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
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
QCA
Quality control active ingredient
F
Format
Q.C
Quality control
Vol
Volume


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