1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Ammonium chloride 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 almost white.
5.1.1.2 Crystalline powder.
5.1.1.3 Colourless.
5.1.2
Solubility:
5.1.2.1 Material and equipment:
5.1.2.1.1
Glassware
(1 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2
Purified
water.
5.1.2.2 Sample:
5.1.2.2.1
Small
quantity.
5.1.2.3 Method:
5.1.2.3.1
Take
a test tube and add small quantity of sample for testing solubility according
to B.P specifications.
5.1.2.3.2
Add
purified water in it and observe.
5.1.2.4 Observations:
5.1.2.4.1
The
sample in test tube containing with water is freely soluble.
5.2 Solution
S:
5.2.1
Material
and equipment:
5.2.1.1 Glassware (1 100.0ml of beaker, 1 spatula,
1 glass rod, 1 pipette).
5.2.1.2 Carbon-dioxide free water.
5.2.1.3 Analytical weighing balance.
5.2.1.4 Magnetic stirrer.
5.2.2
Sample:
5.2.2.1 10.0g.
5.2.3
Preparation
of solution S:
5.2.3.1 Take a beaker of 100.0ml and add sample
10.0g in it.
5.2.3.2 Add in it carbon-dioxide free water which
is prepared from distilled water.
5.2.3.3 Dissolve it by using magnetic stirrer.
5.2.3.4 Dilute it to 100.0ml with same solvent.
5.3 Identification
tests:
5.3.1
Chlorides test:
5.3.1.1 Material and equipment:
5.3.1.1.1
Glassware
(according to requirement).
5.3.1.1.2
Dilute
nitric acid.
5.3.1.1.3
Purified
water.
5.3.1.1.4
0.4ml
of Silver nitrate R1.
5.3.1.1.5
Ammonia.
5.3.1.2 Sample:
5.3.1.2.1
Quantity
of substance to be examined equivalent to about 2.0mg of chloride.
5.3.1.3 Method:
5.3.1.3.1
Take
a test tube add in it 2.0ml of water with the help of pipette.
5.3.1.3.2
Dissolve
in 2.0ml of water a quantity of the substance to be equivalent to about 2.0mg
of chloride.
5.3.1.3.3
Acidify
with dilute nitric acid.
5.3.1.3.4
And
add 0.4ml of silver nitrate R1.
5.3.1.3.5
Shake
and allow it to stand.
5.3.1.3.6
A
curdled, white ppt is formed.
5.3.1.3.7
Centrifuge
it in centrifugation machine, according to SOP.
5.3.1.3.8
The
obtained ppt is wash with 3 quantities, each of 1ml, of water.
5.3.1.3.9
Carry
out this operation rapidly is subdued light, degrading the fact that the
supernatant solution may not become perfectly clear.
5.3.1.3.10 Suspend the precipitate in 2.0ml of water
and add 1.5ml of ammonia.
5.3.1.3.11 Observe the changes.
5.3.1.4 Observations:
5.3.1.4.1
The
precipitate dissolves easily with the possible exception of a few large
particles which dissolves slowly.
5.3.2
Ammonium salts test:
5.3.2.1 Material and equipment:
5.3.2.1.1
Glassware
(according to requirement).
5.3.2.1.2
0.2g
of magnesium oxide.
5.3.2.1.3
1.0ml
of 0.1M hydrochloric acid.
5.3.2.1.4
0.05ml
of methyl red solution.
5.3.2.1.5
1.0ml
of freshly prepared 100g/L solution of sodium cobaltnitrite.
5.3.2.2 Sample:
5.3.2.2.1
10.0ml
of solution S.
5.3.2.3 Method of analysis:
5.3.2.3.1
Take
a test tube and add 10.0ml of solution S in it and 0.2mg of magnesium oxide.
5.3.2.3.2
Pass
a current of air through the mixture and direct the gas that escapes just
beneath the surface of a mixture of 1.0ml of 0.1M hydrochloric acid and 0.05ml
of methyl red solution.
5.3.2.3.3
The
colour of the indicator changes to yellow.
5.3.2.3.4
On
addition of 1.0ml of freshly prepared 100g/L solution of sodium cobaltnitrite.
5.3.2.3.5
Observe
the colour change.
5.3.2.4 Observations:
5.3.2.4.1
A
yellow ppt is formed.
5.4 Assay:
5.4.1
Apparatus:
5.4.1.1 Glassware (according to requirement).
5.4.1.2 Titration apparatus.
5.4.1.3 Magnetic stirrer.
5.4.1.4 Water-bath.
5.4.2
Material and reagents:
5.4.2.1 5.0ml of formaldehyde solution.
