Professional Documents
Culture Documents
( Reaffirmed 2002 )
Indian Standard
(Reaffirmed 2018)
~(-‘“““’
1997
)
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
PART 3 DETERMINATION OF PHOSPHORUS
BY ALKALIMETRIC METHOD
( Third Revision )
UDC 669.14+669.15-194:543.241[543.847]
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ISr228(Part3)-1987
Indian Standard
METHODS FOR
CHEMICAL ANALYSIS 6F STEELS
PART 3 DETERMINATION OF PHOSPHORUS
BY ALKALIMETRIC METHOD
( Third Revision)
Chaimtaa Repenting
Da C. S. P. IYER Bhabha Atomic Research Centre, Bombay
Mrmbrrs
SEW G. M. hPABA0 Steel Authority of India Ltd ( Bhilai Steel Plant),
Bhilai
Snn~ R. D. AQABWU ( Afhndr)
SEBI S. V. BHAQWAT Kbandelwal Ferro Alloys Ltd, Nagpur
SEBI D. N. GUPTA ( Alfanatr )
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SHRI P. CEAKBA Indian Metals t Ferro Alloys Ltd, Koraput
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CHEHIST & MICTALLU~~I~T Ministry of Transport ( Department of Railways)
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AWWITAHTR~~SEAROEO~~IOER
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(MET-~). RDSO. LUOKNOW
( Alm& ) .
f-%iIEF CHEMIST Tata Iron & Steel Co Ltd. Jamshedpur
AS~IETANT Cantr CHEVIOT ( Alhnatr )
Sam M. K. CHAKRAVABTY Ministry of Defence ( DGI )
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Calcutta
SHRI S. N. MOIT~A ( Alfemafr )
SHRI V. B. KHANNA Directorate General of Supplies & Disposals,
New Delhi
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( Continued on pcrgr 2 )
Q Copyright 1987
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reproduction 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.
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IS : 228 ( Part 3 ) - 1987
Mmbus Rqmnting
SHIU P. NABAIN Mahindra Ugine Steel Co Ltd. Bombay
SERI G. R. SABYA ( Altrrnatr )
SEBI N. P. PANDA Steel Authority of India Ltd (Rourkela Steel
Plant ), Rourkela
SEXI B. MAEAPATRA ( Altrmutr )
DB L. P. PANDXY National Metallurttical Laboratory . ( CSIR 1,
Jamrhedpur -
DE D. C. P~CASEAII National Physical Laboratory (CSIR j,
New Delhi
SHEI J. RAI ( Altrrsutt )
SEW C. RAJA~AO Ferro Alloys Corporation Ltd, Shreeramnagar
SX~I K. RAMAXBIsENAN Eraen & Co, Bangalore
DsJ. RAJABAM ( Alternafa )
SHBI A. P. SINEA Steel Authorjty of India Ltd ( Bokaro Steel
Plant ), Bokaro
SHIU K. ANWAH ( Altmafr )
SHBI N. V. SUBBAI~AYAPPA Visvesvaraya Iron & Steel Ltd, Bhadravati
DE P. SUBRAHMANIAM Defence Metallurgical Research Laboratory.
Hyderabad
SEBI T. H. RAO ( Alfrraatr )
DR CH. VPNKATEBWARLU Bhabha Atomic Research Centre, Bombay
SEXI K. RAQHAVENDRAN, Director General, BIS ( Ex-oficio Mnnbcr )
Director ( Strut & Met )
SXRI M. L. SEAWA
As&ant Director ( Metalr ), BIS
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Ferrous Metals Analysis Subcommittee, SMDC 2 : 3
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COWdM
DB C. S. P. IYER Bhabha Atomic ail
Research Centre, Bombay
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Mcmbns
SEW S. BASXARAN Bharat Heavy Electricals Ltd, Hyderabad
SHRI MATA SARAN I Altrraat~ I )
SHBI B. RAHA ( Altehale II )
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IS : 228 ( Part 3 ) - 1937
Indian Standard
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
PART 3 DETERMINATION OF PHOSPHORUS
BY ALKALIMETRIC METHOD
( Third Revision)
0. FOREWORD
0.1 This Indian Standard ( Part 3 ) ( Third Revision ) was adopted by
the Indian Standards Institution on 16 January 1987, after the draft
finalized by the Methods of Chemical Analysis of Ferrous Metals
Sectional Committee had been approved by the Structural and Metals
Division Council.
0.2 IS : 228, which was issued as a tentative standard in 1952 and
revised in 1959, covered the chemical anaIysis ofpig iron, cast iron and
plain carbon and low alloy steels. For the convenience it was decided
to publish a comprehensive series on chemical analysis of steels
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including high alloy steels. Accordingly, revision of IS : 228 was
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taken up again and new series on methods of chemical analysis of steels
including high alloy steels was ublished in various parts as IS : 228
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( Parts 1 to 13 ) ( see Appendix A 3 covering separate method of analysis
for each constituent in steels. However, IS : 228-1959’ ail version has
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been retained for the analysis of pig iron and cast iron till a separate
standard for analysis of pig iron and cast iron is published.
