ISO-22309-2006.pdf
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1、 Reference number ISO 22309:2006(E) ISO 2006 INTERNATIONAL STANDARD ISO 22309 First edition 2006-04-15 Microbeam analysis Quantitative analysis using energy-dispersive spectrometry (EDS) Analyse par microfaisceaux Analyse lmentaire quantitative par spectromtrie slection dnergie (EDS) Copyright Inter
2、national Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 09:06:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 22309:2006(E) PDF disclaimer This PDF file may contain embedded typefaces.
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5、or printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2006 All rights reserved. Unless otherwise specified, no part o
6、f 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 the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 C
7、H-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 2006 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale,
8、 04/16/2007 09:06:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 22309:2006(E) ISO 2006 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references. 2 3 Terms and definitions. 2 4 Specimen preparation 6 5 Preliminary precautio
9、ns. 7 6 Analysis procedure. 7 7 Data reduction. 9 7.1 General. 9 7.2 Identification of peaks 9 7.3 Estimation of peak intensity 9 7.4 Calculation of k-ratios 10 7.5 Matrix effects. 10 7.6 Use of reference materials. 10 7.7 Standardless analysis 11 7.8 Uncertainty of results. 11 7.9 Reporting of resu
10、lts 12 Annex A (informative) The assignment of spectral peaks to their elements. 14 Annex B (informative) Peak identity/interferences . 16 Annex C (informative) Factors affecting the uncertainty of a result. 18 Annex D (informative) Analysis of elements with atomic number 10. Guidance on the analysi
11、s of light elements with Z 10) in the specimen, its concentration can be determined by summing the appropriate proportions of concentrations of the other elements. This is often used for the analysis of oxygen in silicate mineral specimens. c) Calculation of concentration by difference where the lig
12、ht element percentage is 100 % minus the percentage sum of the analysed elements. This method is only possible with good beam-current stability and a separate measurement of at least one reference specimen and it requires very accurate analysis of the other elements in the specimen. Annex D summaris
13、es the problems of light element analysis, additional to those that exist for quantitative analysis of the heavier elements. If both EDS and wavelength spectrometry (WDS) are available, then WDS can be used to overcome the problems of peak overlap that occur with EDS at low energies. However, many o
14、f the other issues are common to both techniques. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 09:06:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 22309:2006
15、(E) 2 ISO 2006 All rights reserved 2 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 the referenced document (including any amendments)
16、applies. ISO 14594, Microbeam analysis Electron probe microanalysis Guidelines for the determination of experimental parameters for wavelength dispersive spectroscopy ISO 15632:2002, Microbeam analysis Instrumental specification for energy dispersive X-ray spectrometers with semiconductor detectors
17、ISO 16700:2004, Microbeam analysis Scanning electron microscopy Guidelines for calibrating image magnification ISO/IEC 17025:2005, General requirements for the competence of testing and calibration laboratories 3 Terms and definitions For the purposes of this document, the following terms and defini
18、tions apply. 3.1 absorption correction matrix correction arising from the loss of X-ray intensity from an element due to photoelectric absorption by all elements within the specimen while passing through it to the detector 3.2 accuracy closeness of agreement between the “true” value and the measured
19、 value 3.3 accelerating voltage potential difference applied between the filament and anode in order to accelerate the electrons emitted from the source NOTE Accelerating voltage is expressed in kilovolts. 3.4 atomic number correction matrix correction which modifies intensity from each element in t
20、he specimen and standards to take account of electron backscattering and stopping power, the magnitudes of which are influenced by all the elements in the analysed volume 3.5 beam current electron current contained within the beam NOTE Beam current is expressed in nanoamperes. 3.6 beam stability ext
21、ent to which beam current varies during the course of an analysis NOTE Beam stability is expressed in percent per hour. 3.7 bremsstrahlung background continuum of X-rays generated by the deceleration of electrons within the specimen Copyright International Organization for Standardization Provided b
22、y IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/16/2007 09:06:15 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 22309:2006(E) ISO 2006 All rights reserved 3 3.8 certified reference material CRM reference material, one or more of whose prop
23、erty values are certified by a technically valid procedure, accompanied by or traceable to a certificate or other documentation which is issued by a certifying body 3.9 characteristic X-ray photon of electromagnetic radiation created by the relaxation of an excited atomic state caused by inner shell
24、 ionisation following inelastic scattering of an energetic electron, or by absorption of an X-ray photon 3.10 dead time the time that the system is unavailable to record a photon measurement because it is busy processing a previous event NOTE This is frequently expressed as a percentage of the total
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