1、 Reference number ISO 9516-1:2003(E) ISO 2003INTERNATIONAL STANDARD ISO 9516-1 First edition 2003-04-01 Iron ores Determination of various elements by X-ray fluorescence spectrometry Part 1: Comprehensive procedure Minerais de fer Dosage de divers lments par spectromtrie de fluorescence de rayons X
2、Partie 1: Procdure dtaille ISO 9516-1:2003(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer perf
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5、Secretariat at the address given below. ISO 2003 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at th
6、e address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2003 All rights reservedISO 9516-1:2003(E) ISO 2003 All rig
7、hts reserved iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references . 2 3 Principle . 2 4 Reagents and materials 2 5 Apparatus. 6 6 Sampling and samples . 7 7 Procedure. 7 8 Calculation of results 17 9 General treatment of results 20 10 Test report 24 Annex A (normative) Prepar
8、ation of flux A 25 Annex B (normative) Preparation of flux B or flux C 27 Annex C (normative) Preparation of synthetic calibration standard 28 Annex D (normative) Standard deviation of specimen preparation 30 Annex E (normative) Spectrometer precision tests 35 Annex F (normative) Determination of th
9、e dead time and maximum count rate of the equipment 39 Annex G (informative) Air cooling block for fused discs . 46 Annex H (informative) Computer program for calculation of results 47 Annex I (informative) Sample of data for use with calculation program 60 Annex J (normative) Flowchart for acceptan
10、ce of results . 65 ISO 9516-1:2003(E) iv ISO 2003 All rights reservedForeword ISO (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 technic
11、al 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 closely wi
12、th the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft Inte
13、rnational Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document ma
14、y be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 9516-1 was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis. This first edition, together with ISO 9516-2, cancels
15、 and replaces ISO 9516:1992 by the augmentation of the range of elements under analysis and the diversification into two procedures. ISO 9516 consists of the following parts, under the general title Iron ores Determination of various elements by X-ray fluorescence spectrometry: Part 1: Comprehensive
16、 procedure Part 2: Simplified procedure ISO 9516-1:2003(E) ISO 2003 All rights reserved vIntroduction In this part of ISO 9516, Table 1 indicates that some determinations may be used for referee purposes and others for routine analysis only. A simplified procedure for routine use with all determinat
17、ion will be published in ISO 9516-2. INTERNATIONAL STANDARD ISO 9516-1:2003(E) ISO 2003 All rights reserved 1Iron ores Determination of various elements by X-ray fluorescence spectrometry Part 1: Comprehensive procedure WARNING This part of ISO 9516 may involve hazardous materials, operations and eq
18、uipment. This part of ISO 9516 does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this part of ISO 9516 to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use. 1
19、Scope This part of ISO 9516 sets out a wavelength dispersive X-ray fluorescence procedure for the determination of iron, silicon, calcium, manganese, aluminium, titanium, magnesium, phosphorus, sulfur, potassium, tin, vanadium, chromium, cobalt, nickel, copper, zinc, arsenic, lead and barium in iron
20、 ores. The method has been designed to cope with iron ores having high ignition losses. The method is applicable to iron ores regardless of mineralogical type. The concentration range covered for each of the component elements is given in Table 1. The determination of total iron cannot be used for r
21、eferee purposes. Table 1 Range of application of the method Component element Concentration range for referee purposes % Concentration range for analysis % Fe 38 to 72 Si 0,2 to 6,5 0,2 to 6,5 Ca 0,019 to 12,7 0,019 to 12,7 Mn 0,02 to 0,82 0,02 to 0,82 Al 0,1 to 3,5 0,1 to 3,5 Ti 0,016 to 4,7 0,016
