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1、BS ISO 11495:2008 ICS 39.060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Jewellery Determination of palladium in palladium jewellery alloys Inductively coupled plasma (ICP) solution- spectrometric method using yttrium as internal standard element Licensed
2、CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2009 BSI 2009 ISBN 978 0 580 57471 9 Amendments/corrigenda issued since publication DateComments BS ISO
3、 11495:2008 National foreword This British Standard is the UK implementation of ISO 11495:2008. The UK participation in its preparation was entrusted to Technical Committee STI/53, Specifications and test methods for jewellery and horology. A list of organizations represented on this committee can b
4、e obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Licensed CopyChinese University of Hon
5、g Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 Reference number ISO 11495:2008(E) ISO 2008 INTERNATIONAL STANDARD ISO 11495 First edition 2008-08-15 Jewellery Determination of palladium in palladium jewellery alloys Inductively coupled plasma (ICP) solution-spectrometric meth
6、od using yttrium as internal standard element Joaillerie, bijouterie Dosage du palladium dans les alliages de palladium pour la joaillerie, bijouterie Mthode par spectromtrie dmission plasma induit en solution, utilisant lyttrium comme talon interne Licensed CopyChinese University of Hong Kong, 11/0
7、4/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 ISO 11495:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and
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10、und, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and mi
11、crofilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO
12、 2008 All rights reserved Licensed CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 ISO 11495:2008(E) ISO 2008 All rights reserved iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards
13、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 organizat
14、ions, 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. International Standards are drafted in accordance with the rules given in th
15、e ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of
16、the member bodies casting a vote. 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. ISO 11495 was prepared by Technical Committee ISO/TC 174, Jewellery
17、. Licensed CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 Licensed CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 INTERNATIONAL STANDARD ISO 11495:2008(E) ISO 2008 All rights reserved 1 Jeweller
18、y Determination of palladium in palladium jewellery alloys Inductively coupled plasma (ICP) solution- spectrometric method using yttrium as internal standard element 1 Scope This International Standard describes a method for the determination of palladium in palladium jewellery alloys, preferably wi
19、thin the range of fineness specified in ISO 9202, by means of inductively coupled plasma (ICP) emission spectrometry. The preferred palladium content of the alloys lies between 500 (parts per thousand) and 950 palladium. NOTE This method can be used to analyse other contents of palladium. Palladium
20、jewellery alloys can contain silver, indium, gallium, copper, cobalt, nickel, tin and ruthenium. The presence of these alloying elements has not been observed to interfere with the determination method. If other elements are alloyed, a check is made as to whether any interference occurs. 2 Normative
21、 references The following referenced documents are indispensable for the application of this document. 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 prec
22、ious metal alloys for and in jewellery and associated products 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 bracketing running of standards and samples in the following sequence: low standard sample high standard sample low standard sample
23、 high standard sample low standard sample high standard 4 Short description of method At 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 mad
24、e up to the standard measuring volume. Using an ICP emission spectrometer, the palladium content of the sample solution is measured by comparison of the ratio intensities of the spectral emission of palladium (at 340,45 nm) and yttrium (at 371,03 nm) with the ratios for solutions containing known ma
25、sses of palladium and yttrium, using the bracketing method. Licensed CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 ISO 11495:2008(E) 2 ISO 2008 All rights reserved Other palladium emission lines may be used, but need to be checked for spectral in
26、terference and instrumental performance. 5 Reagents During the analysis, unless otherwise stated, use only 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); 20 = 1,16 g/cm3; 32 % HCl (mas
27、s fraction). 5.2 Nitric acid (HNO3); 20 = 1,41 g/cm3; 65 % HNO3 (mass fraction). 5.3 Pure palladium (Pd). The palladium content shall be at least 99,99 %. 5.4 Internal standard solution Approximately 680 mg YCl3 6H2O are dissolved in 200 ml water and made up to 1 000 ml with water. Due to the sensit
28、ivity of the instrument, this concentration may be changed to achieve optimum performance. This also applies to the calibration solutions (see 8.1) and the sample solutions (see 8.2). 6 Apparatus Customary laboratory apparatus and the following. 6.1 ICP emission spectrometer capable of simultaneousl
29、y measuring the palladium emission line (at 340,45 nm) and the emission line of the internal standard yttrium (at 371,03 nm), with a minimum optical resolution of 0,02 nm. 6.2 Analytical balance accurate to 0,01 mg. 7 Sampling The sampling procedure shall be performed in accordance with ISO 11596. 8
