BS ISO 10203-2017 Iron ores - Determination of calcium - Flame atomic absorption spectrometric method《铁矿石 钙含量测定 火焰原子吸收光谱法》.pdf

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1、BS ISO 10203:2017Iron ores Determinationof calcium Flame atomicabsorption spectrometricmethodBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 10203:2017 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 10203:2017. It supers

2、edes BS ISO 10203:2015 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee ISE/58, Iron ores.A list of organizations represented on this committee can be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 pr

3、ovisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 91926 8 ICS 73.060.10 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was pub

4、lished under the authority of the Standards Policy and Strategy Committee on 30 April 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 10203:2017 ISO 2017Iron ores Determination of calcium Flame atomic absorption spectrometric methodMinerais de fer Dosage du calc

5、ium Mthode par spectromtrie dabsorption atomique dans la flammeINTERNATIONAL STANDARDISO10203Fourth edition2017-03Reference numberISO 10203:2017(E)BS ISO 10203:2017ISO 10203:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unle

6、ss 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 either ISO at the a

7、ddress 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.orgBS ISO 10203:2017ISO 10203:2017(E)Foreword iv1 Scope . 12 Normative references 13 Ter

8、ms and definitions . 14 Principle 15 Reagents 26 Apparatus . 37 Sampling and samples 37.1 Laboratory sample . 37.2 Preparation of predried 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 p

9、ortion 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 measurem

10、ents . 79 Expression of results 79.1 Calculation of mass fraction of calcium . 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 re

11、sult . 109.3 Oxide factor . 1010 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 internation

12、al analytical trials .13Bibliography .14 ISO 2017 All rights reserved iiiContents PageBS ISO 10203:2017ISO 10203:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Sta

13、ndards 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, governmental and non-governmental, in liaison with ISO, also

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

15、 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 is drawn to the possibility that some of the eleme

16、nts 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/or on the ISO list of patent declarations received

17、 (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 expressions related to conformity assessment, as

18、 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, Iron ore and direct reduced iron, Subcommittee S

19、C 2, Chemical analysis.This fourth edition cancels and replaces the third edition (ISO 10203:2015), of which it constitutes a minor revision with the following changes: in 5.11, minor editorial/grammatical amendments have been incorporated; in 6.1, “with a lid” has been inserted after “crucible”; in

20、 6.3 b), “the ratio between” has been inserted before “the slope” and minor editorial/grammatical amendments have been incorporated; 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 incorporate

21、d; “predried” has been deleted where it is inappropriate in 8.1, 8.2, and 8.3.2; some references to the reagents in 8.4.2, 8.4.3, and Table 2 have been corrected; in the last line of 9.2.3, the formula has been corrected from 1APcto 12P ; in 9.2.4, Formula (7) and the relevant descriptions have been

22、 modified to harmonize this subclause across all International Standards for which ISO/TC 102/SC 2 is responsible.iv ISO 2017 All rights reservedBS ISO 10203:2017INTERNATIONAL STANDARD ISO 10203:2017(E)Iron ores Determination of calcium Flame atomic absorption spectrometric methodWARNING This docume

23、nt might involve hazardous materials, operations, and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this document to establish appropriate health and safety practices and determine the applicability of

24、 regulatory limitations prior to use.1 ScopeThis document specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of calcium in iron ores.This method is applicable to mass fractions of calcium between 0,010 % and 8,00 % in natural iron ores, iron ore conce

25、ntrates, and agglomerates, including sinter products.2 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 document. For dated references, only the edition cited applies. For undated references, the

26、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 Determination of hygroscopic moisture in analytical samples Gravimetric, Karl Fischer and mass

27、-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 for chemical analysisISO 80000-1:2009, Quantities and units Part 1: General3 Terms and defin

28、itionsNo terms and definitions are listed in this document.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 t p :/ www .iso .org/ obp4

29、PrincipleThe test portion is decomposed by the treatment with hydrochloric acid 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 residu

30、e is fused with sodium carbonate and the cooled melt is dissolved in the filtrate. ISO 2017 All rights reserved 1BS ISO 10203:2017ISO 10203:2017(E)The solution obtained is aspirated into the flame of an atomic absorption spectrometer using a dinitrogen oxide-acetylene burner.The absorbance values ob

31、tained for calcium are compared with those obtained from calibration solutions.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), anhydrous.5.2 Hydrochloric acid, ( 1,19 g/ml).5.3 Hydro

32、chloric 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), of mass fraction of calcium less than 0,000 2

33、%.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 200 ml with water. Dissolve 17 g of sodium carbonate

34、 (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 lanthanum chloride (LaCl37H2O) (of mass fraction of calc

35、ium 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 Calcium standard solution, 25 g Ca/ml.Dissolve 1,248 7 g of dried calcium carbonate (CaCO3) minimum purity 99,9 % (mass fraction), dried at 105 C for 1 h in 100 ml of hydrochloric acid (5.

