450TOC Portable TOC Analyzer Standard Operating Procedure For
450TOC Portable TOC Analyzer Standard Operating Procedure For
450TOC Portable TOC Analyzer Standard Operating Procedure For
58130474
This document contains proprietary information, which is protected by copyright. All rights are reserved. No part of this
document may be photocopied (other than where specifically noted), reproduced or translated, into another language without
the prior written consent of Mettler-Toledo Thornton, Inc.
IMPORTANT SAFETY INFORMATION
Please read thoroughly before operating the TOC System Suitability Test Kit and the TOC Calibration Kit -
• Follow all warnings, cautions, and instructions indicated on and supplied with this product.
• Install equipment as specified in this instruction manual. Follow appropriate local and national codes.
• Use only factory documented components for repair. Tampering or unauthorized substitution of parts and procedures can
affect the performance and cause unsafe operation of your process as well as void factory warranties.
• Protective covers must be in place unless qualified personnel are performing maintenance.
• If this equipment is used in a manner not specified by the manufacturer, the protection provided by it against hazards may
be impaired.
• Prior to shipping the sensor back to the factory for repair or re-calibration, water MUST be drained from sensor to avoid
damage due to freezing.
WARNINGS:
• Installation of cable connections and servicing of this product require access to shock hazard voltage levels.
• Main power must employ a switch or circuit breaker as the disconnecting device for the equipment.
• Electrical installation must be in accordance with the National Electrical Code and/or any other applicable national or local
codes.
• Safety and performance require that this Analyzer be connected and properly grounded through a three-wire power source.
This manual includes safety information with the following designations and formats:
2. Scope
This document provides procedures to calibrate the Thornton 450TOC Portable TOC Analyzer (PN 58 036 041). This
document provides strategies for the frequency and content of “As Found” data and the calibration process with respect to lamp
changes and performing System Suitability Tests (SST) to meet specific pharmacopeia requirements.
3. Calibration Process
The complete calibration of the 450TOC Portable TOC Analyzer consists of calibration of the following:
Determination of answers for these questions, as shown in the flowchart, will determine the sequence of operations. The
answers are determined by the users of this Analyzer, but Table 1 lists Thornton's minimum recommended service cycle.
Calibration process
Yes Yes
TOC cal only or
complete cal?
TOC Startup
TOC Only
Complete
Return
Perform Perform to
Get As Found Flow TOC Operation
TOC data Calibration Calibration
Perform
Temperature
Calibration
Change Lamp
(if needed)
Perform SST
Perform
Conductivity
Calibration
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Table 1. Scheduled Calibration, Lamp change, and SST Service
Maintenance Frequency/Schedule Recommendations/Comments
Replace lamp 4500 hours of lamp operation or • TOC Calibration recommended after lamp change.
1 calendar year, whichever is • SST recommended after lamp change (where SST is
shorter. required*). Refer to SST Standard Operating Procedure.
TOC Calibration After UV lamp replacement, not to • Recommended after lamp change, not to exceed 1
exceed one calendar year. calendar year.
Complete Calibration As determined by user. • Recommended not to exceed 1 calendar year.
(includes flow, TOC,
conductivity, temperature)
System Suitability Test As determined by user. • Recommended after UV lamp change.
(SST)
*See USP <643> and EP 2.2.44
4. Equipment Required
4.1. Full Calibration
For a complete calibration (flow, temperature, conductivity, and TOC), the following equipment is required.
• CAL/SST Module Kit (Thornton PN 58 091 566). This kit consists of a calibrated conductivity sensor, patch cable, 316L SS
flow housing, holding brackets, SOP for Calibration, pump, power supply, and miscellaneous connectors and tubing, all
stored in a case.
• An appropriate TOC Calibration Solution Set:
For a Standard Calibration (Up to 1000 ppb)
- 58 091 529: Calibration Standards solution kit for Standard TOC calibration
- 58 091 537: Combination Calibration Standards solution kit for Standard TOC calibration plus
System Suitability Standards
• Stop watch or other timing device with 1 second resolution for flow calibration process.
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• 100 mL or larger volumetric container such as graduated cylinder with <3% accuracy tolerance for flow calibration
process.
• Latex/nitrile gloves are recommended during the procedure when wetted components such as tubing are handled.
• TOC Cal/SST Module Kit (Thornton P/N 58 091 566 or equivalent) is required. The Cal/SST Module Kit is described above.
• TOC Calibration Solution Set (Thornton PN 58 091 529).
1. Record all relevant information regarding the unit under test (UUT) on a copy of the Calibration Worksheet found at the end
of this document (or equivalent) in Section A: Equipment Information.
