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~(-‘“““’ ) 1997
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 3 DETERMINATION OF PHOSPHORUS BY ALKALIMETRIC METHOD (
Third Revision )
Fourth Reprinr NOVEMBER 1998
@ CopyYigh 1987
MANAK BHAVAN. 9 BAHADUR SAH NEW DELlU 11OOUZ c1 3
MUKHERJEE Steel Authority of India Ltd (Durgapur Steel Plant ). N. M. CHATTEBJEE ( Altarnatr ) SHRI C. K. Jamshedpur AS~IETANT Cantr CHEVIOT ( Alhnatr ) Sam M. N. KHANNA Directorate General of Supplies & Disposals. New Delhi SHRI J. DI~~EIT Ordnance Factory Board ( Ministry of Defence ). SLMDC 2 Chaimtaa Da C. S. BHAQWAT Kbandelwal Ferro Alloys Ltd. AQABWU ( Afhndr) SEBI S. B. CHAKRAVABTY Ministry of Defence ( DGI ) SHRI P. Durgapur ( Q Copyright 1987 Continued on pcrgr Authority Bhilai of India Ltd ( Bhilai Steel Plant). S. 2 ) BUREAU OF INDIAN STANDARDS This publication is protected under the Indian Copy@ Ad ( XIV of 1957 ) and 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. V. P. CHAKBABOBTY Indian Iron & Steel Co Ltd. MOIT~A ( Alfemafr ) SHRI V. D. GUPTA ( Alfanatr ) SHRI P. Bombay Snn~ R. CEAKBA Indian Metals t Ferro Alloys Ltd. Nagpur SEBI D. N. . M. RDSO. K. K. f-%iIEF CHEMIST Tata Iron & Steel Co Ltd.ISr228(Part3)-1987 Indian Standard METHODS FOR CHEMICAL ANALYSIS 6F STEELS PART 3 DETERMINATION OF PHOSPHORUS BY ALKALIMETRIC METHOD ( Third Revision) Methods of Chemical Analysis of Ferrous Metals Sectional Committee. Burnpur SERI M. Koraput CHEHIST & MICTALLU~~I~T Ministry of Transport ( Department of Railways) AWWITAHTR~~SEAROE O~~IOER (MET-~). IYER Mrmbrrs SEW G. S&N ( Altwnate ) DE M. Calcutta SHRI S. LUOKNOW ( Alm& ) . hPABA0 Steel Repenting Bhabha Atomic Research Centre.
SUBRAHMANIAM ) ( Altrmutr Rqmnting Mahindra Ugine Steel Co Ltd. Bokaro Laboratory Laboratory . P. Bhadravati Defence Metallurgical Research Laboratory. Hyderabad Bhabha Atomic Research Centre.IS : 228 ( Part 3 ) . Jamrhedpur CHIEB CHEXIST ASSISTANT CHIEY CHEMIST ( Ahmote ) Indian Iron & Steel Co Ltd. SABYA ( Altrrnatr ) SEBI N. P. V. RAMAXBIsENAN DsJ. Hyderabad SEW S. Bombay Director General. DAS ( Altmdr ) Steel Authority of India Ltd ( Rourkela Steel SXXI H. PANDA SEXI B. CHAKEABOBTY SHRI L. DAS Plant ). Sam U. M. SINEA SHIU K. Bombay Steel ) Authority of India Plant ). RAQHAVENDRAN. (CSIR Ltd. N. L. IYER Bhabha Atomic Research Mcmbns Bharat Heavy Electricals Ltd. Rourkela SHRI K. GUPTA New Delhi ( Conlinwd on pegs11) L . RAO ( Alfrraatr ) DR CH. NABAIN SERI G. BIS ( Ex-oficio Mnnbcr ) SEBI T. P. Shreeramnagar Ltd ( Bokaro Steel India Visvesvaraya Iron & Steel Ltd. P. S. RAJABAM ( Alternafa ) SHBI A. P. BISENOI ( Altsrnatr ) Laboratory Physical National (CSIR ). RAHA ( Altehale II ) Steel Authority of India Ltd ( Bhilai Steel Plant ).4. RAJA~AO SX~I K. BOSE Bhilai SHRI E. RAI ( Altrrsutt ) SEW C. C. K. BIS Ferrous Metals Analysis Subcommittee. Bangalore Steel Authorjty of Plant ). SEAWA Director ( Metalr ). COWdM SMDC 2 : 3 Centre. MAEAPATRA DB L. ( CSIR 1. Director ( Strut & Met ) As&ant SXRI M. BASXARAN SHRI MATA SARAN I Altrraat~ I ) SHBI B. Rourkela Ltd (Rourkela Steel National Metallurttical Jamrhedpur Physical National New Delhi Ferro Alloys Corporation Eraen & Co. VPNKATEBWARLU SEXI K. SEBI . j. R. VERQHESE ( Ahma ) Tata Iron & Steel Co Ltd. ANWAH ( Altmafr SHBI N. Bombay DB C. Burnpur DB M. P~CASEAII SHEI J. H. PANDXY DE D. M. K.1987 f Continued from peg* 1 ) Mmbus SHIU P. SUBBAI~AYAPPA DE P.
