Indian Standard: Methods of Test For Coal and Coke
Indian Standard: Methods of Test For Coal and Coke
Indian Standard: Methods of Test For Coal and Coke
(103.27.8.45) VALID UP
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
(Reaffirmed!2015)!
(Reaffirmed 2020)
Indian Standard
METHODS OF TEST FOR COAL AND COKE
PART III DETERMINATION OF SULPHUR
( First Revision)
© Copyright 1970
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN. 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
( First Revision )
(Page 3, clause 0.4, line 1) — Delete the words “ISO/R157 ‘Determination of forms of sulphur in
coal’ and”.
(Page 3, clause 1.1, line 2) — Delete the words ‘and forms of sulphur’.
(PCD 7)
Indian Standard
METHODS OF TEST FOR COAL AND COKE
PART III DETERMINATION OF SULPHUR
(First Revision)
Solid Mineral Fuels Sectional Committee, CDC 14
Clulirman R~tUlllinl
DR A. LARIRI Central Fuel Relearch Institute (CSIR ),Jealgora
Vice-Ciulirman
SHRI A. K. MOITRA Central Fuel Research Institute (CSIR), Jcalgora
M.".bers
SHRI A. BANBRJEB Coal Controller, Calcutta
SHRI K. L. BANERJEE National Telt House, Calcutta
SHRI R. N. Roy (All4nIat.)
SHRI S. K. BOBE National Coal Development Corporation Ltd Ranchl
CHIEI' MINING ADVISER, RAIL- Ministry of RailwaY' '
WAY BoARD, DHANBAD
JOINT ];)IRECTOB, MEOHANI-
c.v, ENGUIEERING ( FUEL ),
RAILWAY BoARD, NIlW
DELHI ( AllmuJl. )
DR A. N. CHOWDHURY Geological Survey of India, Calcutta
SHRI A. R. DAB GUPl'A Bird & Co (Private) Ltd, Calcutta
SBRI L. D. HUGHE8 Joint Working Committee of Indian Mining AssoCI:A
tion, Indian Mining Federahon, IndiAn Collier
Owners Association, and Madhya Pradesh &.
Virlarbha Mining Association, Calcutta
SKRI R. R. KHANNA (Allmlal4)
SUN J. K.JAIN Coal Conauxnen' AIsocaation of India, Calcutta
SHRI S. K. M.A.NDAL Hindu.tan Steel Ltd, Ranchi
SBRI S. N. W UIR ( Allmlal4 )
S.RI A. K. MITRA Coal Board, Calcutta
SHIU U. N. JHA (AI""'a14)
SHRI K. G. RANGREZ Regional Reaearch Laboratory ( CSIR;. Hydeubad
SHJn K. SB8HAGIRI RAO (
DB C. V. S. RATNAM
"',,"",1. )
Neyveli Lignite Corporation LId, :~eYHJ.
SHBI N. SBLVARAJAN ( ..llmraU)
Sliln B. C. Roy GHATAE The Indian Iron and Steel Co Ltd, Calcutta
SHRI S. B. SA BitAR IllItitute of Fuels ( Indian Section ), l..alcutt..
S. SUBRAHIIANYAN
5J11lI
Con~.""r
Saal N. G. BANEBJJ:JI: Cpntral Fuel Resea"h Institute (CSIR), Jealsora
Mnrtbn$
SHBI S. P. DBAlt Dursapur Project. Ltd, Durgapur
Da S. R. Gaol. Hindu.t&n Steeol Ltd, Ranchi
S.RI A. R. P.UI'IKAR ( Alllrfl/JI' )
S8RI A. K. MITRA Coal Board, Calcutta
SKRI S. B. SUItAR ( AltnFlQI' )
Slial H. P. SAIIAXTA ~heTata fron and Steel Co Ltd, Jamahedpur
S.81 SoIlAR 51lX GUPTA Coke Oven Manasen' AuociatioD (Indian Sec-
lion ), BUl"npur
2
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
Indian Standard
METHODS OF TEST FOR COAL AND COKE
PART III DETERMINATION OF SULPHUR
(First Revision)
o. FO REWORD
0.1 This Indian Standard (Part III) (Firat Revision) was adopted by the
Indian Standards Institution on 29 Dt:cember 1969, after the draft
finalized by the Solid Mineral Fuels Sectional Committee had been
approved by the Chemical Division Council.
