| SOP for Operation of TOC Analyzer ( Make Shimadzu) |
1.0 OBJECTIVE 1.1 To lay down the Procedure for Operation of TOC Analyzer ( Make Shimadzu). 2.0 SCOPE 2.1 This Procedure is applicable to Operation of TOC Analyzer in Quality Control department. 3.0 RESPONSIBILITY 3.1 Executive – Quality Control 4.0 ACCOUNTABILITY 4.1 Manager – Quality Control 5.0 PROCEDURE 5.1 SWITCHING ON THE INSTRUMENT 5.1.1 All glass wares should be thoroughly washed with nitric acid, flushed with tap water, rinsed 3 to 4 times with purified water and finally with Milli-Q-water. 5.1.2 Zero air supply from the Gas cylinder shall be opened such that line pressure on the cylinder is shown 4kg/cm2. 5.1.3 Check and ensure that the carrier gas line has been connected. 5.1.4 A high purity zero air shall be used as carrier gas (Total impurities<2ppm). 5.1.5 Switch on the Computer & TOC Instrument. 5.1.6 Double click Double Click on TOC-Control V Icon on desktop. 5.1.7 Double click on “Sample Table Editor”. Log in ID & Password Window will open. 5.1.8 Now Enter Log in Id & Password then click OK. 5.1.9 Select “New” from the File Menu or Clicking the “New” on tool bar. 5.1.10 Select the Appropriate “System”) and click OK. 5.1.11 Give the file name for opening the Sample Table. 5.1.12 Now click on “Connect” button on the Tool Bar Or from the Instrument Menu Select Connect”. 5.1.13 Now Instrument will start Initializing. Initialization Window will disappear after Auto Initializing. 5.1.14 Now Pressure Gauge should show 200 Kpa and flow meter should be 150 ml/min. 5.1.15 Wait for 15 to 20 min. for getting instrument Ready condition.(Go to back Ground monitor to see back ground conditions like Furnace Temp, Dehumidifier Temp, Base line Position, Fluctuation, Noise, from the Instrument Menu.) 5.2 CREATING CALIBRATION FILE 5.2.1 From the Sample Table Window click on File Menu select “New”. The New dialog box is displayed. Double Click on” Calibration Curve Icon”. 5.2.2 Calibration curve wizard page 1 will be displayed. In this page 1 select the System and click on “next”. 5.2.3 In the page 2 click on “Next”. 5.2.4 In the page 3 Select Analysis as NPOC, and enter the Default Sample Name & sample ID. Also select the “Multiple Injections” .Give the Calibration File Name by Browsing and click OK. Click on “Next” on page 3. 5.2.5 In the page 4 Select the measurement parameters and click “Next”. 5.2.6 In the Page 5 Calibration Points list is displayed. In this page click on Add and give the highest cal. point first. And give the cal points from max to min by clicking “Add”. And then Click “Next”. 5.2.7 In the page 6 Click on “Finish”. 5.2.8 Calibration File was created and now we have to Insert It in the Sample Table. 5.3 INSERTING THE CALIBRATION FILE IN THE SAMPLE TABLE 5.3.1 By placing cursor on the Sample Table, Click on Insert Menu and Select Calibration Curve. 5.3.2 Calibration Curve File Window will be displayed, Select the Created File Name and click on “Open” button. 5.3.3 In the sample table row calibration standard will be inserted. 5.3.4 Now click on “START” button on the Tool Bar. Another windows will be displayed on monitor, click on Start. 5.3.5 Now Instrument will analyze the Standards, After completion of each standard a window will be displayed click on “Next” each time. 5.4 SAMPLE MEASUREMENT 5.4.1 From sample table window Click on Insert Menu. 5.4.2 Select sample. 5.4.3 Sample Wizard Page 1 will open, In this page Select calibration curve button. Now browse calibration curves by selecting browse button. Calibration Curve Files list Window will open, In this cal list select the appropriate calibration file which is having extension of Date & Time with file name, and then click on OK. (Zero Shift should be selected before selecting calibration file for sample analysis). 5.4.4 Now Click on “Next” in the 1st Page. 5.4.5 In the Sample Wizard Page 2, Select Analysis as NPOC, And give the Sample Name & sample ID of the sample. 5.4.6 Now Click on “Next” in the 2nd Page. 5.4.7 In the Sample wizard Page 3 click on “Next”. 5.4.8 In the Sample Wizard Page 4 see all the Injection parameters are OK, If not select them and click “Next”. 5.4.9 Now Click on “finish” in the 5th Page. 5.4.10 We can insert any No. of samples like this (From Step 1 to Step 11). 5.4.11 Now select the “Start” from the Tool Bar Or from the Instrument Menu. another window will open click on “Start”. Now Instrument will start Analyzing the samples. To see the Peaks and concentrations select “Sample Window” on the Tool Bar or from View Menu on monitor. 5.4.12 After completion of Analysis it will display on monitor the Windows of “Repeat, after all Next, Stop”. Select next for measuring next sample. 5.5 2 – POINT CALIBRATION 5.5.1 First we have to calibrate the instrument with zero water (0ppb) and Sucrose (500ppb) as mentioned in above ( Creating the calibration file and inserting the calibration file in the sample table.) 5.5.2 From the sample table window click on file menu select “New”. The new dialog box is displayed. Double click on “ on calibration curve icon” on monitor. 5.5.3 Calibration curve wizard page 1 will be displayed. In the page 1 select the system and click on “next”. 5.5.4 In the page 2 click on “Next”. 