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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
S. MOIT~A ( Alfemafr ) SHRI V. B. Burnpur SERI M. Jamshedpur AS~IETANT Cantr CHEVIOT ( Alhnatr ) Sam M. N. CEAKBA Indian Metals t Ferro Alloys Ltd. SLMDC 2 Chaimtaa Da C.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. f-%iIEF CHEMIST Tata Iron & Steel Co Ltd. Durgapur ( Q Copyright 1987 Continued on pcrgr Authority Bhilai of India Ltd ( Bhilai Steel Plant). V. 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. S&N ( Altwnate ) DE M. S. K. hPABA0 Steel Repenting Bhabha Atomic Research Centre. Nagpur SEBI D. Calcutta SHRI S. Bombay Snn~ R. . DI~~EIT Ordnance Factory Board ( Ministry of Defence ). K. P. N. New Delhi SHRI J. M. MUKHERJEE Steel Authority of India Ltd (Durgapur Steel Plant ). CHAKBABOBTY Indian Iron & Steel Co Ltd. LUOKNOW ( Alm& ) . Koraput CHEHIST & MICTALLU~~I~T Ministry of Transport ( Department of Railways) AWWITAHTR~~SEAROE O~~IOER (MET-~). CHATTEBJEE ( Altarnatr ) SHRI C. RDSO. N. CHAKRAVABTY Ministry of Defence ( DGI ) SHRI P. AQABWU ( Afhndr) SEBI S. IYER Mrmbrrs SEW G. K. GUPTA ( Alfanatr ) SHRI P. KHANNA Directorate General of Supplies & Disposals. M. BHAQWAT Kbandelwal Ferro Alloys Ltd. D.
S.1987 f Continued from peg* 1 ) Mmbus SHIU P. Bangalore Steel Authorjty of Plant ). RAO ( Alfrraatr ) DR CH. SEBI . Hyderabad SEW S. DAS Plant ). RAHA ( Altehale II ) Steel Authority of India Ltd ( Bhilai Steel Plant ).IS : 228 ( Part 3 ) . P~CASEAII SHEI J. BIS ( Ex-oficio Mnnbcr ) SEBI T. M. M. VERQHESE ( Ahma ) Tata Iron & Steel Co Ltd. COWdM SMDC 2 : 3 Centre. L. Bombay DB C. ANWAH ( Altmafr SHBI N. SUBBAI~AYAPPA DE P. Bombay Steel ) Authority of India Plant ). BASXARAN SHRI MATA SARAN I Altrraat~ I ) SHBI B. RAJA~AO SX~I K. BOSE Bhilai SHRI E. R. (CSIR Ltd. RAJABAM ( Alternafa ) SHBI A. MAEAPATRA DB L. P. NABAIN SERI G. SEAWA Director ( Metalr ). SUBRAHMANIAM ) ( Altrmutr Rqmnting Mahindra Ugine Steel Co Ltd. Burnpur DB M. BIS Ferrous Metals Analysis Subcommittee. RAMAXBIsENAN DsJ. PANDXY DE D. CHAKEABOBTY SHRI L. Shreeramnagar Ltd ( Bokaro Steel India Visvesvaraya Iron & Steel Ltd. RAQHAVENDRAN. Rourkela Ltd (Rourkela Steel National Metallurttical Jamrhedpur Physical National New Delhi Ferro Alloys Corporation Eraen & Co. IYER Bhabha Atomic Research Mcmbns Bharat Heavy Electricals Ltd. Rourkela SHRI K. Director ( Strut & Met ) As&ant SXRI M. ( CSIR 1. SINEA SHIU K. K. Hyderabad Bhabha Atomic Research Centre. PANDA SEXI B. Bhadravati Defence Metallurgical Research Laboratory. GUPTA New Delhi ( Conlinwd on pegs11) L . C. P. BISENOI ( Altsrnatr ) Laboratory Physical National (CSIR ). j. Bokaro Laboratory Laboratory . P. Bombay Director General. H. P. K. V. VPNKATEBWARLU SEXI K. Sam U. DAS ( Altmdr ) Steel Authority of India Ltd ( Rourkela Steel SXXI H. P. SABYA ( Altrrnatr ) SEBI N.4. N. Jamrhedpur CHIEB CHEXIST ASSISTANT CHIEY CHEMIST ( Ahmote ) Indian Iron & Steel Co Ltd. RAI ( Altrrsutt ) SEW C.
