INTERNATIONAL Iso STANDARD 14284 First eestinn 1986-07-01 Steel and iron — Sampling and preparation of samples for the determination of chemical composition Fontes etaciers — Prélevement et préparation das échantilons pour (a détermnation de a compostion chimique This material is roprocueed ftom 160 documents under Intervationat Organization for Standardlzaion (180) Copyright Licence muarber WSNECHOD6. Nat for resale. Na part of tae 180 documents May De "produced i any form, electronic retreval system or otherwise. except as ‘llowad in the copyright law ofthe couulry of use, er withthe prior vite coneant of ISO (Case postal 56, 1211 Geneva 20, Switzerlancl FAX #41 22 734-1075), IMS oF the ISO Licensor’s members. Reference number 180 14284-19966) Copright bythe Intentional Grganization For Standardization a 04 149:38 20084180 14284:1996(E) Contents Page 1 Seope eres 1 2 Normetive references... 1 3 Definitions. 1 4 Requiremen:s for sempling and sarmole preparation 2 41 Gonera 2 42 sample. 2 43° Selection of a sae nn 4 44 Preparat‘on of a sample 5 45 Safety procautions 2 5 Liquid iton for steetmaking and pig-ron production 7 51 Gonoral 7 52 Spoon samping 7 53 Probe sampling 8 54 Preparation of a sample “or analysis .. 8 8 Liquid iron fer cast iran production .. 8 81 General... 82 Spoon sampling 63 Prove sarvling dente a) 64 Preparation of a sarrple for analysis seis 1 65 Sampling and sample preparation for the detemination of oxygen, nittogan snd hydrogen 12 © 150 19% AIL EQhIs reserved. Unless otienwise speciied, no part of this publication may 8 repro: ‘tuced or uttizac in any form or by any means, skectrenic or mecharieal nelicing phot: copying and microfilm, witout permission in wieing from the publisher Intorrational Organization tor Stardarszation (Case Powsle 56 « CH-1711 Geneve 206 Switzerland Frinted in Switzerand Conmright bythe Internstionl rgsnization For Stondortiration Sal Jan U4 11350 2005also 180 14284:1998(E} 7 Liquid stes! for stee! productior 71 General 7.2 Spoon sampling .. 7.3 Probe sampling 7-4 —Proparation of @ semple for analysis ne 75 Sampling and samo reparation fo tho determination of oxygen .. 7.8 Sarnpling and sample preparation for the determination of hydrogen 8 — Figitons 81 Geneva 82 Incremen: sampling 83 Preparation of a sample for analysis, 9 Castiron products 91 General 92 Sameling and sample preparation 10 Steel products 10.1 General 102 Selection of z preliminary Sample ora sama for analysis from a cast product, 193 Selection of a preliminary sample ora samale for analysis from a wrought product a 10.4 Preparation of a sample for aralysis 105 — Sarnpling of leaded steel 106 Sampling and sample praparation for the de:orminatian, of cxvgen 10.7 Sampling and sampia praparation for tho determination ef Fydrogen Annexes, A Sampling probes for use vith liquid iran and steel 8 Sampling probes for use with liquid steal for the determination of hyUFOger «ern Copright bythe Intentional trganization For Standardization Sal fan 04 1495-50 200 w 2 2 ” 1% " u 6 6 6 6 ” " 18 19 2 19 19 zu 22 FeISO 14284:1996(E) oIsa Foreword ISO {the International Organization for Standardization) is a worldwide fed- sralion of netional standards bodies (SQ member bodies). The work of preparing Intornational Standaros is normaly carried out through ISO technical committess. Each mernber body interested in a subject for which 9 technical committee has been established has the right to be rep- resented on that committee. International organizations, governmental and nan governmental, in faigon with ISO, olao take part in the work. ISO col laborates closely wh the International Electrotechnical Commission (EC) onail matters of electrotechnical standardization. Draft International Standards adopted by “he technical comrittees are cir- culttad to the member bodies for voting, Publication as an Intemational Standard requires approval by at least 75 % of the membe" kodiss casting avote. International Standard ISO 14284 was prepared by Technical Committee. ISOMC 17, Steel, Subcommittee SC1, Methods of determination of chemical composition. It cancels and replaces ISO 377-2:1988, of which it constitutes ¢ technical revision. Annexes A and 6 of this International Standard are for inforsmetion only, Copmright bythe International Crnizaton For Stendarization Sal J OA 14380 200INTERNATIONAL STANDARD ©1SO ISO 14284:1996(E} S—— Steel and iron — Sampling and preparation of samples for the determination of chemical composition 1 Scope ‘Ths Intemational Standard specifies methods for sampling and sample preparaton far te determi- nation of the chemical composition of pig iron, cast iron and steel Methods are specified for use with both liquid and solid metal 2 Normative references The following standards contain provisions which, through reference in this Intesnatianel Standard. At the time of publication, the editions indicated were vail All standards are subjeel to revision, and partes 1a agreaments based on thie Internatonal Standard ara encouraged to investigate the possibilty of apatving the mest recent editions of the standards indicated belaw. Members of IEC and ISO maintain registers of curronty valid International Standards, 1S0.377:—0), Steel and sige! products — Location of samples and test pieces for mechanical testing. 