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IS 11255 (Part 4): 2006

(Reaffirmed - 2012)
(Reaffirmed 2017)
(Reaffirmed 2022)

Indian Standard
METHOD FOR MEASUREMENT OF EMISSION
FROM STATIONARY SOURCES
PART 4 HYDROGEN SULPHIDE AND CARBON DISULPHIDE

(First Revision)

ICS 13.040.40

Q BIS 2006

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

November 2006 Price Group 3

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In\ ironment Protect ion 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.

Carbon disuiphide and hydrogen sulphide are emitted together in processes like cellulosic fibre manufacture. This
standard prescribes a method for determination of these gases in presence of one another.

This standard was originally published in 1985. With a view to upgrade the standard based on the technological
developments in this area, this revision is brought out incorporating the details of the apparatus required for
testing and calculations for more clarity and better accuracy. The precision of the methods are yet to be established.
Aqueous tension at various temperatures are also incorporated in the standard.

There is no 1S0 Standard on the subject. The standard has been developed based on the indigenous methods
avaiiable in India.

The composition of the Committee responsible for the 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 11255 (Part 4) :2006

Indian Standard
METHOD FOR MEASt JREMENT OF EMISSION
FROM STATIONARY SOURCES
PART 4 HYDROGEN SULPHIDE AND CARBON DISULPHIDE

(First Revision )

1 SCOPE 4.2 Gas Meter — wet type, graduated so that one

revolution is equivalent to 0.5 Iitre.
This standard prescribes a method for the measurement
of carbon disulphide and hydrogen sulphide in presence 4.3 Gas Sample Container — of glass, fitted with a
of each other. single way stopcock on the entry and exit leads.

2 PRINCIPLE 4.4 Glassware— Erlenmeyer Flask-capacity 500 ml,

burette 50 ml, measuring cylinders.
2.1 Hydrogen sulphide is absorbed in alkaline
cadmium chloride solution and the cadrnhun sulphide 4.5 Wash Bottle
formed is estimated iodometrically. The reactions
involved are: 5 REAGENTS

CdC12 + H,S — CdS + 2HCI 5.1 Cadmium Chloride Solution — Dissolve 10 g

of cadmium chloride in 450 ml of distilled water to
CdS + 2HCI — CdCl, + H2S
which 10 ml 0.5 N sodium hydroxide solution is
H2S + I, — 2HI+S
added.
2.2 Carbon disulphide is absorbed in alcoholic NOTE — Cadmium sulphate solution (5 percent) may also be
potassium hydroxide solution forming potassium used, if cadmium chloride ia not available.
ethylxanthate. The xanthate is estimated iodometrically.
5.2 Iodine Solution — 0.005 N, standardized against
The reactions involved are:
the standard sodium thiosulphate solution.
CS2 + KOH + C2HjOH — KSCSOCzH~ + H20
5.3 Sodium Thiosulphate Solution — 0.005 N,
2 KSCSOCaH~ + Iz — 2KI + (SCSOCZHJ2
standardized against standard potassium bichromate
3 OUTLINE OF METHOD solution.

The air is passed through an absorber train of five 5.4 Potassium Bichromate Solution — 0.005 N.
absorbers, the first three absorber containing 30 ml 5.5 Potassium Iodide Solution — 20 percent.
each of alkaline cadmium chloride solution and the
last two containing 30 ml each of 5 percent alcoholic Dissolve 20 g of potassium iodide in 100 ml of distilled
potassium hydroxide solution. The first three water.
absorbers arrest H2S and the last two absorbers arrest NOTE — This solution should be prepared fresh.
CS2 in the sample. After passing the air sample (about
8 Iitres), the HZS in the first three absorbers and the 5.6 Hydrochloric Acid — Concentrated.
CS2 in the last two absorbers are estimated by treating
5.7 Alcoholic Potassium Hydroxide Solution —
with standard iodine solution and titrating back the
Dissolve 5 g of potassium hydroxide in 2-3 ml of water
excess iodine with standard sodium thiosulphate
and dtlute to 100 ml with absolute ethyl alcohol.
solution.
NOTE — This solution should be prepared fresh j ust before
4 APPARATUS scrubbing the air.

