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भारतीय मानक IS 3025 (Part 24/Sec 1) : 2022

Indian Standard

जल एवं अपशिष्ट जल के नमूने लेने तथा

परीक्षण ( भौतिक एवं रसायन ) की पद्धतियां
भाग 24 सल्फे ट्स
अनुभाग 1 ग्रैविमेट्रिक एवं टर्बिडिटि विधियाँ
( दसू रा पनु रीक्षण )

Methods of Sampling and Test

( Physical and Chemical ) for Water
and Waste Water
Part 24 Sulphates
Section 1 Gravimetric and turbidity methods

( Second Revision )

ICS 13.060.50

© BIS 2022

भारतीय मानक ब्रयू ो

B U R E A U O F I N D I A N S TA N D A R D S
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Water Quality Sectional Committee, CHD 36

FOREWORD
‘This Indian Standard (Part 24/Sec 1) (Second Revision) was adopted by the Bureau of Indian Standards, after the
draft finalized by the Water Quality Sectional Committee had been approved by the Chemical Division Council’.
Sulphates are present in natural water in low to high concentration. Drainage from mines may have high
concentration of sulphates due to pyrite oxidation. Sulphates also found in effluents from industries. High
concentration of sulphates produce cathartic action when associated with sodium and magnesium.
The Technical Committee responsible for formulation of IS 3025 : 1964 ‘Methods of sampling and test (physical
and chemical) for water used in industry’ and IS 2488 (Part 3) : 1968 ‘Methods of sampling and test for
industrial effluents decided to revise the standard and publish it in separate parts. This standard superseded 6 of
IS 2488 (Part 3) : 1968 and 20 of IS 3025 : 1964 and was one among the different parts published under
IS 3025 series of standards. The first revision of this standard was published in 1986 which prescribed three
methods for detection of sulphates in water and wastewater.
In this second revision the following major modifications have been made:
a) This standard has been renumbered as Part 24/Sec 1 as other sections will be developed for instrument
based methods;
b) Thorin method removed – use of green chemistry concept prohibits use of toxic reagents, thus this method
has been deleted; and
c) Turbidity method has been revised.
In the preparation of this standard, considerable assistance has been derived from the method No. 4500- SO42- C
and E of ― Standard Methods for the Examination of Water and Wastewater, published by the American Public
Health Association, Washington, USA, 23rd Edition, 2017.
ISO 15923-1 : 2013 exists for turbidimetric detection of sulphates, however it is not adopted as the ISO standard
includes determination of other dissolved anions as well. ISO 10304-1 : 2007 exists for determination of sulphates
using liquid ion chromatography and ISO 22743 : 2006 exists for determination of sulphates using continuous
flow analysis.
The composition of the committee, responsible for the formulation of this standard is given at Annex A.
In reporting the results 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 ʻRules for rounding off numerical
values ( revised )’.
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IS 3025 (Part 24/Sec 1) : 2022

Indian Standard
METHODS OF SAMPLING AND TEST
( PHYSICAL AND CHEMICAL ) FOR WATER
AND WASTE WATER
Part 24 Sulphates
Section 1 Gravimetric and turbidity methods

( Second Revision )

