SOP for Operation and Calibration of TOC Analyzer (TOC–VCPH SHIMADZU)


This document details the procedure for the Operation and Calibration of the TOC analyzerIt is the policy of XYZ Limited that the written procedure will be followed for the operation and calibration of the TOC (Total Organic Carbon) Analyser to ensure smooth operation and its use monitored to obtain consistent and reproducible results minimize downtime and meet the regulatory requirements.

This procedure is to be applied at the time of the Operation and Calibration of the TOC analyzer.

RESPONSIBILITY & ACCOUNTABILITY

Persons along with their responsibilities and accountabilities are given below:

Executive-Corporate Quality Assurance:- To prepare  SOP and follow the same

Trainee Analyst/ Jr. Analyst/ Analyst/ Sr. Analyst:- To follow the SOP accordingly

Manager  - Quality Control:- To ensure implementation of SOP.

5.0 Shimadzu TOC Calibration Procedure

5.1 GENERAL INSTRUCTIONS

5.1.1 The instrument should be located at the ambient temperature.  

5.1.2 Ensure the instrument and printer are connected to an uninterrupted power supply.(UPS)

5.1.3 Check the calibration status of an instrument before use.

5.1.4 Clean the instrument with a dry and non-shedding duster before and after use.

5.1.5 Report any discrepancy observed during the operation and calibration of the instrument to the Section Incharge or his representative for corrective and preventive action.

5.1.6 Section In-charge or his representative will report the same to the Manager – Quality Assurance and notify the defect to service engineer to rectify the defect.

5.1.7 Affix the ‘Out of Order’ label on the instrument.

>Environmental Health & Safety Procedure Manual

5.2 PRECAUTIONS

5.2.1 Use high-quality glass bottles for sample collection.

5.2.2 Wash the bottles with pure water.

5.2.3 Prepare 1 molar nitric acid and thoroughly wash bottles and caps.

5.2.4 Wash bottles with pure water 2 to 3 times, by filling them without air gap and emptying.

5.2.5 At the sample collection point, wash glassware with sample water 3 to 4 times.

5.2.6 Leave 2 to 3 liters of water and then collect the sample without any air gap in the container.

5.2.7 Close the cap and if possible seal it with parafilm.

5.2.8 Analyse the samples immediately after they have been brought to the laboratory.

5.3 OPERATION PROCEDURE

5.3.1 Ensure that the instrument is calibrated.

5.3.2 Open the zero air gas regulator before connecting the instrument.

5.3.3 Switch on the computer and TOC instrument.

5.3.4 Open the TOC-Control V software from the desktop

5.3.5 Double Click on the “sample table editor”

5.3.6 Enter the “user name” and “password”(Main User or User) then OK.

5.3.7 Select “ new ” from the “file menu” select “calibration” and press are Ok.

5.3.8 On page 1: press “next” and on page 2 select “Edit calibration points Manually” and select “div. standard solutions/Fixed dilution”. And press “next”.

5.3.9 On page 3 select analysis: NPOC, enter the “sample name” and “Id” Select “Multiple injections” and enter the <calibration file name>in the file Name and press “next”.

5.3.10 On page 4 select Units: ppb, No. of cal points: 2No. Injections 3/5,   No. of washes: 2, SD NMT: 1.0, C.V NMT: 5.0%, Acid ratio:  0.5%, sparge time: 30 seconds press “next”  

5.3.11 On page 5 press the “Add” button and enter the concentration: 500ppb and Press Ok.

5.3.12 Repeat the step5.2.11 and enter the concentration 0ppb and press “OK” Press “next

5.3.13 Press next until “finish”

5.3.14 Select “Connect” from “Instrument Menu”

5.3.15 Select the “Background Monitor” from the “Instrument menu”

5.3.16 Wait 20-30 min to get ready state (all conditions are green) like furnace Temp. Dehumidifier Temp, Baseline position, fluctuation, Noise.

