1、BSI Standards PublicationBS ISO 13547-1:2014Copper, lead, zinc and nickelsulfide concentrates Determination of arsenicPart 1: Iron hydroxide concentration andinductively coupled plasma atomic emissionspectrometric methodBS ISO 13547-1:2014 BRITISH STANDARDNational forewordThis British Standard is th
2、e UK implementation of ISO 13547-1:2014.The UK participation in its preparation was entrusted to TechnicalCommittee NFE/36, Copper lead and zinc ores and concentrates.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to
3、 include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 80906 4ICS 73.060.99Compliance with a British Standard cannot confer immunity fromlegal obligations.This
4、British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 November 2014.Amendments issued since publicationDate Text affectedBS ISO 13547-1:2014 ISO 2014Copper, lead, zinc and nickel sulfide concentrates Determination of arsenic Part 1: Iron hydroxide con
5、centration and inductively coupled plasma atomic emission spectrometric methodConcentrs sulfurs de cuivre, de plomb et de zinc Dosage de larsenic Partie 1: Mthode par digestion acide, co-prcipitation avec le fer et plasma induit par haute frquenceINTERNATIONAL STANDARDISO13547-1First edition2014-11-
6、01Reference numberISO 13547-1:2014(E)BS ISO 13547-1:2014ISO 13547-1:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic
7、or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 7
8、49 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 13547-1:2014ISO 13547-1:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Principle 24 Reagents 25 Apparatus . 36 Sample . 46.1 Laboratory sample . 46.
9、2 Test sample . 46.3 Test portion 47 Procedure. 47.1 Number of determinations . 47.2 Blank test . 47.3 Dissolution of the test portion . 47.4 Removal of lead sulfate 57.5 Dissolution of the insoluble residue . 57.6 Separation of arsenic . 57.7 Preparation of test solutions . 67.8 Preparation of cali
10、bration solutions . 67.9 Preparation of arsenic calibration curve 67.10 Determination of arsenic content in test solutions . 68 Expression of results 79 Precision . 79.1 Expression of precision . 79.2 Procedure for obtaining the final result 89.3 Between-laboratories precision . 89.4 Check of truene
11、ss 910 Test report 10Annex A (normative) Procedure for the preparation and determination of the mass of a pre-dried test portion 11Annex B (normative) Flowsheet of the procedure for the acceptance of analytical values fortest samples 13Bibliography .14BS ISO 13547-1:2014ISO 13547-1:2014(E)ForewordIS
12、O (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 subject for which a technical co
13、mmittee 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) on all matters of electro
14、technical 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 noted. This document was draf
15、ted 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 any or all such patent rig
16、hts. 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 users and does not constit
17、ute 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 - Supplementary informationISO 13547
18、 consists of the following parts, under the general title Copper, lead, zinc and nickel sulfide concentrates Determination of arsenic: Part 1: Iron hydroxide concentration and inductively coupled plasma atomic emission spectrometric method Part 2: Acid digestion and inductively coupled plasma atomic
19、 emission spectrometric methodiv ISO 2014 All rights reservedBS ISO 13547-1:2014INTERNATIONAL STANDARD ISO 13547-1:2014(E)Copper, lead, zinc and nickel sulfide concentrates Determination of arsenic Part 1: Iron hydroxide concentration and inductively coupled plasma atomic emission spectrometric meth
20、odWARNING This International Standard may involve hazardous materials, operations, and equipment. It is the responsibility of the user of this International Standard to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use.1 ScopeThi
21、s International Standard specifies an iron hydroxide concentration and inductively coupled plasma atomic emission spectrometric (ICP-AES) method for the determination of the mass fraction of arsenic in copper, lead, zinc, and nickel sulfide concentrates as follows:a) for copper sulfide concentrates,
