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इंटरनेट मानक Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 15396 (2003): Chemical Analysis of Ferro-Silicon-Zirconium Alloys [MTD 5: Ferro Alloys] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 15396:2003 Indian Standard CHEMICAL ANALYSIS OF FERRO-SILICON- ZIRCONIUM ALLOYS Ics 77.100 0 BIS 2003 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 September 2003 Price Group 2 Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2 FOREWORD This Indian Standard was adopted bytheBureau ofIndian Standards, after the draft finalized by the Methods of Chemical Analysis ofFerrous Metals Sectional Committee hadbeen approved bytheMetallurgical Engineering Division Council. Ferro-silicon-zirconium alloys aremaster alloyswhich arerequired formaking additions ofsilicon andespecially zirconium toprepare iron base alloys. Zirconium isfor refinement and grain size improvement and silicon for imparting strength to the alloys. Inreporting the results ofatest oranalysis made inaccordance with this standard, ifthe final value, observed or calculated, istoberounded off, itshallbe done inaccordance with IS2: 1960‘Rules forrounding off numerical values (revised)’. IS 15396: 2Q03 Indian Standard CHEMICAL ANALYSIS OF FERRO-SILICON- ZIRCONIUM ALLOYS 1SCOPE 5.2 Reagents This standard covers themethods ofchemical analysis 5.2.1 Sodium Peroxide, solid. of various constituents of ferro-silicon-zirconium 5.2.2 Hydrochloric Acid, rd = 1.16 (conforming to alloys, general composition for which isgiven below: IS 265). Composition Percent 5.2.3 Dilute Hydrochloric Acid, (1:1)and (5:95). Silicon .30to 50 Iron 60 to 70 5.2.4 Hydrojluoric Acid, 48 percent. Zirconium 12.01040.0 5.3 Apparatus 2REFERENCES 5.3.1 Zron/lVickef Crucible, 30 ml capacity. The standard listed below contain provisions which 5.3.2 PTFE Beakers, 250 ml capcity. through reference .inthis text, constitute provisions of this standard. At the time of publication, the editions 5.3.3 Platinum Crucible, 30 ml capacity. indicated were valid. All standards are subject to 5.4 Procedure revision and pm-ties to agreements based on this standard are encouraged to investigate the possibility 5.4.1 Transfer 0.5 g of the sample to a 30 ml iron/ of applying the most recent editions of the standards nickel (preferable) crucible. Add 5 g of sodium indicated below: peroxide. Mix thoroughly using an iron/rtickel platinum rod and transfer any adhering particles on IS No. Title the rod tothe crucible by gently tapping. 264:1976 Nitric acid (second revision) 265:1993 Hydrochloric acid ~ourth revision) 5.4.2 Cover the mixture with a layer of 2 g sodium 1070:1992 Reagent grade water (third revision) peroxide. Heat the crucible on a hot plate for 10-15 1472:1977 Methods of sampling of ferro alloys min to expel any moisture. Carefilly fuse over alow for determination of chemical flamemufflefurnace,slowlyrotating thecrucible,until composition (first revision> the contents have melted. Increase the temperature to bright redness for aminute. 3 SAMPLING 5.4.3 Remove the crucible from the flame, cover and The sample shall be drawn and prepared as per the allowtocool.Tapthecruciblegentlyandtransferittoa method given in IS 1472. 250 ml stainless steelPTFE beaker. Add 50 ml water cautiously.Whenthereactionceases,removethecrucible 4QUALITY OF REAGENTS andrinsewithwater,addingthewashingstothebeaker. Unless specified otherwise, analytical grade reagents 5.4.4Acidi& withhydrochloric acid(1:1),addanother anddistilled water (seeIS 1070)shallbe employed for 50 mlhydrochloric acid (1:1). Transfer the solution the test. toa250mlglassbeaker.Washthestainlesssteel/PTFE 5 DETERMINATION OF SILICON BY THE beaker with hydrochloric acid (1:1), transferring the GRAVIMETRIC METHOD washings to theglass beaker. 