5.3.17 Close the background monitor and select the “new row” in the sample table

5.3.18 Select the “calibration curve” form “insert menu”

5.3.19 Select the <calibration curve file name> and press “Open”

5.3.20 Press the “start” form “Instrument menu”

5.3.21 Enter the <filename> for data storage. Select Normal and put the Ist STD press start and so on.

5.4 PROCEDURE FOR SAMPLE ANALYSIS

5.4.1 Select the next row in the “sample table”

5.4.2 Select the “sample” from the “insert menu”

5.4.3 Select “calibration curve “ and enter the <sucrose calibration file name> on page1.

5.4.4 On page 2: enter the Default sample name and sample ID and press the next button.

On page: press the “next” button

5.4.5 Select units: ppb, No injections: 3/5, set the SD NMT: 1.0 & CV NMT: 5.0% No. of washes 2, select “multiple injections” and press the “next” button

5.4.6 Press the “next” button until go to “finish” and press, “start” from the “Instrument” menu.

5.4.7 For a printout of reports Select file menu then select print preview, select Table click OK then select Sample report then click OK.

5.4.8 Maintain the Logbook of TOC on XYZ/CQA/SOP-039/FR-01 as Logbook of TOC Analyser (Appendix I)

5.5 CALIBRATION BY POTASSIUM HYDROGEN PHTHALATE OR SUCROSE

5.5.1 Ensure that the instrument is clean and free from dust.

5.5.2 Operate the Instrument as per step 5.3. to 5.4.7

5.5.3 A calibration curve against known standards is generated. A 7 - point calibration curve can be generated.

5.5.4 Potassium Hydrogen Phthalate (KHP) is used as a calibration standard for TOC.

5.6 CALIBRATION BY POTASSIUM HYDROGEN PHTHALATE :

5.6.1 Identification of Potassium Hydrogen Phthalate

5.6.2 Preparation of Standards

5.6.3 Known standards will be prepared using KHP, For convenience 0.0 ppb, 250ppb, 500ppb,        750ppb, 1000ppb, 2000ppb, and 5000ppb standards are prepared.

5.6.4 Extreme precautions should be taken while preparing standards. Water required for the preparation of standards is to be collected at a time to avoid contamination. Use all 100-ml volumetric flasks.

5.6.5 Mother Solution: TOC calibration solution

5.6.6 Accurately measured 0.2125 g of KHP is dissolved in 100ml water to give 1000ppm    carbon concentration. This is a mother solution and can be stored for further dilutions.

10ppm solution: Take 1ml from 1000ppm solution and add in 100ml Purified water.

Zero ppb solution: Purified water or blank water itself is the Zero standard. Collect it in a                  100ml volumetric flask.

250ppb solution:  Take 2.5ml from 10ppm solution and add in 100ml Purified water.

500ppb solution:  Take  5ml  from 10ppm  solution and add in 100ml Purified water.

750ppb solution:  Take 7.5 ml from 10ppm solution and add in 100ml Purified water.

1000ppb solution:  Take 10 ml from 10ppm solution and add in 100ml Purified water.

2000ppb solution:  Take 20 ml from 10ppm solution and add in 100ml Purified water.

5000ppb solution:  Take 50 ml from 10ppm solution and add in 100ml Purified water.

5.6.7 Generate 8 point calibration curve using the above standards. By using the TOC Control  V software

Note: Calibration shall be done on the day of sample analysis.

SOP for Operation and Calibration of TOC Analyzer

5.7 CALIBRATION PROCEDURE IN SOFTWARE:

Step1: Open the TOC-Control V software from desktop

Step2: Click on the “sample table editor”

Step3: Enter the “user name” and “password”(Main User& User)

Step4: Select “ new ” form “file menu” select “calibration” and press Ok

Step 5: On page 1 press “next” and on page 2 select “Edit calibration points Manually” and select “div. standard solutions/Fixed dilution”. And press “next”.

Step6: On page 3 select analysis: TC, enter the “sample name” and “Id”

Step 7: Select “Multiple injections” enter the <calibration file name>in the file Name and Press “next”.