covered the chemical anaIysis ofpig iron. method for determination 0. Accordingly. 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. However. For the convenience it was decided to publish a comprehensive series on chemical analysis of steels including high alloy steels. 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. FOREWORD 0.2 IS : 228.. nickel chromium alloy steels without tungsten or vanadium. 0.1 This revision of IS : 228 ( Part 3 )-1972t.IS : 228 ( Part 3 ) .2. 0. cast iron and plain carbon and low alloy steels. cast iron and plain carbon and low alloy rteelr ( m&cd). 3 of . tMethods for chemical analyria of rteelr: Part 3 Determination of phosphorus by alkalimetric method ( sscend r&. has been undertaken on the basis of experience gained during the implementation of the standard by the manufacturers and testing labaratories. 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. high chromium.1937 Indian Standard METHODS FOR CHEMICAL ANALYSIS OF STEELS PART 3 DETERMINATION OF PHOSPHORUS BY ALKALIMETRIC METHOD ( Third Revision) 0.1 This Indian Standard ( Part 3 ) ( Third Revision ) was adopted by the Indian Standards Institution on 16 January 1987. ‘Methods chemical analyrir of pig iron. which was issued as a tentative standard in 1952 and revised in 1959.rion ).3 In this revision following alloy steels has been incorporated: of phosphorus in and similar a) Stainless steel.
1 : 5 and 2 : 98 (v/v). SAMPLING method for determination of steel and alloy steels by alkali- 2. if the final value. 2.1 The relevant samples shall be drawn Indian Standard. 4. *Ruler for rounding off numerical valuer ( rruirrd). OUTLINE OF THE METHOD 4.1 Phosphorus is converted to orthophosphoric acid and precipitated The precipitate is dissolved in as ammonium phosphomolybdate. 4 . and up to 0’1 percent.4 In reporting the result of a test or analysis made in accordance with this standard.IS:22S(Part3)-1987 b) 4 4 4 f) Steel containing high silicon. 1 : 3. Austenitic manganese steels containing tungsten steels. Steels containing arsenic 0. tspecification for water for general laboratory use (second rerririon). observed or calculated. known excess of standard sodium hydroxide solution and the excess is titrated against standard nitric acid solution. 1. SCOPE 1. QUALITY OF REAGENTS 3. High speed steels or other without vanadium. is to be rounded off. 4. and prepared as prescribed in the 3.2 Reagents _ 1 : 1.2.1 Dilute Jvitric Acid- 4. 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*. analytical grade reagents and distilled water (see IS : 1070-19771) shall be employed in the test.2. titanium or or zirconium. other steels containing with or Chromium vanadium steels vanadium but no tungsten.1 Unless specified otherwise.1 This standard ( Part 3 ) covers phosphorus content of plain carbon metric method.
040 before use. 5 . water with sulphur dioxide gas.17 Lilute Hydrochloric AcidHydrofluoric Acid Perchloric Acid 1 : 1 (u/u) and 2 percent (v/v).2.14 4.0’1 N.2.Dissolve 100 g of molybdic acid (Moos. 4.2 ) kept cool in a cold waterbath.2. 7H. 5 percent (m/v).2.7 490 ml of concentrated (m/v).16 4.O ) in one litre of dilute sulphuric acid ( 5 : 95 ).2 Solution B .220.127.116.11.2.5 Concentrated Nitric Acid IS : 264-1976* ). nitric acid Potassium Nitrate Solution - 1 percent 4. or 118 g of ammonium molybdate in a mixture of 145 ml of ammonium hydroxide ( rd = 0’90 ) and 270 ml of water.2.15 crystals 4.6 Ammonium Molybdate Solution-Add solution A (see 4. 40 percent.1 ) slowly and with constant stirring to solution B ( see 4.2-3 Sodium Nitrite Solution 5 percent (m/v).0’1 N. and standardize against staudard nitric acid ( 4. 4.2.2. dissolve 4’5 g of sodium hydroxide in one litre of freshly boiled and cooled distilled water. to 4. 4.2. Relative density density 1’42 0’90. 4.2.10 ).2. 1 : 20 (v/v).12 4.2.Add to 1 150 ml of water and cool.13 4.8 Phenolphthalein Solution .4 Concentrated Ammonium Hydroxide 4. Sodium Carbonate - 100 g of ferrous sulphate Ferrous Sulphate Solution -Dissolve ( FeSOa.2. 85 percent ). Filter the solution through Whatman filter paper No.1 Solution A .IS:228(Part3)-1987 4.2. Add 10 ml of ammonium phosphate solution ( 1 g/l) and keep th e solution at least for 24 hours. *Specification for nitric acid ( second rrucsion ).2.9 Sodium Hydroxide Solution .10 Standard . 4. dilute 7 ml of concentrated nitric acid to one litre with freshly boiled distilled water. Standardize against sodium carbonate previously ignited at 350°C and cooled.1 percent. Dissolve phenolphthalein in 100 ml of rectified spirit or methyl 4. 70 percent. Cool the solution.11 4.Nitric Acid Solution .2.6. 1 g of powder alcohol. Relative ( conforming 4. Dilute Ammonium Hydroxide Sulphurous Acid Saturate 1 : 1.6.6.
