1、BSI Standards PublicationBS ISO 23201:2015Aluminium oxide primarilyused for production ofaluminium Determination oftrace elements Wavelengthdispersive X-ray fluorescencespectrometric methodBS ISO 23201:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 23201:
2、2015.The UK participation in its preparation was entrusted to TechnicalCommittee CII/24, Raw materials for the aluminium industry.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions
3、of a contract. Users are responsible for its correctapplication. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 81231 6ICS 71.100.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under
4、the authority of theStandards Policy and Strategy Committee on 30 November 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 23201:2015 ISO 2015Aluminium oxide primarily used for production of aluminium Determination of trace elements Wavelength dispersive X-ray f
5、luorescence spectrometric methodOxyde daluminium utilis pour la production daluminium Dtermination dlments traces Spectromtrie de fluorescence des rayons X par dispersion en longueur dondeINTERNATIONAL STANDARDISO23201First edition2015-11-15Reference numberISO 23201:2015(E)BS ISO 23201:2015ISO 23201
6、:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, 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, or
7、 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 11Fax +
8、41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 23201:2015ISO 23201:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Principle 24 Reagents and materials . 25 Apparatus . 36 Sampling and samples 57 Procedure. 57.1 General . 57.2 Preparation of calibration specimens . 67.2.1 Deter
9、mination of loss of mass on fusion of flux and flux correction 67.2.2 Preparation of intermediate calibration glass (ICG) . 67.2.3 Preparation of the synthetic calibration disk (SCD) . 77.2.4 Preparation of the blank calibration discs . 97.3 Preparation of the sample discs . 97.4 X-ray fluorescence
10、measurement . 107.4.1 General instrumental conditions 107.4.2 Guidelines for instrument optimization .117.4.3 Sample loading .117.4.4 Monitor disc: correction for instrumental drift .117.4.5 Measurements for calibration . 127.4.6 Measurement of test discs 138 Calculations.138.1 Calculation of net in
11、tensity 138.2 Comparison of duplicate measurements for the Al2O3blanks and Synthetic Calibration Discs (SCDs) 148.2.1 SCDs criteria for the acceptability of duplicate measurements .148.2.2 Al2O3blanks criteria for the acceptability of duplicate measurement 148.3 Drift correction of measured intensit
12、ies 158.4 Calculation of the calibration parameters 159 Consistency checks and reporting results 1610 Precision 1611 Accuracy .1712 Quality assurance and control.1713 Test report 17Annex A (informative) Contamination issues and care of platinum ware 19Annex B (normative) Example of instrument optimi
13、zation 21Annex C (informative) Calculation of reagent masses for different sample/flux combinations and synthetic calibration discs when omitting some elements .25Annex D (informative) Preparation of monitor disc .27Annex E (informative) Interlaboratory test program analysis of NIST 699 and ASCRM 27
14、 smelter grade alumina, certified reference materials .29Annex F (informative) Comments on flux purity 31Bibliography .32 ISO 2015 All rights reserved iiiContents PageBS ISO 23201:2015ISO 23201:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of natio
15、nal 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. Internati
16、onal 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 intended
17、 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.iso
18、.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 will
19、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 meaning of ISO specific terms and expression
20、s 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 informationThe committee responsible for this document is ISO/TC 226, Materials for the production of primary
21、 aluminium.iv ISO 2015 All rights reservedBS ISO 23201:2015ISO 23201:2015(E)IntroductionThis International Standard is based on Australian Standard AS 2879.71997, Alumina Determination of trace elements Wavelength dispersive X-ray fluorescence spectrometric method , developed by the Standards Austra
