Limit Test-Sulphate:

The aim of the limit test for sulfate is to qualitatively detect the presence of sulfate ions in a given
sample. This test is particularly useful in situations where a quick and simple determination of the
presence of sulfate ions is needed, rather than quantifying the exact concentration.

 The formation of a white precipitate of barium sulfate indicates the presence of sulfate
ions. The test is sensitive and widely employed in qualitative analysis to identify the
sulfate ion in various substances, such as water, food, or chemical samples. It helps to
assess whether sulfate ions are present within a certain limit in the sample under
investigation.

Here's the breakdown of the principle:

Here's the breakdown of the principle:

 The limit test for sulphate is based on the reaction between barium chloride
c
and soluble sulphates in presence of dilute hydrochloric acid. Then the
turbidity produced is compared with the standard turbidity.

 Potassium sulphate is used to increase the sensitivity of the test

test.

 It react with the barium chloride and forms

forms barium sulphate in small
quantity which will act as a seeding agent.
agent

 The ionic concentration has been so adjusted, such that the solubility
product barium sulphate get exceeded and very small amount of barium
sulphate acts as seeding agent for precipit
precipitation
ation of barium sulphate.
sulphate

 Alcohol is to prevent super saturation and thus produces uniform turbidity.

 Hydrochloric acid helps to make solution acidic and the barium sulphate
precipitate formed is insoluble which gives turbidity
turbidity.
Conclusion:-
In pharmacy analysis, a limit test is often employed to ensure that a pharmaceutical
product meets specific quality standards. This test sets acceptable limits for impurities or
specified substances. If the amount of the substance being tested falls within these
predetermined limits, the product is considered acceptable; otherwise, it may be deemed
unacceptable for use or consumption. The limit test in pharmacy analysis is crucial for
maintaining the safety and efficacy of pharmaceutical products.

References:-
 “google.com”
 “quora.com” etc.
 Limit test-Iron, Sulphate

 Limit = A value or amount that is likely to be present in a substance.

 Test = to examine or to investigate.

 Limit test is defined as quantitative or semi quantitative test designed to identify and control small
quantities of impurity which is likely to be present in the substance.

 Impurity is defined as the presence of one substance in another substance in low

concentration. Impurity can be an organic, in-organic, microbial, dust, moisture
etc. In a pharmaceutical substance, the nature of impurity can be predicted
provided we know the source through which it has been obtained. Impurities are
imparted into the pharmaceutical substance through raw materials,
intermediates, reagents, catalysts, solvents, reaction vessels, improper storage,
cross-contamination, manufacturing errors, packing errors, microbial
contamination, chemical instability, storage containers etc.

 Water is a rich source for chlorides, sulphates, carbonates etc. Reactor materials
used for manufacturing are rich source of steel, copper, iron, zinc, lead.
Reagents, catalysts are rich sources of arsenic, antimony, heavy metals, lead,
cadmium, mercury, which are potent nerve poisons on cumulative accumulation.

 Hence presence of an impurity in a pharmaceutical substance may cause

cumulative toxic effect, decreased therapeutic effect, change in physical and
chemical properties, and difficulty in formulation, in-compatibility, and decrease
in shelf-life, change in odor, color, taste and appearance.

 Limit test is generally carried out to determine the inorganic impurities present in compound.

 Since procuring pure pharmaceutical substance free from impurities is expensive

and difficult process, Indian Pharmacopoeia, which is under the control of
Ministry of Health & Family Welfare, Government of India provides permissible
limit of a impurity and designate the pharmaceutical substance as standard
 Provided it complies the tests given under individual monographs.

 Limit tests are quantitative or semi-quantitative test designed to control small

quantities of in-organic impurities, which are likely to be present in a
pharmaceutical substance. Limit test for chlorides, sulphates, lead, iron, heavy
metals and arsenic are official tests designed and mentioned in the individual
monograph of pharmaceutical substance in Indian Pharmacopoeia.

 In short, limit test is nothing but to identify the impurities present in the substance and compare it with
standard.
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HOOGHLY, WEST BENGAL-712102.

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TITLE OF THE TOPIC: Limit test-Iron,Sulphate.

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NAME: Aayan Mazumdar

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Limit Test-Iron:
Performing a limit test for iron typically involves the following:

 Acidification:*
- Acidify the sample with dilute hydrochloric acid (HCl) to ensure that iron is in the Fe^3+ state
state.

 Addition of Thiocyanate Solution:*

- Add potassium thiocyanate solution (KSCN) to the acidified sample
sample.

 Observation of Color Change:*

- If iron(III) ions are present, a reddish
reddish-brown
brown color will appear due to the formation of the ferric
thiocyanate complex.

 Confirmatory Tests (if necessary):*

essary):*
- Additional confirmatory tests may be performed depending on the specific requirements. For
example, you may use sodium hydroxide (NaOH) to precipitate iron(III) as iron(III) hydroxide or
ammonium thiocyanate (NH4SCN) to confirm the presence of iron(III) ions.

It's crucial to follow the specific procedures outlined in the method you're using, as different analytical
methods may have slight variations. Always ensure the accuracy of measurements and adhere to
safety precautions.

 The limit test for iron is based on the reaction of iron in ammonical solution in
the presence of citric acid with thioglycolic
thioglycolic acid. When a pale pink to deep
reddish purple colour is formed due to the ferrous thioglycote complex. The
color produced from a specific amount of substance from test is compared with
the color produced in standard solution by viewing vertically.

Here's the breakdown of the principle:

 Ferric ammonium sulphate is used as standard.

 The test is very sensitive; interference of other metal cations is eliminated

el by
using of 20 % w/v citric acid.

 The iron free citric acid is used to complex metal cations other than iron if any.

 Ferrous thioglycollate complex is colorless in acidic or neutral solutions.

 Only in the presence of alkali pale pink color will

w be produced.

 Citric acid forms ammonium citrate buffer when ammonia is added to make
alkaline which in turn stabilizes the complex formed.