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
|