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IS 228-9 (1989): Methods of chemical analysis of steels,

Part 9: Determination of sulphur in plain carbon steels by
evolution method (for sulphur 0.01 to 0.25 percent) [MTD 4:
Wrought Steel Products]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 IS228(Part9):1989
( Reaffirmed 1994
( Reaffirmed 2004) )
Indian Standard
METHODS FOR
CHEMICALANALYSISOFSTEELS
PART 9 DETERMfNATfON OF SULPHUR BY EVOLUTION METHOD
( FOR SULPHUR 0’01 TO 0’25 PERCENT)

( Third Revision )

Third Reprint AUGUST 1997

UDC 669’14 + 669’15-194’2 : 543’845

@I BIS 1990

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC
NEW DELHI 110002

August 1990 PrhGromp 2

Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2

FOREWORD

This Indian Standard ( Part 9) ( Third Revision ) was adopted by the Bureau of Indian Standards
on 26 December 1989, after the draft finalized by the Methods of Chemical Analysis of Ferrous
Metals Sectional Committee had been approved by the Metallurgical Engineering Division
Council.

IS 228, which was first published in 1952 and subsequently revised in 1959, covered the chemical
analysis of plain carbon and low alloy steels, along with pig iron and cast iron. This standard
was again revised to make it comprehensive in respect of steel analysis and to exclude pig iron
and cast iron which are being covered in separate standard. 14 parts have already been issued
covering only chemical analysis of steels.

This standard IS 228 ( Part 9 ) was published in 1975. In this revision the part has been updated
and reproducibility of the method incorporated.

In reporting the result of a test 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 >‘.
 Indian Standard
METHODS FOR
CHEMICALANALYSISOFSTEELS
PART 9 DETERMINATION OF SULPHUR BY EVOLUTION METHOD
(FOR SULPHUR 0’01 TO 0’25 PERCENT)

( Third Revision)
1 SCOPE 5 DETERMINATION OF SULPHUR BY
EVOLUTION METHOD
1.1 This standard (Part 9) covers method for
determination of sulphur in plain carbon and 5.1 Outline of the Method
low alloy steel by evolution method.
Sulphur is evolved as hydrogen sulphide and
NOTE - This method is not suitable for steel samp!es precipitated as cadmium sulphide in ammoniacal
containing selenium. cadmium chloride solution. Solution is acidified
and excess of potassium iodate-potassium iodide
2 SAMPLING is added. Excesses of liberated iodine is titrated
against sodium thiosulphate.
2.1 Sample shall be drawn as per relevant
Indian Standard. 5.2 Reagents

5.2.1 Dilute Hydrochloric Acid, 1 : 1 ( v/v ).

3 QUALITY OF REAGENTS
5.2.2 Ammoniacal Cadmium Chloride Solution
3.1 Unless specified otherwise, analytical grade
reagents and distilled water shall be employed Dissolve 22’8 g of cadmium chloride in 1’0 litres
in the tests. of water and add one litre of ammonia
( rd = 0.90).
4 APPARATUS
5.2.3 Standard Iodate Solution ( 0’03 N)
Cl Apparatus as shown in Fig. 1 may be used
with leak proof joints. Dissolve 1’07 g of potassium iodate ( KIO, ),
10 g of potassium iodide and 2 g of potassium
hydroxide in 50 ml water and transfer to one
litre volumetric flask and make up.

5.2.4 Standard Sodium Thiosulphatc Solution

(0’03N)

Mix 8’1 g of sodium thiosulphate ( Na&Os’

5H,O ) with 0’5 g of sodium carbonate and
dissolve in 1 litre of water. Solution is standar-
dized against a primary standard solution of
potassium iodate ( 5.2.3 ).

5.2.5 Starch Solution

Dissolve 0’1 g of soluble starch in 100 ml of hot

water and boil for 2 to 3 minutes and cool.

5.3 Procedure
I
5.3.1 Transfer 5’00 g of sample in a 500 ml dry
florepce flask fitted properly with a rubber cork
attached with a thistle funnel and delivery tube
bend at right angle. The end of the thistle
Fxo. 1 APPARATUS FOR DETERMINATION OF funnel should nearly touch the bottom of the
SULPHUR BY EVOLUTION METHOD flask and delivery tube remain dipped in the

1
measuring cylinder containing 20 ml of starch as indicator till blue colour is discharged.
ammoniacal cadmium chloride solntion and Note the volume of standard sodium thio-
80 ml of water. sulphate solution.

5.3.2 Add dilute hydrochloric acid through 5.3.4 Carry out a reagent blank simultaneously.
thistle funnel in sufficient quantity to cover the
sample completely and some quantity left in 5.3.5 Calculation
the thistle funnel also. Heat the flask gently
until the sample is completely dissolved. The
evolved gas ( H,S ) is passed into the ammoniacal S”~yh~;sI)ercent
=( A - B ) x C x 16
cadmium chloride solution, and cadmium sul- D
phide is precipitated. At the completion of the where
reaction the delivery tube is disconnected.
A = volume, in ml, of potassium iodate
5.3.3 Transfix the contents of the measnring added;
cylinder to a 250 ml conical flak W.ash the
sides of the cylinder with 50 ml of water and B = volume, in ml, of potassium iodate
add the washings to the flask. Add excess of unused;
standard potassium iodate-potassium iodide C = normality of potassium iodate;
solution and cool with ice water for 20-30 and
seconds. Swril the &I& and add 20 ml cold
water and 50 ml dilute hydrochloric acid. D = mass, in g, of sample taken.
Titrate the excess of liberated iodine with
standard sodium thiosulphate solution using 5.3.6 Reproducibili&, f0’005 percent.
Bureati 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.

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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 (Publication), BIS.

Review of Indian Standards

Amendmen& 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 Handbook’ and ‘Standards Monthly Additions’.
This Indian Standard has been developed from Dot: No. MTD 2 (3545)

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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