BS EN 27627-5-1993 Hardmetals - Chemical analysis by flame atomic absorption spectrometry - Determination of cobalt iron manganese molybdenum nickel titanium and vanadium in conten.pdf

1、BRITISH STANDARD BS EN 27627-5:1993 ISO 7627-5: 1985 Hardmetals Chemicalanalysis by flame atomic absorption spectrometry Part 5: Determination of cobalt, iron, manganese, molybdenum, nickel, titanium and vanadium in contents from0.5 to2%(m/m) The European Standard EN27627-5:1993 has the status of a

2、British Standard UDC 669.018.25:620.1:543.422BSEN27627-5:1993 This British Standard, having been prepared under the directionof the Iron and SteelStandards Policy Committee, was published underthe authority of the Standards Board and comes intoeffect on 15 June1993 BSI 12-1999 The following BSI refe

3、rences relate to the work on this standard: Committee reference ISM/65 Special announcement in BSINews January 1993 ISBN 0 580 21928 1 Cooperating organizations The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national stand

4、ards organizations of the following countries: Austria Oesterreichisches Normungsinstitut 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. Greec

5、e Hellenic Organization for Standardization Iceland Technological Institute 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 Standardiseri

6、ngsforbund Portugal Instituto Portugus da Qualidade Spain Asociacin Espaola de Normalizacin y Certificacin Sweden Standardiseringskommissionen i Sverige Switzerland Association suisse de normalisation UnitedKingdom British Standards Institution Amendments issued since publication Amd. No. Date Comme

7、ntsBSEN27627-5:1993 BSI 12-1999 i Contents Page Cooperating organizations Inside front cover National foreword ii Foreword 2 1 Scope and field of application 3 2 Reference 3 3 Reagents 3 4 Procedure 3 5 Expression of results 4 Annex ZA (normative) Normative references to international publicationswi

8、ththeir relevant European publications 5 National annex NA (informative) Committees responsible Inside back cover National annex NB (informative) Cross-reference Inside back cover Table 1 Instrumental parameters and characteristics of calibration functions 3 Table 2 Rounding of results 4BSEN27627-5:

9、1993 ii BSI 12-1999 National foreword This British Standard has been prepared under the direction of the Iron and Steel Standards Policy Committee and is the English language version of EN27627-5:1993 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part5: Determination of cobalt

10、, iron, manganese, molybdenum, nickel, titanium and vanadium in contents from0,5 to2% (m/m), published by the European Committee for Standardization (CEN). It is identical withISO7627-5:1983, prepared by Technical Committee119, Powder metallurgy, of the International Organization for Standardization

11、 (ISO) with theactive participation of the UK. This British Standard supersedesBS5600-4.17.5:1986, which is withdrawn and from which it differs by the addition ofAnnex ZA. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are respon

12、sible 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, pages 2 to 6, an inside back cover and a back cover. Thi

13、s 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 EN27627-5 April 1993 UDC 669.018.25:620.1:543.422 Descriptors: Powder metallurgy, hard

14、metals, chemical analysis, determination of content, transition metals, cobalt, iron, manganese, molybdenum, nickel, titanium, vanadium, spectrometric analysis, atomic absorption spectrophotometry English version Hardmetals Chemical analysis by flame atomic absorption spectrometry Part5: Determinati

15、on of cobalt,iron, manganese, molybdenum, nickel, titanium andvanadium in contents from0,5 to2% (m/m) (ISO 7627-5:1983) Mtaux-durs Analyse chimique par spectromtrie dabsorption atomique dans la flamme Partie5: Dosage du cobalt, du fer, dumanganse, du molybdne, du nickel, du titane et du vanadium des

16、 teneurs comprisesentre0,5 et2% (m/m) (ISO 7627-5:1983) Hartmetalle Chemische Analyse durch Flammenatomabsorptionsspektrometrie Teil5: Bestimmung des Cobalt-. Eisen-, Mangan-, Molybdn-, Nickel-, Titan- und Vanadiumgehaltes von0,5 bis2% (m/m) (ISO7627-5:1983) This European Standard was approved by CE

17、N on1993-04-02. CEN members are bound to comply with the CEN/CENELEC 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

