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MICLAB-115 Operation and Calibration of Sievers 820 TOC Analyser

DepartmentMicro LaboratoryDocument noMICLAB 115
TitleTOC Analyser – Operation and Calibration of Sievers 820 (brand) Analyser
Prepared by: Date: Supersedes: 
Checked by: Date: Date Issued: 
Approved by: Date: Review Date: 

 

Document Owner

Micro Laboratory Manager

Affected Parties

All Microbiology Laboratory colleagues

Purpose

To define the procedures to be followed and the responsibility for the operation, calibration and maintenance of the Sievers 820 TOC Analyser with Autosampler.

Scope

This procedure is to be followed by all personnel who carry out TOC analysis for testing of Purified water for production use and analysis of cleaning validation samples.  This SOP details the operation and calibration of the Sievers 820 model only.

Definition

TCTotal Carbon – including organic carbon plus inorganic carbon
ICInorganic Carbon
TOCTotal Organic Carbon
DIDeionised

 

Related Documents

VAL-020Procedure for Cleaning Validation
Form 615TOC Analyser Calibration Worksheets

 

1.          Inorganic Carbon Standard Worksheet

2.          Organic Carbon Standard Worksheet

3.          Calibration Worksheet for Autosampler Calibration

4.          500 ppb Sucrose Standard Worksheet

5.          500 ppb Benzoquinone Standard Worksheet

6.          Suitability Verification Worksheet

 

EHS Statement

Safety glasses must be worn when using this equipment.

Calibration Procedure

Note:
Calibration of the Instrument including the system suitability test must be performed on a 12 monthly basis.

Preparation of Calibration Standards

1. 25 ppm IC as Sodium Carbonate – standard preparation procedure

Materials and Equipment:

Materials:

Sodium Carbonate anhydrous, Na2CO3 Analytical Reagent Grade (Mol wt. 105.99 g/mol)

Para film

Equipment:

Milli-Q water

100mL volumetric flask, Class A

50mL volumetric pipette, Class A

1 L volumetric flask, Class A

Procedure

1.1.             Obtain required glassware and thoroughly rinse 5 times with Milli-Q water.
Note: For Calibration solutions dedicated glassware must be used, therefore use only glassware identified for the standard being prepared.  Ensure all pipettes are cleaned and thoroughly rinsed with Milli-Q water.

1.2.             Obtain an “Inorganic Carbon Standard Worksheet” (Form 615).

1.2.1.       Record the current date and name of preparer in line 1.

1.2.2.       Record the lot number of the Na2CO3 in line 2.

1.3.             Dry approximately 1-2 grams Na2CO3 in an oven.

1.3.1.       Place the Na2CO3 into a clean beaker and place in a 110C oven for not less than 2 hours.

1.3.2.       Transfer the Na2CO3 into a desiccator and allow the material to cool to room temperature.

1.4.             Weigh dried Na2CO3 for preparation of standard.

1.4.1.       Record the weight of the weigh boat in line 4 of the “Inorganic Carbon Standard Worksheet” (Form 615).

1.4.2.       Accurately weigh out approximately 0.441 + 0.0001g Na2CO3 in the weigh boat, and record the value in line 3 of the “Inorganic Carbon Standard Worksheet”.

1.4.3.       Calculate the difference in line 5 of the “Inorganic Carbon Standard Worksheet”.

1.5.             Transfer to 100mL volumetric flask.

1.5.1.       Dilute solid with Milli-Q water while it is in the weigh boat.

1.5.2.       Verify the water used in preparation contains less than 100 ppb TC and IC.

1.5.3.       Transfer the contents of the weigh boat into the 100mL volumetric flask.

1.5.4.       Using Milli-Q water, wash down the weigh boat, flask neck, and ground glass joint and allow the rinse water to flow into the 100mL volumetric flask.

