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Specifications
S. No.
01.
Test
Description
Specification
02.
Solubility
03.
Identification
a)
By IR
b)
BY UV spectrum
c)
By chloride reaction
Passes.
Melting Point
About 2100C
(with decomposition 205C-215C)
5)
6)
Colour of solution
07)
08)
pH
(1.0 % Aq. solution)
Foreign impurities by TLC
09).
Water content by KF
10).
Loss on drying
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11).
Sulphated Ash
12).
Heavy metals
13)
Sulphates
14).
Assay
Description :
Take about 1 g of the test sample in a watch glass and observe visually with black
back ground.
The material should be Light Yellow or greenish yellow crystalline power, almost
with out odour.
02.
Solubility :
a.
Take about 1 g of the test sample into a 50 mL glass-stoppered cylinder and add 10
mL of Chloroform and mix well.
The resultant solution should be clear and with out any suspended particles.
b.
Take about 1 g of the test sample into a 50 mL glass-stoppered cylinder and add 30
mL of Alcohol (96%) and mix well.
The resultant solution should be clear and with out any suspended particles.
Take about 0.1 g of the test sample into a 50 mL glass-stoppered cylinder and add 10
mL of water and mix well.
The resultant solution should be clear and with out any suspended particles
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03.
Identification :
a.
By IR :
Weigh accurately about 200 mg of KBr, previously dried at 250C and cooled, into a
mortar and grind to a fine powder.
Add about 5 mg of test sample, mix perfectly and grind to a uniform powder.
Take a small quantity of the powder and prepare a thin semi-transparent disk.
Record the IR spectrum of the disk from 3700 sm-1 to 400 sm-1 taking air
as reference.
Standard preparation :
Weigh accurately about 200 mg of KBr, previously dried at 250C and cooled, into a
mortar and grind to a fine powder.
Add about 5 mg of working reference standard, mix perfectly and grind to a uniform
powder.
Take a small quantity of the powder and prepare a thin semi-transparent disk.
Record the IR spectrum of the disk from 3700 sm-1 to 400 sm-1 taking air
as reference.
Specification : The Infra red absorption spectrum is concordant with working
reference standard,.
b)
By UV Spectrum
Take 2 ml of the above solution in to 100ml volumetric flask and make up to 100 ml
with 0.1M hydrochloric acid.
Check the above solution (15mcg/ml) by UV in the wave lengths between 220 to
400 nm. in the ditch with layer thickness 1sm Should exhibit maximums at
241 1nm, 302 2nm and 353 2nm.
c)
Chloride :
REAGENTS :
2M nitric acid.
4.25% v/v silver nitrate solution R.
10M ammonia.
Potassium dichromate
Sulphuric acid
Diphenylcarbazide solution
PROCEDURE
Method - A :
Acidify with 2M nitric acid, add 0.4 ml of silver nitrate solution R, shake and allow
to stand.
A curdy, white precipitate is produced. Centrifuge and wash the precipitate with three
1- ml quantities of water. Carry out this operation rapidly in subdued light,
disregarding the fact that the supernatant solution may not become perfectly clear.
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The precipitate dissolves easily with the possible exception of a few large particles
Which dissolve slowly.
II
Dissolve about 0.01gm of the test sample in a 5ml of concentrated sulphuric acid,
add 1 drop of 0.1M solution of trichloric ferrum.
4)
Melting point
Apparatus : MP apparatus
Pack the capillary tube with sample by tapping on a solid surface so as to form a
Tightly packed column of about 3.5 mm in height
Heat the oil bath in the melting range apparatus by turning ON the heating knob
Heat the oil bath to about 190C. Regulate the rate of raise of temperature to
1 2C per minute.
Insert the capillary tube in to apparatus, when the temperature of the bath reaches
200C
Observe the temperature at which the column of the sample in the capillary tube
collapses definitely against the side of the tube and the temperature at which the
sample becomes liquid throughout.
Specification : The melting point of the test sample about 2100C (with decomposition between
205C and 215C
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Clarity of solution:
Take 0.5 gm of test sample and dissolve in 50ml of water in to a nesslar cylinder.
06)
Colour of solution:
Test preparation: Take 0.5 gm of test sample and dissolve in 50 ml of water.
Preparation of Reference solutios:
I. Solution of Cobalt chloride: 60 mg of COCl 6H2O in 1m of 0.1M solution of
sulphuric acid
II. Solution of Copper sulphate: mg CuSO4 5H2O in 1ml 0.1M solution of sulphuric
acid.
III. Solution of Potassium dichromate: 4.9mg K2Cr2O7 in 1 ml 0.1M solution of
Sulphuric acid.
IV Solution of Chloric (III) Ferrum: 45mg FeCl3 6H2O in 1ml 0.1M solution of
sulphuric acid.
For obtain reference G(green) mix 3.5ml(I), 20.1ml(II), 10.4ml(III), 4.0ml(IV)
solutions in volumetric flask accommodating 100ml and drive the solution volume
Up to the marking with 0.1M solution of sulphuric acid.
For obtaining reference G5 mix 25.5 ml of reference G and 75ml of 0.1M sulphuric
acid solution.
For obtaining reference Y (yellow) mix 9.5 ml of reference I and 1.9 ml of reference
II and 10.7ml of reference III and 4.0ml of reference IV in volumetric flask and
make up to 100 ml with 0.1M sulphuric acid solution.
For obtaining reference Y5 mix 25.5ml of reference Y and 75 ml of 0.1M sulphuric
acid solution.
Compare the test sample solution with reference solutions G5 or Y5 .