22、 the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 2,0 %;b) for lead sulfide concentrates, the method is applicable to the determination of mass fractions of arsenic from 0,05 % to 1,0 %;c) for zinc sulfide concentrates, the method is applicable to the determi
23、nation of mass fractions of arsenic from 0,05 % to 0,6 %;d) for nickel sulfide concentrates, the method is applicable to the determination of mass fraction of arsenic from 0,05 % to 1,0 %.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document
24、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 648, Laboratory glassware Single-volume pipettesISO 1042, Laboratory glassware One-mark volume
25、tric flasksISO 4787, Laboratory glassware Volumetric instruments Methods for testing of capacity and for useISO 8466-2, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second-order calibration fu
26、nctionsISO 9599, Copper, lead and zinc sulfide concentrates Determination of hygroscopic moisture in the analysis sample Gravimetric methodISO 12743:2006, Copper, lead, zinc and nickel concentrates Sampling procedures for determination of metal and moisture contentISO Guide 35:2006, Reference materi
27、als General and statistical principles for certification ISO 2014 All rights reserved 1BS ISO 13547-1:2014ISO 13547-1:2014(E)3 PrincipleThe test portion is decomposed in nitric and sulphuric acids. Arsenic is coprecipitated in ammonia solution by the carriers of iron hydroxide to be separated from t
28、he matrix. The arsenic content is determined by comparison against iron-matched standards using ICP-AES.4 ReagentsDuring the analysis, use only reagents of recognized analytical grade and distilled water, or water of equivalent purity.4.1 Sodium hydroxide (NaOH), AR grade.4.2 Arsenic trioxide (As2O3
29、), AR grade.4.3 Iron(III) chloride hexahydrate (FeCl36H2O), AR grade (ACc(17)If this condition exists, the difference between the reported result and the certified value is statistically significant.wherecis the final result, expressed as a percentage by mass of arsenic of the certified reference ma
30、terial;Acis the certified value, expressed as a percentage by mass of arsenic of the certified reference material;C is a quantity, expressed as a percentage by mass of arsenic depending on the type of certified reference material used as defined in 9.4.2.9.4.2 Type of certified reference material (C
31、RM) or reference material (RM)9.4.2.1 GeneralThe reference materials used for this purpose should be prepared and certified in accordance with ISO Guide 35:2006. ISO 2014 All rights reserved 9BS ISO 13547-1:2014ISO 13547-1:2014(E)9.4.2.2 Reference material certified/characterized by inter-laboratory
32、 test programmeThe quantity C (see 9.4.1), expressed as a percentage by mass of arsenic, is given by the following formula:CssnsA= +()2222Lrc(18)wheres2(Ac) is the variance of the certified value;n is the number of replicate determinations.9.4.2.3 Reference material certified/characterized by one la
33、boratoryThe quantity C (see 9.4.1), expressed as a percentage by mass of arsenic, is given by the following formula:Cssn=+222Lr(19)It is recommended that this type of certified reference material should be avoided, unless the particular CRM is known to have an unbiased certified value.10 Test report
34、The test report shall contain the following information:a) a reference to this International Standard (i.e. ISO 13547-1);b) identification of the sample;c) mass fraction of arsenic in the sample, expressed as a percentage;d) date on which the test was carried out;e) any occurrences noticed during th
35、e determination which may have had an influence on the results.10 ISO 2014 All rights reservedBS ISO 13547-1:2014ISO 13547-1:2014(E)Annex A (normative) Procedure for the preparation and determination of the mass of a pre-dried test portionA.1 GeneralThis annex specifies a method for the preparation
36、and determination of the mass of a pre-dried test portion in the analysis of copper, lead, zinc, and nickel sulfide concentrates. The method is applicable to sulfide concentrates not susceptible to oxidation and with hygroscopic moisture contents ranging from 0,05 % to 2 %.A.2 PrincipleThe test port
