X-Ray Spectral Variability Signatures of Flares in BL Lac Objects

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X-ray Spectrometry

X-ray Spectrometry

X-ray SpectrometryImre Szalo´kiInstitute of Experimental Physics,University of Debrecen,Bem te´r18/a,H-4026Debrecen,HungaryJa´nos Osa´nHungarian Academy of Sciences,KFKI Atomic Energy Research Institute,P.O.Box.49,H-1525Budapest,Hungary Rene´E.Van Grieken*Department of Chemistry,University of Antwerp,B-2610Antwerp,BelgiumReview ContentsOverview4069 Detection4071 Instrumentation and X-ray Optics4074 Quantification and Fundamental Data4078 Tomography,Holography,and X-ray Scattering4081 Total Reflection X-ray Fluorescence Analysis4083 Electron Probe Microanalysis4084 Particle-Induced X-ray Emission4086 X-ray Absorption Spectrometry4087 Applications4089 Sample Preparation4089ED-XRF4089Micro-XRF4089TXRF4090EPMA4090PIXE4091XAS4092Standards4093 Literature Cited4093OVERVIEWIn this review,we focus on the most significant and essential progress in X-ray spectrometry(XRS),published in the period 2004-2005,covering the developments and improvements in the performance of detection and instrumentation of X-ray techniques and X-ray optics,new quantification models in X-ray spectra and data evaluation,calculation and experimental determination of fundamental atomic data,tomography and holography methods for2D or3D imaging of microstructures,electron probe micro-analysis(EPMA),total reflection X-ray fluorescence(TXRF), particle-induced X-ray emission(PIXE)analysis,and X-ray absorp-tion spectrometry(XAS).Finally,different applications in each subfield of XRS are shown.This review involves only a selected minority of the published papers and we try to look over the current trends in this analytical field with a critically selected citing of papers,to support the research activity of the community of X-ray scientists.Since our last review,an international group of scientists published two overviews on XRS(A1,A2)in the Journal of Analytical Atomic Spectrometry,covering the period2003-2004 in the main field of this analytical spectroscopic method and instruments.These review articles involve all the important sections of XRS in nine chapters:reviews,instrumentation, spectrum analysis,matrix correction and calibration,X-ray optics and microfluorescence,synchrotron radiation,TXRF,portable and mobile X-ray fluorescence(XRF),and on-line XRF and applications. In the present review,we follow another way for classification of the information published in the literature in the2004-2005 period:detection,instrumentation(except of detectors)and optics,quantification models and related fundamental data,to-mography,and holography methods as the main tool of X-ray imaging,TXRF,EPMA,PIXE,XAS,and a final chapter that reviews the application of these methods in geology,environmen-tal research,industry,biology.and medicine.Current trends in pixel-type detectors were reviewed by Wermes(A3)showing their necessity in X-ray imaging devices,radiography,autoradiography, protein crystallography,and X-ray astrophysics research.The fundamental aims of R&D activity in the field of detectors are to arrange less material in the detector bulk,to build high-speed readout electronics,and to construct large radiation-tolerant detectors.The author describes the working principle and structure of different categories of pixilated detectors:hybrid pixel detectors when the sensor module and the electronic chips are connected by short bumps,diamond detectors and their applica-tions for protein crystallography and radiography.The author describes the dream of the detector developer:a fully monolithic pixilated detector where both the sensor bulk and the electronic circuits are in one entity and these devices can be produced by commercially available technology,and he outlines that this will not be possible in the future due to the lack of proper technology.In the past decade,the greatest hit in XRS was probably the cryogenically cooled quantum detectors such as superconductive tunnel junction(STJ),transition edge sensors(TESs),and micro-calorimeters.These provide excellent energy resolution for a wide range of X-ray energies,from the optical range up to several kiloelectronvolts.Kurakado published(A4)a short characteriza-tion about nonequilibrium superconductivity and STJ detectors. The tutorial paper introduces the reader into the main features, such as high count rate capability,stability against temperature fluctuation,ultra-high-energy resolution,and the working principle of the STJs.The most common Nb/Al/AlOx/Al/Nb structure has excellent working parameters and very high stability against temperature variation from50to500mK.A100×100µm2AlAnal.Chem.2006,78,406910.1021/ac060688j CCC:$33.50©2006American Chemical Society Analytical Chemistry,Vol.78,No.12,June15,20064069 Published on Web00/00/0000STJ located on a Si3N4membrane,covered by a1.3-µm-thick Pb absorber,was described;this device had an energy resolution of 12.4eV and the noise was4eV at5.9-keV X-ray nkosz et al.(A5)reviewed quantitative X-ray microanalysis for biological and glass material samples in order to verify the fundamental parameter method on the basis of the application of standard samples.The principal aim of their investigation was to determine the analytical capability of a microbeam(X-ray beam diameter of ∼30µm)XRF spectrometer equipped with capillary optics.They considered all the possible sources of uncertainty of the whole analysis:operating stability of the detector and X-ray source, sample movement,and errors originating from the spectral deconvolution calculations.The sample thickness was estimated on the basis of the measurement of the elastic and inelastic scattered intensities of the source radiation,and it was applied for the matrix correction as well.The authors demonstrate their analytical considerations and calculations by some examples using the synchrotron microbeam XRF technique for quantitative analysis of human brain tissue samples with both monoenergetic and polychromatic excitation modes.The accuracy for glass standard samples was found between4and40%relative. Janulewicz et al.(A6)reviewed the state-of-the-art of the tabletop type X-ray lasers(XRLs)and described the working principle of these lasers and their characteristic spectral output properties, from a practical point of view.They concluded that the XRL sources are competitive in comparison with the third-generation synchrotron radiation(SR)facilities:brilliance of the beam and time-resolved measurements.The author details the operating processes of two types of XRFs based on the quantum pumping mechanisms in generating the excitation states:(i)recombination and(ii)collisional-type XRLs.The size of the XRLs is the central problem in development research;it can be decreased in the case of a hybrid-type XRL,when the pumping medium is gas plasma in a capillary tube in which the inverse population is generated by a short picosecond optical laser beam,entering into the axial direction of the capillary.Most observed objects in the sky naturally emit X-ray radiation that transports information on the atomic-level processes occurring in the source objects,on the motion of the bulk material,etc.,or the transmission of X-rays through absorption can be studied.Therefore,the detectors of X-ray telescopes are the central devices in the sky observatories, such as Chandra and XMM-Newton.Porter reviewed(A7)the low-temperature detectors developed for space missions such as X-ray cameras and dispersive X-ray spectrometers.The Astro-E2 launched in2005was the first mission that contained a low-temperature microcalorimeter-based observatory,and three more low-temperature detector-based observatories are being developed (NeXT,Constellation-X,ZEUS).Due to the high-level ionization of the individual atoms in different sky objects,very complex X-ray emission spectra must be detected resolving the satellite lines. The newest spectrometers that suit this requirement are high-energy resolution microcalorimeters.The other essential group of X-ray detectors are the CCD cameras;these have moderate spectral sensitivity and therefore they have to be used with selective absorbing filters for energy-sensitive X-ray imaging.In the future observatories,new detector types are needed,which have∼1000pixels with a high-energy resolution below4eV at 6-keV X-ray energy,in a miniature,monolithic arraying form,having three-dimension wiring layers,cryogenic multiplexing schemes,complex and flexible electronics,and finally an as low as possible mass.SR is widely used for all fields of XRS for the characterization of materials for basic research and for practical aims.In view of the lack of a detailed description of this analytical technique for the nonsynchrotron-expert forensic community,Kempson and co-workers(A8)published a review paper on application of synchro-tron radiation in forensic trace analysis.The authors pointed out the benefits of SR and discuss XRF techniques,described the tomographic method,X-ray diffraction,and scattering applications, and finally,they highlighted the X-ray absorption near edge structure(XANES)and extended X-ray absorption fine-structure (EXAFS)methods and their significant contribution to the characterization of materials.They outlined the unique advanta-geous spectroscopic characters of the synchrotron beams:high brightness,energy tenability,nearly100%of polarization and coherence,and possibility of time-resolved measurements;finally they showed some examples demonstrating the benefit of ap-plication of the SR in this practical field.A general tutorial paper was published by Van der Veen and Pfeiffer(A9)about the properties of coherent hard X-ray beams and their use in structural analysis of solid materials.Because of a fully coherent X-ray beam is provided by SR,it is suitable for such experiments where the interference of the X-ray beam gives information on the inner structure of the investigated object material.In the near-forward scattering direction,the differences in the phases between waves traversing different parts of the object enable imaging the object structure into a phase contrast. In larger scattering angles the interference provides coherent diffractive imaging without lenses and it is called holography without reference beam.The authors give a simple mathematical description of the investigated effects:transverse coherence, longitudinal coherence,phase contrast,X-ray photon correlation spectroscopy,diffracting imaging,and waveguide analysis on the basis of the Fraunhoffer diffraction pattern.In this last review period,an increasing number of papers were published on the1D and2D waveguides due to the strong needs of a microsized X-ray beam,which has a high flux density,for the analysis of submicrometer-sized objects.Egorov and Egorov published a tutorial on state-of-art of X-ray waveguides(A10),with the general description of the operating principles and the spectroscopic characteristic properties and possible applications.X-ray microanalytical methods are more widely applied in archaeometry and in cultural heritage conservation research, especially nondestructive micro-X-ray analytical methods.Selected presentations of the7th International Conference on Nondestruc-tive Testing and Microanalysis for the Diagnosis and Conservation of the Cultural and Environmental Heritage,dealing with different types of instrumental analysis of materials and artifacts of cultural-historical value,were published in Cultural Heritage Conservation and Environmental Impact Assessment by Non-Destructive Testing and Micro-Analysis(A11).The publication gives a survey of the possible solutions for analytical problems in the cultural heritage sector,using portable energy-dispersive XRF spectrometers, TXRF,microfocus X-ray tomography,confocal micro-XRF,and micro-XAS.4070Analytical Chemistry,Vol.78,No.12,June15,2006The in-field analysis of hazardous material and environ-mental samples obviously requires portable XRF spectrometers. Melquiades and Appoloni published a review article(A12)about the basic methodology aspects of laboratory and portable X-ray boratory measurements can be slow,sometimes laborious,and of course more expensive;however,they are more precise in comparison with portable XRF spectrometers.The use of portable spectrometers allows rapid mapping and ranking of contaminated sites,and a large number of semiquantitative data can be generated on site in nearly real time.The authors overview the possible detector types that are suitable for the portable technique and concluded that the Peltier cooled detectors(Si-PIN,CdZnTe,Si drift)are the most appropriate devices because no cryogenic cooling is required.The most significant applications and portable designs were summarized in a separate table involving the characteristic parameters:excitation source,re-quired sample preparation technique,possible matrixes for sample bulk,and minimum detection levels for different elements.The authors give some examples for applications published in the literature,and they discuss the main steps of in-field analysis such as preconcentration techniques and data evaluation methods. Finally,in this introductory section,we mention an article about the direct analysis of biological samples applying TXRF analysis, published Marco and Herna´ndez-Caraballo(A13).They claim that, for the purpose of direct analysis of biological origin samples,the most suitable XRS method is TXRF due to the limited matrix effect and the multielement character.TXRF is used mostly after a sample digestion procedure;however,in some cases,the biologi-cal wet samples can be analyzed without preparation due to the low matrix interference.This technique has advantageous proper-ties such as shorter analysis time,low reagent consumption,and simplified analysis procedure.DETECTIONCryogenic energy-dispersive(ED)detectors have a superior energy resolution due to the very low operating temperature,that reduces the thermal noise,and to the appearance of low excitation states of electron energies.The working principle is based on the fact that one absorbed X-ray photon(the energy is∼1keV) generates an∼100times higher number of charge carriers in the superconductive-type detectors than in conventional Si sensors. This effect leads to the excellent2-4-eV energy resolution in the X-ray energy range of several kiloelectronvolts,while the best energy resolution of the conventional Si(Li)detectors is∼120eV at5.9-keV energy.The microcalorimeters are principally very sensitive solid-state thermometers changing their temperature through the absorption of X-ray energy quanta.The construction of the STJs is based on two superconductive electrodes separated by a tunneling barrier.The tunneling current between the electrodes depends on the absorbed X-ray energy in the barrier layer,and this changing of current can be applied as a signal of detected X-ray quanta.Metallic magnetic calorimeters(MMC)for high-resolution XRS were developed by Fleischmann and co-workers(B1);they show an fwhm of3.4eV for X-ray energies up to6.5keV.This type of detector is based on a paramagnetic sensor placed in a magnetic field and in contact with a metallic absorber. The magnetization of the sensor indicates the temperature of the absorber calorimeter.The spectroscopic capability of this cryo-genic MMC detector was demonstrated by55Fe spectra with separation of the Mn-K R1and Mn-K R2peaks.A German physics research group(B2)developed a prototype of a new construction of an STJ detector having two thin electrode layers separated by a thin tunnel barrier,and on this layer a lead absorber is layered. Due to the high absorption properties of the Pb layer,the quantum efficiency of the STJ detector increased considerably from1%up to50%of X-ray energy of6keV.This structure helps reduce the doubling of the peaks.The achieved energy resolution of the detector was10.8eV at an energy of5.9keV,at a working temperature of70mK.The authors are going to install this type of detector into a new high-resolution cryogenic spectrometer used in an electron microscope.The microcalorimeters offer the most impressive energy resolution,2-3eV,in the energy range of2-6 keV(B3).However,their detectable count rate is low,∼500 counts/s.In contrast with these operating properties the STJs have a little bit less resolution capability,which is∼3-12eV in the energy range of2-6keV,but their maximum count rate should be10times higher than in the case of the microcalorimeters.The authors developed a new STJ with structure of Nb-Al-AlO x-Al-Nb for high count rate detection of synchrotron radiation. They produced an impressive count rate at10000counts/s with an energy resolution between7and15eV fwmh.Their device was able to detect100000counts/s as well,but then the energy resolution deteriorated to43eV.The first industrially applied spectrometer was reviewed by Hollerith et al.