1、BRITISH STANDARD BS EN 27627-4:1993 ISO 7627-4: 1983 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part 4: Determination of molybdenum, titanium and vanadium in contents from0.01 to0.5% (m/m) The European Standard EN 27627-4:1993 has the status of a British Standard UDC 669.01
2、8.25:620.1:543.422BSEN27627-4:1993 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 o
3、n this standard: Committee reference ISM/65 Special announcement in BSINews January 1993 ISBN 0 580 21932 1 Cooperating organizations The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations of the f
4、ollowing 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 for
5、 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 Institu
6、to 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 CommentsBSEN27627-4:1993 BSI 01-
7、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 European
8、 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 4BSEN27627-4:1993 ii BSI 01-2000 Natio
9、nal foreword This British Standard has been prepared under the direction of the Iron and SteelStandards Policy Committee and is the English language version of EN27627-4:1993 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part4: Determination of molybdenum, titanium and vanadiu
10、m in contents from0,1 to0,5% (m/m), published by the European Committee for Standardization (CEN). It is identical with ISO7627-4:1983, prepared by Technical Committee119, Powder metallurgy, of the International Organization for Standardization (ISO) with the active participation of the UK. This Bri
11、tish Standard supersedes BS5600-4.17.4:1986, 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 responsible for their correct application. Compliance with a
12、 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. This standard has been updated (see copyright date) and m
13、ay have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 27627-4 April 1993 UDC 669.018.25:620.1:543.422 Descriptors: Powder metallurgy, hard metals, chemical analysis, determination of content,
14、transition metals, molybdenum, titanium, vanadium, spectrometric analysis, atomic absorption spectrophotometry English version Hardmetals Chemical analysis by flame atomic absorption spectrometry Part4: Determination of molybdenum, titanium and vanadium in contents from 0,01to0,5 % (m/m) (ISO 7627-4
15、:1983) Mtaux-durs Analyse chimique par spectromtrie dabsorption atomique dans la flamme Partie4: Dosages du molybdne, dutitane et du vanadium des teneurs comprises entre0,01 et0,5% (m/m) (ISO7627-4:1983) Hartmetalle Chemische Analyse durch Flammenatomabsorptionsspektrometrie Teil4: Bestimmung des Mo
16、lybdn-, Titan- und Vanadiumgehaltes von0,01 bis0,5% (m/m) (ISO7627-4:1983) 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 sta
17、ndard 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 any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other
18、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. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ire
19、land, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, 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 membe
20、rs Ref. No. EN 27627-4:1993 EEN27627-4:1993 BSI 01-2000 2 Foreword In 1992, ISO7627-4:1983 Hardmetals Chemicalanalysis by flame atomic absorption spectrometry Part4: Determination of molybden, titanium and vanadium in contents from0,01 to0,5% (m/m) was submitted to the CEN Primary Questionnaire proc
21、edure. Following the positive result of the CEN/CS Proposal ISO7627-4:1983 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 l
22、atest 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, Denmark, Finland, France, Germany, Greece, Iceland,
23、 Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. NOTEThe European references to international publications are given inAnnex ZA (normative).EN27627-4:1993 BSI 01-2000 3 1 Scope and field of application This part of ISO7627 specifies the method
24、 to be used for the determination of molybdenum, titanium and vanadium contents of hardmetals within the range0,01 to0,5% (m/m) by flame atomic absorption spectrometry. General requirements concerning the field of application, principle, interfering elements, apparatus, sampling and test report are
25、given in ISO7627-1. 2 Reference ISO 7627-1, Hardmetals Chemical analysis byflame atomic absorption spectrometry Part1:requirements. 3 Reagents 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
26、 stock solutions, for calibration purposes for each element to be determined, containing1,000g of the element perlitre. 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
27、test sample. Transfer it to a100ml 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 then5ml of the nitric acid (3.2), dropby drop, to the beaker containing the test po
28、rtion (4.1) and heat gently until the test portion iscompletely dissolved. Add10ml of the caesium chloride solution (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
29、Prepare the relevant dilution volume for the analysis according toTable 1 as follows: 4.3.1 Dilution 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
30、polypropylene one-mark volumetric flask. Add10ml of the caesium chloride solution (3.4). Add10ml 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 to4.2 with a matrix composition as simila
31、r as possible to the 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 to100ml and mix. 4.4.2 Also prepare calibration solutions w
32、ith 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 addition of the relevant element to be determined. Table 1 Instrumental parameters and characteristics of calibration functions Element Dilution vo
33、lume (V) for1g test portion a Oxidant Wavelength Reciprocal sensitivity, for1% absorption a Linear range a Notes ml nm 4g/ml % Mo Ti V 100 100 100 100 N 2 O N 2 O N 2 O N 2 O 313,3 313,3 364,3 318,4 0,3 6 1,0 0,8 0,003to0,1 0,06to 10,0 0,03to0,5 0,008to0,5 1 1 and 2 1 3 NOTE 1Use a fuel-rich flame.
34、NOTE 2Adjust the burner head at right angles to the light beam or dilute the solutions appropriately. NOTE 3Use of the triplet. a Guidelines for information only.EN27627-4:1993 4 BSI 01-2000 4.5 Adjustment of the atomic absorption spectrometer SAFETY PRECAUTION: Follow the manufacturers recommendati
35、on on igniting and extinguishing the flame. Optimize the response of the instrument at the wavelength given for the element being determined. SeeTable 1. Preheat the burner for about5min and then adjust the fuel and correct the burner to obtain maximum absorption while aspirating a calibration solut
36、ion. Make sure that the absorbance reading is not drifting. Aspirate water and set 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 betw
37、een each solution. Make at least two measurements for each solution. If a build-up of solids occurs on the burner slit, it will cause a decrease of sensitivity and must be removed. 4.6.2 Prepare a calibration curve by plotting the obtained absorbance values of the calibration solutions corrected for
38、 the blank against the concentration, in milligrams per litre, of the element. 4.6.3 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, expr
39、essed as a percentage by mass, is given by the formula where c is the concentration, in milligrams per litre, of the element of 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 independe
40、nt determinations shall not exceed0,2times the element content inpercent (absolute 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 below0,01% (m/m), report it as
41、less than0,01% (m/m). Content Round to the nearest % (m/m) % (m/m) from 0,01 to 0,1 over 0,1 to 0,5 0,01 0,05 c V 10 4 m -EN27627-4:1993 BSI 01-2000 5 Annex ZA (normative) Normative references to international publications with their relevant European publications This European Standard incorporates
42、 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. For dated references, subsequent amendments to or revisions of any of these publications apply to this European St
43、andard 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 Title EN/HD Year ISO 7627-1 Hardmetals Chemical analysis by flame atomic absorption spectrometry Part1: General requ
44、irements EN 27627-16 blankBSEN27627-4:1993 BSI 01-2000 National annex NA (informative) 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
45、 the following bodies were represented: British Hardmetal Association 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 EN 27627
46、-1:1993 ISO 7627-1:1983 BS EN 27627 Powder metallurgical materials and products Part 1:1993 General requirements BS EN 27627-4:1993 ISO 7627-4: 1983 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards
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