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SULPHUR METHOD OF ANALYSIS SOP

1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Sulphur from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analysts.
3.2  Q.C Manager.
4.0  ACCOUNTABILITY:
4.1  Q.C Manager.
5.0  PROCEDURE:
5.1  Characters:
5.1.1        Appearance:
5.1.1.1  Yellow powder.
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        Purified water.
5.1.2.1.3        Carbon disulfide.
5.1.2.1.4        Vegetable oils.
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 carbon disulfide in test tube 2 and observe.
5.1.2.3.4        Add vegetable oils 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 practically insoluble.
5.1.2.4.2        The sample in test tubes 2 containing with carbon disulfide is soluble.
5.1.2.4.3        The sample in test tubes 3 containing with vegetable oils is slightly soluble.
5.2  Identification tests:
5.2.1         
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (stirrer, spatula).
5.2.1.1.2        Bunsen burner.
5.2.1.1.3        Purified water.
5.2.1.1.4        Blue litmus paper.
5.2.1.2  Sample:
5.2.1.2.1        Small quantity.
5.2.1.3  Method of analysis:
5.2.1.3.1        Take a small quantity of substance to be examined on the edge of the stirrer.
5.2.1.3.2        Heat it in the presence of air.
5.2.1.3.3        Observe the change in flame colour.
5.2.1.3.4        Expose off the emitting vapours to moisten blue litmus paper and observe changes.
5.2.1.4  Observations:
5.2.1.4.1        A blue colour flame is produced with the emitting sulphur dioxide.
5.2.1.4.2        On exposure of emitting sulphur to blue litmus paper it will turn into red.
5.2.2         
5.2.2.1  Material and equipment:
5.2.2.1.1        Glassware (according to requirement).
5.2.2.1.2        Filter paper.
5.2.2.1.3        Bunsen burner.
5.2.2.1.4        Bromine water.
5.2.2.1.5        Dilute hydrochloric acid.
5.2.2.1.6        Barium chloride solution.
5.2.2.1.7        Purified water.
5.2.2.2  Sample:
5.2.2.2.1        0.1g.
5.2.2.3  Method of analysis:
5.2.2.3.1        Take a test tube and add in it 0.1g of sample.
5.2.2.3.2        Add 0.5ml of bromine water with the help of pipette.
5.2.2.3.3        Heat it until decolorized.
5.2.2.3.4        Add 5ml of water.
5.2.2.3.5        Filter it.
5.2.2.3.6        Take 5.0ml of the filtrate in a test tube with the help of pipette.
5.2.2.3.7         Add 1.0ml of the dilute hydrochloric acid and 1.0ml of barium chloride solution.
5.2.2.3.8        Observe the changes.
5.2.2.4  Observations:
5.2.2.4.1        A white ppt is formed.
5.3   Assay:
5.3.1        Apparatus:
5.3.1.1  Oxygen-flask combustion apparatus.
5.3.1.2  Titration apparatus.
5.3.1.3  Match stick box.
5.3.1.4  Bunsen burner.
5.3.2        Material and reagents:
5.3.2.1  Dilute hydrogen peroxide.
5.3.2.2  Phenolphthalein solution (as indicator).
5.3.2.3  0.1M sodium hydroxide.
5.3.2.4  Purified water.
5.3.3        Sample:
5.3.3.1  60.0mg.
5.3.4        Method of analysis:
5.3.4.1  Test solution:
5.3.4.1.1        Firstly clean up the oxygen-flask combustion apparatus.
5.3.4.1.2        Weigh 60.0mg of the sample and finely grind the substance to be examined.
5.3.4.1.3        Place it into the center of the piece of the filter paper and measuring about 30mm by 40mm provided with a small strip about 10mm wide and 30mm long.
5.3.4.1.4        The enveloped substance place into the sample carrier e.g. platinum or platinum-iridium.
5.3.4.1.5        In combustion flask add 5.0ml of dilute hydrogen peroxide and 10.0ml of water.
5.3.4.1.6        And also combustion product, displace the air with oxygen by means of a tube having its end just above the liquid.
5.3.4.1.7        Moisten the neck of the flask with water.
5.3.4.1.8        Ignite the paper strip by suitable means with the usual precautions.
5.3.4.1.9        Immediately transfer it to the flask.
5.3.4.1.10    Keep the flask airtight until the combustion is completed.
5.3.4.1.11    After combustion is completed, shake the flask vigorously to completely dissolve the combustion products.
5.3.4.1.12    Cool it.
5.3.4.1.13    After about 5 minutes, carefully unstopper the flask.
5.3.4.1.14    Wash the ground parts and the walls of the flask, as well as the sample carrier with water.
5.3.4.1.15    Combine the combustion products and the washings in a separate beaker.
5.3.4.1.16    Heat to boiling, boil gently for 2 min and cool it (test solution).
5.3.4.1.17    Set the apparatus of titration and perform according to SOP.
5.3.4.1.18    Use 0.2ml of phenolphthalein solution as indicator.
5.3.4.1.19    Titrate the test solution with 0.1M sodium hydroxide until the colour changes from colourless to red.
5.3.4.1.20    Note readings in Annexur-1.
5.3.4.2  Blank solution:
5.3.4.2.1        Firstly clean up the oxygen-flask combustion apparatus.
5.3.4.2.2        In combustion flask add 5.0ml of dilute hydrogen peroxide and 10.0ml of water.
5.3.4.2.3        And also combustion product, displace the air with oxygen by means of a tube having its end just above the liquid.
5.3.4.2.4        Moisten the neck of the flask with water.
5.3.4.2.5        Ignite the paper strip by suitable means with the usual precautions.
5.3.4.2.6        Immediately transfer it to the flask.
5.3.4.2.7        Keep the flask airtight until the combustion is completed.
5.3.4.2.8        After combustion is completed, shake the flask vigorously to completely dissolve the combustion products.
5.3.4.2.9        Cool it.
5.3.4.2.10    After about 5 minutes, carefully unstopper the flask.
5.3.4.2.11    Wash the ground parts and the walls of the flask, as well as the sample carrier with water.
5.3.4.2.12    Combine the combustion products and the washings in a separate beaker.
5.3.4.2.13    Heat to boiling, boil gently for 2 min and cool it (test solution).
5.3.4.2.14    Set the apparatus of titration and perform according to SOP.
5.3.4.2.15    Use 0.2ml of phenolphthalein solution as indicator.
5.3.4.2.16    Titrate the test solution with 0.1M sodium hydroxide until the colour changes from colourless to red.
5.3.4.3  Note down the sample solution titration and blank solution titration readings in Annexures-1.
5.3.4.4  Apply the factor and calculate the percentage content.
Volume used by substance = Blank titration - Sample titration.
%age purity = volume used by substance x factor x 100
                                                           Weight of sample
5.3.5        Factor:
5.3.5.1  1ml of 0.1M Sodium hydroxide is equivalent to 1.603mg of S.
5.3.6        Limit:
5.3.6.1  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 /Sulfur for External use: 2015, pp. 953-954.
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
Q.C
Quality control
B.P
British pharmacopoeia
g
Grams
ml
Milliliter
ppt
Precipitate
M
Molar
mg
Milligram
mm
Millimeter
min
Min
S
Sulphur
%
Percentage
Vol
Volume
QCA
Quality control active ingredient
F
Format


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