1、Iron ores Determination of trace elements Plasma spectrometric methodBS ISO 22682:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Iron ores Determination of trace elements Plasma spectrometric methodMinerais de fer Dtermination dlments traces Mthode par
2、spectromtrie avec plasmaINTERNATIONAL STANDARDISO22682First edition2017-08Reference numberISO 22682:2017(E)National forewordThis British Standard is the UK implementation of ISO 22682:2017.The UK participation in its preparation was entrusted to Technical Committee ISE/58, Iron ores.A list of organi
3、zations represented on this committee can be 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. The British Standards Institution 2017 Published by BSI Standards Limited 2017
4、ISBN 978 0 580 91224 5ICS 73.060.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affe
5、ctedBRITISH STANDARDBS ISO 22682:2017 ISO 2017Iron ores Determination of trace elements Plasma spectrometric methodMinerais de fer Dtermination dlments traces Mthode par spectromtrie avec plasmaINTERNATIONAL STANDARDISO22682First edition2017-08Reference numberISO 22682:2017(E)BS ISO 22682:2017ISO 22
6、682:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying,
7、 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 officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fa
8、x +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 22682:2017ISO 22682:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any for
9、m or by any means, electronic 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 officeCh. de Blandonnet
10、 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgISO 22682:2017(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 24 Principle 25 Reagents 26 Apparatus . 47 Sampling and samples 47.1 Laboratory sample . 47.2 Prep
11、aration of predried test samples 58 Procedure. 58.1 Number of determinations . 58.2 Test portion 58.3 Blank test and check test 58.4 Determination . 58.4.1 Decomposition of the test portion 58.4.2 Adjustment of spectrometer 69 Calculation of results . 79.1 Calibration graph 79.2 Correction of spectr
12、al interference . 89.3 Standardization of calibration graph (drift correction) 99.4 General treatment of results 109.4.1 Repeatability and permissible tolerances .109.4.2 Determination of analytical result .109.4.3 Check for trueness .119.4.4 Calculation of final result . 129.5 Oxide factors 1210 Te
13、st report 12Annex A (informative) Suggested calibration solutions 14Annex B (normative) Plasma spectrometer performance tests .15Annex C (normative) Flowchart of the procedure for the acceptance of analytical values of test samples 18Annex D (informative) Derivation of repeatability and permissible
14、tolerance formulae .19Annex E (informative) Precision data obtained by international analytical trials .20Bibliography .25 ISO 2017 All rights reserved iiiContents PageBS ISO 22682:2017ISO 22682:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of nati
15、onal 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. Internat
16、ional 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 intende
17、d 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 drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www .
18、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 rights. Details of any patent rights identified during the development of the document
19、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 constitute an endorsement.For an explanation on the voluntary nature of standards, the m
20、eaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared b
21、y Technical Committee ISO/TC 102, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis.iv ISO 2017 All rights reservedBS ISO 22682:2017ISO 22682:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO membe
22、r 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 organizations, governmenta
23、l 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 its further maintenance ar
24、e 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/ directives).Attention
25、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 in the Introduction and/
26、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 voluntary nature of standards, the meaning of ISO specific terms and
27、 expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 102
28、, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis.iv ISO 2017 All rights reserved INTERNATIONAL STANDARD ISO 22682:2017(E)Iron ores Determination of trace elements Plasma spectrometric methodCAUTION This document may involve hazardous operations and equipment. This document do
29、es not purport to address all of the safety issues associated with its use. It is the responsibility of the user of this document to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to its use.1 ScopeThis document specifies a method fo
30、r the determination of phosphorus, vanadium, titanium, copper, nickel, chromium, barium and cobalt in iron ores, by inductively coupled plasma atomic emission spectrometry (ICP-AES).This method is applicable to the concentration ranges (mass fraction) given in Table 1, in natural iron ores, iron ore
