BS EN 27627-2-1993 Hardmetals - Chemical analysis by flame atomic absorption spectrometry - Determination of calcium potassium magnesium and sodium in contents from 0 001 to 0 02 %.pdf

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1、BRITISH STANDARD BS EN 27627-2:1993 ISO 7627-2: 1983 Hardmetals Chemicalanalysis by flame atomic absorption spectrometry Part 2: Determination of calcium, potassium, magnesium and sodium in contents from0.001 to 0.02% (m/m) The European Standard EN 27627-2:1993 has the status of a British Standard U

2、DC 669.018.25:620.1:543.422BSEN 27627-2:1993 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 into effect on 15June1993 BSI 01-2000 The following BSI references relate to

3、the work on this standard: Committee reference ISM/65 Special announcement BSI News January 1993 ISBN 0 580 21943 7 Cooperating organizations The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations

4、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. Greece Hellenic Organiza

5、tion 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 Standardiseringsforbund Portugal

6、 Instituto Portugus da Qualidade Spain Asociacin Espaola de Normalizacin y Certificacin Sweden Standardiseringskommissionen i Sverige Switzerland Association suisse de normalisation United Kingdom British Standards Institution Amendments issued since publication Amd. No. Date CommentsBSEN 27627-2:19

7、93 BSI 01-2000 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 publicationswiththeir relevant

8、European publications 5 National annex NA (informative) Committees responsible Inside back cover National annex NB (informative) Cross-reference Inside back cover Table Instrumental parameters and characteristics of calibration function 4BSEN 27627-2:1993 ii BSI 01-2000 National foreword This Britis

9、h Standard has been prepared under the direction of the Iron and Steel Standards Policy Committee and is the English language version of EN27627-2:1993 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part 2: Determination of calcium, potassium, magnesium and sodium in contents f

10、rom 0.001 to 0.02% (m/m), published by the European Committee for Standardization (CEN). It is identical with ISO7627-2:1983, published by the International Organization for Standardization (ISO). This British Standard supersedes BS5600-4.17.2:1986 which is withdrawn and from which it differs by the

11、 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. Summary of pages Th

12、is document comprises a front cover, an inside front cover, pagesi andii, theENtitle page, pages2 to6, 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 table on the inside fron

13、t cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN27627-2 April1993 UDC669.018.25:620.1:543.422 Descriptors: Powder metallurgy, hard metals, chemical analysis, determination of content, calcium, potassium, magnesium, sodium, spectrometric analysis, atomic absorption spectrophotometry Engli

14、sh version Hardmetals Chemical analysis by flame atomic absorption spectrometry Part 2: Determination of calcium, potassium, magnesium and sodium in contents from0,001 to 0,02% (m/m) (ISO 7627-2:1983) Mtaux-durs Analyse chimique par spectromtrie dabsorption atomique dans la flamme Partie 2: Dosage d

15、u calcium, du potassium, du magnsium et du sodium des teneurs comprises entre 0,001 et 0,02% (m/m) (ISO 7627-2:1983) Hartmetalle Chemische Analyse durch Flammenatomabsorptionsspektrometrie Teil 2: Bestimmung des Calcium-, Kalium-, Magnesium- und Natriumgehaltes von 0,001 bis 0,02% (m/m) (ISO 7627-2:

16、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 bibliographical re

17、ferences 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 CEN member

18、 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, Spain, Sweden

19、, 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 27627-2:1993 EEN 27627-2:1993 BSI 01-2000 2 Foreword I

20、n 1992, ISO 7627-2:1983 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part 2: Determination of calcium, potassium, magnesium and sodium in contents from0,001 to0,02% (m/m) was submitted to the CEN Primary Questionnaire procedure. Following the positive result of the CEN/CS Pro

21、posal ISO7627-2:1983 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 standar