(B4),who used an Ir/Au TES in a scanning electron microscopy(SEM).The superconductor layer of the detector is 400×400mm2with a250×250mm2Au absorber with a thickness of500nm.Due to the500times smaller detector area of this TES compared to the conventional Si(Li)detectors,the solid angle has to be decreased by mounting a polycapillary lens in front of the Ir/Au ing this X-ray optics,the detectable count rate was improved by a factor of5at the Si-K R energy.Three American authors(B5)outlined the general and specific properties of the microcalorimeters and their applicability to SEM analysis.They called the attention to the following facts:(i)the spectral resolution of the microcalorimeters is better than the best alternative detection technology in wavelength-dispersive spec-trometry(WDS),(ii)this energy-dispersive property is signifi-cantly better than what Si(Li)technology can provide,(iii)the detection efficiency is between Si(Li)and WDS modes,(iv)the disadvantageous detection characters of this cryogenic detector are the limited count rate and the limited geometrical efficiency capabilities compared to WDS and Si(Li)detection.These nonideal working characteristics can be avoided by the development of appropriate microcalorimeter array detector system that should be the ideal detector for EPMA of low atomic number elements. Bechstein and co-workers(B6)characterized a cryogenic super-conductive tunnel junction detector set that consists of Nb/Al/ AlO x/Al/Nb layers segmented in four individual structures having an area between70×70µm2and200×200µm2.The aim of their investigation was to clarify the dependence of the detection efficiency and the energy resolution properties on the impinging X-ray energy(up to1500eV)and the count rate and its influence on the detector response function.The X-ray microbeam had a 5-µm diameter,and this size allowed scanning the beam vertically and irradiating different parts of the detector surface.The authorsAnalytical Chemistry,Vol.78,No.12,June15,20064071found an unexpected degradation of the energy resolution in a wide edge zone.The laterally resolved measurements provide a better understanding of the physical processes in STJs and promote design of an improved detector layout.A Japanese research group(B7)developed a new design for a set of STJ detectors,capable of providing multispectra of X-rays for purposes of X-ray computer tomography in the energy range below1keV. The typical size of each individual STJ on the multipixel chip is ∼100×100µm2.An energy resolution of41eV fwhm was observed at5.9-keV energy,and that value is three times better than the theoretical limit of conventional Si detectors.The authors carried out experiments with their STJ chip in the5-25-keV energy range and concluded that this type of cryogenic detector is a promising candidate for3-D X-ray absorption and fluorescence CT imaging.Bruijn et al.reported(B8)a new development of a cryogenic5×5matrix-shaped array of microcalorimeters using Ti/Au TES with Cu/Bi absorber and Si3N4cooling connector.The array was tested with irradiation of5.9-keV monoenergetic X-ray, and the response spectra had a6-7eV fwhm.An Italian research group reviewed(B9)a similar experiment with TES that consists of a300×400µm2thin and25-µm-thick polycrystalline Sn foil acting as an energy absorber.The TES surface was protected against possible chemical damaging during the photolithographic procedure.The TES microcalorimeter was tested at radiation beamline GILDA of the European Synchrotron Radiation Facility (ESRF),detecting X-ray fluorescence spectra emitted by a Renais-sance gold luster on ceramic;during this analysis,the energy resolution of the TES was found to be70eV between6-and9-keV X-ray energy.On the basis of their experimental results,the authors concluded that the TES calorimeters are very applicable for the synchrotron based X-ray fluorescence analysis.A special monolithic X-ray detector based on the connection of an SDD and a CsI(Tl)scintillation device was reviewed by Marisaldi et al. (B10).In this coupled detector,the SDD worked as a direct X-ray sensor for photons that interacted in the Si body of the SDD and in parallel as a photodetector for photons generated in the scintillation crystal.The source of the electronic signal is dis-criminated on the basis of the pulse shape evaluation and that process yields the correct determination of the deposited photon energy in the complex detector for both X-ray andγ-ray energy ranges.The authors systematically tested the dependence of the detector efficiency on the operating temperature and found that, at10°C,the energy efficiency is nearly100%for the8-200keV of energy range.They concluded that this type of combined detector would be of great interest in X-andγ-ray detection in astrophysics due to the advantageous spectroscopic capabilities, i.e.,the high detection efficiency from low-energy X-rays up to several hundred kiloelectronvolts.Goulon et al.published(B11) the spectroscopic properties of their advanced detector systems, especially SDD arrays,used for XRF spectrometry at the ID12 beamline in ESRF in Grenoble in the last15years.An improved energy resolution was achieved during this period:82eV at Si-K R and126eV at Fe-K R,by means of mathematical spectral deconvolution.Now,the SDD has become a commercial detector in varying sizes and shapes,in large array form,including200-400detection channels for different applications of conventional and specific X-ray emission analysis such as XRF tomography and holography or EXAFS analysis.They discussed the use of SDD as ED detectors,the modes of minimization of the electronic readout noise,and the first result of a35-element SDD array consisting of7×7individual cylindrical SDDs.A special annular SDD,developed for PIXE analysis,was tested and reviewed(B12). PIXE always suffers from the small solid angle of detection; therefore,this new Peltier-cooled SDD was designed with annular shape in order to maximize the detection angle.The area of the detector is60mm2,and the working distance is only1mm.This commercial ED detector is able to collect at high rate of1 Mcounts/s with an energy resolution better than200eV at6.4-keV X-ray energy.In comparison with conventional Si(Li)detec-tors,the solid angle and the count rate capability are both larger by2orders of magnitude.A novel SDD with integrated FET was published by Lechner and co-workers(B13);it has a new chip layout that allows constructing the readout anode in a smaller size than earlier designed,which reduced the anode capacitance of120fF instead of200-250fF in the case of commercial SDDs. This improved detector structure and properties yielded a better energy resolution:147eV at5.9-keV X-ray energy at-10°C detector temperature.On the basis of these results,the authors proposed a new SDD device with increased effective area in order to achieve higher geometrical efficiency.Eggert and colleagues (B14)also studied the improvement possibilities of SDDs with enlarged active detector surface area,from5to10mm2;that required more intensive cooling from-15°C down to-20°C, reducing the leakage current that causes degradation of the energy resolution.On the basis of their experimental results,they concluded that instead of enlargement of the active area of the SDD detector a group of segmented detectors with a small(5 mm2)sensitive surface is more reasonable to apply.On the other hand,in cases when a low count rate is available,a large sensitive area is more reasonable.The research group of Sokolov reviewed their results(B15)of systematic study about Si(Li),Si PIN,and CdZnTe X-ray detectors,cooled by Peltier effect devices in order to develop a portable ED X-ray spectrometer.They found that the spectroscopic characters of the Peltier-cooled Si(Li)detector was similar to those of detector cooled with liquid nitrogen,and it was selected as the most suitable type of detector for XRF analysis.They showed in this article illustrative spectra from the studied semiconductor detectors using55Fe and241Am radioactive sources.Streli and co-workers(B16)published their experimental comparison of Si(Li)detectors and SDD equipped both with a thin polymer window in order to detect low X-ray energies from 200eV.With the Si(Li),it was possible to detect down to the C K R and the limit for SDD was O.The detection limit for this latter element was found to be36ng in the case of SDD and4ng for a Si(Li)detector,which shows the better applicability of the Si(Li) detector for XRF analysis of low-Z elements.Their results suggest that the SDDs should be a promising candidate as a future detection device for low atomic X-ray radiation especially at the case of a high X-ray flux.In ref B17,Wright et al.emphasized that there is a strong demand for more efficient,more radiation-tolerant sensors in X-andγ-ray physics,SR applications and medical imaging.For these detection tasks,an excellent solution is offered by the3-D detector architecture in which the electrodes traverse the detector bulk,neglecting the limitation of the distance between electrodes by the thickness of the wafer.This3-D structure allows faster charge collection and a very low depletion4072Analytical Chemistry,Vol.78,No.12,June15,2006voltage of1-20kV;on the other hand,the planar pixel detectors need∼80V.The authors performed a simulation model calcula-tion for the charge collection in these two types of detectors and found that the current pulse was produced in∼5ns,and in case of a pixilated planar detector,this value was found to be∼80ns. The3-D Medipix1sensor was created on high-resistivity n-type Si bulk,the electrodes were formed by photochemical etching, and the p-type electrodes were etched and doped with B by diffusion.Finally,the electrode pores were metallized with a Ti layer and Au and Al.The energy resolution of the gaseous ED detectors is more and more comparable to that of the semiconductor detectors;in addition,the structure of this low-cost detector is not complex and constructing it is much easier than for high-purity Ge or Si(Li) detectors.Beyond that they can have large area window for the entering X-rays and they have less sophisticated operating requirements than solid-state detectors,up to25-keV X-ray energy.A Portuguese research group(B18)improved their xenon-filled gas proportional-scintillation counter,applying a polyimide window with6-mm diameter with∼30%transmission at250eV for soft X-ray energies below3keV.The pressure was set as800Torr, and the gas was continuously purified by convection,using nonevaporable getters allowing the same operating gas during several months.The gaseous detector is also one of the most suitable devices for two-dimensional X-ray imaging because this type of detector can be constructed with a large sensitive area.A European research group at ELETTRA(B19)reviewed a two-dimensional X-ray imaging detector based on a single-photon counter that has a gas electron multiplier(GEM)inner structure. The GEM detector was applied for detecting X-rays having energy of8keV,and it was capable of time-resolving spectral data down to millisecond time.The sensitive area of the detector was56×56mm,divided into seven xy cells;the voltage of the drift cathode was set at4000V.On the basis of the electronic signals,each cells of the GEM can be subdivided into virtual pixels(ViP)having a sensitive spatial resolution of∼100µm(fwhm).This detection property depends significantly on the speed of the applied electronics and the gas gain,which was∼104.The authors concluded on the basis of their experience that the ViP detector offers a high quantum efficiency up to25-keV X-ray energy using 2×105Pa pressure of Xe mixture gas,and the time resolution, which determines the special resolution,can be improved down to a few hundred nanoseconds.A special application of large-area gaseous detector was shown by the research group of Despre´s (B20)by construction of a new radiographic scanning system. The detector was built by two orthogonally oriented gas microstrip detectors used for scanning a human body with a speed of15 cm/s.Both detectors consisted of1764channels,and the individual pixel sizes in the obtained X-ray image were0.254×0.254mm2.Due to the favorable detection properties,such as short signal evaluation and large sensitive area,this newly constructed device is a future candidate for low-dose radiography,since the entrance dose rate at the irradiated human skins was0.1mSv while at the case of conventional X-ray films this value is close to1.45mSv.A review article was published by Shekhtman(B21)describing the newest design of micropattern detectors and gap-resistive plate chambers and the general operating effects and processes,the design structure,and their influence on the properties of the gaseous detectors.The efficiency through the absorption strongly correlated with the atomic number of the gas material(Ar,Kr, Xe)and its pressure.The article overviewed the most important application areas of the gaseous detectors:(i)wire chambers for medical radiography applications and for SR,and(ii)micropattern gas detectors and gas electron multiplier-based detectors for high count rate synchrotron experiments.Newbury(B22)tested and applied a silicon multicathode drift detector for X-ray spectrometry on a SEM investigating spectros-copy parameters such as the output count rate,energy resolution, and peak stability in the ED spectra.He demonstrated the capability of this multichannel SDD for recording an X-ray spectrum image of an Al-Ni alloy containing4wt%Fe as well in a128×128pixel size with220-kHz output rate.The X-ray spectrum image was generated by fixing the excitation electron beam,and the SDD array was readout,and in this way the overall mapping time was found to be185s while100Mb information was paring with a Si(Li)detector having a50mm2 area,he found that the array SDD has a better resolution,namely, 134eV fwhm at6.4keV(the resolution of Si(Li)was140-145 eV),and the SDD can achieve a shorter peaking time for a given resolution.The main advantages of the silicon drift detectors(SDD)are the high count rate capability,the possibility of a large effective detection area,and the relatively high working temperature(-10°C to room temperature).The main idea is that the signal charges generated in the bulk crystal are transported to the electrodes in a controlled way,mainly parallel to the large surface of the detector.Gatti and Rehak(B23)reviewed the principal properties of the SDD,discussed different applications in charged particle physics and XRS,and gave a short description about their physical structure and the physical processes in the detector bulk,e.g., for55Fe spectra recorded with a ring-shaped SDD at-10°C,in which spectra the two Mn lines were clearly resolved.The working capabilities of two standard Si PIN and conven-tional Si(Li)detectors were studied by Kump and co-workers (B24)using55Fe and109Cd annular radioactive sources and the same measuring geometrical configuration set up.The0.3-mm-thick PIN diode had a7-mm2active area,and the energy resolution at count rates∼1000counts/s was found to be195eV,while the parameters for the Si(Li)detector were30mm2,and fwhm of175 eV(and this value is worse than the average energy resolution of commercial Si(Li)detectors).The authors compared the analytical capabilities of these detectors by quantitative analysis of SRM2710 soil standard sample,a similar dependence of sensitivities versus atomic number was found up to Z)30,and over this value,much less sensitivity was obtained with the PIN diode due to the lower detection efficiency.A new set of large area HPGe detector was reviewed in ref B25for the purpose of PIXE analysis.The detector set is built in annular form of eight individual detectors,and each item had a 100-mm2effective area;this provides high quantum efficiency.The detector chambers are mounted vertically,and each subdetector acts as an individual detector;however,they use a common main amplifier.The fwhm of the set of detectors was found to be between144and168.The authors outlined the unique spectro-scopic properties of this set,which can be used for detection ofAnalytical Chemistry,Vol.78,No.12,June15,20064073。