1 SCOPE 4.2 Principle

Sulphate is precipitated in hydrochloric acid medium
1.1 This standard (Part 24/Sec 1) specifies the following
as barium sulphate by the addition of barium chloride
methods for determination of sulphates in water and
solution. The precipitation is carried out near boiling
wastewater:
temperature and after a period of digestion, the
a) Gravimetric method; and precipitate is filtered and washed with distilled water
b) Turbidity method. until free of chlorides. It is then ignited or dried and
weighed as barium sulphate (BaSO4).
2 REFERENCES The reaction in its simplest form is:
The following standards contain provisions which
HCl medium
SO42- + BaCl2 -------------------- BaSO4 ↓ + 2Cl-
through reference in this text constitute provisions of
this standard. At the time of publications, the editions
indicated were valid. All standards are subject to 4.3 Interferences
revision, and parties to agreements based on this Suspended matter, silica, barium chloride precipitant,
standard are encouraged to investigate the possibility nitrate and sulphite are the principal factors in positive
of applying the most recent editions of the standards error. Alkali metal sulphates and heavy metals, such
indicated below: as chromium and iron, cause low results. To minimize
solubility of barium sulphate, the acid concentration
IS No. Title should be minimum while precipitating barium
sulphate.
3025 (Part 1) : 1987 Methods of sampling and test
(physical and chemical) for 4.4 Sampling and Storage
water and wastewater: Part 1 Sampling and storage shall be done as prescribed in IS
Sampling 3025 (Part 1). Highly polluted or contaminated samples
7022 (Part 1) : 1973 Glossary of terms relating to should be stored at low temperature or treated with
water, sewage and industrial formaldehyde. Sulphite may be oxidized to sulphate
effluents: Part 1 by dissolved oxygen above pH 8.0; samples containing
sulphite should have their pH adjusted below this value.
7022( Part 2) : 1979 Glossary of terms relating to
water, sewage and industrial 4.5 Apparatus
effluents: Part 2
4.5.1 Steam Bath
3 TERMINOLOGY
4.5.2 Drying Oven, equipped with thermostatic control.
‘For the purpose of this standard, the definitions given
in IS 7022 (Part 1) and IS 7022 (Part 2) shall apply’. 4.5.3 Muffle Furnace, with heat indicator.
4.5.4 Desiccator
4 GRAVIMETRIC METHOD
4.5.5 Analytical Balance, with least count of 0.1 mg.
4.1 Applicability
This method is applicable for all the waters having 4.5.6 Filter Paper, acid washed, ash-less hard finish
sulphate concentrations above 10 mg/l; however, it is a filter paper sufficiently retentive for fine precipitates
time consuming method. (preferably Whatman No. 42/equivalent).

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IS 3025 (Part 24/Sec 1) : 2022

4.5.7 Crucible, porous bottom silica or porcelain 4.6.4 Silver Nitrate – Nitric Acid Reagent.
crucible with a maximum pore size of 5 microns. Dissolve 8.5 g of silver nitrate and 0.5 ml of nitric acid
4.5.8 Ion-Exchange Column, see Fig. 1 for details. The in 500 ml distilled water.
exchange column should be regenerated by passing
hydrochloric acid (see 4.6.2) solution after five or 4.6.5 Ion Exchange Resin, strong cation exchange
six samples have passed through the column, followed resin, amberlite IR-120 or equivalent.
by washing with distilled water. 4.7 Sample Preparation
4.7.1 The sample used for analysis should either be free
from turbidity or filtered through 0.45 µm filter.
4.7.2 If the total cation concentration in the sample
is more than 250 mg/l or if the total heavy metal ion
concentration is more than 10 mg/l, pass the sample
through a cation removing ion exchange column.
4.7.3 If the silica concentration exceeds 25 mg/l,
evaporate the sample nearly to dryness in a platinum
dish on a steam bath. Add 2 ml hydrochloric acid
solution (see 4.6.2), tilt the dish and rotate it until the
acid comes in contact with the residue; continue the
evaporation to dryness. Complete the drying in an
oven at 180 °C and if organic matter is present, char
over the flame of a burner. Moisten the residue with
2 ml distilled water and 2 ml hydrochloric acid solution
(see 4.6.2) and evaporate to dryness on steam bath.
Add 5 ml hydrochloric acid solution (see 4.6.2), take
up the soluble residue in hot water and filter. Wash
the insoluble silica with several small portions of hot
distilled water. Combine the filtrate and washings.
4.8 Procedure
4.8.1 Adjust the clarified sample, treated if necessary
to remove interfering agents, to contain approximately
100 mg of sulphate ion in 500 ml volume.
4.8.2 Add 2 to 3 drops of methyl red indicator solution
(see 4.6.1). Add hydrochloric acid solution (see 4.6.2)
drop by drop till an orange red colour appears. Lower
concentrations of sulphate ion may be tolerated if it is
impracticable to concentrate the sample to the optimum
All diameter in millimeters
level, but in such cases it is better to fix the total volume
Fig. 1 Ion Exchange Column at 150 ml after concentration on hot plate.
4.6 Reagents 4.8.3 Heat the solution to boiling, while stirring
gently, add warm barium chloride solution (see 4.6.3)
4.6.1 Methyl Red Indicator slowly until precipitation appears to be complete, then
Dissolve 100 mg methyl red sodium salt in distilled add about 2 ml in excess. Digest the precipitate at
water and dilute to 100 ml. 80-90 °C for at least 2 h.
4.6.2 Hydrochloric Acid Solution (1 : 4) 4.8.4 Filtration
Dilute one volume of concentrated hydrochloric acid Filter the precipitate through filter paper (see 4.5.6)
with four volumes of distilled water. and wash the precipitate with small portion of warm
distilled water until the washings are free of chloride
4.6.3 Barium Chloride Solution ions as indicated by testing with silver nitrate-nitric
Dissolve 100 g of barium chloride (BaCl2 . 2H2O) in acid reagent (see 4.6.4).
1 l distilled water. Filter through a membrane filter or
4.8.5 Transfer the filter paper along with the precipitate
hard finish filter paper (1 ml of this reagent is capable
in the crucible and dry the precipitate and ignite at
of precipitating approximately 40 mg SO42-).
800 °C for 1 h.

