DIN EN ISO 11210-2016 Jewellery - Determination of platinum in platinum jewellery alloys - Gravimetric method after precipitation of diammonium hexachloroplatinate (ISO 11210 2014).pdf

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1、December 2016 English price group 9No 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!%w“2599184www.din.deDIN E

2、N ISO 11210Jewellery Determination of platinum in platinum jewellery alloys Gravimetric method after precipitation of diammonium hexachloroplatinate (ISO 11210:2014);English version EN ISO 11210:2016,English translation of DIN EN ISO 11210:2016-12Schmuck Bestimmung von Platin in PlatinSchmucklegieru

3、ngen Gravimetrische Bestimmung durch Fllung als Diammoniumhexachloroplatinat (ISO 11210:2014);Englische Fassung EN ISO 11210:2016,Englische bersetzung von DIN EN ISO 11210:2016-12Joaillerie, bijouterie Dosage du platine dans les alliages de platine pour la bijouteriejoaillerie Mthode gravimtrique ap

4、rs prcipitation de lhexachloroplatinate de diammonium (ISO 11210:2014);Version anglaise EN ISO 11210:2016,Traduction anglaise de DIN EN ISO 11210:2016-12SupersedesDIN EN ISO 11210:199508www.beuth.deDocument comprises 13 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language or

5、iginal shall be considered authoritative.12.16 DIN EN ISO 11210:2016-12 2 A comma is used as the decimal marker. National foreword The text of ISO 11210:2014 has been prepared by Technical Committee ISO/TC 174 “Jewellery” (Secretariat: DIN, Germany) and has been taken over as EN ISO 11210:2016 accor

6、ding to the decision CEN/BT C137/2015. The responsible 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. Amendments This standard differs from DIN EN ISO

7、 11210:1995-08 as follows: a) an analytical balance has been added in Clause 5; b) the requirement for sampling has been modified in Clause 6; c) in Subclause 7.1, dissolution in a sealed container under pressure is now permitted; d) in Subclause 7.1, drying of the crucibles in a programmable furnac

8、e is now permitted; e) in Subclause 7.1, the temperature for reduction has been deleted; f) the International Standard has been editorially revised. Previous editions DIN EN ISO 11210: 1995-08 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11210 October 2016 ICS 39.060 Supersedes EN ISO 11

9、210:1995English Version Jewellery - Determination of platinum in platinum jewellery alloys - Gravimetric method after precipitation of diammonium hexachloroplatinate (ISO 11210:2014) Joaillerie, bijouterie - Dosage du platine dans les alliages de platine pour la bijouterie-joaillerie - Mthode gravim

10、trique aprs prcipitation de lhexachloroplatinate de diammonium(ISO 11210:2014) Schmuck - Bestimmung von Platin in Platin-Schmucklegierungen - Gravimetrische Bestimmung durch Fllung als Diammoniumhexachloroplatinat(ISO 11210:2014) This European Standard was approved by CEN on 26 August 2016. CEN memb

11、ers 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 applicati

12、on 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 language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Managem

13、ent 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

14、Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17

15、, 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 11210:2016 EContents PageEuropean foreword .3Introduction 51 Scope . 62 Normative references 63 Principle 64 Reagents 65 Apparatus . 76 Sampling 77 Procedur

16、e. 77.1 Platinum jewellery alloys with less than 5 % iridium, rhodium, ruthenium, or tungsten 77.2 Platinum jewellery alloys with more than 5 % iridium, rhodium, or ruthenium, or more than 0,5 % gold 88 Methods of calculation and expression of results 88.1 Calculation 88.2 Repeatability . 99 Test re

17、port . 9Annex A (informative) Reduction apparatus according to Rose 10Bibliography 11DIN EN ISO 11210:2016-12 EN ISO 11210:2016 (E)2Foreword .4European foreword The text of ISO 11210:2014 has been prepared by Technical Committee ISO/TC 174 “Jewellery” of the International Organization for Standardiz

18、ation (ISO) and has been taken over as EN ISO 11210:2016. 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 national standards shall be withdrawn at the latest by April 2

19、017. 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. This document supersedes EN ISO 11210:1995. According to the CEN-CENELEC Internal

20、 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, Hungary, Iceland, Irela

21、nd, 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 11210:2014 has been approved by CEN as EN ISO 11210:2016 without any modification. DIN EN

22、 ISO 11210:2016-12 EN ISO 11210:2016 (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 committees. Each member b

23、ody 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 International Electro

24、technical 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 different types of I

25、SO 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 shall not be held re

26、sponsible 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 is information giv

27、en 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), see the followi

28、ng 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 11210:1995), which has been technically revised with the following changes: addition of an analytical balance in Clause 5;

29、change of requirement for sampling in Clause 6; addition in 7.1 to allow dissolution in a sealed container under pressure; addition in 7.1 to allow drying of the crucibles in a programmable furnace; deletion of the temperature for reduction in 7.1; International Standard editorially revised.DIN EN I

