SALICYLIC ACID METHOD OF ANALYSIS SOP


1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Salicylic acid 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.
5.1.1.2  White or colourless, acicular crystals.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (test tubes, spatula).
5.1.2.1.2        Ethanol (96%).
5.1.2.1.3        Methylene chloride.
5.1.2.1.4        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 3 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        Add methylene chloride in test tube 3 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with water is slightly soluble.
5.1.2.4.2        The sample in test tube 2 containing with ethanol (96%) is freely soluble.
5.1.2.4.3        The sample in test tube 3 containing with methylene chloride is sparingly soluble.
5.2  Identification tests:
5.2.1        Melting point:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (test tubes, spatula).
5.2.1.1.2        Melting point apparatus.
5.2.1.1.3        Capillary tubes.
5.2.1.2  Sample:
5.2.1.2.1        Small quantity.
5.2.1.3  Method:
5.2.1.3.1        Introduce the sufficient quantity of sample into a capillary tube.
5.2.1.3.2        Set the apparatus and immerse the capillary tube into the apparatus such that the closed end is near the centre of the bulb of thermometer.
5.2.1.3.3        Switch on the melting point apparatus.
5.2.1.3.4        Operate the melting point apparatus according to the SOP
5.2.1.3.5        Raise the temperature of the apparatus.
5.2.1.3.6        Record the temperature at which the last particle passes into the liquid phase.
5.2.1.3.7        Record measurements in annexure-1.
5.2.1.4  Observations:
5.2.1.4.1        The melting point of salicylic acid is about 158oC to 161oC.
5.2.2        Salicylates test:
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        5.0ml of 0.05M sodium hydroxide.
5.2.2.1.3        0.5ml of ferric chloride solution.
5.2.2.1.4        0.1ml of acetic acid.
5.2.2.1.5        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        30.0mg.
5.2.2.3  Method:
5.2.2.3.1        Take a beaker and add 30.0mg of sample in it.
5.2.2.3.2        Dissolve it in 5.0ml of 0.05M sodium hydroxide neutralize it if necessary.
5.2.2.3.3        And dilute it to 20.0ml with purified water.
5.2.2.3.4        Take 1.0ml of this solution in a test tube.
5.2.2.3.5        Add 0.5ml of ferric chloride solution.
5.2.2.3.6        Observe changes (violet colour produced).
5.2.2.3.7        Add 0.1ml of acetic acid
5.2.2.3.8        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        A violet colour is produced that persist after the addition of 0.1ml of acetic acid.
5.3  Loss on drying:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (according to requirement).
5.3.1.1.2        Desiccator.
5.3.1.1.3        Diphosphorous pentaoxide.
5.3.1.1.4        Analytical weighing balance.
5.3.1.1.5        Spatula.
5.3.1.2  Sample:
5.3.1.2.1        1.0g.
5.3.1.3  Method:
5.3.1.3.1        Weigh 1g of the test sample.
5.3.1.3.2        Set the desiccator apparatus with desicant.
5.3.1.3.3        Operate the desiccator according to the SOP.
5.3.1.3.4        Place the sample into the china dish or petri dish.
5.3.1.3.5        Set the room temperature and at atmospheric pressure for at least 45 minutes.
5.3.1.3.6        And wait till the sample loses its moisture.
5.3.1.3.7        After 45 minutes weigh the sample again by using analytical weighing balance i.e. the final weight.
5.3.1.3.8        Note down readings on given Annexure-2.
5.3.1.4  Observations:
5.3.1.4.1        Maximum 0.1%.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Potentiometer.
5.4.2        Material and reagents:
5.4.2.1  30.0ml of ethanol (96%).
5.4.2.2  0.1M sodium hydroxide.
5.4.2.3  0.1ml of phenol red solution.
5.4.2.4  20.0ml of purified water.
5.4.3        Sample:
5.4.3.1  0.120g.
5.4.4        Method of analysis:
5.4.4.1  Take a 50.0ml of beaker and take 0.120g of sample in it.
5.4.4.2  Add 30.0ml of ethanol (96%) and 20.0ml of purified water in it and dissolve properly.
5.4.4.3  Fill the right hand side burette with titrant 0.1M sodium hydroxide.
5.4.4.4  Carry out a Potentiometric titration using 0.1ml of phenol red solution as an indicator.
5.4.4.5  Operate potentiometer according to SOP
5.4.4.6  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-1.
5.4.4.7  Plot a graph, volume used v/s millivolts.
5.4.4.8  Find out the END POINT.
5.4.4.9  Peak of graph indicates END POINT i.e. the point at which maximum millivolts. Note down volume used at that point.
5.4.4.10 Perform blank titration without using sample. Similarly, as sample titration performed. Record observations in annexure-1.
5.4.4.11 Calculate volume used by substance by using formula:
Volume used by substance = Blank titration - Sample titration.
5.4.4.12 Calculate percentage purity of the sample by using formula:
%age purity = volume used by substance x factor x 100
                          Weight of sample
5.4.5        Factor:
5.4.5.1  1ml of 0.1M Sodium hydroxide is equivalent to 31.81mg of C7H6O3.
5.4.6        Limit:
5.4.6.1  99.0% to 100.5% (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 / Salicylic acid: 2015, pp. 784-785.
8.0  ANNEXURES:
Annexure 1: Observations of Melting point apparatus.
Annexure 2: Observations of percentage loss of drying.
Annexure 3: Assay observations and calculations (Potentiometric titration)





                                                        Annexure: 1
Observations of Melting point apparatus
Melting point apparatus
Sample = _____________
Time period = _____________
Sr.#
Initial (Ti)
(oC)
Final (Tf)
(oC)
Tf - Ti
(oC)












Average: _____________

Result: _________________












Remarks: ____________________________________________________________ _____________________________________________________________________


Annexure: 2
Observations of percentage loss of drying
Percentage loss of drying
Apparatus: ____________________
Temperature: __________________
Pressure: _____________________
Weight of Sample = _____________
Time period = _____________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:











Remarks: ____________________________________________________________

Annexure: 3
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
Sr.#
Serial number
Q.C
Quality control
%
Percentage
B.P
British pharmacopoeia
g/L
Grams per liter
mg
Milligram
Min
Minutes
ml
Milligram
oC
Degree centigrade
g
Grams
M
Molar
Vol
Volume
QCA
Quality control active ingredient
F
Format
mV
Millivolts
Ti
Initial temperature
Tf
Final temperature



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