is-00228-part04_chemical analysys of steel

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IS : 228 ( Part 4) l 1997Indian Standard

METHODS FORCHEMICAL ANALYSIS OF~.~TEELSPART 4 DETERMLNATION OF TOTAL ,CARBONBY ~GRAVIMETRIC ME,THOD(FOR. CARBON > 01 PERCENT)

( Third Re?iHon)

UDC 6691++ 66915-1942/3 : 54321 [ 54626 3

@ Cofiyright 1987BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAPAR MARCNEW DELHI 110002

Gr 2 August 1987


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IS : 228 ( Part 4 ) - 1987Indian StandardMETHODS FORCHEMICALANALYSISOFSTEELS

PART 4 DETERMINATION OF TOTAL CARBONBY GARVIMETRIC METHOD(FOR CARBON > 0-l PERCENT I( Third Revision )O.FOREWORD

0.1 This Indian Standard (Part 4 ) (Third Revision) was adopted bythe Indian Standards Institution on 16 January 1987, after the draftfinalized by the Methods ~of Chemical Analysis of Ferrous MetalsSectional Committee had been approved by the Structural and MetalsDivision Council.0.2 IS : 228, which was issued as a tentative standard in 1952 andrevised in 1959, covered the chemical analysis of pig iron, cast iron andplain carbon and low alloy steels. For the convenience it was decidedto publish a comprehensive series on chemical analysis of steelsincluding high alloy steels. Accordingly, revision of IS : 228 wastaken-up again and new series on method of chemical analysis ofsteels including high alloy steels was published in various parts asIS : 228 ( Parts I 1~013 ) (see Appendix A ) covering separate methodof analysis for each constituent in steels. However, IS : 228-1959*version has been retained for the analysis of pig iron and cast iron tilla separate standard for analysis of pig iron and cast iron is published.

0.2.1 This revision of IS : 228 ( Part 4)-1974t has been undertakenon the basis of experience gained during the implementation of thestandard by 111~manufacturers and testing laboratories.0.3 In this revision, methocl has been updarctl

*Methods of chemical analysis of pig iron, cast :ron and plain carbon and lowalloy steels ( rcuised ).*Methods for chemical analysis of steels: Part 4 Determination of carbon bygravimerric method ( for carbon 2 0.1 percent ) ( second evision ),


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Is : 228 ( Part 4 ) - 19870.4 In reporting the result of a test or analysis made in accordancewith this standard, if the final value, observed or calculated, is to berounded off, it shall be donein accordance with IS : Z-1960.

1. SCOPE1.1 This standard (Part 4) covers the method for determination oftotal carbon content of plain carbon, low alloy and high alloy steelsof 01 percent and above by the gravimetric method.2. OUTLINE OF THE METHOD2.1 The sample is burnt in a stream of purified oxygen and thecarbon dioxide formed is absorbed, after purification, in suitableabsorbant and determined.3. REAGENTS3.1 Oxygen (02) - 995 percent minimum.3.2 Accarite or Soda Lime - 080 to 200 mm.3.3 Magnesium Perchlorate - Mg ( C104 )s, 080 to. 200 mm.3.4 Roat/Crucible - Boat/crucible of precise di.mension foraccommodating in the resistance and induction furnace.

3.4.1 Preignite the boats/crucibles in air or oxygen in a furnace foran hour at 1 100C and store in a desiccator and check for consistancyof the blank values.3.5 Flux/Accelerator - Low carbon copper, red lead ( preignitedat 550C), tin and iron of low carbon content.4. APPARATUS4.1 The apparatus recommended in IS : 6226 (Part l)-19717 may beused.4.2 Instead of the resistance furnace, an induction furnace may alsohe used.

*Rules for rounding off numerical value ( r&cd ).tRecommendation for apparatus for clwmical analysis of metals: Part f

Determination of carbon by direct combustion.4


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IS : 228 ( Part 4) - 19875. SAMPLING5.1 The sample shall be drawn as prescribed in the relevant IndianStandards.5.2 The sample is to be cleaned with analar grade ether and acetone,dried in an air oven at 100 f 5C.6. PROCEDURE6.1 Assemble the apparatus. Switch on the furnace, if it is a resistancefurnace, and allow it to attain a temperature of 1 05OC (see Note ), allthe while passing oxygen through the apparatus so that it bubblesfreely at the exit end of the train. Disconnect the absorption bulb,keep in a desiccator till it attains room temperatu.re and take theinitial weight. Repeat the operation till a constant weight isobtained.

