AMMONIUM CHLORIDE SOP


AMMONIUM CHLORIDE SOP

1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Ammonium chloride 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.
5.1.1.2  Crystalline powder.
5.1.1.3  Colourless.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (1 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2        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 a test tube and add small quantity of sample for testing solubility according to B.P specifications.
5.1.2.3.2        Add purified water in it and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube containing with water is freely soluble.
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  Carbon-dioxide free water.
5.2.1.3  Analytical weighing balance.
5.2.1.4  Magnetic stirrer.
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 carbon-dioxide free water which is prepared from distilled water.
5.2.3.3  Dissolve it by using magnetic stirrer.
5.2.3.4  Dilute it to 100.0ml with same solvent.
5.3  Identification tests:
5.3.1        Chlorides test:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (according to requirement).
5.3.1.1.2        Dilute nitric acid.
5.3.1.1.3        Purified water.
5.3.1.1.4        0.4ml of Silver nitrate R1.
5.3.1.1.5        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.
5.3.1.3.11    Observe the changes.
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        Ammonium salts test:
5.3.2.1  Material and equipment:
5.3.2.1.1        Glassware (according to requirement).
5.3.2.1.2        0.2g of magnesium oxide.
5.3.2.1.3        1.0ml of 0.1M hydrochloric acid.
5.3.2.1.4        0.05ml of methyl red solution.
5.3.2.1.5        1.0ml of freshly prepared 100g/L solution of sodium cobaltnitrite.
5.3.2.2  Sample:
5.3.2.2.1        10.0ml of solution S.
5.3.2.3  Method of analysis:
5.3.2.3.1        Take a test tube and add 10.0ml of solution S in it and 0.2mg of magnesium oxide.
5.3.2.3.2        Pass a current of air through the mixture and direct the gas that escapes just beneath the surface of a mixture of 1.0ml of 0.1M hydrochloric acid and 0.05ml of methyl red solution.
5.3.2.3.3        The colour of the indicator changes to yellow.
5.3.2.3.4        On addition of 1.0ml of freshly prepared 100g/L solution of sodium cobaltnitrite.
5.3.2.3.5        Observe the colour change.
5.3.2.4  Observations:
5.3.2.4.1        A yellow ppt is formed.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (according to requirement).
5.4.1.2  Titration apparatus.
5.4.1.3  Magnetic stirrer.
5.4.1.4  Water-bath.
5.4.2        Material and reagents:
5.4.2.1  5.0ml of formaldehyde solution.
5.4.2.2  1M sodium hydroxide.
5.4.2.3  Phenolphthalein solution (as indicator).
5.4.2.4  Purified water.
5.4.3        Sample:
5.4.3.1  1.0g.
5.4.4        Method of analysis:
5.4.4.1  Sample titration:
5.4.4.1.1        Take a flask and add in it 1.0g of sample.
5.4.4.1.2        Dissolve it in 20.0ml of purified water.
5.4.4.1.3        Add a mixture of 5.0ml of formaldehyde solution, previously neutralized to phenolphthalein solution and 20.0ml of purified water.
5.4.4.1.4        Set titration apparatus.
5.4.4.1.5        After 1-2 min, use further 0.2ml of phenolphthalein solution as indicator.
5.4.4.1.6        Titrate slowly with 1M sodium hydroxide.
5.4.4.1.7        Note down the volume used as shown in Annexure-1.
5.4.4.1.8        Take 3 readings at least and take average.
5.4.4.2  Blank titration:
5.4.4.2.1        Take a flask and add in it 20.0ml of purified water.
5.4.4.2.2        Add a mixture of 5.0ml of formaldehyde solution, previously neutralized to phenolphthalein solution and 20.0ml of purified water.
5.4.4.2.3        Set titration apparatus.
5.4.4.2.4        After 1-2 min, use further 0.2ml of phenolphthalein solution as indicator.
5.4.4.2.5        Titrate slowly with 1M sodium hydroxide.
5.4.4.2.6        Note down the volume used as shown in Annexure-1.
5.4.4.2.7        Take 3 readings at least 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 1M Sodium hydroxide is equivalent to 53.49mg of NH4Cl.
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 I., Official Monograph /Ammonium chloride: 2015, pp. 159.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Observations and calculations of assay of Ammonium chloride.

Annexure: 1
Observations and calculations
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
Sr.#
Serial number
Q.C
Quality control
%
Percentage
B.P
British pharmacopoeia
g
Grams
ml
Milliliter
Min
Minutes
ppt
Precipitates
oC
Degree centigrade
mg
Milligram
M
Molar
Vol
Volume
vi
Initial volume
vf
Final volume
QCA
Quality control active ingredient
F
Format
g/L
Gran per liter
R
Reagent


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