BS EN 27627-3-1993 Hardmetals - Chemical analysis by flame atomic absorption spectrometry - Determination of cobalt iron manganese and nickel in contents from 0 01 to 0 5 % (m m)《硬.pdf

1、BRITISH STANDARD BS EN 27627-3:1993 ISO 7627-3: 1983 Hardmetals Chemical analysis by flame atomicabsorption spectrometry Part 3: Determination of cobalt, iron, manganese and nickel in contents from 0.01 to 0.5% (m/m) The European Standard EN 27627-3:1993 has the status of a British Standard UDC 669.

2、018.25:620.1:543.422BSEN27627-3:1993 This British 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 15June 1993 BSI 01-2000 The following BSI references relate to the work

3、 on this standard: Committee reference ISM/65 Special announcement in BSINews January 1993 ISBN 0 580 21942 9 Cooperating organizations The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations of the

4、 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. Greece Hellenic Organization f

5、or 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 Standardiseringsforbund Portugal Insti

6、tuto 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 CommentsBSEN27627-3:1993 BSI 0

7、1-2000 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 publications with their relevant Europe

8、an 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 function 3 Table 2 Rounding of results 4BSEN27627-3:1993 ii BSI 01-2000 Nati

9、onal foreword This British Standard has been prepared under the direction of the Iron and SteelStandards Policy Committee and is the English language version of EN27627-3:1993 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part 3: Determination of cobalt, iron, manganese and ni

10、ckel in contents from 0.01 to 0.5% (m/m), published by the European Committee for Standardization (CEN). It is identical with ISO7627-3:1983, published by the International Organization for Standardization (ISO). This British Standard supersedes BS 5600-4.17.3:1986 which is withdrawn and from which

11、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 responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Su

12、mmary of pages This document comprises a front cover, an inside front cover, pages i and ii, theEN title page, pages2 to 6, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment tab

13、le on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 27627-3 April 1993 UDC 669.018.25:620.1:543.422 Descriptors: Powder metallurgy, hard metals, chemical analysis, determination of content, transition metals, cobalt, iron, manganese, nickel, spectrometric analysis, atom

14、is absorption spectrophotometry English version Hardmetals Chemical analysis by flame atomic absorption spectrometry Part 3: Determination of cobalt, iron, manganese and nickel in contents from 0,01 to0,5%(m/m) (ISO 7627-3:1983) Mtaux-durs Analyse chimique par spectromtrie dabsorption atomique dans

15、la flamme Partie 3: Dosage du cobalt, du fer, dumanganse et du nickel des teneurs comprises entre 0,01 et 0,5% (m/m) (ISO 7627-3:1983) Hartmetalle Chemische Analyse durch Flammenatomabsorptionsspektrometrie Teil 3: Bestimmung des Cobalt-, Eisen-, Mangan- und Nickelgehaltes von 0,01 bis 0,5% (m/m) (I

16、SO 7627-3:1983) This European Standard was approved by CEN on 1993-04-02. 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 bibliogr

17、aphical references concerning such national standards may 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

18、CEN member into its own language and notified to the Central 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, Spa

19、in, Sweden, Switzerland and UnitedKingdom. CEN European Committee 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 27627-3:1993 EEN27627-3:1993 BSI 01-2000 2 F

20、oreword In 1992, ISO 7627-3:1983 Hardmetals Chemicalanalysis by flame atomic absorption spectrometry Part 3: Determination of cobalt, iron, manganese and nickel in contents from 0,01 to0,5% (m/m) was submitted to the CEN Primary Questionnaire procedure. Following the positive result of the CEN/CS Pr

21、oposal ISO 7627-3:1983 was submitted 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 stand

22、ards 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, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Po

23、rtugal, Spain, Sweden, Switzerland, UnitedKingdom. NOTEThe European references to international publications are given in Annex ZA (normative).EN27627-3:1993 BSI 01-2000 3 1 Scope and field of application This part of ISO 7627 specifies the method to be used for the determination of cobalt, iron, ma

24、nganese and nickel contents of hardmetals within the range 0,01 to 0,5% (m/m) by flame atomic absorption spectrometry. General requirements concerning the field of application, principle, interfering elements, apparatus, sampling and test report are given in ISO7627-1. 2 Reference ISO 7627-1, Hardme

