SOP for Polarimeter

Auto Polarimeter

STANDARD OPERATING PROCEDURE

Company Logo	Name of the Company Unit, Address, City
TITLE	Operation and Calibration of Auto Polarimeter
SOP No.	QC-0XX	Department	Quality Control
Revision No.	0.0	Page No.	1 of 10
Effective Date	XX/YY/ZZZZ	Review Date	XX/YY/ZZZZ

1.0     PURPOSE

1.1     This procedure describes the Operation and Calibration of an Auto Polarimeter.

 

2.0     SCOPE

2.1     This procedure is applicable to Pharma Lab at Name of the company, Address.

 

3.0     ABBREVIATIONS/ DEFINITIONS

3.1     USP - United States Pharmacopoeia      

3.2     MCP- Modular circular polarimeter

3.3  Optical Rotation: 

      The optical rotation of a substance is the angle through which the plane of polarization is rotated when polarized passes through the substance, if liquid, or a solution of the substance, if solid Substances are described as dextrorotatory or laevorotatory according to whether the plane of polarization is rotated clockwise or anti-clockwise respectively as determined by viewing the light source. Dextrorotatory is designated (+) and laevorotatory is designated (-). Optical rotation is expressed in degrees.

3.4     Specific Optical Rotation: 

     The specific optical rotation [α]_D²⁵ of a substance is the angle of rotation, ‘α’, of the plane of polarization at the wavelength of the D line of sodium (λ=589.3) measured at 25⁰C unless otherwise specified, calculated with reference to a 1dm thick layer of a solution containing 1 gm of the substance per mL. It is always expressed with reference to a given solvent and concentration. 

4.0     RESPONSIBILITY

4.1     User is responsible for following this procedure.

4.2     QC HOD /  Designee shall responsible for the implementation of this procedure.

4.3     QA shall monitor for compliance with this procedure.

 

5.0     PROCEDURE

5.1     Operation

5.1.1  Ensure that the working bench and instrument are clean.

5.1.2  Switch “ON” the instrument

5.1.3  Log in: Click on the user indicator (right upper corner), and the login dialogue box opens.

5.1.4  Enter the user name and password on the login screen

5.1.5  Enter by pressing <OK>

5.1.6  After logging in, the main screen appears with the following operational functions.

·         Header: Contains current method name and sample

·         Content area: This shows the measuring value.

·         Output field: Shows output parameters.

·         Progress bar: Shows the actual status of the measurement

·         Toolbar: Consists of the menu, measured data, Quick setting, method and start

5.1.7  On the right side of the main screen there is a quick access area that displays the general instrument status as well as all measuring errors that have occurred during the measurement.  The button colour changes its appearance as green, yellow and red depending on the current error status.

5.1.8     Green sign Indicates: The general instrument status is OK all measurement s ok 

5.1.10     Red flash sign Indicates:

The instrument has a major problem.

One or more samples could not be measured.

5.1.11     To reset the diagnosis button to the green sign, confirm all error messages by tapping on the <x> button on the right side of the message.

5.1.12     Wait for min.15 minutes, to initialise the instrument.

5.1.13     Thoroughly flush the sample cell and fill it bubble-free with an optically inactive liquid (usually the sample solvent).

5.1.14     Position the measurement cell in the measuring compartment and close the cover.

5.1.15     Tap the optical button on the right side of the main screen.

5.1.16     The optical zero point is set and the display shows zero value for the optical rotation.

5.1.17     Remove the solvent from the sample cell.

5.1.18     Fill in the Sample homogenously bubble-free & avoid solid particles because they would effect the measurement result.

5.1.19     Click on start. Enter the fields such as sample name; batch No. concentration and temperature again click on start.

5.1.20     The instrument starts the measurement. When the measurement is over the message “finished “appear on the screen.

5.1.21     Repeat the steps 5.1.15 to 5.1.19 for the consecutive measurement of the samples

5.2   Calibration

5.2.1   Temperature calibration:

·      Check the sensor at 20°C and 25°C using a certified calibrated thermometer and allow sufficient time for thermal equilibrium.

·      Fill the sample cell with water and set the desired temperature. Insert the probe of the thermometer in the sample cell

·      Compare the display temperature with a certified thermometer under equilibrium conditions. The difference should be Not more than ±0.5°C.

5.2.2  Accuracy and Linearity with Sucrose solution:

· Optical rotation of the solutions should be determined within 30 minutes of preparation.

·    All the measurements in the calibration activity should be taken at 25± 0.5⁰C at 589nm.

·      Use the same cell for sample and test solution.

·      Place the cell that the light passes through it in the same direction each time.

Preparation of 10% w/v Sucrose solution:

·      Weigh about 10 g of sucrose and transfer it into a 100 mL volumetric flask.

·      Dissolve and makeup to the volume with water.

        Preparation of 20% w/v Sucrose solution:

·      Weigh about 20 g of sucrose and transfer it into a 100 mL volumetric flask.

·      Dissolve and makeup to the volume with water.

      Preparation of 30% w/v Sucrose solution:

·      Weigh about 30 g of sucrose and transfer it into a 100 mL volumetric flask.

·      Dissolve and makeup to the volume with water.

      Preparation of 40% w/v Sucrose solution:

·      Weigh about 40 g of sucrose and transfer it into a 100 mL volumetric flask.