180. 9147:1987, Pigrons — Definition and classifi cation. 3. Definitions For the purposes of this Internationa Slandard, the following definitions apaly 3.1. chemical method of analysis: Method for the determination o* chemical compesition in which the sample is submitted to chernical reactian, 14 Tobe published. (Revision of ISO 977-1:1989 Copright bythe International Grganization For Standardization Sal fan 04 1495-50 200 3.2. physical method of analysis: Method for the determination of chemical compositian in which the cetermination of compostion is carried out without submiting the sample to cteirical reaction, tor example én optical emission spectrometric method, an Y-ray fluorescence spectiometric method, 3.3. thermal method of analysie: Method for tho cetermination of chemical composition in which the sample is submitted to a process of heating, combus- Yon oF fusian 3.4 melt: Liquid metal from which a sample is re- moved. 3.5 spoon sampling: Mettod in which the sample is taken fiom the mek, or during the pouring of the mel, using @ long-handled spoon. and cast into @ small mouid. 3.6 spoon sample: Sample taken from the ill sing @ spoon and cast nto a small mould. 3.7. probe sampling: Method in which the sample is veken from the melt using 4 commercially available sempting probe inserted inte the met 3.8 immersion sampling: Method ot probe sam- pling in which the probe ia immersed in the melt where the sample chamber in the probe fills by ferro- static pressure or gravity, 3.9. suction sampling: Metho¢ ot probe sampling in which the probe is immersed in the mek where the sarmple chamber in the probe fills by asgiration.IV TACOS TSSOE) 3.10 stream sampling: Method of probe sampling which the probe is inserted into a stream of linuid metal vihere the sample chamber in the proba fils by ‘the force of metal flow. 3.11. probe sample: Sample taken from the mett Using commercially available sa:npsing probe, 3.12 cast product: it2rn of Iron or steel which has not been subject to deformation, for exampls, an in- ot, @ semifinished product obtained by continuous casting, a shaped casting, 3.13. wrought product: item of steal which has beer subject ‘o daformation by rolling, drawing, forg- ing or sorne other snethod, for example, a bar, 2 billet, aplate, 2 sifip, a tube, a wire. 3.14 sample product Spocifc item of iron or atoo! selected from a supplied quantity for the purpose of obtaining a sample. 3.15 preliminary sample: Sufficient quantity of metal selected from the samole product ‘or the pur- pose of oblaining one ar more samples for analysis. 3.16 sample tor analysts: Part of the sample prod- at, oF part of the preliminary sample taken from the. sample praduct, or part of the sample taken from the ‘elt, brought to ¢ requited concition for submission to. analysis. The sample for anelysis may comprise the sample product itself or the sample taken from the melt NOTE 1 Tho following cstegorice of sample for anatysie are dstinguished: — sample in the form of a sold mass; — semple that has oeen ramelted — sample in the form of chips obtained by machinag: — sample in the form of fragments obtained by cornmi- nution: = sample in the form of powder odtained by comminution. 3.17 test portion: Part of the sernple for analysis, or part of the sanipls taken from the melt, actually sub- mitted to analysis, In certsin cases, the test portion rray be selected ftom the sarnole product itseif NOTES 2 The following srecisl types of tast rortions in the form of a solid mass obtained fecm a probe sample are dis- tinguished — test portion in the shape of a small disc, commonly do- satibed as a slug, obtained by punching: — test portion in the form of 2 sinall appendege, com- monly described as a iug; — test portion in the form of a smalliameter rod, come snonly descrised as.a pin. obtained by cutting Copright bythe Intoenstional trganiztion For Standardization Sal fou 04 1495:51 200 BIS @ Whan the cample for analysis is in the form of chips or powder, or when a semple in the form of 2 solid ‘ass is analysed by a thermal method, the test portion is obtained bby weighing, in the cose of a physical method of analysis, the part actually analysed wil consttute orly a small mass. of the sample ‘or anaiysis. In an optical emission spectio- metric method, the mass of meial consumed if an elgcrri= cal discharge is about 85mg t> 41mg; in an Xray fluor escence spectrometric method, the characteristic radiation is preduced from avery thin syrtace layer af the sample. 3.18. grinding: Method of preparing a sample ot metal for e physical methed of analysis in which the surface of the sampie for anaysis is abraded using an abrasive wheel 3.19 linishing: Method of preparing a samrle of metal for a physical method ot analysis in which the surface of the sample for analysis 1s abraded using a Floxible rotating dsc or continuous belt costed w'th an abrasive substance. 