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Is 228 part 9 | Ammonia | Sodium
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IS228(Part9):1989 ( Reaffirmed 1994 )
METHODS FOR CHEMICALANALYSISOFSTEELS
PART 9 DETERMfNATfON OF SULPHUR BY EVOLUTION ( FOR SULPHUR 001 TO 025 PERCENT) ( METHOD
66914 + 66915-1942
: 543845
@I BIS 1990
MANAK August 1990
ZAFAR MARC PrhGromp 2
Methods of Chemical Analysis of Ferrous Metals Sectional
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. and reproducibility of the method incorporated. In this revision the part has been updated
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 >.
PART 9 DETERMINATION OF SULPHUR BY EVOLUTION (FOR SULPHUR 001 TO 025 PERCENT) ( 1 SCOPE 1.1 This standard (Part 9) covers method for determination of sulphur in plain carbon and low alloy steel by evolution method.
NOTE - This method is not suitable for steel samp!es containing selenium.
5 DETERMINATION OF SULPHUR EVOLUTION METHOD 5.1 Outline of the Method BY
2 SAMPLING 2.1 Sample shall Indian Standard. 3 QUALITY be drawn as per relevant
Sulphur is evolved as hydrogen sulphide and precipitated as cadmium sulphide in ammoniacal cadmium chloride solution. Solution is acidified and excess of potassium iodate-potassium iodide is added. Excesses of liberated iodine is titrated against sodium thiosulphate. 5.2 Reagents 5.2.1 Dilute Hydrochloric Acid, 1 : 1 ( v/v ). 5.2.2 Ammoniacal Cadmium Chloride Solution Dissolve 228 g of cadmium chloride in 10 litres of water and add one litre of ammonia ( rd = 0.90). 5.2.3 Standard Iodate Solution ( 003 N)
3.1 Unless specified otherwise, analytical grade reagents and distilled water shall be employed in the tests. 4 APPARATUS Cl Apparatus as shown in Fig. with leak proof joints. 1 may be used
Dissolve 107 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 (003N) Sodium Thiosulphatc Solution
Mix 81 g of sodium thiosulphate ( Na&Os 5H,O ) with 05 g of sodium carbonate and dissolve in 1 litre of water. Solution is standardized against a primary standard solution of potassium iodate ( 5.2.3 ).
5.2.5 Starch Solution Dissolve 01 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 500 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 funnel should nearly touch the bottom of the flask and delivery tube remain dipped in the
Fxo. 1
APPARATUS FOR DETERMINATION SULPHUR BY EVOLUTION METHOD
containing measuring cylinder ammoniacal cadmium chloride 80 ml of water.
20 ml of solntion and
starch as indicator till blue colour is discharged. Note the volume of standard sodium thiosulphate solution. 5.3.4 5.3.5 Carry out a reagent blank simultaneously. Calculation C x 16
5.3.2 Add dilute hydrochloric acid through thistle funnel in sufficient quantity to cover the sample completely and some quantity left in the thistle funnel also. Heat the flask gently until the sample is completely dissolved. The evolved gas ( H,S ) is passed into the ammoniacal cadmium chloride solution, and cadmium sulphide is precipitated. At the completion of the reaction the delivery tube is disconnected. 5.3.3 Transfix the contents of the measnring cylinder to a 250 ml conical flak W.ash the sides of the cylinder with 50 ml of water and add the washings to the flask. Add excess of iodate-potassium iodide standard potassium solution and cool with ice water for 20-30 seconds. Swril the &I& and add 20 ml cold water and 50 ml dilute hydrochloric acid. Titrate the excess of liberated iodine with standard sodium thiosulphate solution using
S~yh~;sI)ercent x =( A - B )
A = volume, in ml, of potassium added;
B = volume, in ml, of potassium iodate unused; C = normality and of potassium iodate;
D = mass, in g, of sample taken. 5.3.6 Reproducibili&, f0005 percent.
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