2. Record all relevant information regarding the reference system on a copy of the Calibration Worksheet found at the end of
this document (or equivalent) in Section A: Equipment Information.
This procedure will use conductivity in units of µS/cm and temperature in degrees Celsius. Alternative measurement units may
be used if desired.
For a full system calibration, a separate reference conductivity sensor and transmitter must be used. Please refer to the
appropriate documentation for configuration instructions. It is recommended that the reference transmitter be configured to
display conductivity in µS/cm (resolution: 3 decimal places), and temperature in degrees Celsius (°C, resolution: 1 decimal
place).
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6.1. TOC CAL/SST Module Setup for Temperature and Conductivity
1. Set up the CAL/SST Pump Stand on a clean, flat work surface by placing the four rubber feet on the work surface, and
inserting the tabs at the bottom of the rear panel into the slots on the base.
2. Hang the CALl/SST Module on the mounting hook provided on the stand. Refer to figure 1.
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Figure 2. CAL/SST Pump Module Setup for Cond/Temp
6.2. TOC CAL/SST Module Setup for TOC and Flow Figure 3. Suction Tube Installation
1. Set up the CAL/SST Pump Stand on a clean, flat work surface by placing
the four rubber feet on the work surface, and inserting the tabs at the bottom of the rear panel into the slots on the base.
2. Hang the CAL/SST Module on the mounting hook provided on the stand. Refer to figure 4.
3. Remove the 60 micron filter assembly from the 450TOC inlet.
4. Attach the threaded end of the connection tube equipped with the male quick-disconnect fitting to the 450TOC Sample Inlet
connection. After the threaded connection is made, push the quick-disconnect fitting into mating connector found on the
lower right side of the CAL/SST pump module marked ‘to TOC sample inlet’. Ensure proper connection is made.
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Figure 4. CAL/SST Pump Module Setup for TOC and Flow
5. Set selector valve on CAL/SST pump module to “SST, TOC CAL” position. Figure 4 shows the proper installation of the
CAL/SST pump module.
6. Verify the CAL/SST module power switch is in the off position. The switch is located on the right side of the module.
7. Connect the Universal Power Supply to the pump and to 100–240 VAC 50-60 Hz power. The kit includes a universal AC
adaptor with assorted international standard connectors. Select the appropriate AC connector, and install it onto the AC
adaptor and connect to the AC supply.
8. Remove the grey, threaded, protective cap from the bottom of the CAL/SST Pump Module.
6.3. Final Installation of the TOC CAL/SST Module for Conductivity and Temperature Calibration
1. If calibrating conductivity or temperature, connect the reference conductivity/temperature sensor to an appropriate
transmitter or display.
2. Configure the reference transmitter readout to display the reference sensor temperature and temperature compensated
conductivity.
3. Set the selector valve on the CAL/SST pump module to “Cond/Res CAL and Temp CAL” position. Figure 2 shows the proper
installation of the CAL/SST pump module.
4. Energize the CAL/SST module pump. The setup should now be such that water continuously circulates through the Blank
Water bottle and the 450TOC Analyzer.
5. The system is now ready for temperature or conductivity calibration. The pump may be left on if you are proceeding to the
Section 9 Temperature Calibration.
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Prior to performing any maintenance or calibration steps, collection of as-found TOC readings should be performed if desired.
Perform these steps prior to replacement of the UV Lamp. Record this data in the As-Found portion of Section E of the
Calibration Test Report.
This procedure uses a “volume and time” method for calibrating the flow sensor. Process water may be used for this
calibration. The end of the drain tube at the sample outlet is the measurement point.
NOTE: Since it is possible for the person performing this calibration to come into contact with the process water, use of
protective gloves, or other suitable safety equipment is recommended.
Caution: If the process water is hot, protection from direct contact should be used, or an alternate source of water must be
provided.
Record this data in the As-Found portion of Section B of the Calibration Test Report.
8.2. Flow Rate Verification before Calibration
1. Record the as-found flow calibration factors:
a. Press the Info ( ) key on the 450TOC.
b. Press or to select Calibration Data and press Enter.
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c. Press or to select Flow and press Enter.
d. Record the calibration data displayed.
e. Simultaneously press Menu and Cal (⊳ and ) to return to Measurement Mode.
2. Set up equipment as described in section 6.2 TOC CAL/SST Module Setup for TOC and Flow using Blank Water. Optionally,
the flow rate verification and calibration may be done using process water, with the TOC Analyzer connected to the water
system as normal.