x射线吸收光谱 样品 基底材料

x射线吸收光谱 样品 基底材料

X射线吸收光谱(X-ray absorption spectroscopy,XAS)是一种用于研究材料结构和化学状态的有力技术。

它通过测定材料对X射线的吸收情况,可以提供有关材料内部原子的信息,包括电子态、原子之间的相互作用以及晶格结构等。

在XAS技术中,样品的基底材料对实验结果有着重要的影响,不同的基底材料可能会对样品的反射、吸收等性质产生显著影响。

本文将就X射线吸收光谱中样品基底材料的选择和影响进行讨论。

1. 基底材料的选择在进行X射线吸收光谱实验时,选择合适的基底材料对于获得准确的实验数据至关重要。

一般来说,基底材料需要具备以下特点:(1)化学稳定性:基底材料需要在实验条件下具有良好的化学稳定性,不会与样品发生化学反应,从而影响实验结果的准确性。

(2)透射性:基底材料需要具有较好的透射性,能够充分地透射X射线,使得样品的吸收信号能够得到准确测量。

(3)机械稳定性:基底材料还需要具有良好的机械稳定性,能够确保在实验过程中不会发生形变或破损。

在实际应用中,常用的基底材料包括石英、硅、玻璃等。

这些材料具有良好的化学稳定性和透射性,并且相对容易加工成薄膜样品,适用于XAS实验的要求。

2. 基底材料的影响基底材料的选择不仅仅影响到实验过程中的操作和信号测量,还会对实验结果产生一定的影响。

基底材料对X射线吸收光谱的影响主要包括以下几个方面:(1)背景信号:基底材料本身也会对X射线的透射和吸收产生影响,因此在测量实验时需要对基底材料的背景信号进行准确的修正,以确保获得准确的样品吸收信号。

(2)光能衍射:一些基底材料具有一定的光能衍射性质,会导致X射线的散射,从而影响实验信号的测量。

(3)化学相容性:部分样品可能与特定的基底材料相容性较差,会导致样品在基底上的固定困难或者发生化学反应,从而影响实验结果的稳定性。

对于不同的样品和实验要求,需要针对性地选择合适的基底材料,并针对基底材料可能产生的影响进行充分的考虑和修正,从而得到可靠的实验结果。

X射线衍射分析法 X-Ray diffraction Analysis

X射线衍射分析法 X-Ray diffraction Analysis
It can be used to identify and characterise a diverse range of materials, such as metals, minerals, polymers, catalysts, plastics, pharmaceuticals, proteins, thin-film coatings, ceramics and semiconductors.
Principle
When a single pure crystal cannot be obtained, X-ray powder diffraction can be used instead.
It can still yield important information about the crystalline structure, such as crystal size, purity and texture, but the data set may not be as complete as X-ray crystallography.
晶面间距与晶胞参数之间存在确定的关系,因此 布拉格方程能由衍射方向确定晶胞的形状和大小 。
使用单色X射线与晶体粉末或多晶样品进行衍 射分析称为X射线粉末衍射法或X射线多晶衍射法 。
由瑞士人Debye和Scherrer在1916年首先提出的 。翌年,美国人Hull也独立提出了这一方法。粉 末衍射法的样品可以是粉末或各种形式的多晶聚 集体,可使用的样品面很宽。
1.33322×102Pa,下同。

产生X射线的设备
X射线管示意图
Principle
The two main types of XRD are X-ray crystallography and Xray powder diffraction.

X射线萤光光谱仪XRF检验规范标准

X射线萤光光谱仪XRF检验规范标准

AG-0801-M006-F2Rev.:A1AG-0801-M006-F3 Rev.:A1目錄Content一、目的Purpose二、適用範圍Scope三、樣品檢測條件及方法Test condition & method for sample四、零件及產品測試原則Testing Rule五、測試方法Test Method六、注意事項Attention item七、Attachment1.XRF測試零件及產品類別之有害物質限值表限值表EHS threshold value of ponent type for XRF test2.拆解治工具管理流程The management process for disassembly tools of the ponent.3. XRF治工具季驗證紀錄表(AT-0801-M427-F1)The record of disassembly tools in quarter inspection by XRF (AT-0801-M427-F1).目的:Purpose本規範在建立進料之XRF檢驗標準,以確保品質符合既定之標準。

The purpose of this program is to establish the specification of the XRF inspection for ining materials to assure the quality of materials and ply with specified criteria.一、適用範圍:Scope適用於各大類零件之檢驗。