2.20 milling: Method of preparing sample chips or the surface of 2 sample for a physical method of analysis in which the surface of the sample is ma chined using a sotating, multi-edged cutting tool, 3.21 consignment: Quantity cf metal delivered at ‘one time. 3.22 Increment: Quantity of metal cotaired by sampling at one time from a consignment 4 Requirements for sampling and sample preparation 4.1 General This clause covets tha genaral raquiramanta for +16 sample, and for the sampling and sample preparation of iron and steal. Special requirements apply to cach category of liquid and solid rata: and these are con sidered in the televant subclause. ‘The sequence of samptirg and sample preparation of liguid ircn end steel, and cast iron, ana Steal products is shown in figure 1. Spatial consiverations apply 10 pig irons (see clause 8). 42 Sample 42.1 Quality Sampling practices shall be designed to provide a semple for analyss that ts representative of the mesn chemica! egrnposition of the rrelt oF the eampe product.C~) Prove simple Sime tor anaes ai Ligud ron and steel BOM PEON TOES Product bateh 1 ‘Sample product Prainivery sample Sanple for analysic (bFCast on and steel provers Figure 1 — Sequence of sampling and sample preparation The sample for analysis shall be sufficiently home- geneous with respect to chemical composition such that inhomogeneity does not appreciably contribute to the error variability of the method of analysis, How- ever, in the case of a sample taken from a melt, some variabilty, ‘n analysis. both within and hatwesn samples for analysis, may be unavoidable; this varia bifity will form an inherent part of the repeataoility and reproducibility of the analysis, ‘The sampla for analysis shall be free ftom surlace coatings. and from moisture, dirt or other forme of contamination, ‘As far as nossible, the sample for analysis chould be {ree from vaids, cracks and porosity, and frern fins, laps or other surface defects, Copright bythe International trganiztion For Standardization Sal fou 04 1495:51 200 Particular care shall b= taken wren selacting and pre- paring the sample for analysis, where a sample taker ‘trom a melt is expected to be heterogeneous or con- taminated in eny way, A sample teken from a melt shal! ba cooled in such a manner that the chemical camposition and metallurgt- cal structure of the sample is consistent from sample to sampe. It is important 10 recagrize that anelysis by some physicel methods may be influenced by the metal- turgcal stone of the sample, pariculary in the ¢26e of irona with white and grey’iton structures, and in the ease of steels in the as-cast and weought con- ditions.FO 14eS4. 1990(E} 422 Size The dimensions of a preliminary sample in the form of a soid mass shall be sufficient to permit additional samples for analysis to be taken for wrenalysis, where necessary using an alternative method of analysis. A sample for analysis, of a sufficient mass to provide for any re-analysis nacassary, shall be prepared. Ger erally, a msg of 109 g will be sufficiert for a sample inthe form of chips or powder. The dirrensional requirements for a sample for analy: sis in the form of a solid mass will depend upon the method solecied fer analysis. In the case of optical emission and Xway fluorescens spactiometiic, methods, the shage and size of the sample will be de- termined by te dimensians of tne sample chamber. The dimensions for samples for analysis given in this International Standard should be regarded as indica- tive only. 42.3 Wentification A sample for analysis shall be assigned @ unique identification in orcer to determina the mek of sample product from which it was taken and, if necessary, the Processing conditions of the melt or the location of the preliminary sample or the semple for analysis in the samale preduct. A sample for analysis of pig iron shall be assigned a unique identifieation in ofder to determina “he con. signment or part of consignment and the increment from which it was taken, Labeling or some equivalent method of marking shsit be Used to ensure that the assigned identification remains assocated with the semple ‘ior analysis. The identification, status and condition of the sample shall be recorded to onsure that confusion cannot, arise as to the identity of the item to which anelysis, and racords refer. 42.4 Conservation Adequate storage facilities shell be provided to segre- gate and protect the sample for andysis. During and etter preparation, the sarnpte (or analysis shal be stored in auch a wey 88 to prevent contamination or chemical change. I is permitted to conserve the preliminary sample in the farm of @ sold mass, and a sample for analysis, may then be prepared when required. ‘The sample for analysis, or the preliminary sample in ‘the form of a solid mass, shall be kept for a sufficient period of time to protect the integrity of the test lab- oratary, Coprright by the International Grganization For Standardization Sal fou 04 1495:51 200 Sisv 425 Arbitration In the case of a sample intended for arbitration, the sample for analysis shall d6 prepared joirtly by tre supplier and purchaser, oF by their 1epresentatives. A record shall be kept ef the methods used for pregarirg ‘the sample for analysis. Containers with samples for analysis intended for arbi tration shall bo soaled by both parties or by their rop- resentatives, Unioss agreed to the contrary, these containers shall bs keot by the representatives of each party responsive for tre p-eparation of samplas. 