31、 concentrates and agglomerates, including sinter products.Table 1 Concentration rangesElementConcentration range for referee purpose % (mass fraction)Concentration range for non-referee purpose % (mass fraction)P 0,000 2 to 0,150 0,000 2 to 0,150V 0,003 0 to 0,024 0,003 0 to 0,024Ti 0,015 0 to 0,120
32、 0,015 0 to 0,120Cu 0,0014 to 0,250 0,001 4 to 0,250Ni 0,005 0 to 0,090 0,005 0 to 0,090Cr 0,004 0 to 0,015Ba 0,002 8 to 0,035Co 0,002 0 to 0,1002 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this
33、document. 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 volumetric flasksISO 2596, Iron ores De
34、termination of hygroscopic moisture in analytical samples Gravimetric, Karl Fischer and mass-loss methodsISO 3082, Iron ores sampling and sample preparation proceduresISO 3696, Water for analytical laboratory use Specification and test methodsISO 7764, Iron ores Preparation of predried test samples
35、for chemical analysisISO 11323, Iron ore and direct reduced iron Vocabulary ISO 2017 All rights reserved 1BS ISO 22682:2017ISO 22682:2017(E)3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 11323 apply.ISO and IEC maintain terminological databases for u
36、se in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p s :/ www .iso .org/ obp4 PrincipleThe test portion is decomposed with L-ascorbic acid, hydrofluoric acid, concentrated hydrochloric a
37、cid, concentrated nitric acid and then evaporated to dryness. The dry mass is dissolved in hydrochloric acid (1 + 1) and the solution is made up to 100 ml.The solution is diluted to volume and measured on an ICP spectrometer. Final results are read from a calibration graph prepared using standard ca
38、libration solutions.5 ReagentsDuring the analysis, use only highly pure reagents of recognized analytical grade and only water that complies with grade 2 of ISO 3696.5.1 High-purity iron, metal, of minimum purity grade 99,99 % (mass fraction).5.2 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml, diluted 1
39、+ 1.5.3 Nitric acid, 1,38 g/ml to 1,4 g/ml5.4 Hydrofluoric acid, 1,13 g/ml to 1,16 g/ml.5.5 Sulfuric acid, p.a. grade.5.6 L-ascorbic acid, C6H8O6.5.7 Stock solutions.Stock solutions shall be prepared by convenient handling moisture-free high-purity salts, dried until a constant mass and cooled in a
40、desiccator. High-purity metals of minimum purity grade of 99,9 % (mass fraction) can also be used to prepare vanadium, titanium, copper, nickel and chromium stock solutions. Stock solutions may also be prepared by independent laboratories or reagent suppliers.5.7.1 Phosphorus, 1 000 g/ml.Dissolve 4,
41、393 6 g of potassium dihydrogen orthophosphate (KH2PO4) in about 200 ml of water in a 1 000 ml one-mark volumetric flask. When the dissolution is complete, dilute to volume with water and mix.5.7.2 Vanadium, 1 000 g/ml.Dissolve 1,000 0 g of high-purity vanadium metal or 2,296 3 g of ammonium metavan
42、adate (NH4VO3) in 20 ml of nitric acid (5.3) in a covered tall-form beaker with heating. When dissolution is complete, cool and transfer to a 1 000 ml one mark-volumetric flask, dilute to volume with water and mix.2 ISO 2017 All rights reservedBS ISO 22682:2017ISO 22682:2017(E)3 Terms and definition
43、sFor the purposes of this document, the terms and definitions given in ISO 11323 apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t
44、 t p s :/ www .iso .org/ obp4 PrincipleThe test portion is decomposed with L-ascorbic acid, hydrofluoric acid, concentrated hydrochloric acid, concentrated nitric acid and then evaporated to dryness. The dry mass is dissolved in hydrochloric acid (1 + 1) and the solution is made up to 100 ml.The sol
45、ution is diluted to volume and measured on an ICP spectrometer. Final results are read from a calibration graph prepared using standard calibration solutions.5 ReagentsDuring the analysis, use only highly pure reagents of recognized analytical grade and only water that complies with grade 2 of ISO 3
46、696.5.1 High-purity iron, metal, of minimum purity grade 99,99 % (mass fraction).5.2 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml, diluted 1 + 1.5.3 Nitric acid, 1,38 g/ml to 1,4 g/ml5.4 Hydrofluoric acid, 1,13 g/ml to 1,16 g/ml.5.5 Sulfuric acid, p.a. grade.5.6 L-ascorbic acid, C6H8O6.5.7 Stock soluti
47、ons.Stock solutions shall be prepared by convenient handling moisture-free high-purity salts, dried until a constant mass and cooled in a desiccator. High-purity metals of minimum purity grade of 99,9 % (mass fraction) can also be used to prepare vanadium, titanium, copper, nickel and chromium stock
48、 solutions. Stock solutions may also be prepared by independent laboratories or reagent suppliers.5.7.1 Phosphorus, 1 000 g/ml.Dissolve 4,393 6 g of potassium dihydrogen orthophosphate (KH2PO4) in about 200 ml of water in a 1 000 ml one-mark volumetric flask. When the dissolution is complete, dilute
49、 to volume with water and mix.5.7.2 Vanadium, 1 000 g/ml.Dissolve 1,000 0 g of high-purity vanadium metal or 2,296 3 g of ammonium metavanadate (NH4VO3) in 20 ml of nitric acid (5.3) in a covered tall-form beaker with heating. When dissolution is complete, cool and transfer to a 1 000 ml one mark-volumetric flask, dilute to volume with water and mix.2 ISO 2017 All rights reserved ISO 22682:2017(E)5.7.3 Titanium, 1 000 g/ml.Dissolve 1,000 0 g of high-purity titan
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