Step 8: On page 4 Select Units: ppb, No. of cal points: 7No. Injections 3/5,

No. of washes: 2, SD NMT: 1.0, C.V NMT: 5.0%, and press “next”        

 Step9: In page5 press add and enter the concentration: 5000ppb and press Ok

 Step10: Repeat the step9 and enter the concentrations up to 0ppb and press “next”

 Step11: press next until “finish”

 Step12: select “ new ” from the file menu select “sample run” and press Ok

Step13: select “Connect” from the “Instrument Menu”

Step14: Select the “Background Monitor” from the “instrument menu”

Step15: wait 20-30 minutes to get ready state (all conditions are green)

Setp16: close the background monitor and select the “new row” in the sample table

Setp17: select the “calibration curve” from the “insert menu”

Step18: Select the <calibration curve file name> and press “Open”

Step19: Press the “start” from the “Instrument menu”

Step 20:     Enter the <filename> for data storage. Select “Normal” Put the Ist STD (0ppb) press start and so on.

5.7.1 Record the calibration data on APL/CQA/SOP-039/FR-02 as  Calibration by KHP (Appendix II).

5.8 CALIBRATION  BY SUCROSE (Alternate Method)

5.8.1 Standards Preparation:

5.8.2 Keep Sucrose in the drier at 105  ºC for 2 to 3 hours.

5.8.3 Collect pure water required for Standard preparations.

5.8.4 Mother solution :

5.8.4.1 Accurately measure 11.9mg of Sucrose and dissolve in 100ml water, to get 50ppm-carbon concentration. Use this as the mother's solution.

5.8.4.2 Zero ppb: Use zero water as zero ppb standards.

5.8.4.3 250ppb

5.8.4.4 Take 0.5ml from 50ppm solution and add in 100ml purified water.

5.8.4.5 500 ppb:

5.8.4.6Take 1.0ml from 50ppm solution and add in 100ml purified water.

5.8.4.7 1000ppb

5.8.4.8Take 2.0ml from 50ppm solution and add in 100ml purified water.

5.8.4.9 Generate a Four-point calibration curve using the above standards. By using the TOC Control V software

5.8.4.10 Do the analysis in the NPOC method.

Note: Calibration shall be done on the day of sample analysis.

5.8.5 OPERATING PROCEDURE IN SOFTWARE:

Step1: Open the TOC-Control V software from desktop

Step2: Click on the “sample table editor”

Step3: Enter the “user name” and “password”(Main User or  User)

Step4: Select “ new ” form “file menu” select “calibration” and press Ok

Step 5: On page 1: press “next” and on page 2 select “Edit calibration points Manually” and select “div. standard solutions/Fixed dilution”. and press “next”.

Step 6: On page 3 select analysis: NOPC, enter the “sample name” and “Id” Select “Multiple injections” and enter the <calibration file name>in file Name and press “next”.

Step 8: On page 4 Select Units: ppb, No. of cal points: 2No. Injections 3/5,

            No. of washes: 2, SD NMT: 1.0, C.V NMT: 5.0%,

            Acid ratio:  0.5%, sparge time: 90 seconds press “next”        

Step 9: On page 5 press the “add” button enter the concentration: 500ppb and Press Ok.

Step10: Repeat the step9 and enter the concentration 0ppb and press “OK” Press “next”

Step11: press next until “finish”

Step12: select “ new ” form “file menu” select “sample run” and press Ok

Step13: select “Connect” from the “Instrument Menu”

Step14: Select the “Background Monitor” from the “instrument menu”

Step15: wait 20-30 minutes to get ready state (all conditions are green)

Setp16: close the background monitor and select the “new row” in the sample table

Setp17: select the “calibration curve” from the “insert menu”

Step18: Select the <calibration curve file name> and press “Open”

Step19: press the “start” from the “Instrument menu”

Step 20: enter the <filename> for data storage. Select Normal put the Ist STD press start and so on.