22、lia Committee on Alumina and Materials used in Aluminium Production to provide an XRF method for the analysis of alumina.The objective of this International Standard is to provide those responsible for the analysis of smelting-grade alumina with a standardized, validated procedure that will ensure t
23、he integrity of the analysis. ISO 2015 All rights reserved vBS ISO 23201:2015BS ISO 23201:2015Aluminium oxide primarily used for production of aluminium Determination of trace elements Wavelength dispersive X-ray fluorescence spectrometric method1 ScopeThis International Standard sets out a waveleng
24、th dispersive X-ray fluorescence spectrometric method for the analysis of aluminium oxide for trace amounts of any or all of the following elements: sodium, silicon, iron, calcium, titanium, phosphorus, vanadium, zinc, manganese, gallium, potassium, copper, chromium and nickel. These elements are ex
25、pressed as the oxides Na2O, SiO2, Fe2O3, CaO, TiO2, P2O5, V2O5, ZnO, MnO, Ga2O3, K2O, CuO, Cr2O3,and NiO on an un-dried sample basis.The method is applicable to smelting-grade aluminium oxide. The concentration range covered for each of the components is given in Table 1.Table 1 Applicable concentra
26、tion rangeComponentConcentration range %Na2O 0,10 to 1,00SiO20,003 to 0,05Fe2O30,003 to 0,05CaO 0,003 to 0,10TiO20,000 5 to 0,010P2O50,000 5 to 0,050V2O50,000 5 to 0,010ZnO 0,000 5 to 0,010MnO 0,000 5 to 0,010Ga2O30,000 5 to 0,020K2O 0,000 5 to 0,010CuO 0,000 5 to 0,010Cr2O30,000 5 to 0,010NiO 0,000
27、 5 to 0,0102 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document 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
28、 any amendments) applies.AS 2563, Wavelength dispersive X-ray fluorescence spectrometers Determination of precisionAS 2706, Numeric values Rounding and interpretation of limiting valuesAS 4538.1-1999 (R2013), Guide to the sampling of alumina Sampling proceduresAS 4538.2-2000 (R2013), Guide to the sa
29、mpling of alumina Preparation of samplesINTERNATIONAL STANDARD ISO 23201:2015(E) ISO 2015 All rights reserved 1BS ISO 23201:2015ISO 23201:2015(E)3 PrincipleA portion of the aluminium oxide test sample is incorporated, via fusion, into a borate glass disc using a casting technique. X-ray fluorescence
30、 measurements are made on this disc.Calibration is carried out using synthetic standards prepared from pure chemicals using a two-point regression. Matrix corrections may be employed but, because of the low levels at which the analytes are present in the Al2O3matrix, will have negligible effect with
31、in the scope of the method.Intensity measurements are corrected for spectrometer drift.A certified reference material, (see Annex E) is used to verify the calibration.4 Reagents and materials4.1 Flux, mixture of 12 parts lithium tetraborate to 22 parts lithium metaborate, pre-fused.This flux is avai
32、lable commercially. Flux will absorb atmospheric moisture when exposed to air. Minimize water uptake by storing flux in an airtight container.See Annex F for comments on flux purity.4.2 Aluminium oxide (Al2O3), high purity, nominally 99,999 % Al2O3.Prepared by heating to 1 200 C 25 C for 2 h and coo
33、ling in a desiccator.To ensure the high purity Al2O3is not contaminated with analyte elements, analyse it before use by preparing a disc made from the aluminium oxide (referred to as a “blank disc”) and measuring net intensities for each analyte element.The method for the measurement of blank discs
34、is given in 7.4.5. If a number of differently sourced high purity aluminium oxides are tested select the one with the lowest countrates for impurities for use in calibration and blank discs. A.3 gives instructions for reducing silica contamination in high purity aluminium oxide and may be employed i
35、f required.4.3 Sodium tetraborate (Na2B4O7), nominally 99,99 % Na2B4O7.Prepared by heating to 650 C 25 C for 4 h minimum and cooling in a desiccator.4.4 Silicon dioxide (SiO2), nominally 99,9 % SiO2.Prepared by heating to 1 200 C 25 C for 2 h and cooling in a desiccator.4.5 Iron(III) oxide (Fe2O3),