2
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IS 3025 (Part 24/Sec 1) : 2022

NOTE — Do not allow the filter paper to flame. 5.5.2 Photometer (use one of the following, given in
4.8.6 Cool in a desiccator and weigh. order of preference):
(a) Nephelometer
4.9 Calculation
(b) Spectrophotometer, for use at 420 nm with light
The concentration of sulphates in the sample from the path of up to 5 cm.
equation:
m × 411.5 5.5.3 Stopwatch, to be used if magnetic stirrer is not
sulphate concentration as mg/l BaSO4 = equipped with an accurate timer.
V
where
5.5.4 Measuring Spoon, capacity from 0.2 ml to 0.3 ml.
m = mass of BaSO4, in mg; and
V = volume of sample, in ml. 5.6 Reagents

5 TURBIDITY METHOD 5.6.1 Buffer Solution. Dissolve 30 g magnesium chloride

(MgCl2.6H2O), 5g Sodium acetate (CH3COONa.3H2O),
5.1 Applicability and Range 1 g Potassium nitrate (KNO3)and 20 ml acetic acid
(CH3COOH)in distilled water in a 500 ml volumetric
5.1.1 This method is applicable to ground water, flask and make up volume up to 1 000 ml.
drinking and surface waters as well as domestic and
industrial wastes. 5.6.2 Standard Sulphate Solution
Dissolve 0.1479 g anhydrous Na2SO4 in distilled water
5.1.2 This method can be applied for all concentration
and dilute to 1000 ml (1 ml = 100 µg SO4 2-).
ranges of sulphate; however readings are accurate for
sample aliquots containing not more than 40 mg/l of 5.6.3 Barium Chloride, crystals, 20 to 30 mesh.
SO42-.
5.7 Procedure
5.1.3 The minimum detectable limit is approximately
1 mg/l SO42-. 5.7.1 Preparation of Calibration Curve

