IS

: 228 (Part 8)-1987

( Reaffirmed 1997 )

Indian Standard
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 6 DETERMINATION OF-CHROMIUM PERSULPHATE OXIDATION METHOD (FOR CHROMIUM)04 PERCENT) ( BY

Third Revision )
1991

First Reprint JANUARY

UDC 669.14+669*15-194*2/*3 : 543[546*76]

Q Copyright 1987
BUREAU
MANAK

OF
BHAVAN,

INDIAN
9 BAHADUR NEW DBLHI

STANDARDS
SHAH 110002 ZAFAR MARG

Gr3

August 1987

MOITRA ( Altrmofo) Directorate General of Supplies & Disposals. MUEEERJEE Plant ). Koraput Ministry of Transport ( Department of Railways) CH~XI~T & METALLWRQI~T A~SI. CWAKRAVABTY SHBI P. Durgapur ( con#nued 0” @l## 2 ) Q Cqyrighht 1987 OF INDIAN STANDARDS ( Altanais ) CHIEF CHEXIST Steel Authority Bhilai of India Ltd (Bhilai Steel Plant ). CXATTERJEE ( Altemats ) Ordnance Factory Board ( Ministry of Defence ). N. V. IL DIKSHIT Calcutta SIXXSS.IS I 228 ( Part 6 ) . CHAKRABORTY Indian Iron UCSteel Co Ltd. BUREAU ‘Fbia publication qproduction pub&box is protected under the Indian Copyright Act ( XIV of l957 ) and in whole or in part by any means except with written permission of the of copyright under the said Act. BHAQWAT Khandelwal Ferro Alloys Ltd. IYER Members SERI G. SMDC 2 Rcprcscnting Bhabha Atomic Research Centre. Bombay SHRI R. N. N. SERI C. B. K. KEAHNA New Delhi Steel Authority of India Ltd (Durgapur Steel SExI J. P. K. &all be deemed to be an infringement . Jamshedpur ASSWTANT CHIEP CHEMIST ( Altrmatc ) Ministry of Defence (DGI) SH~I M. Burnpur SHBI M. A~ABWAL ( Altrmata) SHRI S. LUOKNOW Tata Iron & Steel Co Ltd. M. S. APPABAO of Chemical Analysis of Ferrous Metals Sectional Committee. SEN ( Alternate ) DB M. GWPTA ( Altcmotc ) SHRI P.1987 / Indian Standard METHODS FOR CHEMI-CAL ANALYSIS OF STEELS PART 8 DETERMINATION OF CHROMIUM PERSULPHATE OXIDATION METHOD ( FOR CHROMIUM > W PERCENT ) BY ( Third Revision) Methods Chairman DR C.STA~T RESEARCH Ovrraxn (MET-2) RDSO. S. D. SEEI V. CEAK~A Indian Metals & Ferro Alloys Ltd. M. Nagpur Snnr D.

