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IS:228(Part4)-1987

( ReaIhncd
1997 )

Indian

Standard

METHOD FOR CHEMICAL ANALYSIS OF STEELS


PART 4 DETERMINATION OF TOTAL CARBON BY GRAVIMETRIC METHOD ( FOR CARBON r 0.1 PERCENT)

( Third Revision )
I;wflh Reprint NOVEMBER
1998

UDC

669.14 + 669.15-194.2/.3 : 543.21 [546.26]

BUREAU
MANAK

OF
BHAVAN,

INDIAN

STANDARDS
ZAFAR MARG

9 BAHADUR SHAH NEW DELHI 110002

Gr 2

Aqirst

1987

IS:228(Part4)-1987

Indian Standard
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 4 DETERMINATION OF TOTAL CARBON BY GRAVIMETRIC METHOD (FOR CARBON > O-1 PERCENT)

( Third Revision )
Methods of Chemical Analysis of Ferrous Metals Sectional Committee, SlMDC 2
Chuiman
DR C. S. P. IYLR Mcmbnr SHKI G. M. APPAUAO
Steel Authority

Rqmsmting Bhabha Atomic Research Centre, Bombay

of India Ltd ( Bhilai

Steel Plant ),

Sanr D. N. GUPTA ( Aflernnlc ) SEttIP. CHAKRA


CREYWT& METALLVIWUST

SHEI S. V.

SIIBX R. D. AOAIIWAL ( BHAOW~Y

Bhilai

AllmW)

Khandelwnl

Ferro Alloy1 Ltd, Nagpur

Indian Metals & Ferro Alloys Ltd, Koraput Ministry of Transport ( Department of Railways)

AINXVTANT RESEARCHOIFIC~~R (MET-2) RDSO, Luclixow


Tata Iron 8; Steel Co Ltd, Jamshedpur CHIEW CIIEM~ST AWXSTANT CHIEF CHRMMT ( Allnnat~ ) Ministry of Defence (DGI) SIiItIM. K. CEAtiRAVARTY Snug P. K. SEN ( Altrrnotr ) Indian Iron & Steel Co Ltd, Burnpur DR M. M. CEAKRABO~TY SERB M. S. CEATTERJEE ( Altrrnotr ) Ordnance Factory Board ( Ministry of Defence ), SERI C. K. D~KOH~T Calcutta SARI S. N. MOITRA ( Abn~tr ) Directorate General of Supplies & Disposals, SaRI V.B. KIXANXA New Delhi Steel Authority of India Ltd (Durgapur Steel SHR~ J. N. MUIWERJEE Plant ). Durgapur

( Allrmdr )

( Cen8inurd 8n porr 2 ) 0 whr 1987 OF INDIAN STANDARDS

BUREAU

This publication is protected -under the Itin clrprighl Act ( XIV of 1957 ) and rrproduction in whole or in part by any means except with written permission of the publisher shall be deemed to be an infringement of copyright under the said Act.

IS:228(Part4)-1987

Mcmbm SHRI P. NABAIN SHRI G. R. Saalar SHBI N. P. PANDA Mabindra ( Altnncfc) ) Steel

Rtpcmting Ugine Steel Co Ltd. Bombay Ltd (Rourkela Steel

Autbority of India Plant ), Rourkela Metallurgical

SIIIU B. MAIIAPATRA ( Aftn~h Da L. P. PANDEY DR D. C. PRASHAR SHBI J. RAI ( Al~rraa~ ) Saat G. RAJARAO SHRI K. RAMAKBIIHIAN Da J. RAJARAY ( Allma& ) SBRI A. P. !hNEA SHRI N. V. SUEIBAIIA~APPA DB P. S~JBBAHYANIAY SHBI T. H. RAO (Al&m& DE CR. VENKATLBWARLU SABI K. RAOHAVENDBAN, Director ( Strut St Met ) )

National
N

Laboratory Laboratorv

( CSIR ), (CSIR . ). I.

p;h-J~r Pbvsical a
New Delhi

Ferro Alloys Cornoration Eurn & Co, Batgalore Steel Authority of Plant ), Bokaro

Ltd. Shreeramaagar

.
Ltd ( Bokaro Steel

India

Vivervnraya Iron 8t Steel Ltd. Bbadravati Dcfence Metallurgical Rewarcb Laboratory, Hvderabad , Bhabha Atomic Research Centre, Bombay Director General, BIS ( Ex-oficio Member)

Slcrrlary
SFIBI M. L. SHARJ~A Assirtant Director ( Metalr ), BIS

Ferrpus

Metals

Analysis

Subcommittee,
Atomic Research

SMDC
Centre,

2 : 3
Bombay

cono#mr
Ds C. 9. P. IYBR Bhabha hitathrr Bharat Heavy Electricalr Ltd, Hjderahad SHRI S. BASKABAN SHBI MATA SARAN ( A&m& I ) SHRI B. RAEA (Alternate II ) Steel Authority of India Ltd ( Bhilai Steel Plant ), !&RI U.P.bJB Bbilai SIiRI E. M. VERQHEtlE ( Altmatr ) Tata Iron & Steel Co Ltd. Iamrhednur CHlElP CEEMIRT
.