22、ds 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, Port

23、ugal, Spain, Sweden, Switzerland, UnitedKingdom. NOTEThe European references to international publications are given inAnnex ZA (normative).EN 27627-2:1993 BSI 01-2000 3 1 Scope and field of application This part of ISO7627 specifies the method to be used for the determination of calcium, potassium,

24、 magnesium and sodium contents of hardmetals within the range0,001 to0,02% (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. NOTEIn low concentrations,

25、the determination of these elements is very critical. Every care should be taken to avoid contamination from atmosphere and reagents. 2 Reference ISO 7627-1, Hardmetals Chemical analysis by flame atomic absorption spectrometry Part1:General requirements. 3 Reagents If necessary, reagents of the high

26、est purity shall be used. 3.1 Hydrofluoric acid, 1,12g/ml. 3.2 Nitric acid, 1,42g/ml. 3.3 Ammonium fluoride, 0,1g/ml solution. 3.4 Caesium chloride, 0,01g/ml solution. 3.5 High-purity stock solutions, for calibration purposes for each element to be determined, containing1,000g of the element per lit

27、re. 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. Cover the b

28、eaker. 4.2 Dissolution of the test portion Add 10 ml 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 solutio

29、n (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 to theTable as follows: 4.3.1 Dilution volume 100m

30、l: 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 the ammoniu

31、m 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 volumes

32、of properly diluted stock solutions of the elements to be determined according to the concentration ranges to be covered. Make up to100ml and mix. 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 at least

33、two 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 instrument at the wavele

34、ngth given for the element being determined. See theTable. 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

35、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 which build up on t

36、he 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. 4.6.3 Convert the

37、 absorbance values of the test solutions corrected for the blank to milligrams of the element per litre by means of the calibration curve.EN 27627-2:1993 4 BSI 01-2000 5 Expression of results 5.1 Calculation The element content, expressed as a percentage by mass, is given by the formula where c is t

38、he concentration, 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 exceed0,0005% (absolute value) at the l

39、ower limit of determination. It shall not exceed0,002% at the0,02% level. 5.3 Final result Report the arithmetical mean of acceptable determinations rounded to0,001% (m/m). If the element content is below0,001% (m/m) or greater than0,02% (m/m), report the result as less than0,001% (m/m) or greater t

40、han0,02% (m/m) respectively. Table Instrumental parameters and characteristics of calibration functions cV 10 4 m - Element Dilution volume (V) for1 g test portion a Oxidant Wavelength Reciprocal sensitivity, for 1% absorption a Linear range a Notes ml nm 4g/ml % Ca K Mg Na 100 100 100 100 N 2 O air

41、 N 2 O air 422,7 769,9 285,2 589,3 0,03 0,04 0,02 0,02 0,001to 0,02 0,0005 to 0,02 0,0003 to 0,04 0,0005 to 0,02 1 2 NOTE 1Sensitivity is greatly dependent on matrix composition. NOTE 2Use the doublet. a Guidelines for information only.EN 27627-2:1993 BSI 01-2000 5 Annex ZA (normative) Normative ref

42、erences to international publications with their relevant European publications This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter.

43、 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 references the latest edition of the publication referred to applies (including amendments). Publication Year T

44、itle EN/HD Year ISO 7627-1 Hardmetals Chemical analysis by flame atomicabsorption spectrometry Part1:Generalrequirements EN 27627-16 blankBSEN 27627-2:1993 BSI 01-2000 National annex NA (informative) Committees responsible The United Kingdom participation in the preparation of this European Standard

45、 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 Federation of British Engineers (Test Manufacturers) Society of Motor Manufacturers and Traders Limited Coopted member

46、 National annex NB (informative) Cross-reference Publication referred to Corresponding British Standard EN 27627-1:1993 ISO 7627-1:1983 BS EN 27627-1 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part 1:1993 General requirements BS EN 27627-2:1993 ISO7627-2: 1983 BSI 389 Chisw

47、ick 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 am

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