DIN ISO 22309-2015 Microbeam analysis - Quantitative analysis using energy-dispersive spectrometry (EDS) for elements with an atomic number of 11 (Na) or above (ISO 22309 2011)《微光束.pdf

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1、November 2015English price group 14No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 71.040.99!%GF;“2363524www.din.de

2、DIN ISO 22309Microbeam analysis Quantitative analysis using energy-dispersive spectrometry (EDS) for elements with an atomic number of 11 (Na) or above (ISO 22309:2011),English translation of DIN ISO 22309:2015-11Mikrobereichsanalyse Quantitative Analyse mittels energiedispersiver Spektroskopie (EDS

3、) fr Elemente mit der Ordnungszahl 11 (Na) oder hher (ISO 22309:2011),Englische bersetzung von DIN ISO 22309:2015-11Analyse par microfaisceaux Analyse lmentaire quantitative par spectromtrie slection dnergie (EDS) des lments ayant un numro atomique de 11 (Na) ou plus (ISO 22309:2011),Traduction angl

4、aise de DIN ISO 22309:2015-11www.beuth.deDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.Document comprises 26 pages10.15 A comma is used as the decimal marker. Contents Page National foreword . 3 National Annex NA (informative) Bib

5、liography . 3 Introduction 4 1 Scope . 5 2 Normative references . 5 3 Terms and definitions 6 4 Specimen preparation 9 5 Preliminary precautions 10 6 Analysis procedure . 11 7 Data reduction 13 7.1 General. 13 7.2 Identification of peaks . 13 7.3 Estimation of peak intensity . 13 7.4 Calculation of

6、k-ratios . 14 7.5 Matrix effects 14 7.6 Use of reference materials . 14 7.7 Standardless analysis 14 7.8 Uncertainty of results 15 7.9 Reporting of results 16 Annex A (informative) The assignment of spectral peaks to their elements . 17 Annex B (informative) Peak identity/interferences . 19 Annex C

7、(informative) Factors affecting the uncertainty of a result . 21 Annex D (informative) Analysis of elements with atomic number 10.Guidance on the analysis of light elements with Z 10) in the specimen, its concentration can be determined by summing the appropriate proportions of concentrations of the

8、 other elements. This is often used for the analysis of oxygen in silicate mineral specimens.c) Calculation of concentration by difference where the light element percentage is 100 % minus the percentage sum of the analysed elements. This method is only possible with good beam-current stability and

9、a separate measurement of at least one reference specimen and it requires very accurate analysis of the other elements in the specimen.Annex D summarizes the problems of light element analysis, additional to those that exist for quantitative analysis of the heavier elements. If both EDS and waveleng

10、th 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 of the other issues are common to both techniques.2 Normative referencesThe following referenced documents are indispensable for the application of th

11、is document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 14594, Microbeam analysis Electron probe microanalysis Guidelines for the determination of experimental parameters for wavel

12、ength dispersive spectroscopyISO 15632:2002, Microbeam analysis Instrumental specification for energy dispersive Xray spectrometers with semiconductor detectorsISO 16700, Microbeam analysis Scanning electron microscopy Guidelines for calibrating image magnificationISO/IEC 17025:2005, General require

13、ments for the competence of testing and calibration laboratories5DIN ISO 22309:2015-113 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1absorption correctionmatrix correction arising from the loss of X-ray intensity from an element due to photoele

14、ctric absorption by all elements within the specimen while passing through it to the detector3.2accuracycloseness of agreement between the “true” value and the measured value3.3accelerating voltagepotential difference applied between the filament and anode in order to accelerate the electrons emitte

15、d from the sourceNOTE Accelerating voltage is expressed in kilovolts.3.4atomic number correctionmatrix correction which modifies intensity from each element in the specimen and standards to take account of electron backscattering and stopping power, the magnitudes of which are influenced by all the

16、elements in the analysed volume3.5beam currentelectron current contained within the beamNOTE Beam current is expressed in nanoamperes.3.6beam stabilityextent to which beam current varies during the course of an analysisNOTE Beam stability is expressed in percent per hour.3.7bremsstrahlungbackground