43. Selection of a sample 43.1. Sample froma mett Melts aro samplad at various stages in tha manufac- turing process for the purpeses of moritorina and controlling the process. Sanples can be taken during the casting of the melt 10 verity chemical compositicn in accordance with the specification of the cest prod- uct. In che caso of liquid metal intended for the pro- duction of a casting, tha samole for analysis ‘rey be selected from. test ters or blocks specialty cast from the same metal as that of the casting for purposes of mechanical tasting, in accordance with the product standard Sampling practices for malts shall be designed 10 provide samples during 2 porticuler rmenufacturing process in accordance wth requirements for sample quality (see 4.2.1), The sample obtained from @ melt is Usually m the fore of a smal inget, @ eylindical or rac- angular block, @ chiitoast diss or a combination of a disc with one or mere atteched pins; “1 some cases small lugs af@ attached to a disc sarale NOTE4 Sampling probes for use with iguid ron and steal may be obtained from 8 number af supeliers: the main faa tures of the different types of probe ae distinguishad ia annexes & and B, whieh include cimensions tor intorrraticn, only 4.3.2 Sample from a product ‘The preliminary sernple ur the sarnale for analysis can bbe selected from the sample product at the location indiceted in the product specifeation tor th selection of material for mechanical testing. when available, In the case of an iron casting, the sample for analys's cen be selected from a bor or block cast onto the casting, In tha case of 2 forging, the sample for analysis cen 2e sclected from the itiai starting materia from which the forging has baen mace, of from pro- longetions of the forging or from aditional forgings. In the absence of requirements given in the product, standard, or of a specification when orderng theroduc: the sample for analysis may, following agreement between the supplier and tha’ purchaser, be selected from the sample for mechanical testing or irom the test piece, or directly from the sample product. The preliminary saraple or the sample far analysis can te obtained from the sample product by machining or by using a cutting torch. Special considerations apply in the case of sampling for the determination of cer ‘ain elements, 4.4 Preparation of a sample 4.4.1 Preliminary preparation Kt any part of the sample is table to be nan Fepresantative In chemicst composition, for example due to oxidaton, it ray he agreed, following an inves- tigation to establish the nature and extent of any change in composition, t remove from tho sample ‘those parts thai have changed. Fallowing this oper ation, the sample shall then be protected trom any change in composition if necessary, the surface of the metal shall ke laid completely tare at the point of machining, by any suitable moang, to remove any coating that has been applied during manufacture. If necessary, the surface. of the meta! shall be degrecsed by means of a suit- able solvent, tacen cere to ensure that the manner of degreasing does not affect ine comectness of analysis, 4.42 Sample for anslysis in tha form of chips The semple for analysis shall consist of chips of a reguler size anc shape. These may de obtained by methods such 3 dilling, milling, turning or punching. The chips shell rot he taken trom apart of tha sample ‘thot has been effected by the heat of a cutting torch, The tools, machines and containers used during Preparation of the sampfe shall be cleanad beforshend 1p pievent any camamination of the semple for analy- ss. Machiring shall be carried out in such @ way thut the nips are not subject to overheating, as indicated by a change in the colour {blueing or blackening! of the chips. Unavodable coloration of chips obtained fram some types of alloy see's, far example manganese and austenitic steels, can ba minimized oy selaction of approptiate :co's and cutting speeds. Heat treatment may be required te gofton the sample. for machining ‘The use of coolants during machining is only permit- ted in exceptionel cases; ofte which the chips shall be cleanec by maans of a suitable solvent which doos not leave any deposit, Copmright y the fnterastional trganiaton For Standardnation Sado UA 149852 2005, 190 14254. 1S96/E} Chips shall be thoroughly mixed before weighing the test portion. For most purposes. it is satisfactory to mix the chips by rolling tha container on a level sur face ardor gently tumbling the container. 