CHLOROXYLENOL SOP


CHLOROXYLENOL SOP
1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Chloroxylenol 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  White or cream crystals or crystalline powder.
5.1.1.2  Volatile in steam.
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        Purified water.
5.1.2.1.3        Ethanol (96%).
5.1.2.1.4        Ether.
5.1.2.1.5        Terpenes.
5.1.2.1.6        Fixed oil.
5.1.2.1.7        Alkali hydroxides.
5.1.2.2  Sample:
5.1.2.2.1        Small quantity.
5.1.2.3  Method:
5.1.2.3.1        Take 6 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 ethanol (96%) in test tube 2 and observe.
5.1.2.3.4        Add ether in test tube 3 and observe.
5.1.2.3.5        Add terpenes in test tube 4 and observe.
5.1.2.3.6        Add fixed oils in test tube 5 and observe.
5.1.2.3.7        Add alkali hydroxide in test tube 6 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with water is very slightly soluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol (96%) is freely soluble.
5.1.2.4.3        The sample in test tube 3, 4 and 5 containing with ether, terpenes and fixed oils is soluble respectively.
5.1.2.4.4        The sample in test tube 6 containing with alkali hydroxide is dissolved.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (test tube, spatula).
5.2.1.1.2        Chloroform.
5.2.1.1.3        1% w/v solution of anhydrous iron (III) chloride.
5.2.1.1.4        Pyridine.
5.2.1.2  Sample:
5.2.1.2.1        0.1g.
5.2.1.3  Method of analysis:
5.2.1.3.1        Take a test tube and add in it 0.1g of sample and dissolve it in 5.0ml of chloroform.
5.2.1.3.2        And add 0.5ml of filtered 1% w/v solution of anhydrous iron (III) chloride in chloroform and 0.1ml of pyridine.
5.2.1.3.3        Observe changes closely.
5.2.1.4  Observations:
5.2.1.4.1        A blue color is produced.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (test tube, spatula).
5.2.2.1.2        Iron (III) chloride solution.
5.2.2.1.3        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        Saturated solution of active ingredient.
5.2.2.3  Method of analysis:
5.2.2.3.1        Take a test tube and add in it 5ml of a saturated solution in water.
5.2.2.3.2        Add 0.5ml of iron (III) chloride solution.
5.2.2.3.3        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        No blue colour is produced.
5.2.3         
5.2.3.1  Material and equipment:
5.2.3.1.1        Glassware (according to requirement).
5.2.3.1.2        Burner.
5.2.3.1.3        Anhydrous sodium carbonate.
5.2.3.1.4        Nitric acid.
5.2.3.1.5        Silver nitrate solution.
5.2.3.1.6        Purified water.
5.2.3.2  Sample:
5.2.3.2.1        50.0mg.
5.2.3.3  Method of analysis:
5.2.3.3.1        Take a test tube and add 50.0mg of sample in it.
5.2.3.3.2        Mix it with 0.5g of anhydrous sodium carbonate.
5.2.3.3.3        Ignite it strongly.
5.2.3.3.4        Cool it.
5.2.3.3.5        And then boil the residue with 5ml of water.
5.2.3.3.6        Acidify with nitric acid.
5.2.3.3.7        Filter it.
5.2.3.3.8        And then add silver nitrate solution in it.
5.2.3.3.9        Observe the changes.
5.2.3.4  Observations:
5.2.3.4.1        White ppt is produced.
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  Stoppered conical flask.
5.3.2        Material and reagents:
5.3.2.1  Glacial acetic acid.
5.3.2.2  0.0167M of potassium bromate.
5.3.2.3  15% w/v solution of potassium bromide.
5.3.2.4  Hydrochloric acid.
5.3.2.5  Potassium iodide.
5.3.2.6  0.1M sodium thiosulphate.
5.3.2.7  Starch solution.
5.3.2.8  Purified water.
5.3.3        Sample:
5.3.3.1  70.0mg
5.3.4        Method of analysis:
5.3.4.1  Sample titration:
5.3.4.1.1        Take a stoppered flask and add in it 70.0mg of the sample.
5.3.4.1.2        Dissolve the sample in 30.0ml of glacial acetic acid.
5.3.4.1.3        Add 25ml of 0.0167M of potassium bromate, 20ml of a 15% w/v solution of potassium bromide and 10.0ml of hydrochloric acid.
5.3.4.1.4        Stopper the flask.
5.3.4.1.5        Allow it to stand protected from light for 15 minutes.
5.3.4.1.6        Add 1.0g of potassium iodide and 100ml of water.
5.3.4.1.7        Set your titration apparatus.
5.3.4.1.8        Titrate with 0.1M sodium thiosulphate.
5.3.4.1.9        Shake vigorously.
5.3.4.1.10    Use 1.0ml of starch solution as indicator at the end of titration.
5.3.4.1.11    Add only few drops.
5.3.4.1.12    Calculate the sample titration results.
5.3.4.2  Blank titration:
5.3.4.2.1        Repeat the operation without the substance being examined.
5.3.4.2.2        Take a stoppered flask and add in it 30.0ml of glacial acetic acid, 25ml of 0.0167M of potassium bromate, 20ml of a 15% w/v solution of potassium bromide and 10.0ml of hydrochloric acid.
5.3.4.2.3        Stopper the flask.
5.3.4.2.4        Allow it to stand protected from light for 15 minutes.
5.3.4.2.5        Add 1.0g of potassium iodide and 100ml of water.
5.3.4.2.6        Set your titration apparatus.
5.3.4.2.7        Titrate with 0.1M sodium thiosulphate.
5.3.4.2.8        Shake vigorously.
5.3.4.2.9        Use 1.0ml of starch solution as indicator at the end of titration.
5.3.4.2.10    Add only few drops.
5.3.4.2.11    Calculate the blank titration results.
5.3.4.3  The difference between the titrations represents the amount of potassium bromate required.
5.3.5        Limit:
5.3.5.1  98.0% to 103.0%.
5.3.6        Factor:
5.3.6.1  Each ml of 0.0167M Potassium bromate is equivalent to 3.915mg of C8H9ClO.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol I., Official Monograph /Chloroxylenol: 2009, pp. 1286- 1287.
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
%
Percentage
B.P
British pharmacopoeia
w/v
Weight per volume
g
Gram
Ml
Milliliter
mg
Milligram
ppt
Precipitate
M
Molar
Vol
Volume
QCA
Quality control active ingredient
F
Format



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