POTASSIUM CHLORIDE METHOD OF ANALYSIS SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Potassium chloride 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.
5.1.1.3  Colourless crystals.
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        Anhydrous ethanol.
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 anhydrous ethanol 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 freely soluble.
5.1.2.4.2        The sample in test tube 2 containing with anhydrous ethanol 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        Chlorides 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        Centrifugation machine.
5.3.1.1.3        Dilute nitric acid.
5.3.1.1.4        Purified water.
5.3.1.1.5        0.4ml of Silver nitrate R1.
5.3.1.1.6        Ammonia.
5.3.1.2  Sample:
5.3.1.2.1        Quantity of substance to be examined equivalent to about 2.0mg of chloride.
5.3.1.3  Method:
5.3.1.3.1        Take a test tube add in it 2.0ml of water with the help of pipette.
5.3.1.3.2        Dissolve in 2.0ml of water a quantity of the substance to be equivalent to about 2.0mg of chloride.
5.3.1.3.3        Acidify with dilute nitric acid.
5.3.1.3.4        And add 0.4ml of silver nitrate R1.
5.3.1.3.5        Shake and allow it to stand.
5.3.1.3.6        A curdled, white ppt is formed.
5.3.1.3.7        Centrifuge it in centrifugation machine, according to SOP.
5.3.1.3.8        The obtained ppt is wash with 3 quantities, each of 1ml, of water.
5.3.1.3.9        Carry out this operation rapidly is subdued light, degrading the fact that the supernatant solution may not become perfectly clear.
5.3.1.3.10    Suspend the precipitate in 2.0ml of water and add 1.5ml of ammonia
5.3.1.4  Observations:
5.3.1.4.1        The precipitate dissolves easily with the possible exception of a few large particles which dissolves slowly.
5.3.2        Chlorides test:
5.3.2.1  Material and equipment:
5.3.2.1.1        Glassware (test tube, spatula, glass rod).
5.3.2.1.2        0.2g of potassium dichromate R.
5.3.2.1.3        1.0ml of sulfuric acid R.
5.3.2.1.4        Filter paper.
5.3.2.1.5        0.1ml of diphenylcarbazide solution.
5.3.2.2  Sample:
5.3.2.2.1        Quantity of substance to be examined equivalent to about 15.0mg of chloride.
5.3.2.3  Method:
5.3.2.3.1        Take a test tube add in it a quantity of the substance to be equivalent to about 2.0mg of chloride.
5.3.2.3.2        Add 0.2g of potassium dichromate R and 1.0ml of sulfuric acid R.
5.3.2.3.3        Place a filter paper strip impregnated with 0.1ml of diphenylcarbazide solution R over the opening of the test tube.
5.3.2.3.4        Observe the changes.
5.3.2.3.5        The impregnated paper must not come into contact with the potassium dichromate.
5.3.2.4  Observations:
5.3.2.4.1        The paper turns violet-red.
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        Bunsen burner.
5.3.3.1.3        1.0ml of sodium carbonate solution.
5.3.3.1.4        0.05ml of sodium sulfide solution R.
5.3.3.1.5        Iced-water.
5.3.3.1.6        2.0ml of 150g/L solution of tartaric acid R.
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 1.0ml of sodium carbonate solution R and heat it on burner. Observe the changes.
5.3.3.3.3        No ppt is formed.
5.3.3.3.4        Add to the hot solution 0.05ml of sodium sulfide solution R. Observe it again.
5.3.3.3.5        No ppt is formed.
5.3.3.3.6        Cool it in iced-water and add 2.0ml of 150g/L solution of tartaric acid R. Allow it to stand.
5.3.3.3.7        And observe the changes.
5.3.3.4  Observations:
5.3.3.4.1        A white crystalline ppt is formed.
5.3.4        Potassium test:
5.3.4.1  Material and equipment:
5.3.4.1.1        Glassware (1 test tube, 1 pipette, 1 spatula).
5.3.4.1.2        1.0ml of dilute acetic acid.
5.3.4.1.3        1.0ml of a freshly prepared 100g/L solution of sodium cobalt nitrite.
5.3.4.2  Sample:
5.3.4.2.1        1.0ml of Solution S.
5.3.4.3  Method:
5.3.4.3.1        Take a test tube and add 1.0ml of solution S.
5.3.4.3.2        Add 1.0ml of dilute acetic acid and 1.0ml of a freshly prepared 100g/L solution of sodium cobalt nitrite.
