1、BRITISH STANDARD BS EN 14361:2004 Aluminium and aluminium alloys Chemical analysis Sampling from metal melts The European Standard EN 14361:2004 has the status of a British Standard ICS 77.040.30; 77.120.10 BS EN 14361:2004 This British Standard was published under the authority of the Standards Pol
2、icy and Strategy Committee on 8 December 2004 BSI 8 December 2004 ISBN 0 580 44965 3 National foreword This British Standard is the official English language version of EN 14361:2004. The UK participation in its preparation was entrusted to Technical Committee NFE/35, Light metals and their alloys,
3、which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the s
4、ection entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application
5、. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor
6、related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 10, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when th
7、e document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN14361 November2004 ICS77.040.30;77.120.10 Englishversion AluminiumandaluminiumalloysChemicalanalysisSampling frommetalmelts AluminiumetalliagesdaluminiumAnalysechimi
8、que Echantillonnagedumtalfondu AluminiumundAluminiumlegierungenChemische AnalyseProbenahmevonMetallschmelzen ThisEuropeanStandardwasapprovedbyCENon14October2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanatio
9、nalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation underther
10、esponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg
11、,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansrese
12、rved worldwideforCENnationalMembers. Ref.No.EN14361:2004:E:16341 NE4002 (E) 2 Contents page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Sampling from a melt 5 4.1 General5 4.2 Sampling procedure 5 4.3 Form and size of the sampling mould and of the sample
13、 taken from liquid metal.5 4.4 Sampling plan 6 4.5 Preparation of sampling from metal melts6 4.6 Requirements for a sound melt sample 6 4.7 Check of the sampling mould and the sampling ladle.6 Annex A (informative) Example for sampling from metal melts7 A.1 Principle7 A.2 Equipment 7 A.3 Procedure .
14、8 A.3.1 General8 A.3.2 Preparation of the sampling ladle8 A.3.3 Preparation of the sampling mould .8 A.3.4 Sampling.8 Bibliography 10 EN14361:2004:16341 NE4002 (E) 3 Foreword This document (EN 14361:2004) has been prepared by Technical Committee CEN/TC 132 “Aluminium and alumin- ium alloys”, the sec
15、retariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by May 2005, and conflicting national standards shall be withdrawn at the latest by May 2005. Within its programme
16、of work, Technical Committee CEN/TC 132 requested CEN/TC 132/WG 17 “Chemical analy- sis“ to prepare the following document: EN 14361, Aluminium and aluminium alloys Chemical analysis Sampling from metal melts According to the CEN/CENELEC Internal Regulations, the national standards organizations of
17、the following coun- tries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Esto- nia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia,
18、Spain, Sweden, Switzerland and United Kingdom. EN14361:2004:16341 NE4002 (E) 4 Introduction Melts of aluminium alloys are susceptible to segregation when solidifying. Cast products, therefore, have concentration gradients. Axial and radial segregation profiles affect the representative sampling from
19、 melts, cast products or laboratory samples. In the case of direct measurement of solid samples (e.g. spark optical emission spectrometric analysis S-OES, or X-ray fluorescence spectral analysis XRF) measuring signals are influenced by the morphology of solidification and cast structure of the sampl
20、e. This document provides requirements which demonstrate the correspondence between the average chemical com- position of the cast to be tested and the average chemical composition of the test portion. EN14361:2004:16341 NE4002 (E) 5 1 Scope This document specifies criteria for sampling and gives gu
21、idance on the sampling from melts in order to verify if the chemical composition of the product fabricated from a metal melt is in conformance with the specification. NOTE For sampling from product or laboratory samples see EN 14242 or prEN 14726. 2 Normative references The following referenced docu
22、ments are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12258-1:1998, Aluminium and aluminium alloys Terms and definitions Part 1:
23、General terms. EN 12258-2:2004, Aluminium and aluminium alloys Terms and definitions Part 2: Chemical analysis. prEN 14726, Aluminium and aluminium alloys Chemical analysis Guideline for spark optical emission spec- trometric analysis. 3 Terms and definitions For the purposes of this document, the t
24、erms and definitions given in EN 12258-1:1998 and EN 12258-2:2004 ap- ply. 4 Sampling from a melt 4.1 General The form and the size of a sample, the sampling plan, the preparation of the sampling tools and the metallurgical criteria for a useful sample widely depend on local conditions, so this docu
25、ment can only give certain required criteria. 4.2 Sampling procedure As a part of the quality management system, the supplier of the metal (manufacturer) shall lay down and maintain a sampling procedure which shall be in conformance with the requirements of this document and shall reflect the specia
26、l aspects of the casting line, the alloys to be cast and the equipment of the analytical laboratory. Any sample of liquid metal shall be taken in conformance with this procedure. An example for sampling from metal melts is given in Annex A. 4.3 Form and size of the sampling mould and of the sample t
27、aken from liquid metal The form of the sample shall ensure, after sample preparation, a correct analysis. If S-OES is used, the sample shall allow as many sparks as required according to preliminary tests and prEN 14726, to guarantee the compliances with specifications. The sample form shall allow a
28、 portion of drillings, millings or small pieces to be taken that are known, by pre-testing to be representative of the average composition of the whole sample (e.g. a longitudinal segment) for wet chemical analysis. EN14361:2004:16341 NE4002 (E) 6 4.4 Sampling plan A sampling plan shall specify: sam