Apply to all types of materials.二、樣品檢測條件及方法:Test condition & method1.分析方法分為檢量線法及FP法,說明如下:Test methods can be separated to the method of calibration curve and FP method.1.1.檢量線法:對應於XRF之分析條件為〞Cd,Pb, Hg,Br,Cr.bcc〞,適用之材質為塑料、紙張、木材及Mg,Al,Si較輕元素)為主材質之樣品。

trixell 探测器参数

trixell 探测器参数

trixell 探测器参数医疗器械2009-06-01 17:22:55 阅读78 评论0 字号:大中小订阅 Pixium 4600X射线发生器名义电压: 40 - 150 kVpX射线曝光剂量: 1.25 - 2.5uGy / 150 - 300uRX射线最大线性剂量: 30uGy / 3500uR象素尺寸: 143um射线感应区域: 水平3001 象素, 429mm, 垂直3001 象素, 429mm射线窗口时间: 1-500 ms特殊曝光模式: 10-4000ms图像读出时间: 1.25秒动态范围: 14位外形尺寸: 533 * 488 * 45mm重量: 20KGPixium 4700像素尺寸:154 μmX-ray sensitive array:(射线感应区域)in overview mode(全视野)381.9 x 294.1 mmin zoom 1 mode (放大模式1)221.7 x 221.7 mmin zoom 2 mode(放大模式2)157.7 x 157.7 mmImage size (图像点阵大小)2 480 x 1 910 pixelsOperating modes and performancesA/D conversion dynamic range (模拟数字转换器)14 bitsPixel grouping feature(点阵组合方式): 1 x 1, 2 x 2, 4 x 2Maximum frame rate:(最大帧速度)1 x 1 overview mode(1*1全视野), X-window duration射线窗口≤ 70ms毫秒7.5 fr/sec帧/秒.1 x 1 zoom 1 mode1*1放大模式1, X-window duration射线窗口≤ 25 ms 15 fr/sec.1 x 1 zoom2 mode(1*1放大模式2), X-window duration(射线窗口)≤ 10 ms 30 fr/sec.2 x 2 overview mode, X-window duration ≤ 13ms 30 fr/sec.2 x 2 overview continuous mode 30 fr/sec.2 x 2 zoom 1 mode, X-window duration ≤ 5 ms 60 fr/sec.2 x 2 zoom 2 mode, X-window duration ≤ 7 ms 60 fr/se c.4 x 2 overview mode, X-window duration ≤ 8 ms 60 fr/sec.X-ray generator voltage range(X射线发生器名义电压)40 to 150 kVpDose range (剂量范围)5 to 4 500 nGy/frMaximum linear dose(最大线性剂量)45 μGy/frSensitivity:(灵敏度)highest gain(最大增益)( 2 x 2 mode(2*2模式)) 6.41 LSB/nGy typ.(6.41SB/nGy标准值) lowest gain (最小增益)0.14 LSB/nGy typ.(0.14SB/nGy标准值)Signal / Electronic noise:(信噪比)@ 5 nGy/fr in highest gain (1) 14 dB min.(在5nGy/fr,最大增益14DB)@ 1μGy/fr in lowest gain (1) 54 dB min.(在1nGy/fr,最小增益54DB)MTF @ 1 lp/mm, RQA5 (2) 60 % min.(MTF值,1线对/mm,60%)MTF @ 2 lp/mm, RQA5 (2) 30 % min.(MTF值,2线对/mm,30%)DQE @ 0 lp/mm, 1μGy/fr,RQA5 (2) 73 % typ.Residual signal (lag & memory effect) after 10 sec. exposure* at 30 fr/sec.:after 1 sec. ≤ 1.1 %after 10 sec. ≤ 0.25 %* Residual signal values in mode 2 gain 7 with 30 fr/sec.Electrical interfaces电源Single DC input voltage 24 V直流24VElectrical power (功率)75 WMechanical characteristicsOverall dimensions(外形尺寸)478 x 366 x 85 mm max.Weight 20 kg typ.(1) 1nGy = 0.115 μR @ RQA(2) RQA5 = 70 kVp, filtration = 2.5 + 21 mm aluminium。

x射线荧光光谱法 英文

x射线荧光光谱法 英文

x射线荧光光谱法英文X-Ray Fluorescence Spectrometry (XRF)。

X-ray fluorescence spectrometry (XRF) is an analytical technique used to determine the elemental composition of materials by measuring the X-rays emitted by the material when it is exposed to a high-energy X-ray beam. This method is widely used in various fields, including geology, environmental science, forensic science, archaeology, and materials science.Principle of Operation.XRF is based on the principle that when a material is irradiated with high-energy X-rays, electrons in the atoms of the material are excited and ejected from their orbits. The resulting vacancies are filled by electrons from higher energy levels, releasing X-rays with energiescharacteristic of the elements present in the material.The energy of the emitted X-rays is specific to each element, and the intensity of the X-rays is proportional to the concentration of the element in the material. By measuring the energies and intensities of the emitted X-rays, it is possible to identify and quantify the elements present in the sample.Instrumentation.A typical XRF spectrometer consists of the following components:X-ray source: Generates high-energy X-rays that bombard the sample.Sample chamber: Holds the sample to be analyzed.Detector: Converts X-rays into electrical signals.Multichannel analyzer (MCA): Digitizes and analyzes the electrical signals from the detector.Types of XRF Spectrometers.There are several types of XRF spectrometers, each with its own advantages and limitations:Energy-dispersive XRF (EDXRF): Uses a solid-state detector to measure the energies of the emitted X-rays. EDXRF is relatively inexpensive and easy to operate, but it has lower energy resolution compared to other types of XRF spectrometers.Wavelength-dispersive XRF (WDXRF): Uses a crystal monochromator to separate the emitted X-rays by wavelength. WDXRF offers higher energy resolution than EDXRF, but it is more complex, expensive, and time-consuming to operate.Total reflection XRF (TXRF): Utilizes total reflection conditions to enhance the sensitivity for analyzing trace elements in liquids. TXRF is highly sensitive, but it requires sample preparation and is not suitable for solid samples.Applications of XRF.XRF is a versatile analytical technique with a wide range of applications:Geochemistry: Determining the elemental composition of rocks, minerals, and soils.Environmental science: Monitoring pollutants in air, water, and soil.Forensic science: Analyzing trace evidence, such as gunshot residue and paint chips.Archaeology: Studying the composition of artifacts and ancient materials.Materials science: Characterizing the elemental composition of metals, alloys, and other materials.Advantages of XRF.Nondestructive: Does not damage the sample being analyzed.Multi-elemental: Can identify and quantify multiple elements simultaneously.Rapid: Provides real-time analysis results.Sensitive: Can detect elements at trace levels.Versatile: Can be applied to various sample types, including solids, liquids, and powders.Limitations of XRF.Limited sensitivity: Cannot detect elements present in very low concentrations.Matrix effects: The presence of other elements in the sample can affect the accuracy of the analysis.Sample preparation: May require sample preparation,such as grinding or homogenization.Cost: XRF spectrometers can be expensive, especially WDXRF systems.Conclusion.X-Ray Fluorescence Spectrometry is a powerful analytical technique that provides valuable information about the elemental composition of materials. It is widely used in various fields and offers advantages such as non-destructiveness, multi-elemental analysis, and rapid results. However, it has limitations in sensitivity and potential matrix effects, which should be considered when selecting this technique for specific applications.。

x荧光光谱法

x荧光光谱法

x荧光光谱法X荧光光谱法(X-ray fluorescent spectroscopy,XRF)是现代分析科学中常用的一种无损表面分析技术。

它通过测量物质被激发后放射出的X射线能谱图,从而确定样品中各种基本元素的相对含量和结构信息。

X荧光光谱法具有高灵敏度、高分辨率、广泛适用性等优点,在材料科学、地球科学、环境科学、矿业勘探等领域有着广泛的应用。

本文将详细介绍X荧光光谱法的原理、仪器设备以及应用领域。

一、X荧光光谱法的原理1.1 X射线的产生和相互作用X射线是电磁波谱中波长最短的一种辐射。

X射线的产生主要有两种途径:一种是由高能电子通过急剧的减速过程产生的,称为广义X射线;另一种是由高能粒子与物质相互作用而产生的,如β粒子与重原子核相互作用产生的射线,称为硬X射线。

当高能电子与物质相互作用时,会发生三种主要的相互作用过程:电离作用、激发作用和散射作用。

这些相互作用过程对物质的特性有很大的影响。

其中,电离作用是指电子与物质原子中的电子发生碰撞,导致电子被打出原子,产生电离现象。

激发作用是指电子与物质原子中的内层电子发生碰撞,使内层电子被激发到高能级,然后返回基态时放出能量。

散射作用是指电子与物质原子中的电子发生弹性碰撞,改变方向后出射。

1.2 X荧光光谱法的原理X荧光光谱法是利用物质受激发后放射出的X射线能谱图来分析样品中的成分和结构信息。

当X射线照射到物质上时,物质原子的内层电子可以被激发到高能级,然后返回基态时会放出能量。

这些能量的大小和原子的电子能级差有关,不同元素的电子能级差是不同的。

当物质被X射线照射时,其中的原子会被激发,激发后返回基态时放出的能量就形成了一系列特定的X射线能谱线。

这些能谱线对应着不同元素的电子能级差,因此可以通过测量物质放射出的X射线能谱图来确定样品中各种基本元素的相对含量和结构信息。

1.3 X荧光光谱法的仪器设备X荧光光谱法主要的仪器设备有X射线发生器、样品支架、能谱仪和数据处理系统。

x-ray稳定性测试步骤(精)

x-ray稳定性测试步骤(精)

对FISCHERSCOPE X-RAY测厚仪进行测量稳定性测试的步骤
(基于WinFTM 软件)
1.打开仪器和电脑,并联线。

选择菜单“一般”――“服务程式”――“检查测量稳定度”,
选择“Stabi. Test”程式
2.选择“产品程式”――“复制”,复制一个“Stabi. Test”程式,为了便于筛选,将复制
的程式取名为日期,例如“Stabi. Test 20070101”。

按“复制”后关闭窗口。

3.打开仪器和电脑,并联线。

选择菜单“一般”――“服务程式”――“检查测量稳定度”,
选择“Stabi. Test 20070101”程式。

4.选择“调校”――“归一化”,按“是”确认。

5.选择“产品程式”――“连续测量”,进行测试。

6.放入Ag基准,连续测量24或48小时后,停止测量。

选择“产品程式”――“复制文
件由/到”,在“产品程式>>>文件”卡中,在“复制那个产品程式?”中选择刚才进行稳定性测试的程式,例如“Stabi. Test 20070101”;在“产品程式复制到那里?”中选择目标目录,例如C盘,D盘等。

7.把复制出来的文件,如“Stabi. Test 20070101.sv1”,通过电子邮件传送到FISCHER公
司,以便进行分析。

元素分析仪器介绍

元素分析仪器介绍

成分分析四大家——XRF、ICP、EDS、WDS XRFXRF(X-Ray Fluorescence spectrometer)指的是X射线荧光光谱仪,可以快速同时对多元素进行测定的仪器。

在X射线激发下,被测元素原子的内层电子发生能级跃迁而发出次级X射线(X-荧光)。

从不同的角度来观察描述X射线,可将XRF分为能量散射型X射线荧光光谱仪,缩写为EDXRF或EDX和波长散射型X射线荧光光谱仪,可缩写为WDXRF或WDX,但市面上用的较多的为EDX。

