1、BRITISH STANDARDBS EN 14726:2005Aluminium and aluminium alloys Chemical analysis Guideline for spark optical emission spectrometric analysisThe European Standard EN 14726:2005 has the status of a British StandardICS 77.120.10; 77.040.30g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g
2、3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14726:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2005 BSI 31 October 2005ISBN 0
3、580 46792 9National forewordThis British Standard is the official English language version of EN 14726:2005.The UK participation in its preparation was entrusted to Technical Committee NFE/35, Light metals and their alloys, which has the responsibility to:A list of organizations represented on this
4、committee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the
5、 “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard does not of itself confer immunity from lega
6、l obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary
7、 of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 22 an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsEUROP
8、EAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14726September 2005ICS 77.120.10; 77.040.30English VersionAluminium and aluminium alloys - Chemical analysis - Guidelinefor spark optical emission spectrometric analysisAluminium et alliages daluminium - Analyse chimique -Directives pour lanalyse par spec
9、tromtrie dmissionoptique tincellesAluminium und Aluminiumlegierungen - ChemischeAnalyse - Leitfaden fr die optischeFunkenemissionsspektralanalyseThis European Standard was approved by CEN on 22 July 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the co
10、nditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three
11、official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria,
12、 Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONC
13、OMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14726:2005: EEN 14726:2005 (E) 2 Contents Page Foreword 3 Introduc
14、tion4 1 Scope .5 2 Normative references .5 3 Terms and definitions.5 4 Symbols and abbreviations5 5 Review and principle of test method.6 6 Consumables and calibration materials6 6.1 Consumables 6 6.2 Reference material and recalibration samples .6 7 Testing equipment 7 7.1 Spark spectrometer 7 7.2
15、Equipment for sample preparation8 8 Samples .8 8.1 Requirements on test samples 8 8.2 Sampling8 9 Sample preparation.9 10 Operating conditions of the spectrometer10 11 Taking measurements 10 12 Calibration and evaluation (methods of calculation) .11 12.1 Fundamental principles11 12.2 Standard and re
16、ference materials12 12.3 Base calibration 13 12.4 Recalibration .14 12.5 Alloy group calibration with simultaneous calibration 16 13 Accuracy (precision and trueness)16 13.1 General 16 13.2 Possibility of error 16 13.3 Measuring and calibration uncertainty17 13.4 Comprehensive investigation of accur
17、acy18 14 Inspection19 14.1 General 19 14.2 Continuous supervision .19 14.3 Checking the analytical sample .19 14.4 Analytical capability19 15 Availability of the analytical system20 16 Test report .20 Annex A (informative) Representative sparking area21 Bibliography.22 EN 14726:2005 (E) 3 Foreword T
18、his European Standard (EN 14726:2005) has been prepared by Technical Committee CEN/TC 132 “Alumin-ium and aluminium alloys”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsemen
19、t, at the latest by March 2006, and conflicting national standards shall be withdrawn at the latest by March 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following coun-tries are bound to implement this European Standard: Austria, Belgium, Cypr
20、us, Czech Republic, Denmark, Esto-nia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 14726:2005 (E) 4 Introduction In optical atomi
21、c emission spectral analysis (OES) with excitation by electric spark discharges, (S-OES), a small portion of the sample is thermally atomized through the erosion of an electric spark. In the spark discharge, the aerosol is atomized, partially ionised and excited to emit optical radiation. The charac
22、teristic radiation for each element is used in OES for element detection and for the quantitative determination of the element contents. The test result obtained on a small test portion (mostly less than one milligram per spark spot) of one or more laboratory samples is referred either to a laborato
23、ry sample or to many tons of a melt or a cast product of aluminium or aluminium alloys. Cast structure and segregation interfere with measurement. S-OES is suitable for determining the chemical composition of metal samples as defined in technical specifications. S-OES serves as inspection, test and
24、measuring equipment for alloy compositions to control and inspect the manufacturing and casting processes. For those purposes, laboratory samples are taken from the liquid metal after melting down of the alloying constituents and during casting in different process stages. Besides process inspection
25、, S-OES, within the framework of a chemical-analytical service, facilitates the preparation of a test report which refers to the laboratory sample or to an agreed sample area of that sample. The testing equipment, including software used in the testing laboratories, is subject to change. Therefore,
26、these guidelines describe the common principles. It gives guidance to specific criteria which should be met and the detailed documentation for the laboratory procedures to obtain traceable test results with uncertainty intervals. EN 14726:2005 (E) 5 1 Scope This European Standard gives guidance on t
27、he criteria and the fundamental operation procedure governing the spark optical emission spectral analysis (S-OES) of metal samples, beginning with sampling, through sample preparation to reporting the test, as well as the requirements of the whole spark source spectrometric procedure which shall be
28、 fulfilled with respect to: observance of the agreed precision and trueness ISO 3534-1, ISO 5725-1 of the analytical results with refer-ence to the agreed sample or sample area; traceability of the analytical results to the international base units mass (kg) and amount of substance (mol); proof of a
