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POTASSIUM CITRATE METHOD OF ANALYSIS SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Potassium citrate 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, granular powder or translucent crystals.
5.1.1.2  Hygroscopic.
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 1containing with purified water is very soluble.
5.1.2.4.2        The sample in test tube 2 containing with Ethanol (96%) is practically insoluble.
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  Magnetic stirrer.
5.2.1.4  Carbon-dioxide free water.
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 sufficient quantity of carbon-dioxide free water prepared from distilled water.
5.2.3.3  Dilute it to 100.0ml with the same solvent.
5.3  Identification tests:
5.3.1        Citrates test:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (test tube, spatula, beaker, glass rod).
5.3.1.1.2        Analytical weighing balance.
5.3.1.1.3        Water-bath.
5.3.1.1.4        Sulfuric acid.
5.3.1.1.5        1.0ml of potassium permanganate solution.
5.3.1.1.6        0.5ml of a 100g/L solution of sodium nitroprusside.
5.3.1.1.7        4g of sulfamic acid.
5.3.1.1.8        Excess of concentrated ammonia.
5.3.1.1.9        Purified water.
5.3.1.2  Sample:
5.3.1.2.1        1.0ml of solution S.
5.3.1.3  Method:
5.3.1.3.1        Take a test tube and add 1.0ml of solution S.
5.3.1.3.2        And add 4.0ml of purified water in it.
5.3.1.3.3        To this 5.0ml of prescribed solution
5.3.1.3.4        Add 0.5ml of sulfuric acid and 1.0ml of potassium permanganate solution.
5.3.1.3.5        Warm it on water-bath until the colour of the permanganate is discharged.
5.3.1.3.6        Add 0.5ml of a 100g/L solution of sodium nitroprusside in dilute sulfuric acid and 4g of sulfamic acid.
5.3.1.3.7        Make alkaline with concentrate ammonia, added drop-wise until all the sulfamic acid has dissolved.
5.3.1.3.8        Add excess of concentrated ammonia and observe the changes.
5.3.1.4  Observations:
5.3.1.4.1        A violet colour is produced which turn to violet-blue.
5.3.2        Potassium test:
5.3.2.1  Material and equipment:
5.3.2.1.1        Glassware (1 test tube, 1 pipette, 1 spatula).
5.3.2.1.2        1.0ml of dilute acetic acid.
5.3.2.1.3        1.0ml of a freshly prepared 100g/L solution of sodium cobaltnitrite.
5.3.2.2  Sample:
5.3.2.2.1        0.5ml of solution S.
5.3.2.3  Method:
5.3.2.3.1        Take a test tube and add 0.5ml of solution S.
5.3.2.3.2        Add 1.0ml of dilute acetic acid and 1.0ml of a freshly prepared 100g/L solution of sodium cobaltnitrite.
5.3.2.3.3        Observe the changes.
5.3.2.4  Observations:
5.3.2.4.1        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  20.0ml of anhydrous acetic acid.
5.4.2.2  0.1M Perchloric acid.
5.4.2.3  0.25ml of naphtholbenzein solution as an indicator.
5.4.3        Sample:
5.4.3.1  0.150g.
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 0.150g of sample.
5.4.4.1.2        Dissolve it in 20.0ml of anhydrous acetic acid, and heat to about 50oC on water-bath.
5.4.4.1.3        Allow it to cool.
5.4.4.1.4        Set titration apparatus.
5.4.4.1.5        Use 0.25ml of naphtholbenzein solution as an indicator.
5.4.4.1.6        Titrate with 0.1M Perchloric acid, until a green colour is obtained.
5.4.4.1.7        Note down the volume used as shown in Annexure-1.
5.4.4.1.8        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 20.0ml of anhydrous acetic acid, and heat to about 50oC on water-bath.
5.4.4.2.2        Allow it to cool.
5.4.4.2.3        Set titration apparatus.
5.4.4.2.4        Use 0.25ml of naphtholbenzein solution as an indicator.
5.4.4.2.5        Titrate with 0.1M Perchloric acid, until a green colour is obtained.
5.4.4.2.6        Note down the volume used as shown in Annexure-1.
5.4.4.2.7        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 0.1M Perchloric acid is equivalent to 10.21mg of potassium citrate C6H5K3O7.
5.4.6        Limit:
5.4.6.1  99.0% to 101.0% (anhydrous substance).
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 citrate: 2015, pp. 622-623.
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.


                                                              Annexure: 1
Assay observations and calculations
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
%
Percentage
g
Grams
ml
Milliliter
M
Molar
g/L
Grams per liter
mg
Milligram
vi
Initial volume
vf
Final volume
B.P
British pharmacopoeia
oC
Degree centigrade


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