@bcommittee. II ) Steel Authority of India Ltd ( Bhilai Steel Plant ). Vmoansa ( Altrrnotr ) CHIEB CEEHIST Tata Iron -6 Steel Co Ltd. P. Hyderabad Bhabha Atomic Research Centre. X.1987 ( Continued from page 1 ) Membrrs SERI P. Burnpur DRM. S. P. National -New Delhi ( Conrinwdon pa# 9 ) 2 . PANDA Mahindra Rqhessntiq Ugine Steel Co Ltd. VENKAT~WARLU SH~I K. Hyderabad SHRI MATA~SARAN ( Allcrnalr I ) SRRX B. Bltadravati Defence Metallurgical Research Laboratory. Ferro Alloys Corporation Enen & Co. RAJARAO SERI K. PRASHAR SHRI J. L. Bombay SHWI B. M. K. RAOEAVENDRAN. NARAIN SHRIG. V. Rourkela Metatluraical Laboratory ( CSIR 1. RAJABAX (Altan&) SHRI A. N. SARMA ( Alfrrnofs) SHRI N. BOSE Bhilai SERI E. BIS %lARYA Ferrous Metals Analysis. t.IS : 228 ( Part 6 ) . Bokaro Ltd. Jamrhedpur AIWISTANTCEIE~ CHIWIST ( Altrrnotr ) Indian Iron & Steel Co Ltd. RAHA ( Allernak.Jayh*pur a Physical New Qelhi Laboratory (CSIR). Rourkela SERI K. Bangalore Steel Authority of Plant ). ANNIAH ( Ahrnotr SHRI N. DAS ( Altrrnoh ) Steel Authority of India Ltd ( Rourkela Steel SHRI H. SMDC Centre. RAO ( Affrrn& Da CR. SVBBARAYAPFA DEP. BIS ( Ex-o&i0 M&u) SHRX h’f. BASKARAN Bharat Heavy Electrical1 Ltd. P.P. Shresramnagar Ltd (Bokaro Steel India ) ) Visvervaraya Iron & Steel Ltd. Bombay Director General. C. CEAXBABORTY SHRI L. PANDEY DR D. RAMAKSWXXNAN DR J. 2 :3 Bombay conocnrr DR C. H. IYER Bhabha Atomic Research Mtimbcrs SERI S. Assistant Director ( Metals ). R. SHRI U. MAHAPATBA ( Ahrnutr ) National DK L. SUBRAHMANIAM SEBI T.M. Director ( Strut & Met ) N Steel Authority of India Ltd (Rourkela Steel Plant ). RAI ( Altcrnae ) SHBI G. DAE Plant ). GVPTA Phydcal Laboratory ( CSIR ). SINHA SHRI K. P. BIS~NOI ( Altsrrak) SHEI -4.

0.1 This revision of IS : 228 (Part 6 )-1974t has been undertaken on the basis of experience gained during the implementation of the standard by the manufacturers and testing laboratories. covered the chemical analysis of pig iron. 0. IS : 228-1959* version has 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. cast iron and plain carbon and low alloy rteelr ( &sad).3 In this revision. after thedraft finalized by the Methods of Chemical Analysis of Ferrous Metals Sectional Committee Chad been approved by the Structural and Metals Division Council. revision of IS : 228 was 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 for each constituent in steels. *Methodr of chemical analysis of pig iron.2 IS : 228 which was issued -as a tentative standard in 1952 and revised in 1959. 3 . cast iron and plain carbon and low alloy steels.1 This Indian Standard ( Part 6 ) ( Third Revision ) was adopted by the Indian Standards Institution on 16 January 1987. -. Accordingly. major modifications are: a) scope of the method has been modified by lowering the limit for determination of chromium from 0’5 to 0’1 percent. 0. For convenience. FOREWORD 0. However. *Methods for chemical analyak of steels: Part 6 Determination of chromium by pcrsulphate oxidation method ( for chromium > 0’5 percent ) ( sacond rcuirion).IS:228(Pw6)-iW7 Indian Standard METHODS FOR CHEMICAL ANALYSIS OF STEELS PART 8 DETERMINATION OF CHROMIUM PERSULPHATE OXIDATION METHOD (FOR CHROMCUM > 0’1 PERCENT ) ( BY Third Revision ) 0.2. it was decided to publish a comprehensive series on chemical analysis of steels including high alloy steels.

REAGENTS 5. if the final value. is to be rounded off. SAMPLING samples shall be drawn Indian Standard.1 Phosphoric Water.t.various 0. analytical grade reagents ( see IS : 1070-1977t ) shall be employed in the test. OUTLINE OF THE METHOD 4. SCOPE 1.. QUALITY 3.nd 1 Acid . 5.1987 in the colour levels b) only one method has been prescribed for the correction titration of chromium for dilution effect and interference. This method is not applicable for steels containing tungsten. 4 . cool and *Rulea for rounding off numerical values ( rcmkd ). of the method at the .1 After d.Sulphuric Acid Mixture -To 600 ml of continuously 165 ml of concentrated sulphui-ic acid 132 ml of phosphoric acid ( rd = 1’75 ). manganese and ( vanadium if present) are oxidized by ammomum persulphate in presence of silver nitrate as catalyst.ssolution of the sample in dilute sulphuric acid and phosphoric acid mixture and further treated with nitric acid. and prepared as prescribed in the 2.1 This standard ( Part 6) covers the persulphate oxidation method for determination of chromium content of low alloy and high alloy steels containing more than or equal to 0’1 percent chromium.IS : 228 ( Part 6 ) . 1. Mix. observed or calculated.tLy. 4.1 Unless water OF REAGENTS and distilled specified otherwise.lt. add irP.1 The relevant 3. tSpecification for water for general laboratory use (-second revision ). chromi.4 In reporting the result of a test or analysis made in accordance with this standard. and c) inclusion of reproducibility of chromium content. 2.nm. Permanganic acid is then destroyed by dilute hydrochloric acid. Chromium is reduced by ferrous ammonium sulphate and excess of ferrous ammonium sulphate is back titrated with standard potassium permanganate solution. it shall be done in accordance with IS : Z-1960*.