5.2 Principle Take 1.0 ml, 5.0 ml, 10.0 ml, 20.0 ml and 40.0 ml
of the standard sulphate solution (see 5.6.2) into
Sulphate ion is converted into barium sulphate 250 ml conical flasks and make up to the 100 ml
suspension under controlled conditions. This mark with distilled water. Take 100 ml distilled water
suspension can be measured by using a nephelometer in a 250 ml flask for preparing distilled water blank.
or spectrophotometer and light absorbance is measured The concentration of the standards corresponding to
at different concentrations; sample concentrations may 1.0 ml, 5.0 ml, 10.0 ml, 20.0 ml and 40.0 ml standard
be evaluated from standard curve. sulphate solution (1 ml = 100 μg SO4 2-) are 100 μg
(1 mg/l), 500 μg (5 mg/l), 1000 μg (10 mg/l), 2000 μg
5.3 Interferences
(20 mg/l) and 4000 μg (40 mg/l) respectively. Add
5.3.1 Suspended matter if present in large quantity may 10 ml of buffer solution (see 5.6.1) and mix using
interfere and hence sample has to be pre filtered for magnetic stirrer. While stirring, add a spoonful of BaCl2
reliable result. crystals (see 5.6.3) and begin timing immediately. Stir
for 30 seconds at constant speed. After stirring has
5.3.2 Silica in excess of 500 mg/l will interfere in
ended, pour the solution into absorbance cell. Measure
precipitation.
turbidity at 420 nm against distilled water in 30 seconds
5.3.3 Large quantity of organic materials and color of interval for 5 minutes. Record the maximum reading
the sample will interfere with this method and have to obtained in the 5 min period. The corrected absorbance
be accounted for by use of blanks. readings of the standard solutions are obtained by
subtracting the absorbance readings of the standard
5.4 Sampling and Storage solutions from that of distilled water blank. Plot the
Sampling and storage shall be done as prescribed in corrected absorbance readings of the standard solutions
IS 3025 (Part 1). The bottles shall be capped tightly as against concentrations.
soon as the sample is collected.
5.7.2 SampleAnalysis
5.5 Apparatus
5.7.2.1 Measure 100 ml sample, or suitable portion
5.5.1 Magnetic Stirrer, constant stirring speed so that it made up to 100 ml into a 250 ml conical flask. Prepare a
can be held constant just below splashing. Use identical distilled water blank by taking 100 ml distilled water in
sizes and shapes of magnetic stirrer bars. another 250 ml conical flask. Add 10 ml buffer solution

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IS 3025 (Part 24/Sec 1) : 2022

(see 5.6.1) and mix using magnetic stirrer. Follow 5.8 Calculation
the next procedures as done for standard solutions. The concentration of sulphate (as SO42-) in
Measure the absorbance reading of sample and distilled
water blank against distilled water as reference. The A × 1000
corrected absorbance reading of sample is obtained by mg/l =
V ×k
subtracting absorbance reading of distilled water blank where
from that of sample. A = corrected absorbance reading of sample;
5.7.2.2 For samples having turbidity or colour, prepare k = slope from calibration curve; and
a sample blank by taking 100 ml of the turbid or V = volume of sample taken (in ml).
colured sample in a 250 ml conical flask. Add 10 ml of If the sulphate content of sample is found to be greater
buffer solution (see 5.6.1) and take absorbance reading than 10 mg/L, then the sample analysis is repeated using
at 420 nm (without adding BaCl2) against distilled buffer solution A. A distilled water blank is prepared
water as reference. The corrected absorbance reading by using buffer solution A. The corrected absorbance
of sample is obtained by subtracting the absorbance reading of sample is obtained by subtracting absorbance
reading of distilled water blank and sample blank from reading of distilled water blank from absorbance
the observed absorbance reading of sample. reading of sample.