30、SO 11210:2016-12 EN ISO 11210:2016 (E)4 IntroductionThe following definitions apply in understanding how to implement an ISO International Standard and other normative ISO deliverables (TS, PAS, IWA). “shall” indicates a requirement “should” indicates a recommendation “may” is used to indicate that

31、something is permitted “can” is used to indicate that something is possible, for example, that an organization or individual is able to do somethingISO/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 fu

32、lfilled 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 “expression in the content of a document conveying that among several possibilities, one is recommended as particu

33、larly 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 of action is deprecated but not prohibited.”DIN EN ISO 11210:2016-12 EN ISO 11210:2016 (E)5 1 ScopeThis

34、 International Standard specifies a gravimetric method for the determination of platinum in platinum jewellery alloys, preferably within the range of fineness stated in ISO 9202.These alloys can contain palladium, iridium, rhodium, copper, cobalt, gold, ruthenium, gallium, chromium, indium, and less

35、 than 5 % tungsten. Some modifications are indicated where palladium, iridium, rhodium, gold, or ruthenium are present.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

36、 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 associated products3 PrincipleThe sample is dissolved in aqua regia. After converting t

37、he sample solution to a slightly acid medium, the platinum is precipitated as diammonium hexachloroplatinate. The precipitate is converted to metallic platinum. Coprecipitated alloying elements are tested in the re-dissolved platinum sponge and measured using, for example, an atomic absorption spect

38、rometer (AAS) or an inductively coupled plasma optical emission spectrometer (ICP-OES), and a correction applied.4 ReagentsDuring the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity.4.1 Hydrochloric acid (HCI)

39、, approximately 30 % to 37 % HCI (mass fraction).4.2 Dilute hydrochloric acid, 18 % HCl (mass fraction).4.3 Nitric acid (HNO3), approximately 65 % to 69 % HNO3(mass fraction).4.4 Ammonium chloride solution (NH4CI), cold saturated solution.4.5 Reducing gas, such as hydrogen or a hydrogen/nitrogen mix

40、ture.4.6 Inert gas, such as carbon dioxide or nitrogen.4.7 Aqua regia, mix three volumes of hydrochloric acid (4.1) and one volume of nitric acid (4.3).DIN EN ISO 11210:2016-12 EN ISO 11210:2016 (E)6 5 Apparatus5.1 Ordinary laboratory apparatus.5.2 Reduction apparatus, see Figure A.1.5.3 AAS or ICP-

41、OES, capable of determining traces of metals.5.4 Muffle furnace, capable of attaining at least 1 000 C.5.5 Ashless filter paper, capable of retaining 3 m particles.5.6 Analytical balance, with a reading accuracy of 0,01 mg.6 SamplingThe sampling procedure shall be performed in accordance with ISO 11

42、596.7 ProcedureWARNING Suitable health and safety procedures should be followed.7.1 Platinum jewellery alloys with less than 5 % iridium, rhodium, ruthenium, or tungstenWeigh the sample containing approximately 250 mg to 300 mg of platinum, accurately to the nearest 0,01 mg, and transfer it to a 100

43、 ml glass beaker. Dissolve the sample in 20 ml of aqua regia (4.7) in the glass beaker covered with a watch glass, while heating gently, or in a sealed container under pressure.Any insoluble material remaining after this procedure shall be filtered off at this stage and its composition established f

44、or possible correction of the results.Evaporate the solution five times without letting the residue become dry and without exceeding a temperature of 90 C, each time adding 2 ml of dilute hydrochloric acid (4.2) before recommencing evaporation.If this temperature is exceeded, the platinum can be red

45、uced to Pt(ii) or even Pt(i) and require re-oxidation with approximately 0,1 ml of nitric acid (4.3). After the last evaporation, dissolve the still moist platinum salt in 1 ml of dilute hydrochloric acid (4.2) and add 4 ml of water. Add 40 ml of saturated ammonium chloride solution (4.4) at (85 5)

46、C to this clear solution. The platinum is precipitated as yellow (NH4)2PtCI6.The solution with the precipitated (NH4)2PtCI6 is evaporated almost to dryness at this temperature. Further gentle heating shall continue until hydrogen chloride is no longer emitted. Allow to cool. Add just sufficient wate

47、r while agitating to dissolve the residual ammonium chloride crystals.Immediately filter the (NH4)2PtCI6 precipitate over a filter paper (5.5) which has been moistened with ammonium chloride solution (4.4). Thoroughly wash the precipitate with ammonium chloride solution. Wipe the glass beaker and wa

48、tch glass with a second filter paper. Check the filtrate for residual platinum by suitable means, such as an AAS or ICP-OES (5.2) .The filter paper containing the precipitate is folded into the second one, transferred to a porcelain crucible and covered with a thin layer (2 mm) of ammonium chloride. This crucible is then placed inside a covered crucible. Cautiously dry the contents of the crucibles on a hotplate which can be gradually