SODIUM BICARBONATE METHOD OF ANALYSIS SOP
1.0 OBJECTIVE:
To
lay down a procedure of analytical report for the active raw material of the Sodium bicarbonate 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, crystalline powder.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (2 test
tubes, 1 spatula).
5.1.2.1.2
Ethanol (96%).
5.1.2.1.3
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 2 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.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 containing with water is soluble.
5.1.2.4.2
The sample in test
tube 2 containing with ethanol (96%) is practically insoluble.
5.1.2.4.3
When heated in the
dry state or in solution, it gradually changes into sodium carbonate.
5.2 Solution S
preparation:
5.2.1
Material and equipment:
5.2.1.1
Glassware (1
beaker, spatula).
5.2.1.2
Analytical
weighing balance.
5.2.1.3
Carbon dioxide-free
water (q.s).
5.2.2
Sample:
5.2.2.1
5.0g
5.2.3
Method:
5.2.3.1
Take a beaker of
100.0ml and add 5.0g of the sample in it.
5.2.3.2
And dissolve it in
90.0ml of carbon dioxide-free water.
5.2.3.3
Dilute it to
100.0ml with the same solvent.
5.3 Identification
tests:
5.3.1
5.3.1.1
Material and equipment:
5.3.1.1.1
Glassware
(according to requirement).
5.3.1.1.2
0.1ml of phenolphthalein
solution.
5.3.1.2
Sample:
5.3.1.2.1
5.0ml of solution
S.
5.3.1.3
Method:
5.3.1.3.1
Take a beaker and
add 5.0ml of solution S in it.
5.3.1.3.2
And add 0.1ml of
phenolphthalein solution.
5.3.1.3.3
Observe the
changes.
5.3.1.3.4
Heat it on burner.
5.3.1.3.5
Again observe
changes.
5.3.1.4
Observations:
5.3.1.4.1
A pale pink colour
is produced but upon heating gas is evolved and the solution becomes red.
5.3.2
Carbonates/
bicarbonates test:
5.3.2.1
Material and equipment:
5.3.2.1.1
Glassware (test
tubes, beakers, spatula, stirrer & stoppers of test tube).
5.3.2.1.2
Magnetic stirrer.
5.3.2.1.3
3.0ml of 2M acetic
acid.
5.3.2.1.4
5.0ml of 4.73% w/v
solution of barium chloride.
5.3.2.1.5
Excess of 7M
hydrochloric acid.
5.3.2.1.6
Magnesium sulfate.
5.3.2.1.7
Purified water
(q.s).
|
Test no.
|
Sample
|
Method
|
Observation
|
|
1.
|
0.1g
|
Take a
test tube and add 0.1g of sample in it. Dissolve in 2.0ml of purified water.
Add 3.0ml
of 2M acetic acid in another test tube.
Close
the test tube immediately using a stopper fitted with a glass tube bent at
two right angles.
The suspension
produces effervesce.
Heat
it gently on burner & collect gas in 5.0ml of 4.73% w/v solution of barium
chloride which is in another test tube taken.
Observe
change in colour and appearance of suspension after addition of an excess of
7M hydrochloric acid.
|
A
white ppt is produced which dissolves on addition of an excess of 7M
hydrochloric acid.
|
|
2.
|
Solution S
|
Take a
test tube and add solution S in it.
Add in
it solution of magnesium sulfate.
Observe
changes.
Boil
it on burner.
Observe
changes again.
|
No ppt
produced indicates presence of bicarbonate. When heated or boiled white ppt
is produced.
|
|
3.
|
Solution S
|
Take a
test tube and add solution S in it.
Boiled
it on burner.
Observe
changes.
|
Liberation
of CO2.
|
5.3.3
Sodium
test:
5.3.3.1
Material and equipment:
5.3.3.1.1
Glassware (test
tube, spatula, beaker, glass rod).
5.3.3.1.2
Analytical
weighing balance.
5.3.3.1.3
Burner.