4.4.3 Sample for analysis in the farm of » powder or fragments Where atiling of the sample to obtain chips is imprac- ticable, it shall be cut or broken into pisces. These pieces shall then be crushed using a percussiar. mar- ter of a vbratory grinding mill, alsu known as a cise ‘mill of ring mill, to obtain a sarnple for analyais in the form of a powder, the whole of which passes throug a sieve of a specified aperture size In some appications for the determination of carbon using a thermal method of analysis, the sample is, crushed in a percussion mortar to obtan a sample for analysis in the form of fraaments with a particle size range of approximately 1 mm to 2 men Equipment used for comminution shall be construcied. fram material which doas not alter the sample com- position. Suitable tests may be necessary 10 shaw that the use of such equipment does not effect zhe ‘composition of the sarnple tor analysis in any wey. Comminution shatt not be used for the preperation of samples of giaphite-bearing irons, The sieving operation shall be performed taking all Precautions necessary to avoid contamination of lees of material. When seving hare materials, care shall be taken tp avoid damaging the fabric of the sieve. Tho sample for analysis shall be homogenized befor weighing the tast portion. Powders can ke homogan- ized by stirring CAUTION — Finely-divided metals of particle size loss than approximately 150 yn can procent a fire tsk. Ensure that there is adequate ventilation during comminution. 4.4.4 Sample for analysis in the form of a solid ry 1, Salection of the sample for analysis The sample far analysis shall be obtained by cutting, fram the sample oroduct or preliminary sample. 3 place of size ard shape suitable for the method of analysis. Samples shall be cut by sawing, abrasive cutthg, shearing or punching, In the absence of any ingication in the product stan- dard, analysis by a physical methed shall be carred ‘out on that part of the sample corresponding to transverse section of the product, provided that the matarial has sufficient thiccness.WO MOR TSE! 44.42. Surface preparation of the sample for analysis The sample for analysis shall be presared to expose 4 surfece suitable for the method of analysis. Preo- atation of a surtace for analysis shall not be carried out on any part of a sample that has been affected by he heat of a cutting torch. The equipment used for sample preparation shall be designed to minmize overheating the sample and, where appropriate, shall incomorate systems of cooling Four mein types of equiprrent used for surface prea: aration may be distinguished, a} A milling machine capable of removing a pre- selected depth of matal in 2 reproducible manner, ‘or use with samples that are within a hardness range sultable for miling. The equipment sould bo able to be used, if required, with a sampio taken from a melt where the sample is still hot, b) A grinding machine with a fixed, rotating of oscil lating head capable of removing @ preselected depth of metal in a eptoducible manner. ©) A flat-bed linishing machire with abras¥ve grinding discs, of a machine with continuous abresive- bolts, able to be used to prepere the eurface of the sample for analysis to varying grades of finish, 4} A machine tor blasting with sand, grt, or metal shot, able to be used in special applications 10 clean the surface of the sample for analysis er the ‘est portien. Arter preparation, the surtace of the sample for anelysis shell be flat and ire from defects which alfect the cortactnass of analysis. Cutting and surface preparation can be performed ether manually of automatically. In the casa of samples taken ftom melts, commercially avaiable systems, which perform each stage_af preparation automatically, may be used. Systems for the auto- rratic preparerion of surfaces of dualthickness probe semiples {see A.2.8 ¢} in annex Al, and for the punch ing of slugs forming test pottions, may incorporste fatiliies for the sand-blastng of the sample and for heat treatment to soften the sample befcre punching. The abrasive substances used ia the final stage of preparing the sample for aralysie shal be salected so as to avoid contaminating the surface with elements that are to be determined by the analysis method. The iit size of the abrasive shall be In accordance with the grade of surface finish raquirad for the anclysis, method. {mn the cese of optical errission spectrometric methods, an abrasive with @ giade of 60 git to 120 grit is nor mally sutabie. In the caee of ¥-tay fluorascarce spec- ‘trometric methods, it is essentia to ensure shat the Copright bythe Intentional trganiztion For Standardization Sal don 04 1495:32 2005 Sot method selected for surface proparation praduces a ofade of surtace finsh that is reproducible from sample to sample. In addition, there should be no smearing of the surface. The effect of abrasive materials depends on the ano- I\ticel method. ‘When using optical emission spectra metne methods, the action of oresparking wil. nar- rally clean the Surface of the sample for analysis by volatiizing any grinding contaminants. However, par ticular caro is soquired to avoid surface contamination when using a neve abrasive disc. When using X-ay fluorescence spectioetric methods, all the phases of surtace preparation shall bo cxam ined for potential surface contaminate effscts, The sample for anelysis shall ke examined