1.5.5.       Add Milli-Q water until the 100mL volumetric flask is approximately 50% full.

1.5.6.       Ensure that the Na2CO3 is fully dissolved.

1.6.             Dilute the solution to 100mL.

1.6.1.       Add Milli-Q water to the 100mL volumetric flask to bring the total volume to 100mL.

1.6.2.       Cover the flask with volumetric lid and than with the clean side of a 4″ x 4″ square of Para film.

1.6.3.       Invert the flask not less than 3 times and mix well.

1.7.             Calculate the carbon concentration of the stock solution
conc. of stock IC std (ppm) = Weight of Na2CO3 (g) x 12.01g C/mol x 1000
(0.1L) x (105.99 g/mol Na2CO3)

1.7.1.       Record the result in line 6, table 1 of the “Inorganic Carbon Standard Worksheet”.

1.8.             Prepare the dilute IC standard.

1.8.1.       Rinse a 50mL pipette with stock solution twice and drain.

1.8.2.       Pipette 50mL of stock solution into a 1L volumetric flask.

1.8.3.       Dilute to 1L with Milli-Q water, washing down the neck and ground glass joint of the 1L volumetric flask.

1.8.4.       Cover the flask with volumetric lid and than with a 4″ x 4” square of Para film.

1.8.5.       Invert the flask not less than three times and mix well.

1.8.6.       Calculate the final carbon content of the dilute solution
Conc. of dilute IC standard (ppm) = Conc. of stock (ppm) x 0.05

1.8.7.       Record the final concentration of the dilute standard in line 7, table 2 of the “Inorganic Carbon Standard Worksheet”.

2. 25 ppm TOC as KHP standard preparation procedure

Materials and Equipment:

Materials:

Potassium Acid Phthalate, Primary Standard Grade (Mol wt. 204.22 g/mol)

Para film

Equipment:

Milli-Q Water

100mL volumetric flask, Class A

25mL volumetric pipette, Class A

2 L volumetric flask, Class A

Procedure:

2.1.             Obtain required glassware and ensure it has been cleaned in the Laboratory dishwasher and thoroughly rinsed 5 times with Milli-Q Water.
Note: For Calibration solutions dedicated glassware must be used, therefore use only glassware identified for the standard being prepared.  Ensure all pipettes are cleaned and thoroughly rinsed with Milli-Q Water.

2.2.             Obtain an “Organic Carbon Standard Worksheet” (Form 615).

2.2.1.       Record the current date and name of preparer in line 1

2.2.2.       Record the lot number of the KHP in line 2.

2.3.             Dry approximately 1-2 grams KHP in an oven

2.3.1.       Place the KHP into a clean beaker and place in a 110C oven for not less than 2 hours.

2.3.2.       Transfer the KHP into a desiccator and allow the material to cool to room temperature.

2.4.             Weigh dried KHP for preparation of standard.

2.4.1.       Record the weight of the weigh boat in line 4 of the “Organic Carbon Standard Worksheet”.

2.4.2.       Weigh out approximately 0.425 + 0.0001g KHP in the weigh boat, and record the value in line 3 of the “Organic Carbon Standard Worksheet”.

2.4.3.       Calculate the difference in line 5 of the “Organic Carbon Standard Worksheet”.

2.5.             Transfer to 100mL volumetric flask

2.5.1.       Dilute solid with Milli-Q water while it is in the weigh boat

2.5.2.       Verify the water used in preparation contains less than 100 ppb TC and IC.

2.5.3.       Transfer the contents of the weigh boat into the 100mL volumetric flask.

2.5.4.       Using Milli-Q water, wash down the weigh boat, flask neck, and ground glass joint and allow the rinse water to flow into the 100mL volumetric flask.

2.5.5.       Add Milli-Q water until the 100mL volumetric flask is approximately 50 % full.

2.5.6.       Ensure that the KHP is fully dissolved.

2.6.             Dilute the solution to 100mL.

2.6.1.       Add Milli-Q water to the 100mL volumetric flask to bring the total volume to 100mL

2.6.2.       Cover the flask with volumetric lid and than with the clean side of a 4″ x 4″ square of Para film.

2.6.3.       Invert the flask not less than 3 times and mix well.

2.7.             Calculate the carbon concentration of the stock solution
conc. of stock TC std (ppm) = Weight of KHP (g) x 8 mol C/mol KHP x 12.01g C/mol x 1000
(0.1L) x (204.22 g/mol KHP)