17、continuum of X-rays generated by the deceleration of electrons within the specimen3.8certified reference materialCRMreference material, one or more of whose property values are certified by a technically valid procedure, accompanied by or traceable to a certificate or other documentation which is is

18、sued by a certifying body3.9characteristic X-rayphoton of electromagnetic radiation created by the relaxation of an excited atomic state caused by inner shell ionization following inelastic scattering of an energetic electron, or by absorption of an X-ray photon6DIN ISO 22309:2015-113.10dead timetim

19、e that the system is unavailable to record a photon measurement because it is busy processing a previous eventNOTE This is frequently expressed as a percentage of the total time (see also live time).3.11energy-dispersive spectrometryEDSform of X-ray spectrometry in which the energy of individual pho

20、tons are measured and used to build up a digital histogram representing the distribution of X-rays with energy3.12electron probe microanalysisa technique of spatially resolved elemental analysis based on electron-excited X-ray spectrometry with a focused electron probe and an interaction/excitation

21、volume with micrometre to sub-micrometre dimensions3.13escape peakspeaks that occur as a result of loss of incident photon energy by fluorescence of the material of the detectorNOTE 1 These occur at an energy equal to that of the incident characteristic peak minus the energy of the X-ray line(s) emi

22、tted by the element(s) in the detector (1,734 keV for silicon).NOTE 2 They cannot occur below the critical excitation potential of the detector material, e.g. Si K escape does not occur for energies below 1,838 keV.3.14fluorescencephotoelectric absorption of any X-ray radiation (characteristic or br

23、emsstrahlung) by an atom which results in an excited atomic state which will de-excite with electron shell transitions and subsequent emission of an Auger electron or the characteristic X-ray of the absorbing atom3.15fluorescence correctionmatrix correction which modifies the intensity from each ele

24、ment in the specimen and standards to take account of excess X-rays generated from element “A” due to the absorption of characteristic X-rays from element “B” whose energy exceeds the critical (ionization) energy of “A”3.16full width at half maximumFWHMmeasure of the width of an X-ray peak in which

25、the background is first removed to reveal the complete peak profileNOTE FWHM is determined by measuring the width at half the maximum height.3.17incident beam energyenergy gained by the beam as a result of the potential applied between the filament and anode3.18k-rationet peak intensity (after backg

26、round subtraction) for an element found in the specimen, divided by the intensity, recorded or calculated, of the corresponding peak in the spectra of a reference material7DIN ISO 22309:2015-113.19live timetime the pulse measurement circuitry is available for the detection of X-ray photonsSee also d

27、ead time (3.10).NOTE 1 Live time is expressed in seconds (s).NOTE 2 Live time = real time for analysis dead time. Real time is the time that would be measured with a conventional clock. For an X-ray acquisition, the real time always exceeds the live time.3.20overvoltage ratioratio of the incident be

28、am energy to the critical excitation energy for a particular shell and sub-shell (K, LI, etc.) from which the characteristic X-ray is emitted3.21peak intensitytotal number of X-rays (counts) under the profile of a characteristic X-ray peak after background subtractionNOTE This is sometimes referred

29、to as the peak integral.3.22peak profiledetailed shape of a characteristic peak which depends on the relative intensities and energies of the individual X-ray emissions that are unresolved by the energy-dispersive spectrometer3.23precisioncloseness of agreement between the results obtained by applyi

30、ng the experimental procedure several times under prescribed conditions3.24quantitative EDSprocedure leading to the assignment of numerical values or expressions to represent the concentrations of elements measured within the analysis volume3.25reference materialRMmaterial or substance, one or more

31、properties of which are sufficiently well established to be used for the calibration of an apparatus, the assessment of a method, or for assigning values to materialsNOTE A reference material is said to be homogeneous with respect to a specified property if the property value, as determined by tests

32、 on specimens of specified size, is found to lie within the specified uncertainty limits, the specimens being taken either from a single or different supply unit.3.26repeatabilitycloseness of agreement between results of successive measurements of the same quantity carried out by the same method, by

33、 the same observer, with the same measuring instruments, in the same laboratory, at quite short intervals of time3.27reproducibilitycloseness of agreement between the result of measurements of the same quantity, where the individual measurements are made by different methods, with different measurin

