IS .

: 228 (Part 2) - 1987 ( Reaffirmed 1997 )

Indian Standard
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 2 DETERMINATION OF MANGANESE IN PLAIN-CARBON AND LOW ALLOY STEELS BY ARSENITE METHOD

( Third Revision >

( Second Reprint NOVEMBER 1998 )

UDC

66914+66915-194.2

: 543 [ 546711

0 Copyright BUREAU OF INDIAN

1987 STANDARDS

MANAK

BHAVAN,

9 BAHADUR SHAH NEW DELHI IlOO

ZAFAR

MARC

Gr 2

August

1987

IS : 228 ( Part

2 ) - 1987

Indian Standard
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 2 DETERMINATION OF MANGANESE IN PLAIN-CARBON AND LOW ALLOY STEELS BY ARSENITE METHOD

( Third Revision)
Methods
Chairman DR C. S. I. IYER Members SHRI G. M. APPA~~AO Stce~~;;a~ori(y of India Ltd ( Bhilai Steel Plant ),

of Chemical Analysis Sectional Committee,

of Ferrous SX1DC 2
Reprasenfing

Metals

Bhabha Atomic Research Centre,

Bombay

SERI R. D. AQABWAL ( Altrrnatr ) Khandclwal Fcrro Alloys Ltd, Nagpur SHBI S. V. BHAQWAT SHRI D. N. GUPTA ( Allcrnala ) Indian Metals & Ferro Alloys Ltd, Koraput SHRI P. CHAKRA Ministry of Transport ( Department of Railways ) CHEMIST & METALLURGIST AESIST~NT RESEARCH OBPICER (MET-2) RDSO, LUCKNUW ( Allrrnafc ) CHIEF CHEMIST Tata Iron & Steel Co Ltd, Jamshedpur ASSISTANT CHIEF CHEMIST( Alternate ) Ministry of Defence (DGI) SHRI M. K. CJXAKRAVARTY SHRI P. K. SEN ( Allernale ) Indian Iron & Steel Co Ltd, Burnpur DR M. M. CHAKRABORTY SHRI M. S. CEATTERJEE( Alternate ) Ordnance Factory Board ( Ministry of Defence ), SHRI C. K. DIKSHIT Calcutta SHRI S. N. MOITRA ( Altrrnafr ) Directorate General of Supplies & Disposals, SHRI V. B. KEANNA New Delhi Steel Authority of India Ltd (Durgapur Steel SHRI.J. N. MUKHERJEE Plant ), Durgapur ( Continued on pug 2 )
Q Gpyright

BUREAU

3F

INDIAN

1987 STANDARDS

This publication is protected under the Indian Copyright Act ( XIV of 1957 ) and reproduction in whole or in part by any means except wirh written permission of the publisher shall be deemed to be an infringement of copyright under the said Act.

IS : 228 ( Part 2) - 1987 ( Continued from page 1 )

Members SHRI P. NARAIN SHRI G. R. SAR~A ( Altrmote SHRI N. P. PANDA SBRI B. MAHAPATRA DR L. P. PANDEY DR D. C. PRASHAR SHRI J. RAI ( Altrrnafr ) SABI G. RAJA~AO SHRI K. RAMAKRISENAN DR J. RAJARAM (Alternate) SHRI A. P. SINEA SHRI K. ANNIAH ( Aknotr SHRI N. V. SUBBARAYAPPA DR P. SUBRAHMANiAM ) Visvesvaraya Iron & Steel Ltd, Bhadravati Defence Metallurgical Research Laboratory, Hyderabad Bhabha Atomic Research Centre, Bombay Director General, BIS ( Ex-ojicio Member) Mahindra ) he1 Authority of Plant ), Rourkela India Ltd (Rourkela Steel Reprcrcnting Ugine Steel Co Ltd, Bombay

( Altrmott )

National Metallurgical Jamshedpur National Physical New Delhi Ferro Alloys Corporation Essen & Co, Bangalore Steel Authority of Plant ), Bokaro

Laboratory Laboratory

(CSIR), (CSIR j,

Ltd, Shreeramnagar

India

Ltd

( Bokaro

Steel

SHRI T. H. RAO ( Alternote ) DR CE. VENKATESWAHLU SHBI K. RAOHAVENDRAN, Director ( Strut & Mer )