4.1 Absorbers — Five Drechsel bottles (see Fig. 1), 5.8 Acetic AcM — 5 percent.
capacity 250 ml each.
5.9 Starch Solution — Dissolve about 0.1 g starch
NOTE — Gas scmbbers containing sintered glass plates are in 25 ml hot distilled water and cool before use.
not recommended for this method owing to the difllculty of
removing the precipitate from the sintered plate. NOTE — This solution is to be prepared fresh.

1
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1S 11255 (Part 4) :2006

250 ml

3 7*lmm

FIG. 1 DRECHSELBOTTLE

5.10 Phenolphthalein Indicator, 1 percent — 6.2 Standardization of Sodium Thiosulphate

Dissolve 1.0 g phenolphthalein in 100 ml of 50 percent Solution
ethyl alcohol.
Fill the burette with sodium thiosulphate solution and
5.11 Sodium Bicarbonate adjust the liquid level to the zero mark. Put 5-7 ml of
20 percent potassium iodide solution and 10-15 ml of
6 PROCEDURE 2 N sulphuric acid using measuring cylinder into 500 ml
6.1 Sampling coilical flask. Add 25 ml of potassium bichromate
(0.005 N) solution by a transfer pipette, add 0.5 g
Set up the absorber train with five absorbers in series, the sodium bicarbonate quickly, cover the flask with a
fwst three containing 30 ml of alkaline cadmium chloride watch glass and leave the mixture for 5 min in a dark
solution each and the last two absorbers containing 30 ml place. Then remove the watch glass and rinse it with
of alcoholic potassium hydroxide solution each, with the distilled water into the flask. Dilute the content with
gas meter to measure the air flow on line. Regulate the distilled water titrate with sodium thiosulphate solution
flow of the sample at 0.5 litre per minute and pass about 8 using starch indicator. Calculate the strength of the
Iitre of sample. Disconnect the sample container and the thiosulphate using the formula:
gas meter. Take the first three absorbers in the train for
N, V, = NZVZ
the estimation of hydrogen sulphide and the last two for
the estimation of carbon disulphide. where

NOTE — Care has to be taken for exposure to light. N, = normality of sodium thiosulphate;

2
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IS 11255 (Part 4) :2006

V, = volume of the thiosulphate consumed for alcohol. Neutralize the content with 5 percent acetic
25 ml of potassium bichromate solution, acid using the phenolphthalein indicator. The acid
in ml; solution must be added slowly keeping the flask
Nt = normality of potassium bichromate solution; immersed in an ice bath during neutralization. After
and neutralization add starch and immediately titrate with
Vz= volume of potassium bichromate solution. standardized iodine solution. For clear end point, dilute
the content with 4 times volume of ice cooled distilled
6.3 Determination of the Strength of Iodine Solution water. Run a blank taking 60 ml alcoholic potassium
hydroxide in place of absorber content and following
Titrate 25 ml of Iodine solution in a conical flask with
exactly the above procedure.
standard sodium thiosulphate (0.05 N) using starch
indicator. Calculate the strength of the iodine solution NOTE — Alcoholic potassium hydroxide solution should be
fresh every time. During neutralization of potassium
using the formula:
ethylxanthate with acetic acid and prior to titration with iodine
N, V, = Nz Vz the soIution should be kept in ice bath.

where 7 CALCULATIONS

N, = normality of sodium thiosulphate, 7.1 Hydrogen Sulphide

V, = volume of the thiosulphate consumed for Subtract the volume of sodium thiosulphate solution
25 ml of iodine solution, in ml; consumed f.om that required for a blank. Find out the
N2 = normality of iodine solution; and equivalent volume of iodine solution to this difference.
V2= volume of iodine solution, This volume is the amount of iodine solution consumed.

