DIN EN ISO 11495-2016 Jewellery - Determination of palladium in palladium jewellery alloys - ICP-OES method using yttrium as internal standard element (ISO 11495 2014) German versi.pdf

1、December 2016 English price group 10No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 39.060!%l“2599273www.din.deDIN

2、EN ISO 11495Jewellery Determination of palladium in palladium jewellery alloys ICPOES method using yttrium as internal standard element (ISO 11495:2014);English version EN ISO 11495:2016,English translation of DIN EN ISO 11495:2016-12Schmuck Bestimmung von Palladium in Palladiumschmucklegierungen IC

3、POESVerfahren unter Verwendung von Yttrium als Internem Standardelement (ISO 11495:2014);Englische Fassung EN ISO 11495:2016,Englische bersetzung von DIN EN ISO 11495:2016-12Joaillerie, bijouterie Dosage du palladium dans les alliages de palladium pour la joaillerie, bijouterie Mthode par ICPOES uti

4、lisant lyttrium comme talon interne (ISO 11495:2014);Version anglaise EN ISO 11495:2016,Traduction anglaise de DIN EN ISO 11495:2016-12www.beuth.deDocument comprises 15 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.01.17 DIN

5、EN ISO 11495:2016-12 2 A comma is used as the decimal marker. National foreword The text of ISO 11495:2014 has been prepared by Technical Committee ISO/TC 174 “Jewellery” (Secretariat: DIN, Germany) and has been taken over as EN ISO 11495:2016 according to the decision CEN/BT C137/2015. The responsi

6、ble German body involved in its preparation was DIN-Normenausschuss Feinmechanik und Optik (DIN Standards Committee Optics and Precision Mechanics), Working Committee NA 027-04-04 AA Analysenmethoden. The DIN Standard corresponding to the International Standard referred to in this document is as fol

7、lows: ISO 9202 DIN EN ISO 9202 National Annex NA (informative) Bibliography DIN EN ISO 9202, Jewellery Fineness of precious metal alloys EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11495 October 2016 ICS 39.060 English Version Jewellery - Determination of palladium in palladium jeweller

8、y alloys - ICP-OES method using yttrium as internal standard element (ISO 11495:2014) Joaillerie, bijouterie - Dosage du palladium dans les alliages de palladium pour la joaillerie, bijouterie - Mthode par ICP-OES utilisant lyttrium comme talon interne (ISO 11495:2014) Schmuck - Bestimmung von Palla

9、dium in Palladiumschmucklegierungen - ICP-OES Verfahren unter Verwendung von Yttrium als Internem Standardelement (ISO 11495:2014) This European Standard was approved by CEN on 26 August 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions fo

10、r 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-CENELEC Management Centre or to any CEN member. This European Standard exists in thre

11、e 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-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bod

12、ies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, S

13、pain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwi

14、de for CEN national Members. Ref. No. EN ISO 11495:2016 EContents PageEuropean foreword .3Introduction 51 Scope . 62 Normative references 63 Terms and definitions . 64 Short description of method 65 Reagents 76 Equipment . 77 Sampling 78 Procedure. 78.1 Internal standard solution 78.2 Calibration so

15、lutions 88.3 Sample solutions . 88.4 Measurements . 88.5 Calculation and expression of results 99 Repeatability . 1210 Test report 12Bibliography . 13DIN EN ISO 11495:2016-12EN ISO 11495:2016 (E)2Foreword 4European foreword The text of ISO 11495:2014 has been prepared by Technical Committee ISO/TC 1

16、74 “Jewellery” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 11495:2016. 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 April 2017, and conflicting

17、 national standards shall be withdrawn at the latest by April 2017. 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. According to the C

18、EN-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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hung

19、ary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 11495:2014 has been approved by CEN as EN ISO 11495:2016 without any m

20、odification. DIN EN ISO 11495:2016-12EN ISO 11495:2016 (E)3 ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committ

21、ees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the Int

22、ernational Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the di

23、fferent types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO sh

24、all not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document

25、is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT

26、) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 174, Jewellery.This second edition cancels and replaces the first edition (ISO 11495:2008), which has been technically revised with the following changes:a) change in the scope that thi

27、s method is the referee method;b) addition of a warning in Clause 8 that suitable health and safety procedures should be followed;c) addition of a standard solution in 8.1;d) addition of an alternative calibration solution in 8.2.2;e) addition of an alternative sample solution in 8.3.2;f) addition o

28、f an alternative route for calculation in 8.5.4;g) International Standard editorially revised.DIN EN ISO 11495:2016-12EN ISO 11495:2016 (E)4 IntroductionThe following definitions apply in understanding how to implement an ISO International Standard and other normative ISO deliverables (TS, PAS, IWA)

29、: “shall” indicates a requirement; “should” indicates a recommendation; “may” is used to indicate that something is permitted; “can” is used to indicate that something is possible, for example, that an organization or individual is able to do something.ISO/IEC Directives, Part 2 (sixth edition, 2011

30、), 3.3.1 defines a requirement as an “expression in the content of a document conveying criteria to be fulfilled if compliance with the document is to be claimed and from which no deviation is permitted.”ISO/IEC Directives, Part 2 (sixth edition, 2011), 3.3.2 defines a recommendation as an “expressi

