BS ISO 10204-2017 Iron ores Determination of magnesium Flame atomic absorption spectrometric method《铁矿石 镁含量测定 火焰原子吸收光谱测定法》.pdf

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1、Iron ores Determination of magnesium Flame atomic absorption spectrometric methodBS ISO 10204:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Iron ores Determination of magnesium Flame atomic absorption spectrometric methodMinerais de fer Dosage du magns

2、ium Mthode par spectromtrie dabsorption atomique dans la flammeINTERNATIONAL STANDARDISO10204Fourth edition2017-07Reference numberISO 10204:2017(E)National forewordThis British Standard is the UK implementation of ISO 10204:2017. It supersedes BS ISO 10204:2015, which is withdrawn.The UK participati

3、on in its preparation was entrusted to Technical Committee ISE/58, Iron ores.A list of organizations 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 correc

4、t application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 95194 7ICS 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 Strateg

5、y Committee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 10204:2017 ISO 2017Iron ores Determination of magnesium Flame atomic absorption spectrometric methodMinerais de fer Dosage du magnsium Mthode par spectromtrie dabsorption atomique

6、dans la flammeINTERNATIONAL STANDARDISO10204Fourth edition2017-07Reference numberISO 10204:2017(E)BS ISO 10204:2017ISO 10204:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publicati

7、on may be reproduced or utilized otherwise in any form 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 o

8、f the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 10204:2017ISO 10204:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll ri

9、ghts 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, or posting on the internet or an intranet, without prior written permission. Permission can be requested from

10、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 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgISO 10204:2017(E)Foreword iv1 Scope . 12 Normative references 13 T

11、erms and definitions . 14 Principle 15 Reagents 26 Apparatus . 37 Sampling and samples 47.1 Laboratory sample . 47.2 Preparation of test samples . 47.2.1 General 47.2.2 Method specified in ISO 2596 . 47.2.3 Method specified in ISO 7764 . 48 Procedure. 48.1 Number of determinations . 48.2 Test portio

12、n 48.3 Blank test and check test 58.3.1 Blank test 58.3.2 Check test . 58.4 Determination . 58.4.1 Decomposition of the test portion 58.4.2 Treatment of the residue 58.4.3 Preparation of the test solution 68.4.4 Adjustment of the atomic absorption spectrometer. 68.4.5 Atomic absorption measurements

13、. 79 Expression of results 79.1 Calculation of mass fraction of magnesium . 79.2 General treatment of results . 79.2.1 Repeatability and permissible tolerance 79.2.2 Determination of analytical result 89.2.3 Between-laboratories precision . 89.2.4 Check for trueness 89.2.5 Calculation of final resul

14、t 99.3 Oxide factor 910 Test report 10Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples 11Annex B (informative) Derivation of repeatability and permissible tolerance formulae 12Annex C (informative) Precision data obtained by international analyt

15、ical trials .13Bibliography .14 ISO 2017 All rights reserved iiiContents PageBS ISO 10204:2017ISO 10204:2017(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

16、 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, governmental and non-governmental, in liaison with ISO, also take part

17、 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 are described in the ISO/IEC Directives, Part 1. In particul

18、ar 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 is drawn to the possibility that some of the elements of th

19、is 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/or on the ISO list of patent declarations received (see www

20、 .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 expressions related to conformity assessment, as well as

21、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, Iron ore and direct reduced iron, Subcommittee SC 2, Chem

22、ical analysis.This fourth edition cancels and replaces the third edition (ISO 10204:2015), of which it constitutes a minor revision with the following changes: in 7.2, reference to ISO 2596 has been incorporated and 7.2 has been rearranged in a more appropriate layout/format; in 8.2, reference to IS

23、O 2596 has been incorporated; “predried” has been deleted where it is inappropriate in 8.1, 8.2, and 8.3.2; in Table 1, some minor changes have been made; in 9.2.4, Formula (7) and relevant descriptions have been modified to harmonize this subclause across all documents for which ISO/TC 102/SC 2 is

24、responsible.iv ISO 2017 All rights reservedBS ISO 10204:2017ISO 10204:2017(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

25、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, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates clo

26、sely 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 are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria

27、 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 is drawn to the possibility that some of the elements of this document may be the subject of

28、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/or on the ISO list of patent declarations received (see www .iso .org/ patents).Any trade nam

29、e 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 expressions related to conformity assessment, as well as information about ISOs adherence t

30、o 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, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis.This fourth edition

31、cancels and replaces the third edition (ISO 10204:2015), of which it constitutes a minor revision with the following changes: in 7.2, reference to ISO 2596 has been incorporated and 7.2 has been rearranged in a more appropriate layout/format; in 8.2, reference to ISO 2596 has been incorporated; “pre

32、dried” has been deleted where it is inappropriate in 8.1, 8.2, and 8.3.2; in Table 1, some minor changes have been made; in 9.2.4, Formula (7) and relevant descriptions have been modified to harmonize this subclause across all documents for which ISO/TC 102/SC 2 is responsible.iv ISO 2017 All rights