Boil to expel oxides of nitrogen. 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. 5. Wash the flask. 5.2. Add 30 ml of subsides. Add sodium nitrite solution dropwise till the brown precipitate is dissolved. flask.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.2.6 Transfer the pulp along with the precipitate to the flask. 6 . 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. Dissolve the precipitate adding dilute nitric acid(1: 1)d ro p wise and add 2 to 3 ml of concentrated nitric acid. NOTE .18 Comentruted Hydrochloric Acid IS : 265-1976* ). The analyst will ensure that the acidity of the solution before precipitation of phosphomolybdate complex is maintained at 5-10 percent. 5. PROCEDURE ALLOY STEEL FOR PLAIN CARBON WITHOUT VANADIUM STEEL AND LOW 5. 5. stopper the flask.4 Warm the solution to about 60-80°C and add 50 ml of ammonium molybdate solution.Quantity of nitric acid added at this stage will depend upon the actual volume of the solution.19 1 : 4 (v/v). If manganese dioxide does not precipitate add further permanganate solution till a precipitate of manganese dioxide appears and boil for few minutes. 5. 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 ).IS:228(Part3)-1987 ing to 4. Dilute Hydrobromic Acid - Relative d.ensity 1’ 16 ( conform- 4. l Specification for hydrochloric acid ( second rcuision ).2 Add 5 to 10 ml of potassium permanganate solution and boil for few minutes. Add about 25 ml of water. shake vigorously for a few minutes and allow to stand for half an hour. Keep the 5.3 Add ammonium hydroxide till brown precipitate of ferric hydroxide appears.5 Filter the precipitate through a filter paper pulp pad by suction. titrate with standard nitric acid solution to the disappearance of pink colour .
Collect the filtrate in 500-ml conical flask and proceed as in 5. 60 ml concentrated nitric acid and few drops of hydrofluoric acid and evaporate to dryness. and shake to mix well. 6. Nickel Chromium and Similar Alloy Steel Without Tungsten or Vanadium . 6.2 Steel Containing 6. Proceed further as in 5. Dissolve the melt in water. Acidify the filtrate with concentrated nitric acid and add to the main filtrate. High Chromium.3 Chromium Vanadium But Vanadium No Tungsten Steels or Other Steels is Containing for the 6. Take the precipitate and pulp ( as in 6.2.IS:228(Part3)-1987 6.3.1 Follow follows. boil for few minutes.1 Stainless Steel. filter through paper pulp and wash with sodium carbonate solution. 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 5.4 High Speed with or Without Steels or. ready 6.2 Cool the solution to lo-2O”C. add 5 ml of ferrous sulphate solution and 2 to 3 drops of sulphurous acid. Place the beaker at low heat until the reaction subsides and then add 15 ml of perchloric acid.Transfer 2 g of the sample in a 400-ml beaker. stopper the flask. High Silicon. acid.1 Transfer 2 g of the sample to a 400-ml beaker.1 when the solution precipitation of phosphomolybdate complex. Titanium or Zirconium and proceed as the procedure given in 6. Proceed further as in 5.4. sodium carbonate.1 Proceed as in 6.6.2 Collect the filtrate in a 500-ml conical flask and preserve it. Add 50 ml of a 1 : 1 mixture of concentrated hydrochloric acid and nitric acid and a few drops of hydrofluoric acid. filter through paper pulp and wash with hot dilute nitric acid (1 : 5). if required. Cool. 6.2. Evaporate to copious fumes and fume for a few minutes.6.2 to 5. PROCEDURE FOR ALLOY STEELS 6. Add 50 ml of ammonium molybdate solution.3.1 ) in a platinum crucible and ignite. fume with 1 ml hydrofluoric acid and a few drops of Fuse the residue with concentrated nitric acid at low temperature. Other Vanadium Steels Containing Tungsten 6. shake vigorously for a few minutes and allow to stand overnight. take up with 4-O ml of water and 10 ml c f concentrated nitric acid.1 up to filtration 6. Digest with 20 ml of concentrated 7 .6.2 to 5.
