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METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART XIII DETERMlNATlON OF ARSENIC ( Third Reprint NOVEMBER 1998 )
: 543 : 546.19
(0 Copuright 1982
BAHADURSHAHZAFARMARG NEW DELHI 110002
CHEMIST & So~rrt CENTRI\L RAII~WAY.:WT CHIEF CREMIST ( Alternate ) Geological Survey of India. DUTTA Members SHRI G. N. GUPTA ( Alternate I ’ Ministry of Defence ( DGI ) SRRI J. Calcutta Da A. W. M.%NT DIRECTOR ( MET ). SMDC 2 Chairman Da R.\KI~A Indian Iron and Steel Co Ltd. CHOWDIWRY Snnt B. _&PA Representing Steel Authority of India Plant ).1982 Indian Standard METHODS FOR CHEMICAL ANALYSIS OF STEELS PART Xill DETERMINATION OF ARSENIC Methods of Chemical Analysis Sectional Committee. C~AKRABORTY Snnr M. M. CH. MUKIIEHJEE ( z‘. BHATTACKARJEE SHRI M. New Delhi DR V. SIIRI A. K. DUTTA SHt(t K. BH%TT. . CHA~RAVORTY ( Alternat ) National Physical Laboratory ( CSIR ). M.IS : 228 ( Part XIII ) . N.\CHAHYA( Alternate ) National Test House. Rourkela SJWI B. K. CHITTA~ANJAN ( Alternate) The Tata Iron & Steel Company Ltd. S. HOHIDER Plant ). Burnpur DIG M.hrTUJte ) ( Continued on page 2 ) @ wright 1982 BUREAU OF INDLW STANDARDS This publication is protected under the Indian Copyright Act ( 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.ority of India Ltd ( Bhilai Steel Plant ). Jamshedpur CH”EEFCHEMIST AYSIS'T. Bharat Aluminium Company Ltd. RDSO. SECU~l~ER. DUREY H. P. Calcutta Stc~tr P.. SHRI R. K. CHAWATHE Bombay Minist:y of Railways MRTALLUILCIST. C. MAHAPATRA ( Alfernate ) Indian Metals & Ferro Alloys Ltd. CHATTEXJEE ( Alternate ) India Government Mint ( Ministry of Finance ). Durgapur Ltd ( Durgapur Steel RAO Steebt. BHUCHAR Steel Authority of India Ltd ( Rourkela Steel SHRI S. N. New Delhi DR B. Koraput SHRI P.~R 9D ASSIST.
RAXAKRISENAN ( Alternate ) Bharat Heavy Electricals Ltd. C. P. B. RAJA RAO ( Alternate ) Directorate General of Ordnance Factories ( Ministry SH~I D. JAIN SHRI D. Bombay DR CH.1982 Members SHRI S. N. SHARMA Central Glass & Ceramic Research Institute DR B. G. SAXENA ( Alternate ) Hindustan Copper Ltd. Calcutta DR P. V. PATEL ( Alternate II ) Saru Smelting Pvt Ltd. PAX-TDEY ( CSIR ). RAJARAX SHRI K. SEN ( Alternate ) Ministry of Defence ( R & D ) DR P. Meerut Smzl D. C. PRASAD Bokaro Essen & Co. SEN of Defence ). DASCVJTTA Deputy Director ( Met ). Tiruchchirappalli SERI D. Calcutta SHRI R. R. Udaipur SERI G. VENKATESWARLU DR C. Bangalore DR J. IYER ( Alternate I ) SERI P. P. SHRI B. Director ( Strut & Met ) SHRI 0. N. IS1 2 . JETHWANI Directorate General of Supplies & Disposals.IS : 228 ( Part XIII ) . Bombay N. RAO ( Alternate ) Bhabha Atomic Research Centre. RAMA RAO. IS1 ( Ex-oficio Membn ) SHRI C. D. SINHA ( CSIR ). S. CF~AKRABORTY( Alternate ) Hindustan Zinc Ltd. KRANNA Delhi SHRI M. HO~AVAR SHRI J. P. CEOWDHARY ( Ahmate ) National Metallurgical Laboratory DR L. SIJBRAMANIAN SHRI B. Representing Italab Pvt Ltd. N. P. UNNI ( Alternde ) Ferro Alloys Corporation Ltd. New SHRI V. Shreeramnagar SHRI A. DEY ( Alter ‘le I ) SHRI J. L. P. RAMAXOORTHY SHRI M. Calcutta SHRI U. B. SAN~AMESWARA RAO SHRI G. Jamshedpur Steel Authority of India Ltd ( Bokaro Steel Plant ). MURVOAIYAN ( Alternate II ) Director General.
