is.3025.53.2003
is.3025.53.2003
is.3025.53.2003
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IS 3025 (Part 53): 2003
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Indian Standard
METHODS OF SAMPLING AND TEST (PHYSICAL AND
CHEMICAL) FORWATERAND WASTEWATER
PART 53 IRON
(First Revision )
ICS 13.060.50
Q BIS 2003
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
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Environment Protection and Waste Management Sectional Committee, CHD 32
FOREWORD
This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized
by the Environment Protection and Waste Management Sectional Committee had been approved by the Chemical
Division Council.
Pollution caused by substances, on which biotic and abiotic agencies of decomposition are ineffective, is a
unique type of pollution. Toxic trace elements and heavy metals come under the category of non-degradable
pollutants. The problem caused by these elements is in fact due to their concentration in the environment in the
bio-available state and above a certain concentration become harmful to the living organism.
Iron (Fe) is naturally abundant in earth’s crust. Amount of iron available in soluble from depends upon the
concentration of the complex forming ions, pH and oxidation conditions. In the absence of the complex forming
ions, ferric iron is not significantly soluble unless thepH is very low. Oxygenated surface waters seldom contain
more than 1 mg/1 of iron. Ground waters and the surface waters which are acidic, may, on the other hand,
contain considerably more iron. In water samples, iron may be present, as free hydrated ions, in the form of
organic/inorganic complex ions, in a colloidal state or as relatively coarse suspended particles. Iron in water
can cause staining of laundry and porcelain. A bitter sweet astringent taste is imparted to the drinking water at
levels above 1 mg/1 of iron. Iron appears to be an essential element for all organisms — both plant and animals.
In animals iron is found in many important proteins, major functions of these proteins are in oxygen storage
and transport and electron transport.
As per IS 10500:1991 ‘Drinking water specification (first revision)’, the permissible limits of iron in drinking
water is 0.3 mg/1, Max. Beyond this limit, taste/appearance are affected, has adverse effect on domestic uses and
water supply structures, and promotes iron bacteria.
In view of the environmentally prevalent nature of iron (Fe) compounds in levels should be closely monitored to
avoid any likelihood of toxicity caused by this element.
The technical committee responsible for the formulation of IS 3025:1964 had decided to revise the standard
and publish it as separate parts.This standard supersedes 32 of IS 3025:1964.
[n the preparation of this standard, considerable assistance is derived from ‘Standard Methods for the Examination
of Water and Wastewater’, 19th Edition-1995, published by the American Public Health Association, Washington,
U.S.A.
The spectrometric method for determination of total dissolved iron and total (both dissolved and undissolved)
iron using 1,10 phenanthroline are technically equivalent to 1S0 6632: 1988 ‘Water quality — Determination
of iron —— Spectrometric method using 1,10 phenanthroline’.
The composition of the Committee responsible for formulation of this standard is given at Annex A.
In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or
calculated, is to be rounded off, it shall be done in accordance with IS 2:1960 ‘Rules for rounding off numerical
values (revised)’.
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IS 3025 (Part 53) :2003
Indian Standard
METHODS OF SAMPLING AND TEST (PHYSICAL AND
CHEMICAL) FOR WATER AND WASTEWATER
PART 53 IRON
( First Revision)
1 SCOPE concentrated nitric acid (2 ml of cone nitric acid in
1 litre sample, just to bring down the pH below 2).
1.1 This standard prescribes two methods for the
The acidified samples can be stored for a few days (up
determination of iron:
to 5 days) in a refrigerator.
a) 1,10 phenanthroline method, and
Iron in water may vary in concentration and form with
b) Atomic absorption method. duration and degree of flushing when taking a sample.
1.2 Depending upon the concentration range and Shake bottle vigoroulsy to obtain uniform suspension
interference levels, choice of the method is made. of precipitated iron. Use particular care for when
colloidal iron addheres to the sampling bottle. The
2 REFERENCES problem is more accute with plastic bottle.
The standards listed below contain provisions which 5 PURITY OF THE REAGENTS
through reference in this text, constitute provisions of
this standard . At the time of publication, the editions Unless specified otherwise, only pure chemicals and
indicated were valid. All standards are subject to iron free distilled water shall be used in tests.
revision and parties to agreements based on this NOTE — ‘Pure chemicals’ shall mean chemicals that do not
standard are encouraged to investigate the possibility contain impurities which affect the result of analysis.
of applying the most recent editions of the standards.
6 1,10 PHENANTHROLINE METHOD
IS No. Title
3025 (Part 1) : Methods of sampling and test 6.1 Principle
1987 (physical and chemical) for water
‘Iron in the solution is reduced to the ferrous state by
and wastewater : Part 1 Sampling
boiling with hydrochloric acid and hydroxylamine, and
(@l revision)
treated with 1,10 phenanthroline at pH to 3.3. Three
7022 (Part 1): Glossary of terms relating to water,
molecules of phenanthroline chelate each atom of
1973 sewage and industrial effluents, Part 1
ferrous iron to form an orange-red complex. The
7022 (Part 2) : Glossary of terms relating to water,
coloured solution obeys Beer’s law. Its colour intensity
1979 sewage and industrial effluents,
is independent of pH from 3 to 9. A pH between 2.9
Part 2
and 3.5 insures rapid colour development in the
3 TERMINOLOGY presence of an excess of phenanthroline. This method
is applicable in the range of 75 to 500 kg/1 of iron.