visually otter preperation to establish that the suriace is free from particulate matter and that thare are no defects; ‘the sample shat, be lesutfeced 01 discarded If defects are procent. The sample for analysis shall be dry and care shall be teken to protect the prepared surface from contamination 4.4.5 Preparation of a sample for analysis by remelting A sample in the forn of small pieces or chins, or 2 part of the sample product itself, can be remeltad in an atmosphere of argon using commeicialy available Traiting equipment. The sample is converted into a ise, 40 mim to S0mm in diameter and € mm thick, which is suitable for analysis by a physical method Some types of rematting equipment incorrorete facil tias for the centatugal casting of tha dis. Partial losses of some slements can be expsriencsd during the remelting process, It is essential to ensue that any selective volatilization or segregation of ef ements, or ary ether change in composition, which oceu's Is quantitatively known and does not signti- cantly influence the analysis results. Suitable seste shall be cartied out to show that any change in com- position is both smallin magnitude and reproducible ‘The ecuipment used and the method adopted for remetting shall be designed to prevent or minimize a change in composition and to ensure that any chance is reproducible, A deoxidant, for examole 0,1. % ba/m) Zitconium, should be used during remelting. The method ussct for caliaration of the analytical measure- ment ahall toke account of any charge that does occur, Not ll ferrous metals cen be remalted in this manner. ‘This method shall not be used for sample preparation for the determiration of an element which is subject to a significant and nor-reproducible change in com. position, when remated.me TON 45. Sofety precautions 45.1 Pessonal protection Personal protective equipment shall be provided to minimize the risk of injury during sampling and sampls preparation methods. Provisions shall in- clothing, hand protection and mnt to splashes, for usa during the sampling of liquld metal. Provisions shall also include protective clothing, hand, eye and hearing protection, for use during the sampling and sampfe preparetion of solid matal; and respiratory Protection for use where necessary. 452 Mal ny The use of machinery for sampling snd sample preparation shall be in aecordence with eppro- priete national standards. Grinding operations used for surface preparation may be covered by national legislation. 453 Hazardous substances Reference shall be made to appro} regulations with regard to the use of solvents for the cleaning end drying of samples and test portions, 5. Liquid iron for steelmaking and pig-Iron production 5.1 General ‘The fotowing methods are applicable to the sampling of liquid blasturnace ion inended for steelmaking, and commonly dascribad as hot metal, o: for the casiing of piciten, The liquid iran is normally samaed, from the blast furnace runner wrile the melt is poured inte torpedo lacles, or trom transfer vessels, ar durng, secondary treatment processes in the ladle, or during, ‘the casting of the rrett into rig-iran. ‘The chemical composition of irar may fluctuate during run-out from the blast furnacs. Two or more sampes, should be taken frorn the melt at Umed intervals end an average analysis detcrmined. When physical methods are used for analysis, the method of sampling should be designed to chill the que motal in a manner which ensures that the metal luigea. structure of the sample is suitable for the re quirements of the analysis method selected. Conmrght by the Internstionl Grganization For Stendortization SalJau WF 352 200s ISO 14284:1996(E) 5.2 Spoon sampling For sampling trom a melt, immerse a preheated steel spoon into the melt and fil with liguic iron, Withdraw the spoon and remove eny slag by skimming the sur- face of the liquid iron in tha spoon. For sampling from a streurn, intraduce a preheated: steel aneen into the streem from the ladle and Till it with Tiqurd on Pour the liquid iron from the spoon without delay into 2 metal mould t0 chill the iren 2s rapidly as passibie, Remove the sample from the mould ard reek off any fiser. It's essential thet the lquid iron should be poured into. a mould that is cold tc ensure adequate chilling; It necessary, the mould should be air-cocled before use, The mould shall be free from moisture. A dise-shaped semple, commonly cescribed 48 a cain sample, can be obtained using « two-piece steel mould; the sample in typically 38 mm to 40 mm in de ameter with @ thickness varing from 8mm to 12 mm The mould s constructed in two pieces which are clamped togethor while 'n use: one piece is a flat chill pleta, the athar is a block with the mould cavity. The eege of the mouia cavity may be tanered, for example, fram 38 mm to 32 mr, te “acilitate removal of the sample from the mould, & coin sample is verti cally orhorizontally cast in the mould. A coin sample with one or more attached pins can be ‘obtéined using @ combination-type moud. The pins ore broken off from the disc and used, if required, a8 test portions for analysis by a thermal ~rethod, ‘A combinationtype mould for use with fiquid iran intended for the production of cast iron is syown in figure 2.) A thin slab-shaped sample with 4 roundad and can oe obtzined using a cast iron ar steel split-moule: the di- mensiens of the sample ars typically 70 mmm x 35 mm, with a thickness of 4mm. The two halves of the mould are aeveliad at the top to give a feoder head and are clamped logsther white use. This type of mould may be preferred ‘or use with liquid an von taining high percentages of carbon. 