18、be obtained on application to the Central Secretariat or to any 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 Centr

19、al Secretariat has the same status as the official versions. CEN 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 Co

20、mmittee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1993 Copyright reserved to CEN members Ref. No. EN 27627-5:1993 EEN27627-5:1993 BSI 12-1999 2 Foreword In1992,ISO7627-5:1983 Hardmetals Chemical analysis

21、 by flame atomic absorption spectrometry Part5: Determination of cobalt, iron, manganese, molybden, nickel, titanium and vanadium in contents from0,5 to2% (m/m) was submitted to the CEN Primary Questionnaire procedure. Following the positive result of the CEN/CS ProposalISO7627-5:1983 was submitted

22、to the CEN 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 of an identical text or by endorsement, at the latest by October1993, and conflicting national standards shall be withdrawn at the latest

23、 byOctober1993. According to the Internal Regulations of CEN/CENELEC, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and

24、 UnitedKingdom. NOTEThe European references to international publications are given inAnnex ZA (normative).EN27627-5:1993 BSI 12-1999 3 1 Scope and field of application This part ofISO7627 specifies the method to be used for the determination of cobalt, iron, manganese, molybdenum, nickel, titanium

25、and vanadium contents of hardmetals within the range0,5 to2% (m/m) by flame atomic absorption spectrometry. General requirements concerning the field of application, principle, interfering elements, apparatus, sampling and test report are given inISO7627-1. NOTEDetermination of element contents in h

26、igh concentration by the atomic absorption spectrophotometry method yields a wider scattering of results than are obtainable by other methods, i.e.ISO3909, ISO4501, ISO4503 and ISO4883. Seealsoclause4.2. 2 Reference ISO 7627-1, Hardmetals Chemical analysis by flame atomic absorption spectrometry Par

27、t1:General requirements. 3 Reagents 3.1 Hydrofluoric acid, 1,12g/ml. 3.2 Nitric acid, 1,42g/ml. 3.3 Ammonium fluoride,0,1 g/ml solution. 3.4 Caesium chloride,0,01 g/ml solution. 3.5 High-purity stock solutions, for calibration purposes for each element to be determined, containing1,000g of the eleme

28、nt per litre. NOTEThis value is understood to establish a maximum limit of1,0005g and a minimum limit of0,9995g. 4 Procedure 4.1 Test portion Weigh, to the nearest0,001g, approximately1g of the test sample. Transfer it to a100ml polytetrafluorethylene beaker or a beaker of other suitable material. C

29、over the beaker. 4.2 Dissolution of the test portion Add10ml of water,5ml of the hydrofluoric acid(3.1),and then5ml of the nitric acid(3.2), drop by drop, to the beaker containing the test portion(4.1) and heat gently until the test portion is completely dissolved. Add10ml of the caesium chloride so

30、lution(3.4) and10ml of the ammonium fluoride solution(3.3). Then transfer the solution totally to a100ml polypropylene one-mark volumetric flask and dilute to the mark. 4.3 Dilution volume Prepare the relevant dilution volume for the analysis according toTable 1 in the following way. 4.3.1 Dilution

31、volume100ml: use the solution in4.2. 4.3.2 The concentration of the solution may be reduced by a factor of10 for instruments of higher sensitivity by transferring10ml of the solution in4.2 to a100ml polypropylene one-mark volumetric flask. Add10ml of the caesium chloride solution(3.4). Add10ml of th

32、e ammonium fluoride solution(3.3) and dilute to the mark. 4.4 Preparation of calibration and blank solutions 4.4.1 Prepare at least six solutions according to4.2 with a matrix composition as similar as possible to the test portion to be analysed, but without making up to volume. Then add increasing

33、volumes of properly diluted stock solutions of the elements to be determined according to the concentration ranges to be covered. Make up to100ml and mix. Table 1 Instrumental parameters and characteristics of calibration functions Element Dilution volume (V) for1g test portion a Oxidant Wavelength

