SOP For Operation and Calibration of Total Organic Carbon (TOC)

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  1. OBJECTIVE: 

The purpose of this SOP is to lay down a procedure for Handling, Operation, Maintenance and Calibration of Total Organic Carbon (TOC) analyser in Quality Control Department.

  1. SCOPE:

This SOP is applicable to TOC analyser in Quality Control Department at manufacturing facility.    

  1. RESPONSIBILITY:  
  1. Officer/ Executive shall be responsible for the effective handling, operation, Calibration and maintenance of TOC analyser.
  2. Head of Quality Control Department shall be responsible for the effective implementation of the procedure.
  3. PROCEDURE:
  1. PRELIMINARY CHECK : 
  2. Check that the instrument and surroundings are clean. If not clean, then clean with soft cloth duster. 
  3. Before starting analysis flush the carrier gas line with carrier gas (Compressed air or Nitrogen)
  4. Ensure the molecular sieve and CO2 absorber is in well condition.
  5. Ensure sufficient samples in bottle.
  6. Ensure that the door of system is closed.
  7. Ensure sample bottles are kept properly in sealed condition and volume inside the bottle is proper at specified levels.
  8. Check daily the levels of dilution water, 2 M Hydrochloric acid, drain vessel and humidifier water.
  9. Ensure proper pressure and flow of carrier gas i.e. 150 ml/minute.
  10. BASIC OPERATION:
  1. Switch on the Air cylinder, Ensure cylinder pressure is at 4 Kg/cm2.
  2. Press the power button on the bottom right of the front panel of the instrument.
  3. Conform that the pressure of the carrier gas (Compressed air or Nitrogen) is 200 kPa and Flow rate is 150 ml/min.
  4. Switch ON the computer and TOC Instrument.
  5. Double click on TOC-Control V icon on desktop.
  6. Double click on “Sample Table Editor”. Window for Login ID and password will open.
  7. Enter login ID and password and click on “OK” button.
  8. Select “New” from the file menu or Click “New” on tool bar.
  9. Screen will display “New” dialog box showing:

-Sample run

-Calibration curve

-Method

-Control sample template

  1. Select sample run and click on “OK” button.
  2. General information Dialog box will appear on the screen. Press “OK” button.
  3. “Save As” dialog box will appear on the screen.
  4. Select particular folder and Enter file name. Press “Save” button in the dialog box.
  5. Screen will show TOC Control V sample table for that particular file name.
  6. Go to “Instrument” key of main window and press “Connect” button.
  7. Click on “User settings on PC” and wait till initialization menu will disappear.
  8. Go to “Instrument key” of main window and select “Background monitor”.
  9. Wait till system stabilizes and light given on the front panel of the instrument becomes green.
  10. Ensure that instrument shows carrier gas flow rate of 150-ml/min and gas pressure gauge shows pressure of carrier gas 200 kPa.
  11. If the flow rate and pressure of carrier gas is not so, then adjust the flow rate and Pressure with the help of knobs of the instrument.
  12. Wait for 15 to 20 minutes to get the instrument ready.
  13. Go to “Back ground monitor” from the instrument menu to see back ground conditions like Furnace temperature, Dehumidifier temperature, Base line position, Fluctuation, Noise.
  14. CREATING THE CALIBRATION FILE 
  1. For creating new calibration file Select “New” from the file menu or Click “New” on tool bar.
  2. “New” dialog box will appear on the screen.
  3. Double click on “Calibration curve icon”.
  4. “Calibration curve wizard (Page 1)” dialog box will appear on the screen.
  5. Press “Next”.
  6. “Calibration curve wizard (Page 2)” dialog box showing calibration curve type will appear on the screen.
  7. Press “Next” button in the dialog box.
  8. “Calibration curve wizard (Page 3)” dialog box showing Analysis information will appear on the screen.
  9. In this dialog box select Analysis (TC for calibration with Potassium hydrogen phthalate and NPOC for system suitability with Sucrose and 1,4-Benzoquinone), enter default sample name, default sample ID, Multiple injections.
  10. Select folder and give the Calibration file name rowsing and click “OK”. Press “Next” button on page 3.
  11. “Calibration curve wizard (Page 4)” dialog box showing calibration measurement      Parameters will appear on the screen.
  12. Select calibration measurement parameters as follows:

– Units-ppb

– No. of injections- 3 to 5

– No. of washes-0 to 10

– SD max-0.5000%

-CV max-3.0%

– Acid Addition-0.5ml

  1. Press “Next” button in page 3 dialog box.
  2. “Calibration curve wizard (Page 5)” dialog box will appear on the screen.
  3. Edit Calibration point parameters dialog box will appear on screen. Press “Add”  button in this page and enter the highest calibration point first.
  4. Click “Add” button again and enter the calibration points from maximum to Minimum and click “Next” button.
  5. “Calibration curve wizard (Page 6)” dialog box will appear on the screen.
  6. Press “Next” button.
  7. “Calibration curve wizard (Page 7)” dialog box will appear on the screen. Press “Next button”.
  8. “Calibration curve wizard (Page 8)” dialog box will appear on the screen. Then  click the “finish button”.
  9. INSERTING THE CALIBRATION FILE IN THE SAMPLE TABLE
  1. Place the cursor on the sample table and click on “Insert” menu of the main window for selecting the calibration curve.
  2. Calibration curve file window will appear on the screen. Select the calibration file that was created earlier and click on “Open” button.
  3. Click on “Start button” from tool bar.
  4. For seeking peeks and areas, select sample window. After analysis it will give results.
  5. SAMPLE MEASUREMENT
  1. Click on “Insert” menu of the main window and select “Sample” button.
  2. “Sample wizard (Page 1)” dialog box will appear on the screen.
  3. Select calibration curve button in this page. Browse calibration curve by selecting browse button. 
  4. Calibration curve files list will open. Select the appropriate calibration file which is having extension of date and time with file name.
  5. Click on “Ok” button. 
  6. Press “Next” button in Ist page.
  7. “Sample wizard (Page 2)” dialog box will appear on the screen.
  8. Select analysis as NPOC, Give sample name and sample ID of the sample.
  9. Press “Next” button in this page.
  10. “Sample wizard (Page 3)” dialog box will appear on the screen.
  11. Press “Next” button in this page.
  12. “Sample wizard (Page 4)” dialog box will appear on the screen.
  13. Ensure that all the injection parameters are Ok.
  14. Press “Next” button in this page.
  15. “Sample wizard (Page 5)” dialog box will appear on the screen. Press “Next” button.
  16. “Sample wizard (Page 6)” dialog box will appear on the screen. Press “Next” button.
  17. “Sample wizard (Page 7)” dialog box will appear on the screen. Press “Finish” button.
  18. Any No. of samples can be inserted like this repeating steps 5.4.1 to 5.4.17.
  19. Click on “Start button” from tool bar.
  20. For seeking peeks and areas, select sample window. After analysis it will give results.
  21. SHUT DOWN PROCEDURE OF THE INSTRUMENT
  1. Go to “Instrument” menu and select “Standby” button on tool bar after completion of analysis.
  2. Instrument will turn off automatically after 30 minutes.
  3. Turn off the computer by closing instrument software.
  4. CALIBRATION 
  1. Calibration of instrument shall be done using reference standard of potassium hydrogen phthalate (KHP).
  2. Five point calibration curve is generated by using different concentrations of potassium hydrogen phthalate.
  3. Weigh accurately 0.2125g of KHP (equivalent to 100mg of carbon in KHP) and dissolve in 100ml of water. It will give 1000ppm carbon concentration (Mother Solution).
  4. Mother solution can be stored for further dilutions.
  5. Take 1ml from 1000ppm solution and dilute to 100ml to prepare 10ppm solution.
  6. Take blank water in 100ml volumetric flask. Blank water itself is a zero ppb solution.
  7. Take 2.5ml from 10ppm solution and dilute to 100ml to prepare 250ppb solution.
  8. Take 5ml from 10ppm solution to prepare 500ppb solution.
  9. Take 7.5ml from 10ppm solution to prepare 750ppb solution. 
  10. Take 10ml from 10ppm solution to prepare 1000ppb solution.
  11. Generate a five point calibration curve using zero ppb, 250ppb, 500ppb, 750ppb, 1000ppb solution.
  12. Observe the area counts, Mean area, S.D area, C.V area for each solution and Record in Annexure- I.

ACCEPTANCE CRITERIA

For each solution:     

-S.D Area- NMT 0.5

-C.V Area (RSD)- NMT 3.0%

-For Linearity- Correlation coefficient NLT 0.98.

*Either S.D Area or C.V Area limits will be accepted.

  1. FREQUENCY: Quarterly
  2. SYSTEM SUITABILITY TEST 
  3. USP reference standards Sucrose and 1,4-Benzoquinone are used for performing System suitability test.
  4. PREPERATION OF SUCROSE SOLUTION
  1. Keep Sucrose (reference standard) in oven at 105°C for 2 to 3 hours.
  2. Weigh accurately 23.5mg of sucrose and dissolve in 100ml to get 100ppm carbon Concentration (Mother solution).
  3. Mother solution can be stored for further dilutions for a period of a month.
  4. Use blank water for zero ppb standard solution.
  5. Dilute 0.5ml of mother solution to 100ml of water to prepare 500ppb carbon concentration.
  6. Generate two-point calibration curve using zero ppb and 500ppb solution.
  7. Observe the area counts, Mean area, S.D area, C.V area for each solution and note down in Annexure- II.

*ACCEPTANCE CRITERIA

For each solution:     

-S.D Area- NMT 0.5

-C.V Area (RSD)- NMT 3.0%

*Either S.D Area or C.V Area limits will be accepted.

  1. PREPERATION OF 1,4-BENZOQUINONE SOLUTION
  1. Weigh accurately 15.1mg of 1,4-Benzoquinone (reference standard) and dissolve in 100ml to get 100ppm carbon Concentration (Mother solution).
  2. Dilute 0.5ml of mother solution to 100ml with water to get 500ppb carbon concentration of 1,4-Benzoquinone.
  3. Analyze 500ppb solution as a sample in NPOC method.
  4. Observe the area counts, Mean area, S.D area, C.V area for each solution and Record in Annexure- II.

*ACCEPTANCE CRITERIA

For each solution:     

-S.D Area- NMT 0.5

-C.V Area (RSD)- NMT 3.0%

*Either S.D Area or C.V Area limits will be accepted.

  1. System suitability shall be performed daily.
  2. TRAINING :

Trainer:   Head Quality Control

Trainees: Quality Control Chemist / Section Heads

  1. DISTRIBUTION: 

Controlled Copy No.1 :  Head of Department – Quality Assurance 

Controlled Copy No.2 :  Head of Department – Quality Control

Original Copy :  Head – Quality Assurance 

  1. ANNEXURES : 

Nil

  1. REFERENCES :

Nil

  1. REVISION HISTORY : 
Sr. No.Revision No.Change Control NumberDetails of RevisionReasons(s) for Revision
100———–New SOPNew SOP





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