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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