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
Average volume: _________________
Blank titration
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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