Heat Oxidize black residue by addition the flask to decompose the sample. 250 ml of Hydrochloric Acid .1 : 3 hydrochloric acid (rd = 1’16 j Sulphate Solution 5. through a sintered glass crucible and keep in an 24 hours.5 Potassium 5.1987 5. PROCEDURE less than 2 percent) 6. amber-coloured glass bottle.1 Take 2 g of sample (for chromium and 0’2 to 0’5 g of sample for high alloy steels in a wide mouth conical flask. . Acid Relative density = 1’42 (conformDissolve 5 g of 5. Dissolve 3. and keep in a stoppered glass bottle.8 Standard Potassium Permanganate Solution .8) every time it is used. stir and allow to stind in a closed vessel for Filter. of concentrated nitric acid dropwise and heating the solution simultaneously till all carbides are decomposed and brown fumes are Dilute to 300 ml with hot water. *Specification for nitric acid (second retision ). 5. [ 1 ml of potassium permanganate solution (0’1 N) = 0’006 7 g of sodium oxalate 1.IS z 228 ( Part 6 ) . Standardize the solution as follows: Dissolve 9’134 g of sodium oxalate crystals. 5. solution. dried for 1 hour at 105°C in 200 ml of dilute sulphuric acid (1 : 50). Standardize against standardpotassium permanganate solution ( given under 5.Approximately 0’1 N. expelled. silver nitrate crystals in water and diluteto 1 litre. Add 50 ml of phosphoric acid-sulphuric acid mixture. 6.2 g of potassium permanganate crystals in 1 000 ml of water. Dissolve 40 g of ferrous ammonium sulphate in Filter. 5.4 Ammonium Persulphate Solution .2 Concentrated Nitric ing to IS : 264-1976* ).Dissolve 15 g of Use a freshiy prepared ammonium persulphate in 100 ml of water.3 Silver Nitrate Solution0’5 percent (m/v). Heat to 70°C and titrate with potassium permanganate solution until one drop produces a permanent pink colouration. sulphuric acid ( 5 percent) and dilute to 1 litre.7 Standard Ferrous Ammonium Approximately 0’1 N.6 Dilwte concentrated Permanganate Solution 1 percent ( m/v). (ZJ/II). if necessary. Dilute to 1 litre.

1 Add same amount of ferrous ammonium sulphate as used for the sample. 6. 6.5 The titration should be corrected for dilution effect and colour interference.IS t 228 ( Part 6 ) . Titrate back with dropwise addition of standard potassium permanganate solution to a permanent pink end point which persists for 30-40 seconds. 6. ferrous ammonium sulphate B = volume in ml of standard potassium permanganate solution equivalent to 1 ml of ferrous ammonium sulphate solution. CALCULATION 7.1 Calculate the chromium Chromium. 7. The correction may be made by the following method: 6. Wash the sides of the conical flask with water. titrate carefully to a pmk ends point which persists for at least.1987 heat the solution to boiling and add 20 ml of silver nitrate solution and 20 ml of ammonium persulphate solution adding little at a time and continue boiling till the permanganate colour develops fully (volume should be maintained at 300 ml by addition of hot water. Cool and add a known volume of standard ferrous ammonium sulphate solution until an excess of at least 5 ml is present. c = volume in ml of standard potassium solution required for titration.3 Add dilute hydrochloric acid dropwise to the boiling solution till permanganic acid colour is destroyed. 6 .5. If the colour does not develop add a few drops of potassium permanganate solution till the pink colour develops.C) D x 0’017 33 x 100 E A = volume in ml of standard solution added. Boil for 10 minutes more. 30 to 40 seconds. corrected permanganate for the blank. to ensure complete re-oxidation of the vanadium.4 In presence of vanadium. It should be ensured that sufficient persulphate is added. if necessary and also boiling should be a period of 8-10 minutes). Titrate with standard potassium permanganate to pink end point which lasts for 30 to 40 seconds. where percent = content (AB of the steel as follows: .2 Add a few pieces of glass beads. to the already titrated solution. 6.