0.2.1 This revision of IS : 228 ( Part 3 )-1972t.. has been undertaken
on the basis of experience gained during the implementation of the
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of
‘Methods chemical analyrir of pig iron, cast iron and plain carbon and low alloy
rteelr ( m&cd).
tMethods for chemical analyria of rteelr: Part 3 Determination of phosphorus by
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IS:22S(Part3)-1987
1. SCOPE
2. SAMPLING
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relevant Indian Standard,
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3. QUALITY OF REAGENTS
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3.1 Unless specified otherwise, analytical grade reagents and distilled
water (see IS : 1070-19771) ail
shall be employed in the test.
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IS:228(Part3)-1987
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standardize against staudard nitric acid ( 4.2.10 ).
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4.2.10 Standard .Nitric Acid Solution - 0’1 N, dilute 7 ml of concentrated
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nitric acid to one litre with freshly boiled distilled water. Standardize
against sodium carbonate
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previously ignited at 350°C and cooled.
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IS:228(Part3)-1987
NOTE - Quantity of nitric acid added at this stage will depend upon the actual
volume of the solution. The analyst will ensure that the acidity of the solution
before precipitation of phosphomolybdate complex is maintained at 5-10 percent.
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5.4 Warm the solution to about 60-80°C and add 50 ml of ammonium
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molybdate solution, stopper the flask, shake vigorously for a few
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minutes and allow to stand for half an hour.
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5.5 Filter the precipitate
Wash the flask, precipitate
through
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a filter paper pulp pad by suction.
and filter pad twice with 5 ml portions of
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dilute nitric acid (2 : 98) and five times with 5 ml portions of potassium
nitrate. Continue washing of the precipitate and filter pad with
potassium nitrate solution until the washings are acid free ( 10 ml
portion of the washings in presence of phenolphthalein should turn
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5.6 Transfer the pulp along with the precipitate to the flask. Add
about 25 ml of water, few drops of phenolphthalein and a known
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IS:228(Part3)-1987
6.2.2 Collect the filtrate in a 500-ml conical flask and preserve it.
Take the precipitate and pulp ( as in 6.1 ) in a platinum crucible and
ignite, fume with 1 ml hydrofluoric acid and a few drops of
concentrated nitric acid at low temperature. Fuse the residue with
sodium carbonate. Dissolve the melt in water, filter through paper
pulp and wash with sodium carbonate solution. Acidify the filtrate
with concentrated nitric acid and add to the main filtrate. Proceed
further as in 5.2 to 5.6.
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6.3 Chromium Vanadium Steels or Other Steels Containing
gm as
Vanadium But No Tungsten
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6.3.1 Proceed as in 6.1 when the solution is ready for the
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precipitation of phosphomolybdate complex.
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IS:228(Part3)-1987
6.4.3 Treat the filtrate as in 5.2 and 5.3. If the sample contains
vanadium, proceed further as in 6.3.2. In the absence of vanadium,
complete the determination as in 5.4 to 5.6.
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in a 400-ml beaker in 40 ml of dilute nitric acid (1 : 3). Add 15 ml
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of perchloric acid and evaporate just to white fumes. Add hydrotluoric
acid drop by drop until all the hydrated silica is dissolved and a few
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drops in excess. Heat so that perchloric acid refluxes on the sides of
the beaker for about 25 minutes.
10 ml concentrated nitric acid and boil for few minutes.
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Cool, add about 40 ml of water and
Proceed
further as in 5.2 to 5.6.
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7. BLANK DETERMINATION
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IS:228(Part3)-1987
8. CALCULATION
(B-A) x C x 100
Phosphorus ( percent ) =
D
where
A = millilitres of standard nitric acid solution required in the
sample in the titration of the excess sodium hydroxide
( see 5.6 ),
B = millilitres of standard nitric acid solution required in the
blank determination (see 7.1),
C = phosphorus equivalent of 1 ml standard nitric acid
solution, and
D = quantity of sample in g.
APPENDIX A
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( Clause 0.2 )
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IS : 228 Methods for chemical analysis of steels:
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(Part 1 )-1972 Determination of carbon by volumetric method
( for carbon > 0’1 percent ) ( second revision )ail
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revision )
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IS:228(Part3)-1987
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IS : 228 ( Part 3) - 1987
( Con&4rdfiom pqc 2 )
Mmbrrs Represcntin~
S_HRIJ. MUKEERJEE Steel Authority of India Ltd (Durgapur Steel
Plant ), Durgapur
SRRI P. K. BANERJEE f Alternate )
Sam P. NARAIN Mahindra Ugine Steel Co Ltd, Bombay
SRRI G. R. SARYA ( Aftmate )
SRRI R. S. NATH Steel Authority of India Ltd ( Bokaro Steel
Plant ), Bokaro
SEW N. Gnwnapp~ ( Alternate )
DR L. P. PANUEY National Metallurgical Laboratory ( CSIR ),
Jamshedpur
SEBI G. RAMDAL~ Visvesvaraya Iron & Steel Ltd, Bhadravati
SHRI R. D. VANDRIWAI.T.A Italab Pvt Ltd. Bombay
SHRI J. C. DEY ( Akcmate )
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