1、BS EN ISO 11495:2016Jewellery Determinationof palladium in palladiumjewellery alloys ICP-OESmethod using yttrium asinternal standard element(ISO 11495:2014)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 11495:2016 BRITISH STANDARDNational forewordThis Brit
2、ish Standard is the UK implementation of EN ISO 11495:2016.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.Th
3、is 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 93672 2ICS 39.060Compliance with a British Standard cannot confer immun
4、ity 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 11495:201430 November 2016as BS EN ISO 11495:2016It is
5、 identical to ISO 11495:2014. It supersedes BS ISO 11495:2014which is withdrawn.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11495 October 2016 ICS 39.060 English Version Jewellery - Determination of palladium in palladium jewellery alloys - ICP-OES method using yttrium as internal stand
6、ard 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 Palladium in Palladiumschmucklegierungen - ICP-OES Verfahren u
7、nter 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 for giving this European Standard the status of a national
8、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 (English, French, German). A version
9、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, Bulgaria, Croatia, Cyprus, Czech
10、 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, Turkey andUnited Kingdom. EURO
11、PEAN 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 Members. Ref. No. EN ISO 11495:2016 E
12、EN ISO 11495:2016 (E) European foreword The text of ISO 11495:2014 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 11495:2016. This European Standard shall be given the status of a national
13、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 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights
14、. CEN and/or 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, Cyp
15、rus, 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, Turkey and the Unite
16、d Kingdom. Endorsement notice The text of ISO 11495:2014 has been approved by CEN as EN ISO 11495:2016 without any modification. iiBS EN ISO 11495:2016ISO 11495:2014(E)Contents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Short description of method 15
17、 Reagents 26 Equipment . 27 Sampling 28 Procedure. 28.1 Internal standard solution 28.2 Calibration solutions 38.3 Sample solutions . 38.4 Measurements . 38.5 Calculation and expression of results 49 Repeatability 710 Test report . 7Bibliography 8 ISO 2014 All rights reserved iiiBS EN ISO 11495:2016
18、ISO 11495:2014(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 technical committees. Each member body interested in a subje
19、ct 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 Electrotechnical Commission (IEC
20、) 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 ISO documents should be no
21、ted. 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 responsible for identifying
22、 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 given for the convenience of
23、 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 following URL: Foreword - Supplem
24、entary 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 this method is the referee method;b) addition
25、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 of an alternative route for calculation in 8
26、.5.4;g) International Standard editorially revised.iv ISO 2014 All rights reservedBS EN ISO 11495:2016ISO 11495:2014(E)IntroductionThe following definitions apply in understanding how to implement an ISO International Standard and other normative ISO deliverables (TS, PAS, IWA): “shall” indicates a
27、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), 3.3.1 defines a req
28、uirement 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 “expression in the content of a
29、 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 of action is deprecat
30、ed but not prohibited.” ISO 2014 All rights reserved vBS EN ISO 11495:2016BS EN ISO 11495:2016Jewellery Determination of palladium in palladium jewellery alloys ICP-OES method using yttrium as internal standard element1 ScopeThis International Standard describes a method for the determination of pal
31、ladium in palladium jewellery alloys, preferably within the range of fineness specified in ISO 9202, by means of inductively coupled 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 c
32、an be used to analyse other contents of palladium.This method is intended to be used as the recommended method for the determination 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 indis
33、pensable 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 associated products3 Terms and
34、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 standard4 Short description of m
35、ethodAt 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 palladium content of the
36、 sample solution is measured by comparison of the ratio intensities of the spectral emission of palladium (recommended line is 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
37、.Other palladium emission lines may be used, but have to be checked for spectral interferences and the instrumental performance.INTERNATIONAL STANDARD ISO 11495:2014(E) ISO 2014 All rights reserved 1BS EN ISO 11495:2016ISO 11495:2014(E)5 ReagentsDuring the analysis, unless otherwise stated, use only
38、 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 % HCl (mass fraction).5.2 Nitric acid (HNO3), approximately 65 % to 70 % HNO3(mass fraction).5.3 Pure palladium
39、(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 yttrium chloride (YCl3 6H2O) or yttrium oxide (Y2O3) in analytical grade.5.5 Aqua regia.Mix 3 volumes of hydroch
40、loric 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 emission line of the internal standard yttrium with a minimum optical resolution of 0,02 nm.6.3 Analytical balance, wi
41、th 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 YCl3 6H2O (5.4) in 200 ml water and make up to 1 0
42、00 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.This also applies to the calibration solu
43、tions (see 8.2) and the sample solutions (see 8.3).2 ISO 2014 All rights reservedBS EN ISO 11495:2016ISO 11495:2014(E)8.2 Calibration solutions8.2.1 Weigh approximately 100 mg of palladium accurately to 0,01 mg into a tared 100 ml volumetric flask and add 40 ml of aqua regia (5.5). Heat gently until
44、 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 g of the palladium stock solution accurately to at least 0,001 g, each into a 100 ml volumetr
45、ic 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. silver), it can be necessary to increase the HCl concentration to a maximum of 50 ml. The acid
46、 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 flask and dissolve in 100 ml HCl (5.1) plus 30 ml HNO3 (5.2). Add 100 g accurately to 0,01 g
47、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 concentration of calibration solutions and sampl
48、e solutions shall be consistent.NOTE Depending on the range of the palladium contents in the samples, not all the standards are necessary.8.3 Sample solutions8.3.1 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 approximatel
49、y 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 HCl (5.1) and make up to 100 ml. 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 and sample solutions shall be consistent.8.3.2 Alternatively weigh 100 mg sample accurately to 0,01 mg into a 1 l fl