WDX用晶体分光而后由探测器接收经过衍射的特征X射线信号。

如分光晶体和探测器做同步运动,不断地改变衍射角,便可获得样品内各种元素所产生的特征X射线的波长及各个波长X射线的强度,并以此进行定性和定量分析。

EDX用X射线管产生原级X射线照射到样品上,所产生的特征X射线进入Si (Li)探测器,便可进行定性和定量分析。

EDX体积小,价格相对较低,检测速度比较快,但分辨率没有WDX好。

XRF用的是物理原理来检测物质的元素,可进行定性和定量分析。

即通过X射线穿透原子内部电子,由外层电子补给产生特征X射线,根据元素特征X射线的强度,即可获得各元素的含量信息。

这就是X射线荧光分析的基本原理。

它只能测元素而不能测化合物。

但由于XRF是表面化学分析,故测得的样品必须满足很多条件才准,比如表面光滑,成分均匀。

如果成分不均匀,只能说明在XRF测量的那个微区的成分如此,其他的不能表示。

XRF的优点:•分析速度高。

测定用时与测定精密度有关,但一般都很短,2-5分钟就可以测完样品中的全部元素。

•非破坏性。

在测定中不会引起化学状态的改变,也不会出现试样飞散现象。

同一试样可反复多次测量,结果重现性好。

•分析精密度高。

•制样简单,固体、粉末、液体样品等都可以进行分析。

•测试元素范围大,WDX可在ppm-100%浓度下检测B5-U92,而EDX可在1ppm-100ppm下检测大多数元素,Na11-U92。

X荧光光谱分析标准方法

X荧光光谱分析标准方法

5.1.1Surface Grinder ,with 60to 600-grit aluminum oxidebelts or disks capable of providing test specimens with auniform flat finish.5.2Excitation Source :5.2.1X-Ray Generator ,providing constant potential orrectified power of sufficient energy to produce secondaryradiation of the sample for the elements specified.The genera-tor may be equipped with a line voltage regulator and a currentstabilizer.5.2.2X-Ray Tubes ,with targets of various high-purityelements,that are capable of continuous operation up to thepotentials and currents shown in Table 1.N OTE 4—X-ray tubes with tungsten,gold,and rhodium targets wereused in the testing of this method.5.3Spectrometer ,designed for X-ray emission analysis,using air or vacuum,and equipped with specimen holders andspecimen chamber.The chamber should contain a samplespinner.5.3.1Analyzing Crystal ,flat or curved lithium fluorideLiF(200)or LiF(220).5.3.2Collimator ,for limiting the characteristic X-rays to aparallel bundle when flat crystals are used in the instrument.For curved crystal optics,no collimator is necessary.5.3.3Detectors —Sealed or gas-flow proportional countersor equivalent.5.3.4Vacuum System ,if used,should consist of a vacuumpump,6gage,and electrical controls to provide automaticpumpdown of the optical path and to start the analysis at apressure of 100µm or less,controllable to 620µm.5.4Measuring System —An electronic circuit capable ofamplifying and integrating pulses received from the detectortube.The system should be equipped with visual and automaticrecording devices.6.Reagents6.1Detector Gas (P-10),consisting of 90%argon and10%methane.7.Hazards7.1Guidelines on ionizing radiation given in OccupationalHealth and Safety Standards 7shall be observed at all X-rayemission spectrometer installations.It is also recommended that personnel follow the guidelines of safe operating proce-dures given in the NIST Handbook X-Ray Protection,HB76,8the booklet Radiation Safety Recommendations for X-Ray Diffraction and Spectrographic Equipment ,9#MORP 68-14,by T.M.Moore and D.J.McDonald,1968,and the ernment Handbook 93,Safety Standard for Non-Medical X-Ray and Sealed Gamma-Ray Sources,Part 1,general,or similar handbooks of latest issue.7.2X-ray equipment should be used only under the guid-ance and supervision of a responsible,qualified person.7.3Suitable monitoring devices,either film badges or do-simeters,shall be worn by all personnel using the equipment.10To meet local,state,and federal radiation standards,periodic radiation surveys of the equipment for leaks and excessive scattered radiation shall be made by a qualified person using an ionization-chamber detector.11The personal film badge survey record,the radiation survey records,and a maintenance record shall be available upon request.7.4Special precautions for the operator shall be posted.7.5X-ray caution signs shall be posted near the X-ray equipment and at all entrances to the radiation area.7.6Fail-safe “X-ray On”warning lights shall be used at the X-ray tube.8.Preparation of Reference Materials and Samples 8.1Grind the samples to provide a flat,clean area over the entire surface to be exposed to the X-ray beam.Adhere rigorously to the preparation technique established.9.Reference Materials 9.1Certified Reference Materials are available from the National Institute of Standards and Technology 12and other sources.9.2Reference Materials can be used,provided they are analyzed in accordance with Test Methods E 353.10.Preparation of Apparatus 10.1Start-up —Energize the power supply and electronic circuits for at least 1⁄2h prior to taking measurements.10.2Power Supply —Adjust the voltage of the power supply to produce secondary fluorescence according to the expression:V f 512350/l K abs (1)where:V f =the minimum voltage required for exciting the element,and l K abs =wavelength of the K adsorption edge of the fluorescent element.6A two-stage mechanical pump meeting the requirements can be purchased fromPrecision Scientific Co.,Chicago,IL 60647,or Sargent-Welch Scientific Co.,Skokie,IL 60076.7Federal Register,V ol.36,No.105,May 29,1971,Section 1910.96or of latestissue of Subpart G,available from Superintendent of Documents,ernmentPrinting Office,Washington,DC 20025;or National Bureau of Standards Handbook111,ANSI N43.2-1971.8Available from Superintendent of Documents,ernment Printing Office,Washington,DC 20025.9Available from U.S.Department of Health,Education,and Welfare,Rockville,MD 20850.10Available from Siemens Gammasonics,Inc.,2000Nuclear Drive,Des Plaines,IL 60018.11A survey meter called Cutie-Pie has been found satisfactory for this purpose and is available from Nuclear Associates,Westbury,Long Island,NY 11590.12Available from National Institute of Standards and Technology,U.S.Depart-ment of Commerce,Gaithersburg,MD 20899.TABLE 1Typical Operating Voltages and CurrentsElement Voltage,kV (Current,mA)Chromium 60(45)60(24)50(40)20(8)40(8)Nickel 60(45)60(32)50(40)60(32)40(16)Copper 60(45)60(32)50(40)60(32)40(24)Molybdenum 60(45)60(32)50(40)60(32)40(24)Manganese 60(45)60(32)50(40)60(32)40(24)Columbium (Niobium)60(45)60(32)50(40)60(32)40(24)Cobalt 60(45)60(32)50(40)60(32)40(24)10.2.1Ideally,the operating voltage should approximate orexceed V =3V f .Adjust the current to produce rate of secondaryfluorescence within the desired limits of statistical precisionand detector linearity.Typical operating voltage and currentused by different laboratories for testing the method are shownin Table 1.The values in Table 1should be used as a guideonly.N OTE 5—The voltage and current established as optimum for the X-rayemission power supply in an individual laboratory is reproduced forsubsequent measurements.10.3Detector Gas Flow —Adjust the flow of P-10gas inaccordance with the equipment manufacturer’s instructions.Some detectors require a rapid flow rate and others only abubble per second.Optimum rate should be determined byeach laboratory,and the detectors should be adequately flushedwith detector gas before the instrument is used.10.4Loading Samples —Orient the reference materials andspecimens in the sample chamber so that the relationshipbetween the X-ray beam and the grinding striations are thesame for all measurements.The precaution need not be takenwhen a sample spinner is utilized.11.Procedure11.1Excitation —Expose the sample to primary X radiationin accordance with the conditions described in Section 9.11.2Radiation Measurements —Measure the radiation in-tensities of the analytical lines listed in Table 2.11.2.1Counting —Obtain and record the counting rate mea-surement for each element.Fixed time or fixed count modescan be used.Obtain at least 16000counts for the lowestconcentrations within the specification.11.2.2Voltage Integration —Obtain and record the voltageintegration measurement for each element.Fixed time or fixedvoltage modes can be used.A minimum of 30-s integrationtime is necessary for the lowest concentrations.11.2.3Interference of Chromium on Manganese —Manyspectrometers will not completely resolve Mn Ka from Cr Kb .Care must be exercised in theinterpretation of manganese intensities for samples with varying chromium concentration.Manganese must be determined by means of curves establishedfrom reference materials with a chromium content equivalentto that of the sample,or mathematical calculations must beused to correct for chromium interference.N OTE 6—The use of LiF(220)as the analyzer crystal may resolve Cr K b and Mn K a sufficiently to simplify the manganese determination.12.Calibration,Standardization,and Verification 12.1Calibration —Irradiate the calibrants and potential standardants in a random sequence,bracketing these radiations with irradiations of any materials intended for use as verifiers.(A verifier may be used as a calibrant even though it is irradiated only as a verifier.)There will be several calibrants for each element and for each alloy group spanning the required concentration ranges.Repeat with different random sequences at least three ing the averages of the data for each point,determine analytical curves as directed in Practice E 305.12.2Standardization —Following the manufacturer’s rec-ommendations,standardize on an initial setup or any time that it is known or suspected that readings have shifted.Make the necessary corrections either by adjusting the controls on the readout or by applying arithmetic corrections.Standardization will be done any time verification indicates that readings have gone out of statistical control.12.3Verification —Verification shall be done at least at the beginning of a work shift.Analyze verifiers in replicate to confirm that they read within the expected confidence interval,as defined in 12.4.12.3.1Check verification after standardizing.If confirma-tion is not obtained,run another standardization or investigate why the instrument is malfunctioning.12.3.2Repeat the verification at least every 4h or if the instrument has been idle for more than 1h.If readings are not in conformance,repeat the standardization.12.4The confidence interval will be established from ob-servations of the repeatability of the verifiers and determining the confidence level as prescribed in Practice E 876or by establishing the upper and lower limit of a control chart as prescribed in Manual MNL 7.The latter is the preferable approach since it also monitors the consistency of the statistics of the measurements and provides a way of maintaining a record of performance.13.Calculation 13.1Read the percent concentration of each element from the appropriate analytical curve.N OTE 7—Radiation measurements can be automatically printed on an electric typewriter.The output signals can also be entered directly into a computer so that the concentrations can be read directly.13.1.1If plotting is done in terms of ratio of radiation measured to a selected reference,determine the ratio of the observed radiation measurement to that of the selected refer-ence and read concentration from the appropriate analytical curve.13.1.2Concentrations can be read from tables prepared from the analytical curves relating radiation measurements and concentrations.14.Precision and Bias 214.1Precision —The precision of this test method was determined by submitting nine stainless steel alloys to five different ing their own reference samples asTABLE 2Analytical LinesElement Line Designation 2u angle,deg A Wavelength,nm CrystalChromium K }69.350.2291LiFNickel K }48.660.1659LiFCopper K }45.030.1542LiFMolybdenum K }20.290.0710LiFManganese K }62.970.2103LiFColumbium (Niobium)K }21.400.0748LiFCobalt K }52.790.1790LiFA The 2u angles represent the theoretical values for a lithium fluoride crystal.The actual position for the peak intensities of the elements should be experimen-tally determined for eachspectrometer.well as NBS Certified Reference Materials for calibration,these five laboratories analyzed the nine unknowns on five different days.The precision data are shown in Table 3.14.2Bias —The agreement between results obtained by chemical methods and those obtained by this test method is shown in Table 3.15.Keywords 15.1spectrometric analysis;stainless steels;X-ray emissionTABLE 3Precision and Bias DataElement Sample Number of Determina-tionsRelative Standard Deviation,RSD %AB Concentration,%X-ray C Chemi-cal D Chromium 1250.2718.5518.502250.3717.5417.443250.3017.3417.244250.2617.2517.205250.2615.9115.936250.2417.7817.707250.2017.0017.108250.3313.3413.319250.2611.7211.73Nickel 1250.459.199.132250.629.919.823250.708.248.164250.5112.3512.295250.53 4.63 4.746252.220.240.247252.220.290.298253.070.210.229252.110.310.31Copper 1250.750.270.2452252.720.160.1533252.220.210.204254.900.100.1055251.17 3.33 3.386254.690.0740.0607256.850.0750.0688255.420.0860.0789256.160.0740.065Molybdenum 1251.040.360.352251.300.270.263251.830.320.304250.36 2.73 2.735251.680.230.2362516.210.0170.0197250.940.480.488253.850.0980.1019254.760.0790.075Manganese 1250.88 1.42 1.412250.92 1.63 1.613250.90 1.85 1.784250.53 1.60 1.605251.620.520.556252.360.390.407252.400.450.478250.94 1.09 1.009251.630.450.46Columbium 2250.820.700.66(Niobium)5251.470.340.36Cobalt 1201.800.220.2042202.880.190.203204.910.140.134252.370.36(0.37)5157.930.044(0.050)6159.320.029(0.020)7158.500.041(0.031)81514.650.025(0.018)920 6.650.046(0.040)AThese relevant standard deviation values are reproducibility data and wereobtained by pooling data from five cooperating laboratories.Repeatability data forthe individual laboratories are on file at ASTM Headquarters.B Relative standard deviation,RSD,in this method is calculated as follows:RSD 5~100/X¯!=(d 2/~n 21!where:X¯=average concentration,%,d =difference of determination from the mean,andn =number of determinations.C The X-ray values are pooled data from five cooperating laboratories.Data foreach of the five individual laboratories are on file at ASTM Headquarters.D The samples used for this program are commercial reference materials.Theestablished values are the average of either chemical or chemical and spectro-chemical results by several laboratories.The values in parentheses are notcertified.The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this ers of this standard are expressly advised that determination of the validity of any such patent rights,and the risk of infringement of such rights,are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years and if not revised,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards,at the address shown below.This standard is copyrighted by ASTM,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959,United States. Individual reprints(single or multiple copies)of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585(phone),610-832-9555(fax),or service@(e-mail);or through the ASTM website().。

