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IS:228(Part4)-1987 ( ReaIhncd

Indian

1997 )

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

UDC

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

BUREAU MANAK

Gr 2

1998

OF BHAVAN,

INDIAN

STANDARDS

9 BAHADUR SHAH NEW DELHI 110002

ZAFAR

MARG

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

Rqmsmting Bhabha

DR C. S. P. IYLR

Atomic

Research

Centre,

Bombay

Mcmbnr Steel Authority

SHKI G. M. APPAUAO SIIBX R. D. AOAIIWAL ( BHAOW~Y

AllmW)

SHEI S. V.

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

of India Ltd ( Bhilai

Steel Plant ),

Bhilai

METALLVIWUST

Khandelwnl

Ferro Alloy1 Ltd, Nagpur

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

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

( Allrmdr )

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

( Cen8inurd 8n porr 2 )

BUREAU

0 whr 1987 OF INDIAN STANDARDS

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

Rtpcmting

Mcmbm SHRI P. NABAIN SHRI G. R. Saalar SHBI N. P. PANDA

Mabindra ( Altnncfc)

SIIIU B. MAIIAPATRA ( Aftn~h Da L. P. PANDEY DR D. C. PRASHAR

Steel )

Steel Co Ltd. Bombay

Autbority of India Plant ), Rourkela

National N

Ugine

Ltd

Metallurgical

Laboratory

p;h-J~r Pbvsical a

Laboratorv

New Delhi’

SHBI J. RAI ( Al~rraa~ ) Saat G. RAJARAO SHRI K. RAMAKBIIHIAN Da J. RAJARAY ( Allma& ) SBRI A. P. !hNEA

Ferro Alloys Cornoration Eurn & Co, Batgalore Steel

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 )

)

Authority of Plant ), Bokaro

(Rourkela

Steel

( CSIR ), (CSIR .

,

). I.

Ltd. Shreeramaagar

.

India

Ltd

( Bokaro

Steel

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,

SMDC

2 : 3

cono#mr Bhabha

Ds C. 9. P. IYBR

Atomic

Research

Centre,

Bombay

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

Steel

Iron & Steel Co Ltd.

Authority of India Plant ), Rourkela

Physical National New Delhi

Burnpur Ltd

Labor&y

( hourkela

Steel

( 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.

*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 ).

3

carb’on of

and low

carbon

by


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 Iw clone in accordance 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

of steels

METHOD

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

(On) -

3.2 Accarite

90’5 percent

minimum.

or Soda Lime -- 0’80 to 2’00 mm.

3.3 Magnesium

Perchlorate

-

Mg (CIO(

)2, 0.80 to 2’00 mm.

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

for

3.4.1 Preignitc the boats/crucibles in air or oxygen in a furnace for an hour at 1 100°C 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.

red

lead

( preignited

4. APPARATUS 4.1 The 11setl

apparatus

4.2 Instead be used.

01‘ the

recommended

resistance

in IS : 6226 (Part

furnace,

an induction

l)-1971t

furnace

may

may

be

also

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

analysis

of metals:

Put

I


IS:228(Part4)-1987 5. SAMPLING 5.1 The sample shall be drawn Standards.

as prescribed

in the relevant

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

ether

Indian

and acetone,

6. PROCEDURE 6.1 Assemble the apparatus. Switch on the furnace, if it is a resistance furnace, and allow it to attain a temperature of 1 05O’C (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 1 250°C in recommended for complete comburtion.

6.2 Weigh to the nearest 0’001 g, 2’0 to 3’0 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 2’0 to 3’0 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 0’001 g, 0’9 Add an to 1’1 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,

carbon

content

A-B = --x c

percent

of the sample

as follows:

27’29

where

A = increase carbon

B = increase carbon C=

in mass in g of the absorption dioxide from the sample,

bulb

in mass in g of the absorption dioxide from the blank determination,

bulb

mass in g of the sample

due

to

due and

to

taken.

8. ACCURACY 8.1 The range

above

accuracy

of 0’1

to 0’75 percent.

of the 0’75

method percent

in the

is & 0’01 percent for carbon and f 0’02 percent for

APPENDIX

carbon

A

( Clause 0.2 ) INDIAN STANDARDS

ON ANALYSIS

IS : 228

Methods

for chemical

METHODS FOR OF STEELS

analysis

CHEMICAL

of steels:

( Part

1 )-I972 Determination of carbon by volumetric ( for carbon > 0’1 percent ) ( second revision )

( Part

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

( Part

3 )-1972 Determination ( second rcvisiorr )

( Part

4 )-1987 Determination of total carbon by gravimetric ( for carbon ) 0’1 percent ) ( third revision )

( Part

5 )-I974 Determination ravimetric ) method ?!Xon )

of phosphorus

of nickel ( for nickel

G

by alkalimetric

method and

method method

by dimethyl lyoxime > 0’5 percent s ( second


IS

(Part

(

S)-1974 Determination oxidation method rcuision )

: 228

( Part

of chromium hy persi!ipha?e ( for chromium > 0‘5 percent : I serond

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

by a-bcnzoinoxirne ) ( ~vtond rFi/iJiott )

( Part

8)-1975 Determination of silicon by the_ ~ravimetric ( for silicon > 0’ 1 percent ) ( second reutszon )

(Part

9)-1975 Determination of sulphur in plain evolution met hod (second revirion )

(

10 )-1976 Determination (photometric) method in low and high alloy

Parr

4 ) - 1987

method

CW~J(JII

steels

by

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 0’01 to 0’05 percent ) ( second relision )

(

Part

12 )-I976 Determination Of manganese hy (photometric) method in low and high i\lloy manganese up to 2 percent ) ( second revision )

(

Part

13 )-1982

Determination

of arsenic

7

periodate steels ( for


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

(

Altarnatr )

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

Authority of India Plant ), Durgapur

) hahindra Steel

Ugine

Ltd

(Durgapur

Steel

Steel CO Ltd, Bombay

Authority of Plant ), Rokaro

India

Ltd

(Bokaro

Steel

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

8


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OF INDIAN STANDARDS

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228_4