EN 14726:2005

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Aluminium und Aluminiumlegierungen - Chemische Analyse - Leitfaden für die optische FunkenemissionsspektralanalyseAluminium et alliages d'aluminium - Analyse chimique - Directives pour l'analyse par spectrométrie d'émission optique a étincellesAluminium and aluminium alloys - Chemical analysis - Guideline for spark optical emission spectrometric analysis77.120.10Aluminij in aluminijeve zlitineAluminium and aluminium alloys77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 14726:2005SIST EN 14726:2005en01-december-2005SIST EN 14726:2005SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14726September 2005ICS 77.120.10; 77.040.30 English VersionAluminium and aluminium alloys - Chemical analysis - Guidelinefor spark optical emission spectrometric analysisAluminium et alliages d'aluminium - Analyse chimique -Directives pour l'analyse par spectrométrie d'émissionoptique à étincellesAluminium und Aluminiumlegierungen - ChemischeAnalyse - Leitfaden für 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 conditions 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 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, 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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2005 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14726:2005: ESIST EN 14726:2005

Contents Page Foreword.3 Introduction.4 1 Scope.5 2 Normative references.5 3 Terms and definitions.5 4 Symbols and abbreviations.5 5 Review and principle of test method.6 6 Consumables and calibration materials.6 6.1 Consumables.6 6.2 Reference material and recalibration samples.6 7 Testing equipment.7 7.1 Spark spectrometer.7 7.2 Equipment for sample preparation.8 8 Samples.8 8.1 Requirements on test samples.8 8.2 Sampling.8 9 Sample preparation.9 10 Operating conditions of the spectrometer.10 11 Taking measurements.10 12 Calibration and evaluation (methods of calculation).11 12.1 Fundamental principles.11 12.2 Standard and reference materials.12 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 uncertainty.17 13.4 Comprehensive investigation of accuracy.18 14 Inspection.19 14.1 General.19 14.2 Continuous supervision.19 14.3 Checking the analytical sample.19 14.4 Analytical capability.19 15 Availability of the analytical system.20 16 Test report.20 Annex A (informative)
Representative sparking area.21 Bibliography.22
3 Foreword This 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 endorsement, 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, Cyprus, 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. SIST EN 14726:2005

Introduction In optical atomic 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 characteristic 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 laboratory 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 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, 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, 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. SIST EN 14726:2005

5 1 Scope This European Standard gives guidance on the 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 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 agreement 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 spectrometer. 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 applies. 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/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, 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 12258-2:2004 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). SIST EN 14726:2005

5 Review and principle of test method a) Spark spectrometric 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 material 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 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 agreed 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
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