X射线衍射和小角X射线散射

X射线衍射和小角X射线散射

晶体的X射线衍射特征
[Crystal Structure Analysis, 3rd Edition, p. 48]
晶体结构及其晶胞类型
[Methods of Experimental Physics Volume 16: Polymers, Part B Crystal Structure and Morphology, p. 5]
X射线衍射需要在广角范围内测定,因此又 被称为广角X射线衍射(Wide-Angle X-ray Scattering, WAXS)。
小角X射线散射
如果被照射试样具有不同电子密度的非周 期性结构,则次生X射线不会发生干涉现象, 该现象被称为漫射X射线衍射(简称散射)。
X射线散射需要在小角度范围内测定,因此 又被称为小角X射线散射(Small-Angle Xray Scattering, SAXS)。
晶面指数与晶胞参数
[Fundamentals of Powder Diffraction and Structural Characterization of Materials, 2nd Edition, p. 9]
Bragg方程
设晶体的晶面距为 d,X射线以与晶面间交
角为 的方向照射,从晶面散射出来的X射
粉末衍射条纹摄制及处理
[Fundamentals of Powder Diffraction and Structural Characterization of Materials, 2nd Edition, p. 265]
粉末衍射平板图案摄制
[Fundamentals of Powder Diffraction and Structural Characterization of Materials, 2nd Edition, p. 153]

2019年X-Ray检测器可靠性验证报告

2019年X-Ray检测器可靠性验证报告

X-Ray检测器可靠性验证报告Distribution:Local QA Manager :Local Production Manager :Local Supply Chain Director :Table of Contents1.0. 验证报告审批1.1.报告准备Prepared by:Reviewed by:1.2.报告批准Approved by:2.0.验证范围2.1.背景为加强对产品中潜在的异物、特别是金属和玻璃形成的危害进行有效控制,特购买一台X-Ray检测器对黄埔工厂袋装生产线产品进行在线检测。

2.2.目的2.2.1.验证X-Ray检测器对不同材质异物剔除的灵敏度,确认设备能否有效剔除0.8mm不锈钢标准样本和2.5mm玻璃标准样本。

2.2.2.通过验证设定X-Ray检测器对不同产品的灵敏度参数。

2.3.接受标准2.3.1.能成功检测出分别含有不锈钢和玻璃的标准样本,连续30次检测不得出现一次漏报。

2.3.2.产品误报率不超过0.5% 。

2.4.验证原则2.4.1.根据X-Ray的特性,小包装的检验与大包装的检验相比,其灵敏度较高,因此只需对400g袋装产品进行验证。

2.4.2.按产品特性,现将公司所有袋装产品分为四大类:证:EFM、EFP A+、EFK A+、ALA1。

2.5.步骤2.5.1.验证场所验证将在设备安装现场进行。

2.5.2.检测样品的准备2.5.2.1.标准样本:由供应商提供0.8mm不锈钢和2.5mm玻璃标准样本。

2.5.2.2.产品样本:400g EFM、400g EFP A+、400g EFK A+、400g ALA1。

2.5.3.样品的验证2.5.3.1.针对某一品种,根据调试所确定的参数,用400g的样本过机测试,要求连续30次不出现误报;2.5.3.2.用小刀割破400g样品,将用小塑料袋包装好的0.8mm不锈钢样本放入样品中;2.5.3.3.过机测试,连续30次均能准确检出;2.5.3.4.用小刀割破400g样品,将用小塑料袋包装好的2.5mm玻璃样本放入样品中;2.5.3.5.过机测试,连续30次均能准确检出;2.5.3.6.将使用过的所有样品剪袋,将奶粉倒入30目的筛子中过筛,若在粉料中发现任何异物,之前使用该样品所做的调试和验证须全部重新进行。

X-射线荧光光谱仪测定铅精矿中多种元素含量实验

X-射线荧光光谱仪测定铅精矿中多种元素含量实验

第43卷第1期2021年2月甘肃冶金GANSU METALLURGYVol.43No.1Feb.,2021文章编号:1672-4461(2021)01-0112-03X-射线荧光光谱仪测定铅精矿中多种元素含量实验李金明,方彦霞,王红燕(西北矿冶研究院,甘肃白银730900)摘要:主要讨论X-射线荧光仪检测铅精矿中多种元素含量的方法。

X-射线荧光仪常用的分析样品类型有融片样和粉末压片样,粉末压片制样简单、成本低、速度快,是X-射线荧光仪常用的制样方式。

X-射线荧光仪分析粉末压片样中多种元素的含量,在实际应用中比化学分析有明显的优势,耗时少,效率高。

波长色散X-射线荧光仪的优点就是能依据批量样品的化学定值,建立相应的多元素分析工作曲线,做到一次制样,一次检测多种元素的含量,省时省力,在现场和实验室得到广泛应用。

关键词:X-射线荧光;铅精矿;粉末压片;工作曲线;漂移校正中图分类号:0657.34文献标识码:BDetermination of Multi Elements in Lead Concentrateby X-Ray Fluorescence SpectrometerLI Jin-ming,FANG Yan-xia,WANG Hong-yan(Northwest Research Institute of Mining and Metallurgy,Baiyin730900,China)Abstract:This paper mainly discusses the method of X-ray fluorescence detection for the content of various elements in lead concentrate.The commonly used analytical sample types of X-ray fluorescence analyzer are melting sample and powder pressed sample.Powder compression sample preparation is simple,low cost and fast,which is the common sample prepara­tion method of X-ray fluorescence instrument.X-ray fluorescence analyzer has obvious advantages over chemical analysis in analyzing the contents of various elements in powder pressed tablets.It takes less time and has higher efficiency.The advan­tage of wavelength dispersive X-ray fluorescence spectrometer is that it can establish the corresponding multi-element analy­sis working curve according to the chemical fixed value of batch samples.It can make sample preparation at one time and detect the content of multiple elements at one time,which saves time and effort,and is widely used in the field and labora­tory^.Key Words:X-ray fluorescence;lead concentrate;powder pressing;working curve;drift correction1引言白银有色集团厂坝铅锌矿在引进X-射线荧光分析仪之前,在我院理化中心对该矿生产的多个批次的矿样进行了X-射线荧光分析测试的前期实验工作,我中心X-射线荧光实验室承担了全部矿样的标准工作曲线建立实验,为厂坝铅锌矿X-射线荧光仪引进及使用提供了技术支持。

