .......................... 168
CAL CURVE #.................................... 106, 112 Caution, definition of ....................................... 2
CAL CURVE screen ......................................82 Chart paper..................................................... 55
CAL DATA RECORD screen......................127 Check sheet .................................................. 191
CAL INTERVAL ...........................................89 Chemiluminescence detector ....................... 151
CAL REWRITE COND .................................89 CN .................................................................. 90
Calibration curve ............................................34 CO2 absorber.................................................. 49
CALIBRATION CURVE carrier gas purification ........................... 49
MEASURING screen ...................113 MSDS................................................... 183
CALIBRATION START screen ..................112 optical system purge............................... 50
CALIBRATION TYPE ..................................88 platform installation ............................... 49
CALIBRATION/CONDITIONS screen ........78 POC measurement.................................. 52
CARRIER GAS..............................................97 POC, replacing ..................................... 152
Carrier gas replacement .......................................... 141
CO2 absorber ..........................................49 short cell purge....................................... 50
flow rate..................................................62 sparge ..................................................... 50
purification .............................................28 Combustion tube
purifier ....................................................44 filling...................................................... 39
CAT REGENE INT........................................89 replacement .......................................... 141
Catalyst washing ................................................ 141
carrier gas purification............................44 CONDITION NO...................................95, 104
filling ......................................................39 Contact
POC combustion tube.............................45 input ....................................................... 20
regeneration ..........................................139 output ..................................................... 19
replacement...........................................140 Conventions ...............................................2, 63
TC ...........................................................61 COUNTER (1) screen.................................. 116
TOC ........................................................41 COUNTER (2) screen.................................. 117
TOC/TN..................................................40 CV %....................................................104, 108
washing.................................................140
Index-1
Index
D
Dehumidifier drain water level .................... 137 Dilution
Detector function .................................................134
chemiluminescence .............................. 151 water .......................................................48
NDIR .................................................... 150 water, inspection ...................................137
DETECTOR SENS ...................................... 106 DILUTION FACTOR ..................................107
DF option ..................................................... 162 DL ...................................................................84
DIL ................................................................. 79 Drain
tubing ......................................................16
vessel ......................................................54
DS ............................................................ 79, 84
E
EEPROM WRITE ERROR.......................... 167 Exhaust tubing ................................................17
Error messages ............................................. 167
F
Flow line switching ...................................... 158 FORM .............................................................93
Flow rate FULL SCALE...............................................106
carrier gas ............................................... 62 FURNACE......................................................97
controllers............................................... 62 Furnace drawer ...............................................43
sparge gas ............................................... 62 FURNACE OVERHEAT .............................168
G
Gas, pressure and supply................................ 17 Grounding .......................................................15
GENERAL CONDITIONS screen ................ 76
H
Halogen scrubber HOLD ...................................................... 90, 93
MSDS................................................... 189 Humidifier ......................................................54
replacement .......................................... 142 installation ..............................................47
type-B................................................... 153 water level.............................................137
High sensitivity catalyst, MSDS .................. 178 Hydrochloric acid, MSDS ............................179
I
IC Installation (cont.)
measurement .......................................... 25 drain vessel .............................................54
removal acid ........................................... 47 humidifier ........................................ 47, 54
standard preparation ............................... 58 main unit .................................................11
INITIAL CAL ................................................ 95 NOx absorber..........................................53
INITIAL CAL DEFECT .............................. 169 optical system purge CO2 absorber ........50
INITIAL screen.............................................. 73 ozone treatment tube...............................51
Injection.......................................................... 32 plunger tip.............................................144
INJECTION VOL ........................................ 106 POC CO2 absorber..................................52
Injector POC combustion tube .............................45
inspection ............................................. 138 sample injector O-rings ........................145
O-ring replacement............................... 145 short cell purge CO2 absorber ................50
INJV .........................................................79, 84 site requirements.....................................14
Input, contact.................................................. 20 sparge CO2 absorber ...............................50
Inspection ..................................................... 137 standard bottle.........................................47
Installation syringe holder .........................................46
acid bottle ............................................... 47 Instrument shutdown ....................................135