22、to 4,7 Mg 0,2 to 2,0 0,2 to 2,0 P 0,006 to 0,6 0,006 to 0,6 S 0,04 to 0,6 0,007 to 0,6 K 0,008 to 0,45 0,012 to 0,45 Sn 0,006 to 0,015 V 0,001 7 to 0,3 0,001 7 to 0,3 Cr 0,006 to 0,024 Co 0,006 to 0,018 Ni 0,011 to 0,013 Cu 0,012 to 0,061 Zn 0,006 9 to 0,166 0,005 to 0,166 As 0,008 to 0,06 Pb 0,018
23、to 0,32 0,018 to 0,32 Ba 0,036 to 0,4 ISO 9516-1:2003(E) 2 ISO 2003 All rights reserved2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of
24、 the referenced document (including any amendments) applies. ISO 3082:1998, Iron ores Sampling and sample preparation procedures ISO 7764:1985, Iron ores Preparation of predried test samples for chemical analysis 3 Principle The glass discs for X-ray fluorescence measurement are prepared by incorpor
25、ating the test portion of the iron ore sample, via fusion, into a borate glass disc using a casting procedure. By using a fused glass disc, particle size effects are eliminated. Sodium nitrate is added to the flux to ensure complete oxidation of all components, particularly iron and sulfur. Any of t
26、hree methods for glass disc preparation may be used: two use lithium borate as flux; the other uses sodium borate. X-ray fluorescence measurements are based on the “line only” principle. It is not necessary to measure backgrounds on each glass disc, as background equivalent concentrations (BEC) are
27、determined on several blank glass discs at the line position using concentration-based line-overlap corrections. If desired, backgrounds can be measured to obtain net line intensities. The method is applicable to data from simultaneous and sequential X-ray fluorescence spectrometers. The method reli
28、es on measuring all components of the sample, other than volatiles. If some components are not measured, then errors will result in the measured components (see 7.2.2). Calibration is carried out using pure chemicals. Results are obtained after matrix corrections for inter-element effects. 4 Reagent
29、s and materials During analysis, only reagents of recognized high purity shall be used. NOTE 1 Where reagents have been ignited, they should be covered during cooling in the desiccator and weighed as soon as possible. NOTE 2 Reagents 4.2, 4.5, 4.7, 4.8, 4.9, 4.11, 4.13, 4.15, 4.16, 4.18 and 4.20 are
30、 used only for the preparation of the synthetic calibration standard, and are not required if the synthetic calibration standard is available commercially. 4.1 Silicon dioxide, (SiO 2 ), nominally 99,999 % SiO 2The silicon dioxide shall contain less than 3 g/g of each of the other elements listed in
31、 Table 1. It shall be heated to 1 000 C in a platinum crucible for a minimum of 2 h and cooled in a desiccator. 4.2 Aluminium oxide, (Al 2 O 3 ), analytical reagent grade, form If the form is used, it shall be heated to 1 000 C in a platinum crucible for a minimum of 2 h. If the aluminium oxide is n
32、ot the form, it shall be converted to the form by heating to 1 250 C in a platinum crucible for a minimum of 2 h. It shall be cooled in a desiccator and weighed as soon as it is cool. ISO 9516-1:2003(E) ISO 2003 All rights reserved 34.3 Iron(III) oxide, (Fe 2 O 3 ), nominally 99,999 % Fe 2 O 3The ir
33、on(III) oxide shall contain less than 3 g/g of each of the other elements listed in Table 1. It shall be heated at 1 000 C in a platinum crucible for a minimum of 1 h and cooled in a desiccator. 4.4 Titanium dioxide, (TiO 2 ) Analytical grade titanium dioxide shall be heated at 1 000 C in a platinum
34、 crucible for a minimum of 1 h and cooled in a desiccator. Phosphorus is a common impurity in TiO 2and a reagent low in phosphorus shall be selected. The selected reagent shall be checked, as even nominally high-purity reagents can be significantly contaminated, e.g. a supposed 99,99 % TiO 2grade re
35、agent has been found to contain about 0,5 % P 2 O 5 . 4.5 Potassium dihydrogen orthophosphate, (KH 2 PO 4 ) Analytical grade potassium dihydrogen orthophosphate shall be dried at 105 C for 1 h and cooled in a desiccator. 4.6 Calcium carbonate, (CaCO 3 ) Analytical grade calcium carbonate shall be dr
36、ied at 105 C for 1 h and cooled in a desiccator. 4.7 Calcium sulfate, (CaSO 4 . 2H 2 O) Analytical grade calcium sulfate dihydrate shall be dehydrated at 700 C for 1 h and cooled in a desiccator. 4.8 Manganese oxide, (Mn 3 O 4 ) Manganese oxide shall be prepared by heating analytical grade manganese