30、 Procedure 8.1 Calibration solutions Weigh approximately 100 mg of palladium (5.3) accurately to at least 0,01 mg and dissolve in 30 ml of hot HCl (5.1) and 10 ml of HNO3 (5.2) in a tared 100 ml volumetric flask. Add water until the mass of the solution is approximately 100 g, weighed accurately to
31、at least 0,01 g. This palladium stock solution is used to prepare the calibration solutions. 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 volumetric flask. Add 10 g of the internal standard s
32、olution (5.4) accurate to at least 0,01 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 an
33、d sample solutions shall be consistent. Licensed CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 ISO 11495:2008(E) ISO 2008 All rights reserved 3 8.2 Sample solutions Weigh approximately 100 mg of the sample accurately to at least 0,01 mg, dissolve
34、 and treat the sample as described in 8.1. Weigh approximately 10 g of this “sample stock solution” accurate to at least 0,001 g into a 100 ml volumetric flask, and add 10 g of the internal standard solution (5.4) accurate to at least 0,01 g. Add 10 ml of HCl (5.1) and make up to 100 ml. Mix thoroug
35、hly. 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. NOTE Attention is drawn to the possibility that smaller samples will al
36、so be more affected by any variation of homogeneity in the material sampled. 8.3 Measurements The data processing unit of the ICP spectrometer is used to establish a measuring programme in which the intensities of the palladium emission lines (at 340,45 nm) and of the internal standard element yttri
37、um (at 371,03 nm) can be measured simultaneously. After ignition, allow the ICP torch at least 15 min to stabilize before use. Aspirate the calibration solutions and the sample solutions sequentially. Each standard and sample solution shall have a minimum 30 s preintegration period, followed by the
38、integration times and the number of integrations required to obtain a maximum relative standard deviation (RSD) of 0,2 % see 8.4.1, Equation (1). The accurate mass of palladium of the sample solution is derived from the measurement of the two calibration solutions bracketing the rough value of the s
39、ample solution see 8.4.2, Equation (4). 8.4 Calculations 8.4.1 The method of internal standardization is based on the linear relation between the intensity ratios IPd/IY and the concentration ratios CPd/CY or, better, mass ratios mPd/mY. Using the same mass of yttrium (internal standard solution) to
40、 prepare all solutions, it is not necessary to have an exact volume of the measuring solutions. The accuracy of the 100 ml volumetric flask is satisfactory. The other important advantage of always referring to the same mass of the internal standard is that all calculations can be done with mPd inste
41、ad of mPd/mY, nominal. In general, the data processing unit provides the quotients from the simultaneously registered single measurements of the palladium and the yttrium intensities. If the mean value, Q, of the five intensity quotients (Q1, Q2, Q3, Q4, Q5) belonging to each solution is calculated
42、as follows: 5 Pd Y 1 1 5 n I Q I = = (1) then this mean value shall have an RSD from Q not larger than 0,2 %. 8.4.2 In view of deviations from the nominal mass, mIS, in grams, of the internal standard solution (mIS = 10,000 g), each intensity quotient belonging to a measuring solution shall be corre
43、cted by the corresponding real mass of internal standard solution WIS,n, in grams, used to prepare this measuring solution. The corrected quotient, QC, is calculated as follows: IS, C IS n W QQ m = (2) Licensed CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO
44、11495:2008 ISO 11495:2008(E) 4 ISO 2008 All rights reserved To determine the palladium content of the sample using the corrected intensity quotient, the exact masses of palladium in the calibration solutions mPd,Cs,n, in milligrams, are required. These masses shall be calculated individually for eac
45、h calibration solution or calibration point as follows: Pd,SS Pd,Cs,SS,Pd, SS,Pd nn W mW m = (3) where WPd,SS is the mass, in milligrams, of palladium used to prepare the palladium stock solution; mSS,Pd is the mass, in grams, of the prepared palladium stock solution; WSS,Pd,n is the mass, in grams,
46、 of palladium stock solution used to prepare the calibration solution n. The two calibration points nearest to the palladium sample content, corresponding to the low mass a and to the high mass b, are used to determine the palladium mass in the sample solution as follows: ()() () C,sC, Pd C,C, a ba
47、baQQ ma QQ =+ (4) where a is the mass, in milligrams, of palladium in the calibration solution used as “low standard”, according to Equation (3); b is the mass, in milligrams, of palladium in the calibration solution used as “high standard”, according to Equation (3); QC,a is the corrected intensity
48、 ratio IPd/IY of the “low standard”; QC,b is the corrected intensity ratio IPd/IY of the “high standard”; QC,s is the corrected intensity ratio IPd/IY of the sample measuring solution. The final mass of palladium of the sample solution corresponds to the mean value of five measuring cycles and evalu
49、ations of this type, Pd, m and is calculated as follows: 5 PdPd 1 1 5 n mm = = (5) The RSD of Pd m shall not exceed 0,30 %. Once Pd m has been determined from the five single determinations of the sample solution, the palladium content of the sample, XPd, expressed in parts per thousand, is calculated as follows: PdSS,Sa Pd SaSS,Sa 1000 mm X WW = (6) Licensed CopyChinese University of Hong Kong, 11/04/2009 08:32, Uncontrolled Copy, (c) BSI BS ISO 11495:2008 ISO
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