LIMIT TEST FOR IRON:
The Limit Test for iron is designed to determine the allowable limit of iron
contained in a sample.
PRINCIPLE:
• Limit test of Iron is based on the reaction of iron in ammoniacal solution
with thioglycolic acid in presence of citric acid to form iron thioglycolate
(Ferrous thioglycolate complex) which produces pale pink to deep
reddish-purple colour in alkaline media.
• Thioglycolic acid is used as reducing agent.
• The colour of the Ferrous thioglycolate complex fades in the presence of
air due to oxidation.
• Also, the colour is destroyed in presence of oxidizing agents and strong
alkalis.
• The purple colour is developed only in alkaline media, so ammonia
solution is used.
• But ammonia reacts with iron, forms precipitate of ferrous hydroxide.
Thus, citric acid is used which prevents the precipitate of iron with
Ammonia by forming a complex with iron as iron citrate.
Procedure:
Preparation of standard solution: 0.173g of ferric ammonium sulphate
NH4Fe (SO4)2.12H2O to 1.5ml of HCl and adding sufficient water to produce
1000ml.
Each ml of solution contains .02mg of iron
Test solution Standard solution
Sample is dissolved in specific 2ml of standard solution of iron
amount of water and then volume diluted with water upto 40ml
is made upto 40ml
Add 2ml of 20% w/v of citric acid Add 2ml of 20% w/v of citric acid
Add 2 drops of thioglycolic acid Add 2 drops of thioglycolic acid
Add ammonia to make the Add ammonia to make the
solution alkaline and adjust the solution alkaline and adjust the
volume to 50ml volume to 50ml
Keep aside for 5min Keep aside for 5min
Colour developed is viewed Colour developed is viewed
vertically and compared with vertically and compared
standard solution
*All the reagents used in the limit test for Iron should
themselves be iron free.
Observation:
The purple colour produce in sample solution should not be greater than
standard solution. If purple colour produced in sample solution is less than
the standard solution, the sample will pass the limit test of iron and vice
versa.
Reasons:
• Citric acid forms complex with metal cation and helps precipitation of
iron as iron citrate and prevent the formation of ferrous hydroxide.
• Thioglycolic acid reduces iron (II) to iron (III).
• Ammonia is added to make solution alkaline. The pale pink colour is
visible only in the alkaline media. The colour is not visible in acidic media
as ferrous thioglycolate complex decomposes in high acidic media.