6. Heat so that perchloric acid refluxes on the sides of the beaker for about 25 minutes.6.6.2 to 5. dilute to about 25 ml and boil for a few minutes.IS:228(Part3)-1987 hydrochloric acid.4. Wash twice with hot dilute hydrochloric acid ( 2 percent ). 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.6 Steels Containing High Arsenic Up to 0’1 Percent 6. 6. 6. add about 40 ml of water and 10 ml nitric acid. Proceed further as in 5. keeping back the precipitate of tungstic acid in the beaker. Proceed further as in 5. Add hydrotluoric acid drop by drop until all the hydrated silica is dissolved and a few drops in excess.3 Treat the filtrate as in 5. Filter through Whatman filter paper No. BLANK DETERMINATION the same procedure and 7. Dissolve the precipitate in minimum hot dilute nitric acid (1 : 5) and add to the main filtrate (see 6. 7.2 and 5.1 ).1 Decompose 2 g of the sample in 400-ml beaker in 40 ml of’ dilute nitric acid (1 : 3). wash the beaker and the filter pad with dilute ammonium hydroxide (1 : 1) until all of the tungstic acid has been dissolved and collected. and evaporate to syrupy liquid. Cool. Add 30 ml concentrated nitric acid. add about 80 ml of dilute hydrobromic acid and evaporate to copious fumes.4. Add dilute ammonium hydroxide (1 : 1) in slight excess and heat to flocculation.2 to 5. Cool.2. 6.6. Add 15 ml of perchloric acid and evaporate just to white fumes.1 ) to’ this solution and slightly acidify with dilute nitric acid (1 : 1). Add a few ml of the main filtrate ( end of.3.6.4. Filter through a paper pulp as far as possible by decantation.4.4 to 5. Add 5 ml concentrated nitric acid. In the absence of vanadium. Add 20 ml of perchloric acid and fume to expel1 nitric acid. complete the determination as in 5. dilute to 50 ml with water and boil. 42 and wash with dilute ammonium hydroxide (1 : 20). Collect the filtrate in a 500-ml conical flask and evaporate to a small volume.3. proceed further as in 6.5 Austenitic Manganese Steels .6.1 Make a blank determination following using the same quantity of all reagents. Cool. If the sample contains vanadium. 8 .2 To recover phosphorus from the precipitate of tungstic acid.Decompose 2 g of the sample in a 400-ml beaker in 40 ml of dilute nitric acid (1 : 3). add about 40 ml of water and 10 ml concentrated nitric acid and boil for few minutes.
( percent as: ) = (B-A) D x C x 100 APPENDIX ( Clause 0. B = millilitres of standard nitric acid solution blank determination (see 7.2 Reproducibility of sample in g. C = phosphorus equivalent solution. f 0’001 5 percent.6 ). Phosphorus where A = millilitres of standard nitric acid solution required in the sample in the titration of the excess sodium hydroxide ( see 5.IS:228(Part3)-1987 8.1 Calculate phosphorus.1).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 . of 1 ml standard required nitric in the acid percent. and D = quantity 8. CALCULATION 8.
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 .IS:228(Part3)-1987 ( Part 7 ).
Durgapur Steel SRRI P. Bhadravati SEBI G. R. Bombay Sam P. VANDRIWAI. National DR L. NARAIN SRRI G. PANUEY Jamshedpur Visvesvaraya Iron & Steel Ltd. Gnwnapp~ ( Alternate ) Metallurgical Laboratory ( CSIR ).A SHRI J. RAMDAL~ Italab Pvt Ltd. Bombay SHRI R. S. P. NATH Plant ). D. K.IS : 228 ( Part 3) . Steel Represcntin~ Authority of India Ltd (Durgapur Plant ). DEY ( Akcmate ) 11 . Bokaro SEW N. BANERJEE f Alternate ) Mahindra Ugine Steel Co Ltd. SARYA ( Aftmate ) Steel Authority of India Ltd ( Bokaro Steel SRRI R.T. C.1987 ( Con&4rdfiom pqc 2 ) Mmbrrs S_HRI MUKEERJEE J.
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