POTASSIUM BICARBONATE METHOD
OF ANALYSIS SOP
1.0 OBJECTIVE:
To
lay down a procedure for the active raw material of the Potassium bicarbonate from the
Pharmacopoeial specifications.
2.0 SCOPE:
This
SOP shall be applicable in Q.C laboratory.
3.0 RESPONSIBILITY:
3.1
Q.C Analyst.
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
or colourless.
5.1.2
Solubility:
5.1.2.1
Material and equipment:
5.1.2.1.1
Glassware (2 test
tubes, 1 spatula, 1 pipette).
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.
5.1.2.3.4
When heating the
both solution on burner. Observe changes too.
5.1.2.4
Observations:
5.1.2.4.1
The sample in test
tube 1 containing with purified water is freely 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 is gradually converted to potassium carbonate.
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
Analytical
weighing balance.
5.2.1.3
Water bath.
5.2.1.4
Magnetic stirrer.
5.2.1.5
Carbon-dioxide
free water.
5.2.2
Sample:
5.2.2.1
5.0g.
5.2.3
Preparation of solution
S:
5.2.3.1
Take a beaker of
100.0ml and add sample 5.0g of sample.
5.2.3.2
Add in it 90.0ml
of carbon-dioxide free water prepare from distilled water.
5.2.3.3
Dilute it to
100.0ml with 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 dilute acetic
acid.
5.3.2.1.4
5.0ml of barium
hydroxide solution.
5.3.2.1.5
Excess of
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 dilute 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 solution
or suspension produces effervescent and gives off a colourless and odorless
gas.
Heat
it gently on burner & collect gas in 5.0ml of barium hydroxide solution which
is in another test tube taken.
Observe
change in colour and appearance after addition of an excess of hydrochloric
acid.
|
A
white ppt is formed which dissolves on addition of an excess of hydrochloric
acid.
|
5.3.3
Potassium
test:
5.3.3.1
Material and equipment:
5.3.3.1.1
Glassware (1 test
tube, 1 pipette, 1 spatula).
5.3.3.1.2
1.0ml of dilute
acetic acid.
5.3.3.1.3
1.0ml of a freshly
prepared 100g/L solution of sodium cobalt nitrite.
5.3.3.2
Sample:
5.3.3.2.1
1.0ml of solution
S.
5.3.3.3
Method:
5.3.3.3.1
Take a test tube
and add 1.0ml of solution S.
5.3.3.3.2
Add 1.0ml of
dilute acetic acid and 1.0ml of a freshly prepared 100g/L solution of sodium
cobaltnitrite.
5.3.3.3.3
Observe the
changes.
5.3.3.4
Observations:
5.3.3.4.1
A yellow or
orange-yellow ppt is formed immediately.
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
Water-bath.
5.4.2
Material
and reagents:
5.4.2.1
50.0ml of carbon
dioxide-free water.
5.4.2.2
1.0M hydrochloric
acid.
5.4.2.3
0.1ml of methyl
orange solution as an indicator.
5.4.3
Sample:
5.4.3.1 0.8g
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 0.8g 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 0.1ml of methyl
orange solution as indicator.
5.4.4.1.5
Titrate with 1.0M
hydrochloric acid, until the yellow colour begins to change to yellowish-pink.
5.4.4.1.6
Heat cautiously
and boil for at least 2min on water-bath.
5.4.4.1.7
Observe the
changes.
5.4.4.1.8
The solution
becomes yellow.
5.4.4.1.9
Cool it and
titrate again until a yellowish-red colour is obtained.
5.4.4.1.10 Note
down the volume used as shown in Annexure-1.
5.4.4.1.11 Take
at least 3 readings 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 0.1ml of methyl
orange solution as indicator.
5.4.4.2.4
Titrate with 1.0M
hydrochloric acid, until the yellow colour begins to change to yellowish-pink.
5.4.4.2.5
Heat cautiously
and boil for at least 2min on water-bath.
5.4.4.2.6
Observe the
changes.
5.4.4.2.7
The solution
becomes yellow.
5.4.4.2.8
Cool it and
titrate again until a yellowish-red colour is obtained.
5.4.4.2.9
Note down the
volume used as shown in Annexure-1.
5.4.4.2.10 Take
at least 3 readings 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 1.0M hydrochloric acid is equivalent to 0.1001g of potassium KHCO3.
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 /Potassium bicarbonate: 2015, pp. 619.
7.2
The British
Pharmacopoeia. Vol V.,
Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
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: ____________
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
|
|
QCA
|
Quality
control active ingredient
|
|
F
|
Format
|
|
Q.C
|
Quality
control
|
|
Vol
|
Volume
|