LINDANE SOP


1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Lindane from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
4.0  ACCOUNTABILITY:
4.1  Q.C Manager.
5.0  PROCEDURE:
5.1  Characters:
5.1.1        Appearance:
5.1.1.1  A white or almost white.
5.1.1.2  Crystalline powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (test tubes, spatula).
5.1.2.1.2        Acetone.
5.1.2.1.3        Purified water.
5.1.2.1.4        Ethanol.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 3 test tubes and add small quantity of sample for testing solubility according to B.P specifications.
5.1.2.3.2        Add purified water in test tube 1 and observe.
5.1.2.3.3        Add acetone in test tube 2 and observe.
5.1.2.3.4        Add ethanol in test tube 3 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with water is practically insoluble.
5.1.2.4.2        The sample in test tube 2 containing with acetone is freely soluble.
5.1.2.4.3        The sample in test tube 3 containing with ethanol is soluble.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        Melting point apparatus (beaker, stirrer, thermometer, capillary tube, burner, thread).
5.2.1.1.3        Purified water.
5.2.1.2  Sample:
5.2.1.2.1        A small quantity.
5.2.1.3  Method of analysis:
5.2.1.3.1        Melting point determination method:
5.2.1.3.1.1  Firstly set the apparatus.
5.2.1.3.1.2  Fill 100ml beaker with water and place wire gauze on tripod stand, put beaker on it.
5.2.1.3.1.3  Heat up the capillary tube on burner from center such that it divides into two by pulling the capillary tube from both sides in opposite directions.
5.2.1.3.1.4  Introduce a sufficient quantity into a capillary tube to give a compact column 4mm to 6mm in height.
5.2.1.3.1.5  Tie up the capillary tube near the thermometer bulb with the help of thread.
5.2.1.3.1.6  And hang the thermometer on stand such that the capillary tube is not fully immersed in water. The immersion mark of which is at the level of the surface of the liquid.
5.2.1.3.1.7  Allow the burner to heat up the liquid in beaker.
5.2.1.3.1.8  Observe it closely.
5.2.1.3.1.9  Record the temperature at which the last particle passes into the liquid phase.
5.2.1.4  Observations:
5.2.1.4.1        The melting point of sample is 112oC to 115oC.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Centrifugation machine.
5.2.2.1.3        Alcohol.
5.2.2.1.4        0.5M potassium hydroxide alcoholic.
5.2.2.1.5        Dilute nitric acid.
5.2.2.1.6        Silver nitrate solution.
5.2.2.1.7        Ammonia.
5.2.2.1.8        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        5.0mg.
5.2.2.3  Method of analysis:
5.2.2.3.1        Take a test tube and add in it 5.0mg of sample.
5.2.2.3.2        Dissolve it in 4.0ml of alcohol.
5.2.2.3.3        Add 1.0ml of 0.5M potassium hydroxide alcoholic.
5.2.2.3.4        Allow it to stand for 10 min.
5.2.2.3.5        Use 2ml of the above solution.
5.2.2.3.6        Acidify with dilute nitric acid.
5.2.2.3.7        And add 0.4ml of silver nitrate solution.
5.2.2.3.8        Shake and allow it to stand.
5.2.2.3.9        A curdled, white ppt is formed.
5.2.2.3.10    Centrifuge it. Operate it according to SOP.
5.2.2.3.11    Wash the ppt with 3 quantities, each of 1ml, of water.
5.2.2.3.12    Carry out this operation rapidly is subdued light, degrading the fact that the supernatant solution may not become perfectly clear.
5.2.2.3.13    Suspend the precipitate in 2ml of water and add 1.5ml of ammonia.
5.2.2.3.14    Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        The precipitate dissolves easily with the possible exception of a few large particles which dissolves slowly.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Titration apparatus.
5.3.1.3  Water-bath.
5.3.2        Material and reagents:
5.3.2.1  Alcohol.
5.3.2.2  0.5M alcoholic potassium hydroxide.
5.3.2.3  Dilute nitric acid.
5.3.2.4  0.1M silver nitrate.
5.3.2.5  Ferric ammonium sulphate solution.
5.3.2.6  0.1M ammonium thiocyanate.
5.3.2.7  Purified water.
5.3.3        Sample:
5.3.3.1  0.2g.
5.3.4        Method of analysis:
5.3.4.1  Take a beaker of 50.0ml and take in it 0.2g of sample.
5.3.4.2  And add 10.0ml of alcohol.
5.3.4.3  Warm it on water bath until dissolved.
5.3.4.4  Cool it.
5.3.4.5  Add 20.0ml of 0.5M alcoholic potassium hydroxide.
5.3.4.6  And allow it to stand for 10 min.
5.3.4.7  Swirl it frequently.
5.3.4.8  Add 50.0ml of water, 20.0ml of dilute nitric acid, and 25.0ml of 0.1M silver nitrate and 5.0ml of ferric ammonium sulphate solution.
5.3.4.9  Set titration apparatus.
5.3.4.10    Titrate the above solution with 0.1M ammonium thiocyanate until a reddish-yellow colour is obtained.
5.3.5        Factor:
5.3.5.1  1ml of 0.1M Silver nitrate is equivalent to 9.694mg of C6H6Cl6.
5.3.6        Limit:
5.3.6.1  99.0% to 100.5%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph /Lindane: 2009, pp. 3499- 3500.
8.0  ANNEXURES:
8.1  Not Applicable.








9.0  ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number  
Ltd.
Limited
Q.C
Quality control
B.P
British pharmacopoeia
ml
Milliliter
mm
Millimeter
oC
Degree centigrade
M
Molar
mg
Milligram
Min
Minutes
ppt
Precipitate
g
Grams
%
Percentage
Vol
Volume
QCA
Quality control active ingredient
F
Format


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