5.4.5 Evaporate to dryness on awater bath when the 5.1 Outline of the Method residue isdry, allow to-cool. Add 20 ml hydrochloric The sample is decomposed by fusion with sodium acid, stir well cover the beaker, and heat for a few peroxide. Silica is separated by dehydration with minutes. Dilute with 200 mlofhot water, digest fora hydrochloric acid. The solution is filtered. Silica is fewminutesandfilterthrough afilterpaper,containing ignited and weighed. It is then volatilized with some filter pulp. Wash with hot hydrochloric acid hydrofluoric acid. The residue isignited andweighed. (5 :95)eighttimesandthenthoroughly withhotwater. The lossinmass represent silica. Reserve thepaper and residue. 1 IS 15396:2003 5.4.6 Evaporate the filtrate to dryness and bake to after addition of asmall quantity of tin. 11O(’Cfor 1h.Cool,add20mlhydrochloric acid,digest 6.2.6 Dilute Sufphuric Acid, (1:19). onawater bath for 10min. Add 20mlwater, stirwell, filter andwashwith hothydrochloric acid(5:95) eight 6.2.7 Ferrous Ammonium Sulphate Solution times and then with hot water, till free from chloride. (O.10N)—Dissolve 40gofFeSO, (NH,),.SO,. 6H,0 Preserve the filtrate, after making itup to 250 ml. indilute sulphuric acid. Transfer to a 1Iitreflask and dilute tovolume with the same acid. 5.4.7 Place the filter paper with residue in a 50 ml platinum crucible, heat slowly to remove,the water, Pipette out 50 ml of the solution in a 600 ml beaker, raise the heat to char the paper and finally ignite at diluteto400mlwithwater. Add 20mlofacidmixture 1 IOO”C, after covering the crucible. Cool in a and 5drops of indicator. Titrate with hot bichromate desiccator. Weigh andagain igniteat 11O“Cfor 10min to purple end point. and check for constancy inmass. 6.2.8 Potassium Bichromate Standard Solution (O.1 Add 2 to 3 ml sulphuric acid (1:1) to moisten the N)—Transfer 4.9015 gofK2Crz07,previously dried residue, followed by 5ml hydrofluoric acid. at 11O°Ctoa 1litre flask. Dissolve inwater anddilute to the mark. Evaporate to dryness, ignite at 1100”Cand weigh. 6.2.9 Phosphoric Acid (H3POJ and Sulphuric Acid 5.5 Blank (H#O,) Carry out a blank determination following the 6.2.10 Diphenylamine Sulphonate procedure, but without the sample. 6.3 Procedure 5.6 Calculation 6.3.1 Pipette out analiquot, containing approximately Silicon, percent =[(A-B)-C]X0.4674 X100 50 to 100 mg iron, from the solution preserved10 by mass D under 5.4.6 and transfer to a 600 ml beaker. Add where stannous chloride solution, dropwise till the yellow colourofthesolutiondisappears.Add3dropsinexcess. A = mass, in g, of the crucible before Dilute to 200 mlwith water and cool to 10“C.Add 15 hydrofluorization; ml of saturated mercuric chloride solution, allatonce. B = mass, in g, of the crucible after Mixwell andkeep onthe water bath for 3to5min. hydrofluorization; 6.3.2 Add 20 ml of acid mixture and 5 drops of C = correction for the blank, ing; and indicator solution. Dilute to 400 ml and titrate with D = mass, ing, of the sample taken. standard potassium bichromate solution to a distinct purple end point. 6 DETERMINATION OF IRON 6.3.3 Blank 6.1 Outline of the Method Determine the blank valueof the reagents, using the [nthe filtrate, after removal of silica, iron isreduced same amount of all reagents and following the with a slight excess of stannous chloride. The excess procedure. Before titration withpotassium bichromate isoxidized by addition of mercuric chloride solution. solution, add 1.0 ml of ferrous ammonium -sulphate After addition of sulphuric-phosphoric acid mixture, solution. Inanother beaker, place 400 mlofcolddilute ferrous iron is titrated with potassium bichromate, sulphuric acid and add 1 ml of ferrous ammonium using diphenylamine sulphonate, as indicator. sulphate solution. Add 20 ml of acid mixture and 5dropsofindicator. Titratewithpotassium bichromate 6.2 Reagents solution. Record this titration and substract the value 6.2.1 Hydrochloric Acid, rd = 1.16 (conforming to obtained from the bIank, to get the corrected blank. IS 265). 6.4 Calculation 6.2.2 Dilute Hydrochloric Acid, (1:1)and (1:9). 