SOP Title: Operation, Cleaning and Calibration of Automatic Polarimeter
- Objective:
To lay down the procedure for Operation, Cleaning and Calibration of Automatic Polarimeter.
- Scope:
This SOP is applicable for Operation, Cleaning and Calibration of Automatic Polarimeter located in Quality Control Laboratory.
- Responsibility:
- Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Polarimeter as per this SOP.
- Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
- Quality Assurance Department: To review and approve the SOP and Annexure.
- Accountability:
Head Quality Control Department, Head Quality Assurance Department.
- Procedure :
| 5.1 | Safety Precautions/Instructions: | |
| 5.1.1 | Ensure all the electrical connections are properly earthed. Ensure the power plug of the automatic Polarimeter is fixed in the socket properly. | |
| 5.1.2 | Wear personal protective equipments such as safety glasses, hand gloves during operation of instrument. | |
| 5.1.3 | Ensure that the ON/OFF switch is working properly by switching “ON” the Polarimeter. | |
| 5.1.4 | Clean the Automatic Polarimeter with dry lint free duster. | |
| 5.1.5 | Do not move the automatic Polarimeter during cleaning | |
| 5.1.6 | Do not attempt to do any repairs unless trained. | |
| 5.1.7 | After switch ON instrument wait for 10 minute to allow stable temperature. | |
| 5.1.8 | Ensure sample cell foot is clean. | |
| 5.1.9 | Clean the sample cell and temperature transmission surface with isopropyl alcohol | |
| 5.1.10 | Fill sample cell with sample solution in such a way that, there should not be any gap/empty space at both ends. Then cap the both ends and observe from lens of Polarimeter cell that no air bubble present inside the cell. | |
| 5.1.11 | Take sample reading within 30 minutes of sample preparation because some compounds are optically unstable and may impact on the results. | |
| 5.2 | Operational Procedure: | |
| 5.2.1 | Switch ON the mains and the Automatic Polarimeter switch. | |
| 5.2.2 | Press “Zero” key to zero the instrument which is present on main screen after the instrument is just ON. | |
| 5.2.3 | Ensure the instrument is clean and free from dust. | |
| 5.2.4 | Check due date of instrument calibration before starting measurements. | |
| 5.2.5 | Wait for 10 minute to allow stable temperature. | |
| Note: For Sample measurement two paths are given
1. By selecting main window screen parameter like Temperature, Scale, Wavelength, measurement mode in setup menu. |
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| 2. By Selecting Sample Method | ||
| For Sample Measurement | ||
| 5.2.6 | Click on ‘Scale’ key on main screen. It contains measurement option
1. Optical rotation 2. Specific optical rotation 3. Concentration 4. Specific rotation plus 5. ‘Z’ Scale (589) |
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| 5.2.7 | If scale ‘optical rotation’ selected then a display shows parameters
1. Cell Length 2. Multiplier |
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| 5.2.8 | Select cell length 100 mm and multiplier as ‘1’& click on ‘Set’ key . | |
| 5.2.9 | If Scale ‘Specific Optical rotation’ selected then the display will show Parameter
1. Cell length 2. Concentration |
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| 5.2.10 | Select cell length 100 mm and put concentration as g/100 ml and click on set key. e.g. 10 % Sucrose solution then concentration value is 10.0 | |
| 5.2.11 | Note: 1. “Specific Rotation plus” mode is selected only when measuring sample has water content/ Loss on drying. The multiplier used to compensate for changes in a sample due to loss on drying/water content. Put “Multiplier” value by manually calculating by formula as
100/(100-water /LOD) e.g. Paracetamol Water content is 5.5 then multiplier value is 100/(100-5.5) = 1.06 2. If scale “Specific Rotation plus” selected then a display will show parameter 1.Cell length 2. Concentration 3. Multiplier 3. Put value of parameter and click on “SET” key. |
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| 5.2.12 | Click on ‘Temperature’ key on main screen display. Then screen shows parameters as
1. Temperature Control 2.Temperature correction 3.TempTrol 4.Water bath |
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| 5.2.13 | Select the ‘Temperature Control’ parameter. Then click on “TempTrol” option and select input temperature as 20ºC or 25ºC as per sample requirement and click on ‘Set’ key. | |
| NOTE: Put Temperature control option “ON” only when, in-built temperature probe kept in sample cell with sample solution. Otherwise keep “OFF” when in-built temperature probe is placed in the cap holder. | ||
| 5.2.14 | Select the Measurement mode: Single or Multiple from the Measurement mode menu in the Setup menu present on main screen. | |
| 5.2.15 | If single selected- It Measures sample one time
If Multiple mode selected, Enter the no. of measurement selected between 1 and 999 . Several measurement of sample made. For routine analysis ‘5’ number of measurement shall be selected. |
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| 5.2.16 | Press the ‘Wavelength ‘key on main screen and select the desired wavelength. | |
| 5.2.17 | Fill sample cell with sample blank (Diluent) and keep in sample chamber. Put in-built temperature probe in sample cell and close the door of sample compartment. | |
| 5.2.18 | After attaining set temperature click on ‘Zero’ key on main screen to nullify blank interference. | |
