EN ISO 11494-2016 en Jewellery - Determination of platinum in platinum jewellery alloys - ICP-OES method using yttrium as internal standard element《珠宝首饰-铂合金首饰中使用钇作为内标元素ICP-OES法测定铂(.pdf

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1、BS EN ISO 11494:2016Jewellery Determination ofplatinum in platinum jewelleryalloys ICP-OES method usingyttrium as internal standardelement (ISO 11494:2014)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 11494:2016 BRITISH STANDARDNational forewordThis Briti

2、sh Standard is the UK implementation of EN ISO 11494:2016.The UK participation in its preparation was entrusted to TechnicalCommittee STI/53, Specifications and test methods for jewellery andhorology.A list of organizations represented on this committee can beobtained on request to its secretary.Thi

3、s publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016. Published by BSI StandardsLimited 2016ISBN 978 0 580 93671 5ICS 39.060Compliance with a British Standard cannot confer immuni

4、ty fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 November 2014.Amendments/corrigenda issued since publicationDate Text affectedThis corrigendum renumbers BS ISO 11494:201431 October 2016as BS EN ISO 11494:2016which i

5、s withdrawn.It is identical to ISO 11494:2014. It supersedes BS ISO 11494:2014 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-OES method using yttrium as internal standard

6、 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 Platinschmucklegierungen - ICP-OES Verfahren unter Verwendu

7、ng 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 Standard the status of a national standard with

8、out 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 (English, French, German). A version in any other

9、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, Bulgaria, Croatia, Cyprus, Czech Republic, De

10、nmark, 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, Turkey andUnited Kingdom. EUROPEAN COMMITTE

11、E 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 Members. Ref. No. EN ISO 11494:2016 EEN ISO 11494:

12、2016 (E) European foreword The text of ISO 11494:2014 has 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, eit

13、her by publication of an identical text or by endorsement, 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

14、CENELEC shall not be held responsible for identifying any 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 Re

15、public, 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, Turkey and the United Kingdom. En

16、dorsement notice The text of ISO 11494:2014 has been approved by CEN as EN ISO 11494:2016 without any modification. iiBS EN ISO 11494:2016ISO 11494:2014(E)Contents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Reagents 16 Equipment . 27 Sam

17、pling 28 Procedure. 28.1 Internal standard solution 28.2 Calibration solutions 38.3 Sample solution 38.4 Preparation of the platinum alloy solution containing ruthenium, iridium, or tungsten 38.5 Measurements . 38.6 Calculation and expression of results 49 Repeatability 710 Test report . 7Bibliograp

18、hy 8 ISO 2014 All rights reserved iiiBS EN ISO 11494:2016ISO 11494:2014(E)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 tec

19、hnical 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 the work. ISO collaborates closel

20、y 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 the different approval criteria nee

21、ded 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 document may be the subject of patent

22、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/patents).Any trade name used in

23、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 principles in the Technical Barriers

24、 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 following changes:a) change in the

25、 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 alternative sample solution in 8.3.

26、2;f) addition of an alternative route for calculation in 8.6.4;g) International Standard editorially revised.iv ISO 2014 All rights reservedBS EN ISO 11494:2016ISO 11494:2014(E)IntroductionThe following definitions apply in understanding how to implement an ISO International Standard and other norma

27、tive 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 something.ISO/IEC Dir

28、ectives, 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, 2011), 3.3.2 defi

29、nes 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 the negative f

30、orm) a certain possibility or course of action is deprecated but not prohibited.” ISO 2014 All rights reserved vBS EN ISO 11494:2016BS EN ISO 11494:2016Jewellery Determination of platinum in platinum jewellery alloys ICP-OES method using yttrium as internal standard element1 ScopeThis International

31、Standard describes a method for the determination of platinum in platinum jewellery alloys, preferably within the range of fineness specified in ISO 9202, by means of inductively coupled plasma optical emission spectrometry (ICP-OES).This method applies to platinum jewellery alloys that might contai

32、n silver, indium, iridium, gallium, copper, cobalt, nickel, tin, and ruthenium. However, this list is not exhaustive and care is always 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 c

33、overed by ISO 9202 up to 990 .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 of the referenced

34、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 samples in the foll

35、owing sequence: low standard sample high standard sample low standard sample high standard sample low standard sample high standard4 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 sampl

36、e solutions are mixed with the internal standard and made up to the standard measuring volume.Using ICP-OES, the platinum content 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

37、306,47 nm) and appropriate yttrium lines with the ratios for solutions containing known masses of platinum and yttrium using the bracketing method.Minor modifications are required when the alloy contains ruthenium, rhodium, iridium, or tungsten.5 ReagentsDuring the analysis, unless otherwise stated,

38、 use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. All reagents shall be platinum free.INTERNATIONAL STANDARD ISO 11494:2014(E) ISO 2014 All rights reserved 1BS EN ISO 11494:2016ISO 11494:2014(E)5.1 Hydrochloric acid (HCl), approximately 30 % to

39、 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 content (999,5 ) is used, appropriate corrections should be applied.5.4 Internal standard, an yttrium compound li

40、ke 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 fraction).5.7 Aqua regia.Mix 3 volumes of hydrochloric acid (5.1) and 1 volume of nitric acid (5.2).6 Equipment6.

41、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 resolution of 0,02 nm.6.3 Analytical balance, with a reading accuracy of 0,01 mg.7 SamplingThe sampling procedure shal

42、l 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 (5.4) in 200 ml water and make up to 1 000 ml with water. Alternatively, dissolve approximately 250 mg Y2O3in a

43、 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.This also applies to the calibration solutions (see 8.2) and the sample solutions (see 8.3).2 ISO 2014 All right

44、s reservedBS EN ISO 11494:2016ISO 11494:2014(E)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 (5.7). Heat gently until dissolution of the sample is complete. Allow to cool. Make up with wate

45、r 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 to at least 0,001 g, each into a 100 ml volumetric flask. Add 10 g of the internal standard so

46、lution (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 the HCl concentration to a maximum of 50 ml. The acid concentration of calibration solutions a

47、nd 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 ml HNO3(5.2). Add 100 g accurately to 0,01

48、 g of the internal standard solution (8.1). Add 100 ml HCl (5.2) and make up to 1 000 ml 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 concentration of calibration solutions a

49、nd sample solutions shall be consistent.NOTE Depending on the range of the platinum contents in the samples, not all standards are necessary.8.3 Sample solution8.3.1 Weigh approximately 100 mg of the sample to the nearest 0,01 mg, dissolve and treat the sample as described in 8.2.1. Weigh approximately 10 g of this sample stock solution accurately to 0,001 g into a 100 ml volumetric flask and add 10 g of the internal standard solution (8.1) accurately to 0,001 g. Add 10 ml of HCl (5.1) and make up to 100 ml with wate