BS-ISO-15632-2002.pdf

BRITISH STANDARD BS ISO 15632:2002 M i c r o b e a m a n a l y s i s Instrumental specification for energy dispersive X-ray spectrometers with semiconductor detectors ICS 71.040.99 ? Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 15632:2002 This British Standard, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 19 December 2002 © BSI 19 December 2002 ISBN 0 580 40967 8 National foreword This British Standard reproduces verbatim ISO 15632:2002 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee CII/9, Microbeam analysis, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 8, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 15632 First edition 2002-12-01 Reference number ISO 15632:2002(E) Microbeam analysis Instrumental specification for energy dispersive X-ray spectrometers with semiconductor detectors Analyse par microfaisceaux Spécifications instrumentales pour spectromètres à rayons X à dispersion d'énergie avec détecteurs à semiconducteurs BS ISO 15632:2002 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO :23651(2002)E ii© ISO 2002 Ar llithgr seresvde FDP dicslaimre This FDP fam elitnoc yt deddebme niayfep.seca In roccatiw ecnadA hycilop gnisnecil s'ebod, thf sim eliarp eb ytnieiv ro dewb detu sllah ton eb tidesselnu de tt ehyfepseca hwich rae meil era deddebct desneo tsni dnalat no delmoc ehtupre epfrromign tide ehti.gn In odaolnwt gnidhis file, rapticca setpe trehiet neh serilibisnopty fo ton fniris'ebodA gnign ilop gnisnecilcy. 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ISO copyrithg fofiec tsop esaCael 65 G 1121-HCeneva 02 Te.l + 22 14 10 947 11 Fax + 14 47 2290 9 74 E-liam copyrightsio.ch Web wwwsi.oc.h Prni detni Sztiwerldna BS ISO 15632:2002 ii Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 36512002:2)E( © ISO 2002 r llAithgs reservde iii 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 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 take part in the work. ISO collaborates closely with 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 3. Draft International 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 International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 15632 was prepared by Technical Committee ISO/TC 202, Microbeam analysis. Annexes A and B form a normative part of this International Standard. BS ISO 15632:2002 iii Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO :23651(2002)E vi© ISO 2002 Ar llithgr seresvde Introduction Recent progress in energy dispersive X-ray spectrometry (EDS) by means of improved manufacturing technologies for detector crystals, new materials for the detector's X-ray entrance window and the application of advanced pulse processing techniques have increased the general performance of spectrometers and extended their application to low energies (below ). In the past, a spectrometer was commonly specified by its energy resolution at high energies defined as the full width at half maximum (FWHM) of the Mn-K line. To specify the properties in the low energy range, values for the FWHM of C-K, F-K or the zero peak are given by the manufacturers. Some manufacturers also specify a peak to background ratio, which may be defined as a peak to shelf ratio in a spectrum from an Fe55 source or as peak to valley ratio in a boron spectrum. Definitions of the same quantity may be different. The sensitivity of the spectrometer at low energies related to that at high energies depends strongly on the construction of the detector crystal and the X-ray entrance window used. Although high sensitivity at low energies is important for the application of the spectrometer in the analysis of light element compounds, normally the manufacturers do not specify an energy dependence for spectrometer efficiency. This International Standard was developed in response to a worldwide demand for minimum specifications of EDS spectrometers. EDS is one of the most applied methods used to analyse the chemical composition of solids and thin films. This International Standard should permit comparison of the performance of different spectrometer designs on the basis of a uniform specification and help to find the optimum spectrometer for a particular task. In addition, this International Standard contributes to the equalization of performances in separate test laboratories. In accordance with ISO/IEC 17025, such laboratories have to periodically check the calibration status of their equipment according to a defined procedure. This International Standard may serve as a guide for similar procedures in all relevant test laboratories. 1 keV BS ISO 15632:2002 iv Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ANRETNIITOTS LANDNADRAISO 36512002:2)E( © ISO 2002 r llAithgs reservde 1 Microbeam analysis Instrumental specification for energy dispersive X-ray spectrometers with semiconductor detectors 1Scope This International Standard defines the most important quantities that characterize an energy dispersive X-ray spectrometer (EDS) consisting of a semiconductor detector, a pre-amplifier and a signal processing unit as the essential parts. This International Standard is only applicable to spectrometers with semiconductor detectors operating on the principle of solid state ionization. This International Standard specifies minimum requirements for such spectrometers attached to an electron probe microanalyser (EPMA) or a scanning electron microscope (SEM). Realization of the analysis is outside the scope of this International Standard. 2Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. NOTEWith exception of 2.1 these definitions are given in the same or analogous form in ISO 18115. 