6.4 Determination of Hydrogen Sulphide Concentration of

HZS, ppm, v/v = (17/1 000)x Al x B] x (24 450/34)
Transfer the contents of the first three absorbers into a x (1/1 000)x (1OW)
500 ml Erlenmeyer flask. Rinse the absorbers with little
distilled water. Collect the rinsed water into the same
= (12400x A, XB1)/(Vx F)

flask and then add 25 ml standardized iodine solution where

and 5 ml of concentrated hydrochloric acid. Wait for
Al = volume of iodine solution consumed;
10 min and then titrate the excess iodine with standard
sodium thiosulphate solution using starch indicator. Run 2?1= normality of the iodine solution:
a blank simultaneously with 90 ml cadmium chloride V = volume of the air sample passed, in Iitres; and
solution to which 25 ml of standardized iodine solution F = dryness factor calculated from barometric
and 5 ml concentrated hydrochloric acid are added. pressure and temperature.
Wait for 10 min and titrate the excess iodine with = (PB -fl/PB
standard sodium thiosulphate solution using starch where
indicator.
PB= barometric pressure, and
6.5 Determination of Carbon Disulphide f = aqueous tension.

Transfer the contents of last two absorbers into a 500 ml Aqueous tension values at different temperatures are
Erlenmeyer flask. Rinse the absorbers with little given in Table 1.

Table 1 Water Vapour Pressure (Aqueous Tension) at Various Temperatures

Temperature Vapour Pressure Temperature Vapour Pressure

“c / A Y ‘c A
e \
(mm of Hg) (millibar) (mm of Hg) (millibar)
(1) (2) (3) (19 (2) (3)
16.0 13.6 18.1 28.0 28.3 37,-I
18,0 15.5 20.6 30.0 31.8 42.4
20.0 17.5 23.3 32.0 35.7 47.6
22.0 19.8 26.4 34.0 39.9 53.2
24.0 22.4 29.4 36.0 44.6 59.5
26.0 25.2 33.6 38.0 49.7 66.3

3
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IS 11255 @art 4): 2006

7.2 Carbon Disulphide where

Subtract the volume of sodium thiosulphate solution A2 = volume of iodine solution consumed in ml;
consumed fkom that required for a blank. Find ~llf the B2 = normality of the iodine solutio~
equivalent volume of iodine solution to this difference. V = volume of the air sample paased in litres; and
This volume is the amount of iodine solution F = dryness factor calculated from barometric
consumed. pressure and temperature (see 7.1),

Concentration of 8 PRECISION
CSZ (pp~ V/V) = (76/1 000)xAzxB2X(24450/76)
The precision of this standardis not established due to
x (1/1 000)x (1OW)
the difficulties in handling samples and the reactivity
= (24 800x A2 x BJ(V xo of hydrogen sulphide with the sample vessels.

ANNEX A
(Foreword)
COMMITTEE COMPOSITION
Environment Protection and Waste Management Sectional Committee, CHD 32

Organization Representative(s)

In personal capacity (40/14, C. R. Park, New Delhi 110019) PROFDILIPBISWAS

(Chairman)

Bhabha Atomic Research Centre, Mumbai DR (Smrmn) G G PANorr

DR L V: SARAOHJ
(Alternate)

Bharat Heavy Electricsds Limited, Hardwar DiI N. G SHJUVASTAVA

Cement Manufacturers’Association,New Delhi DR K. C. NARANO
Central Fuel Research Institute, Dhanbad DR L. C. RAM
Central Lesther Research Institute, Chennai DR S. RAJAMANI
Central Pollution Control Board, New Delhi DR S. D. MAKHUANI
DR C. S. SNARMA (Alternate 9
DR S. K. TYAGI(Afternate II)

Central Road Research Institute, New Delhi SHRJMATI

ANURADHA
SHUKLA
Confederation of Indiao Industries, New Delhi SNRJA. K. GHGSE
SHSUR. P. SHARMA
(Alternate)

Crop Care Federation of Indi& New Delhi SHRI P. N. PARMSSHAWARAN

Department of Civil Engineerin& Indian Institute of Technology, DR MUKESH

KHARS
Ncw Delhi DRATULMrrrAL(Afternate I)
DRARVJND
NEMA(Afternate II)
Delhi College of Engineering, Delhi DR RARESHMEHROTRA
SHRIV. K. MSNOCHA(Alternate 1)
DR (SHRJMATI)
A. MANDAL (Alternate II)