X射线荧光光谱理论强度计算中激发因子的选择

X射线荧光光谱理论强度计算中激发因子的选择

2001年第59卷第1期,129~132化学学报ACT A CHIMICA SINICAV ol.59,2001N o.1,129~132・研究简报・X 射线荧光光谱理论强度计算中激发因子的选择卓尚军Ξ 陶光仪 殷之文 吉 昂(中国科学院上海硅酸盐研究所 上海 200050)摘要 激发因子是X 射线荧光强度理论计算中的重要参数.对目前常用的四种激发因子算法进行了较为详细的比较,并设计了一种评价激发因子算法的实验方法,即用人工合成试样测定了八对能量接近的X 射线特征谱线的强度比,然后根据不同的激发因子算法用理论方法计算出这些谱线对的强度比值,以两者的接近程度来判断这四种激发因子算法的适用性.结果表明,使用NR LXRF 程序修改版中的激发因子算法计算出来的理论强度比与实测值之间的相对偏差最小.关键词 X 射线荧光光谱,激发因子,理论强度Selection of Excitation F actors in X -ray Fluorescence SpectrometryZH UO Shang -Jun 3 T AO G uang -Y i YI N Zhi -Wen J I Ang(Shanghai Institute o f Ceramics ,The Chinese Academy o f Sciences ,Shanghai ,200050)Abstract Excitation factor is one of the key factors in the calculation of theoretical intensities in X -ray fluorescence spectrometry.In this w ork ,four comm only used com pilations for calculating excitation factors were com pared.An experiment was carefully designed and performed to test the validity of these calculated excitation factors in which eight pairs of X -ray lines that were close to each other in energy were measured using synthetic sam ples.The ratios of the measured intensities of the line pairs were then com pared with those from theoretical calculation using different com pilations of excitation factors.It was found that the relative errors between calculated theoretical intensity ratios using the excitation factors in the m odified version of NR LXRF program and the measured values were the least.K eyw ords X -ray fluorescence spectrometry ,excitation factor ,theoretical intensity X 射线荧光强度的理论计算在现代X 射线荧光光谱分析中具有非常重要的作用.正是由于X 射线荧光强度理论计算公式的提出,才使得基本参数法成为可能,同时为目前广泛使用的理论α系数计算奠定了基础.从X 射线荧光强度的理论计算公式可以看出,影响理论计算X 射线荧光强度准确度的因素相当复杂.T ao 等[1~3]对其主要影响因素(谱仪几何因子、X 射线原级谱强度分布、质量衰减系数和X 射线激发因子)已有论述,特别是对质量衰减系数(M AC )算法的比较进行了仔细研究.但是,对X 射线荧光激发因子的常用算法及如何评价未予详细展开.文ΞE -mail :sjzhuo @收稿日期:2000-03-14,修回日期:2000-06-26,定稿日期:2000-08-15,国家自然科学基金(29975032)资助项目(Received M arch 14,2000.Revised June 26,2000.Accepted August 15,2000)献[1,3]的初步比较表明,采用不同的算法[4~7],计算所得的激发因子特别是对L和M系谱线相差很大.所以,在实际应用中,激发因子计算方法的选用将直接影响理论相对强度的计算准确性,同时也影响到用于基体效应数学校正的理论α系数的计算准确性.激发因子是荧光产额(ω),谱线分数(g)和吸收限陡变因子(J)三者的乘积.本工作对文献[4~7]中的激发因子算法进行详细比较研究,比较它们在计算激发因子时所引用的荧光产额、谱线分数和吸收限陡变因子的来源或者计算方法.由于在定量分析中,常用的谱线为Kα,Kβ,Lα,Lβ1,Lβ2和Mα,所以仅对这些谱线激发因子的计算进行比较.然后,用人工方法仔细配制一系列试样,在相同的测量条件下分别对波长相近的几组谱线对进行测量,通过X光强度比的测量值与理论计算值的比较,对这些激发因子的算法进行评价.1 理论考虑1.1 荧光产额由X射线激发所产生的二次光子(X射线荧光)在离开原子的过程中,有一部分会在原子内部被吸收(俄歇效应).荧光产额就是二次光子不被原子吸收而产生X射线荧光的几率.它随原子序数的增大而增大,同一原子的荧光产额则按ωK,ωL和ωM的顺序急剧减小.荧光产额可以通过理论或实验方法确定.几种激发因子算法中所采用荧光产额的来源或算法列于表1.著名美国海军研究实验室的计算机程序NR LXRF[4]中,ωK是用实验值通过多项式[ωK/(1-ωK)]1/4=A+B Z+CZ3拟合求得,其中A,B和C 为常数,Z为原子序数.ωL2,ωL3和ωM5则用实验值通过内插的方法得到.在NR LXRF的修改版[5]中,荧光产额的计算方法未作修改.在Broll的算法[6]中,荧光产额的值是在文献[8]中表列值的基础上,综合了Freund[9]所收集的实验值后重新列表.另外,该作者将ωL2和ωL3当作近似相等,而且未提供ωM5的算法.在de Boer的算法[7]中,ωK,ωL2和ωL3均采用K rause[10]中的拟合值,其中ωL2采用了所谓有效荧光产额(考虑了C oster-K ronig产额影响后的值).而ωM5则是de Boer对文献[8]中的值进行内插平均后得到的.表1 不同激发因子计算中所采用的荧光产额T able1 Fluorescence yields used in different excitation factor calculation methods NR LXRF NR LXRF修改版Broll de Boer ωK多项式拟合多项式拟合表列值[6]表列值[10]ωL2内插值内插值=ωL3表列值[10]ωL3内插值内插值表列值[6]表列值[10]ωM5内插值内插值未提供表列值[7]1.2 谱线分数当原子中某一能级出现空穴时,较高能级的电子跃迁填补该空穴的可能性不只一种,从而产生不同的谱线.导致产生某一谱线的几率就是该谱线的谱线分数.所以,同一谱系中,所有谱线的谱线分数之和应该为1.例如,在K系谱线中,g Kα+g Kβ=1.在比较的四种算法中所引用的Kα,Kβ,Lα,Lβ1,Lβ2和Mα的谱线分数列于表2.Kα的谱线分数在NR LXRF及其修改版的激发因子算法中,均采用内插值.Broll采用的表列值是根据Scofield[11]的谱线强度计算出来的.de Boer则采用了Salem[12]用实验值通过最小二乘拟合得到的表列值.所有算法中Kβ的谱线分数都用1-g Kα计算值.在NR LXRF中,Lα,Lβ1,Lβ2和Mα的谱线分数均近似处理为常数.在其修改版中则将Lα和Lβ2的谱线分数用内插值代替.Broll也根据Scofield[11]的谱线强度值计算g Lα,并近似认为g Lβ1和g Lα相等,同时忽略Lβ5,Lβ6和Ll的贡献,所以g Lβ2=1-g Lα.de Boer 的g Lα和g Lβ1仍采用Salem的表列值,同时对原子序数从21至25的元素分别用外推法得到的近似常数表示,g Lβ2则采用与Broll相同的近似处理,并将g Mα近似为1.0.031 化学学报V ol.59,2001表2 不同激发因子计算中所引用的谱线分数T able2 Relative X-ray emission rates used in different excitation factor calculation methods NR LXRF NR LXRF修改版Broll de Boer g Kα内插值内插值表列值[6]表列值[12] g Kβ1-g Kα1-g Kα1-g Kα1-g Kαg Lα0.9内插值表列值[6]表列值[12] g Lβ1 1.0 1.0=g Lα表列值[12] g Lβ20.1内插值1-g Lα1-g Lαg Mα 1.0 1.0未提供 1.01.3 吸收限陡变因子吸收限陡变因子是入射光子电离某一特定能级电子的几率,它与吸收限陡变比(γ)有关.本文比较的四种激发因子算法中的J K都采用了J K=1-γK 的计算值,只是γK的来源不同.J L2,J L3和J M5的计算比较复杂,因为要考虑C oster-K ronig效应的影响,而且其计算公式也随激发能量所处的吸收限能量段不同而变.de Boer所采用的计算公式及表列值可参考文献[7],在实际计算J M5值中,de Boer所采用的是随入射线能量范围不同和原子序数范围不同的固定常数.在NR LXRF修改版中,对原有J L2,J L3和J M5的计算方法作了较大的改动,作为一个例子,表3列出了当入射线能量大于K吸收限能量时两者计算J L3的区别.Broll采用的则是McMaster[13]的表列J L3值,并近似认为J L2和J L3相等,未提供J M5值.表3 NR L XRF及其修改版中的J L3算法的比较3T able3 C omparis on of J L3used in NR LXRF andits m odified versionNR LXRF NR LXRF修改版V Z=1-1/γK V Z=1-1/γKV1=1-(1/γL1γK)V1=(1-1/γL1)/γKV2=1-(1/γL1γL2γK)V2=1-(1/γL2)/γKγL1V3=1-(1/γL1γL2γL3γK)V3=1-(1/γL3)/γKγL1γL23当入射线能量大于待测元素的K吸收限能量时:J L3=V3+V23f L23 +V13(f L13+f L123f L23)+V Z3[f K L3+f K L23f L23+f K L13(f L13+f L123 f L23)]其中f为C oster-K ronig产额.2 实验部分2.1 实验设计由X射线荧光强度的理论计算公式可知,影响X荧光强度的因素包括谱仪的几何因子、X光管原级谱的强度分布、质量衰减系数和激发因子等.对于能量非常接近的两条谱线,在同样的激发条件下测量,则谱仪的几何因子、X光管原级谱的强度分布、分光晶体的反射效率和探测器的探测效率等都非常接近,所以,用两条谱线的实测强度比和用不同的激发因子算法计算出的理论强度比进行比较,就能够反映出激发因子的影响.2.2 样品制备,测量和计算用m(Li2B4O7)∶m(LiBO2)=12∶22的熔剂和光谱纯的氧化物精心挑选和配制一系列的熔融片(每种均做两份平行样),选择能量相近的谱线分别在相同的激发条件下测量其强度,并将强度比与理论计算的强度比进行比较.测量条件为:铑靶,40kV(Pb Lα/As Kα用80kV),X光管取出角18°,铍窗厚度0.3 mm.计算理论强度比时,分别采用本文比较的四种激发因子算法,而其他条件保持不变.3 结果与讨论3.1 实验结果共选择了八对谱线(六对Lα/Kα和二对Mα/ Kα),它们的测定强度比、用四种激发因子算法计算的理论强度比及与实测强度比的相对偏差列于表4.从表中比较的结果看,用NR LXRF修改版的激发因子所计算出的谱线强度比与实测值最为接近(平均相对偏差为28.5%),而用NR LXRF原始版的激发因子所计算出的谱线强度比与实测值差别最大(平均相对偏差为165.9%).131January2001卓尚军等:X射线荧光光谱理论强度计算中激发因子的选择表4 用不同激发因子算法计算的理论强度比与实测强度比的比较T able4 C omparis on of theoretical and measured ratios of relative intensities using different excitation factor calculation methods 实测值NR LXRF计算值RE3 NR LXRF修改版计算值REBroll计算值REde Boer计算值REPb Lα/As Kα0.3760.984161.7 0.46724.2 0.352-6.4 0.46824.5 Ba Lα/T i Kα0.3160.749137.0 0.38521.8 0.229-27.5 0.34910.4 Z r Lα/P Kα0.339 1.075217.1 0.63286.4 1.489339.2 0.58973.7 Y b Lα/Ni Kα0.3520.711102.0 0.368 4.5 0.266-24.4 0.358 1.7 M o Lα/S Kα0.3520.756114.8 0.45027.8 1.101212.8 0.44025.0 Sr Lα/S i Kα0.428 1.095155.8 0.63448.1 1.710299.5 0.67958.6 Pb Mα/S Kα0.2420.702190.1 0.228-5.8 — 0.39764.0 W Mα/S i Kα0.362 1.262248.6 0.329-9.1 — 0.70594.8 Ave.RE33165.928.5151.644.1 3RE为与实测值比较的相对偏差(%).33Ave.RE为平均相对偏差(%).3.2 讨论(1)由于计算激发因子的三个参数,荧光产额、谱线分数和吸收限陡变因子都存在不同程度的不确定性,特别是对L和M系列的谱线而言尤为如此.所以,计算出来的激发因子误差也较大.但E K比E L 和E M要准确得多.部分原因是K层只有一个能级,而L和M层分别对应三个和五个能级,因此计算公式也复杂得多.(2)本文实验测定了能量接近的八对谱线的X 光荧光强度,实际上是重点考察了Lα和Mα谱线的X光激发因子的准确性.从所作的比较可以看出,造成四种算法计算所得激发因子有较大差异的主要原因,是它们选用的参数来源或计算公式不同.(3)从表4可以看出,引用NR LXRF修改版中的激发因子算法计算出来的理论强度比与实测值之间的相对偏差最小,说明NR LXRF修改版提供的激发因子算法较为可靠.但是,理论计算的强度比与实验测得值之间仍有约28%的平均相对偏差,说明要提高L和M系列主要谱线理论强度计算的准确性,很大程度上将取决于L和M系列谱线的荧光产额、谱线分数和吸收限陡变因子的实测值或计算值准确度的进一步提高.R eferences1T ao,G.Y.;Zhuo,S.J.;Ji,A.Acta Chimica Sinica1998,56,873(in Chinese).2T ao,G.Y.;Zhuo,S.J.;Ji,A.;N orrish,K.;Fazey,P.;Sen ff,U.E.X -Ray Spectrometry1998,27,357.3T ao,G.Y.;Zhuo,S.J.;Ji,A.Fenxi Huaxue1998,26,1251(in Chinese).4Criss,J.W.NR LXRF,COSMIC Program and Documentation DOD-65,Computer So ftware Management and Information Center,University ofG eorgia,Athens,G A30602,US A,1977.5T ao,G.Y.;N orrish,K.;Fazey,P.Fenxi Huaxue1992,20,94(in Chinese).6Broll,N.X-Ray Spectrometry1986,15,271.7de Boer,D.K.G.Spectrochim.Acta1989,44B,1171.8Bambynek,W.;Crasemann,B.;Fink,R.W.;Freund,H.U.;M ark,H.;S wift,C.D.;Price,R.E.;Rao,P.V.Rev.Mod.Phys.1972,44,716.9Freund,H.U.X-Ray Spectrometry1975,4,90.10K rause,M.O.J.Phys.Chem.Re f.Data1979,8,307.11Scofield,J.H.Phys.Rev.1969,179,9.12Salem,S.I.;Panossian,S.L.;K rause,R.A.At.Data Nucl.Data Tables1974,14,91.13M cM aster,W.H.;Del G rande,N.K.;M allett,J.H.;Hubbell,J.H.Report UCR L-50174,Liverm ore,1969.(Ed.CHE NG Biao)(DONG Hua-Zhen)231 化学学报V ol.59,2001。

