PRACTICAL MANUAL PHARMACEUTICAL ANALYSIS
Experiment No: 3
Aim: To perform limit test of given sample of Sulphate
Reference: Jooti Gupta, Mohit Sanduja and Madhuri Jover, A practical book of pharmaceutical
inorganic chemistry, Nirali Prakashan, 1st Edition 2017, Page no. 1 - 18
Requirement: Nesselar’s cylinder, measuring cylinder, glass rod, potassium sulphate, standard
solution, Hcl, barium sulphate reagent and distilled water
Principle:
Limit test of sulphate is based on the reaction of soluble sulphate with barium chloride in
presence of dilute hydrochloric acid to form barium sulphate which appears as solid
particles(turbidity) in the solution and Barium sulphate reagent contains barium chloride,
sulphate free alcohol and small amount of potassium sulpahte.
Procedure:
Test Sample Standard Compound
Specific weight of compound is dissolved in
water or solution is prepared as directed in the Take 1ml of 0.1089 % W/V solution of
pharmacopoeia and transferred in Nessler potassium sulphate in Nessler cylinder
cylinder
Add 2ml of dilute hydrochloric acid Add 2ml of dilute hydrochloric acid
Dilute to 45 ml in Nessler cylinder Dilute to 45 ml in Nessler cylinder
Add 5ml of barium sulphate reagent Add 5ml of barium sulphate reagent
Keep aside for 5 min Keep aside for 5 min
Observe the Turbidity Observe the Turbidity
Observation:
The turbidity produce in sample solution should not be greater than standard solution. If
Mr. Prashant B. Patil, Assistant Professor, HRPIPER, Shirpur, 2017-18 1
PRACTICAL MANUAL PHARMACEUTICAL ANALYSIS
turbidity produces in sample solution is less than the standard solution, the sample will
pass the limit test of sulphate and vice versa.
Reasons:
1. Hydrochloric acid helps to make solution acidic.
2. Potassium sulphate is used to increase the sensitivity of the test by giving ionic.
3. Concentration in the reagent and alcohol helps to prevent super saturation.
Mr. Prashant B. Patil, Assistant Professor, HRPIPER, Shirpur, 2017-18 2
PRACTICAL MANUAL PHARMACEUTICAL ANALYSIS
Experiment No: 4
Aim: To perform limit test of given sample Iron
Reference: Jooti Gupta, Mohit Sanduja and Madhuri Jover, A practical book of pharmaceutical
inorganic chemistry, Nirali Prakashan, 1st Edition 2017, Page no. 1 - 18
Requirement: Nesselar’s cylinder, measuring cylinder, glass rod, citric acid, thioglycollic acid,
ammonia solution, standard iron solution, and sulphuric acid
Principle:
Limit test of Iron is based on the reaction of iron in ammonical solution with thioglycollic
acid in presence of citric acid to form iron thioglycolate which is pale pink to deep
reddish purple in color.
Procedure:
Test sample Standard compound
Sample is dissolved in specific amount of 2 ml of standard solution of iron diluted with
water and then volume is made up to 40 ml water upto 40ml
Add 2 ml of 20 % w/v of citric acid (iron Add 2 ml of 20 % w/v of citric acid (iron
free) free)
Add 2 drops of thioglycollic acid Add 2 drops of thioglycollic acid
Add ammonia to make the solution alkaline Add ammonia to make the solution alkaline
and adjust the volume to 50 ml and adjust the volume to 50 ml
Keep aside for 5 min Keep aside for 5 min
Mr. Prashant B. Patil, Assistant Professor, HRPIPER, Shirpur, 2017-18 3
PRACTICAL MANUAL PHARMACEUTICAL ANALYSIS
Color developed is viewed vertically and Color developed is viewed vertically and
compared with standard solution compared with standard solution
`Earlier aamonium thiocyanate reagent was used for the limit test of iron. Since
thioglycolic acid is more sensitive reagent, it has replaced ammonium thiocyanate in the
test.
