1.0 PURPOSE
To lay down a procedure for Operation, Calibration and System Suitability of Total organic carbon (TOC) Analyzer.2.0 SCOPE
This Procedure is applicable to TOC Analyzer in the quality control department.3.0 RESPONSIBILITY
Microbiologist4.0 ACCOUNTABILITY
Head of Department5.0 PROCEDURE
5.1 Checks before starting of equipment
5.1.1 Use oxygen with a minimum purity of 99.995% & It should be free from CO2 content.5.1.2 Check & ensure that the oxygen cylinder is opened & the output pressure is between 6.0-8.0 bars.
5.1.3 Also check the pressure on the oxygen purification system, It should be between 5.0-6.0 bars (Output which is going to the instrument)
5.1.4 Use high purity water (Reagent water), having TOC level less than 100 ppb.
5.1.5 Stabilized Power supply of 230 V, 50 hz.
5.1.6 In NPOC Method fill the Phosphoric acid bottle with high purity water.
5.1.7 In NPOC Method Add 1.0 ml of 2 N Hydrochloric acid in each of 100.0 ml sample.
5.1.8 Use 5-10 liter bottle for drain, the drain water should flow freely.
5.1.9 Note: If TOC analyzer is not in working condition then perform the oxidizable test.
5.2 Glassware
5.2.1 Use dedicated glassware for the preparation of standard & Sample.5.2.2 Clean the sample bottle with approximately 10 % nitric acid and rinse with high purity water five times and dry the bottles in the oven and close the cap.
5.2.3 While collecting the sample completely fill the bottle by sample and cap the bottle.
5.3 Operation
5.3.1 Open the valve of oxygen gas cylinder & gas supply pressure reducer.5.3.2 Switch on the main switch of TOC Analyzer present on the right top backside of Analyzer. Wait for 5 V, 24 V & LOCKIN LED to glow.
5.3.3 Switch on the computer.
5.3.4 Switch on the Sampler while using it.
5.3.5 Double-click on Multiwin icon, log on by giving the login name and Password.
5.3.6 Initialize the system by click on yes.
5.3.7 During the warm-up period the system will be stabilized for Temperature, Gas flow and NDIR values. Observe these values by on the systems.
Non-Dispersible Infra Red - OK
Gas flow - OK
Temperature - OK
5.3.8 If the analyzer is not ready for measuring after 45 minutes (one or more components are still shown red in the system window) check the tube connections and search for faults like gas leakages in the system etc.
5.4 Measurement with Manual Sampling
5.4.1 Select manual sampling in the system window by clicking on the manual button.5.4.2 Click on the Method – Load, mark an existing method in the Load Method database window and confirm the selection by clicking on the OK button.
5.4.3 Open the menu, Measurement click on start measurement, enter the sample ID in the Measurement start window and click on the Start button.
5.4.4 Start the measurement by clicking on the Start F2 button.
5.4.5 At the end of analysis take the printout.
5.5 Measurement with Sampler
5.5.1 Select sampling with a sampler in the system state window by clicking on the sampler button.5.5.2 Keep the TOC sample in the sample rack.
5.5.3 Click on the Method – Load, mark an existing method in the load method database window and confirm the selection by clicking on the OK button.
5.5.4 Open the menu item Measurement click on start measurement, give the name of analysis table and click on the start button, or select an existing analysis table by clicking on the edit button.
5.5.5 Click on, all sample with the current method then click OK.
5.5.6 Start the measurement by clicking on the start F2 button.
5.5.7 Enter the sample ID in rack table than click on Activation, sample ready, then click OK.
5.5.8 Start the measurement by clicking on the start F2 button in the Measurement window.
5.5.9 At the end of analysis take the printout.
5.6 Method Creation
5.6.1 Click on the method – Select New-Give file Name -Select the method of analysis NPOC- Select replicates-Min 2 Max 3 and Select Rinse Cycle 2 1 1
5.6.2 Click on Process Parameter – Sample volume 2000 – Rinse Volume-
2000 Purge time 1- 60 or 180 sec –Purge time 2- 10 sec – Max integration time
240 or 360 sec.Threshold 1 -0.20 –Threshold 2 - 0.20. Save the method.
5.6.3 Follow the instructions of Software i.e. Adopt calibration data of Previous method Click on NO. Adopt newly created method as current method Click on YES.
5.7 Calibration
5.7.1 Use reagent water as a blank solution having TOC level shall be less than 100 ppb.5.7.2 Preparation of 500 ppb Sucrose solution:
5.7.2.1 Dry Sucrose at 105°C for 1 to 2 hours. Accurately weigh and transfer 29.75 mg of previously dried sucrose to a 100 ml volumetric flask (Solution A) and make up the volume with high purity reagent water. Dilute 1.0 ml of the solution A with high purity reagent water to 250 ml (500 ppb carbon), Dilute 0.5 ml of the solution A with high purity reagent water to 250 ml (250 ppb carbon) and Dilute 1.5 ml of the solution A with high purity reagent water to 250 ml (750 ppb carbon)
5.7.2.2 In Calibration window select – Calibration with constant volume – No of samples – 1 – Analytical Parameter – NPOC – constant sample volume 2000 microliter – preparation blank – Measure – feed the concentration in NPOC table – 0.500 mg/l – Click on measurement & follow the software instruction.
5.7.2.3 At the end of calibration Click on LINK WITH THE METHOD – Accept Values.
Now the calibration values are included in the method.
5.7.3 Calibration Frequency – Single Point calibration shall be carried out within a week.
Acceptance criteria : Regression coefficient 0.4 to 0.8
Four point calibration - Once in three months.
Acceptance criteria: Correlation coefficient greater or equal to 0.999
5.8 System Suitability Test
5.8.1 Use reagent water as a blank solution having TOC level shall be less than 100 ppb.5.8.2 Preparation of 500 ppb para-benzoquinone solution: Accurately weigh and transfer 18.75 mg of para-benzoquinone into 100 ml of volumetric flask. Make up the volume up to mark with reagent water (Solution B) Dilute 1.0 ml of solution to 250 ml with reagent water to obtain a concentration of 0.75 mg/ liter. (500 ppb carbon)
5.8.3 Click on SST – Click on F2-Follow the software instructions – At the end of SST, you will get the SST report – Print.
5.8.4 The response efficiency is calculated by the formula
R = Rss- Rw /Rs- Rw
Where, Rss - Mean area count of para-benzoquinone
Rs - Mean area count of Sucrose
Rw - Mean area count of reagent water
Acceptance Criteria: Between 0.85 to 1.15
System suitability test frequency: Once in a week
5.9 Acceptance criteria for Standard Deviation
5.9.1 Standard deviation for individual sample should not be more than 115.5.9.2 If it exceeds the limit then test shall be repeated.
6.0 ABBREVIATIONS
6.1 SOP - Standard Operating Procedure6.2 NPOC - Non-Purgeable Organic carbon
6.3 SST - System Suitability Test
6.4 TOC - Total Organic Carbon
6.5 % - Percent
6.6 Ppb - Parts per billion
6.7 N - Normality
6.8 NDIR - Non-Dispersible infrared
6.9 V - Volt
6.10 hz - Hertz
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