6.2.3 Nitric Acid, rd= 1.42(conforming to IS 264). Iron, percentbymass= =(A-~)xcxloo 6.2.4 Mercuric Chloride Solution, saturated. 6.2.5 Stannous Chloride (10 percent) — Dissolve 100 g of stannous chloride in 500 ml hydrochloric A = volume, in ml, of potassium bichromate acid, dilute to 1 litre. Keep in a dark closed bottle, solution required for titration of sample; 2 IS 15396:2003 B= volume, in ml, of potassium bichromate 7.3.3 Dissolve theprecipitate onthe filter using 30ml sokuion required for titration of blank; ammonia (1:4) and collect the solution in the same c= iron equivalent of potassium bichromate beaker inwhich precipitation was carried out. Repeat solution, in gper ml; and this operation twice, using each time, 30mlammonia (1:4). Finally give 2washings to the filter paper with D= mass, ing, of sample taken for titration; 5mlofammonia (1:9).Seethat the ammonia solution 7 DETERMINATION OF ZIRCONIUM BY comes incontact with all sides of the beaker and that GRAVIMETRIC METHOD any adhering precipitate isbrought into solution. 7.3.4 .Add 25 ml mandelic acid solution, 3 drops of 7.1 Outline of the Method methyl.red indicator, andneutralize with hydrochloric In the tihrate, after removal of silica, zirconium is acid. Add 10ml of hydrochloric acid, in excess, stir precipitated as the mandelate, by the addition of and allow to digest on the water bath for I h. mandelic acid. Zirconium mandelate, thus obtained, isignited and weighed asthe oxide, Zr02. 7.3.5Filter warm, through aclose textured filterpaper and wash the precipitate six times with 1.0ml of 7.2 Reagents 10percent cold mandelic acid wash solution. 7.2.1 Dilute Ammonia, (1:40) and (1:9). 7.3.6 Transfer the paper and precipitate to a tared platinum crucible, dry,charandfinallyheatto.1OOO°C. 7.2.2 Hydrochloric Acid, rd = 1.16 (conforming to Keep atthis temperature for 30 min. Cool and weigh IS 265). asZr02. 7.2.3 A4andelic Acid(15 percent) —.Dissolve 15gof 7.4 Blank mandelic acid inwater and make up to 100ml. Carry out a blank determination following the same 7.2.4 Mandelic Acid Wash Solutwn — Dissolve 10g procedure, but without sample aliquot(s). of mandelic acid in 100ml hydrochloric acid. 7.5 Calculation 7.3 Procedure 7.3.1 Pipette out-50mlof the filtrate, after removal of Zirconium, percentbymass =‘A-B)xO-7403 XIOO silica, asgiven in5.4.6 to a250 mlbeaker. Adjust the o G acidity to4from 6inhydrochloric acid. Add 35mlof mandelic acid solution and dilute to 150 ml. Digest where thesolution for 1honawaterbath, untiltheprecipitate A= mass, in g, of Zr02 obtained from in the settles down, leaving aclear supematant liquid. sample aliquot; 7.3.2 Filter through a close textured filter paper and B= mass, ing, of ZrOzin g inthe blank; and wash 3 times with 10 ml portion s of cold mandelic c. mass, ing,of sample inthe aliquot taken. acid wash solution. Bureau of Indian Standards BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote harmonious development of the activities of standardization, marking and quality certification of goods and attending to connected matters inthe country. Copyright BIS has the copyright of all its publications. No part of these publications may be reproduced in any form without the prior permission in writing of BIS. This does not preclude the free use, in the course of implementing the standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating to copyright be addressed to the Director (Publications), BIS. Review of tndidn Standards Amendments are issued to standards asthe need arises on the basis of comments. Standards are also reviewed periodically; a standard along with amendments isreaffirmed when such review indicates that no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards should ascertain that they are inpossession ofthelatest amendments oredition by referring tothe latest issue of ‘BIS Catalogue’ and ‘Standards: Monthly Additions’. This Indian Standard has been developed from Doc :No. MTD 2(4237). 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