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IS 3025 (Part 24/Sec 1) : 2022

ANNEX A
( Foreword )
COMMITTEE COMPOSITION
Water Quality Sectional Committee, CHD 36

Organization Representative(s)

Chief Scientist, EPTRI, Hyderabad Shri N. Raveendhar (Chairman)

Avantha Centre for Industrial Research and Dr Nishi Kant Bhardwaj
Development, Yamuna Nagar Dr Sunil Kumar (Alternate)
Bhabha Atomic Research Centre, Mumbai Dr S. K. Sahu
Shri I. V. Saradhi (Alternate)
Central Ground Water Board, Faridabad Shri G. C. Pati
Shrimati Rumi Mukherjee (Alternate)
Central Institute of Mining and Fuel Research, Dr (Mrs) Bably Prasad
Dhanbad Dr Abhay Kumar Singh (Alternate)
Central Pollution Control Board, New Delhi Shri N. C. Durgapal
Dr J. C. Babu (Alternate)
Confederation of Indian Industry, New Delhi Shri Shikhar Jain
Ms Kamal Sharma (Alternate)
Delhi Technological University, New Delhi Dr (Mrs) Anubha Mandal
Delhi Jal Board Shri D. R. Arya
Shri Sanjeev Kumar (YP) (Alternate)
Department of Civil Engineering, IIT Madras Dr Ligy Philip
Dr S. Mathava Kumar (Alternate)
Envirocare Laboratories Pvt Ltd, Thane Dr Priti Amritkar
Shri Nilesh Amritkar (Alternate)
Environment Protection and Training Research Dr J. S. Sriniva
Institute, Hyderabad
Member Secretary, FAD 14 Ms Nitasha Doger
Gujarat Pollution Control Board, Gandhinagar Dr D. N. Vansadia
Shri K. B. Vaghela (Alternate)
Himachal Pradesh State Pollution Control Board Dr D. K. Sharma
Shri Harish Sharma (Alternate)
In personal capacity (1221, Mahatma Gandhi Road, Shri Sanjib Kumar Goswami
P. O. - Haridevpur, Kolkata, 700082)
In personal capacity (House No. 514, SSST Nagar, Dr H. K. Parwana
Rajpura Road, Patiala 147003)
Indian Agricultural Research Institute – Water Dr Khajanchi Lal
Technology Centre, New Delhi Dr Ravinder Kaur (Alternate)
Indian Chemical Council, Mumbai Shri J. I. Sevak
Dr Mritunjay Chaubey (Alternate I)
Dr N. D. Gangal (Alternate II)
Indian Council for Agricultural Research, New Delhi Dr M. J. Kaledhonkar
R. K. Yadav (Alternate)
Indian Institute of Toxicology Research, Lucknow Dr S. C. Barman
Dr Satyakam Patnaik (Alternate)
Indian Water Works Association Shri Vijay Charhate

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IS 3025 (Part 24/Sec 1) : 2022

Organization Representative(s)

Karnataka State Pollution Control Board, Bengaluru Dr B. R. Balagangadharan

Dr H. Rupadevi (Alternate)
Maharashtra State Pollution Control Board, Mumbai Dr V. R. Thakur
Shri S. C. Kollur (Alternate)
National Environmental Engineering Research Dr S. K. Goyal
Institute,Nagpur Dr P. K. Labhasetwar (Alternate I)
Dr Noor A. Khan (Alternate II)
NTPC Ltd, New Delhi Shri V. Ravi Babu
Shri Sudhir Dahiya (Alternate I)
Sriram Institute for Industrial Research, New Delhi Ms Shobha Kumar
Shri Sumant Shekhar (Alternate)
Telangana State Pollution Control Board, Hyderabad Shri N. Murali Mohan
West Bengal Pollution Control Board, Kolkata Dr Ujjal Kumar Mukhopadhyay
Shri Shyam Kumar Adhikari (Alternate)
BIS Directorate General Shri Ajay Kumar Lal, Scientist ‘E’ and Head (CHD)
[ Representing Director General ( Ex-officio ) ]

Member Secretary
Ms Shubhanjali Umrao
Scientist ‘B’ (CHD), BIS

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development of the activities of standardization, marking and quality certification of goods and attending to
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standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating to
copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards

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 36 (12616).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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