1、BSI Standards Publication PD ISO/TR 18336:2016 Guidelines for good XRF laboratory practice for the iron ore industryPD ISO/TR 18336:2016 PUBLISHED DOCUMENT National foreword This Published Document is the UK implementation of ISO/TR 18336:2016. The UK participation in its preparation was entrusted t
2、o 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 correct application. The British Standard
3、s Institution 2016. Published by BSI Standards Limited 2016 ISBN 978 0 580 79534 3 ICS 73.060.10 Compliance with a British Standard cannot confer immunity from legal obligations. This Published Document was published under the authority of the Standards Policy and Strategy Committee on 29 February 2
4、016. Amendments issued since publication Date Text affectedPD ISO/TR 18336:2016 ISO 2016 Guidelines for good XRF laboratory practice for the iron ore industry Lignes directrices de bonnes pratiques de laboratoire de spectromtrie de fluorescence de rayons X pour lindustrie du minerais de fer TECHNICA
5、L REPORT ISO/TR 18336 Reference number ISO/TR 18336:2016(E) First edition 2016-02-15PD ISO/TR 18336:2016ISO/TR 18336:2016(E)ii ISO 2016 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may
6、 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 of the
7、requester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.orgPD ISO/TR 18336:2016ISO/TR 18336:2016(E)Foreword iv Introduction v 1 Scope . 1 2 Reagents 1 3 Apparatus . 2 4 Fused glass beads . 5 4
8、.1 General . 5 4.2 Storage . 5 4.3 Disc making precision . 5 4.4 Bead distortion (curvature and flatness) . 6 5 Quality control 6 5.1 Selection of QC samples and frequency of preparation . 6 5.2 Analysis of QC and analytical samples 7 5.3 Control charts 7 5.4 Participation in proficiency test progra
9、ms . 8 Annex A (informative) Results for flux loss on ignition testing 9 Annex B (informative) Procedure to check disc making precision 10 Annex C (informative) Method to determine relationship between height and concentration.11 Annex D (informative) Production of a height adjustable cup .12 Annex
10、E (informative) Bead measurement apparatus 13 Annex F (informative) Flow sheet for fused bead quality 14 Annex G (informative) Microsoft Excel program for calculating disc precision .15 Annex H (informative) Data input screen for calculating disc precision .19 Annex I (informative) Loss of accuracy
11、with no loss of precision .20 Annex J (informative) Loss of accuracy with loss of precision 22 Annex K (informative) Loss of accuracy and precision Loss of bead making precision .23 Annex L (informative) Results for spectrometer precision test 25 Annex M (informative) Drift correction .26 Bibliograp
12、hy .27 ISO 2016 All rights reserved iii Contents PagePD ISO/TR 18336:2016ISO/TR 18336:2016(E) Foreword 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 carrie
13、d 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 in the work. IS
14、O 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 particular the different
15、 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 this document may be
16、 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.iso.org/patents).
17、 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 expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles
18、in the Technical Barriers to Trade (TBT), see the following URL: Foreword Supplementary information. The committee responsible for this document is ISO/TC 102, Iron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis.iv ISO 2016 All rights reservedPD ISO/TR 18336:2016ISO/TR 18336:2016(
19、E) Introduction This Technical Report is intended for use in conjunction with other International Standards for the chemical analysis of iron ores. Although it was written for a high through-put iron ore laboratory, the procedures described can be modified to suit other industry or laboratory requir
20、ements. Some laboratories may find the recommended frequency of testing recommended by this Technical Report to be excessive for their situation or the precision required by them. In this case, the operator may use their informed discretion to adapt the recommendations of the guidelines to their sit
21、uation. ISO 2016 All rights reserved vPD ISO/TR 18336:2016PD ISO/TR 18336:2016Guidelines for good XRF laboratory practice for the iron ore industry 1 Scope This Technical Report specifies recommended quality control procedures for XRF laboratories operating within the iron ore industry. 2 Reagents A
22、ll reagents (including fusion fluxes and calibration reagents) should be purchased from reputable suppliers and should meet the minimum requirements for purity as listed in ISO 9516-1. All reagents should have a batch number and, where available, a certificate of analysis. Details of purchased reage
23、nts (supplier, amount purchased, quality, and batch number) should be recorded. These records should include what the reagents are used for. For batches of flux, the records should indicate which samples were analysed with a particular batch. 2.1 Fusion flux As the levels of contamination may vary f
24、rom batch to batch of flux, the purity of fusion fluxes should be checked prior to use. This can be achieved by fusing duplicate beads of pure silica and iron with the new flux, and analysing these along with beads prepared using a previously tested (certified) flux. Background concentrations should
25、 not exceed 10 ppm to 20 ppm (as compared to a certified batch of flux) for each of the following oxides Mn 3 O 4 , SnO 2 , V 2 O 5 , Cr 2 O 3 , Co 3 O 4 , NiO, CuO, ZnO, As 2 O 3 , PbO, BaO, Na 2 O and Cl and the sum of the positive differences should not exceed 40 ppm to 50 ppm. The concentrations
26、 of the oxides should not exceed 0,01 % for each of the following oxides Fe 2 O 3 , SiO 2 , CaO, Al 2 O 3 , TiO 2 , MgO, K 2 O and P 2 O 5 , (the absolute sum of the differences should not exceed 0,02 %), while backgrounds should not differ by more than 0,01 %. Sulfur (reported as SO 3 ) can frequen
27、tly vary by 0,05 %. Where flux does not conform to specifications, a second duplicate set of beads (made with old and new flux) should be prepared by a different operator on the same day, or by the same operator on a different day. If the material fails to meet the minimum specifications, the suppli
28、er of non-conforming flux should be contacted and a replacement batch obtained and tested. Where non-significant deviations are observed for major and trace elements between flux batches, these beads can be used to update calibration intercepts. In all cases, records of calibration prior and after a