AIWSTANT CIIIBP CEBYIST ( A&m&


DB M. M. CHAKBABORTT SHRI L. N. Dbs ( Altmmtr ) SEBI H. K. DAE SHRI K. Bmaror SHBI A. K. GIJPTA ( Aitrrnats )

Indian

Iron & Steel Co Ltd.

Burnpur Ltd ( hourkela Steel ),

Steel

Authority of India Plant ), Rourkela

Physical National New Delhi

Labor&y

( C8IR

( Cetttirurd on pap 8 ) 2

IS : 228( Part

4 ) - 1987

Indian Standard
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 4 DETERYlNATlON OF TOTAL CARBON BY GARVIMETRIC METHOD (FOR CARBON > O-1 PERCENT )

( Third Revision )
0. FOREWORD

I)y R cvision ) was adopted 0.1 This Indian Standard ( Part 4 ) (Third the Indian Standards Institution on 16 January 1987, afirr the draft finalized by the Methods of Chemical Analysis of Pcrrous Metals Sectional Committre had been approved by the Structural and Mct;~ls Division Council. 0.2 IS : 228, which was issued as a tentative standard in 1952 and revised in 1959, covered the chemical analysis of pig iron, cast iron and For the convenience it was decidctl plain carbon and low alloy steels. to publish a comprehensive series on chemical analysis of steels including high alloy steels. Accordingly, revision of IS : 228 was taken-up again and new series on method of chemical analysis of steels including high alloy steels was published in various parts as IS : 228 ( Parts 1 to 13 ) ( see Appendix A ) covering separate method However, IS : 228-195!)* of analysis for each constituent in steels. version has been rctainc tl for the analysis of pig iron and cast iron till a separate standard for analysis of pig iron and cast iron is phlishctl. 0.2.1 This revision of IS : 228 (Part 4)-19747 has been undcrtnkcn on the basis of experience gained during the implementation of \he standard by the manufacturers and testing laboratories. 0.3 In this revision, method has been updated.
carbon of and low by

*Methods of chemical analysis of pig iron, cast won and plain alloy 1teela [ rruiud )* tMethod1 for chemical analysis of steels: Part 4 Determination gravimetric method ( for carbon > 0.1 percent ) (rend rmi~ion ).

carbon

IS : 228 ( Part 4 ) - 1987 8.4 In rr,porting 111~ reslllt of a test or analysis made in accordance r\.itIl tItis 51;~ntlartl, if the final value, ohservcd or calculated, is to be I r)~~trcIt~tI011; it >11;111 clone in accordance Iw with IS : 2-1960*.

1. SCOPE 1.1 This standard (Part 4) covers the method for determination low alloy and high alloy total carljon content of plain carbon, nfO.1 pcrccnt and above by the grnvimctric method. 2. OUTLINE OF THE METHOD of steels

2.1 The sample is burnt in a stream of purified oxygen and the carhnn dioxide formctl is al~wrlwtl, after purihation, in suitable ahorhant and tlc~tcrminc~cl. 3. REAGENTS 3.1 Oxygen 3.2 Accarite (On) 905 percent minimum.

or Soda Lime -- 080 to 200 mm. Perchlorate Mg (CIO( )2, 0.80 to 200 mm. for

3.3 Magnesium

3.4 Boat/Crucible - Boat/crucible of precise dimension accommodating in the r&stance and induction furnace.

3.4.1 Preignitc the boats/crucibles in air or oxygen in a furnace for an hour at 1 100C and stnrc in a desiccator and check for consistancy of the blank values. 3.5 Flux,Accelerator - Low carbon copper, at 550(Z), tin and iron of low carbon content. 4. APPARATUS 4.1 The 11setl apparatus recommended in IS : 6226 (Part l)-1971t may be red lead ( preignited

4.2 Instead be used. ---

01 the

resistance

furnace,

an induction

furnace

may

also

*Rules for rounding ofl numerical valuer ( mid). tRecommcndation for apparatus for chemical Determination of carbon by direct combustion. 4

analysis

of metals:

Put

IS:228(Part4)-1987 5. SAMPLING 5.1 The sample shall be drawn Standards. as prescribed in the relevant ether Indian

5.2 The sample is to be cleaned with analar grade dried in an air oven at 100 f 5C. 6. PROCEDURE

and acetone,

6.1 Assemble the apparatus. Switch on the furnace, if it is a resistance furnace, and allow it to attain a temperature of 1 05OC (see Note ), all the while passing oxygen through the apparatus so that it bubbles freely at the exit end of the train. Disconnect the absorption bulb, till it attains room temperature and take the keep in a desiccator Repeat the operation till a constant weight is initial weight. obtained.
NOTB- For high chromium and high nickel rteelr, the temperature of 1 250C in recommended for complete comburtion.