Delhi Jal Board, Delhi THS CHIEFENGJNEER

(SSWER)
Dmctomte General, Factory Advice Service arrd Labour Institute, SHRJS. S, GAUTAM
Mumbai SHRIBRJJMOHAN(Alternde)
Directorate General of Health Services, New Delhi DR (SHJUMATJ)
MADHUIW
SHARMA
Engineers India Limited, New Delhi SNRJB. B. LAL
SHRISUSHEELSADH(Alternate)
Envirotech Instruments Private Limited, New Delhi Stuu RAKESH
AGARWAL
DR RAJSNDJLA
PRASAD
(Alternate)

4
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IS 11255 (Part 4) :2006

Organization Representative(s)

Federation of Indian Chambers of Commerce & Industry (FICCI), Ms ANTARA

ROY
New Delhi
Gujarat Pollution Control Board, Ahmedabad SHJUD, C. DAVE
Hinduatan Lever Limited, Mumbai SHCUB. B. DAVE
SHRtADtTVAJHAVAR
(Alternate)
Indian Centre for Plaatics in the Environment, Mumbai Swu S. P. CHAKRARORTY
SHRJT. K. BANDYOPADHAYAY
(A/lemate)
Indian Cbernical Manufacturers’ Association, Mumbai SHRJPRAXASH WAGLE
SHRJA. A. PANJWANI
(Wfemafe)
Indian Council of Agricultural Research, New Delhi DR R. C. MAHESHWARJ
Indian Council of Medical Research, New Delhi DR H. N. SAIYAD
Indian Oil Corporation Limited, Faridabad DR M. P. StNGH
IPCL, Vadodara SHRtANUPAMDESAI
SHRJMtHtRBANERJI
(Alternate)
Industrial Toxicology Research Centre, Lucknow DR S. K. BHARGAVA
Ministry of Defencce (R&D), DRDO, New Delhi SHRJ J. C. KAPOOR

Ministry of Environment and Foresta, New Delhi IL125E5ENTATNE

Ministry of Non-Conventional Energy Sources, New Delhi Smu VtNODKUMARJAtN

Town & Country Planning Organization, Ministry of Urban SHRJK. K. JOADDER
Development, New Delhi DR SAN?OSHVtDHVA
DHARAN
(Alfemare)

Municipal Corporation of Delhi, Delhi SW RAW DASS

SHPJSURENDER
PAL(Alfernafe)
Municipal Corporation of Greater Mumbai, Mumbai DEPUTYCrTYE~OtNEER
CtvrL (ENVT)
DEPUTYEX~tVE ENGINEER
(EMISSION
LWENTORYGROUP)(Mfernafe)
National fnstitute of Occupational Health (lCMR), Abmedabad DR V. KJUSHNA
MURTHY
DRA. K. MUKHERJEE
(Aliernafe)
National Environmental Engineering Research Institute, Nagpur DR V. I. PA~DIT
DR TAPANNA~DY(Ahemafe)
National Thermal Power Corporation Limited, New Delhi SHRJR. GOPAL
NCCBM, New Delhi SHRJM. S. BHAGWAT
DR S. N. PATI(Alternate)
Reliance Industries Llmitcd, Mumbai DR E. SUNDERASAN
DR U. K. SARGGP
(Alternate)

Shriram Institute of fnduatrial Research, New Delhi SHRJV. G K. NAIR

DR JAGDBHKUMAR(Ahernare)

SGS India Limited, Chennai SHR[S. RAw

Steel Authority of India Limited, New Delhi SHRIV. M. SHASTRt
SHRJK. B. LAL(Alfemafe)
l%e Energy and Resources Institute, New Delhi COLR. K. JOHRJ(RETD)
DR SONILPANDEY (Altemafe)
Thapar Centre for industrial Research and Development, Patiala DR MAHESHWAR ROY
DR S. K. CHAKRARORTV
(Altemafe)

The Fertilizer Association of India, New Delhi DR (SHIUMATI)

B. SWAMINATHA~
DR S. NAND(Alternate)
BIS Directorate General DR U. C. SRJVASTAVA, Scientist ‘F’ and Head (CHD)
[Representing Director General (Ex-ojTcio)]

Member Secretary
SHIUN. K. PAL
Scientist ‘E’ (Chemical), BIS

5
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This Indian Standard has been developed from Dot: No. ClIll 32 (111(,)).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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