33、 reserved INTERNATIONAL STANDARD ISO 10204:2017(E)Iron ores Determination of magnesium Flame atomic absorption spectrometric methodWARNING This document might involve hazardous materials, operations, and equipment. This document does not purport to address all of the safety problems associated with

34、its use. It is the responsibility of the user of this document to establish appropriate health and safety practices and determine the applicability of any limitations prior to use.1 ScopeThis document specifies a flame atomic absorption spectrometric method for the determination of the mass fraction

35、 of magnesium in iron ores.This method is applicable to mass fractions of magnesium between 0,010 % and 2,00 % in natural iron ores, iron ore concentrates, and agglomerates, including sinter products.2 Normative referencesThe following documents are referred to in the text in such a way that some or

36、 all of their content constitutes requirements 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 648, Laboratory glassware Single-volume pipettesISO 1042, Laboratory gla

37、ssware One-mark volumetric flasksISO 2596, Iron ores Determination 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 methodsIS

38、O 7764, Iron ores Preparation of predried test samples for chemical analysisISO 9516-1:2003, Iron ores Determination of various elements by X-ray fluorescence spectrometry Part 1: Comprehensive procedure3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain

39、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 t p :/ www .iso .org/ obp4 PrincipleThe test portion is decomposed by the treatment with hydrochloric acid

40、and a small amount of nitric acid, and then evaporated to dehydrate silica, followed by dilution and filtration.The residue is ignited and silica is removed by evaporation with hydrofluoric and sulfuric acids. The residue is fused with sodium carbonate and the cooled melt is dissolved in the filtrat

41、e. ISO 2017 All rights reserved 1BS ISO 10204:2017ISO 10204:2017(E)The solution obtained is aspirated into the flame of an atomic absorption spectrometer using an air-acetylene burner.The absorbance values obtained for magnesium are compared with those obtained from calibration solutions.NOTE A dini

42、trogen oxide/acetylene flame can be used for the determination, in which case, the sensitivity is decreased by a factor of about 3.5 ReagentsDuring the analysis, use only reagents of recognized analytical grade and only water that complies with Grade 2 of ISO 3696.5.1 Sodium carbonate, (Na2CO3), anh

43、ydrous.5.2 Hydrochloric acid, 1,19 g/ml.5.3 Hydrochloric acid, 1,19 g/ml, diluted 1 + 9.5.4 Nitric acid, 1,4 g/ml.5.5 Hydrofluoric acid, 1,13 g/ml, 40 % (mass fraction) or 1,185 g/ml, 48 % (mass fraction).5.6 Sulfuric acid, 1,84 g/ml, diluted 1 + 1.5.7 Pure iron, minimum purity 99,9 % (mass fraction

44、), of mass fraction of magnesium less than 0,0002 %.5.8 Background solution.Dissolve 5,0 g pure iron (5.7) in 50 ml of hydrochloric acid (5.2) and oxidize by adding nitric acid (5.4) drop by drop. Evaporate until a syrupy consistency is obtained. Add 20 ml of hydrochloric acid (5.2) and dilute to 20

45、0 ml with water. Dissolve 17 g of sodium carbonate (5.1) in water, add carefully to the iron solution, and heat to remove carbon dioxide. Transfer the cooled solution to a 1 000 ml one-mark volumetric flask, dilute to volume with water, and mix.5.9 Lanthanum chloride solution.Dissolve 50 g of lantha

46、num chloride (LaCl37H2O) (of mass fraction of magnesium less than 0,002 %) in 50 ml of hydrochloric acid (5.2) and 300 ml of hot water. Cool and dilute to 1 l.5.10 Magnesium standard solution, 25 g Mg/ml.Dissolve 0,500 0 g of oxide-free magnesium metal minimum purity 99,9 % (mass fraction) or 0,829

47、2 g of analytical grade magnesium oxide (dried and weighed in accordance with ISO 9516-1:2003, 4.9) by slowly adding 75 ml of hydrochloric acid (5.2), diluted 1 + 3. When dissolved, cool, transfer to a 1 000 ml one-mark volumetric flask, dilute to volume with water, and mix. Transfer 10 ml of this s

48、olution to a 200 ml one-mark volumetric flask, dilute to volume with water, and mix.5.11 Magnesium calibration solutions.Using pipettes, transfer 2,0 ml, 5,0 ml, 10,0 ml, 15,0 ml, and 20,0 ml portions of magnesium standard solution (5.10) to 200 ml volumetric flasks (see next paragraph). Add 6 ml of

49、 hydrochloric acid (5.2), 60 ml of background solution (5.8), and 40 ml of lanthanum chloride solution (5.9) to each flask. Dilute the solution to volume with water and mix. Prepare a zero magnesium calibration solution 2 ISO 2017 All rights reservedBS ISO 10204:2017ISO 10204:2017(E)The solution obtained is aspirated into the flame of an atomic absorption spectrometer using an air-acetylene burner.The absorbance values obtained for magnesium are compared with those obta