5.4.2.2 1M sodium hydroxide.
5.4.2.3 Phenolphthalein solution (as indicator).
5.4.2.4 Purified water.
5.4.3
Sample:
5.4.3.1 1.0g.
5.4.4
Method of analysis:
5.4.4.1 Sample titration:
5.4.4.1.1
Take
a flask and add in it 1.0g of sample.
5.4.4.1.2
Dissolve
it in 20.0ml of purified water.
5.4.4.1.3
Add
a mixture of 5.0ml of formaldehyde solution, previously neutralized to
phenolphthalein solution and 20.0ml of purified water.
5.4.4.1.4
Set
titration apparatus.
5.4.4.1.5
After
1-2 min, use further 0.2ml of phenolphthalein solution as indicator.
5.4.4.1.6
Titrate
slowly with 1M sodium hydroxide.
5.4.4.1.7
Note
down the volume used as shown in Annexure-1.
5.4.4.1.8
Take
3 readings at least and take average.
5.4.4.2 Blank titration:
5.4.4.2.1
Take
a flask and add in it 20.0ml of purified water.
5.4.4.2.2
Add
a mixture of 5.0ml of formaldehyde solution, previously neutralized to
phenolphthalein solution and 20.0ml of purified water.
5.4.4.2.3
Set
titration apparatus.
5.4.4.2.4
After
1-2 min, use further 0.2ml of phenolphthalein solution as indicator.
5.4.4.2.5
Titrate
slowly with 1M sodium hydroxide.
5.4.4.2.6
Note
down the volume used as shown in Annexure-1.
5.4.4.2.7
Take
3 readings at least and take average.
5.4.4.3 Calculate percentage purity.
5.4.4.4 Calculations:
5.4.4.4.1
After
taking average volume of both blank titration and sample titration. Calculate
the volume used by the examined substance by using formula:
Volume
used by substance = Blank titration - Sample titration.
5.4.4.4.2
For
percentage purity use formula:
%age
purity = volume used by substance x factor x 100
Weight of sample
5.4.4.4.3
Put
values and calculate %age purity.
5.4.5
Factor:
5.4.5.1 1ml of 1M Sodium hydroxide is equivalent
to 53.49mg of NH4Cl.
5.4.6
Limit:
5.4.6.1 99.0% to 100.5% (dried substance).
6.0 REVISION
LOG:
Revision No.
|
Effective Date
|
Reason
|
00
|
New
SOP
|
7.0 REFERENCES:
7.1 The British Pharmacopoeia. Vol I., Official Monograph /Ammonium
chloride: 2015, pp. 159.
7.2 The British Pharmacopoeia. Vol V., Official Monograph /Qualitative
Reactions and Tests: 2015, pp. 266-270.
8.0 ANNEXURES:
Annexure 1: Observations
and calculations of assay of Ammonium chloride.
Annexure:
1
Observations
and calculations
Indicator:
___________________
Weight
of sample: ____________
Factor: _____________
Titrant:
_____________________
Sample titration
Sr.#
|
Initial volume (vi)
(ml)
|
Final volume (vf)
(ml)
|
vf-vi
(ml)
|
1.
|
|||
2.
|
|||
3.
|
Average volume: _________________
Blank titration
Sr.#
|
Initial volume (vi)
(ml)
|
Final volume (vf)
(ml)
|
vf-vi
(ml)
|
1.
|
|||
2.
|
|||
3.
|
Average volume: _________________
Calculations:
Volume used by substance
= Blank titration - Sample titration.
%age purity = volume
used by substance x factor x 100
Weight of sample
Result:
____________________________________________________________________
9.0 ABBREVIATIONS:
Abbreviation
|
Expanded Form
|
SOP
|
Standard
operating procedure
|
&
|
And
|
No.
|
Number
|
Ltd.
|
Limited
|
Sr.#
|
Serial
number
|
Q.C
|
Quality
control
|
%
|
Percentage
|
B.P
|
British
pharmacopoeia
|
g
|
Grams
|
ml
|
Milliliter
|
Min
|
Minutes
|
ppt
|
Precipitates
|
oC
|
Degree
centigrade
|
mg
|
Milligram
|
M
|
Molar
|
Vol
|
Volume
|
vi
|
Initial
volume
|
vf
|
Final
volume
|
QCA
|
Quality
control active ingredient
|
F
|
Format
|
g/L
|
Gran
per liter
|
R
|
Reagent
|