5.2.2 Maintenance of equipment It is essentiel to keep samaling spoons and metal ‘moulds clean and dry. After use, remove any seg and skull and clean the surfaces of the roule with 8 wire brush, Moulds should be remachined if the intemal surfaces become worn. This aveids the need for additional ma- hiring of the sample curing surface praperation,ISO 14284:1996(E) 5.3 Probe sampling 53.1 General The different types of probes used for sampling blast, fumace iron are described in annex A. Probes shoutd be cesigned to provide a dise-shaped sample with white iten st-ucture which is suffigiently deep for the Fequremens of the physical methad selected for analysis. Probe sampling is influenced by such faciors as the angle and depth of iinmersion of the sampter in the elt, ard immersion times can vary depending on the ternperaturs of the fquld iron, These factors shoud be deteimired for the particular ironmeking practice and thereafter strictly controlled to maintain the standard of quality of the sample for analysis. 53.2 Mathads For sampling from a melt, immerse a suitable immer sion probe sampler into the melt at an angle as near 8 possiole To the vertical plane. When samaling from the runner of a blast fumace, select the position of immersion to give a sufficient depth of ligud metal for the use of 4 probe sarrpler. A-depth of approximately 200 min is adequate for most types of sampling prose. For sarnpling from a stream of liquid iron, introduce a Suitable suction proke sampler into the metal flow from a ladle, at an anglo of approximately 45° to tho vertical plane, at a position as near as possible to the nozzle of the vessel. Withdraw the probe sempler from the melt after a predetermined interval of time, break it apart and allow the sample to cool in air 5.4. Preparation of a sample for analysis 34.1. Preliminary preparation Remove any surface oxidation from a sample taken trom the melt, that may contaminate the sample ‘or analysis during subsequent preparation. 5.42 Sample for analysis by a chemical method Bieak the sample into small plecas and crush pieces using @ percussion moriar or a vibratcry grinding mill to obtain a sutficient mass of sample for anelysis of particle size preferably less than adout 150 ym. Atematively, cbtein chips by dling the sample at a low speed as cescribad in 83.1 Copmright bythe International Crgnization For Stondarization SalJau U4 1133 2005 eso 5.44.3. Sample for analysis by a thermal method Break the pin of a disc-shaped sample into pieves of 3 suitable mass for use as test porions, or use the lugs, ol 8 probe sample. Analyse a representa‘ive number cof test portions to abtain an avorago valuo. Alternatively, crush the pin or lugs in @ percussion mortar to obtain a sufficient mass of sample for analysie of particle size approximately 11mm to 2 rom. Avoid the production of fine material during crushing. Inthe case of a slab-shapad sample, break the sarple into small pieces and ctush the pieces in a senilar mrenmer, 5.4.4 Sample for analysis by a physical method Inthe case of a disesheped sample, remove any lugs or pins, as necessary, and then grind the surface of ‘he sample to expos? 4 white lion structure whichis representative of the sample. The amount of material ‘to be removed in this way shall be devermined for the chemical composition of the particular iron and the condtions of sampling; the thickness of the layat to be removed norrrally lies batween 0.6 mm and 1mm, (se AG. In the case of a slab-shapad sample, break the stb into two pieces to obtain a samiply of suitable size tor analysis, Prepare the surface of the sample by grinding and li ishing, Grinding shall be cartied out wet to avoic over- heating the semple Sut the final surface presaration shall be dry linishing. Alternatively, cool the sample after grinding by immersion in water and then firist by dry linishing, Particular oarc is roquired when preparing the surface of thin samples. A chuck shall be specially designed to hold the sample securely grinding and linishing oper- ations. & Liquid iron for cast iron production 6.1 General The follewing methods are applicable to the sampling cf liquid iron from cupola furnaces and electric fur neces, frorn holding furnaces in duplex procasses, and from ladies and treatment voseels. Liquid iron intended for the production of iran castings may be subject to inhomogeneity, and particular cars is recuired in the doagn of strategies and methods of sampling to meet the requirements of the particular procuction provass. For exemple, liquid iron in hoiding furaces tends to stratify and sampling should ensurd