MAGNESIUM HYDROXIDE SOP


MAGNESIUM HYDROXIDE SOP


1.0  OBJECTIVE:
To lay down a procedure of analytical report for the active raw material of the Magnesium hydroxide from the Pharmacopoeia 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, fine, amorphous powder.
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        Dilute acid (e.g. dilute HCl, dilute H2SO4).
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 dilute acid in test tube 2 and observe.
5.1.2.4  Observations:
5.1.2.4.1        The sample in test tube 1 containing with purified water is practically insoluble.
5.1.2.4.2        The sample in test tube 2 containing with dilute acid is dissolved.
5.2  Identification tests:
5.2.1        Magnesium test:
5.2.1.1  Material and equipment:
5.2.1.1.1        Glassware (according to requirement).
5.2.1.1.2        2.0ml of dilute nitric acid.
5.2.1.1.3        Dilute sodium hydroxide.
5.2.1.2  Sample:
5.2.1.2.1        15.0mg.
5.2.1.3  Method:
5.2.1.3.1        Take a test tube and add 15.0mg of sample in it and add 2.0ml of dilute nitric acid dissolve it.
5.2.1.3.2        And also add dilute sodium hydroxide to neutralize it.
5.2.1.3.3        Take 2.0ml of this prescribed solution and add 1.0ml of dilute ammonia.
5.2.1.3.4        A white ppt is formed.
5.2.1.3.5        Add 1.0ml of ammonium chloride solution you can observe that ppt has been dissolved.
5.2.1.3.6        Add 1.0ml of disodium hydrogen phosphate solution.
5.2.1.3.7        Observe the changes.
5.2.1.4  Observations:
5.2.1.4.1        A white crystalline ppt is formed.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Analytical weighing balance.
5.3.1.3  Water bath.
5.3.1.4  Magnetic stirrer.
5.3.1.5  Titration apparatus.
5.3.2        Material and reagents:
5.3.2.1  2.0ml of dilute hydrochloric acid.
5.3.2.2  Purified water (q.s).
5.3.2.3  10.0ml of ammonium chloride buffer solution pH=10.
5.3.2.4  50.0mg of mordant black 11 triturate (as indicator).
5.3.2.5  0.1M sodium edetate.
5.3.3        Sample:
5.3.3.1  0.1g
5.3.4        Method of analysis:
5.3.4.1  Sample titration:
5.3.4.1.1        Take a conical flask and add 0.1g of sample in it.
5.3.4.1.2        Mix it with 20.0ml of water and 2.0ml of dilute hydrochloric acid by using magnetic stirrer.
5.3.4.1.3        Dilute this prescribed solution to 300.0ml with purified water.
5.3.4.1.4        Add 10.0ml of ammonium chloride buffer solution pH 10 and about 50.0mg of mordant black 11 triturate (as indicator) mix it thoroughly.
5.3.4.1.5        Heat it to about 40oC on water bath.
5.3.4.1.6        Set titration apparatus.
5.3.4.1.7        Titrate with 0.1M sodium edetate at the same temperature until the colour changes from violet to full blue.
5.3.4.1.8        Note down the volume used as shown in Annexure-1.
5.3.4.1.9        And take average.
5.3.4.2  Blank titration:
5.3.4.2.1        Take a conical flask and add in it with 20.0ml of water and 2.0ml of dilute hydrochloric acid mix it by using magnetic stirrer.
5.3.4.2.2        Dilute it to 300.0ml with purified water.
5.3.4.2.3        Add 10.0ml of ammonium chloride buffer solution pH 10 and about 50.0mg of mordant black 11 triturate (as indicator) mix it thoroughly.
5.3.4.2.4        Heat it to about 40oC on water bath.
5.3.4.2.5        Set titration apparatus.
5.3.4.2.6        Titrate with 0.1M sodium edetate at the same temperature until the colour changes from violet to full blue.
5.3.4.2.7        Note down the volume used as shown in Annexure-1.
5.3.4.2.8        And take average.
5.3.4.3  Calculate percentage purity.
5.3.4.4  Calculations:
5.3.4.4.1        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.
5.3.4.4.2        For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                                         Weight of sample
5.3.4.4.3        Put values and calculate %age purity.
5.3.5        Factor:
5.3.5.1  1ml of 0.1M sodium edetate is equivalent to 5.832mg of Mg(OH)2.
5.3.6        Limit:
5.3.6.1  95.0% to 100.5%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol II., Official Monograph / Magnesium hydroxide: 2015, pp. 169-170.
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: 5.832mg.
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
q.s
Quantity sufficient
ppt
Precipitate
g
Grams
ml
Milliliter
e.g.
For example
M
Molar
g/L
Grams per liter
mg
Milligram
oC
Degree centigrade
vi
Initial volume
vf
Final volume
B.P
British pharmacopoeia
Vol
Volume
QCA
Quality control active ingredient
F
Format


No comments:

Post a Comment