BS EN ISO 11210-2016 Jewellery Determination of platinum in platinum jewellery alloys Gravimetric method after precipitation of diammonium hexachloroplatinate《珠宝 铂珠宝合金中铂的测定 二铵六氯铂沉淀.pdf

1、BS EN ISO 11210:2016Jewellery Determinationof platinum in platinumjewellery alloys Gravimetric method afterprecipitation of diammoniumhexachloroplatinate(ISO 11210:2014)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 11210:2016 BRITISH STANDARDNational fore

2、wordThis British Standard is the UK implementation of EN ISO11210:2016. It is identical to ISO 11210:2014. It supersedesBS EN ISO 11210:1995 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee STI/53, Specifications and test methods for jewellery andhorolog

3、y.A list of organizations represented on this committee can beobtained on request to its secretary.This 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 Standar

4、ds Limited 2016ISBN 978 0 580 96189 2ICS 39.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 October 2016.Amendments/corrigenda issued since publicationDate T

5、 e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11210 October 2016 ICS 39.060 Supersedes EN ISO 11210:1995English Version Jewellery - Determination of platinum in platinum jewellery alloys - Gravimetric method after precipitation of diammonium hexachloroplatinate (ISO

6、11210:2014) Joaillerie, bijouterie - Dosage du platine dans les alliages de platine pour la bijouterie-joaillerie - Mthode gravimtrique aprs prcipitation de lhexachloroplatinate de diammonium (ISO 11210:2014) Schmuck - Bestimmung von Platin in Platin-Schmucklegierungen - Gravimetrische Bestimmung du

7、rch Fllung als Diammoniumhexachloroplatinat (ISO 11210:2014) 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 11210:2016 EBS EN ISO 112

12、10:2016EN ISO 11210:2016 (E) 3 European foreword The text of ISO 11210:2014 has been prepared by Technical Committee ISO/TC 174 “Jewellery” of theInternational Organization for Standardization (ISO) and has been taken over as EN ISO 11210:2016. This European Standard shall be given the status of a n

13、ational standard, either by publication of anidentical text or by endorsement, at the latest by April 2017, and conflicting national standards shall bewithdrawn at the latest by April 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject ofpatent r

14、ights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patentrights. This document supersedes EN ISO 11210:1995. According to the CEN-CENELEC Internal Regulations, the national standards organizations of thefollowing countries are bound to implement this European Sta

15、ndard: 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, Spai

16、n, 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. BS EN ISO 11210:2016ISO 11210:2014(E)Contents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Rea

17、gents 15 Apparatus . 26 Sampling 27 Procedure. 27.1 Platinum jewellery alloys with less than 5 % iridium, rhodium, ruthenium, or tungsten 27.2 Platinum jewellery alloys with more than 5 % iridium, rhodium, or ruthenium, or more than 0,5 % gold 38 Methods of calculation and expression of results 38.1

18、 Calculation 38.2 Repeatability . 49 Test report . 4Annex A (informative) Reduction apparatus according to Rose 5Bibliography 6 ISO 2014 All rights reserved iiiBS EN ISO 11210:2016ISO 11210:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national

19、standards bodies (ISO member bodies). The work of preparing International Standards is normally 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

20、 organizations, governmental and non-governmental, in liaison with ISO, also take part in 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

21、 its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the 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

22、/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 responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be i

23、n 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 given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions re

24、lated to conformity assessment, as well as information about ISOs adherence to the WTO principles 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

25、replaces the first edition (ISO 11210:1995), which has been technically revised with the following changes: addition of an analytical balance in Clause 5; 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 all

26、ow drying of the crucibles in a programmable furnace; deletion of the temperature for reduction in 7.1; International Standard editorially revised.iv ISO 2014 All rights reservedBS EN ISO 11210:2016ISO 11210:2014(E)IntroductionThe following definitions apply in understanding how to implement an ISO

27、International Standard and 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

28、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 fulfilled if compliance with the document is to be claimed and from which no deviation is permitted.”ISO/IEC Directives, Part 2

29、 (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 particularly suitable, without mentioning or excluding others, or that a certain course of action is preferred but not necessarily r

30、equired, or that (in the negative form) a certain possibility or course of action is deprecated but not prohibited.” ISO 2014 All rights reserved vBS EN ISO 11210:2016BS EN ISO 11210:2016Jewellery Determination of platinum in platinum jewellery alloys Gravimetric method after precipitation of diammo

31、nium hexachloroplatinate1 ScopeThis 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,

32、gallium, chromium, indium, and less 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 appl

33、ication. 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 associated products3 PrincipleThe sample is dissolve

34、d in aqua regia. After converting the 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

35、example, an atomic absorption spectrometer (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

36、 purity.4.1 Hydrochloric acid (HCI), 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

37、hydrogen or a hydrogen/nitrogen mixture.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).INTERNATIONAL STANDARD ISO 11210:2014(E) ISO 2014 All rights reserved 1BS EN ISO 11210:2016ISO 11210:2014(E)5 App

38、aratus5.1 Ordinary laboratory apparatus.5.2 Reduction apparatus, see Figure A.1.5.3 AAS or ICP-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 ac

39、curacy of 0,01 mg.6 SamplingThe sampling procedure shall be performed in accordance with ISO 11596.7 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 approxim

40、ately 250 mg to 300 mg of platinum, accurately to the nearest 0,01 mg, and transfer it to a 100 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 remai

41、ning after this procedure shall be filtered off at this stage and its composition established for 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

42、 (4.2) before recommencing evaporation.If this temperature is exceeded, the platinum can be reduced 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

43、(4.2) and add 4 ml of water. Add 40 ml of saturated ammonium chloride solution (4.4) at (85 5) 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

44、 continue until hydrogen chloride is no longer emitted. Allow to cool. Add just sufficient water 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)

45、. Thoroughly wash the precipitate with ammonium chloride solution. Wipe the glass beaker and watch 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,

46、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 adjusted or in a programmable furnace. By drying initially at 50 C

47、to 70 C and heating subsequently to 340 C, all ammonium chloride is lost. Ash the filter paper (5.5) and (NH4)2PtCI6 residue at a temperature of 500 C to 600 C without a flame. Finally, remove the cover of the crucible and calcine in a muffle furnace 2 ISO 2014 All rights reservedBS EN ISO 11210:201

48、6ISO 11210:2014(E)(5.4) for 1 h to 3 h at a temperature of 900 C to 1 000 C. To ensure complete decomposition, the solid in the crucible might need breaking into several pieces during calcination.NOTE The ammonium chloride decomposes at 340 C.Significant absorption of oxygen can take place during ig

49、nition if palladium, iridium, ruthenium, rhodium, or copper are present in the platinum sponge. Oxidation can be avoided by calcining under reducing gas (4.5) followed by cooling under inert or reducing gas (4.6).Weigh the platinum sponge obtained.Measure the co precipitated elements by suitable means such as AAS or ICP-OES (5.3).7.2 Platinum jewellery alloys with more than 5 % iridium, rhodium, or ruthenium, or more than 0,5 % goldThe procedure described results in the complete precipitation of the platinum in t