3. If using the CAL/SST Module, ensure the selector valve is set to the ‘SST/TOC Cal’ position.
4. Arrange the drain tube at the atmospheric drain such that the water dripping from it may be collected into the volumetric
container.
5. Energize the pump on the CAL/SST module, or restore flow to the TOC Analyzer as necessary. If using the CAL/SST module,
allow 30 seconds for the flow to stabilize. Place a dry volumetric container under the drain line to capture the water, and
begin the time measurement using the stop watch. It is important that the water collection and start time be closely
matched.
6. Collect a known volume of water with the volumetric container for a specific time, at least 2 minutes.
7. Turn off the CAL/SST pump.
8. In Section B of the calibration sheet under Flow As-Found Data, record the volume of water in mL and the elapsed time in
seconds. These two values determine the reference flow rate, Fref.
9. Calculate the reference flow rate and record as Fref according to the equation below. The volume may also be determined
by weight. Measure the mass increase of the container in grams, and divide the mass by the density of the water
(typically, 1.00 g/mL at room temperature).
60 sec/min × volume collected (mL)
Flow Rate (mL/min) = Fref = Eq. 1
Elapsed Time (sec)
10. If (Fref- - 20) is within the limit, then flow rate adjustment is not required. If no flow adjustment is required, proceed to
Section 9. Temperature Calibration. Otherwise, proceed to the next section to perform a flow rate calibration.
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8.4. Flow Rate Verification After Calibration
1. Repeat steps described in Section 8.2 Flow Rate Verification before Calibration to verify the flow sensor is in calibration.
2. Record data in section B of the calibration worksheet under Flow Sensor Verification After Calibration.
Flow Calibration is complete.
9. Temperature Calibration
This procedure is to be performed on T1 and T2, which correspond to the temperature sensors embedded in the two
conductivity sensors within the 450TOC. In order to record as-left readings, configure the 450TOC to display the temperature
reading.
1. Record data in section C of the calibration worksheet under Temperature Sensor Calibration and Verification.
2. Turn off the UV lamp (if not already off) by pressing the lamp button so that the green UV Lamp On LED is off. The lamp
shall remain off throughout this procedure.
3. Set up the Cal/SST Module using Blank Water as described in Section 6.1.
4. Ensure the selector valve on the CAL/SST module is set to “Cond/Res and Temp Cal’ position.
5. On the 450TOC, press 'Cal' ( ) to enter calibration mode.
6. Press or to select Temperature1 and press Enter.
7. Press enter. A 1-Point Offset calibration is the only method available for calibration of the TOC temperature measurement.
8. Turn on the pump. Water should now be continuously circulating through the pump, 450TOC Analyzer, Reference
Conductivity Sensor, the bottle containing the blank water, and back through the pump.
9. Press Enter.
10. Allow the pump to run until thermal equilibrium is achieved, typically 1/2 hour (less if the lamp has been off).
11. Enter the reference value into the 450TOC once the reference reading has stabilized. To avoid inaccuracy due to changes in
ambient temperature, this value should be entered as soon as possible after reading the Reference Sensor.
12. Record the multiplier (M) and adder (A) for the calibrated temperature measurement in section C of the calibration
worksheet under Temperature Sensor Calibration and Verification.
13. Press Enter to save the new calibration data within the 450TOC. If 'No' is selected, the previous calibration will be restored.
14. After returning to measurement mode on the 450TOC, record the temperature of Tref and Tafter for T1 on the calibration
worksheet. Under Temperature Sensor Calibration and Verification.
a. Record the temperature reading of the reference temperature sensor as Tref.
b. Record the temperature reading as indicated by the TOC Analyzer as Tafter.
15. Verify that Tref – Tafter is within limits for T1. If they exceed limits, repeat the temperature calibration procedure.
16. Repeat steps 5-13, selecting Temperature2 at step 6.
1. Record data in section D of the calibration worksheet under Conductivity Sensor Calibration and Verification.
2. Turn off the UV lamp (if not already off) by pressing the lamp button so that the green UV Lamp On LED is off. The lamp
shall remain off throughout this procedure.
3. If not already done, set up the CAL/SST Module using Blank Water as described in section 6.1.
4. Ensure the selector valve on the CAL/SST module is set to “Cond/Res Cal and Temp Cal’ position.
5. If a Temperature calibration has just been performed, continue using the same Blank Water bottle. Verify that the water
conductivity is <1.5 µS/cm (>0.67 MΩ-cm) as reported by the Reference Conductivity sensor. If the water conductivity
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has increased above 1.5 µS/cm, then turn off the pump, install a fresh bottle of Blank Water, and restart the pump. Note
that the conductivity sensors can be calibrated above 1.5 µS/cm with no adverse measurement impact, but it is
recommended a calibration value that closely matches values found in the process water being monitored by the Analyzer.
