SOP for Operation and Calibration of the Polarimeter as per IP

The procedure for the operation and calibration of the polarimeter. It is the policy of XYZ Pharmaceuticals Limited that a written procedure shall be followed for the operation and calibration of the polarimeter.

This SOP is applicable at the time of the operation and calibration of the polarimeter.

RESPONSIBILITY AND ACCOUNTABILITY

Persons along with their responsibilities and accountability are given below:

Executive  - Corporate Quality Assurance:- To prepare the SOP. Maintain the record as per SOP.

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

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

Operation and Calibration of Polarimeter

Operation of the Polarimeter

5.1.1 Connect the instrument to the main power supply (if not connected).

5.1.2 Ensure that the instrument is clean and free from dust particles.

5.1.3 Ensure that the polarimeter tube is cleaned each time before and after use.

5.1.4 Switch “ON” the instrument and allow sufficient time to achieve the maximum brightness of the sodium lamp.

5.1.5 Adjust the eyepiece after viewing through it to get a clear focus.

5.1.6 Ensure that the settings are done in the zero-zero position.

5.1.7 Open the polarimeter tube compartment and place the polarimeter tube, which is filled with a blank solution in such a way as to avoid air bubbles at 25oC.

5.1.8 Close the open end of the polarimeter tube and bring the air bubble (if any) into the central bulged portion of the tube.

5.1.9 Determine the five readings of blank solution and calculate the average of blank readings.

5.1.10 The specific rotation observations are done by viewing through the telescope when the half-dark and half portion of the cycle are in equilibrium.

 The half-dark and half-light are matched with the knob rotating it in the clockwise and anticlockwise directions. It is also defined as Dextro (+) or Levo (-) rotating respectively.

Note the observation readings.

Now fill the polarimeter tube with the test solution (maintained at 25 ˚C) determine the zero point of the polarimeter and then make five readings of the observed rotation of the test solution.

The zero correction is the average of the blank readings and is subtracted from the average observed rotation if the two figures are of the same sign or added if they are opposite in sign to obtain the corrected observed rotation

5.1.15  In the case of the liquids, adjust the temperature of the substance under examination to 25 ˚ C unless specified in the monograph, transfer it to a polarimeter tube, and proceed as described above.

Switch “OFF”, clean the instrument, and keep it under cover when not in use.

5.1.17  The logbook shall be maintained as per XYZ/CQA/SOP-061/FR-01, Logbook for Polarimeter (Appendix I).

Calibration of polarimeter as per IP

The frequency of calibration shall be every quarter and after the maintenance of the instrument.

Switch “ON” the instrument and warm up the sodium lamp to its maximum brightness.

Set the alignment of the sodium lamp compartment to the optical bench.

Ensure that all the settings are done in the zero position.

Open the polarimeter tube compartment and place the polarimeter tube, which is filled with water in such a way as to avoid air bubbles at 25oC.

The specific rotation observations are done by viewing through a telescope when the half-dark and half-light portions of a circle are in equilibrium.

This half-dark and a half-light portion are matched with a knob by rotating it in a clockwise or anti-clockwise direction. It is also defined as Dextro (+) or Levo (-) rotatory respectively.

Note the observation readings.

Preparation of Standard Solutions used for calibration of polarimeter

5.2.9.1 Dried the sucrose used for calibration for 2 hours in a vacuum oven (60 ˚C).

5.2.9.2 10 % w/v solution:  Weigh accurately about 10 gm of the standard (sucrose) in a 100 ml volumetric flask, add a sufficient amount of distilled water to dissolve, and then make up the volume up to the mark with distilled water.

5.2.9.3 20% w/v solution:  Weigh accurately about 20 gm of standard (sucrose) in a 100 ml volumetric flask, add a sufficient amount of water to dissolve, and then finally make up the volume up to the mark with distilled water.

5.2.9.4 30 % w/v solution:  Weigh accurately about 30 gm of standard (sucrose) in a 100 ml volumetric flask, add a sufficient amount of distilled water to dissolve, and then finally make up the volume to the mark with distilled water.

5.2.9.5 40%w/v solution:  Weigh accurately about 40 gm of standard (sucrose) in a 100 ml volumetric flask, add a sufficient amount of distilled water to dissolve, and then finally make up the volume up to the mark with distilled water.

5.2.9.5 50 % w/v solution:  Weigh accurately about 50 gm of standard (sucrose) in a 100 ml volumetric flask, add a sufficient amount of distilled water to dissolve, and then finally make up the volume up to the mark with distilled water.