For the purpose of this standard, definitions given in
IS 7022 (Part 1) and IS 7022 (Part 2) shall apply. 6.2 Interference
Among the interfering substances are strong oxidizing
4 SAMPLING AND STORAGE agents, cyanide, nitrite, and phosphates (polypho-
The sampling shall be done as prescribed in IS 3025 sphates more so than orthophosphates), chromium,
(Part 1). The sampling bottles shall be cleaned zinc in concentrations exceeding 10 times that of iron,
thoroughly with dilute nitric acid (6N), prior to the cobalt and copper in excess of 5 mgfl, and nickel in
final rinsing with water. The water samples should be excess of 2 mg/1. Bismuth, cadmium, mercury,
collected and stored preferably in polypropylene bottle molybdate, and silver precipitate phenanthroline. The
or chemically resistant glass containers. For the initial boiling with acid converts polyphosphates to
determination of dissolved iron content, filtration orthophosphate and removes cyanide and nitrite that
through 0.45 ~m membrane filter, at the time of otherwise would interfere. Adding excess
sampling, is required. The analysis of such samples is hydroxylamine eliminates errors caused by excessive
to be carried out within 24 h of sampling. For concentrations of strong oxidizing reagents. In the
preservation, the samples should be acidified with presence of interfering metals, if noticible amount of
IS 3025 (Part 53): 2003
colour or organic matter is present evaporate the volumetric flask and make upto the mark with water
sample and dissolve the residue in acid Ashing is and mix well (1.0 ml = 10.0 mg of Fe). Pipette 5.0 ml
carried out in silicon, porceline or platinum crucible stock solution into a 1000 ml volumetric flask
that have been boiled for several hours in 6 N HCI. and make upto the mark with water and mix well
Use a larger excess of phenanthroline to replace that (1.0 ml= 1.0 ~g of Fe).
complexed by the interfering metals. The presence of NOTE — Prepare standard iron solutions dail y for use.
excessive amounts of organic matter may necessitate
digestion of sample before extraction of iron. 6.4.8 Diisopropyl Ether
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IS 3025 (Part 53): 2003
6.5.5.2 For samples after digestion and extraction Interferences of cobalt, copper, nickel can be controlled
by using a very lean (hot) flame. Silicons depressed
Add 1 ml of NH20H.HC1 solution, add 10 ml the iron response, and can be overcome by the addition
ammonium acetate buffer solution and then add
of 0.2 percent calcium chloride.
10 ml 1,10 phenanthroline solution to each flask.
Ten ml of phenanthroline solution in to the volumetric 7.3 Apparatus
tlasks containing extracted iron (see 6.5.2 and 6.5.3).
Dilute to 100 ml with water, mix thoroughly and allow 7.3.1 Atomic absorption spectrophotometer with air-
to stand for 10 min. Measure the absorbance of the acetylene flames. Multi-element hollow-cathode lamp
iron-complex at 510 nm against the reagent blank or electrodeless discharge lamp for use at 248.3 nm.
prepared in an identical manner (using water instead
7.4 Reagents
of the sample solution). Determine micrograms of iron
in the solution from the absorbance reading, by 7.4.1 Hydrochloric Acid — concentrated (11 N)
referring to the calibration curve. and dilute to 1:1.
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IS 3025 (Part 53) :2003
7.4.2 Nitric Acid — concentrated (16N) and dilute Add 0.5 ml of cone nitric acid to a suitable volume of
(1 : 499). the sample taken (or the solution obtained after
digestion, which contains 50 to 60 pg iron) in a 100 ml
7.4.3 Sulp/zuric Acid — concentrated ( 36 N).
volumetric flask. Make upto the mark. Transfer the
7.4.4 Calcium Chloride Solution contents of the volumetric flask to a 150 ml beaker.
Dissolve 630 mg CaCOJ, in 50 ml of 20 percent VIV Add 25 ml CaC12solution to this. Prepare a reagent
HC1. If required, boil gently to obtain complete blank with 100 ml water. Rinse the nebulizer by
solution. Cool and dilute to 1 000 ml with water. aspirating water containing 1.5 ml cone HNO#.
Aspirate the reagent blank and carry out zero
7.4.5 Stock Iron Solution adjustment. Aspirate the sample solution and measure
Dissolve 0.100 g of iron wire in a mixture of 10 ml 1:1 the absorbance at 248.3 nm. Determine micrograms
HCI and 3 ml of cone HNO~and dilute to 1000 ml with of iron in the solution from the absorbance reading,
water in a volumetric flask (1.0 ml = 100 pg of Fe). by referring to the calibration curve.
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IS 3025 (Part 53) :2003
ANNEX A
(Foreword)
COMMITTEE COMPOSITION
Organization Representative(s)
Central Pollution Control Board, Delhi SHRIDnx BISWAS(Chairman)
(Contiuued on page 6)
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(Comimdfmrrt page 5)
Organization Representative
Member Secretary
SHRIN. K. Pm
Director (CHD), BIS
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Bureau of Indian Standards
BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality certification of goods
and attending to connected matters in the country.
Copyright
BIS has the copyright of all its publications. No part of these publications may be reproduced in any form
without the prior permission in writing of BIS. This does not preclude the free use, in the course of
implementing the standard, of necessary details, such as symbols and sizes, type or grade designations.
Enquiries relating to copyright be addressed to the Director (Publications), BIS.
Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed
periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are
needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards
should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of
‘BIS Catalogue’ and ‘Standards: Monthly Additions’.
This Indian Standard has been developed from Doc : No. CHD 32 (1012).
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