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
BUREAU
OF INDIAN STANDARDS
Headquarters: Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002 Telephones: 323 0131,323 3375,323 9402 Fax : 91 11 3234062, 91 11 3239399, 91 11 3239382 Telegrams : Manaksansths (Common to all Offices) Central Laboratory : Telephone Plot No. 20/9, Site IV, Sahibabad Industrial Area, Sahibabad 201010
8-77 00 32
Regional Offices: Central
: Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002
*Eastern
: l/l 4 CIT Scheme VII M, V.I.P. Road, Maniktola, CALCUTTA 700054
Northern : SC0 335336, Southern
Sector 34-A, CHANDIGARH
160022
32376
17
337 86 62 60 38 43
: C.I.T. Campus, IV Cross Road, CHENNAI 600113
235 2315
tWestem : Manakafaya, E9, Behind Marol Telephone Exchange, Andheri (East), MUMBAI 400093
832 92 95
Branch Offices:: ‘Pushpak’, Nurmohamed Shaikh Marg, Khanpur, AHMEDABAD $Peenya Industrial Area, 1 st Stage, Bangalore-Tumkur BANGALORE 560058
380001
5501348
Road,
839 49 55
Gangotri Complex, 5th Floor, Bhadbhada Road, T.T. Nagar, BHOPAL 462003
55 40 21
Plot No. 6263,
40 36 27
Unit VI, Ganga Nagar, BHUBANESHWAR
Kalaikathir Buildings, 670 Avinashi Road, COIMBATORE Plot No. 43, Sector 16 A, Mathura Road, FARIDABAD Savftri Complex, 116 G.T. Road, GHAZIABAD
751001 641037
21 01 41
121001
8-28 88 01
201001
8-71 1996
53/5 Ward No.29, R.G. Barua Road, 5th By-lane, GUWAHATI
781003
5-8-56C, L.N. Gupta Marg, Nampafly Station Road, HYDERABAD
541137
500001
E-52, Chitaranjan Marg, C- Scheme, JAIPUR 362001
37 29 25
117/418 8, Sarvodaya Nagar, KANPUR 208005 Seth Bhawan, 2nd Floor, LUCKNOW 226001
Behind
Leela
201083
21 68 76
Cinema,
Naval
Kishore
Road,
NIT Building, Second Floor, Gokulpat Market, NAGPUR 440010
2389 23 52 51 71
Patfiputra Industrial Estate, PATNA 800013
26 23 05
Institution of Engineers (India) Building 1332 Shivaji Nagar, PUNE 411005
32 36 35
T.C. No. 14/l 421,
Unhsity P. 0. Palayam, THlRUVANANTH4PURAM
695034
621 17
*Sales office is at 5 Chowringhee Approach, P.O. Princep Street, CALCUTTA 700072
271085
tSales Dfffce is at Novelty Chambers, Grant Road, MUMBAI 400067
3096528
$Sales Dffice is at ‘F’ Block, Unity Building, Narashimaraja Square, BANGALORE 560002
222 39 71
Reprography Unit, BIS, New Delhi, India