Now fill the polarimeter tube with 10% w/v solution of sucrose and carry out the determination in a similar manner as blank at 25oC.

Operation and Calibration of the Polarimeter


Repeat the steps 5.2.4 to 5.2.8 for 20, 30, 40, and 50% w/v concentration of sucrose solution.

Clean the instrument and keep it under cover when not in use.

The table containing concentration and corresponding angle of rotation in a 2-dm tube at 25oC is indicated below:

Concentration (gm/100ml)              The angle of rotation (+) at 25°C

10.0                                                 13.33 ± 0.05

20.0                                                 26.61 ± 0.05

30.0                                                 39.86 ± 0.05

40.0                                                 53.06 ± 0.05

50.0                                                66.23 ± 0.05

The polarimeter is calibrated and a graph for linearity and Acceptance criteria of the correlation coefficient should not be less than 0.99.

Record the observations of the calibration as per XYZ/CQA/SOP-061/FR-02, Calibration Data Sheet (Appendix II).

Compare the result with acceptance criteria and take valid calibration authorization from the Manager – Quality Assurance. Affix the calibration sticker on the instrument as per SOP no. XYZ/CQA/SOP-006, Labelling policy and fill in all the details carefully.

Report any discrepancy observed during the calibration of the instrument to the Manager of Technical Quality Control or his authorized representative for corrective and preventive action.

The manager of Technical Quality Control or his authorized representative will report the same to quality assurance and notify the defect to Engineering Department service engineer to rectify the defect.

If the instrument has any discrepancy, affix the ‘Out of Order’ label on the instrument as per SOP no. XYZ/CQA/SOP-006, Labelling policy.

CALCULATIONS

Calculate the specific optical rotation using the following formulae, dextrorotation, and laevo - rotation being designated by (+) and (-) respectively.

For liquids        [α] 25D               =          α / Ld 25

For solids         [α] 25D               =          100 α / Lc

Where,

α          =          corrected observed rotation, in degrees, at 25˚

D         =          D line of sodium light (L = 589.3 nm)

L          =          length of the polarimeter tube in dm

d2525       =          specific gravity of the liquid or solution at 25 ˚

c          =          concentration of the substance in percent w/v

CLEANING OF POLARIMETER TUBE

Never use a brush to clean the polarimeter tube.

Clean the polarimeter tube using the purified water or any organic solvent (acetone or methanol) and dry the polarimeter tube.

Add about 1 ml of the solution to be measured. Tilt and turn the polarimeter tube so that the solution has contact with the entire surface. Discard the solution and repeat this rinse once more.

5.4.5    Wash the polarimeter knurled rings and glass with the solvent used for the preparation of the solution for a test. Reassemble the polarimeter tube and keep it in a closed container.

5.4.6    Wipe the optics with soft tissue paper.

Wipe the outside of the polarimeter tube with a lint-free, soft tissue to remove any moisture or fingerprints from the outside surface.

Do not use acid/alkali solution or solvent for the cleaning of the instrument

PRECAUTION OF POLARIMETER

The instrument must be in good condition. The optical element must be very clean and in exact alignment. The match point should be close to the normal zero mark.

The light source should be properly aligned concerning the optical bench. It should be supplemented by a filtering system capable of isolating the D line from sodium light.

Specific attention should be paid to the temperature control of the solution and of the polarimeter.

Differences between the initial readings or between observed and corrected optical rotation, calculated as either specific optical rotation or optical rotation, should not be more than one-fourth of the range specified in the monograph for the substance.

Polarimeter tubes should be filled in such a way as to avoid air bubbles. Particular care is necessary for semi-micro or micro-tubes.

For tubes with removable end-plates fitted with gaskets and caps, tighten the endplates only enough to ensure a leak-proof seal between the endplate and the body of the tube.

For substances with low rotatory power, the end-plates should be loosened and tightened again after each reading, in the measurement of both the rotatory and the zero point.

5.5.8 Liquids and solutions of solid must be clear

6.0 GENERATION OF INSTRUMENT CALIBRATION NUMBER

Generate the instrument calibration number on the calibration datasheet as INSCALXXYYZZZ where INS denotes the instrument, XX denotes the year, YY denotes the month and ZZZ denotes the sequence number.

7.0   ABBREVIATIONS

            XYZ                 XYZ Pharmaceutical Limited

            CQA                Corporate Quality Assurance

            SOP                Standard Operating Procedure

 >Procedure for Operation and Calibration of Photofluorimeter.


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