0.2 IS: 1350 was originally issued in 1959. Later a study of various
recommendations made by International Organization for Standardization
(ISO), as well as the experience gained with the adoption of thete
methods in the country necessitated the present revision. This standard
is now issued in three parts as follows to cover separate methods in
individual parts:
Part I Proximate analysis,
Part II Determination of calorific value, and
Part III Determination of sulphur.
0.3 To keep in line with the suggestions of ISO to avoid adoption. of
alternative methods, the titrimetric method of sulphur determination and
procedure for alkaline extraction of the same have been omitted from this
standard.
0.4 This standard is based on ISO/RI57 'Determination of forms of
sulphur in coal' and ISO/R334 'Determination of total sulphur in coal by
the Eschka method'.
0.5 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·.
1. SCOPE
1.1 This standard (Part III) prescribes the method. of telt for coal and
coke relating to the determination of total sulphur and forml of sulphur.
·ltulee for roweliog off oumerical valuee ( ,willd).
:3
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
2. TERMINOLOGY
2.0 For the purpose of this standard, the following definition shall apply.
2.1 Air-Dried Coal- The sample of coal which, for the purposes of
1nalysis, is expos(·d to the atmosphere of the laboratory to bring it in
~quilibrium with the humidity conditions prevailing in the laboratory,
so that the sample docs not lose or gain weight during weighing.
3. Q.UALITY OF REAGENTS
3.1 Unless spt·cified otherwise, pure chemicals and distilled water con-
forming to IS: 1070-1960· shall be employed in test.
NOTF. - • Pure chemicals' shall mean chemicals that do not contain impurities
which affect the n',ults of analysis.
4. SAMPLING
4.1 Methods of Sampling -- Methods of sampling shall be as prescribed
in IS: 436 (Part I)-1964t for coal and IS: 436 (Part II)-196S: for coke.
4.2 Preparation of Sample. for Tellt
4.2.0 General-- Besides the laboratory samples of coal and coke to be
used for the analysis, special samples are recommended for moisture.
4.2.1 The samples prepared in accordance with IS: 436 (Part I )-1964t
and (Part II )-1965: shall be received in sealed containers and shall
consist of the following:
a) Analysis sample of about 300 g of air-dried coal or coke, ground
to pass 212-micron IS Sieve; and
b) Special moisture sample of 1 kg of coal or 2'5 kg of coke, crushed
to pass IS Sieve 12'5 mm (C) to be sent in duplicate.
4.2.2 Where air-drying has been adopted in the preparation of the
samples, the percentage loss of moisture in this operation shall be recorded
on the labt'l together with the method of sampling used.
4.2.' Samples received in the laboratory,-if already ground to pass the
212-rnicron IS Sieve. shall ue re-sieved to verify that all the material
passes through this sieve, and then air-dried for 24 hours ana mixed and
bottled as above. Should a sample of coal or COMe be transported to any
djstance between the point of preparation and the laboratory under
conditions in which it may be shaken down and may cause segregation to
.Speclfication for water, distilled q.uality ( rluis.d ).
tNetbocb for .. mplinr of coal and coke: Part I Sampling of coal ( rlllis,d).
tMethoda for !l&mpling of coal and coke: Pact II Sampling of coke ( r,/iud ).
4
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
e
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
contents by tapping gently on the bench and cover uniformly with one
gram of Eschka mixture. Place the charged crucible into the cold muffle
furnace. Raise the temperature to 800 :i: 25°C in about one hour and
then heat for a further 90 minutes. Alternatively. place the charged
cruc·ible on the silica plate and place in the hot muffle furnace and keep
for 90 minutes. Withdraw the plate with its crucible and cool.
NOTII: - Weigh out the total of 4 I{ of E.chka's mixturr and remove from thit the
0'5 g and I g portions required for the bottom and top layers. For this purpose, calibrate
a Imall glass tube, for each batch of Esch"a', mixture, to deliver 0'5 and I g. The
layer of Eschka mixture brlow the coal mixture reduces attack of the porcelain aurfac:e
10 that extraction of sulphate with hot water il complete, even when the lurface
deterioratel. Cracking of porcelain is prevented if they are slowly cooled on removal
from the muffle by insertion in lupports of light poroul firebrick •.