FOREWORD 0. ‘Methods chemical analyrir of pig iron. which was issued as a tentative standard in 1952 and revised in 1959. 0. has been undertaken on the basis of experience gained during the implementation of the standard by the manufacturers and testing labaratories. 0..2 IS : 228.1937 Indian Standard METHODS FOR CHEMICAL ANALYSIS OF STEELS PART 3 DETERMINATION OF PHOSPHORUS BY ALKALIMETRIC METHOD ( Third Revision) 0. Accordingly.2.rion ). For the convenience it was decided to publish a comprehensive series on chemical analysis of steels including high alloy steels. high chromium.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. 3 of . method for determination 0.1 This revision of IS : 228 ( Part 3 )-1972t. tMethods for chemical analyria of rteelr: Part 3 Determination of phosphorus by alkalimetric method ( sscend r&. revision of IS : 228 was 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 ( Parts 1 to 13 ) ( see Appendix A 3 covering separate method of analysis version has for each constituent in steels. However. covered the chemical anaIysis ofpig iron.3 In this revision following alloy steels has been incorporated: of phosphorus in and similar a) Stainless steel. IS : 228-1959’ 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 steels. cast iron and plain carbon and low alloy rteelr ( m&cd).IS : 228 ( Part 3 ) . nickel chromium alloy steels without tungsten or vanadium.
2. titanium or or zirconium. High speed steels or other without vanadium. QUALITY OF REAGENTS 3. 4. and up to 0’1 percent. known excess of standard sodium hydroxide solution and the excess is titrated against standard nitric acid solution. is to be rounded off. 4.IS:22S(Part3)-1987 b) 4 4 4 f) Steel containing high silicon. Dissolve 2 g of potassium 4.2 Potassium Permanganate Solution permanganate in 100 ml of water. it shall be done in accordance with IS : 2-1960*. OUTLINE OF THE METHOD 4. other steels containing with or Chromium vanadium steels vanadium but no tungsten. 4 .2. tspecification for water for general laboratory use (second rerririon).1 Unless specified otherwise. SCOPE 1.2 Reagents _ 1 : 1. 1 : 3.4 In reporting the result of a test or analysis made in accordance with this standard. if the final value. and prepared as prescribed in the 3. Steels containing arsenic 0. *Ruler for rounding off numerical valuer ( rruirrd).1 Phosphorus is converted to orthophosphoric acid and precipitated The precipitate is dissolved in as ammonium phosphomolybdate.1 The relevant samples shall be drawn Indian Standard.1 Dilute Jvitric Acid- 4. analytical grade reagents and distilled water (see IS : 1070-19771) shall be employed in the test.1 This standard ( Part 3 ) covers phosphorus content of plain carbon metric method. 2. observed or calculated. 1. Austenitic manganese steels containing tungsten steels. SAMPLING method for determination of steel and alloy steels by alkali- 2. 1 : 5 and 2 : 98 (v/v).