6. If the Blank Water bottle has been changed, allow the pump to run until complete mixing and thermal equilibrium is
achieved, typically 30 minutes. Otherwise, continue to the next step
7. On the 450TOC, press 'Cal' ( ) to enter calibration mode.
8. Press or to select Conductivity1 and press Enter.
9. Press or to select the conductivity compensation method to be used during calibration. 'Standard' compensation is
recommended.
10. Press Enter. A 1-Point calibration is the only method available for calibration of the TOC conductivity measurement.
11. Turn on the pump. Water should now be continuously circulating through the pump, 450TOC Analyzer, Reference
Conductivity Sensor, the bottle containing the blank water, and back through the pump.
12. Press Enter.
13. Once the readings from the reference sensor and C1 have stabilized, enter the conductivity reading of the Reference Sensor
into the 450TOC using the arrow keys and press Enter. To avoid inaccuracy due to changes in ambient temperature, this
value should be entered as soon as practical after reading the Reference Sensor.
14. Record the multiplier (M) and adder (A) for the calibrated conductivity measurement in section D of the calibration
worksheet under Conductivity Sensor Calibration and Verification.
15. Press Enter to save the new calibration data within the 450TOC. If 'No' is selected, the previous calibration will be restored.
16. After returning to measurement mode on the 450TOC, record the indicated conductivity for C1 and Cref on the calibration
worksheet under Conductivity Sensor Calibration and Verification.
a. Record the conductivity reading of the reference sensor as Cref.
b. Record the conductivity reading as indicated by the TOC Analyzer as Cafter.
17. Compute the % difference according to eq 2.
100 × (Cafter - Cref )
Eq. 2
Cref
18. Verify that the % difference is within limits. If not, repeat the Conductivity Calibration process.
19. Repeat steps 7-15, selecting Conductivity2 at step 8.
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11. TOC Calibration
Calibration is performed using TOC Standard Solutions of known concentration. Mettler-Toledo Thornton provides Calibration
Solution Sets for this purpose. Refer to Section 4.1 for more detail on which kits should be used for calibration. If performing a
1-point slope calibration, then use only the bottle of 500 ppb TOC (sucrose) calibration solution.
1. Record data in section E of the calibration worksheet under TOC Measurement Calibration and Verification.
2. If not already completed, set up the CAL/SST kit as described in Section 6.2 TOC CAL/SST Module Setup for TOC and Flow
and attach the 250 ppb calibration solution bottle to the CAL/SST module.
3. On the 450TOC, press 'Cal' ( ) to enter calibration mode.
4. Press or to select TOC and press Enter.
5. Select the calibration method to be performed:
a. Normally, the Standard calibration method is performed, and is ideal for most applications monitoring TOC
levels below 1000 ppbC. Solution Kit PNs 58 091 529 or 58 091 537 should be used for this calibration.
b. 1-point Slope calibration is a special purpose calibration which should only be used in very specific
situations. Please refer to the 450TOC instruction manual for guidance.
6. Turn on the pump.
7. Press Enter.
8. Allow the 250 ppb TOC solution to flow the 450TOC Analyzer until the readings stabilize, approximately 5 minutes.
9. Use the arrow keys on the 450TOC to enter the TOC value of the Reference Solution as written on the label or its certificate
into the 450TOC for Cal point 1 and press Enter.
10. Turn off the pump.
11. Remove the 250 ppb TOC solution bottle from the calibration apparatus and replace it with the 500 ppb TOC solution.
12. Turn on the pump.
13. Verify the UV lamp is on. The lamp must be on to measure and display TOC. If the 450TOC is not set to automatically
restart, the lamp will need to be energized manually.
14. Allow the 500 ppb TOC solution to flow the 450TOC Analyzer until the readings stabilize, approximately 5 minutes.
15. Use the arrow keys on the 450TOC to enter the TOC value of the Reference Solution as written on the label or its certificate
into the 450TOC for Cal point 2and press Enter.
16. Record the multiplier(s) (M) and adder(s) (A) for the calibrated TOC measurement in section E of the calibration worksheet
under TOC Measurement Calibration and Verification.
17. Press Enter to save the new calibration data within the 450TOC. If 'No' is selected, the previous calibration will be restored.
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13. Record As-Found Temperature Data
If required for retention, collect as-found temperature calibration data using the following procedure.
