BS EN 24883-1993 Specification for hardmetals - Determination of contents of metallic elements by X-ray fluorescence - Solution method《硬质合金规范 用X射线荧光分析法对金属元素含量的测定 溶液法》.pdf

1、BRITISH STANDARD BS EN 24883:1993 ISO 4883:1978 Specification for Hardmetals Determination of contents of metallic elements by X-ray fluorescence Solution method The European Standard EN24883:1993 has the status of a British Standard UDC 669.018.25:620.1:543.422.8:546.3.047BSEN24883:1993 This Britis

2、h Standard, having been prepared under the directionof the Iron and Steel Standards Policy Committee, waspublished under the authorityof the Standards Boardand comes into effect on 15June1993 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference ISM/65 Spe

3、cial announcement BSI News January 1993 ISBN 0 580 21927 5 Cooperating organizations The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations of the following countries: Austria Oesterreichisches Nor

4、mungsinstitut Belgium Institut belge de normalisation Denmark Dansk Standardiseringsraad Finland Suomen Standardisoimisliito, r.y. France Association franaise de normalisation Germany Deutsches Institut fr Normung e.V. Greece Hellenic Organization for Standardization Iceland Technological Institute

5、of Iceland Ireland National Standards Authority of Ireland Italy Ente Nazionale Italiano di Unificazione Luxembourg Inspection du Travail et des Mines Netherlands Nederlands Normalisatie-instituut Norway Norges Standardiseringsforbund Portugal Instituto Portugus da Qualidade Spain Asociacin Espaola

6、de Normalizacin y Certificacin Sweden Standardiseringskommissionen i Sverige Switzerland Association suisse de normalisation UnitedKingdom British Standards Institution Amendments issued since publication Amd. No. Date CommentsBSEN24883:1993 BSI 12-1999 i Contents Page Cooperating organizations Insi

7、de front cover National foreword ii Foreword 2 1 Scope 3 2 Field of application 3 3 Principle 3 4 Interfering elements 3 5 Reagents 3 6 Apparatus 3 7 Sampling 3 8 Procedure 3 9 X-ray fluorescence analysis 3 10 Preparation of calibration curves 4 11 Expression of results 4 12 Test report 4 National a

8、nnex NA (informative) Committees responsible Inside back cover Table 1 3 Table 2 3 Table 3 4 Table 4 4BSEN24883:1993 ii BSI 12-1999 National foreword This British Standard has been prepared under the direction of the Iron and SteelStandards Policy Committee and is the English language version of EN2

9、4883:1993 Hardmetals Determination of contents of metallic elements byX-ray fluorescence Solution method, published by the European Committee for Standardization (CEN). It is identical with ISO4883:1978, prepared by Technical Committee 119 “Powder metallurgy”, of the International Organization for S

10、tandardization (ISO) with the active participation of the UK. This British Standard supersedes BS5600-4.10:1980, which is withdrawn. This edition makes no technical changes to the standard. A British Standard does not purport to include all the necessary provisions of a contract. Users of British St

11、andards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theEN title page, pages2 to 4, an inside back cover and

12、a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 24883 April 1993 UDC 669.018.25:620.1:543.422.8:546.3.047 Descripto

13、rs: Powder metallurgy, hard metals, chemical analysis, determination of content, metals, spectrophotometric analysis, X-ray fluorescence spectrometry English version Hardmetals Determination of contents of metallic elements by X-ray fluorescence Solution method (ISO 4883:1978) Mtaux-durs Dosage des

14、lments mtalliques par fluorescence de rayons X- Mthode par solution (ISO 4883:1978) Hartmetalle Bestimmung des Gehaltes metallischer Elemente durch Rntgenfluoreszenz Lsungsverfahren (ISO4883:1978) This European Standard was approved by CEN on1993-04-02. CEN members are bound to comply with the CEN/C

15、ENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to an

16、y CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. C

17、EN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Eur

18、opisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1993 Copyright reserved to CEN members Ref. No. EN 24883:1993 EEN24883:1993 BSI 12-1999 2 Foreword In 1992, ISO4883:1978 Hardmetals Determination of contents of metallic elements by X-ray fluorescence Solution metho

19、d was submitted to the CEN Primary Questionnaire procedure. Following the positive result of the CEN/CS Proposal ISO4883:1978 was submitted to the Formal Vote. The result of the Formal Vote was positive. This European Standard shall be given the status of a national standard, either by publication o

20、f an identical text or by endorsement, at the latest by October1993, and conflicting national standards shall be withdrawn at the latest by October1993. According to the Internal Regulations of CEN/CENELEC, the following countries are bound to implement this European Standard: Austria, Belgium, Denm

21、ark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom.EN24883:1993 BSI 12-1999 3 1 Scope This International Standard specifies an X-ray fluorescence solution method for the determination of cobalt, iron