2.1 energy dispersive spectrometer spectrometer that records the whole X-ray spectrum simultaneously NOTEThe spectrometer consists of a solid state detector, a preamplifier and a pulse processor to convert the X-ray photons in electronic pulses, pulse height analysis being used to sort the pulses formed by the processor according to X-ray energy in spectral channels. 2.2 spectral channel interval of the measured energy for a measured spectrum with a width defined by a regular energy increment 2.3 instrumental detection efficiency ratio of quantity of detected photons and quantity of the photons available for measurement 2.4 signal intensity strength of the signal in counts per channel or counts per second per channel at the spectrometer output after pulse processing 2.5 peak intensity signal intensity of a spectral peak measured as height of the peak above a defined background 2.6 peak area net peak area area under a peak in a spectrum after background removal 2.7 background signal signal present in a spectral channel due to bremsstrahlung or instrumental background BS ISO 15632:2002 1 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO :23651(2002)E 2© ISO 2002 Ar llithgr seresvde 2.8 background, instrumental signal contribution, generally unwanted, arising from one or more parts of the spectrometer, which adds to that emitted from the sample, so distorting the measured spectrum 3Requirements 3.1General description The manufacturer shall describe, using appropriate reference texts, the essential constructive elements of the spectrometer in order to permit the user to evaluate the performance of the spectrometer. Constructive elements that are indispensable for the evaluation of the suitability of a spectrometer for a certain field of applications shall be given explicitly. These are the type of crystal material (silicon or germanium), the thickness of the crystal, the active crystal area and the type of the window (beryllium, thin film window or windowless). Parameters which may not be encompassed by this International Standard, but that may influence detector performance; e.g. maximum count rates, construction principle of cooling etc. shall be explained in the reference text. 3.2Energy resolution The energy resolution shall be specified as FWHM of the Mn-K peak and determined in accordance with annex A. Spectrometers that claim detection of X-rays lower than shall also be specified by the FWHM of the C-K and the F-K lines. The specified FWHM shall be an upper limit. The resolution determined in accordance with annex A is guaranteed to be less than the specified value. The resolution figure shall be accompanied by a statement of count rate for which the specification is valid (e.g. . 3.3Peak to background ratio The peak to background ratio shall be derived from an acquired spectrum of an 55Fe source as a characteristic spectrometer parameter. The ratio shall be given by the peak intensity of the Mn-K line divided by the instrumental background. The instrumental background shall be calculated as the mean number of counts per channel within the energy range from to . Sufficient counts shall be recorded in the spectrum to make the measure statistically significant and the electronics shall be set up to be effective in responding to pulses produced by signals in the to energy band. NOTE 1The peak to background ratio depends on spectrometer resolution. Therefore, the ratio is only relevant for the comparison of spectrometers with similar resolution performance. NOTE 2In an electron microscope, the bremsstrahlung background from a manganese specimen may be considerably greater than the instrumental background, due to degraded events. Therefore, a manganese specimen cannot be used to measure the peak to background ratio. 3.4Energy dependence of instrumental detection efficiency The minimum specification for the energy dependence of the instrumental detection efficiency shall be the intensity ratio of a low energy line and a high energy line in the characteristic X-ray spectrum of a given material. This ratio shall be given as the net peak area ratio of the L series and K lines in the spectrum of a pure nickel or copper specimen, excited by a electron beam perpendicular to the specimen surface and collected by the detector at a take-off angle of . NOTE 1These measures are only appropriate for a detector thick enough to absorb at least of the incident X-ray energy at . NOTE 2If the specimen chamber containing ports to fix the detector does not allow a take-off angle of , the L/K ratio at any other take-off angle can be converted to that for by applying the absorption correction formalism of quantitative electron probe microanalysis (see annex B). 1 KeV 1 000 counts/s 0,91,1 KeV 100 % 0,91,1 KeV 20 keV 35 95 % 8 keV 35 35 BS ISO 15632:2002 2 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 06:03:51 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 36512002:2)E( © ISO 2002 r llAithgs reservde 3 Annex A (normative) Measurement of line widths (FWHM) to determine the energy resolution of the spectrometer A.1Specimens Specimens shall be an encapsulated 55Fe source to measure the manganese K line and a polytetrafluoroethylene (PTFE, Teflon®) piece or foil for the carbon and fluorine K lines. In order to check the FWHMs in the user laboratory, a polished manganese specimen can be used if 55Fe is not available or may not be used in the laboratory due to safety regulations. Alternatives to PTFE to measure the carbon and fluorine K-lines are respectively glassy carbon and a fluorine-containing mineral such as CaF2. A.2Specimen preparation The PTFE specimen sha