Indian Standard

METHODS FOR
CHEMICAL ANALYSIS OF STEELS
P A R T 8 OLTLRMINATIOM OF SULPHUR BY EVOLUTION METHOD
( FOR SULPHUR 0'01 TO W2S PERCENT)

( Third Revision )

Third Reprint AUGUST 1997

UDC 669'14 + 669'15-1942 : 543'845

B U R E A U OF I N D I A N S T A N D A R D S
MANAK MAVAN. 9 BAHADUR SHAH ZAPAR MARC
NEW DELHI 110002
Methods of Chemical Analydr of Ferrous Metals Sectional Committee, MTD 2

FOREWORD
This Indian Standard (Part 9 ) ( Third Revision ) war ado ted by the Bureau of Indian Standard1
d'
on 26 December 1989, after the draft 5alizcd b the ethodr of Chemical Analysir of Ferrous
Metala Sectional Committee had been approved) by the Metallurgical Engineering Division
Council.
IS 228, which w u first published in 1952 and subsquently revised in 1959, covered the chemical
analysis of plaln carbon and low alloy steel:, along with ig iron and w t iron. Tht n a n d u d
f
was again r e v i d to make i t comprehensive in respect o ateel analysis and to exelude pie iron
and cart iron which are baing covered in separate standard. 14 parts have already been w e d
covering only chemical analysis of steel#.
This standard IS 228 ( Part 9 ) was publidmi in 1975. In this revision the part has been updated
and reproducibility of the method incorporated.
In reporting the result of a t a t made in accordance with thin standard, if the final value,
observed or calculated, ia to be rounded off, it shall be done in accordance with I8 2: 1960 'Rmlr
for rounding off numerical valun ( rcutrd)'.
 PsZa(P..8*)ll#

Indian Standard
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
PART 9 OLTERMlNATlON OF SULPHUR BY EVOLUTION METHOD
( FOR SULPHUR 091 T O 9 2 5 PERCENT)

( Third Revision )
1 #COPE OF 8ULPHUIL BY
5 DEIZBMINATION
EVOLrnON MFFaOD
1.1 Thh standud (Part 9 ) coven method for
determination of sulphur in plain carbon and $1 Outfie of* Method
low alloy rtwl by wolution method.
Sulphur is e.vo1ved u hydroqen sulphide and
NOTE -TUl wrhod ia not suitable l o r a t n l wp!ea precipitated u cadmium sulph~dein ammoniaul
eoocniuiq wknium. cadmium chloride solution. Sohttion is acidi5ed
and cxccar of potauium iodatrpotauium iodide
2MMPuNG is added. Excener of liberated iodine in titrated
against ~ d i u mthiorulphate.
21 Sam le shall be drawn as per relevant
Ef
Indian tandard. 5.2 R r ~ e n t s
3 QUALITY OF REAGENT8 5.2.1 Dilute tfjdmchloric Acid, 1 : 1 ( vlu ).
5.23 Ammaniacal Cadnium Uloridr Solution
S.1 Unless spsci6ed otharwk, analytical grade
rea eats and diutilled water shall be employed D~~~~~12.8 of &loride in l.Olitra
&
in e test:. of water a n i add one litre of ammonia
(rd=0'90).
4 UPARArn
5.23 Standard Io&U Sokrl~nn( 0'03 N )
4.1 Apparatus y shown in Fig. 1 may be wed
with leak proof pints. Dirsolve 1'07 g of potmium iodate (KIO.),
10 of potruium iodide and 2 g of tanium

n f
litre volumetric flask and make up.
5.2.4 Standard Sodium 3AiowlpkIr
P"
hy roxide in 50 ml water and traxu er to one

SoIuIhz
i 0.03 N )
of sodium thiorulphate ( Na,S,Os'
th 0'5 g of s o d i ~ ~ m
carbonate and
dissolve in 1 litre of water. Solution is standar-
dized against a imary standard solution of
potarrium iodate k . 3 ) .
500 m l
FLASK 53.5 Starch Solulion
Diuolve 0'1 g of soluble starch in 100 ml of hot
water and boil for 2 to 3 minutes and cool.

FIO. I APPAUATUI POI I ~ R L Y I N A
OF~ Ofunnel
SULPHUR BY EVOLUTION MIITHOD
C d Clz
5.3 ProC.d~w
I
SoLU"
5.3.1 Tranafer YO0 g oframple in a 500 ml dry
floreoce flask fitted properly with a rubber wrk
attached with a thistle funnd +nd delivary tube
bend at rinht annle. The end of the thiatle
N sho;ld w ; l y touch the bottom of the
flaak and delivery tube remain dipped in the
i
measuring cylinder containing 20 ml of
ammoniacal cadmium chloride solution md
80 ml of water.
Note the volume of standard r o d i w t 'o-
1ulpht4 rolotioo.
c'.
starch u indicator till blue colour is dirchu

i
5.33 Add dilute hydrochloric acid thro h 5.3.4 Qrxy out a reagent blank dmultaneowly.
thistle funnel in sv5ticnt quantity t o cover t e
sample com letely and 10me quantit left in
"t
f
the thistle unnd dm. Heat the fld gently
until the sample is completely diuolved. The
evolved gar ( HIS) is pasred into the ammoniacal
cadmium chloride solution, and cadmium rul-
phide in preci itated. At the wmpledon of the
Sulphur, percent
by m a s
-(A-B)xCxl6

8
reaction the elivery tube is d i i o n n u t e d . where

-
A = volume, in ml, of potadum iodate
5.3.3 T r r d a the watenm of the mmnriw added;
cylinder to a 250 ml c o d d R a L . W n h the
rider of the cylinder with50 mml of water and B = volume, in ml, of potassium iodate
add the wuhingr to tha flJ. Add of unused;
standard potauium iodate-potas~ium iodide C = nornnlity of potdurn iodatq
solution and cool with ice watar for 20.30
seconds. Swril the &rk and uld 20 ml c d d
water and 50 ml dih& hydrochloric d.
Titrate the axcan of liberated iodine with
- and
D m u , in g, of sample tab.
standard sodium thiosulphaie mlution using
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of 'BIS Handbook' and 'Standards Monthly Additions'.
This Indian Standard has been developed from Doc: No. MTD 2 (3545)

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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