29、mendment should be kept. Prior to calibration amendment, the concentration levels of all previously analysed blank beads (prior to calibration amendment) should be plotted, and trends noted. If consecutive sets of duplicate beads show consistent positive concentration increases, previous beads shoul
30、d be refused and re-run, and the trends confirmed or negated. Where laboratories elect to use additive fluxes (oxidizing, release agents or internal standard compounds), the homogeneity of the flux should be tested, assessed and compared against the quoted quality or against a flux batch that is kno
31、wn to be homogenous. Testing methods include direct measurement of added analytes, or indirect measurement of a quality parameter (ignition loss). An example of flux testing results can be found in Annex A. As calibrations would have been amended, trends will be seen as negative values progressing t
32、owards a more positive result. If past expected trends cannot be replicated, the XRF instrument (calibration, monitor) should be inspected. If previously seen trends are repeated, flux suppliers should be contacted, and the problem discussed. TECHNICAL REPORT ISO/TR 18336:2016(E) ISO 2016 All rights
33、 reserved 1PD ISO/TR 18336:2016ISO/TR 18336:2016(E) 2.2 Calibration reagents Reagents used for XRF recalibration should be checked in a similar manner to that used to check flux (by preparing both the old reagent and the new reagent in the same type of flux). Here the level of contaminants should no
34、t exceed those reported on the reagent suppliers certificate of analysis. Please note that it is common for reagent suppliers to report reagent purity based on an “as difference” basis. Consequently, a 99,999 % reagent may have only been analysed for a single contaminant whose content is less than 1
35、 ppm. However, this reagent may contain other contaminants which have not been analysed whose concentration may be significant. Alternatively, if no in-house high purity reagent is available, small quantities of analysed reagents may be obtained from reputable laboratories. In addition, where reagen
36、ts are suspected of contamination, they can be externally analysed. 3 Apparatus All equipment used to prepare and measure fused glass beads should be checked on a regular basis in accordance with the schedule set out in Table 1. The frequencies defined in Table 1 are those required by a high through
37、-put iron ore laboratory. As this Technical Report is a guideline rather than a prescriptive standard, laboratories with lesser demands can modify the figures accordingly. 3.1 Bead preparation equipment All equipment used for the production of fused glass beads (such as balances, fusion ware, fusion
38、 furnaces and sample drying equipment) should be installed, maintained and operated in accordance to the manufacturers recommendations. The external surfaces of all fusion furnaces should be inspected at the commencement of each shift for excessive dust and glass fragments or glass spills. If any sp
39、illage is detected it should be cleaned up before further use. On a weekly basis, or if spillage has occurred, fusion furnaces should be allowed to cool and the interior should be inspected for faults (broken or loose furnace linings that may contaminate samples) and cleaned (and repaired if necessa
40、ry). Fusion furnace temperatures should be checked weekly for accuracy and uniformity of temperature using a calibrated reference thermocouple. As a general rule, an independent performance audit of bead making equipment (including any environmental factors) should be performed yearly. Table 1 Summa
41、ry of frequency of tests and procedures Frequency Test Each shift Run Monitors a . Monitor data should be checked for drift (3.2.4). If problems/issues are suspected within the instrument, then increased monitor samples should be run throughout the day. At the commencement of every shift, all labora
42、tory personnel involved in the produc- tion of XRF fusion beads should prepare at least one quality control sample (reference or certified reference material) in duplicate (5.1). At the commencement of every shift, all laboratory personnel involved in the produc- tion of XRF fusion beads should prep
43、are at least one quality control sample (reference or certified reference material) in duplicate (5.1). These specimens should be meas- ured and the results evaluated before any unknown specimens are validated. Monitor chilled water flow rate and temperature (3.2.2). Monitor compressed air pressure
44、(3.2.2). Monitor detector gas flow rate and pressure (3.2.2). Monitor instrument error logs (3.2.2). Inspect fusion furnaces and clean if necessary (3.1). aMonitor is used exclusively for drift correction. Where the power settings have not changed more than 1 kW from the nominal operating power and
45、the spectrometer has been shown to have achieved stability over a desired time frame ( 3.2). Monitor updates can be performed for the corresponding time frame.2 ISO 2016 All rights reservedPD ISO/TR 18336:2016ISO/TR 18336:2016(E) Frequency Test Weekly Check resolution and pulse shift for flow detect
46、ors (3.2.2). Perform disc making precision tests for new operators. Once competent, perform checks monthly (4.3). Clean interior and exterior of fusion furnaces (3.1). Check furnace temperature and uniformity of temperature (3.1). Fortnightly Back up spectrometer data files, calibrations and configu
47、rations (3.2.3). Measure flatness of moulds and casting dishes (4.4). Monthly Perform disc making precision tests for competent operators (4.3) or automated equipment. Clean monitors (3.2.4). Three-monthly Prepare synthetic calibration standards (SynCals) in quadruplicate and compare results to cali
48、bration data (5.3). Half-yearly and prior to calibration or after major repairs Perform precision tests in ISO/TR 18231. Perform long-term stability tests in ISO/TR 18231. Perform detector linearity tests in ISO/TR 18231. Yearly Check all bead preparation equipment (balances, fusion ware, fusion fur
49、naces and environmental conditions) (3.1). aMonitor is used exclusively for drift correction. Where the power settings have not changed more than 1 kW from the nominal operating power and the spectrometer has been shown to have achieved stability over a desired time frame ( 3.2). Monitor updates can be performed for the corresponding time frame. 3.2 XRF Spectrometer 3.2.1 General All XRF instruments should be tested to ensure conformance to ISO/TR 18231 for instrument precision and detector linearity. Precision testing should be performed twice yearl