37、ion to be used for analysis is dried in air in an oven maintained at 105C 5C. The dried test portion is then weighed and used for the analysis. No correction for moisture is required.A.3 ReagentsA.3.1 Desiccant, such as self-indicating silica gel or anhydrous magnesium perchlorate.WARNING Care needs
38、 to be taken whenever disposing of exhausted magnesium perchlorate and all other laboratory chemicals. Environmental regulations often apply. Users should seek specialists advice to determine an appropriate, effective, health-conscious, safety-conscious, and environmentally sound means of disposal.A
39、.4 ApparatusOrdinary laboratory equipment and the following.A.4.1 Analytical balance, sensitive to 0,1 mg.A.4.2 Weighing vessels, of glass or silica or corrosion resistant metal with externally fitting airtight covers. For small test portions (of mass less than 3 g), the mass of the vessel should be
40、 as small as possible (i.e. less than 20 g).A.4.3 Laboratory oven, capable of maintaining a temperature of 105C 5C.A.5 ProcedureA.5.1 Preparation of the weighing vesselDry the weighing vessel and its cover (A.4.2) by heating in a laboratory oven (A.4.3) at 105C 5C for 1 h. Transfer the vessel and it
41、s cover to a desiccator containing suitable fresh desiccant (A.3.1) and allow cooling to ambient temperature. ISO 2014 All rights reserved 11BS ISO 13547-1:2014ISO 13547-1:2014(E)A.5.2 Test portionTare the dried weighing vessel and vessel cover (A.5.1). Immediately, add the mass of laboratory sample
42、 specified for analysis. An accurate total mass of the test portion and weighing vessel is not required at this point.A.5.3 Determination of the test portion dry massTransfer the uncovered weighing vessel, the test portion, and the vessel cover to the laboratory oven (A.4.3) and dry at 105C 5C for 2
43、 h. After the 2 h period, remove the weighing vessel and dry test portion from the oven, replace the vessel cover, and allow cooling to ambient temperature in the desiccator. When cool, remove the weighing vessel containing the dry test portion and the vessel cover from the desiccator and weigh to t
44、he nearest 0,1 mg (m1a) after slightly lifting the cover and quickly replacing it.Transfer the test portion into the appropriate analytical apparatus and immediately reweigh the empty weighing vessel and vessel cover. Record the mass (m2) to the nearest 0,1 mg.For new concentrates of unknown charact
45、eristics, it is advisable to repeat the drying for another 2 h at 105C 5C and to reweigh the weighing vessel and test portion plus vessel cover to the nearest 0,1 mg (m1b). The test portion can be considered stable if the difference between m1aand m1bis within 0,5 mg. If this condition is not achiev
46、ed, the drying and weighing steps should be repeated.A.6 Calculation of the test portion dry massThe dry mass of the test portion (m3) in grams is calculated using the following formula:mm m31 2=a(A.1)wherem1ais the mass of the dried test portion plus weighing vessel and its vessel cover, in grams;m
47、2is the mass of the empty weighing vessel plus its cover, in grams.The mass of the dry test portion is the mass to be used to calculate the element concentration in the laboratory sample on a dry basis. No correction for hygroscopic moisture is required.12 ISO 2014 All rights reservedBS ISO 13547-1:
48、2014ISO 13547-1:2014(E)Annex B (normative) Flowsheet of the procedure for the acceptance of analytical values fortest samplesxmaxxminc45c163 1,3Rdxmaxxminc45c163 1,2Rdc16321xx c45dRStartwithindependence duplicateresultsOnemoredeterminationOnemoredeterminationYesYesNoNoNoc109=221xx c43c109=33x2x1x c4
49、3c43Yesc109=43x4x2x1x c43c43c43=Median(x1, x2, x3, x4 )c109Figure B.1 Flowsheet of the procedure for the acceptance of analytical values for test samplesWhere R is given in 9.2. ISO 2014 All rights reserved 13BS ISO 13547-1:2014ISO 13547-1:2014(E)Bibliography1 ISO 385-1, Laboratory glassware Burettes Part 1: General requirements2 ISO 3696, Water for analytical laboratory use Specification and test methods14 ISO 2014 All rights reservedBS ISO 13547-1:2014BS ISO 13547-1:2