| 5.2.19 | Remove blank solution from sample cell and rinse the cell with sample solution for 2-3 times. | |
| 5.2.20 | Fill sample cell with measuring sample solution. Care should be taken that no air bubble will be observed inside wall of the cell. | |
| 5.2.21 | Keep sample cell with sample solution in sample chamber. Place in-built temperature probe in it. | |
| 5.2.22 | After attaining required sample temperature on digital display press “Start” key from main screen. The system will prompt for sample ID. Put sample ID and press “Enter” | |
| 5.2.23 | After completion of measurement, the result will display on main screen. | |
| 5.2.24 | To save or Print the measurement result click on ‘printer’ key on main screen window. Results will get saved in of ‘C’ drive with auto generated file name. | |
| 5.2.25 | Remove the sample cell from chamber; flush it with water and isopropyl alcohol. Clean outside surface of sample cell foot and temptrol surface with isopropyl alcohol. | |
| Note: 1. “Specific Rotation plus” mode is selected only when measuring sample has water content/ Loss on drying. The multiplier used to compensate for changes in a sample due to loss on drying/water content. Put “Multiplier” value manually calculating by formula as 100/(100-water/LOD) | ||
| 5.3 | Calibration Procedure: | |
| Frequency: Quarterly or after carrying out any major maintenance work. | ||
| 5.3.1 | Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA department for calibration formats of instruments on the due date of calibration. | |
| 5.3.2 | For issuance of calibration report refer SOP “Control of documents, Preparation, Approval, Issuance and Maintenance. | |
| 5.3.3 | Perform the calibration of instrument as per Annexure and procedure mentioned below. | |
| 5.3.4 | Calibrate the instrument using a solution of previously dried sucrose at 105º C for 1 hour. Measure the optical rotation in a 100 mm tube at 250 C by using the sucrose concentrations as follow:
1) 10 % sucrose solution: Dissolve 10 gm sucrose to 100 ml with water. 2) 20 % sucrose solution: Dissolve 20 gm sucrose to 100 ml with water. 3) 30 % sucrose solution: Dissolve 30 gm sucrose to 100 ml with water. 4) 40 % sucrose solution: Dissolve 40 gm sucrose to 100 ml with water. 5) 50 % sucrose solution: Dissolve 50 gm sucrose to 100 ml with water. |
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| 5.3.5 | Follow the same procedure of measurement as above mentioned in point number 5.2.1 to 5.2.25 | |
| 5.3.6 | Enter the details in calibration report. Ensure that the results obtained, comply with the acceptance criteria. If instrument fails to meet acceptance criteria then file a incident and investigate the cause of failure. | |
| NOTE: 1. Acceptance criterion for calibration of instrument by sucrose is given for 2 dm tube in USP/IP.
2. However, 1 dm tube is used in Polarimeter. Hence, manufacturer recommended the sensitivity of reading in 1 dm tube is exactly half of that 2 dm tube. The acceptance criteria is set according to manufacturer recommendation. |
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| 5.3.7 | Update the “Instrument/Equipment Usage Log Book”, “Annual Calibration Schedule” and “Quarterly Calibration Schedule” as per SOP “Calibration of Instruments and Equipments”. | |
| 5.3.8 | Affix the “Calibration Status Label” on the Instrument as per SOP “Calibration of Instruments and Equipments”. | |
| 5.3.9 | If calibration activity is outsourced, the values are to be transcribed in the Annexure, and external party certificate to be attached. | |
- Definitions / Abbreviations:
- Definitions:
- Calibration: Tests performed to ensure that the instrument is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
- Temperature Probe : It measure temperature of sample cell and main body of
- Optical Rotation : Substance are optically in the sense that they rotate incident plane polarized light so that the transmitted light energes at a measurable angle to the plane of the incident light.
- Polarimeter Principle :
| The optical rotation of a substance is the angle through which the plane of polarization is rotated when polarized light passes through the substance.
Substances are described as Dextro-rotatory (+) or Laevo-rotatory (-) according to whether the plane of polarization is rotated clockwise or anticlockwise.
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- Abbreviations:
| Abbreviation | Expansion |
| SOP | Standard Operating Procedure |
| QC | Quality Control |
| QA | Quality Assurance |
| 0C | Degree Celsius |
| % | Percentage |
| dm | decimeter |
| No. | Number |
| A. R. No. | Analytical Reference Number |
Calibration Report
| Sr. No. | Parameters | Standards | Acceptance Criteria | Observed Values |
| 1. | Optical Rotation
(at 25ºC) |
10 % sucrose solution | 6.665°
(6.590° to 6.700°) |
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| 20 % sucrose solution | 13.305°
(13.180 °to 13.400°) |
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| 30 % sucrose solution | 19.930°
(19.770° to 20.100°) |
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| 40 % sucrose solution | 26.530°
(26.360° to 26.800°) |
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| 50 % sucrose solution | 33.115°
(32.950° to 33.500°) |
Remark: The result Complies/Does not complies as per acceptance criteria.
Performed By: ________________ Date: ___________ Checked By: ______________ Date: ______________
*Note – Ready to use SOP available in “DOWNLOAD” Section.