NOTE For high chromium and high nickel steels, the temperature of 1250%is recommended for complete combustion.6.2 Weigh to the nearest 0001 g, 20 to 30 g of the test sample.Transfer to the preignited combustion boat covered at the bottomwith a thin layer of calcined alumina. Spread the sample evenly overthe top of the alumina and cover it with 20 to 30 g of the flux.Introduce the boat slowly m the hot zone of the combustion tube.6.3 In the case of induction heating, weigh 13 the nearest 0001 g, 09to 11 g of the sample and transfer to a preignited crucible. Add anequal quantity of the flux. Place the crucible in position on thepedestal post of the furnace, raise to the combustion position andlock the system. Pass oxygen through the system and ignite the sample.6.4 Maintain a rapid How of oxygen ( 800 to 1000 ml/min ) throughoutthe combustion, then reduce to 400 to 500 ml per min and maintainit for another 6 to 8 min in order to sweep out the carbon dioxide.6.5 Remove the absorption bulb and weigh it after keeping it indesiccator till it attains room temperature. The increase in weight ofthe bulb represents the carbon dioxide.6.6 Remove the boat or crucible and examine for any incompletecombustion. If the sample is not thoroughly fused, repeat thedetermination with a fresh sample.6.7 Blank -- Charge a preignited boat or crucible, as the case may be,with the same amount of flux used in the determination and followthe procedure as in 6.2 to 6.5.

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IS : 228 ( Part 4) - 19877. CALCULATION7.1 Calculate the total carbon content of the sample as follows:

Carbon, percent = A-Bc x 2729where

A = increase in mass in g of the absorption bulb due tocarbon dioxide from the sample,B = increase in mass in g of the absorption bulb due tocarbon dioxide from the blank determination, andC = mass in g of the sample taken.

8. ACCURACY8.1 The accuracy of the method is f 001 percent for carbon in therange of 01 to 075 percent and & 002 percent for carbonabove 075 percent.

APPENDIX A( Clause 0.2)INDIAN STANDARDS ON METHODS FOR CHEMICALANALYSIS OF STEELS

IS : 228 Wlethods for chemical analysis of steels:(Part 1 )-I972 Determination of carbon by volumetric method( for carbon > 01 percent ) ( second reuision )( Part 2)-1972 Determination of manganese in plain carbon andlow alloy steels by arsenite method ( second revision )( Part 3 )-I972 Determination of phosphorus by alkalimetric method

( second revision )( Part 4 )-1987 Determination of total carbon by gravimetric method( for carbon > a.1 percent ) ( third revision)( Part 5 )-1974 Determination of nickel by dimethylglyoxime

( gravimetric ) method ( for nickel 2 05 percent ) (secondrevision )


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IS : 228 ( Part 4 ) - 1987(Part S)-1974 Determination of chromium by persulphateoxidation method ( for chromium > 05 percent) (second

revision)(Part 7 )-I974 Determination of molybdenum by a-benzoinoximemethod ( for molybdenum > 1 percent ) (second revision )( Part 8 )-I975 Determination of silicon by the gravimetric method(for silicon > 01 percent ) (second revision)(Part 9)-1975 Determination of sulphur in plain carbon steels byevolution method (second revision )( Part 10 )-1976 Determination of molybdenum by thiocyanate

( photometric ) method ( for molybdenum up to 1 percent )in low and high alloy steels (second revision)( Part 11 )-I976 Determination of silicon by photometric method incarbon steels and low alloy steels ( for silicon 001 to 005percent ) ( second evision )(Part 12)-1976 Determination of manganese by periodate(photometric) method in low and high alloy steels ( formanganese up to 2 percent ) ( second revision )( Part 13 )-I982 Determination of arsenic

is-00228-part04_chemical analysys of steel

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