2.7.1.       Record the result in line 6, Table 1 of the “Organic Carbon Standard Worksheet”.

2.8.             Prepare the dilute TC standard

2.8.1.       Rinse a 25mL pipette with approximately 20mL of stock solution and discard.

2.8.2.       Pipette 25mL of stock solution into a 2L volumetric flask.

2.8.3.       Dilute to 2L with Milli-Q water, washing down the neck and ground glass joint of the 2L volumetric flask.

2.8.4.       Cover the flask with volumetric lid and than with a 4″ x 4″square of Para film.

2.8.5.       Invert the flask not less than three times and mix well.

2.8.6.       Calculate the final carbon content of the dilute solution.
Conc. of dilute TC standard (ppm) = Conc. of stock (ppm) x 0.0125

2.8.7.       Record the final concentration of the dilute standard in line 7, Table 2 of the “Organic Carbon Standard Worksheet”.

3. Calibration Procedure

Materials and Equipment:

25 ppm Inorganic Carbon standard (Sodium Carbonate Anhydrous)

25 ppm Total Carbon standard (Potassium Acid Phthalate)

“Calibration Worksheet for Autosampler Calibration” (Form 615).

Powder-free gloves

Model 820 TOC analyser

Autosampler

40mL sample vials.

3.1.             Instrument Set-up for Calibration or Analysis

3.1.1.       Check level of DI reservoir

Prolonged operation of the Model 820 with an Autosampler can lead to loss of water from the internal deionized water reservoir.

Setup Autosampler system

Connect the printer to the parallel printer port on the Laboratory personal computer.

Connect the instrument RS-232 port to the appropriate serial port on the Laboratory personal computer using the cable provided with the Autosampler system.

Connect the Autosampler to the instrument auxiliary port using the cable provided with the Autosampler system.

Power up the instrument and place it in on-line standby if it is not already in on-line mode.  To change from offline to on-line mode do the following:

  • From the Main/Standby Menu on the TOC analyzer, Select SETUP, and press ENTER.
  • Scroll to SAMPLE MODE, and press ENTER.
  • Select ONLINE MODE, and press ENTER.
  • Press CLEAR to return to the Setup Menu.
  • If the instrument is not at the standby menu, (i.e., displays SETUP as the upper left menu choice), press CLEAR until the standby menu appears.

Note
If the instrument begins a measurement cycle, (i.e. displays the measurement display “TOC = xxxx” with the timer counting down), press the ENTER key, scroll to STOP TOC, and press the ENTER key again.

3.1.2.       Power up the Autosampler.

3.1.3.       Power up the Laboratory computer and run Windows, if necessary.

3.1.4.       Locate the Sievers icon and run the Sievers program from Windows.  The instrument is now ready to commence analysing.

3.1.5.       Prior to starting analysis run a low TOC water blank (4 injections) to ensure instrument is functioning and is clean.  The TOC result must be less than 200 ppb and show consistency between injections.  Note the first sample is always discarded in average calculations by the software.

4. Performing Calibration – Prepare the following Calibration Protocol file using the Sievers program

The sampling schedule is as follows:

 

Sample

Sample

No.

Acid Flow°

Rate No.

Oxidizer Flow°

Rate (mL/min)

No. of Replicates/

Sample (mL/min)

DI blank 1,2,3 0.75 0.00 4
25 ppm TC (KHP) 4,5,6 0.75 2.50 4
25 ppm IC (Na2CO3) 7,8,9 0.75 0.00 4
Cleanup (DI)    10 –.— –.—
           

Select Create New Protocol from the Files menu.

Enter the protocol file name without an extension at the prompt.

An empty protocol file will be displayed for editing.

Highlight the protocol file window then use the       button to zoom the window to full screen.

Edit the protocol by typing in the following:

No. Group Name Samp./group Rep./Sample Acid Rate Oxid. Rate
1 DI water blank 1 4 0.75 0.00
2 25 ppm TC (KHP) 1 4 0.75 2.50
3 25 ppm IC (Na2CO3) 1 4 0.75 0.00

The software will automatically add the cleanup vial to the Table when you save the protocol.

Type over any defaults in the columns for each group.

Check the table in the protocol program to ensure it is correct.

Select Save Displayed Protocol from the Files menu.

Use Save and return to menu to save the protocol.

Use Save As ____ and return to menu to select a new name or path.’

Use the    button to zoom the windows to normal size.