Dissolve 100 g of molybdic acid (Moos.1 Solution A . 40 percent.220.127.116.11.O ) in one litre of dilute sulphuric acid ( 5 : 95 ). nitric acid Potassium Nitrate Solution - 1 percent 4. 4.2.1 ) slowly and with constant stirring to solution B ( see 4.16 4.2.5 Concentrated Nitric Acid IS : 264-1976* ).2.14 4.2. 1 g of powder alcohol. 4. 85 percent ).2 Solution B . Dissolve phenolphthalein in 100 ml of rectified spirit or methyl 4. water with sulphur dioxide gas. and standardize against staudard nitric acid ( 4.2.6 Ammonium Molybdate Solution-Add solution A (see 4.10 ). Filter the solution through Whatman filter paper No.12 18.104.22.168.8 Phenolphthalein Solution . Relative ( conforming 4. 4. 1 : 20 (v/v). 70 percent.2.7 490 ml of concentrated (m/v).4 Concentrated Ammonium Hydroxide 4. Standardize against sodium carbonate previously ignited at 350°C and cooled.6.2.Nitric Acid Solution . 5 percent (m/v). 040 before use. to 4.Add to 1 150 ml of water and cool.1 percent. dilute 7 ml of concentrated nitric acid to one litre with freshly boiled distilled water.9 Sodium Hydroxide Solution .2.10 Standard . Add 10 ml of ammonium phosphate solution ( 1 g/l) and keep th e solution at least for 24 hours. Dilute Ammonium Hydroxide Sulphurous Acid Saturate 1 : 1. Relative density density 1’42 0’90. 4. 5 . 7H.6. dissolve 4’5 g of sodium hydroxide in one litre of freshly boiled and cooled distilled water.0’1 N.11 4. Cool the solution.6.2. Sodium Carbonate - 100 g of ferrous sulphate Ferrous Sulphate Solution -Dissolve ( FeSOa.2.2 ) kept cool in a cold waterbath.13 4.2. *Specification for nitric acid ( second rrucsion ).IS:228(Part3)-1987 4.15 crystals 4. 4.0’1 N.17 Lilute Hydrochloric AcidHydrofluoric Acid Perchloric Acid 1 : 1 (u/u) and 2 percent (v/v).2. or 118 g of ammonium molybdate in a mixture of 145 ml of ammonium hydroxide ( rd = 0’90 ) and 270 ml of water.2.2-3 Sodium Nitrite Solution 5 percent (m/v).
4 Warm the solution to about 60-80°C and add 50 ml of ammonium molybdate solution. Add about 25 ml of water. Add sodium nitrite solution dropwise till the brown precipitate is dissolved. l Specification for hydrochloric acid ( second rcuision ). precipitate and filter pad twice with 5 ml portions of dilute nitric acid (2 : 98) and five times with 5 ml portions of potassium Continue washing of the precipitate and filter pad with nitrate.Quantity of nitric acid added at this stage will depend upon the actual volume of the solution.ensity 1’ 16 ( conform- 4.19 1 : 4 (v/v). 5. Dissolve the precipitate adding dilute nitric acid(1: 1)d ro p wise and add 2 to 3 ml of concentrated nitric acid. Dilute Hydrobromic Acid - Relative d. flask.6 Transfer the pulp along with the precipitate to the flask. stopper the flask. 5. Keep the 5. Wash the flask. potassium nitrate solution until the washings are acid free ( 10 ml portion of the washings in presence of phenolphthalein should turn pink on adding one drop of 0’1 N sodium hydroxide solution ). The analyst will ensure that the acidity of the solution before precipitation of phosphomolybdate complex is maintained at 5-10 percent.1 Transfer 2 g of the sample in a 250-ml conical dilute nitric acid (1 : 1) till the vigorous reaction flask at low heat till it dissolves.3 Add ammonium hydroxide till brown precipitate of ferric hydroxide appears.IS:228(Part3)-1987 ing to 4.18 Comentruted Hydrochloric Acid IS : 265-1976* ). Boil to expel oxides of nitrogen. titrate with standard nitric acid solution to the disappearance of pink colour .2. 5.2.2 Add 5 to 10 ml of potassium permanganate solution and boil for few minutes. If manganese dioxide does not precipitate add further permanganate solution till a precipitate of manganese dioxide appears and boil for few minutes. Add 30 ml of subsides. 5. 6 . 5. shake vigorously for a few minutes and allow to stand for half an hour. PROCEDURE ALLOY STEEL FOR PLAIN CARBON WITHOUT VANADIUM STEEL AND LOW 5. few drops of phenolphthalein and a known volume of sodium hydroxide solution (which should be l-2 ml in excess) Dilute to about 100 ml and and shake to dissolve the precipitate.5 Filter the precipitate through a filter paper pulp pad by suction. NOTE .
