LIMIT TESTS
PART-C
By: Ms Preeti Avasthi Sub: Inorganic Chemistry
Assistant Professor B. Pharmacy 1st semester.
Maharaja Agrasen School of Pharmacy
Maharaja Agrasen University
LIMIT TESTS FOR HEAVY METALS
Principle: Limit test of heavy metals is based on the reaction of metallic
impurities with hydrogen sulfide in acidic medium to form brownish colour
solution. Metals that response to this test are lead, mercury, bismuth, arsenic,
antimony, tin, cadmium, silver, copper, and molybdenum. The metallic impurities
in substances are expressed as parts of lead per million parts of the substance. The
usual limit as per Indian Pharmacopoeia is 20 ppm
The precipitate of heavy metal sulphide formed gives colour. Dilute acetic acid and
ammonia are used to maintain pH between 3.0 and 4.0 so that the precipitate
formed is colloidal and uniform. The saturated solution of hydrogen sulphide has to
be prepared freshly for the experiment. Here hydrogen sulphide gas is generated
using a specially devised apparatus called as Kipp’s apparatus in which ferrous
sulphide sticks are made to react with equal volumes of concentrated hydrochloric
acid and water. Indian pharmacopoeia 1996, provides four methods depending on
the resulting solution of substance (i.e., based on solubility, colour etc).
Method A uses hydrogen sulphide solution, method B uses hydrogen sulphide
solution after igniting the substance, method C uses sodium sulphide solution after
treating the substance with sodium hydroxide solution, and in method D
thioacetamide solution is used.
the methods can be categorized as follows:
Method I: It is used for the substance which gives a clear, colorless solution
under specified conditions.
Method II: It is used for the substance which does not give a clear, colorless
solution.
Method III: It is used for the substance which gives a clear, colorless solution in
sodium hydroxide medium.
Observation: The color produce in sample solution should not be greater than
standard solution. If color produces in sample solution is less than the standard
solution, the sample will pass the limit test of heavy metals and vice versa.
Method D :
Standard Solution: Pipette 10.0 ml of either standard lead solution (1 ppm Pb) or
standard lead solution (2 ppm Pb) into a small Nessler cylinder labeled as
“Standard”. Add 2.0 ml of the test solution and mix.
Test Solution: Prepare as directed in the individual monograph and pipette 12 ml
into a small Nessler cylinder labeled as “Test”.
Procedure: Add 2 ml of acetate buffer pH 3.5 to each of the above Nessler
cylinders, mix, add 1.2 ml of thioacetamide reagent and allow to stand for 2
minutes. Compare the colour by viewing vertically downwards over a white
surface. The colour produced with the test solution is not more intense that than
produced with the standard solution.
MODIFIED LIMIT TEST FOR CHLORIDES
Principle:
Modified limit test is performed; if the limit tests for a sample (Coloured
compound) cannot be done by normal method. For example, potassium
permanganate is de-colourised by boiling with ethanol, filtered to remove
precipitated manganese dioxide and the filtrate is subjected to the test. It is based
upon the chemical reaction between silver nitrate and soluble chlorides to obtain
silver chloride in presence of dilute nitric acid. The silver chloride produced in the
presence of dilute nitric acid makes the test solution turbid, the extent of
turbidity/opalescence depending upon the amount of chloride present in the
substance is compared with a standard turbidity/opalescence produced by addition
of silver nitrate to a standard solution having a known amount of chloride and the
same volume of dilute nitric acid as used in the test solution.
If the turbidity/opalescence from the sample has been less than the standard
solution, the sample will pass the limit test and vice versa. Dilute nitric acid is used
in the limit test of chloride to make solution acidic and which helps silver chloride
precipitate to make solution turbid at the end of process.
Procedure: Preparation of Test Solution (KMnO4): Dissolve 1.5 g in 50 mL of
distilled water, heat on a water-bath and add gradually 6 mL of ethanol (95%), cool,
dilute to 60 mL with distilled water and filter.
Take two 50 mL Nessler Cylinders. Label one as “Test” and the other as „Standard‟.
Observation: The opalescence produce in sample solution should not be greater
than standard solution. If opalescence produces in sample solution is less than the
standard solution, the sample will pass the limit test for chloride and vice-versa.
MODIFIED LIMIT TEST FOR
SULPHATES
Principle: Modified limit test is performed; if the limit tests for a sample (Coloured
compound) cannot be done by normal method. For example, potassium
permanganate is de-colourised by boiling with ethanol, filtered to remove
precipitated manganese dioxide and the filtrate is subjected to the test. The limit test
for sulphate is carried out on the basis of the reaction between barium chloride and
soluble sulphates in the presence of acetic acid. Then, the comparison of the
turbidity produced by a given amount of the substance is done with a standard
turbidity obtained from a known amount of sulphate. The barium chloride has been
replaced by barium sulphate reagent which is having barium chloride, sulphate-free
alcohol, and a solution of potassium sulphate.
Potassium sulphate has been added to increase the sensitivity of the test. The ionic
concentrations in the reagent has been so adjusted that the solubility product of
barium sulphate gets exceeded, and the very small amount of barium sulphate
present in the reagent acts as a seeding agent for precipitation of barium sulphate,
if sulphate be present in the substance under test. Alcohol helps to prevent super-
saturation and thus produces a more uniform opalescence/turbidity. Acetic acid
helps to make solution acidic and barium sulphate precipitate formed is insoluble
which gives turbidity/opalescence.
Observation: The opalescence produce in sample solution should not be greater
than standard solution. If opalescence produces in sample solution is less than the
standard solution, the sample will pass the limit test for sulphates and vice-versa.
REFERENCES
A Textbook of pharmaceutical chemistry by SIA publications
[Link] by Madhusudhana Reddy Induri Ph
[Link]