DIN EN ISO 11494-2016 Jewellery - Determination of platinum in platinum jewellery alloys - ICP-OES method using yttrium as internal standard element (ISO 11494 2014) German version.pdf

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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!%“2599188www.din.deDIN E

2、N ISO 11494Jewellery Determination of platinum in platinum jewellery alloys ICPOES method using yttrium as internal standard element (ISO 11494:2014);English version EN ISO 11494:2016,English translation of DIN EN ISO 11494:2016-12Schmuck Bestimmung von Platin in Platinschmucklegierungen ICPOESVerfa

3、hren unter Verwendung von Yttrium als Internem Standardelement (ISO 11494:2014);Englische Fassung EN ISO 11494:2016,Englische bersetzung von DIN EN ISO 11494:2016-12Joaillerie, bijouterie Dosage du platine dans les alliages de platine pour la joaillerie, bijouterie Mthode par ICPOES utilisant lyttri

4、um comme talon interne (ISO 11494:2014);Version anglaise EN ISO 11494:2016,Traduction anglaise de DIN EN ISO 11494:2016-12www.beuth.deDocument comprises 15 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.12.16 DIN EN ISO 11494:

5、2016-12 2 A comma is used as the decimal marker. National foreword The text of ISO 11494:2014 has been prepared by Technical Committee ISO/TC 174 “Jewellery (Secretariat: DIN, Germany) and has been taken over as EN ISO 11494:2016 according to the decision CEN/BT C137/2015. The responsible German bod

6、y 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 follows: ISO 9202

7、 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 11494 October 2016 ICS 39.060 English Version Jewellery - Determination of platinum in platinum jewellery alloys - ICP-O

8、ES method using yttrium as internal standard element (ISO 11494:2014) Joaillerie, bijouterie - Dosage du platine dans les alliages de platine pour la joaillerie, bijouterie - Mthode par ICP-OES utilisant lyttrium comme talon interne (ISO 11494:2014) Schmuck - Bestimmung von Platin in Platinschmuckle

9、gierungen - ICP-OES Verfahren unter Verwendung von Yttrium als Internem Standardelement (ISO 11494:2014) 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 for giving this European Sta

10、ndard 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 three official versions (Engli

11、sh, 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 bodies of Austria, Belgium, B

12、ulgaria, 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, Spain, Sweden, Switzerland,

13、 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 worldwide for CEN national Member

14、s. Ref. No. EN ISO 11494:2016 EContents PageForeword .4Introduction 51 Scope . 62 Normative references 63 Terms and definitions . 64 Principle 65 Reagents 66 Equipment . 77 Sampling 78 Procedure. 78.1 Internal standard solution 78.2 Calibration solutions 88.3 Sample solution 88.4 Preparation of the

15、platinum alloy solution containing ruthenium, iridium, or tungsten 88.5 Measurements . 88.6 Calculation and expression of results 99 Repeatability .1210 Test report 12Bibliography .13EN ISO 11494:2016 (E) DIN EN ISO 11494:2016-12 2European foreword .3European foreword The text of ISO 11494:2014 has

16、been prepared by Technical Committee ISO/TC 174 “Jewellery” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 11494:2016. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement,

17、 at the latest by April 2017, and conflicting 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

18、or all such patent rights. 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, Former Yugoslav Republi

19、c of Macedonia, France, Germany, Greece, Hungary, 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 11494:2014 has been appro

20、ved by CEN as EN ISO 11494:2016 without any modification. EN ISO 11494:2016 (E) DIN EN ISO 11494:2016-12 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 nor

21、mally carried out through ISO technical committees. 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

22、the work. ISO collaborates closely with the International 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 th

23、e different approval criteria needed for the different 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 docum

24、ent may be the subject of patent rights. ISO shall 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

25、/patents).Any trade name used in this document 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 pri

26、nciples in the Technical Barriers to Trade (TBT), see the following URL: Foreword Supplementary information .The committee responsible for this document is ISO/TC 174, Jewellery.This second edition cancels and replaces the first edition (ISO 11494:2008), which has been technically revised with the f

27、ollowing changes:a) change in the scope that this 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 al

28、ternative sample solution in 8.3.2;f) addition of an alternative route for calculation in 8.6.4;g) International Standard editorially revised.EN ISO 11494:2016 (E) DIN EN ISO 11494:2016-12 4 IntroductionThe following definitions apply in understanding how to implement an ISO International Standard a

