DRIED ALUMINIUM HYDROXIDE SOP


DRIED ALUMINIUM HYDROXIDE SOP


1.0  OBJECTIVE:
To lay down a procedure of the active raw material of the Dried Aluminium hydroxide 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, amorphous powder.
5.1.2        Solubility:
5.1.2.1  Material and equipment:
5.1.2.1.1        Glassware (3 test tubes, 1 spatula, 1 pipette).
5.1.2.1.2        Dilute mineral acid (e.g. dilute HCl, dilute H2SO4, HNO3).
5.1.2.1.3        Solutions of alkali hydroxide (e.g. NaOH, KOH).
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 dilute mineral acid in test tube 2 and observe.
5.1.2.3.4        Add solution of alkali hydroxide in test tube 3 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 & 3 containing with dilute mineral acid & solution of alkali hydroxide is dissolved.
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  Water bath.
5.2.1.4  Magnetic stirrer.
5.2.2        Sample:
5.2.2.1  2.5g.
5.2.3        Preparation of solution S:
5.2.3.1  Take a beaker of 100.0ml and add sample 2.5g of dried aluminium hydroxide in it.
5.2.3.2  Add in it 15.0ml of hydrochloric acid by using pipette.
5.2.3.3  Heat it on water-bath.
5.2.3.4  Dilute it to 100.0ml with distilled water.
5.3  Identification tests:
5.3.1        Aluminium test:
5.3.1.1  Material and equipment:
5.3.1.1.1        Glassware (1 test tube, 1 pipette).
5.3.1.1.2        0.5ml of dilute hydrochloric acid.
5.3.1.1.3        0.5ml of thioacetamide reagent.
5.3.1.1.4        Dilute sodium hydroxide.
5.3.1.1.5        Ammonium chloride solution.
5.3.1.2  Sample:
5.3.1.2.1        2.0ml of the solution S.
5.3.1.3  Method:
5.3.1.3.1        Take 2.0ml of the solution S and add about 0.5ml of dilute hydrochloric acid and about 0.5ml of thioacetamide reagent. Dissolve it.
5.3.1.3.2        Observe the changes.
5.3.1.3.3        No ppt is formed.
5.3.1.3.4        Add drop-wise dilute sodium hydroxide solution.
5.3.1.3.5        Observe the changes.
5.3.1.3.6        A gelatinous white ppt is formed.
5.3.1.3.7        When further dilute sodium hydroxide solution is added, gelatinous white ppt is dissolved.
5.3.1.3.8        Gradually add ammonium chloride solution.
5.3.1.3.9        Observe the changes.
5.3.1.4  Observations:
5.3.1.4.1        The gelatinous white ppt is re-formed.
5.4  Assay:
5.4.1        Apparatus:
5.4.1.1  Glassware (1 100.0ml of beaker, 1 50.0ml of beaker, 1 spatula, 1 glass rod, 1 pipette).
5.4.1.2  Analytical weighing balance.
5.4.1.3  Water bath.
5.4.1.4  Magnetic stirrer.
5.4.1.5  Titration apparatus.
5.4.2        Material and reagents:
5.4.2.1  10.0ml of hydrochloric acid R1.
5.4.2.2  Purified water (q.s).
5.4.2.3  10.0ml of dilute ammonia R1.
5.4.2.4  Smallest quantity of dilute hydrochloric acid.
5.4.2.5  0.1M sodium edetate.
5.4.2.6  155g/L solution of ammonium acetate R.
5.4.2.7  Dilute acetic acid.
5.4.2.8  50.0ml of ethanol.
5.4.2.9  3.0ml of a freshly prepared 0.25g/L solution of dithizone.
5.4.3        Sample:
5.4.3.1  0.8g
5.4.4        Method of analysis:
5.4.4.1  Take a 100.0ml of beaker and add 0.8g of sample in it.
5.4.4.2  Add 10.0ml of hydrochloric acid R1 in it, dissolve by using glass rod and heat on water-bath.
5.4.4.3  Cool it and dilute it to 50.0ml with purified water.
5.4.4.4  Take 10.0ml of the above solution in another 50.0ml beaker.
5.4.4.5  Add dilute ammonia R1 until a ppt begins to appear.
5.4.4.6  Add the smallest quantity of dilute hydrochloric acid to dissolve the ppt.
5.4.4.7  And finally dilute it to 20.0ml with purified water.
5.4.4.8  Take a conical flask of 500.0ml and add 20.0ml of the above prepared solution.
5.4.4.9  Add 25.0ml of 0.1M sodium edetate and 10.0ml of a mixture of equal volumes of a 155g/L solution of ammonium acetate R and dilute acetic acid.
5.4.4.10    Boil it for 2mins and then cool it.
5.4.4.11    Add 50.0ml of ethanol and 3.0ml of a freshly prepared 0.25g/L solution of dithizone in ethanol.
5.4.4.12    Set titration apparatus.
5.4.4.13    Titrate the excess of 0.1M sodium edetate with 0.1M zinc sulfate until the colour changes from greenish-blue to reddish-violet.
5.4.4.14    The above procedure is for sample titration and similarly performs the blank titration without using sample.
5.4.4.15    Note down the volume used as shown in Annexure-1.
5.4.4.16    And take average.
5.4.4.17    Calculate percentage purity.
5.4.4.18    Calculations:
5.4.4.18.1    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.
5.4.4.18.2    For percentage purity use formula:
%age purity = volume used by substance x factor x 100
                                                                               Weight of sample
5.4.4.18.3    Put values and calculate %age purity.
5.4.5        Factor:
5.4.5.1  1ml of 0.1M sodium edetate is equivalent to 5.098mg of Al2O3.
5.4.6        Limit:
5.4.6.1  47.0% to 60.0%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
7.2  The British Pharmacopoeia. Vol I., Official Monograph / Dried Aluminium hydroxide: 2015, pp. 117-118.
7.3  The British Pharmacopoeia. Vol V., Official Monograph /Complexometric Titration: 2015, pp. 281-282.
8.0  ANNEXURES:
Annexure 1: Assay observations and calculations (Complexometric titration).




Annexure: 1
Assay observations and calculations (Complexometric titration)
Complexometric 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
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


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