4.1.             Prepare a water blank flask

Fill 3 x 40mL vials with the same water used to prepare the 25 ppm standards.  Label as “DI Blank”.

4.2.             Fill the sample vials and load in Autosampler

4.2.1.       Always use clean sample vials, caps, and septa and rinse the solution to be analyzed 3 times into the vial.

4.2.2.       Label each vial with the standard name, including the blanks and the cleanup vial.

4.2.3.       Obtain a standard or blank to be measured in the protocol.

4.2.4.       Fill three vials directly from the standard flask.

4.2.5.       Re-seal the standard flask.

4.2.6.       Repeat for each remaining standard.

4.2.7.       Fill one cleanup vial with Milli-Q water.

4.2.8.       Load the vials sequentially into the Autosampler according to the sampling schedule.

4.2.9.       Ensure that the cleanup vial is the last vial in the sequence.

4.2.10.    Using the index button on the left rear of the Autosampler, index the vials until the first blank vial is directly under the sampling needle.

4.3.             Run the protocol file from the Autosampler software

4.3.1.       Select the Run Current Protocol from the Start menu.

4.3.2.       The operator is prompted with a default data file name always use this default name.  DO NOT type in your own otherwise potential data loss is possible.  The default filename is based on the date analyzed and a sequential number, e.g. 10299704.DAT is the fourth run analyzed on 29.10.97.

4.3.3.       The analysis will start once filename is accepted.

4.3.4.       Wait for the system to complete the measurement protocol.

4.3.5.       The system will automatically measure each sample, update the results table, and print a report.

4.4.             Record results and calculate calibration constants

4.4.1.       Obtain an Autosampler “Calibration Worksheet for Autosampler Calibration”
(Form 615).

4.4.2.       Record the date and name of analyst on the “Calibration Worksheet for Autosampler Calibration”.

4.4.3.       At the completion of the run, select Quit, go into TOC mode and return to Windows.  Record the average TC for the third blank sample on the “Calibration Worksheet for Autosampler Calibration” as TCDI blank.

4.4.4.       Record the average TC for the third TC(KHP) sample on the “Calibration Worksheet for Autosampler Calibration” as TCave,TC.

4.4.5.       Record the average TC for the third IC (Na2CO3) sample on the “Calibration Worksheet for Autosampler Calibration” as TCave,IC.

4.4.6.       Record the average IC for the third IC (Na2CO3) sample on the “Calibration Worksheet for Autosampler Calibration”) as ICave,IC.

4.4.7.       Record the concentration of the TC (KHP) standard from formulation on the “Calibration Worksheet for Autosampler Calibration” as TCstd.

4.4.8.       Calculate the adjusted TC value of the TC standard:

TCadj,TC = TCstd + TCDI blank

4.4.9.       Record the adjusted value of the TC standard on the “Calibration Worksheet for Autosampler Calibration” as TCadj,TC.

4.4.10.    Recall the current TC calibration factor from the front panel of the instrument:

On the PC go to quit and select Quit, go to TOC panel and make changes.

4.4.11.    Scroll to CALIBRATE, and press ENTER.

4.4.12.    Select 50Hz Calibration

4.4.13.    Scroll to TC CALIB. CONSTANT and press ENTER.

4.4.14.    The current TC calibration constant is displayed along with the highlighted cursor.

4.4.15.    Record the current TC calibration constant on the “Calibration Worksheet for Autosampler Calibration” as TCcal,old.

4.4.16.    Calculate the new TC calibration constant using the formula:

TCcal,new   =    TCcal,old   x   TCadj,TC
TCave,TC

4.4.17.    Scroll to select the first digit of the new TC calibration constant, and press ENTER to save this value. If a mistake is made in entering the value, press CLEAR to start again.

4.4.18.    Scroll to the decimal point, and press ENTER.

4.4.19.    Repeat this process to enter and save the remaining values for the TC calibration constant, and press ENTER each time to store the value.  Five significant figures are used for the calibration constants.

4.4.20.    The display asks if the numbers are correct. If the numbers are correct, press ENTER.

4.4.21.    Record the value of the new TC calibration constant as TCcal,new on the “Calibration Worksheet for Autosampler Calibration”.