Transfer the ignited mixture as completely as possible from the
crucible to a beaker containing 25 to 30 mt of water. If un burnt particles
are present, reject the determination. Wash out the crucible thoroughty
with about 50 ml of hot distilled water and add the washings to the
contents of the beaker.
5.1.5.2 Extraction by acid-Place a cover-glass on the beaker, and then
carefully add sufficient concentrated hydrochloric acid ( 17 ml wilJ .Iormally
be required,) to dissolve the solid matter, warming the contents of the
beaker to effect solution. Boil for 5 minutes to expel carbon dioxide and
filter through a filter pad or medium textured double acid-washed filter
paper. collecting the filtrate in a 400-011 conical beaker. Wash the residue
on the filter pad or filter paper with four 20-ml portions of hot distilled
water. To the combined filtrate and washings, add/2 to 3 drops of methyl
red indicator and then add cautiollSly ammonium hydroxide solution until
the colour of the indicator changes and a trace of precipitate is formed.
Add sufficient amount of concentrated hydrochloric acid to just redissolve
the precipitate and then add one millilitre in excess.
5.1.5.3 Precipitation of barium lulplrfJl4- If necessary, make up the
volume of the solution to approximately 300 ml with water. Cover the
beaker and heat until the solution boils and then reduce the heating
slightly until ebullition ceases. Then add within approximately 20
seconds, 10 ml of barium chloride solution from a pipette held such -that the
barium chloride falls into the middle of the hot solution which is being
agitated. Keep the solution just below boiling point, for 30 minutes
(III 5.1.5.6).
5.1.5.f Filter, using one of the following techniques:
i) By gravity, through an ashlen fine-textured double acid-
washed tilter paper in a fluted, long-stemmed 60" funnel
(Whatman No. 42 filter paper is suitable for thie purpose ).
or
ii) Under suction, using good quality asbeeto. in a Gooch crucible
which has been dried for one hour at 130:1: 10"0 and
weighed.
7
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
8
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
9
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
10
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
Wash the filter with hot distilled water, using not more than 250 ml,
until 20 ml of the washings give not more than a faint opalescence with
silver nitrate solution. Place the wet filter paper in an ignited and weighed
silica or platium carsule on the silica plate and insert into the mume furnace
for 15 minutes at 800 ± 25° e. If a Gooch crucible is used, dry it for one
hour at 130 ± lOoC. Cool and weigh.
NOTII: - Carry out a blank dett!'rmination under the same conditiuns hut omittiOIJ
the malerial. Pipette 10 ml of th .. standard sulphate solution to the filtrate before
precipitation of harium sulphate. The weight of the barium lulphate found in the
blan" determination, less the equivalent of the standard solution, is deducted rrom
that obr:lined in the full determination.
11
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
WATER
INLET
• t'""\._--....
..
20
7S
12
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18
wherE'
A =-, weight ill g of barium sulphate found in the detf'rmination;
B = weigh ill g of barium sulphate found in the blank deter-
mination, less that due to addition of standard sulphate;
and
W = weight in g of material taken filr the test under 5.2.4.1.
l' -- V
b) 'Pyritic' sulphur, perc!'nt by weight = . ~\' _ W· 0'115
where
U = volume in ml of standard potassium dichromate solution
equivalent to the total iron (see 5.2.4.2),
V = volume in ml of standard potassium dichromate solution
equivalent to the non-pyritic iron (set! 5.2.4.1 ),
X = weight in g of the material taken for the test under 5.2.4.2,
and
W = weight in g of the material taken for the test under 5.2.4.1.
c) rOr.~anic' sulphur - Deduct the sum of the percentages of ' sulphate'
and 'pyritic' sulphurs [see 5.2.5 (a) and (0) 1from the percentage of
total sulphur in the coal obtained in a separate determination by
the Eschka method (set 5.1) and report as 'organic' sulphur.
IS
BOOK SUPPLY BUREAU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18 (103.27.8.45) VALID U
AU UNDER THE LICENSE FROM BIS FOR INDIAN INSTITUTE OF TECHNOLOGY - DELHI ON 20/11/2021 11:25:18