·      Dissolve and makeup to the volume with water.

     Preparation of 50% w/v Sucrose solution:

·      Weigh about 50 g of sucrose and transfer it into a 100 mL volumetric flask.

·      Dissolve and makeup to the volume with water.

5.2.3                    Procedure

·      Allow the instrument to warm up for 30 minutes.

·      Take 100mm Polarimeter cell and rinse and fill with water which is at 25 ± 0.5⁰C.

·    Clean the tissue with tissue paper and care should be taken that there are no air bubbles in the tube.

·  Place the cell in the sample compartment and measure the reading. After stabilization, press the set Zero switch, and the Polarimeter should show zero. If not, rinse the cell with water and repeat the operation until zero reading is obtained.

·      Remove the cell from the compartment, rinse with 10% w/v sucrose solution, fill it with the same, clean the cell with tissue paper and place it in the sample compartment. Ensure that the temperature of the solution is 25 ± 0.5⁰C.

·      Measure the angle of rotation five times and determine the average reading.

·      Ensure that the %RSD of the above five readings is less than 2.0.

·  Similarly measure the angle of rotations for 20%w/v, 30%w/v, 40%w/v and 50%w/v sucrose solutions.

Accuracy check:

l Check the accuracy of the instrument with sucrose solution at 589nm and determine through % RSD.  The % RSD shall be NMT 2.0%

Calculation:

·      Angle of rotation equivalent to standard concentration (10%, 20%, 30%, 40% & 50% w/v solutions):

                      Observes rotation × standard weight

                          Weight of sucrose taken in g

Linearity Check:

·   Determine the linearity by using 10%, 20%, 30%, 40% and 50% sucrose solutions and calculate the correlation coefficient.  The correlation coefficient shall be NLT 0.995.

Acceptance criteria:

Accuracy with Sucrose (At wavelength 589 nm)	10% w/v solution	+6.665 ± 0.1°
	20% w/v solution	+13.305 ± 0.1°
	30% w/v solution	+19.930± 0.1°
	40% w/v solution	+26.530 ± 0.1°
	50% w/v solution	+33.115 ± 0.1°
Linearity with Sucrose	Correlation Coefficint Not Less Than 0.995

 5.3  Maintenance

5.3.1        Sample cell should be clean with ethanol/acetone before performing the test.

5.3.2        Preventive maintenance performed by service engineer before calibration.

5.3.3        Backup schedule performed every 1 month by IT personnel.

5.4   Calibration frequency: 6 months.

6.           ANNEXURES

6.1       Annexure I:  Autopolarimeter usage logbook

6.2      Annexure II: Calibration Record for Autopolarimeter

             REFERENCES

7.1      Operating instructions manual of Auto polarimeter

7.2      USP <781> Optical rotation

8.0     REVISION HISTORY

Version no.	Effective date	Summary of revision
0.0		Original Version

                                                                            

  END OF THE DOCUMENT

 

 

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Annexure-I

AUTOPOLARIMETER USAGE LOGBOOK

 

S.No.	Date	Reg. No	Sample particulars	Start Time	End time	Analyst Sign & Date	Checked by Sign & Date	Remarks

 

 

 

                                                                                                  

         

CompanyLogo

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Annexure-II

CALIBRATION RECORD FOR AUTOPOLARIMETER

Equipment ID:		Sucrose Make/Grade/Lot No.
		Sucrose Expiry date:
Balance ID:		Balance Calibration due date:
Thermometer ID:		Thermometer calibration due:
Calibration start date:		Calibration end date:

 

S. No.	Set Temperature (A)	Observed  value (B)	Deviation (A-B)
1.	20°C
2.	25°C

 

    1)   Temperature Test:

Acceptance criteria: deviation is NMT ± 0.5°C

Result: Pass / Fail

 

          Performed by (Sign& Date)                                                                Reviewed by (Sign& Date)

    2) Accuracy and Linearity with Sucrose solution

  Sno  WL(λ)  Conc(w/v)   A.R.at 25°c Conc(w/v) Conc(w/v) Conc(w/v) Conc(w/v) 

     1    589        10%                                  20%          30%             40%           50%

     2    589        10%                                  20%          30%             40%           50% 

     3    589        10%                                  20%          30%             40%           50%

     4    589        10%                                  20%          30%             40%           50%

     5    589        10%                                  20%          30%             40%           50%

*Conc. – Concentration and A.R. Angle of Rotation

Acceptance criteria: for 10% =+6.665 ±0.1°, for 20%= +13.305 ±0.1°, for 30%= +19.930±0.1°, for 40%= +26.530 ±0.1°, and for 50%=+33.115 ±0.1°

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Linearity of Sucrose solution:

S. No	Avg. Conc. 10% (w/v)	Avg. Conc. 20% (w/v)	Avg. Conc. 30% (w/v)	Avg. Conc. 40% (w/v)	Avg. Conc. 50% (w/v)
Correlation Coeffiecient : NLT 0.995

 

 

Result: Pass / Fail

 Performed by (Sign& Date)                                                                Reviewed by (Sign& Date)

 The results of calibration are “within /out of” acceptance limit and the instrument is ready for further  use /requires maintenance.

Next Calibration date:

 Remarks:  

	Performed by	Reviewed by HOD/ Designee	Reviewed by QA
Name
Designation
Sign & Date