29、greement between the spark spectrometric result and the average composition of the supplied metal sample within the given uncertainty ISO 3534-1 of the analytical result; comparability of the test results between different laboratories; as far as possible, a trouble-free operation of the spark spect
30、rometer. These guidelines refer to computer-controlled simultaneously measuring spectrometers for the analysis of solid samples. 2 Normative references The following referenced documents are indispensable for the application of this European Standard. For dated references, only the edition cited app
31、lies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12258-2:2004, Aluminium and aluminium alloys Terms and definitions Part 2: Chemical analysis EN 14361, Aluminium and aluminium alloys Chemical analysis Sampling from metal melts EN ISO/
32、IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) ISO 3534-1, Statistics Vocabulary and symbols Part 1: Probability and general statistical terms ISO 3534-2, Statistics Vocabulary and symbols Part 2: Statistical quality control ISO 5725-1
33、, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions ISO Guide 30, Terms and definitions used in connection with reference materials 3 Terms and definitions For the purposes of this European Standard the terms and definitions given in EN 1
34、2258-2:2004 apply. 4 Symbols and abbreviations Symbols and formula signs are defined immediately by the relevant formulae. Abbreviations are put in brackets immediately after a term first appears in the text (e.g. S-OES). EN 14726:2005 (E) 6 5 Review and principle of test method a) Spark spectrometr
35、ic measurement executed after mechanical preparation of the metal sample, which, if nec-essary, is taken from the metal melt. b) Evaluation of the measuring signal: 1) alloy calibration and universal calibration: with stored evaluation functions, which are evaluated by calibra-tion using reference m
36、aterial of a similar chemical composition; 2) master curve calibration: with recalculated evaluation functions after measuring reference material of known chemical composition. c) Evaluation and correction of measuring results as determined in preliminary testing or in accordance with data supplied
37、by the manufacturer of the spectrometer. d) Control, documentation and statistical evaluation of all parameters which codetermine the uncertainty (ISO 3534-1) of the analytical results with reference to the mean chemical composition of the supplied sample (see clause 9) or with reference to the agre
38、ed sample area. 6 Consumables and calibration materials 6.1 Consumables 6.1.1 General The consumables shall be specified in the analytical procedures or in the handbook of the equipment according to the instructions of the equipment manufacturer or according to preliminary tests. 6.1.2 Feed gas of s
39、pecified purity (argon for spectrometry, high purity, see instrument manufacturer recommen-dation). 6.1.3 Gas purification cartridge for the feed gas (if required to meet the instrument manufacturer specifications). 6.1.4 Cleaning brushes for the counterelectrode, if needed (the filaments should not
40、 contaminate the electrode to any measurable extent). 6.1.5 Particle trap for filtering the metal condensate out of the waste-gas stream. 6.1.6 Spare and expendable parts for the spark spectrometer in accordance with the manufacturers instructions (e.g. counter electrode, insert for sample table). 6
41、.2 Reference material and recalibration samples 6.2.1 General The reference materials (ISO Guide 30) and recalibration samples shall be listed and documented in the testing procedure. 6.2.2 Recalibration samples for drift correction (see clause 12). 6.2.3 Blank sample, high-purity aluminium or alumi
42、nium alloy based on high-purity constituents (e.g. AlSn30) (see clause 12). 6.2.4 Binary samples (if required e.g. for line interference correction (see clause 12). 6.2.5 Calibration samples (see clause 12). EN 14726:2005 (E) 7 6.2.6 Analytical control samples (see clauses 12 and 13). 6.2.7 Spectrom
43、eter control samples (see 14.2). 7 Testing equipment 7.1 Spark spectrometer Optical atomic emission spectrometer with excitation by spark discharge, suitable for the chemical analysis of aluminium and aluminium alloys for major, minor and trace constituents. Spark spectrometers comprise the followin
44、g main functional groups: a) system for atomization and excitation: 1) spark generator (spark source); 2) spark stand with counter electrode. b) spectral apparatus (system for spectral isolation or radiation splitting). c) system designed for radiation measurement (radiation detector). d) system for
45、 acquisition of the measured values, data processing and evaluation. NOTE In addition, there are units for power supply, gas supply, instrument control and supervision, for the further process-ing of analytical results, as well as input and output devices (keyboard, screen, printer, interface module
46、). In the documentation of spark spectrometer testing equipment, at least the following information shall be recorded (see also EN ISO/IEC 17025): designation of device (including internal identification number); manufacturer, type designation, serial number; procurement documents; condition when re
47、ceived (e.g. new, used, reconditioned); date placed in service (provisional taking over and taking over or acceptance of the equipment); description of the equipment. The description of the equipment shall include the main properties and characteristic features of the equipment or give information a
48、bout the relevant manufacturers notes and instructions, as follows: type of spectrometer (e.g. computer-controlled simultaneous measuring spectrometer with 20 detector (meas-urement) channels for the analysis of ); spectral apparatus and range of wavelengths (e.g. vacuum polychromator with diffracti
49、on grating lines/mm for wavelengths of .nm to . nm); mounting (type) of spectral apparatus (e.g. 1 metre Paschen-Runge mounting); list of measuring channels (element, wavelength, calibration range); spark stands, feed gas (sample table, type of counter electrode); spark source; computer with peripherals; software. EN 14726:2005 (E) 8 7.2 Equipment for sample preparation Lathes, milling machines, circular and band saws, a grinder or any suitable device can be used for the preparation of samples. For each m