carrier gas CO2 absorber ........................ 49 INTERVAL ....................................................86
carrier gas purification ........................... 44
CO2 absorber platform ........................... 49
Index-2
Index
L
LCD AUTO-OFF ...........................................77 Lithium hydroxide (monohydrate), MSDS.. 180
LIMIT .............................................................93
M
Maintenance .................................................140 MECHANICAL CHECK screen ................. 120
check sheet............................................191 MENU screen................................................. 74
parts ........................................................13 MONITOR(C) screen .................................. 123
MAINTENANCE screen..............................114 MONITOR(N) screen .................................. 124
MARGIN TO RESET ....................................92 MSDS
Material Safety Data Sheets (MSDS)...........178 CO2 absorber........................................ 183
MAX...............................................................87 halogen scrubber .................................. 189
MAX NUMBER OF INJ..................... 104, 108 high sensitivity catalyst........................ 178
Measurement hydrochloric acid (HCl) ....................... 179
conditions auto-modify...........................37 lithium hydroxide (monohydrate) ........ 180
conditions auto-set..................................36 normal sensitivity catalyst............181, 182
IC ............................................................25 ozone treatment catalyst....................... 182
NPOC .....................................................26 phosphoric acid .................................... 188
off-line ....................................................69 potassium hydrogen phthalate.............. 186
on-line.....................................................64 sodium bicarbonate .............................. 184
peak area.................................................33 sodium carbonate ................................. 185
POC ................................................... 2, 26 sodium persulfate ................................. 187
TC ...........................................................25 MX ................................................................. 79
TN...................................................... 2, 27
TOC ........................................................27
N
NDIR Note.................................................................. 2
detector .................................................150 Note, definition of ............................................ 2
zero adjustment.....................................150 NOx absorber ................................................. 53
NO ..................................................................93 NPOC, measurement...................................... 26
NO OF INJECT..............................................87 NUMBER OF INJECTION .................104, 108
Normal sensitivity catalyst, MSDS ..... 181, 182 NUMBER OF WASHES ............................... 77
Notation conventions........................................2
O
OFF-LINE MEAS COND (1) screen ...........103 Operation........................................................ 63
OFF-LINE MEAS COND panel ....................................................... 38
(2)-SPECIFIC screen....................106 precautions ............................................... 3
OFF-LINE MEAS COND (3) screen ...........108 Optical system purge...................................... 50
OFF-LINE MEAS COND Output
(2)-SELECT screen ......................104 analog ..................................................... 21
Off-line measurement .....................................69 contact .................................................... 19
OFF-LINE MEASURING screen ................110 OUTPUT TERMINAL STATUS screen..... 128
ON-LINE MEAS START screen ...................95 Ozone
ON-LINE MEAS START-PAUSE generator............................................... 152
SETTING screen ............................97 treatment catalyst ................................. 142
On-line measurement......................................64 treatment tube...................................49, 51
ON-LINE MEASURING screen....................99 Ozone treatment catalyst, MSDS ................. 182
OZONIZER.................................................... 97
P
Parts Peak area measurement.................................. 33
inspection of ...........................................11 PEAK(C) PROFILE screen ......................... 101
maintenance............................................13 PEAK(N) PROFILE screen ......................... 101
PAUSE ...........................................................97 PERIOD ......................................................... 87
PAUSE PERIOD ............................................97 Phosphoric acid, MSDS ............................... 188
Index-3
Index
Plunger tip, replacement............................... 144 Power
POC connection...............................................15
CO2 absorber.......................................... 52 shut down..............................................135
CO2 absorber, replacement .................. 152 Pretreatment....................................................32
combustion tube catalyst ........................ 45 Principles ........................................................25
measurement ......................................2, 26 Printer .................................................... 55, 165
standard preparation ............................... 58 inspection..............................................138
Potassium hydrogen phthalate, MSDS......... 186 Pure water .......................................................56
Q
Quantitation.................................................... 36
R
R# ................................................................... 90 Replacing (cont.)
RAM ERROR .............................................. 167 halogen scrubber...................................142
RANGE ....................................................84, 90 injector O-rings.....................................145
Recorder .................................................55, 165 ozone treatment catalyst .......................142
inspection ............................................. 138 plunger tip.............................................144
Regeneration ................................................ 139 rotor ......................................................146
Replacing stator .....................................................146
catalyst ................................................. 140 Rotor, replacement........................................146
CO2 absorber........................................ 141 RP ...................................................................79
combustion tube ................................... 141
S
S#........................................84, 87, 90, 93, 104 Screen descriptions (cont.)