acid. PROCEDURE FOR ALLOY STEELS 6.2 to 5. add 5 ml of ferrous sulphate solution and 2 to 3 drops of sulphurous acid. High Silicon.1 Transfer 2 g of the sample to a 400-ml beaker. Cool.6.2 Cool the solution to lo-2O”C. filter through paper pulp and wash with sodium carbonate solution.4 High Speed with or Without Steels or.2 to 5.3 Chromium Vanadium But Vanadium No Tungsten Steels or Other Steels is Containing for the 6.4.6. take up with 4-O ml of water and 10 ml c f concentrated nitric acid.3. 6.1 when the solution precipitation of phosphomolybdate complex. fume with 1 ml hydrofluoric acid and a few drops of Fuse the residue with concentrated nitric acid at low temperature. filter through paper pulp and wash with hot dilute nitric acid (1 : 5). Proceed further as in 5. Titanium or Zirconium and proceed as the procedure given in 6. Collect the filtrate in 500-ml conical flask and proceed as in 5.2. Acidify the filtrate with concentrated nitric acid and add to the main filtrate. boil for few minutes. if required.Transfer 2 g of the sample in a 400-ml beaker.2 Steel Containing 6. and shake to mix well. 60 ml concentrated nitric acid and few drops of hydrofluoric acid and evaporate to dryness.1 up to filtration 6. Decompose the sample in 60 ml of dilute nitric acid (1 : 3) and a few drops of Add 20 ml concentrated hydrochloric hydrofluoric acid.5 to 5. Proceed further as in 5.2.IS:228(Part3)-1987 6.1 Proceed as in 6. High Chromium.6. ready 6. Other Vanadium Steels Containing Tungsten 6.1 ) in a platinum crucible and ignite.3. Add 50 ml of ammonium molybdate solution. shake vigorously for a few minutes and allow to stand overnight.1 Stainless Steel. Place the beaker at low heat until the reaction subsides and then add 15 ml of perchloric acid. Evaporate to copious fumes and fume for a few minutes. stopper the flask. sodium carbonate. Take the precipitate and pulp ( as in 6. Dissolve the melt in water. Digest with 20 ml of concentrated 7 . 6. 6.1 Follow follows. Add 50 ml of a 1 : 1 mixture of concentrated hydrochloric acid and nitric acid and a few drops of hydrofluoric acid.2 Collect the filtrate in a 500-ml conical flask and preserve it. Nickel Chromium and Similar Alloy Steel Without Tungsten or Vanadium .
6. Dissolve the precipitate in minimum hot dilute nitric acid (1 : 5) and add to the main filtrate (see 6. 6. Filter through Whatman filter paper No. Add 20 ml of perchloric acid and fume to expel1 nitric acid. Cool. Add hydrotluoric acid drop by drop until all the hydrated silica is dissolved and a few drops in excess.3.2 and 5. BLANK DETERMINATION the same procedure and 7.6. 6.2. and evaporate to syrupy liquid. add about 40 ml of water and 10 ml concentrated nitric acid and boil for few minutes. dissolve the precipitate in the beaker with minimum quantity of dilute ammonium hydroxide (1 : 1) and pour it through the filter pad collecting the solution in a beaker.1 ). Proceed further as in 5. Add 30 ml concentrated nitric acid. add about 40 ml of water and 10 ml nitric acid. complete the determination as in 5.IS:228(Part3)-1987 hydrochloric acid.6. add about 80 ml of dilute hydrobromic acid and evaporate to copious fumes.6.3 Treat the filtrate as in 5. wash the beaker and the filter pad with dilute ammonium hydroxide (1 : 1) until all of the tungstic acid has been dissolved and collected.5 Austenitic Manganese Steels . dilute to about 25 ml and boil for a few minutes. proceed further as in 6.6 Steels Containing High Arsenic Up to 0’1 Percent 6.4 to 5. If the sample contains vanadium.1 Make a blank determination following using the same quantity of all reagents. 8 . keeping back the precipitate of tungstic acid in the beaker. Add a few ml of the main filtrate ( end of. In the absence of vanadium. Add 15 ml of perchloric acid and evaporate just to white fumes.2 to 5. Cool.4.4. 42 and wash with dilute ammonium hydroxide (1 : 20). 7.6.4. dilute to 50 ml with water and boil.Decompose 2 g of the sample in a 400-ml beaker in 40 ml of dilute nitric acid (1 : 3).4.3. Heat so that perchloric acid refluxes on the sides of the beaker for about 25 minutes. Add dilute ammonium hydroxide (1 : 1) in slight excess and heat to flocculation. Add 5 ml concentrated nitric acid. 6. Wash twice with hot dilute hydrochloric acid ( 2 percent ).1 ) to’ this solution and slightly acidify with dilute nitric acid (1 : 1).1 Decompose 2 g of the sample in 400-ml beaker in 40 ml of’ dilute nitric acid (1 : 3).2 To recover phosphorus from the precipitate of tungstic acid. Cool. Proceed further as in 5. Collect the filtrate in a 500-ml conical flask and evaporate to a small volume. Filter through a paper pulp as far as possible by decantation.6.2 to 5.