18:2ZS(Part6)-1987 D = normality solution.2 Reproducibility a) f0’025 b) f0’036 c) fO’l20 percent at 0’1 to 0’5 percent percent percent chromium.2 ) A INDIAN STANDARDS ON METIIODS FOR CHEMICAL ANALYSIS OF STEELS IS : 228 Methods for chemical (Part analysis of steels: method and 1 )-1972 Determination of carbon by volumetric ( for carbon > 0’ 1 percent ) ( second rev&ion ) D e t ermination of manganese in plain carbon ( Part 2 )A987 low alloy steels by arsenite method ( thid revision > (Part 3 )-1987 Determination method ( third revision ) of phosphorus by alkalimetric method ( Part 4)-1987 Determination of carbon by gravimetric ( for carbon > 0‘1 percent ) ( third revision ) ( Part 5 )-1987 Determination of nickel by dimethyl lyoxime ( gravimetric ) method ( for nickel > 0’ 1 percent 3 (second revision ) ( Part 6 )-1987 Determination of chromium by persulphate oxidation method ( for chromium > 0’1 percent ) (third revision ) ( Part 7 )-1974 Determination of molybdenum by a-benzoinoxime method ( for molybdenum > 1 percent ) (second revision) 7 . and of standard potassium permanganate E = mass in g of the sample taken for the test. at 1 to 5 percent chromium. APPENDIX ( Clause 0. 7. at 0’5 to 1 percent chromium. for chromium 5 percent and d) ~fO’20 percent and above.

in plain carbon steels by evolution method (second revision ) of molybdenum by thiocyanate ( Part 10 )-1976 Determination (photometric) method ( for molybdenum up to 1 percent ) in low and high alloy steels ( second revision ) ( Part 11 )-1976 Determination of silicon by photometric method carbon steels and low alloy steels (for silicon 0’01 0’05 percent ) ( second revision ) in to ( Part by periodate manganese 12 )-1976 Determination of ( photometric ) method in low and high alloy steels ( for manganese up to 2 percent ) ( second revision ) 13)-1982 Determination of arsenic (Part 8 .IS:228(Part6)-1987 ( Part 8 )-1975 Determination of silicon by the gravimetric ( for silicon > 0’1 percent ) ( second revision ) ( Part 9)-1975 method Determination of sulphur .

C. D.IS : 228 ( Part 6 ) .1987 ( Continuedfrom page 2 ) Mnnbcrs SH~I J. P. VANDRIWALLA SHRI J. GUNDAPEA DR L. NARAIN SHRI G. Jamshedpur Visvesvaraya Iron & Steel Ltd. S. RAMDA~ SHRI R. Bombay 9 . R. BANERJEE (Altarnate P. K. Bhadravati Italab Pvt Ltd. DEY ( Altcmarc) National Metallurgical Laboratory ( CSIR ). PANDEY ( Altnnatc Represanting Steel Authority of India Ltd (Durgapur Plant ). Bokaro ) Sxsx G. SARMA ( AItrrnats ) Saab R. NATH Soar SHRI N. Bombay India Ltd (Bokaro Steel Steel ) Mahindra Steel Authority of Plant ). Durgapur Ugine Steel Co Ltd. MUXHERJEE Saxr P.

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