1 FOREWORD This Indian Standard ( Part XIII ) was adopted by the Indian Standards Institution on 22 February 1982.2 Earlier. and distilled do not water ( ~ee No~g -.IS : 228 ( Part XIII ) . observed or calculated. after the draft finalized by the Methods of Chemical Analysis Sectional Committee had been approved by the Structural and Metals Division Council.3 In reporting the result a test or analysis made in accordance with this standard. 3 . With the publication of this part.Rules for rounding off numerical values ( revised ). tMethods for chemical analysis of steels. it shall be done in accordance with IS : 2-1960:. &Specification for water for general laboratory use ( second revision ). of 1. chemicals contain impurities *Method for delermination of arsenic in iron and steel. QUALITY OF REAGENTS pure chemicals that 2. SCOPE 1.1982 Indian Standard METHODS FOR CHEMICAL ANALYSIS OF STEELS PART XIII DETERMINATION OF ARSENIC 0. for the determination of arsenic in iron. $. IS : 1070-1977s ) shall be used. ) prescribes the method for determination 2.1 Unless specified otherwise. determination of arsenic in iron and steel was covered in The Sectional Committee responsible for the revision IS : 1546-1960*. of this standard decided to publish this as a part of IS : 2287 for comHowever this method could also be applied prehensive analysis of steel. IS : 1546-1960* will be withdrawn. is to be rounded off. 0. 0. if the final value. 0.1 This of arsenic standard ( Part XIII in steel.‘Pure chemicals’ shall mean which affect the results of analysis.
Sodium Hypopkosphite - *Specification tspecification for nitric acid ( wend rcvisim ).42 ( conforming 1. Arsenic acid is reduced quantitatively in acid medium by sodium hypophosphite to metallic arsenic and the metal is then oxidized by a The measured excess of standard iodine solution to pentavalent arsenic.2.2. DETERMINATION OF ARSENIC IN STEEL 4. and 75 ml of concentrated nitric acid to 400 ml of water.7 Dilute Nitric Acid 1 : 50 ( v/v ).Add 200 ml of syrupy phosphoric acid.9 dioxide 4.2.6 Mixed Acids .10 - Potassium Permanganate Sulphurous Acid Solution in water.2 Reagents 4. pared by shaking small pieces of filter paper with a mixture of one part of saturated solution of bromine in concentrated hydrochloric acid When sufficiently disintegrated.3 Concentrated Ntric 1976* ). 4. excess iodine is back titrated with standard arsenious oxide solution.2.2.1982 3.2. 4. ( rd = l-1 6 ) and seven parts of water.8 4.16 to IS : 264to 4. GENERAL 3. ) when the alloy is dissolved in a mixture of sulphuric acid and nitric acid.2 Dilute Sulpkuric Acid - 1 : 3 ( v/v ). Add carefully 150 ml of dilute sulphuric acid ( 1 : 3 ) and make up to one litre. 4 . 4. filter paper pulp pad shall be used.4 Concentrated IS : 265-1976t ).IS : 228 ( Part %I11 ) . fbr hydrochloric acid ( second rcvirion ). I.1 Electrolytic Copper 4. the mixture shall be heated on the steam bath for 30 minutes and diluted with an equal volume of water. 100 ml of concentrated hydrochloric acid.2. shaken and bottled.1 Outline. 4.2. rd = Acid 85 percent. Mix well and cool.For the filtration of It shall be prearsenic precipitate. Prepare solid.5 Acid - Hydrochloric rd = ( conforming Syrupr Phosphoric Acid - 4. solid.1 Preparation of Filter Paper Pulp Pad .of the Method -Arsenic which in steel exists mainly as iron arsenide ( FeAse ) is converted into arsenic acid ( HyAsO. A filter pad shall be made of this pulp and washed well with water. 4.2. a saturated solution of sulphur 62.