CALCULATION 8. and D = quantity 8. Phosphorus where A = millilitres of standard nitric acid solution required in the sample in the titration of the excess sodium hydroxide ( see 5. B = millilitres of standard nitric acid solution blank determination (see 7. f 0’001 5 percent. of 1 ml standard required nitric in the acid percent.2 ) IS : 228 Methods (Part ( Part ( Part (Part for chemical analysis A of steels: method and 1 )-1972 Determination of carbon by volumetric ( for carbon > 0’1 percent ) ( second revision ) 2 )-1972 Determination of manganese in plain carbon low alloy steels by arsenite method ( secona’retiion ) 3 )-1972 Determination of method ( sechd revision ) phosphorus by alkalimetric method 4)-1974 Determination of carbon by gravimetric ( for carbon ) 0’ 1 percent ) (second revision ) of nickel ( for nickel ( Part 5 )-I974 Determination ( gravimetric ) method revision ) by dimethylglyoxime > 0’5 percent ) (second chromium by persulphate ( Part S)-1974 Determination of oxidation method ( for chromium ) 0’5 percent ) (second revision ) 9 .IS:228(Part3)-1987 8.6 ).2 Reproducibility of sample in g.1). C = phosphorus equivalent solution.1 Calculate phosphorus. ( percent as: ) = (B-A) D x C x 100 APPENDIX ( Clause 0.
IS:228(Part3)-1987 ( Part 7 ).1974 Determination of molybdenum by a-benzoinoxime method ( for molybdenum > 1 percent ) ( second revlion) (Part Determination of silicon by the gravimetric 8)-1975 ( for silicon > 0’1 percent) (second revision ) method ( Part 9 )-I975 Determination of sulphur in plain carbon steels by evolution method (second revision ) (Part of molybdenum by thiocyanata la)-1976 Determination ( photometric ) method ( for molybdenum up to 1 percent ) in low and high alloy steels (second revision ) 11 )-1976 Determination of silicon by photometric method in carbon steels and low alloy steels (for silicon 0’01 to 0’05 percent ) ( second revision) 12)-1976 Determination of manganese by periodate ( photometrie ) method in low and high alloy steels ( for manganese up to 2 percent ) (second revision ) 13 )-1982 Determination of arsenic (Part (Part (Part 10 .
T. RAMDAL~ Italab Pvt Ltd. NARAIN SRRI G. NATH Plant ). Gnwnapp~ ( Alternate ) Metallurgical Laboratory ( CSIR ). R. Durgapur Steel SRRI P. Steel Represcntin~ Authority of India Ltd (Durgapur Plant ). Bhadravati SEBI G.IS : 228 ( Part 3) . K. Bokaro SEW N. DEY ( Akcmate ) 11 . P.1987 ( Con&4rdfiom pqc 2 ) Mmbrrs S_HRI MUKEERJEE J. D. C. BANERJEE f Alternate ) Mahindra Ugine Steel Co Ltd. PANUEY Jamshedpur Visvesvaraya Iron & Steel Ltd. Bombay SHRI R. SARYA ( Aftmate ) Steel Authority of India Ltd ( Bokaro Steel SRRI R. National DR L. S.A SHRI J. Bombay Sam P. VANDRIWAI.
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