Observation:
The purple color produce in sample solution should not be greater than standard solution.
If purple color produces in sample solution is less than the standard solution, the sample
will pass the limit test of iron and vice versa.
Reasons:
1. Citric acid helps precipitation of iron by ammonia by forming a complex with it.
2. Thioglycolic acid helps to oxidize iron (II) to iron (III).
3. Ammonia to make solution alkaline.
Mr. Prashant B. Patil, Assistant Professor, HRPIPER, Shirpur, 2017-18 4
PRACTICAL MANUAL PHARMACEUTICAL ANALYSIS
Experiment No: 5
Aim: To perform limit test of given sample of Arsenic
Reference: Jooti Gupta, Mohit Sanduja and Madhuri Jover, A practical book of pharmaceutical
inorganic chemistry, Nirali Prakashan, 1st Edition 2017, Page no. 1 - 18
Requirement: Gutzeit’s apparatus, measuring cylinder, conical flask, glass rod, dropper, test
solution, stannous chloride solution, stannous hyderochloric acid, standard arsenic
solution, granulated zinc, potassium iodide, mercuric chloride paper etc.
Principle:
Limit test of Arsenic is based on the reaction of arsenic gas with hydrogen ion to form
yellow stain on mercuric chloride paper in presence of reducing agents like potassium
iodide. It is also called as Gutzeit test and requires special apparatus.Arsenic, present as
arsenic acid in the sample is reduced to arsenious acid by reducing agents like potassium
iodide, stannous acid, zinc, hydrochloric acid, etc. Arsenious acid is further reduced to
arsine (gas) by hydrogen and reacts with mercuric chloride paper to give a yellow stain.
H3AsO4 + H2SnO2 H3AsO3 + H2SnO3
Arsenic acid Arsenious acid
H3AsO3+ 3H2 AsH3+ 3H2O
Arsenious acid Arsine
The depth of yellow stain on mercuric chloride paper will depend upon the quality of
arsenic present in the sample.
Procedure:
Test Solution
1. The test solution is prepared by dissolving specific amount in water and stannated HCl
(arsenic free) and kept in a wide mouthed bottle.
2. To this solution 1 gm of KI, 5 ml of stannous chloride acid solution and 10 gm of zinc
Mr. Prashant B. Patil, Assistant Professor, HRPIPER, Shirpur, 2017-18 5
PRACTICAL MANUAL PHARMACEUTICAL ANALYSIS
is added (all this reagents must be arsenic free)
3. Keep the solution aside for 40 min and stain obtained on mercuric chloride paper is
compared with standard solution.
Standard solution:
A known quantity of dilute arsenic solution is kept in wide mouthed bottle and rest
procedure is followed as described in test solution.
Figure: Arsenic Limit test apparatus
Where,
A. Approximately 60 ml generator bottle with 40 ml indicating line
B. Glass tube with 6.5 mm inner diameter
C. and D: a ground joint glass tube with 6.5 mm inner diameter and 18 mm outer
diameter at the joint. Inner joint and the outer joint form a concentric circle.
E. Rubberstopper
F. Narrow part of the glass tube B. Glass wool is inserted up to this part.
G. Rubber board (Lead acetate cotton plug)
H. Clamp
Reasons:
Mr. Prashant B. Patil, Assistant Professor, HRPIPER, Shirpur, 2017-18 6
PRACTICAL MANUAL PHARMACEUTICAL ANALYSIS
1. Stannous chloride is used for complete evolution of arsine.
2. Zinc, potassium iodide and stannous chloride is used as a reducing agent.
3. Hydrochloric acid is used to make the solution acidic.
4. Lead acetate pledger or papers are used to trap any hydrogen sulphide which may be
evolved along with arsine.
Mr. Prashant B. Patil, Assistant Professor, HRPIPER, Shirpur, 2017-18 7
