SIST EN 15622:2010

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kupfer und Kupferlegierungen - Bestimmung des Bleigehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)Cuivre et alliages de cuivre - Dosage du plomb - Méthode par spectrométrie d'absorption atomique dans la flammeCopper and copper alloys - Determination of lead content - Flame atomic absorption spectrometry method (FAAS)77.120.30Baker in bakrove zlitineCopper and copper alloysICS:Ta slovenski standard je istoveten z:EN 15622:2010SIST EN 15622:2010en,fr,de01-maj-2010SIST EN 15622:2010SLOVENSKI
STANDARD



SIST EN 15622:2010



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15622
March 2010 ICS 77.120.30 English Version
Copper and copper alloys - Determination of lead content - Flame atomic absorption spectrometric method (FAAS)
Cuivre et alliages de cuivre - Dosage du plomb - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
Kupfer und Kupferlegierungen - Bestimmung des Bleigehaltes -Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This European Standard was approved by CEN on 23 January 2010.
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 references concerning such national standards may be obtained on application to the CEN Management Centre 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 into its own language and notified to the CEN Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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EN 15622:2010 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Principle .44Reagents .45Apparatus .56Sampling .57Procedure .57.1Preparation of the test portion solution .57.1.1Test portion .57.1.2Test portion solution .57.1.3Lead mass fractions between 0,01 % and 0,15 % .67.1.4Lead mass fractions between 0,1 % and 0,75 % .67.1.5Lead mass fractions between 0,5 % and 5,0 % .67.2Blank test .67.3Check test .67.4Establishment of the calibration curve .67.4.1Preparation of the calibration solutions .67.4.2Adjustment of the atomic absorption spectrometer .87.4.3Spectrometric measurement .87.4.4Calibration curve.87.5Determination .87.5.1General .87.5.2Preliminary spectrometric measurement .97.5.3Spectrometric measurements .98Expression of results .98.1Use of calibration curve .98.2Use of bracketing method .99Precision . 1010Test report . 11Bibliography . 12 SIST EN 15622:2010



EN 15622:2010 (E) 3 Foreword This document (EN 15622:2010) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. 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 September 2010, and conflicting national standards shall be withdrawn at the latest by September 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 "Methods of analysis" to prepare the following European Standard: EN 15622, Copper and copper alloys — Determination of lead content — Flame atomic absorption spectrometric method (FAAS). According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 15622:2010



EN 15622:2010 (E) 4 1 Scope This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the lead in copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having lead mass fractions between 0,01 % and 5,0 %. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1811-1, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 1: Sampling of cast unwrought products ISO 1811-2, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 2: Sampling of wrought products and castings 3 Principle Dissolution of a test portion in fluoroboric-nitric acid mixture followed, after suitable dilution, by aspiration of the test solution into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 217,0 nm line emitted by a lead hollow-cathode lamp. NOTE During the validation exercise of this standard method some laboratories have also carried out the measurements at 283 nm line. These measurements showed a satisfactory trueness. However, the number of results produced was too few and, therefore, insufficient for the estimation of the corresponding precision data. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Nitric acid, HNO3 (ρ = 1,40 g/ml). 4.2 Nitric acid solution (1 + 1). Add 100 ml of nitric acid (4.1) to 100 ml of water. 4.3 Hydrofluoric acid, HF, 40 % solution (ρ = 1,13 g/ml). WARNING — Hydrofluoric acid is a hazardous substance. Care shall be taken and it shall be used under an efficient fume hood. 4.4 Boric acid, H3BO3, 40 g/l solution. 4.5 Fluoroboric-nitric acid mixture. Add 300 ml of boric acid (4.4), 30 ml of hydrofluoric acid (4.3) and 500 ml of nitric acid (4.1) to 150 ml of water and mix well. 4.6 Lead stock solution, 1,0 g/l Pb. SIST EN 15622:2010



EN 15622:2010 (E) 5 Weigh (1 ± 0,001) g of lead (Pb ≥ 99,9 %) and transfer it into a 250 ml beaker. Add 20 ml of nitric acid solution (4.2), cover with a watch glass and heat gently until the lead is completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, add 100 ml of water and 9 ml of nitric acid solution (4.2). Dilute to the mark with water and mix well. 1 ml of this solution contains 0,001 g of Pb. 4.7 Lead standard solution, 0,1 g/l Pb. Transfer 25,0 ml of the lead stock solution (4.6) into a 250 ml one-mark volumetric flask, add 100 ml of water and 9 ml of nitric acid solution (4.2). Dilute to the mark with water and mix well. 1 ml of this solution contains 0,1 mg of Pb. 4.8 Copper base solution, 20 g/l Cu. Weigh (10 ± 0,01) g of pure, lead-free copper (Pb < 0,000 2 %) and transfer it into a 600 ml polytetrafluorethylene, polyethylene or low-pressure polypropylene beaker. Add 400 ml of the fluoroboric-nitric acid mixture (4.5) and cover with a watch glass. Heat until the copper is completely dissolved, then boil until the nitrous fumes have been expelled. Allow to cool and transfer the solution into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 50 ml of the solution contain 1,0 g of copper and 40 ml of the fluoroboric-nitric acid mixture. 5 Apparatus 5.1 Beakers, polytetrafluorethylene, polyethylene or polypropylene. 5.2 One-mark volu
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