Secrrtar)
SHRI M. L. SRARMA A:sirtant Director ( Metals ), BIS

Ferrous COtlV~flCf DR C. S. P. IYER Membrrs SHRI S. BASKARAN

SHRI MATA

Metals

Analysis

Subcommittee,

SMDC: 2 : 3

Bhabba Atomic

Research

Centre,

Bombay

Bharat Heavy I ) II

Electricals

Ltd, Hyderabad

SARAN ( Altcrnatc

St-eel Authority of India Ltd ( Bbilai Steel Plant ), Bhilai SHRI E. M. V~RQEESE ( Alternate ) Tata Iron & Steel Co Ltd, Jamshedpur CHIEF CHEMIST ASSIS~~ANT CHIEF CHBMIST ( Alternate ) Indian Iron & Steel Co Ltd, Burnpur DB M, M. CHAKBABORTY SHRI L. N. Dlra ( ~~ternotr ) Steel Authority of India Ltd (Zourkela Steel SERI H. K. DAS Plant ), Rourkela SHRI K. BISHNOI ( Altcrnntc ) Physical Laboratory National SHRI .4. K. GUPTA (CSIR ), New Delhi ( Continurd en pags 8 )

SBRI B. RAHA (Alternate SEIRI ff. P. BOSE

IS:228(Part2)-1987

lndian Standard
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 2 DETERMINATION OF MANGANESE IN PLAIN-CARBON AND LOW ALLOY STEELS BY ARSENlTE METHOD

( Third Revision)
0. FOREWORD
0.1 This Indian Standard ( Part 2 ) ( 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 analysis of pig iron, cast iron and For the convenience it was decided plain carbon and low alloy steels. series on chemical analysis of steels to publish a comprehensive Accordingly, revision of IS : 228 -was including high alloy steels. taken-up again and new series on methods 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 of analysis However, IS : 228-1959* version has for each constituent in steels. been retained for the analysis of pig n-on 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 2)-1972t has been undertaken on the basis of experience gained during the implementation of the standard by the manufacturers and testing laboratories. 0.3 In this revision a) modification major modifications are: of low alloy steels, and

of method

for dissolution

*Methods of chemical analysis of pig iron, cast iron and plain carbon and low-alloy steels ( revised ). tMethods for chemical analysis of steels: Part 2 Determination of manganese in plain-carbon and low alloy steels by arsenite method ( second revision ).

IS : 228 ( Part

2 ) - 1987
of the method at the various

b) inclusion of reproducibility levels of rnanganese content.

0.4 Photometric method for determination to 2 percent has been covered in IS : 228 (Part

of manganese 12 )-1976*.

up

0.5 In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or calculated, is to be rounded off, it shall be done in accordance with IS : 2-1960f.

1. SCOPE 1.1 This standard ( Part 2 ) covers method for the determination manganese in plain carbon and low alloy steels by arsenite method.
2. SAMPLING of

2.1 The relevant

samples shall be drawn Indian Standard.

and

prepared

as prescribed

in the

3. QUALITY

OF REAGENTS
and distilled

analytical grade reagents 3.1 Unless specified otherwise, water (see IS : 1070-1977 )$ shall be employed in the test.

4. DETERMINATION OF MANGANESE ( 01 TO 15 PERCENT ) IN PLAIN CARBON AND LOW ALLOY STEELS BY THE ARSENITE METHOD (IN ABSENCE OF TUNGSTEN ) 4.1 Outline of the Method - Manganese is oxidized, in presence of silver nitrate, to permanganic acid by ammonium persulphate and titrated with sodium arsenite solution. 4.2 Reagents Dilute Nitric Acid Phosphoric Acid I : 2 (lJ/lJ). 85 percent. 1 : 4 (I,I,).
by up

4.2.1 4.2.2 4.2.3

Dilute &iphuric Acid -

*hlvthods for rhr~ntcal anal\sis of sterlr: Part 12 Dvt. rrninarion of manganese pe$indate ( phwometric ) nlethtid in luw and high alloy steels ( for manganese to 2 percent ) ( 11c0nd rcuision ). ~liulea for rounding off numerical valets (ruircd). tS;p-ciclration for wa!cr for ~rnrral laboratoq use ( src0ndrcuion j.

IS : 22% ( Part 2 ) - 1987 4.2.4 Concentrated IS : 264-1976* ).