nations have to be carried out. Boil for two to three minutes and cool.2.495 g of arsenious oxide in about 4 ml of sodium hydroxide solution ( 10 percent ).3. dilute toone litre with water ml of water. ( In case of high silicon iron.01 N.0. and dissolve in a mixture* of 30 ml of dilute sulphuric acid.2. Standardize against and store in a dark-coloured glass-stoppered bottle.Make a suspension of one gram of soluble starch in about 10 ml of water and add it carefully to 100 ml of boiling water. standard arsenious oxide solution. Dissolve 1. 4.3.12 Ammonium Chloride Solution Acid 40 percent. use 200 ml of the mixed acids ( see 4.2 Dilute the mixture slightly with hot water and filter off any graphite. 4.27 g of re-sublimed iodine and 4 g of potassium iodide in 25 When the solution is complete.2. and dilute to about 200 ml. 4.1982 4. 5 . 4. 4.0.1 Weigh accurately 5 g of the sample and 0. washing the beaker with 75 ml of concentrated hydrochloric acid. Add 2 g of sodium hypophosphite and warm to brisk effervescence avoiding boiling. Add dilute hydrochloric acid ( 1 : 20 ) until just acidic.5 g of electrolytic copper.3 Procedure 4. 15 ml of concentrated nitric acid and If a large number of determi20 ml of concentrated hydrochloric acid.2.11 Dilute Hydrochloric 4.14 Standard Iodine Solution ( 1 ml .01 N.0’000 15 g of As ) . Prepare the solution fresh as needed. Dissolve 0. transfer them to a 600-ml squat beaker.IS : 228 ( Part XIII ) .16 Starch Solution . To the filtrate add O-5 g of potassium permanganate and boil the mixture for at least 5 minutes.6 ) for each determination.17 Sodium Bicarbonate ( carbonate-free ) solid.13 HydroJuoric Acid - 1 : 3 ( VIU )* 5 percent. Add *In case of tmgsten steel. ) Concentrate the filtrate to 75 ml and transfer to 750-ml conical flask.2.2.2. silica should be filtered off at this stage.3 Evaporate the solution to fumes and heat until all the nitric acid is expelled. 4. Add about 75 ml of hot water and boil.2. 4. Wash the residue with hot dilute nitric acid and discard it.2. Add about two grams of sodium bicarbonate and dilute to one Iitre in a volumetric flask. Add enough sulphurous acid solution dropwise till the filtrate is clear.3. 4. mixed acids ( see 4.6) only hall be used for the dissolution of the sample.15 Standard Arsenious Oxide Solution .
and add by instalments 2-g portions of hypophosphite till effervescence ceases.3.3. allow to stand for 5 minutes and dilute to 250 ml.5 and 4. ‘4. add 80 ml of concentrated hydrochloric acid and 40 ml of water.3. 6 iodine solution added = [(A--B)- C] x 0~000 15 x 100 M .1982 by instalments 2-g portions of hypophosphite till effervescence ceases and finally add 12 g of sodium hypophosphite. Add 10 drops of hydrofluoric acid and 12 g of sodium hypophosphite.3. to the pentavalent state. Further proceed in accordance with 4.1.IS : 228 ( Part XIII ) . Boil under reflux tube and filter and wash the reduced arsenic as described under 4.5 Discard the filtrate and transfer the residue along with the filter pad to an 800-ml tall-form beaker. percent where A =-1 total volume in ml of the standard in the test. 4. 30 ml are usually adequate ). Cool the solution and filter through a pad of pulp prepared in accordance with 3. of water.3.4 Procedure for Reduction of Arsenic Acid ( in Case of Tungsten Steel ) Transfer the clear solution from 4. therefore 10 ml of standard arsenious oxide solution used in blank estimation represent 25 ml in the final titration. warm to brisk effervescence avoiding boiling.4 Calculation Arsenic. Stir to disintegrate the filter pad. 4. Since arsenic is oxidized from the elemental state. Insert a cork carrying a reflux condenser tube ( 600 x 10 mm ) in the mouth of the conical flask and boil the contents of the flask for 15 minutes.3. cool. discharge the coloration by adding about 3 ml more of standard arsenious oxide solution and about 2 g of sodium bicarbonate. until the blue colour just re-appears.3.6 Carry out a blank determination following through all steps of the procedure and using the same amounts of reagents ( including 10 ml of the standard arsenious oxide solution ) but without the material. Add a few ml of starch solution.3. and add 40 ml Boil the solution to expel nitric acid fumes completely. shaking vigorously for each addition. Add 2 g of sodium hypophosphite. Any amount in excess of this 25 ml that is required in titrating the blank represents volume of the standard iodine solution required for the blank. rinsing the funnel with 50 ml of Run in a measured excess of the standard iodine solution ( about water.2 to a quartz flask. Titrate with the standard arsenious oxide solution to pronounced lightening of the iodine colour. Wash the arsenic precipitate with 100 ml of dilute hydrochloric acid containing 3 g of sodium hypophosphite and then 7 times with ammonium chloride solution. 4.6. Back-titrate cautiously with the standard iodine solution.
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