Automatic Polarimeter Calibration SOP


1.0  OBJECTIVE:
To lay down the calibration procedure for reliable and accurate results.
2.0  SCOPE:
This shall be applicable to the pH meter of Quality Control Laboratory.
3.0  RESPONSIBILITY:
3.1  Technical Assistant/ Helper.
3.2  Q.C Analyst.
4.0  ACCOUNTABILITY:
4.1  Manager-Quality Control.
5.0  MATERIAL AND EQUIPMENT:
5.1  Polarimeter.
5.2  Desiccator.
5.3  Magnetic stirrer.
5.4  Glassware (6 beaker of 100.0ml, 1 stirrer, spatula).
5.5  Tissue paper.
5.6  Standard refined sucrose previously dried at 105oC for 3 hours.
5.7  Acetone.
5.8  Purified water.
6.0  PROCEDURE:
6.1  Switch ON the mains.
6.2  Operate the Polarimeter according to the SOP
6.3  Wait till sodium lamp glows with full intensity of yellow light.
6.4  Rinse the Polarimeter tube with distilled water.
6.5  Adjust the vernier scale and main dial scale to zero.
6.6  If two halves intensity is not metering then adjust it by turning knurled screw of the prism box slightly. If not possible then adjust the field by rotating milled knob and vernier scale note the reading (+) or (-) side as a zero and to be consider while calibrating.
6.7  Fill the purified water in Polarimeter tube.
6.8  Clean the sides of the tube with tissue paper.
6.9  Entrap any air bubble in space at center of the tube.
6.10    Keep the Polarimeter tube in the place provided in the Polarimeter.
6.11    Adjust the zero with the help of control wheel.
6.12    Focus circular disc of light with the help of field telescope.
6.13    Observe the field, which is divided into two halves, light and dark.
6.14    Adjust the control wheel to get equal intensity of the two halves.
6.15    Measure optical rotation of the blank solution.
6.16    Note the + or – reading in degree of rotation.
6.17    Repeat the step no. 6.5 to 6.15 for 5 times.
6.18    Take average of the 5 readings.
6.19    Remove the Polarimeter tube from Polarimeter & discard the purified water from the tube.
6.20    Prepare 10%, 20%, 30%, 40% & 50% solution in purified water of standard refined sucrose previously dried at 105oC for 3 hours.
6.21    Rinse the tube with 10% solution and fill the solution in Polarimeter tube.
6.22    Clean the sides of the tube with tissue paper.
6.23    Entrap any air bubble in the space at the centre of tube.
6.24    Keep the Polarimeter tube in the space provided in the Polarimeter and measure the optical rotation of sample solution.
6.25    Note the reading in degree of rotation.
6.26    Repeat the operation 5 times and record the readings.
6.27    Remove the tube from Polarimeter & discard the solution from the tube.
6.28    Repeat the operation with 20%, 30%, 40% & 50% solution after rinsing with the same solutions.
6.29    Note the readings of each concentration.
6.30    Remove the tube from Polarimeter and discard the solution from the tube.
6.31    Wash the tube from Polarimeter and discard the solution from the tube.
6.32    Wash the tube with purified water and rinse with acetone and keep in Polarimeter tube box.
6.33    Switch OFF the mains.
6.34    Enter the calculated readings in calibration record.
6.35    Record the result on the “Calibration Record”, “Calibration Log Book” & paste the “Calibration Status Sticker” on Polarimeter.
6.36    Acceptance criteria (if any):
6.36.1 Difference between std. value and calculated value must not be more than 0.05o for 10% & 20% and not more than 0.1o for 30%, 40% & 50% solution.
6.37    If the value does not meet the acceptance criteria, inform the QA/QC manager for further action.
6.38    Frequency of calibration: Monthly or after any maintenance.
6.39    Precautions:
6.39.1 Polarimeter tube should be filled in such a way so as to avoid air bubbles.
6.39.2 Before taking the reading clean the Polarimeter tube with tissue appear.
6.39.3 Set the field telescope for better observation.
6.39.4 The optical elements must be cleaned and at exact alignment.
6.39.5 Tighten the end plate with caps and seal so as to make it leak proof.
7.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

8.0  REFERENCES:
8.1  Not Applicable.
9.0  ANNEXURES:
Annexure 1: Calibration sheet of Polarimeter.


Annexure: 1
Calibration sheet of Polarimeter
Calibration of Polarimeter
Instrument: ___________________                                              Date: _______________
Model: _______________________        Length of Polarimeter tube: ________________
Calibration solution: Sucrose solution of different concentration.
Blank solution: Purified water.
Blank solution:
Sr.#
Blank solution
Temperature
Optical rotation
(α)
1.



2.



3.



4.



5.



Average: _________________________
*Specific optical rotation of blank solution by using formula:
[α]λ T = α/lc










Sample solution:
Sr. #
Sample solution
Temperature
T
Optical rotation
(α)
Calculated value of specific optical rotation
(A=[α]λ T)
Standard value of specific optical rotation
(B=[α]λ T)
Standard value – calculated value
(B-A)
1.
10%





2.
20%





3.
30%





4.
40%





5.
50%





*Specific optical rotation of sample solution by using formula:
[α]λ T = α/lc
* Difference between std. value and calculated value must not be more than 0.05o for 10% & 20% and not more than 0.1o for 30%, 40% & 50% solution.












10.0    ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number  
Ltd.
Limited
Q.C
Quality control
Q.A
Quality assurance
QCEB
Quality control equipment calibration
F
Format
oC
Degree centigrade
ml
Milliliter
%
Percentage
o
Degree (angle)
l
Length
g
Grams
c
Concentration (g/ml)
α
Alpha (here it is denoted as observed optical rotation)
λ
Lambda
T
Temperature
[α]λ T
Specific optical rotation
Sr.#
Serial number


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