5.5.5 In the page 3 select analysis as NPOC, and give the sample name as sucrose + blank and sample ID. Also give the calibration file name. 5.5.6 Click on “Next” on page. 5.5.7 In the page 4 select the calibration parameters and then click on next. 5.5.8 In the page 5 calibration points list is displayed. In the page click on add and give the highest calibration points first and give the cal points from max to min by clicking “Add”. And then Click “Next”. 5.5.9 In Page 6 click on “Finish”. 5.5.10 Now Insert the calibration file on the sample table. 5.6 For System Suitability Test 5.6.1 After completing the calibration, select “New” in the Tool Bar Or from the File Menu. Then Double Click on “Control Sample Templates”. 5.6.2 Control Sample Page 1 will be displayed, in this page select the System and click on “Next”. 5.6.3 In Page 2 select the “System Suitability Test for USP/EP” also give the file name for this control sample template, and then click on “Next”. 5.6.4 In page 3 Select the “Calibration Curve” and Browse for the calibration curve. Select the cal curve and click on “open”. Click on “Next” in page 3. 5.6.5 In page 4 select the Analysis as NPOC, give sample Name and sample ID as 1,4 Benzoquinone. Then Click on: Next”. 5.6.6 In Page 5 Set the Injection Parameters, and select Multiple Injection. After that click on “Next”. 5.6.7 In Page 6 click on “Next”. 5.6.8 In Page 7 Click on “Finish”. 5.6.9 Now we have to insert the “Control Sample” in the sample table row. 5.6.10 On the Sample Table place the cursor in the row where the control sample will be inserted. 5.6.11 From the Insert Menu select Control and the file name dialog box will be displayed, select the file name and click on open. 5.6.12 Now control sample will be inserted in the sample table row. 5.6.13 Now Click on “START” after inserting sample tube in to 1,4 Benzoquinone Standard, from the Tool Bar or From the Instrument Menu. 5.6.14 Window will be displayed click on “Start”. 5.6.15 Instrument will analyze sample and will give result automatically (Instrument will calculate the % system suitability). System is suitable if the response efficiency is not less than 85% and not more than 115%. Calculate Response efficiency : 100 [ ( rss – rw)/ ( rs – rw)] rw- Millipore water 000ppb, rs- Sucrose Solution 500ppb, rss- 1,4 Benzoquinone 500ppb 5.6.16 Frequency- Weekly ± 1 Day 5.7 4 – POINT CALIBRATION 5.7.1 After completing the System suitability test, select “New” in the Tool Bar Or from the File Menu.Then Double Click on “Calibration curve”. 5.7.2 Calibration curve Wizard (Page 1) will be displayed, in this page select the System and click on “Next”. 5.7.3 In Page 2 select the “use dilution from the standard solution”. click on “Next”. 5.7.4 In page 3 select the Analysis as NPOC, give sample Name and sample ID as Potassium Hydrogen Phathalate (KHP) and ok the Zero shift.Also give the file name as 4-Point calibration and Then Click on Next”. 5.7.5 In Page 4 Set all calibration Parameters. After that click on “Next”. 5.7.6 In the Page 5 Calibration Points list is displayed. In this page click on Add and give the highest calibration point first. And give the calibration points from max to min by clicking “Add”. And then Click “Next”. 5.7.7 In Page 6 Click on “Finish”. 5.7.8 Now we have to insert the “4-Point calibration curve” in the sample table row. 5.7.9 On the Sample Table place the cursor in the row where the calibration curve will be inserted. 5.7.10 From the Insert Menu select Calibration curve and the file name dialog box will be displayed, select the file name and click on open. 5.7.11 Now select the “Start” from the Tool Bar Or from the Instrument Menu. Another window will open click on “Start”. Now Instrument will Start Analyzing the calibration curve. To see the Peaks and concentrations Select “Sample Window” on the Tool Bar or from View Menu. 5.7.12 Frequency- Monthly ± 3 Days 5.8 PREPRATION OF STANDARD SOLUTION 5.8.1 Sucrose 500 ppb:- Weigh accurately about 119 mg of sucrose and dissolve and diluted it to 100 reagent water. Dilute 10ml of the solution to 100 ml (50ppm). Dilute 1ml of the solution to 100 ml (500ppb). 5.8.2 1,4-Benzoquinone (500 ppb):- Weigh accurately 75 mg of 1,4-Benzoquinone dissolve it in 100 ml reagent water. Dilute 10ml of the solution to 100 ml (50ppm). Dilute 1ml of the solution to 100 ml (500ppb). 5.8.3 Potassium Hydrogen phthalate (KHP10000 ppb):- Weigh accurately 212.5 mg KHP and dissolve it in 100 ml reagent water (1000 ppm). Dilute 1 ml of this solution to 100 ml (10 ppm or 10000ppb) 5.9 SHUT DOWN THE INSTRUMENT PROCEDURE 5.9.1 After completing the Analysis, to shut down the instrument, Select “Stand By” by selecting Instrument Menu and by clicking “Stand By” Or By clicking “Stand By” on the tool bar it self. Stand By window will be displayed, select “Shut Down Instrument” and then Click on “Stand By” (Instrument will Turn Off automatically after 30 min.). Now we can turn off the Computer after analysis. 6.0 ANNEXURES 6.1 Annexure-I – Operation log book for TOC Analyzer 6.2 Annexure-II – Calibration of TOC Analyzer. 6.3 Annexure-III – System Suitability Test of TOC Analyzer 7.0 ABBREVIATIONS 7.1 SOP – Standard Operating Procedure. 7.2 cGMP – Current Good Manufacturing Practices. 7.3 GLP – Good Laboratory Practice. 7.4 PPB – Part Per Billion 7.5 PPM – Part Per Million |