that the analysis is “epresentatie of the melt as a whole,|r batch processes, two or mere samples should ba taken from melting fumaces, preferably when ap- proximately one-thrd and two-thirds of the melt has been discharged, and an average analysis determined, In continuous srocasses, samples ehould be taken at regular intervals of time. Metheds of sampling are normally designed 10 chill the fiouid rretsl of a samplo cast from a spoon as rapidly as possitle :o produce a metallurgical structure ‘of white iton that is free from graphite. A white iron structure obralted by cnil-easting is generally required For analysis by physical metnods, Non-chilled samples may also be used, In this case, sainples can be specially cast from a spoon, or @ somple for analysis cen be selected from a tast bar oF 00 26 5ISO 14664) FOE) 822 Methods During unloading or losdirg operations, or any cther displacement of a consigumen, cbtain pigs. 28 ine srerrental samples at intarvals of time or mace that ate epproximately eaust In the case of a consignment suppied ‘n wagons or trucks, the points of sempling shall be disposed in 8 dafirita order. For example, from five positons, that is at tha centre of the wagon, and at one-sixth of tha dis tance from the comers of the wagons along the two diagonals. in the case of a stockpile, thiow a rope having a cer- xein number of knots anto tha pile and texe the pigs touched by these knots. Repast the operation until a sufficient number of pigs is obtained. Where itis not possible to gain access to the whole of the surface of the stockpile, or where access to the stockpila is unsata, the points of sampling shall bo disposed in a definite orcer cn ite surlacs of the stockpile. Altemotively, use @ mechanical shovel io obtain» rumbar of sussamples from postions in the stockpile selected vt rendom. Then select one pig at random 4rom each subsample 82.3 Consignment of mixed pig-frans A consignment of pia-ron may contain a number of different batchas of pig-iron which mey be from dif- ferent sources. If pigs of dlfterent shapes end sizes can be distinguished in the consign nen, a visual es- sessment should be made of the proportions of each, type of pigiron presen Incremental samples shall :hen be taken of each type af pasion in the consignment to constitute separate subsamples of pigs in order to cbtein 2 weighted average analysis for tha consignment, &3 Preparation of a sample for analysis. 83.1. General tha pigs taken as incremental samples contain rem anent magnetism a5 a result of hending wth snag natic grabs, they should ke derragnotzod by moans of @ demagnetizing coll to prevent separation of coarse and fine particles during diilirg. Machining of the sample to obtain chips should be carricd out by deling at 2 low sosed (100 r/min to 130 /min) using a freshly sharpenad tool, adjusting the speed and feed to produce chips of uniform size witha minimum amount oF fine partcles. A dill with a damater of 12 mm to 14mm is surable for obtaining, 16 Copright bythe International trganiztion Por Standardization Sal fou 04 143 50 2008 “ae chips. The dill shall be resharsened at frequent intervals and care taken to avoid overheating beth the sample and the tool, For some types of iron, for example oxygerblown iran, it may be necessary to use a tungstan-carbice- tipped cil. Chips should be as solid end compact #8 possible in order to prevent crumbling and loss ef giaphite, The particle size rang o° chips intended for the determi- nation of carbon should be approxivrately 1 mm to 2mm. Milling shall not be employee owng to the high pro- pottion of fines produced, ‘The prepared sample shell not be washed with a sok vent or treated magnetically because of the risk of atering the diotribution of motal and grephite. 83.2. Sample for analysis by a chemical method The method of preparation of each of the incremental samolas shall be in accordanca with one of tha follow ing methods, al For machinable iron, clean one face of the pig ay grinding at a position mrievey afong the leneth and width to expose an area of metallic surface ot at least 60 mm in diaater, Drill a hole through the crose-soction of sho pigi coase driling at 5 point apprcximatey S mm from the opposite face. F necessary, drill another hole paral! to the first hole. [See figuies 3a}, 3b), Sc} and 3d).] bt For non-machinsble iron, raak the pig at @ pes- ition midway along its length. Break off zieces from the frectured face. crush these pieces to a Particle size of approximately 8mm and then grind using a vibratory grincing mili t2 9 particle siza of lees than 180 im Mix equal quantities cf the material obtained from gach pig. From inis mikture, obtain a sample of suf ficient mass for analysis ky coning aad quartering. Altemativaly, analyse the material ootained from each ig separately te obtain an avarage value for the cove signment 8.3.3. Sample for analysis by a thermal method 83.3.1 General ‘The method of preparation for each of the incremantat samples should be in accordanca with either 83.3.2 oF 83.2.3, depesding upon the condition of the pigs and the type of sample required for analysis,