34、Reciprocal sensitivity, for1% absorption a Linear range a Notes ml nm 4g/ml % Co Fe Mn Mo Ni Ti V 100 1000 1000 100 1000 100 1000 N 2 O N 2 O N 2 O N 2 O N 2 O N 2 O N 2 O 352,7 248,3 279,8 313,3 232,0 364,3 318,4 20 0,3 0,1 6 0,3 30 1,0 0,1 0,03 0,01 0,06 0,05 0,2 0,1 to to to to to to to 15 2,0 2,

35、0 10,0 5,0 10 5,0 1 2 3 and 4 2 1 NOTE 1Use of the triplet. NOTE 2Use a fuel-rich flame. Adjust the burner head at right angles to the light beam or dilute the solution appropriately. NOTE 3Sensitivity is greatly dependent on matrix composition. NOTE 4Use of a narrow-spectral band pass and a single-

36、element hollow-cathode lamp is mandatory. a Guidelines for information only.EN27627-5:1993 4 BSI 12-1999 4.4.2 Also prepare calibration solutions with a diluted matrix in accordance with4.3 for dilution volumes of1000ml, if necessary. 4.4.3 Prepare one or more blank solutions (see4.4.1) without the

37、addition of the relevant element to be determined. 4.5 Adjustment of the atomic absorption spectrometer SAFETY PRECAUTION: Follow the manufacturers recommendation on igniting and extinguishing the flame. Optimize the response of the instrument at the wavelength given for the element being determined

38、. SeeTable 1. Preheat the burner for about5min and then adjust the fuel and correct the burner to obtain maximum absorption while aspirating a calibration solution. Make sure that the absorbance reading is not drifting. Aspirate water and set the initial reading to zero absorbance. 4.6 Atomic absorb

39、ance measurements 4.6.1 Aspirate first the blank solution and then the calibration and test solutions consecutively and record the readings. Aspirate water between each solution. Make at least two measurements for each solution. Solids which build up on the burner slit must be removed, otherwise the

40、y will cause a decrease of sensitivity. 4.6.2 Prepare a calibration curve by plotting the obtained absorbance values of the calibration solutions corrected for the blank against the concentration, in milligrams per litre, of the element. 4.6.3 Convert the absorbance values of the test solutions corr

41、ected for the blank to milligrams of the element per litre by means of the calibration curve. 5 Expression of results 5.1 Calculation The element content, expressed as a percentage by mass, is given by the formula where c is the concentration, in milligrams per litre, of the element in the test solu

42、tion; V is the dilution volume, in millilitres; m is the mass, in grams, of the test portion. 5.2 Permissible tolerances The deviations between three independent determinations shall not exceed0,1times the element content in per cent (absolute value). 5.3 Final result Report the arithmetical mean of

43、 acceptable determinations rounded to the nearest value as shown inTable 2. Table 2 Rounding of results If the element content is below0,5% (m/m), use the relevant part of this standard. If the element is greater than2% (m/m), report it as greater than2% (m/m). Content % (m/m) Round to the nearest %

44、 (m/m) from 0,5 to 1 over 1 to 2 0,02 0,05 cV 10 4 m -EN27627-5:1993 BSI 12-1999 5 Annex ZA (normative) Normative references to international publications with their relevant European publications This European Standard incorporates by dated or undated reference, provisions from other publications.

45、These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For un

46、dated references the latest edition of the publication referred to applies (including amendments). Publication Year Title EN/HD Year ISO 7627-1 Hardmetals Chemical analysis by flame atomicabsorption spectrometry Part1: General requirements EN 27627-16 blankBSEN27627-5:1993 BSI 12-1999 National annex

47、 NA (informative) Committees responsible The UnitedKingdom participation in the preparation of this European Standard was entrusted by the Iron and Steel Standards Policy Committee (ISM/-) to Technical Committee ISM/65, upon which the following bodies were represented: British Hardmetal Association

48、Federation of British Engineers (Test Manufacturers) Society of Motor Manufacturers and Traders Limited Coopted member National annex NB (informative) Cross-reference Publication referred to Corresponding British Standard ISO 7627-1:1983 BS EN 27627 Hardmetals Chemical atomic absorption spectrometry

49、 Part1:1993 General requirementsBS EN 27627-5:1993 ISO7627-5: 1985 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions BritishStandards are updated by amendment or revision. Users of BritishStandards should make sure that they possess the latest amendments or edit