1. Record the As Found Temperature T1 data in Section C of the calibration worksheet under Temperature As-Found Data.
2. Record the as-found T1 calibration factors:
a. Press the Info ( ) key on the 450TOC.
b. Press or to select Calibration Data and press Enter.
c. Press or to select Temperature and press Enter.
d. Record the calibration data displayed.
e. Simultaneously press Menu and Cal (⊳ and ) to return to Measurement Mode.
3. Turn off the UV lamp (if not already off) by pressing the lamp button so that the green UV Lamp On LED is off. The lamp
shall remain off throughout this procedure.
4. If not already done, set up the Cal/SST Module using Blank Water as described in section 6.1.
5. Ensure the selector valve on the CAL/SST module is set to “Cond/Res Cal and Temp Cal’ position.
6. Turn on the pump. Water should now be continuously circulating through the pump, 450TOC Analyzer, Reference
Conductivity Sensor, the bottle containing the blank water, and back through the pump.
7. In Section C of the calibration sheet under Temperature As-Found data, record the Reference Sensor temperature, Tref
8. Record the T1 temperature displayed on the 450TOC, Tbefore.
9. Compute the difference, Tbefore-Tref.
10. If the absolute value of the difference is less than the limit, then a temperature calibration is not required.
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15. Restore to Operation
1. Restore the drain and supply connections to the 450TOC to the same operational configuration prior to calibration.
2. Connect the process water line to the 450TOC Analyzer sample inlet.
3. Turn on the process water supply to the 450TOC Analyzer using the shut off valve (recommended in the 450TOC Portable
TOC Analyzer Operation Manual). Ensure the process water supply is turned on by viewing the discharge line from the TOC
analyzer at the atmospheric drain.
4. Turn on the UV Lamp.
5. Flush the CAL/SST Module and connected tubing with blank water for 3 to 5 minutes. If there is not adequate blank water
remaining, a blank water bottle may be filled with RO quality water or better. Flush the CAL/SST Module. Ensure that the
drain tube is directed to an appropriate drain. If an adequate drain is not available, use an empty test solution bottle to
collect the flushing water.
6. If a temperature and/or conductivity calibration was performed, proceed to the next section to flush and drain the reference
conductivity sensor and housing. Otherwise, remove the blank water bottle from the CAL/SST module, remove and discard
the silicon suction tube, and replace the protective cap for the solution bottle interface. Remove the CAL/SST module and
mounting bracket from the TOC Analyzer.
9. Connect both provided tubes to the quick-disconnect fittings on the lower right side of the CAL/SST Module.
10. Set the selector valve to the “Cond/Res and Temp Cal’ position.
11. Connect a bottle of the supplied blank water to the CAL/SST Module. If the remaining blank water is not sufficient, a blank
water bottle may be filled with process water of RO quality or better to flush the CAL/SST Module.
12. Turn the pump on and flush the CAL/SST Module for a minimum of 5 minutes. Ensure that the discharge tube from the
CAL/SST module (marked “To TOC Sample Inlet”) is directed to an appropriate drain. If an adequate drain is not available,
use an empty test solution bottle to collect the flushing water.
13. Remove the blank water bottle from the CAL/SST module. Allow the CAL/SST Module pump to run until all solution has
been discharged from the CAL/SST module.
14. Remove and discard the silicon suction tube from the solution bottle interface, and replace the protective cap.
15. With both lines attached to the CAL/SST module and the selector valve in the Con/Res and Temp Cal position, connect the
provided syringe and quick-disconnect assembly to the quick-disconnect fitting located at the bottom of the CAL/SST
module. Pull the plunger of the syringe back to draw the residual water out of the Conductivity sensor flow housing.
Remove the syringe from the silicone tubing and empty the syringe into an appropriate drain or container. If necessary,
repeat this process until all solution has been removed.
Remove the CAL/SST module and mounting bracket from the TOC Analyzer. Remove all connected tubing from the CAL/SST
module and return all components to the supplied storage case.
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450TOC Analyzer Calibration Worksheet Page 1 of 2
Performed By:
Name (Print) Signature Date
450TOC Analyzer Calibration Worksheet Page 2 of 2
*Required for Standard only. Mark N/A if not needed for current calibration method
Performed By:
Name (Print) Signature Date
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Mettler-Toledo Thornton, Inc. www.mt.com/thornton
900 Middlesex Turnpike, Bldg 8
Billerica, MA 01821
Tel. +1-781-301-8600
Fax +1-781-301-8701
Toll Free +1-800-510-PURE (US and Canada only)
thornton.info@mt.com
Part 58130474
Rev.B 1/18