Salt................................................................ 133 MONITOR(C) ......................................123
deposits................................................. 134 MONITOR(N) ......................................124
Sample OFF-LINE MEAS COND (1) ..............103
acidic, alkaline and saline .................... 132 OFF-LINE MEAS COND
delivery lines .......................................... 18 (2)-SPECIFIC .......................106
injection.................................................. 32 OFF-LINE MEAS COND (3) ..............108
injection stream inspection................... 138 OFF-LINE MEAS COND
injection volume..................................... 59 (2)-SELECT..........................104
injector O-rings .................................... 145 OFF-LINE MEASURING....................110
pretreatment............................................ 32 ON-LINE MEAS START ......................95
suspended substances ........................... 132 ON-LINE MEAS START-PAUSE
SAMPLE # ...........................................104, 106 SETTING................................97
SAMPLE WASH ........................................... 77 ON-LINE MEASURING .......................99
Sampling ........................................................ 28 OUTPUT TERMINAL STATUS.........128
pipe set ................................................. 158 PEAK(C) PROFILE .............................101
SAMPLING TIME......................................... 76 PEAK(N) PROFILE .............................101
Screen descriptions......................................... 72 SERVICE..............................................119
CAL CURVE ......................................... 82 SMPL MEAS/CONDITIONS (1) ..........83
CAL DATA RECORD ........................ 127 SMPL MEAS/CONDITIONS
CALIBRATION CURVE (1) help....................................85
MEASURING ...................... 113 SMPL MEAS/CONDITIONS
CALIBRATION START ..................... 112 (2)-SCHEDULE .....................86
CALIBRATION/CONDITIONS ........... 78 SMPL MEAS/CONDITIONS
COUNTER (1) ..................................... 116 (3)-AUTO CAL,CAT REG ....88
COUNTER (2) ..................................... 117 SMPL MEAS/CONDITIONS
GENERAL CONDITIONS.................... 76 (4)-ANALOG OUTPUT.........90
INITIAL ................................................. 73 SMPL MEAS/CONDITIONS
MAINTENANCE ................................ 114 (5)-ALARM............................92
MECHANICAL CHECK .................... 120 TERMINAL TABLE..............................94
MENU .................................................... 74 TREND GRAPH ..................................126
Scrubber, connection ......................................43
SD ........................................................ 104, 108
Index-4
Index
SELECT VALVE DEFECT.........................167 Specification
SERVICE screen ..........................................119 differences................................................ 2
SET DATE AND TIME ...............................168 TN-4110 ................................................... 9
Shifting to origin.............................................34 TOC-4110 ................................................ 7
Short cell purge, CO2 absorber.......................50 TOCN-4110 ............................................. 5
SHORT CYCLE TIME ..................................77 SPG ................................................................ 85
Shut down .....................................................135 Standard
Signal interval.................................................20 bottle installation.................................... 47
Site requirements ............................................14 IC............................................................ 58
SLIDER DEFECT ........................................167 POC........................................................ 58
SMPL MEAS/CONDITIONS solution inspection ............................... 137
(1) help screen ...............................85 solution switching set........................... 161
SMPL MEAS/CONDITIONS TC........................................................... 57
(1) screen ........................................83 TC/TN .................................................... 58
SMPL MEAS/CONDITIONS TN .......................................................... 57
(2)-SCHEDULE screen ..................86 Standard accessories ...................................... 11
SMPL MEAS/CONDITIONS STARTING TIME ......................................... 95
(3)-AUTO CAL,CAT REG screen.88 Stator, replacement....................................... 146
SMPL MEAS/CONDITIONS STD ................................................................ 79
(4)-ANALOG OUTPUT screen .....90 Suspended particle flow line switcher ......... 159
SMPL MEAS/CONDITIONS (5)-ALARM Suspended solids unit
screen..............................................92 multi-stream ......................................... 154
Sodium bicarbonate, MSDS .........................184 single stream ........................................ 155
Sodium carbonate, MSDS ............................185 Suspended substances .................................. 132
Sodium persulfate, MSDS ............................187 Syringe
SP....................................................................80 assembly................................................. 46
Sparge holder ..................................................... 46
cleaning tubing .....................................145 plunger tip ............................................ 144
CO2 absorber ..........................................50 SYRINGE HOME POSITION
gas flow rate ...........................................62 DEFECT...................................... 168
standard...................................................35 SYRINGE PUMP DEFECT ........................ 168
SPARGE TIME ............................................107 SYRINGE ZERO POINT
Special accessories ................................ 12, 157 DEFECT....................................... 168
T
TC TOC/TN
catalyst....................................................61 catalyst ................................................... 40
measurement...........................................25 TOC1.............................................................. 27
standard preparation ...............................57 TOC2.............................................................. 27
TC/TN TOC-4110
standard preparation ...............................58 flow line ................................................. 30
TERM .............................................................93 specification ............................................. 7
Terminal board ...............................................19 TOCN-4110
TERMINAL TABLE screen ..........................94 flow line ................................................. 29
THERMOCOUPLE DISCONNECTED ......168 specification ............................................. 5
THERMOCOUPLE SHORTEN ..................168 TOLERANCE (CAL) .................................... 77
TN TREND GRAPH screen............................... 126
measurement...................................... 2, 27 Troubleshooting ........................................... 170
standard preparation ...............................57 Tubing
TN-4110 exhaust ................................................... 17
flow line..................................................31 sample delivery ...................................... 18
specification..............................................9 sparge, cleaning.................................... 145
TOC TYP ................................................................ 79
catalyst....................................................41 TYP. ............................................................... 87
measurement...........................................27 TYPE........................................ 84, 90, 93, 106
Type-B halogen scrubber ............................. 153
V
VALVE SELF-PROT INT .............................76
Index-5
Index
W
Warning, definition of...................................... 2 Water
WASH BEWTEEN SMPL ............................ 77 dilution....................................................48
Washing.......................................................... 33 pure .........................................................56
catalyst ................................................. 140
combustion tube ................................... 141
Z
Zero adjustment, NDIR................................ 150 ZS....................................................................80
Zero correction ............................................... 59
Index-6