34、g instruments, by different observers, in different laboratories, after intervals of time that are quite long compared with the duration of a single measurement, under different normal conditions of use of the instruments employedN1) National footnote: In the English version of ISO 22309:2011 these

35、units are presented as LI and LII, while in the German version of DIN ISO 22309:2015 they are presented as L and L . I IILII , N1)8DIN ISO 22309:2015-113.28resolutionenergy width of a peak measured by an energy-dispersive spectrometer and expressed as the peak width at half the maximum peak intensit

36、yNOTE This is usually expressed as the value for Mn K (5,894 keV), although peaks from other suitable elements can be used.3.29resolutionspatial spatial specificity of microanalysisNOTE This is usually expressed in terms of a linear or volumetric measure of the region of the specimen that is sampled

37、 by the measured characteristic radiation.3.30standardless analysisprocedure for quantitative X-ray microanalysis in which the reference peak intensity in the k-value expression (unknown/reference) is supplied from purely physical calculations or from stored data from a suite of reference materials,

38、 adjustments being made to match analysis conditions and augment incomplete reference data3.31sum peaksartefact peaks that occur as a result of pulse co-incidence effects that occur within the pulse pair resolution of the pile-up inspection circuitryNOTE These peaks appear at energies corresponding

39、to the sum of those energies of the two photons that arrive simultaneously at the detector.3.32traceabilityability to trace the history, application or location of an entity by means of recorded identifications3.33uncertaintythat part of the expression of the result of a measurement that states the

40、range of values within which the “true” value is estimated to lie for a stated probability3.34validationconfirmation by examination and provision of objective evidence that the particular requirements for a specific intended use are fulfilled3.35X-ray absorptionattenuation of X-rays passing through

41、matter, arising primarily from photoelectric absorption for X-ray energies and ranges appropriate to EPMA/EDS and SEM/EDS4 Specimen preparation4.1 Material for analysis shall be stable under variable pressure conditions and the electron beam. As-received specimens can be examined after simple cleani

42、ng, but surface inhomogeneity or topography will adversely affect the quality of the quantitative analysis.4.2 For reliable quantitative analysis, the specimen shall present a flat, smooth surface normal to the electron beam. This requirement is usually met by the application of conventional metallo

43、graphic or petrographic techniques. The area for analysis should be homogeneous over a region, typically a few micrometres in diameter, around the electron beam.9DIN ISO 22309:2015-114.3 Solid specimens can be reduced to an appropriate size, making sure they undergo no transformation during the proc

44、ess. Prior to examination in the as-received condition, all surface debris should be removed using appropriate techniques, such as ultrasonic cleaning.4.4 Specimens for sectioning should be embedded, where possible, in a conducting medium prior to metallographic or petrographic polishing using stand

45、ard procedures. The medium shall be chosen with care, to avoid the possibility of the conducting component becoming smeared onto the specimen surface and being mistaken for a component of the specimen by effectively altering the composition of the analysed volume.NOTE 1 Polishing may be carried thro

46、ugh to 1/4 m grade diamond, provided this can be done without introducing relief effects. Complete removal of all scratches is not essential, provided areas for analysis are clean and relief-free.Damage to the specimen during preparation should be avoided. Potential damage mechanisms include:a) the

47、effects of lubricant;b) the removal of second phases (precipitates);c) differential polishing of phases with different hardness, thus introducing relief to the surface;d) strain introduced into the surface;e) edge curvature.With cross-sections, the specimen can be coated with a harder material to im

48、prove edge retention.NOTE 2 See ASTM E39for further guidance.4.5 If optical examination is to be used for the location of areas for analysis, either prior to or while in the instrument, etching of the specimen may be necessary. The depth of etching should be kept to a minimum, being aware of the pos

49、sibility of surface compositional changes or the development of undesirable topographic effects. Polishing away the etching may be needed after locating and marking the regions for analysis by reference to existing or added features, such as a scratch or hardness indent.4.6 The specimen should have a good conductivity to avoid charge-up generated by electron beam irradiation. The specimen shall be connected to the instrument ground either through a conducting mount, or by