36、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 solution to a 200 ml one-mark volumetric flask, dilute to volume with water, and mix.5.11 Calcium calibration solutions.Using pipettes, transfer 2,0

37、 ml, 5,0 ml, 10,0 ml, 15,0 ml, and 20,0 ml portions of calcium standard solution (5.10) to 200 ml volumetric flasks (Clause 6). Add 6 ml of 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 wa

38、ter and mix. Prepare a zero calcium calibration solution by transferring 60 ml of the background solution to a 200 ml volumetric flask. Then add 6 ml of hydrochloric acid (5.2) and 40 ml of lanthanum chloride solution (5.9). Dilute the solution to volume with water and mix.2 ISO 2017 All rights rese

39、rvedBS ISO 10203:2017ISO 10203:2017(E)6 ApparatusOrdinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with the specifications of ISO 648 and ISO 1042, respectively, and the following.All glassware, volumetric flask lids, and the platinum crucibles shall

40、 first be washed in hydrochloric acid (diluted 1 + 1) and then in water.6.1 Platinum crucible with a lid, of minimum capacity 30 ml.6.2 Muffle furnace, capable of maintaining a temperature of approximately 1 100 C.6.3 Atomic absorption spectrometer, equipped with a dinitrogen oxide/acetylene burner.

41、WARNING Follow the manufacturers instructions for igniting and extinguishing the dinitrogen oxide-acetylene flame to avoid possible explosion hazards. Wear tinted safety glasses whenever the flame is burning.The atomic absorption spectrometer used in this method shall meet the following criteria.a)

42、Minimum sensitivity: The absorbance of the most concentrated calcium calibration solution (see 5.11) shall be at least 0,3.b) Graph linearity: The ratio between the slope of the calibration graph covering the top 20 % of the concentration range (expressed as a change in absorbance) and the value of

43、the slope for the bottom 20 % of the concentration range determined in the same way shall not be less than 0,7.c) Minimum stability: The standard deviation of the absorbance of the most concentrated calibration solution and that of the zero calibration solution, each being calculated from a sufficie

44、nt number of repetitive measurements, shall be less than 1,5 % and 0,5 %, respectively, of the mean value of the absorbance of the most concentrated calibration solution.The use of a strip chart recorder and/or digital readout device is recommended to evaluate criteria a), b), and c) and for all sub

45、sequent measurements.NOTE Instrument parameters can vary with each instrument. The following parameters were successfully used in several laboratories and they can be used as guidelines. Solutions were aspirated into a dinitrogen oxide-acetylene flame of a premix burner.In systems where the values s

46、hown below for gas flow rates do not apply, the ratio of the gas flow rates may still be a useful guideline. Hollow cathode lamp, mA 15 Wavelength, nm 422,7 Dinitrogen oxide flow rate, I/min 13,8 Acetylene flow rate, I/min 6,67 Sampling and samples7.1 Laboratory sampleFor analysis, use a laboratory

47、sample of 100 m particle size which has been taken and prepared in accordance with ISO 3082. In the case of ores having significant contents of combined water or oxidizable compounds, use a particle size of 160 m.NOTE A guideline on significant contents of combined water and oxidizable compounds is

48、incorporated in ISO 7764. ISO 2017 All rights reserved 3BS ISO 10203:2017a) processed ores containing metallic iron (direct-reduces iron);b) natural or processed ores in which the sulfur content is higher than 0,2 %;c) natural or processed ores in which the content of combined water is higher than 2

49、,5 % by mass.Thoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a way that it is representative of the whole contents of the container.8 Procedure8.1 Number of determinationsCarry out the analysis at least in duplicate in accordance with Annex A, independently, on one test sample (see 7.2).NOTE The expression “independently” means that the second and any subsequent result is not affected by the previous result(s). For this particu