DIN EN ISO 11490-2016 Jewellery - Determination of palladium in palladium jewellery alloys - Gravimetric determination with dimethylglyoxime (ISO 11490 2015) German version EN ISO .pdf

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!%z“2599187www.din.deDIN E

2、N ISO 11490Jewellery Determination of palladium in palladium jewellery alloys Gravimetric determination with dimethylglyoxime (ISO 11490:2015);English version EN ISO 11490:2016,English translation of DIN EN ISO 11490:2016-12Schmuck Bestimmung von Palladium in PalladiumSchmucklegierungen Gravimetrisc

3、he Bestimmung mit Dimethylglyoxim (ISO 11490:2015);Englische Fassung EN ISO 11490:2016,Englische bersetzung von DIN EN ISO 11490:2016-12Joaillerie Dosage du palladium dans les alliages de palladium pour la bijouteriejoaillerie Dosage gravimtrique par la dimthylglyoxime (ISO 11490:2015);Version angla

4、ise EN ISO 11490:2016,Traduction anglaise de DIN EN ISO 11490:2016-12SupersedesDIN EN ISO 11490:199508www.beuth.deDocument comprises 13 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.12.16 DIN EN ISO 11490:2016-12 2 A comma is

5、 used as the decimal marker. National foreword The text of ISO 11490:2015 has been prepared by Technical Committee ISO/TC 174 “Jewellery (Secretariat: DIN, Germany) and has been taken over as EN ISO 11490 according to the decision CEN/BT C137/2015. The responsible German body involved in its prepara

6、tion 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 DIN EN ISO 9202 Amendmen

7、ts This standard differs from DIN EN ISO 11490:1995-8 as follows: a) an analytical balance has been added in Clause 5; b) the requirement for sampling has been changed in Clause 6; c) a warning has been added in Clause 7 that suitable health and safety procedures should be followed; d) the standard

8、has been editorially revised. Previous editions DIN EN ISO 11490: 1995-08 National Annex NA (informative) Bibliography DIN EN ISO 9202, Jewellery Fineness of precious metal alloys EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11490 October 2016 ICS 39.060 Supersedes EN ISO 11490:1995Engli

9、sh Version Jewellery - Determination of palladium in palladium jewellery alloys - Gravimetric determination with dimethylglyoxime (ISO 11490:2015) Joaillerie - Dosage du palladium dans les alliages de palladium pour la bijouterie-joaillerie - Dosage gravimtrique par la dimthylglyoxime(ISO11490:2015)

10、 Schmuck - Bestimmung von Palladium in Palladium-Schmucklegierungen - Gravimetrische Bestimmung mit Dimethylglyoxim (ISO 11490:2015) 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

11、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 application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in th

12、ree 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 Management Centre has the same status as the official versions. CEN members are the national standards b

13、odies of 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,

14、 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, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved world

15、wide for CEN national Members. Ref. No. EN ISO 11490:2016 EContents PageForeword .4Introduction .51 Scope . 62 Normative references 63 Principle 64 Reagents 65 Apparatus . 76 Sampling 77 Procedure. 78 Calculation and expression of results . 88.1 Calculation 88.2 Repeatability . 99 Test report . 9Ann

16、ex A (informative) Reduction apparatus according to Rose .10Bibliography .11EN ISO 11490:2016 (E) DIN EN ISO 11490:2016-12 2European foreword .3European foreword The text of ISO 11490:2015 has been prepared by Technical Committee ISO/TC 174 “Jewellery” of the International Organization for Standardi

17、zation (ISO) and has been taken over as EN ISO 11490:2016. 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

18、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 or all such patent rights. This document supersedes EN ISO 11490:1995. According to the CEN-CENELEC Interna

19、l 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, Irel

20、and, 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 11490:2015 has been approved by CEN as EN ISO 11490:2016 without any modification. EN IS

21、O 11490:2016 (E) DIN EN ISO 11490:2016-12 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 normally carried out through ISO technical committees. Each member

22、 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 closely with the International Elect

23、rotechnical 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

24、 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 rights. ISO shall not be held

25、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 this document is information g

26、iven 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 follo

27、wing 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 11490:1995), which has been technically revised with the following changes:a) addition of an analytical balance in Clause

28、 5;b) change of requirement for sampling in Clause 6;c) addition of a warning in Clause 7 that suitable health and safety procedures should be followed;d) standard editorially revised.EN ISO 11490:2016 (E) DIN EN ISO 11490:2016-12 4 IntroductionThe following definitions apply in understanding how to

29、 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 something is permitted; “can” is used to indicate that something is possible, for example, that an organi

30、zation or individual is able to do something.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/

31、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 particularly suitable without mentioning or excluding others, or that a certain course of action is preferred,

32、 but not necessarily required, or that (in the negative form) a certain possibility or course of action is deprecated, but not prohibited.”EN ISO 11490:2016 (E) DIN EN ISO 11490:2016-12 5 1 ScopeThis International Standard specifies a gravimetric method for the determination of palladium in palladiu