4.2.5 (&). 4.2.6 4.2.7 Silver Ntrate Solution 1 percent 1 percent (m/v). (m/v). Ammonium .Nitric Acid Relative density 142 (conforming to

Persulphate

Solution -

Freshly

prepared,

10 percent

Sodium Chloride Solution -

4.2.8 Standard Sodium Arsenite Solution - Take 16 g of arsenious oxide in a 800-ml beaker. Add 10 g of sodium carbonate and 500 ml of water in the beaker and heat at low temperature until the solution is comlrlete. Filter the solution through a filter pad in a bottle and make up the volume of the solution to 2 litres by addition of water. Shake the bottle vigorously. Standardize the arsenite solution as in 4.3 against 02 g of steel sample (having approximately similar composition as the sample under test ) of known manganese content. 4.2.8.1 Adjust the strength of the sodium arsenite solution in such that each millilitre of the solution will be equivalent a way to il.1 iwlcc*nt manganese when 0.2 g of sample is taken. 4.3 Procedure

4.3.1 J)issolution
4.3.1.1 P!ain carbon .rteelTake 02 g of an accurately weighed sample in a 250-ml conical flask. .4dd 10 ml of dilute nitric acid and 3 to 4 ml of phosphoric acid, and heat to dissolve the sample, boil to expel oxides of nitrogen and dilute to 100 ml. 4.3.1.2 Low al& steel -Take 02 g of an accurately weighed sample in a 2X)-ml conical flask. Add 20 ml sulphuric acid and 2-3 ml of phosphoric acid. Heat until the reaction ceases. Add concentrated Iritlic acid drop by drop until the dissolution is complete, boil off niLrolls fumes and dilute to 100 ml with water. 4.3.2 Add 20 ml of ammonium persulphate solution and boil. After f<:\\, minutes of boiling, when the solution becomes clear, add 10 ml of solver nitrate and allow the colour of permnnganic acid to develop. Boil to destroy the excess of pcrsulphate. Cool quickly to room Ic~rnperaturt~ *Sptcification for nitric acid ( .trcondrcui.rion ),

IS:228(Part2)-1987 4.3.3 Add 10 ml of sodium chloride solution to precipitate silver chloride. Titrate rapidly the permanganic acid with standard sodium arsenite solution until the pink colour is discharged.
5. CALCULATION

5.1 Calculate

the manganese Manganese,

content

of the steel as follows: x 100

percent

AxB = -Cp

where A volume of titration, standard sodium of arsenite standard solution sodium used for

B = maganese equivalent solution in g/ml, and C = mass in g of sample.

arsenite

5.2 Reproducibility
a) &-001 percent for manganese for content below 006 percent, 0.06 to

b) f0.02 percent 1 percent, and c) f003 percent

manganese

content

between

for manganese

above

1 percent.

APPENDIX ( CZause0.2 )
IS : 228 (Part ( Part Methods for chemical analysis

of steels: method and

1 )-1972 Determination of carbon by volumetric ( for carbon > 01 percent ) ( second revision )

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

( Part 3 )-1972 Determination ( second revision )

method method

of carbon by gravimetric ( Part 4 )-1974 Determination ( for carbon > 0 1 percent ) ( second revision ) 6

IS : 228 ( Part 2 ) - 1987 ( Part 5 )-I974

Determination ( gravimetric ) method revision ) of nickel by dimethylglyoxime ( for nickel > 05 percent ) (second

( Part

chromium by persuiphate 6 )-1974 Determination of oxidation method ( for chromium > 05 percent ) (second revision j method Determination of molybdenum ( for molybdenum > 1 percent by a-benzoinoxime ) (second revision) method steels by

( Part 7 )-1974
(Part (Part

8)-1975 Determination of silicon by the gravimetric ( for silicon > 01 percent ) ( second revision) 9 )-1975 Determination of sulphur in plain evolution method (second revision ) 10 )-1976 Determination ( photomewic ) method in low and high alloy carbon

( Part

of molybdenum by thiocyanate ( for molybdenum up to 1 percent ) steels ( second revision)

( Part

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

(Part

( Part

IS : 228 ( Part 2 ) - 1987

Members SHYII J. MIJKEERJEE Steel

Rcprcrcnting Authority of India Ltd (Durgapur Plant ), Durgapur Steel

STIRI P. K. BANERJEE ( Alfrrnotc ) Mahindra Ugine Steel Co Ltd, Bombay SARI P. NARAIN SHRt G. R. SARMA ( ~hrnafc ) Steel Authoritv of India Ltd (Bokaro Steel SHRI R. S. NITH Plant ), Bokaro Sa~r N. GUNDAPPA ( Alternote ) National Metallurgical Laboratory ( CSIR ), DR L. P. PANDEY Jamshedpur Visreyvaraya Iron & Steel Ltd, Rhadravati SHRI G. RAMDAY ltalab Pvt Ltd, Bombay SHRI R. D. VANDRIWALLA SHRI J. C. Dey ( Altematc )

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