29、nd other normative ISO deliverables (TS, PAS, IWA): “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 somethi

30、ng.ISO/IEC Directives, Part 2 (sixth edition, 2011), 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, 201

31、1), 3.3.2 defines a recommendation as an “expression 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

32、the negative form) a certain possibility or course of action is deprecated but not prohibited.”EN ISO 11494:2016 (E) DIN EN ISO 11494:2016-12 5 1 ScopeThis International Standard describes a method for the determination of platinum in platinum jewellery alloys, preferably within the range of finenes

33、s specified in ISO 9202, by means of inductively coupled plasma optical emission spectrometry (ICP-OES).This method applies to platinum jewellery alloys that might contain silver, indium, iridium, gallium, copper, cobalt, nickel, tin, and ruthenium. However, this list is not exhaustive and care is a

34、lways to be taken to investigate potential interference effects.This method is intended to be used as the recommended method for the determination of fineness in alloys covered by ISO 9202 up to 990 .2 Normative referencesThe following documents, in whole or in part, are normatively referenced in th

35、is document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 11596, Jewellery Sampling of precious metal alloys for and in jewellery and associ

36、ated products3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1bracketingrunning of standards and samples in the following sequence: low standard sample high standard sample low standard sample high standard sample low standard sample high standar

37、d4 PrincipleAt least two accurately weighed samples are dissolved in aqua regia and made up to an exactly weighed mass. Exactly weighed portions (aliquots) of these sample solutions are mixed with the internal standard and made up to the standard measuring volume.Using ICP-OES, the platinum content

38、of the sample solution is measured by comparison of the ratio intensities of the spectral emission of platinum (recommended lines are 265,95 nm, 214,42 nm, 299,80 nm, or 306,47 nm) and appropriate yttrium lines with the ratios for solutions containing known masses of platinum and yttrium using the b

39、racketing method.Minor modifications are required when the alloy contains ruthenium, rhodium, iridium, or tungsten.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 pl

40、atinum free.EN ISO 11494:2016 (E) DIN EN ISO 11494:2016-12 6 5.1 Hydrochloric acid (HCl), approximately 30 % to 37 % HCl (mass fraction).5.2 Nitric acid (HNO3), approximately 65 % to 70 % HNO3(mass fraction).5.3 Pure platinum (Pt).The platinum content shall be at least 999,9 . If a lower platinum co

41、ntent (999,5 ) is used, appropriate corrections should be applied.5.4 Internal standard, an yttrium compound like yttrium chloride (YCl3 6H2O) or yttrium oxide (Y2O3) in analytical grade.5.5 Pure copper.Copper content shall be 999,9 . and platinum free.5.6 Orthophosphoric acid (H3PO4), 85 % (mass fr

42、action).5.7 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 ICPOES, capable of simultaneously measuring the platinum emission and the emission line of the internal standard yttrium, with a minimum optical resolut

43、ion 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 followed.8.1 Internal standard solutionDissolve approximately 680 mg YCl36H2O

44、(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 instrument, the concentration may be changed to achieve optimum performance.T

45、his also applies to the calibration solutions (see 8.2) and the sample solutions (see 8.3).EN ISO 11494:2016 (E) DIN EN ISO 11494:2016-12 7 8.2 Calibration solutions8.2.1 Weigh approximately 100 mg of platinum accurately to 0,01 mg into a tared 100 ml volumetric flask and add 40 ml of aqua regia (5.

46、7). Heat gently until dissolution of the sample is complete. Allow to cool. Make up with water to 100 ml and mix thoroughly. Weigh this platinum stock solution.Weigh approximately 4,5 g, 5,5 g, 6,5 g, 7,5 g, 8,25 g, 8,5 g, 8,75 g, 9,25 g, 9,5 g, and 9,75 g of the platinum stock solution accurately t

47、o at least 0,001 g, each into a 100 ml volumetric flask. Add 10 g of the internal standard solution (8.1) accurately to at least 0,001 g. Add 10 ml of HCl (5.1) and make up to 100 ml with water. Mix thoroughly.In the presence of certain other elements (e.g. silver), it can be necessary to increase t

48、he 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, 82,5 mg, 85 mg, 87,5 mg, 92,5 mg, 95 mg, and 97,5 mg platinum accurately to 0,01 mg each into a 1 000 ml flask and dissolve in a mixture of 100 ml HCl (5.1) and 30 m