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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
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
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


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