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 bottom Spread the sample evenly over with a thin layer of calcined alumina. the top of the alumina and cover it with 20 to 30 g of the flux. Introduce the boat slowly In the hot zone of the combustion tube. 6.3 In the case of induction heating, weigh to the nearest 0001 g, 09 Add an to 11 g of the sample and transfer to a preignited crucible. equal quantity of the flux. Place the crucible in Position on the pedestal post of the furnace, raise to the combustion position and lock the system. Pass oxygen through the system and ignite the sample. 6.4 Maintain a rapid flow of oxygen ( 800 to 1 000 ml/min) throughout the combustion, then reduce to 400 to 500 ml per min and maintain it for another 6 co 8 min in order to sweep out the carbon dioxide. 6.5 Remove the absorption bulb and weigh it after keeping it in The increase in weight of desiccator till it attains room temperature. the bulb represents the carbon dioxide. 6.6 Remove the boat or crucible and examine combustion. If the sample is not thoroughly determination with a fresh sample. for any incomplete fused, repeat the

6.7 Blank - Charge a prei nited boat or crucible, as the case may be, with the same amount of Bux used in the determination and follow the procedure as in 6.2 to 6.5. 5

IS:228(Part4)-1981 7. CALCULATION 7.1 Calculate the total Carbon, where carbon content of the sample as follows:

percent

A-B = --x c

2729

A = increase
carbon

in mass in g of the absorption dioxide from the sample, in mass in g of the absorption dioxide from the blank determination, taken.

bulb bulb

due

to to

B = increase
carbon C= 8. ACCURACY 8.1 The
range

due and

mass in g of the sample

above

to 075 percent.

of 01

accuracy

of the 075

method percent

is & 001 percent for carbon and f 002 percent for

in the

carbon

APPENDIX ( Clause 0.2 )


INDIAN STANDARDS
IS : 228 ( Part ( Part ( Part ( Part ( Part Methods ON ANALYSIS

METHODS FOR OF STEELS of steels:

CHEMICAL

for chemical

analysis

1 )-I972 Determination of carbon by volumetric ( for carbon > 01 percent ) ( second revision )

method and

2)-1972 Determination of manganese in plain carbon low alloy steels by arsenite method ( second revision ) 3 )-1972 Determination ( second rcvisiorr ) of phosphorus by alkalimetric

method method

4 )-1987 Determination of total carbon by gravimetric ( for carbon ) 01 percent ) ( third revision ) 5 )-I974 Determination ravimetric ) method ?!Xon ) of nickel ( for nickel

by dimethyl lyoxime > 05 percent s ( second

IS

: 228

( Part

4 ) - 1987

(Part

S)-1974 Determination oxidation method rcuision )

of chromium hy persi!ipha?e ( for chromium > 05 percent : I serond by a-bcnzoinoxirne ) ( ~vtond rFi/iJiott ) method steels by

Part 7 )-1974 Determination of molybdenum method ( for molybdenum > 1 pwccnt

( Part (Part
(

8)-1975 Determination of silicon by the_ ~ravimetric ( for silicon > 0 1 percent ) ( second reutszon ) 9)-1975 Determination of sulphur in plain evolution met hod (second revirion ) 10 )-1976 Determination (photometric) method in low and high alloy
CW~J(JII

Parr

of molybdenum by thiocyannte ( for molybdenum up to 1 perwnt steels ( second reviJir,tl )

Part

11 )-1976 Determination of silicon by photometric method in carbon steels and low alloy steels ( for silicon 001 to 005 percent ) ( second relision ) 12 )-I976 Determination Of manganese hy (photometric) method in low and high i\lloy manganese up to 2 percent ) ( second revision ) 13 )-1982 Determination of arsenic periodate steels ( for

Part

Part

IS : 228 ( Part

4 ) - 1987

RaprcsraIing Steel SJIRI P. K. BANEHJEE ( Altrrnafr SMHI P. NAI~AIN SHXI G. 11. SIRMA ( Altrrndr ) SJIRI R. S. NATH 8n1u N. GUNL)APPA 1)~ L. P. PANDEY
(

Authority of India Plant ), Durgapur Ugine

Ltd

(Durgapur

Steel

) hahindra Steel

Steel CO Ltd, Bombay India Ltd (Bokaro Steel

Authority of Plant ), Rokaro

Altarnatr )

Sun1 G. Rnnlons SIIHI R. D. VANDRIWALLA SJIRI J. C. DEY ( Afterme )

Metallurgical Laboratory ( CSIR ), National Jamrhedpur _ Visvervarava Iron & Steel Ltd. Bbadravati ltalab Pvt Ltd. Bombay

BUREAU

OF INDIAN STANDARDS

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695034

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