25、tals Chemical analysis by flame atomic absorption spectrometry Part1:General requirements. 3 Reagents 3.1 Hydrofluoric acid, 1,12 g/ml. 3.2 Nitric acid, 1,42 g/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 pur

26、poses for each element to be determined, containing 1,000 g of the element per litre. NOTEThis value is understood to establish a maximum limit of 1,0005g and a minimum limit of 0,9995g. 4 Procedure 4.1 Test portion Weigh, to the nearest 0,001g, approximately1g of the test sample. Transfer it to a 1

27、00ml polytetrafluorethylene beaker or a beaker of other suitable material. Cover the beaker. 4.2 Dissolution of the test portion Add 10 ml of water, 5ml of the hydrofluoric acid(3.1), and then 5ml of the nitric acid (3.2), dropby drop, to the beaker containing the test portion(4.1) and heat gently u

28、ntil the test portion is completely dissolved. Add 10ml of the caesium chloride solution (3.4) and 10ml of the ammonium fluoride solution (3.3). Then transfer the solution totally to a 100ml polypropylene one-mark volumetric flask and dilute to the mark. 4.3 Dilution volume Prepare the relevant dilu

29、tion volume for the analysis according toTable 1 as follows: 4.3.1 Dilution volume 100 ml: 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 transferring 10ml of the solution in4.2 to a 100ml polypropylene one-mar

30、k volumetric flask. Add 10ml of the caesium chloride solution (3.4). Add 10ml of the 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 to 4.2 with a matrix composition as similar as possible to t

31、he test portion to be analysed, but without making up to volume. Then add increasing volumes of properly diluted stock solutions of the elements to be determined according to the concentration ranges to be covered. Make up to 100ml and mix. 4.4.2 Also prepare calibration solutions with a diluted mat

32、rix in accordance with4.3 for dilution volumes of 1000ml, if necessary. Table 1 Instrumental parameters and characteristics of calibration functions Element Dilution volume (V) for 1 g test portion a Oxidant Wavelength Reciprocal sensitivity, for 1% absorption a Linear range a Notes ml nm 4g/ml % Co

33、 Fe Mn Ni 100 100 1 000 100 1 000 100 1 000 N 2 O N 2 O N 2 O N 2 O N 2 O N 2 O N 2 O 240,7 248,3 248,3 279,8 279,8 232,0 232,0 0,7 0,3 0,3 0,1 0,1 0,3 0,3 0,007 to 0,5 0,003 to 0,05 0,03to 2,0 0,001 to 0,03 0,01to 2,0 0,003 to 0,05 0,05to 5,0 1 2 2 3 3 NOTE 1When a broad spectral band pass is used,

34、 a single-element hollow cathode lamp is mandatory. NOTE 2Use of the triplet. NOTE 3Sensitivity is greatly dependent on matrix composition. Use of a narrow-spectral band pass and a single-element hollow-cathode lamp is mandatory. a Guidelines for information only.EN27627-3:1993 4 BSI 01-2000 4.4.3 P

35、repare one or more blank solutions (see4.4.1) without the 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 instrumen

36、t at the wavelength given for the element being determined. See Table 1. Preheat the burner for about 5min 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 s

37、et the initial reading to zero absorbance. 4.6 Atomic absorbance 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 whic

38、h build up on the burner slit must be removed, otherwise they 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.

39、6.3 Convert the absorbance values of the test solutions corrected 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 concentrati

40、on, in milligrams per litre, of the element in the test solution; 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 exceed0,2 times the element content in per cent (abso

41、lute value). 5.3 Final result Report the arithmetical mean of acceptable determinations rounded to the nearest value as shown inTable 2. Table 2 Rounding of results If the element content is below 0,01% (m/m), report it as less than 0,01% (m/m). Content Round to the nearest % (m/m) % (m/m) from 0,01

42、 to 0,1 over 0,1 to 0,5 0,01 0,05 cV 10 4 m -EN27627-3:1993 BSI 01-2000 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. These nor

43、mative 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 undated ref

44、erences 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 atomic absorption spectrometry Part1:General requirements EN 27627-16 blankBSEN27627-3:1993 BSI 01-2000 National annex NA (info

45、rmative) Committees responsible The United Kingdom 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 Federatio

46、n 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 EN 27627-1 ISO 7627-1:1983 BS EN 27627-1 Hardmetals Chemical analysis by flame atomic a

47、bsorption spectrometry Part 1:1993 General requirements BS EN 27627-3:1993 ISO7627-3: 1983 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 th

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