29、ple volume (defined by the sampling ladle and the sampling mould form); number of samples to be taken; locations in the liquid metal container (e.g. furnace, crucible or launder), in the cast product where the samples shall be taken; timings in the melt holding or casting process when the samples sh
30、ould be taken. The supplier of the metal shall verify with preliminary tests, that the metal at the sampling location is sufficiently mixed so that the average chemical composition of the sample is representative of the average chemical composition of the whole melt. If the sample is taken from the
31、launder and any evidence exists that there might be variations in the chemical composition of the liquid metal at particular phases of the cast, e.g. the beginning or the end of the cast, then the samples shall be taken at such phases. 4.5 Preparation of sampling from metal melts Before each samplin
32、g, the tools shall be prepared in such a way that the liquid metal does not come into contact with solidified aluminium, dross, moisture, iron or dust. During the transfer from the melt to the sampling mould, the sampled liquid metal shall only come in contact with suitable and appropriate materials
33、 which are proven not to react with the metal and thus change the chemical composition of the sample. NOTE Any metal sticking on the walls of the tools after solidification indicates the possibility of a chemical reaction. The filling of the sampling mould shall be done as quickly as possible and do
34、ne at an even rate. The sampling mould shall be filled in one single operation without interruption. With one drawing process only one sample shall be poured. 4.6 Requirements for a sound melt sample After solidification the samples shall be complete. Samples shall be free from cracks, cold shuts, s
35、urface irregularities, inclusions and shrinkage holes. Special care shall be taken to make sure that segregation is minimized and reproducible. The supplier of the metal shall demonstrate, e.g. by a series of tests, that, with regard to the subsequent sample preparation and analytical procedure, the
36、 segregation is under control. 4.7 Check of the sampling mould and the sampling ladle The sampling mould shall be periodically checked and repaired, if necessary. Residues in the sampling mould shall be removed. Attention shall be paid that the specified dimensions of the sampling mould are not bein
37、g changed during repair. The sampling ladle shall be periodically checked, recoated and repaired, if necessary. Checks and repairs shall be recorded. EN14361:2004:16341 NE4002 (E) 7 Annex A (informative) Example for sampling from metal melts A.1 Principle With a sampling ladle, a representative port
38、ion of molten metal is taken and poured into the sampling mould. The laboratory sample is allowed to solidify, removed from the sampling mould, quenched, if required, and identified. The sampling conditions obtained by pre-tests, which influence the reproducibility of the segregation and cast struct
39、ure, are recorded (see prEN 14726). The materials and the shape of the sampling mould, the sampling conditions and the sampling plan are investigated by preliminary tests with respect to reproducible segregation behaviour and cast structures as well as range and uncertainty of the chemical compositi
40、on. The ranges of application and the accuracy of the method or any alternative step should be validated by the testing laboratory or other approved laboratory. In order to conform to the procedures for sampling and identification of laboratory samples, the responsibilities and control measures shou
41、ld be documented. Further instructions about sampling conditions, especially the number of laboratory samples per cast and shape of sampling moulds depend on the production and measuring equipment, the requirements for the accuracy of the chemical composition or the process capability. NOTE Taking a
42、 representative laboratory sample for analysis requires well-trained personnel and proper pre-treatment of the sampling tools. Safety instructions are recommended. A.2 Equipment A.2.1 Sampling ladle, long enough to reach into the furnace, trough, launder or crucible. The spoon size should be large e
43、nough to cast one sample but no more than one sample per sampling. A.2.2 Devices, auxiliary materials and documented procedures for cleaning and coating according to experience or preliminary tests. NOTE There are different ways for cleaning and protection of sampling ladles and sampling moulds. The
44、 selection of equipment (e.g. the sampling ladle steel or graphite or protective coating) depends on the purity of the aluminium or on the composition of the aluminium alloys to be analysed. A.2.3 Sampling mould (e.g. for cylindrical, plate-type or mushroom sample shape). NOTE The material, the shap
45、e of the sampling mould and the sampling conditions should be investigated by preliminary tests with respect to reproducible segregation behaviour and cast structures. Therefore, the distance from the analytical face and from the edge of the laboratory sample at which the analysis is to be performed
46、 should be determined for each laboratory sample shape and for each alloy type (criteria see prEN 14726). The shape of sample, the form and material of the sampling mould should allow a rapid solidification free of shrinkage cavities or porosity. EN14361:2004:16341 NE4002 (E) 8 A.3 Procedure A.3.1 G
47、eneral The procedure should be as follows: A.3.2 Preparation of the sampling ladle A.3.2.1 Clean the area of the sampling ladle which is contaminated with metal. Remove any adherent metal from the sampling ladle. NOTE Metal or oxide residues can contaminate the sample to be taken (inclusions). A.3.2
48、.2 If necessary, coat the sampling ladle (A.2.2). The coated sampling ladle should be free from any mois- ture (risk of explosion). NOTE After preparation, the sampling ladle is ready for immediate and repeated use. A.3.2.3 The sampling ladles should be checked at regular intervals for its perfect condition. A.3.3 Preparation of the sampling mould A.3.3.1 Clean and dry the sampling mould. Check the good functioning of the mobile parts, if any. A.3.3.2 The sampling mould should be checked at regular intervals for their perfect condition. A.3.3.3 If the