The intensity of the test sample should not more than the intensity of G5 or Y5
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Apparatus : pH meter
Dissolve in and make up to the volume with water and mix well.
Transfer the prepared test solution into a 100 mL beaker for examination of pH.
Examine the pH of the test solution and note down the result.
08)
Apparatus : KF apparatus
Fill the burette with K.F reagent with the help of the rubber bellow.
Rotate the stop cock to half open position and press the start button.
Weigh accurately and transfer about 0.2 g of the test sample (W) into the titration
vessel.
Note down the final burette reading (F) when the sound of siren is heard.
Calculate the water content of the test sample by the following equation.
Water content, % w/w
Specification : The water content by KF of the test sample should not more then 2.0% w/w.
Note : 1.
2.
10.
Loss on drying :
Weigh accurately about 1 g of the test sample and transfer it to a weighing bottle
of weight W1 with a stopper previously dried at 120 + 2OC for 30 minutes.
Note down the weight of the weighing bottle with the test sample (W2).
Place the weighing bottle uncovered at 80 + 2oC in an Vacuum oven for 3 hours,
leaving the stopper also in the oven.
After 3 hours, open the Vacuum oven and immediately place the stopper on the
weighing bottle.
Place the weighing bottle in a desiccator to reduce the temperature to room temperature.
( W2 W3 ) x 100
( W2 - W1 )
Specification :
The Loss on drying of the test sample should not be more than 5.0% w/w.
11.
Sulphated Ash :
Weigh accurately about 0.5 g of test sample and transfer to a platinum crucible of
weight W1, previously ignited at 800C for 30 minutes, cooled in a desiccator.
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Note down the weight of the crucible with the test sample W2.
Find out the weight of the test sample taken, W , (W2 -W1)
Cool the residue and moisten with 1 mL of sulphuric acid and heat gently until
white fumes no longer evolve.
Place the crucible in a desiccator, cool and weigh the crucible with residue (W3).
= W1
= W2
= (W2 -W1)
= W3
(W3 - W1)
Wn
( Wn - W1)
( Wn - W1) x 100
W
Specification : The Sulphated ash of test sample should not be more than 0.20 % w/w.
12.
Heavy Metals:
Preparation of Standard Lead Solution:
Pipette out 10 mL of the Lead Nitrate Stock Solution to a 100 mL volumetric flask.
Add 2 mL of Nitric acid and 5 drops of Sulphuric acid to the carbonized mass.
Ignite the contents in a muffle furnace at 500 to 600OC until the carbon is
Completely burned.
Cover and digest over a steam bath / water bath for 10 minutes.
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Rinse the crucible with 5 mL of 6N Hydrochloric acid, and transfer the rinsing to the
test tube.
Monitor Preparation :
Ignite at the same time, in the same muffle furnace ,and under the same conditions
used for the Test preparation.
Cover and digest over a steam bath / water bath for 10 minutes
Rinse the crucible with 5 mL of 6N Hydrochloric acid, and transfer the rinsing to the
test tube.
Procedure:
Adjust the pH of the solutions in each of the tubes containing the standard
preparation, the test preparation, and the monitor preparation with ammonium
hydroxide by cautiously and dropwise to 9 .
Cool, and adjust the pH of the solutions in each of the tubes with glacial acetic acid add
dropwise to 8.
The pH of the solutions to between 3.0 and 4.0 with1N acetic acid or 6N Ammonium
hydroxide
using short range pH indicator paper as external indicator.
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Add 10mL of freshly prepared hydrogen sulphide solution to each of the test tubes
containing the standard preparation, the test preparation, and the monitor preparation
and mix.
The colour of the solution from the test preparation is not darker than that of the
solution from the standard preparation.
For Monitor Preparation
The colour of the solution from the monitor preparation is equal to or darker than that
of the solution from the Standard Preparation .
13.
Sulphates:
Test preparation:
Use 50ml identical test tube for test preparation and reference preparation. Dissolve
about 1.0g of the substance in 10ml of distilled water. Shake this solution with 5.0ml
of sulphate reagent and evaluate after 10 min. by comparison with the
simultaneously prepared test with the solution of comparison.
Reference preparation:
Shake 10ml of distilled water with 2.0ml of sulphate reagent. Acidify with 1 ml of
2M HCl and add 1.0 ml of 100g/ml sulphate limit test solution.
Observe the turbidity and record the results. Turbidity of test preparation shall not
be more than that of reference preparation.
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14.
Chemicals :
Glacial Acetic acid
AR grade.
Mercuric acetite
AR grade.
Crystal Violet
AR grade
Weigh accurately about 0.20 g of test sample into above flask and note down
the weight of the test sample taken, W gram.
Add 10ml of Glacial Acetic acid and 5.0ml of 3%solution of Mercuric acetate(II) in
glacial acetic acid.
Swirl the conical flask to dissolve the contents and cool it to room temperature.
Titrate the contents of the flask with 0.1N Perchloric acid solution until the
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Note down the final burette reading (F). The difference between (F) and (I) gives
the volume, in mL of 0.1N Perchloric acid solution consumed by the test sample
(TV).
Calculate the assay on Dryed basis of the test sample using the following formula
TV X N of 0.1 N Perchloric acid X 0.43397 X 100 X 100
W x (100- Loss on drying of the test sample)
Where,
W = Weight of test sample taken in g.
T.V = (F- I) = Volume, in mL of 0.1N Perchloric acid solution consumed in the
titration.
N
Specification :
Assay (non aqueous titration) of the test sample should be between 98.0 % -101.0 w/w.
Note :
1.
2.
The difference between two trials should not be more than 1.0
3.
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