5.8.6 Record the observations on APL/CQA/SOP-039/FR-03 as Calibration by Sucrose (Appendix III)

5.9 SYSTEM SUITABILITY TEST (WEEKLY):

5.9.1 System Suitability is performed below

5.9.2 1,4 Benzoquinone are used as standards

5.9.3 Initially injecting pure water performs Peak Stabilization.

5.9.4 PREPARATION of 1,4 BENZOQUINONE SOLUTION:

5.9.4.1 Dissolve 7.5 mg of 1,4 Benzoquinone in 100ml water, to get 50ppm carbon concentration. Use this as the mother's solution.

5.9.4.2 Zero ppb: Use zero water as zero ppb standards.

5.9.4.3 500 ppb: Take 1.0ml from 50ppm solution and add in 100ml zero water And then analyze 500 ppb 1,4 Benzoquinone solution as a Sample. By using the sucrose calibration curve.

5.9.4.4 Analyse the solution in the NPOC method.

5.10 PROCEDURE FOR SAMPLE Run (1,4 BENZOQUINONE):

Step 1: select the 2nd row in the “sample table”

Step 2: select the “sample” from the “insert menu”

Step 3: Select “calibration curve “ and enter the <sucrose calibration file name> on page 1.

Step 4: On page 2: enter the Default sample name and sample ID and press the next button.

Step 5: On page 3: press the “next” button

Step6: select units: ppb, no injections: 3/5,set the SD NMT: 1.0 & CV NMT: 5.0% 

No. of washes 2, select “multiple injections” and press the “next” button.

Step 7: press the “next” button until going to “finish” and press “start” from the “Instrument” menu.

5.10.1 RESPONSE EFFICIENCY:

The response efficiency (% recovery) can be calculated by the following formula

        %R = 100 [ ( Rss - Rw )  / ( Rs - Rw )

Where Rss = Mean area counts of 1,4 Benzoquinone solution

Rs   = Mean area counts of sucrose 

Rw  = Mean area counts of pure water

5.10.2  Criterion Judgment:   

The system is said to be passing the test if the % recovery is between 85% to 115%.

5.10.3   SAMPLE ANALYSIS:

5.10.3.1Procedure for a sample run:

Step 1: select the 3rd row in the “sample table”

Step 2: select the “sample” from the “insert menu”

Step 3: Select “calibration curve “ and enter the <sucrose calibration file name>in page 1.

Step 4: In page2: enter the Default sample name and sample ID and press the next button.

Step 5: In page3: press the “next” button.

Step6: select units: ppb, No injections: 3/5,set the SD NMT: 1.0 & CV NMT: 5.0%

No. of washes 2, select “multiple injections” and press the “next” button.

Step7: press the “next” button until going to “finish” and press, “start” from the “Instrument” menu

5.10.4  Analysis:

5.10.4.1 Analyse the samples using the latest Sucrose calibration curve and observe the results.

5.10.4.2 Record the observation on XYZ/CQASOP-039/FR-04 as System Suitability by 1,4 Benzoquinone Appendix IV.   

5.10.4.3 Calibration by KHP or Sucrose and weekly system suitability shall be considered for the half-yearly calibration.

5.10.4.4 Record observations  on XYZ/CQA/SOP-039/FR-05 as Calibration by KHP or Sucrose, 1,4 Benzoquinone Appendix V

5.10.4.5Summarize the data on XYZ/CQA/SOP-039/FR-06  as Summary sheet   Appendix VI           

5.11 GENERATION OF INSTRUMENT CALIBRATION NUMBER

Generate the Instrument calibration number on the calibration datasheet as INSCALXXYYZZZ

Where INS denotes  Instrument, CAL denotes Calibration

XX denotes the year, YY denotes the Month and ZZZ denotes the sequence number

5.12  ABBREVIATIONS

INSCAL:  Instrument Calibration Number.

NPOC:   Non Purgable Organic Carbon 

KHP:   Potassium hydrogen phthalate

>SOP For Annual Product Review 

Note:- Download All  Appendix(I, II, III, etc.) 

>SOP For Operation and Calibration of FTIR

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