33、m jewellery alloys, preferably within the range of fineness stated in ISO 9202.These alloys may contain silver, indium, gallium, copper, cobalt, nickel, tin, and ruthenium. Coprecipitated elements have to be determined by a suitable method and a correction applied.2 Normative referencesThe following

34、 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 document (including any amendments) applies.ISO 11596, Jewellery

35、Sampling of precious metal alloys for and in jewellery and associated products3 PrincipleThe sample is dissolved in aqua regia. Palladium is precipitated with dimethylglyoxime. If present, silver is separated as silver chloride. The palladium dimethylglyoxime compound is converted to metallic pallad

36、ium by ignition and the latter is then determined gravimetrically.4 Reagents4.1 During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity.4.2 Nitric acid (HNO3), approximately 65 % to 70 % HNO3(mass fraction)

37、.4.3 Hydrochloric acid (HCl), 30 % to 37 % HCl (mass fraction).4.4 Diluted hydrochloric acid, 8,5 % (mass fraction).4.5 Dimethylglyoxime solution.Dissolve 10 g of dimethylglyoxime in 1 000 ml of ethanol.4.6 Ammonium chloride.4.7 Diluted nitric acid, 1,39 %.Cautiously add 10 ml of nitric acid (4.2) t

38、o 1 000 ml of water and mix.4.8 Hydrofluoric acid, 40 % (mass fraction).EN ISO 11490:2016 (E) DIN EN ISO 11490:2016-12 6 4.9 Diluted sulphuric acid, 50 % (mass fraction).4.10 Reducing gas, such as hydrogen or a hydrogen/nitrogen mixture.4.11 Inert gas under pressure, carbon dioxide or nitrogen are u

39、sual.4.12 Aqua regia.Mix three volumes of hydrochloric acid (4.3) and one volume of nitric acid (4.2).5 Apparatus5.1 Customary laboratory apparatus.5.2 Reduction apparatus, see Figure A.1.5.3 Platinum dishes, of volume 10 ml.5.4 AAS or ICP-OES, or other means of determining traces of metal.5.5 Muffl

40、e furnace, capable of attaining at least 900 C.5.6 Ashless filter paper, capable of retaining particles greater than 3 m.5.7 Analytical balance, with a reading accuracy of 0,01 mg.6 SamplingThe sampling procedure shall be performed in accordance with ISO 11596.7 ProcedureWARNING Suitable health and

41、safety procedures should be followed.7.1 Flatten the sample to less than 0,5 mm thick and weigh a sample containing 150 mg to 200 mg of palladium accurately to 0,01 mg. Transfer it to an 800 ml tall-form beaker. Add 10 ml of nitric acid (4.2) and heat at 70 C to 80 C for 20 min in the beaker covered

42、 with a watch glass before adding 30 ml of hydrochloric acid (4.3) to complete the dissolution.7.2 If insoluble silver chloride forms, break this up with a glass rod to ensure that all the metal is dissolved.7.3 Remove the watch glass and gently evaporate to dryness. Dissolve the residue in 10 ml of

43、 hydrochloric acid (4.3) and dilute to about 100 ml.7.4 If a precipitate forms, allow it to settle for 12 h in a dark place. Filter and wash with dilute nitric acid (4.7), retaining the precipitate for the determination of traces of palladium using suitable apparatus (5.4).7.5 Add 20 ml of hydrochlo

44、ric acid to the clear solution from 7.3 (or filtrate and washings from 7.4). Dilute to approximately 400 ml, cool to 15 C, and add dimethylglyoxime solution in 5 ml portions up to a total of 30 ml for every expected 100 mg of palladium.EN ISO 11490:2016 (E) DIN EN ISO 11490:2016-12 7 7.6 Leave to se

45、ttle for 1 h, filter and wash with dimethylglyoxime solution (4.5) diluted 10 times with water. Retain the combined filtrate and washes for determination of palladium using suitable apparatus (5.4) and correct the final result.7.7 Transfer the precipitate and filter to a tared porcelain crucible. Ta

46、p the filter to obtain a flat surface and dry in an oven at 110 C to 120 C for 3 h. Cover with a layer of ammonium chloride (4.6) about 3 mm thick (about 4 g for a crucible of diameter 40 mm) to prevent loss of palladium during ignition.7.8 Heat the crucible gently (for about 40 min) first to char t

47、he paper and then to decompose the palladium complex and drive off the ammonium chloride. When all fuming has ceased, ignite at 800 C 50 C for 1 h.NOTE The ammonium chloride decomposes at 340 C.7.9 The partially oxidized palladium is reduced to the metallic state by heating in the presence of reduci

48、ng gas (4.10) and allowing to cool in an inert gas atmosphere (4.11).7.10 Weigh the product to obtain an approximate mass of palladium.7.11 Transfer the impure palladium to a platinum dish (5.3). Moisten with hydrofluoric acid (4.8) and add three drops of dilute sulfuric acid (4.9). Heat until fumes start to evolve from the solution, cool, then extract the residue wit