4.4.22.    Recall the current IC calibration factor from the front panel of the instrument.

4.4.23.    Scroll to CALIBRATE, and press ENTER.

4.4.24.    Scroll to IC CALIB. CONSTANT and press ENTER.

4.4.25.    The current IC calibration constant is displayed along with the highlighted cursor.

4.4.26.    Record the current IC calibration constant on the “Calibration Worksheet for Autosampler Calibration” as ICcal,old.

4.4.27.    Calculate the new IC calibration constant using the formula:

ICcal,new   =    ICcal,old   x     TCadj,TC  x   TCave,IC
                                     TCave,TC           ICave,IC

4.4.28.    Scroll to select the first digit of the new IC calibration constant, and press ENTER to save this value.  If a mistake is made in entering the value, press CLEAR to start again.

4.4.29.    Scroll to the decimal point, and press ENTER.

4.4.30.    Repeat this process to enter and save the remaining values for the IC calibration constant, and press ENTER each time to store the value.  Five significant figures are used for the calibration constants.

4.4.31.    The display asks if the numbers are correct.  If the numbers are correct, press ENTER.

4.4.32.    Record the value of the new IC calibration constant as ICcal,new on the “Calibration Worksheet for Autosampler Calibration”.

4.5.             Verify the calibration by repeating the analysis of the standards

4.5.1.       Repeat analysis of calibration standards using the same protocol file.

4.5.2.       Use the same TC and IC standards that were analysed previously.

4.5.3.       Prepare a fresh blank flask.

4.5.4.       Rinse and fill the same vials, using new septa.

4.5.5.       Record the average TC for the TC check as TCave,chk,TC on the “Calibration Worksheet for Autosampler Calibration”.

4.5.6.       Record the average TC for the IC check as TCave,chk,IC on the “Calibration Worksheet for Autosampler Calibration”.

4.5.7.       Record the average IC for the IC check as ICave,chk,IC on the “Calibration Worksheet for Autosampler Calibration”.

4.6.             Calibration Acceptance Criteria

4.6.1.       The average TC value measured for the TC standard should be within ± 3% of the adjusted TC value of the TC standard, or the calibration must be repeated.

4.6.2.       The average TC value and average IC value measured for the IC standard should differ by no more than 3% of the value of the IC standard, or the calibration must be repeated.

5. System Suitability Procedure

5.1.             Preparation of 500 ppb Sucrose Standard Preparation

Materials and Equipment

Sucrose, Analytical reagent grade, 99+ % (Mol wt. 342.30 g/mol)

Para film

Milli-Q water

1L volumetric flask, Class A

500mL volumetric flask, Class A

10.0mL volumetric pipette, Class A

Procedure:

5.1.1.       Obtain required glassware and ensure it has been cleaned in the Laboratory dishwasher and thoroughly rinsed 5 times with Milli-Q Water.
Note: For Calibration solutions dedicated glassware must be used, therefore use only glassware identified for the standard being prepared.  Ensure all pipettes are cleaned and thoroughly rinsed with Milli-Q water.

5.1.2.       Record relevant Sucrose information in the “500 ppb Sucrose Standard Worksheet” (Form 615) for Sucrose preparation.

5.1.3.       Prepare nominal 25,000 ppb stock standard solution.

  1. Dry the sucrose at 105°C for 4 hours.  Let it cool in a desiccator.
  2. Accurately weigh approximately 0.059 ± 0.0001g sucrose for preparation of stock standard solution and record in “500 ppb Sucrose Standard Worksheet”.
  3. Transfer to 1L volumetric flask and make up to volume using Milli-Q water washing down weigh boat and flask to ensure 100% transfer.  Verify that water used is low TOC i.e. less than 100ppb and prepare a blank sample of this water.

5.1.4.       Calculate the concentration of the stock as follows:
conc. of stock (ppb C) = weight of sucrose (g) x carbon content x 106

5.1.5.       Prepare the dilute standard.

  1. Use standards as soon after preparation as possible.
  2. Using a 500mL volumetric flask, partially fill it with Milli-Q water.
  3. Using a 10mL volumetric pipette, pipette the stock solution into the partially filled 500mL volumetric flask, mix and make up to 500mL.