5.3.4.3.3        Observe the changes.
5.3.4.4  Observations:
5.3.4.4.1        A yellow or orange-yellow ppt is formed immediately.
5.4  Loss on drying:
5.4.1        Material and equipment:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Analytical weighing balance.
5.4.1.3  Oven.
5.4.2        Sample:
5.4.2.1  1.0g.
5.4.3        Method:
5.4.3.1  Weigh 1.0g of the test sample.
5.4.3.2  Set the oven apparatus. Operate it according to the SOP.
5.4.3.3  Place the sample into the tray and dry it.
5.4.3.4  Set the temperature of oven at 105oC for at least 3 hours.
5.4.3.5  And wait till the sample loses its moisture.
5.4.3.6  After 3 hours weigh the sample again by using analytical weighing balance i.e. the final weight.
5.4.3.7  Note down readings on given Annexure-1.
5.4.4        Observation:
5.4.4.1  Maximum 1.0%.
5.5  Assay:
5.5.1        Apparatus:
5.5.1.1  Glassware (according to requirement).
5.5.1.2  Potentiometer.
5.5.1.3  Magnetic stirrer.
5.5.2        Material and reagents:
5.5.2.1  5.0ml of dilute nitric acid.
5.5.2.2  0.1M silver nitrate.
5.5.2.3  Purified water.
5.5.3        Sample:
5.5.3.1  60.0mg.
5.5.4        Method of analysis:
5.5.4.1  Take a 50.0ml of beaker and add 60.0mg of sample in it.
5.5.4.2  Dissolve it in sufficient quantity of purified water by using magnetic stirrer.
5.5.4.3  Add 5.0ml of dilute nitric acid and dilute it to 50.0ml with purified water.
5.5.4.4  Fill the right hand side burette with titrant 0.1M silver nitrate.
5.5.4.5  Carry out a Potentiometric titration.
5.5.4.6  Operate potentiometer according to SOP.
5.5.4.7  To neutralize analyte add titrant fixed volume (1ml, 0.5ml or 0.1ml) from burette every time note the reading of change in potential difference (millivolts) for each addition in given annexure-2.
5.5.4.8  Plot a graph, volume used v/s millivolts.
5.5.4.9  Find out the END POINT.
5.5.4.10    Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.5.4.11    Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-2.
5.5.4.12    Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.5.4.13    Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
Weight of sample
5.5.5        Factor:
5.5.5.1  1ml of 0.1M silver nitrate is equivalent to 7.46mg of potassium chloride KCl.
5.5.6        Limit:
5.5.6.1  99.0% to 101.0% (dried 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 chloride: 2015, pp. 621-622.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Observations of Percentage Loss of drying by using oven.
Annexure 2: Assay observations and calculations (Potentiometric titration).


Annexure: 1
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using Oven
Weight of Sample = _____________
Time period = _____________
Pressure= _________________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:










Remarks: _______________________________________________________________



Annexure: 2
Assay observations and calculations (Potentiometric titration)
Potentiometric titration
Reference electrode: ___________________
Indicator electrode: ____________________
Speed of magnetic stirrer: _______________
Titrant used: __________________________
Indicator: ____________________________
Blank titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












Plot a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT of blank titration.
Sample titration:
Sr.#
Volume used
(ml)
Voltmeter
(mV)












Plot a graph, volume used v/s millivolts and find out peak of graph i.e. END POINT of sample titration:
Volume used by Blank titration: __________________
Volume used by Sample titration: _________________
Volume used by substance = Blank titration - Sample titration.


mV used by Blank titration: __________________
mV used by Sample titration: _________________
mV used by substance = Blank titration - Sample titration.

Volume used by substance: _______________________
Voltmeter (mV) used by substance: _________________












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
B.P
British pharmacopoeia
oC
Degree centigrade
R
Reagent
v/s
Verses
mV
Millivolts
H
Hours


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