31、on in the content of a document conveying that among several possibilities one is recommended as particularly suitable, without mentioning or excluding others, or that a certain course of action is preferred but not necessarily required, or that (in the negative form) a certain possibility or course

32、 of action is deprecated but not prohibited.”DIN EN ISO 11495:2016-12EN ISO 11495:2016 (E)5 1 ScopeThis International Standard describes a method for the determination of palladium in palladium jewellery alloys, preferably within the range of fineness specified in ISO 9202, by means of inductively c

33、oupled plasma optical emission spectrometry (ICP-OES).The preferred palladium content of the alloys lies between 500 (parts per thousand) and 950 palladium.NOTE This method can be used to analyse other contents of palladium.This method is intended to be used as the recommended method for the determi

34、nation of fineness in alloys covered by ISO 9202.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition

35、 of the referenced document (including any amendments) applies.ISO 11596, Jewellery Sampling of precious metal alloys for and in jewellery and associated products3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1bracketingrunning of standards and

36、samples in the following sequence: low standard sample high standard sample low standard sample high standard sample low standard sample high standard4 Short description of methodAt least two accurately weighed samples are dissolved in aqua regia and made up to an exactly weighed mass. Exactly weigh

37、ed portions (aliquots) of these sample solutions are mixed with the internal standard and made up to the standard measuring volume.Using ICP-OES, the palladium content of the sample solution is measured by comparison of the ratio intensities of the spectral emission of palladium (recommended line is

38、 340,45 nm) and yttrium (at 371,03 nm) or other appropriate lines, with the ratios for solutions containing known masses of palladium and yttrium, using the bracketing method.Other palladium emission lines may be used, but have to be checked for spectral interferences and the instrumental performanc

39、e.DIN EN ISO 11495:2016-12EN ISO 11495:2016 (E)6 5 ReagentsDuring the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. All reagents shall be palladium free.5.1 Hydrochloric acid (HCl), approximately 30 % to 37

40、 % HCl (mass fraction).5.2 Nitric acid (HNO3), approximately 65 % to 70 % HNO3(mass fraction).5.3 Pure palladium (Pd).The palladium content shall be at least 999,9 . If a lower palladium content (999,5 ) is used, appropriate corrections could be applied.5.4 Internal standard.An yttrium compound like

41、 yttrium chloride (YCl3 6H2O) or yttrium oxide (Y2O3) in analytical grade.5.5 Aqua regia.Mix 3 volumes of hydrochloric acid (5.1) and 1 volume of nitric acid (5.2).6 Equipment6.1 Customary laboratory apparatus.6.2 ICP-OES, capable of simultaneously measuring the palladium emission line and the emiss

42、ion line of the internal standard yttrium with a minimum optical resolution of 0,02 nm.6.3 Analytical balance, with a reading accuracy of 0,01 mg.7 SamplingThe sampling procedure shall be performed in accordance with ISO 11596.8 ProcedureWARNING Suitable health and safety procedures should be follow

43、ed.8.1 Internal standard solutionDissolve approximately 680 mg YCl3 6H2O (5.4) in 200 ml water and make up to 1 000 ml with water. Alternatively, dissolve approximately 250 mg Y2O3in a mixture of 25 ml water and 25 ml nitric acid and make up to 1 000 ml with water. Due to the sensitivity of the inst

44、rument, the concentration may be changed to achieve optimum performance.This also applies to the calibration solutions (see 8.2) and the sample solutions (see 8.3).DIN EN ISO 11495:2016-12EN ISO 11495:2016 (E)7 8.2 Calibration solutions8.2.1 Weigh approximately 100 mg of palladium accurately to 0,01

45、 mg into a tared 100 ml volumetric flask and add 40 ml of aqua regia (5.5). Heat gently until complete dissolution of the sample. Allow to cool. Make up with water to 100 ml and mix thoroughly. Weigh this palladium stock-solution.Weigh approximately 4,5 g, 5,5 g, 6,5 g, 7,5 g, 8,5 g, 9,5 g, and 9,8

46、g of the palladium stock solution accurately to at least 0,001 g, each into a 100 ml volumetric flask. Add 10 g of the internal standard solution (8.1) accurate to at least 0,001 g. Add 10 ml HCl (5.1) and make up to 100 ml with water. Mix thoroughly.In the presence of certain other elements (e.g. s

47、ilver), it can be necessary to increase the HCl concentration to a maximum of 50 ml. The acid concentration of calibration solutions and sample solutions shall be consistent.8.2.2 Alternatively weigh 45 mg, 55 mg, 65 mg, 75 mg, 85 mg, 95 mg, and 98 mg palladium accurately to 0,01 mg each into a 1 l

48、flask and dissolve in 100 ml HCl (5.1) plus 30 ml HNO3 (5.2). Add 100 g accurately to 0,01 g of the internal standard solution (8.1). Add 100 ml HCl (5.2) and make up to 1 l with water. Mix thoroughly.In the presence of certain other elements (e.g. silver), it can be necessary to increase the HCl concentration to a maximum of 500 ml. The acid concentra