5.1.6.       Calculate the dilute standard concentration:
conc. of dilute standard (ppb C) = conc. of stock (ppb C)
                                                                         50

5.1.7.       Record the calculated concentration on line 8 of the “500 ppb Sucrose Standard Worksheet”.

6. Preparation of 500 ppb Benzoquinone standard

Materials and Equipment

1,4-Benzoquinone (Mol wt. 108.10g/mol)

Para film

Milli-Q water

Two x 1L volumetric flasks, Class A

10.0mL volumetric pipette, Class A

Procedure

6.1.             Obtain required glassware and ensure it has been cleaned in the Laboratory dishwasher and thoroughly rinsed 5 times with Milli-Q Water.
Note: For Calibration solutions dedicated glassware must be used therefore use only glassware identified for the standard being prepared.  Ensure all pipettes are cleaned and thoroughly rinsed with Milli-Q Water.

6.2.             Record the relevant Benzoquinone information in the “500 ppb Benzoquinone Standard Worksheet” (Form 615) for 500 ppb Benzoquinone preparation.

6.3.             Prepare nominal 50,000 ppb stock standard solution.

6.3.1.       Accurately Weigh out approximately 0.075 ± 0.0001g benzoquinone in the weigh boat, and record the gross weight in line 4 of the “500 ppb Benzoquinone Standard Worksheet”.

6.3.2.       Transfer to 1L volumetric flask and make up to volume using Milli-Q water, washing down the weigh boat and flask to ensure 100% transfer.

6.4.             Calculate the concentration of the stock as follows:
conc. of stock (ppb C) = weight of benzoquinone (g) x carbon content x 106

6.5.             Prepare the dilute standard.

6.5.1.       Use standards as soon after preparation as possible.

6.5.2.       Using a 1L volumetric flask, partially fill it with Milli-Q water.

6.5.3.       Using the 10mL volumetric pipette, pipette the stock solution into the partially filled 1L volumetric flask, mix and make up to 1L.

6.6.             Calculate the dilute standard concentration:
conc. of dilute standard (ppb C) = conc. of stock (ppb C)
                                                                        100

6.7.             Record the calculated concentration on line 8 of the “500 ppb Benzoquinone Standard Worksheet”.

7. System Suitability Analysis Procedure

Materials and Equipment

500 ppb Sucrose standard

500 ppb Benzoquinone standard

Model 820 TOC Analyser

Milli-Q water

40mL sample vials (cleaned), with caps and new septa.

Procedure

Configure the instrument in Autosampler sampling mode as in section 3 – Instrument set up for analysis.

Rinse the sample line prior to low level measurements by analysing a low TOC Milli-Q water sample 5 times or until readings are consistent i.e. within 20ppb and less than 100ppb.

The sampling schedule is as follows:

Sample Sample
No.
Acid Flow
Rate (
mL/min)
Oxidizer Flow
Rate (mL/min)
Number of
Replicates/Sample
Low TOC blank 1, 2 0.75 0.01 4
500 ppb sucrose 3, 4 0.75 0.01 4
500 ppb suitability 5, 6 0.75 0.01 4
Cleanup 7 1 1 1

7.1.             Create an Autosampler protocol file from the sampling schedule.

7.2.             Prepare and label the sample vials for the Autosampler.

7.3.             Run the protocol file from the Autosampler software.

7.4.             At the completion of the run, transfer the average measured TOC for the second sample of each solution to the appropriate line of the “Suitability Verification Worksheet” (Form 615):

7.5.             Calculate the response efficiency.

7.6.             Calculate the response efficiency (in %) using the formula below:

Response Efficiency

7.7.             Response efficiency values between 85% and 115% are acceptable.

8. Routine Analysis

Materials and Equipment

Samples to be analyzed

Powder-free gloves

Model 820 TOC Analyzer

Autosampler

40mL sample vials (cleaned) with caps and new septa.

All Necessary glassware (cleaned and thoroughly rinsed).

8.1.             Instrument Set-up for Analysis

As per Section 3.  Note: Always run a Water blank before commencing analysis to check that the instrument has been rinsed and primed of all air bubbles.  Check the waste stream from the analyzer for air bubbles, they should be successfully primed after 4 injections.