37、 oxide (MnO 2 , MnO or Mn 3 O 4 ) for 15 h at 1 000 C in a platinum crucible and then cooling. The lumpy material shall be crushed to a fine powder, heated for 1 h at 200 C and cooled in a desiccator. 4.9 Magnesium oxide, (MgO) Analytical grade magnesium oxide shall be dried in a platinum crucible b
38、y slowly heating from room temperature to 1 000 C. After 1 h at 1 000 C, the crucible containing the magnesium oxide shall be placed in a desiccator and weighed as soon as it is cool, as magnesium oxide readily absorbs carbon dioxide from the atmosphere. 4.10 Sodium nitrate, (NaNO 3 ) Analytical gra
39、de sodium nitrate shall be dried at 105 C for 1 h and cooled in a desiccator. 4.11 Tin oxide, (SnO 2 ) Analytical grade tin oxide shall be heated at 400 C for a minimum of 1 h and cooled in a desiccator. 4.12 Vanadium(V) oxide, (V 2 O 5 ) Analytical grade vanadium(V) oxide shall be heated at 400 C f
40、or a minimum of 1 h and cooled in a desiccator. 4.13 Chromium(III) oxide, (Cr 2 O 3 ) Analytical grade chromium(III) oxide shall be heated at 400 C for a minimum of 1 h and cooled in a desiccator. ISO 9516-1:2003(E) 4 ISO 2003 All rights reserved4.14 Cobalt oxide, (Co 3 O 4 ) Analytical grade cobalt
41、 oxide shall be heated at 400 C for a minimum of 1 h and cooled in a desiccator. 4.15 Nickel oxide, (NiO) Analytical grade nickel oxide shall be heated at 400 C for a minimum of 1 h and cooled in a desiccator. 4.16 Copper oxide, (CuO) Analytical grade copper oxide shall be heated at 400 C for a mini
42、mum of 1 h and cooled in a desiccator. 4.17 Zinc oxide, (ZnO) Analytical grade zinc oxide shall be heated at 400 C for a minimum of 1 h and cooled in a desiccator. 4.18 Di-sodium hydrogen arsenate, (Na 2 HAsO 4 . 7H 2 O) The analytical grade reagent shall be weighed as received. 4.19 Lead oxide, (Pb
43、O) Analytical grade lead oxide shall be heated at 400 C for a minimum of 1 h and cooled in a desiccator. 4.20 Barium carbonate, (BaCO 3 ) Analytical grade barium carbonate shall be heated at 105 C for a minimum of 1 h and cooled in a desiccator. 4.21 Ammonium iodide, (NH 4 I) Laboratory reagent grad
44、e ammonium iodide need not be dried, but shall be stored in a desiccator. 4.22 Desiccant The desiccant shall be freshly regenerated self-indicating silica gel. 4.23 Flux 4.23.1 General Flux A, flux B or flux C, as described in 4.23.2, 4.23.3 and 4.23.4, may be used. The levels of contamination in th
45、e flux shall be checked (see 9.1). Because levels of contamination may vary from batch to batch, the same batch of flux shall be used for all discs (iron ore, blank and calibration) involved in the batch of determinations. 4.23.2 Flux A Flux A shall be prepared by fusion of a mixture of anhydrous li
46、thium tetraborate (Li 2 B 4 O 7 ) and anhydrous lithium metaborate (LiBO 2 ) using the procedure specified in Annex A. Flux shall be dried at 500 C for a minimum of 4 h and stored in a desiccator. 4.23.3 Flux B Flux B shall be prepared using sodium tetraborate using the procedure specified in Annex
47、B. Flux shall be dried at 500 C for a minimum of 4 h and stored in a desiccator. ISO 9516-1:2003(E) ISO 2003 All rights reserved 54.23.4 Flux C Flux C shall be prepared using lithium tetraborate using the procedure specified in Annex B. Flux shall be dried at 500 C for a minimum of 4 h and stored in
48、 a desiccator. NOTE If this flux is used, sulfur will not be reported. 4.24 Calibration standard Two independent (i.e. prepared on different days) batches (labelled Day 1 and Day 2) of calibration standard shall be prepared by the procedure specified in Annex C. The composition of the calibration st
49、andard, given in Table 2, approximates that of an iron ore. The contents of some elements are higher than would be expected in an iron ore, but this is advantageous for obtaining a reliable calibration. Prior to weighing, a sufficient aliquot of the calibration standard shall be heated at 900 C for 20 min and cooled in a desiccator. Table 2 Composition of the calibration standard Component element Content % Oxide content % Fe 44,764 64,000 Fe 2 O 3Si 4,44 9,500 SiO 2Ca 3,067 4,291