22、, manganese, molybdenum, nickel, niobium, tantalum, titanium, tungsten, vanadium and zirconium contents of carbides and hardmetals. 2 Field of application The method is applicable to carbides of niobium, tantalum, titanium, vanadium, tungsten and zirconium, mixtures of these carbides and binder meta

23、ls, all grades of presintered or sintered hardmetals, produced from these carbides, with the minimum element contents shown in Table 1. Table 1 3 Principle Measurement of the intensity of the characteristic X-ray spectrum of the elements being determined. To eliminate the effects of particle size an

24、d inter-element effects, the test portion is dissolved in a mixture of hydrofluoric and nitric acids. 4 Interfering elements The effect of interfering elements, such as line interference of titanium and tungsten on vanadium, shall be taken into account. 5 Reagents During the analysis, use only reage

25、nts of recognized analytical grade, and only distilled water or water of equivalent purity. 5.1 Hydrofluoric acid, 1,12g/ml. 5.2 Nitric acid, 1,42g/ml. 5.3 Solvent solution Mix 2 parts of the hydrofluoric acid (5.1), 1 part of the nitric acid (5.2) and 2 parts of distilled water. 5.4 Tartaric acid s

26、olution, 200g/l. 6 Apparatus Ordinary laboratory apparatus and 6.1 X-ray spectrometer, suitable for solution analysis. 6.2 Sample cells, resistant to hydrofluoric-nitric acid mixture, with a window consisting of64m thick film of polyethylene terephthalic acid ester. 7 Sampling 7.1 The sample shall b

27、e crushed in a mortar made of a material which does not alter the sample composition. The crushed material shall pass a2mm sieve. 7.2 The analysis shall be carried out on two or three test portions. 8 Procedure 8.1 Weigh2 0,001g of the test sample into a150ml polypropylene beaker. NOTEIf the sample

28、includes lubricant, a correction for the lubricant content must be applied. 8.2 Add 20ml of the solvent solution (5.3). Dissolve the test portion completely by heating on a water bath for30min. 8.3 Cool and transfer the solution into a50ml polypropylene volumetric flask containing10ml of the tartari

29、c acid solution (5.4). Make up to volume with water and mix. 8.4 Filter the solution through a dry filter paper into a polypropylene beaker. 8.5 Fill the cell (6.2) to a height of at least10mm with the solution. 8.6 Analyse with the X-ray spectrometer. 9 X-ray fluorescence analysis 9.1 All measuring

30、 parameters, including the target material of the X-ray tube, shall be chosen to obtain the optimal number of impulses. 9.2 The analytical lines shown inTable 2 shall be used. Table 2 Element Minimum content % (m/m) Co Fe Mn Mo Nb Ni Ta Ti V W Zr 0,05 0,05 0,05 0,05 0,07 0,05 0,10 0,2 0,05 0,10 0,05

31、 Element Co, Fe, Mn, Mo, Nb, Ni, Ti, V, Zr Ta, W Analytical line K 1,2 L 1EN24883:1993 4 BSI 12-1999 9.3 Background corrections shall be made when necessary. 10 Preparation of calibration curves 10.1 The calibration shall be performed with at least five calibration samples prepared according to clau

32、se8 from mixtures of accurately known amounts of pure metals or their suitable compounds. It is essential to construct separate calibration curves for different types of hardmetals. A calibration sample of approximately the same composition as the sample to be analysed shall be used as an external s

33、tandard. A calibration curve shall be drawn for each element by plotting its concentration versus the ratio of the count rate of each calibration sample to that of the external standard. 10.2 Elements in the test sample shall be determined by calculating the ratio of the count rates in the test samp

34、le to the external standard, and taking the concentration from the appropriate calibration curve. 11 Expression of results 11.1 Tolerances The deviations between two or three independent determinations shall not exceed the values shown inTable 3. Table 3 11.2 Final result Report the arithmetical mea

35、n of acceptable determinations rounded to the nearest value as shown inTable 4. Table 4 12 Test report The test report shall include the following information: a) reference to this International Standard; b) all details necessary for identification of the test sample; c) the result obtained; d) all

36、operations not specified by this International Standard, or regarded as optional; e) details of any occurrence which may have affected the result. Content Range for two determinations Range for three determinations % % % from0,05 to0,4 0,04 0,05 over0,4 to2 0,20 0,25 over2 to 10 0,30 0,35 over 10 to

37、 30 0,4 0,5 over 30 to 95 1,0 1,2 Content Round to the nearest % % from0,05 to0,4 0,01 over0,4to 30 0,1 over 30to 95 1BSEN24883:1993 BSI 12-1999 National annex NA (informative) Committees responsible The UnitedKingdom participation in the preparation of this European Standard was entrusted by the Ir

38、on and Steel Standards Policy Committee (ISM/-) to Technical Committee ISM/65 upon which the following bodies were represented: British Hardmetal Association Federation of British Engineers (Test Manufacturers) Society of Motor Manufacturers and Traders Limited Coopted membersBS EN 24883:1993 ISO488

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