8.2.             Prepare Sample Analysis Protocol File using the Sievers Program

8.2.1.       Follow the same procedure outlined in Calibration Section 4.  Enter the relevant name of the samples to be analyzed, e.g. 10 ppm Glucose.

8.2.2.       Selection of Acid and Oxidizer Flowrates must be set accordingly when analyzing the sample types listed in the following table:

Sample Type/TOC concentration Recommended Acid Flow Rates
Deionised water 0.2 – 0.75 mL/min
0 – 50 ppm TOC 0.75 – 1.5 mL/min
50 – 100 ppm TOC ³ 1.5 mL/min
Purified Water/WFI 0.5 mL/min
TOC concentration Recommended Oxidiser Flow Rates
< 1 ppm 0.0 – 0.5 mL/min (NMT 1.0)
1 – 5 ppm 0.5 – 1.0 mL/min
5 – 10 ppm 1.0 – 2.0 mL/min
10 – 25 ppm 2.0 – 4.5 mL/min
25 – 50 ppm ³ 4.5 mL/min

8.2.3.       Acid flow rate is correct if the pH of the outlet water from the TOC analyser is less than 2.  This should be verified by pH paper or calibrated pH meter.

8.3.             Prepare a water blank

A blank vial should be taken for each water sample used to make up sample dilutions i.e. if two separate bulk volumes of water are taken to do dilutions at separate times then both should be collected as blanks.  This is not necessary for analysis of Purified Water samples.

8.4.             Fill the sample vials and load into the Autosampler

Prepare in the same manner described in Calibration section 6.  Fill each sample into two separate vials as a duplicate.

8.5.             Run the protocol file from the Sievers Program – As per Calibration section 7.

8.6.             Collect Result Print out and Calculate and Document Results

8.6.1.       To calculate actual TOC result, subtract the relevant average blank TOC reading from the average Sample TOC reading.  This does not apply to analysis of Purified Water samples.

9. Routine Maintenance

Item

Part

No.

Replacement

Schedule

Notes
60 mm filter element MRF 94401 Every 3 months or as required In-line filter applies only to on-line measurement.  The filter element replacement schedule depends on the level of particulates in the water being sampled.  A clogged filter may be detected by decreasing pressure on the sample inlet pressure gauge, or by a decrease in flow from the sample bypass waste line.  At a minimum, the filter status should be checked every 3 months on the same schedule as replacement of the oxidiser reagent reservoir.

Continued

15% Ammonium Persulfate Reagent reservoir APF 80020 Every 3 months Because of loss of activity of the oxidiser over time, the 3-month replacement schedule is independent of whether the instrument is used for measurements, or is idle.  The lifetime of the oxidizer reagent is tracked by the instrument with date/time information in non-volatile RAM, and Error 14 is reported when the lifetime has been exceeded.  Error 13 is reported when the amount of oxidizer available is less than 10 percent of the full reservoir value.
6M Phosphoric Acid Reagent reservoir APF 80010 as required Replacement schedule of the acid reservoir, sample pump tubing, and ultraviolet lamp depends on the total time the instrument is on and/or making measurements.  Lifetime of these items is tracked by the instrument with date/time information in non-volatile RAM, and specific errors are reported when the lifetime has been exceeded for any item.  Error 12 is reported when the amount of acid available is less than 10 percent of the full reservoir value.
Sample Pump Tubing assembly ATU 00644 Every 12 months Error 16 is reported when the age of the sample pump tubing has exceeded the planned life expectancy.
Ultraviolet Lamp assembly EMI 00800 Every 6 months Error 15 is reported when the age of the UV lamp has exceeded the planned life expectancy.
Refill DI Water reservoir n/a Every 2-12 weeks as required Small amounts of DI water can be lost from the DI reservoir over time.  The level of water in the DI reservoir should be periodically checked and the reservoir refilled if necessary.  The procedure for checking and filling the reservoir is detailed in the Operation and Service Manual.  The required inspection schedule depends on the mode of measurement.  For on-line use, check the reservoir every 3 months, on the same schedule as replacement of the oxidiser reagent reservoir.  For container sampling or Autosampler use, check the reservoir every 2 weeks.

10. Summary of Changes

Version # Revision History
MICLAB 115 New