5.3.3.1.4
2.0ml of 150g/L
solution of potassium carbonate.
5.3.3.1.5
4.0ml of potassium
pyroantimonate solution.
5.3.3.1.6
Iced water.
5.3.3.1.7
Purified water.
5.3.3.2
Sample:
5.3.3.2.1
2.0ml of solution
S.
5.3.3.3
Method:
5.3.3.3.1
Take a test tube
and add 2.0ml of solution S.
5.3.3.3.2
Add 2.0ml of
150g/L solution of potassium carbonate and heat it to boiling on burner.
5.3.3.3.3
Observe the
changes.
5.3.3.3.4
No ppt is formed.
5.3.3.3.5
Add 4.0ml of
potassium pyroantimonate solution again heat it to boiling on burner.
5.3.3.3.6
And then take a
beaker of filled with iced water, put test tube in it and allow it to cool.
5.3.3.3.7
If necessary rub
the inside of the test tube with a glass rod.
5.3.3.3.8
Observe the
changes.
5.3.3.4
Observations:
5.3.3.4.1
A dense white ppt
is formed.
5.4 Assay:
5.4.1
Apparatus:
5.4.1.1
Glassware (according
to requirement).
5.4.1.2
Titration
apparatus.
5.4.2
Material
and reagents:
5.4.2.1
50.0ml of carbon
dioxide-free water.
5.4.2.2
1M hydrochloric
acid.
5.4.2.3
0.2ml of methyl
orange solution as an indicator.
5.4.3
Sample:
5.4.3.1 1.5g
5.4.4
Method
of analysis:
5.4.4.1 Sample
titration:
5.4.4.1.1
Take a titration flask
and add in it 1.5g of sample.
5.4.4.1.2
Dissolve it in 50.0ml
of carbon dioxide-free water.
5.4.4.1.3
Set titration
apparatus.
5.4.4.1.4
Use 0.2ml of methyl
orange solution as indicator.
5.4.4.1.5
Titrate with 1M
hydrochloric acid.
5.4.4.1.6
Note down the volume
used as shown in Annexure-1.
5.4.4.1.7
And take average.
5.4.4.2 Blank
titration:
5.4.4.2.1
Take a titration
flask and add in it 50.0ml of carbon dioxide-free water.
5.4.4.2.2
Set titration
apparatus.
5.4.4.2.3
Use 0.2ml of methyl
orange solution as indicator.
5.4.4.2.4
Titrate with 1M
hydrochloric acid.
5.4.4.2.5
Note down the
volume used as shown in Annexure-1.
5.4.4.2.6
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 0.1M hydrochloric acid is equivalent to 84mg of NaHCO3.
5.4.6
Limit:
5.4.6.1
99.0% to 101.0%.
6.0 REVISION LOG:
|
Revision No.
|
Effective Date
|
Reason
|
|
00
|
|
New SOP
|
7.0 REFERENCES:
7.1
The British
Pharmacopoeia. Vol II.,
Official Monograph / Sodium bicarbonate: 2015, pp. 825.
8.0 ANNEXURES:
Annexure 1: Assay
observations and calculations (Acid-base titration).
Annexure:
1
Assay
observations and calculations (Acid-base titration)
|
Acid-base titration
Indicator: ___________________
Weight of sample: ____________
Factor: 84mg.
Titrant: _____________________
Sample
titration
Average volume: _________________
Blank
titration
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
|
|
q.s
|
Quantity
sufficient
|
|
g
|
Grams
|
|
ml
|
Milliliter
|
|
w/v
|
Weight
per volume
|
|
M
|
Molar
|
|
g/L
|
Grams
per liter
|
|
mg
|
Milligram
|
|
vi
|
Initial
volume
|
|
vf
|
Final
volume
|
|
B.P
|
British
pharmacopoeia
|
|
Vol
|
Volume
|
|
QCA
|
Quality
control active ingredient
|
|
F
|
Format
|