36、nominally 99,9 % Fe2O3.Prepared by heating to 1 000 C 25 C for a minimum of 1 h and cooling in a desiccator.4.6 Calcium carbonate (CaCO3), nominally 99,9 % CaCO3.Prepared by heating to 105 C 5 C for 1 h and cooling in a desiccator.4.7 Titanium dioxide (TiO2), nominally 99,9 % TiO2.Prepared by heatin
37、g to 1 000 C 25 C for a minimum of 1 h and cooling in a desiccator.4.8 Ammonium dihydrogen orthophosphate (NH4H2PO4), nominally 99,9 % NH4H2PO4.Prepared by heating to 105 C 5 C for 1 h and cooling in a desiccator.2 ISO 2015 All rights reservedBS ISO 23201:2015ISO 23201:2015(E)4.9 Vanadium pentoxide
38、(V2O5), nominally 99,9 % V2O5.Prepared by heating to 600 C 25 C for 1 h and cooling in a desiccator.4.10 Zinc oxide (ZnO), nominally 99,9 % ZnO.Prepared by heating to 1 000 C 25 C for a minimum of 1 h and cooling in a desiccator.4.11 Manganese oxide (Mn3O4), nominally 99,9 % pure.Heat manganese diox
39、ide (99,9 % pure, MnO2) for 24 h at 1 000 C 25 C in a platinum crucible and cool in a dessicator. Crush the resultant lumpy material to a fine powder. The product material is Mn3O4.4.12 Gallium oxide (Ga2O3), nominally 99,9 % Ga2O3.Prepared by heating to 1 000 C 25 C for a minimum of 1 h and cooling
40、 in a desiccator.4.13 Potassium carbonate (K2CO3), nominally 99,9 % K2CO3.Prepared by heating to 600 C 25 C for a minimum of 2 h and cooling in a desiccator.4.14 Copper oxide (CuO), nominally 99,9 % CuO.Prepared by heating to 1 000 C 25 C for a minimum of 1 h and cooling in a desiccator.4.15 Chromiu
41、m(III) oxide (Cr2O3), nominally 99,9 % Cr2O3.Prepared by heating to 1 000 C 25 C for a minimum of 1 h and cooling in a desiccator.4.16 Nickel(II) oxide (NiO), nominally 99,9 % NiO.Prepared by heating to 1 000 C 25 C for a minimum of 1 h and cooling in a desiccator.4.17 Certified Reference Material (
42、CRM), one or both of the alumina materials NIST699 and ASCRM027.Prepared by heating to 300 C 10 C for a minimum of 2 h and cooling in a desiccator. Details for NIST699 can be found at www.nist.gov. A test report for ASCRM027 is available from SAI-Global, , details of availability can be found within
43、 this International Standard.5 Apparatus5.1 Platinum crucible, non-wetting, platinum-alloy with a platinum lid and having a capacity compatible with the bead requirements.Typical crucibles have a volume of 25 mL to 40 mL.Crucibles shall be free of all elements to be determined.NOTE Silica has been f
44、ound to be a common contaminant of platinum metal alloys, and a suggested method for cleaning platinum ware to remove silica is given in A.2.5.2 Desiccator, provided with an effective, non-contaminating desiccant.All heat treated reagents (4.2 to 4.17) shall be stored in a desiccator.NOTE Pelletized
45、 molecular sieves and phosphorous pentoxide have been found to be satisfactory desiccants. Silica gel is not suitable. ISO 2015 All rights reserved 3BS ISO 23201:2015ISO 23201:2015(E)5.3 Electric furnace, fitted with an automatic temperature controller and capable of maintaining a temperature of 1 2
46、00 C 25 C.5.4 Platinum mould, non-wetting, platinum or platinum-alloy, circular-shaped of the type shown in Figure 1 and with dimensions compatible with sample holders employed in the particular spectrometer used.An example of a 35 mm mould is given in Figure 1.The surfaces of moulds shall be free o
47、f all elements to be determined, flat and polished to a mirror finish.Dimensions in mm (not in scale)352632Figure 1 Drawing of platinum/5 % gold mouldNOTE Silica has been found to be a common contaminant, and a suggested method for cleaning platinum ware and to remove silica is given in A.2.5.5 X-ra
48、y fluorescence spectrometer, wavelength dispersive, vacuum path X-ray fluorescence spectrometer, provided that the performance of the instrument has been verified and found to comply with the manufactures specifications or the performance requirements given in AS 2563, “Wavelength dispersive X ray f
49、luorescence spectrometers Determination of precision.”5.6 Vibratory mill, having grinding components that do not contaminate the intermediate calibration glass (ICG) with analyte elements.Take care to ensure that contaminants from the grinding equipment do not affect the analysis.NOTE Alumina, tungsten carbide and zirconia grinding components have been found to be satisfactory.5.7 Fusion equipment, an electric furnace capable of main