电气专业英汉词汇对照X,Y,Z

电气专业英汉词汇对照X,Y,Z

电气专业英汉词汇对照Xx-radiation thickness meter x射线厚度计X-ray X射线;伦琴射线;X光X-ray absorption spectrometer X射线吸收式光谱仪X-ray analysis X射线分析法X-ray analyzer X射线分析器X-ray apparatus for structure analysis 结构分析用X射线分析X-ray beam stop X射线光束截捕器X-ray cinematography X射线电影摄像法X-ray controller X射线控制器X-ray crystal spectrometer X射线晶体光谱仪X-ray detector X射线探测器X-ray diffraction analysis X射线衍射分析法X-ray diffractometer X射线衍射仪X-ray energy dispersive spectrometr X-射线能量分散谱仪X-ray energy spectrometr X射线能谱仪X-ray filter X射线过滤器X-ray fluoremetry logger X射线荧光测井仪X-ray fluoresce readout analyser X射线荧光直读分析仪X-ray fluorescence analysis X射线荧光分析法X-ray fluorescent emission spectrometer X射线荧光发射光谱仪X-ray fluorimeter X射线荧光仪X-ray fluorimeter in borehole 井下X射线荧光仪X-ray goniometer X射线测角仪X-ray high voltage generator X射线高压发生器X-ray intensity X射线强度X-ray monochromator X射线单色器X-ray photo-electron spectrometer (XPS) X射线光电子能谱仪X-ray photo electron spectroscopy (XPS) X射线光电子能谱法X-ray powder diffractometer X射线粉末衍射仪X-ray spectrograph X射线摄谱仪X-ray spectrometer X射线光谱仪X-ray spectrometer arrangement X射线分光装置X-ray spectrum X射线光谱X-ray television apparatus for industry 工业X射线电视装置X-ray transducer [sensor] X射线传感器X-ray tube X射线管X-ray tube current X射线管电流X-ray tube head X射线管头X-ray tube rating charts X射线管负荷特性曲线X-ray tube shield X射线管防护罩X-ray tube voltage X射线管电压X-ray tube window X射线管窗口X-ray wave length dispersive spectrometer X射线波长色散谱仪X-Y recorder XY记录仪电气专业英汉词汇对照YY-modulation Y调制角yaw probe 偏流侧向探头yield point 屈服点yield strength 屈服强度yoke 支架;磁轭yoke method 极间法电气专业英汉词汇对照Zz-domain Z域z-plane Z平面z-transfer function Z(变换)传递函数z-transform Z变换zenith distance 天顶距zero 零点;零位zero adjustment 调零装置zero-based conformity 零基一致性zero-based linearity 零基线性度zero calibration gas 零点校准气zero capacitance 零电容zero displacement value 零位位移植zero drift 零点漂移zero elevation 零点提升zero error 零点误差zero inductance 零电感zero-input response 零输入响应zero knives linear 零刀联线zero-length spring gravimeter 零长弹簧重力仪zero-line oscillating 零线抖动zero-line [reference] marker 零线装置zero-measurand output 零输出zero output base line 零输出基线zero point 零点zero-point output 零点输出zero scale mark 零(标度)标记;零标度线zero shift 零点迁移[偏移]zero-state response 零状态响应zero suppression 零点下降zero variation 不回零位zigzag scan Z形扫查;锯齿形扫查zinc oxide series gas sensor ZnO系气敏元件zinc oxide varistor 氧化锌电压敏电阻器zirconia sensor 氧化锆传感器zirconium doxide oxygen analyzer 氧化锆氧分析器Zoom lens Zoom透镜。

费希尔X射线系列产品数据表说明书

费希尔X射线系列产品数据表说明书

DATA SHEETCoating Thickness Material AnalysisFISCHERSCOPE® X-RAY XDL® 210 FISCHERSCOPE® X-RAY XDL® 220 FISCHERSCOPE® X-RAY XDL® 230 FISCHERSCOPE® X-RAY XDL® 240X-ray fluorescence spectrometer for manual or automated coating thickness measurements on protective and decorative coatings, mass-produced parts and pc-boardsFISCHERSCOPE X-RAY2 FISCHERSCOPE X-RAY XDLDescriptionThe FISCHERSCOPE ®-X-RAY XDL ® instruments are universally applicable energy-dispersive x-ray spectrometers. They represent the next step in the development of the proven FISCHERSCOPE X-RAY XDL-B model series. Like their predecessors, they are particularly well suited for non-destructive thickness measurements and analysis of thin coatings, for measurements on mass-produced parts and pc-boards as well as for the solution analysis.A high count rate is achieved by using a proportional counter tube, which allows for precise measurements. Using the Fischer fundamental parameter method, coating systems as well as solid and liquid samples can be analyzed standard-free. It is possible to detect up to 24 elements in the range from chlorine (17) to uranium (92) simultaneously.The XDL x-ray spectrometers have an excellent long-term stability, which among other things is reflected in a significantly reduced calibration effort.The instruments of the XDL series are especially well suited for measurements in quality assurance, reception inspection and production monitoring. Typical areas of application are:∙ Measurement of electro-plated mass-produced parts ∙ Inspection of thin coatings, e.g., decorative chromium-plating ∙ Analysis of functional coatings in the electronics and semiconductor industries∙ Automated measurements, e.g., on pc-boards ∙Solution analysis in the electroplatingDesignThe FISCHERSCOPE X-RAY XDL spectrometers are designed as user-friendly bench-top instruments. According to the intended use, different versions are available with different support stages and with fixed or adjustable Z-axis. XDL 210: Plane support stage, fixed Z-axis XDL 220: Plane support stage, motor-driven Z-axis XDL 230: Manually operable X/Y stage, motor-driven Z-axisXDL 240: Motor-driven X/Y stage that moves into the loading position automatically, when the protective hood is opened. Motor-drivenZ-axis with two speedsA high-resolution color video camera with powerful magnification simplifies the precise determination of the measurement location and visualizes the measurement procedure in process. In models equipped with a X/Y stage a laser pointer serves as a positioning aid and supports the quick alignment of the sample to be measured.A gap in the housing allows for measurements on large flat specimens, which do not fit in the measuring chamber, e.g. large pc-boards.The entire operation, the evaluation of the measurement as well as the clear presentation of the measurement data is done on a PC using the powerful and user-friendly WinFTM ® software.XDL spectrometers are fully protected instruments with type approval according to the German regulations …Deutsche Röntgenverordnung-RöV“.XDL3General SpecificationsIntended use Energy dispersive x-ray fluorescence spectrometer (EDXRF) to determine thin coatings and for the solution analysis.Element range Chlorine Cl (17) to Uranium U (92) – up to 24 elements simultaneously DesignBench-top unit with hood opening upwards Measuring direction From top to bottomX-ray sourceX-ray source Tungsten tube with beryllium window High voltage Adjustable 30 kV, 40 kV, 50 kVAperture (collimator) Ø 0.3 mm (optional Ø 0.1 mm, Ø 0.2 mm, slot 0.3 mm x 0.05 mm)Measurement spotDepending on the measuring distance and on the aperture, the actual measurement spot size is shown in the video image.Smallest measurement spot: approx. Ø 0.16 mmMeasuring distance e.g., for measurements in recesses 0 ... 80 mm, in the non-calibrated range using the patented DCM method 0 ... 20 mm, in the calibrated range using the patented DCM methodX-ray detectionX-ray detector Proportional counterSample orientationVideo microscopeHigh-resolution CCD color camera for optical monitoring of the measurement location along the primary beam axis, manual focusing and auto-focus, crosshairs with a calibrated scale (ruler) and spot-indicator, adjustable LED illumination of the measurement locationZoom faktor 20x ... 180x (optical: 20x … 45x; digital: 1x, 2x, 3x, 4x)Sample support stageXDL 210 XDL 220 XDL 230 XDL 240 Design Fixed sample supportFixed sample support Manual X/Y-stage Programmable X/Y-stage Maximum travel X/Y - - 95 x 150 mm255 x 235 mm Travel speed X/Y- - - ≤ 80 mm/s Repeatability precision X/Y ---≤ 0,01 mm (*1) Usable sample placement area463 x 500 mm 463 x 500 mm 420 x 450 mm 300 x 350 mm Z-axis Fixed Position (Top/Middle/Bottom)Electrically adjustable Electricallyadjustable Electrically adjustable Travel Z-axis - 140 mm 140 mm 140 mm Max. sample mass 20 kg 20 kg 20 kg 5 kg / 20 kg (*2) Max. sample height155/90/25 mm140 mm140 mm140 mmLaser pointer to support accurate sample placement- Yes Yes Yes(*1) unidirectional (*2) with reduced approach travel precisionFISCHERSCOPE X-RAY XDLCoating Thickness Material Analysis Microhardness Material TestingElectrical dataLine voltage, line frequency AC 115 V or AC 230 V 50 / 60 Hz Power consumption Max. 120 W (measuring head without PC) Protection classIP40DimensionsExterior dimensions Width x depth x height [mm]: 570 x 760 x 650WeightXDL 210: 90 kg; XDL 220: 95 kg; XDL 230: 105 kg; XDL 240: 120 kg Interior dimensions measurement chamberWidth x depth x height [mm]: 460 x 495 x (see max. sample height)Environmental ConditionsTemperature: Operation 10 °C – 40 °C / 50 °F – 104 °F Temperature: Storage/Transport 0 °C – 50 °C / 32 °F – 122 °F Humidity of ambient air ≤ 95 %, non-condensingEvaluation unitComputer PC system with extension cards Software Fischer WinFTM ®StandardsCE conformity EN 61010X-ray standards DIN ISO 3497 and ASTM B 568ApprovalFully protected instrument with type approval according to the German regulations …Deutsche Röntgenverordnung-RöV“OrderFISCHERSCOPE X-RAY XDL 210 604-492 FISCHERSCOPE X-RAY XDL 220 604-494 FISCHERSCOPE X-RAY XDL 230604-496 FISCHERSCOPE X-RAY XDL 240604-498Helmut Fischer GmbH Institut für Elektronik und Messtechnik , 71069 Sindelfingen, Germany ,Tel.+4970313030,**********************Fischer Instrumentation (GB) Ltd, Lymington/Hampshire SO41 8JD, England ,Tel.+441590684100,*****************.uk Fischer Technology, Inc., Windsor, CT 06095, USA ,Tel.+18606830781,***************************Helmut Fischer AG , CH-6331 Hünenberg, Switzerland ,Tel.+41417850800,*****************************Fischer Instrumentation Electronique , 78180 Montigny le Bretonneux, France ,Tel.+33130580058,************************Helmut Fischer S.R.L., Tecnica di Misura, 20128 Milano, Italy ,Tel.+39022552626,***********************Fischer Instruments, S.A., 08018 Barcelona, Spain ,Tel.+34933097916,***********************Helmut Fischer Meettechniek B.V., 5627 GB Eindhoven, The Netherlands ,Tel.+31402482255,*****************************Fischer Instruments K.K., Saitama-ken 340-0012, Japan ,Tel.+81489293455,***********************Fischer Instrumentation (Far East) Ltd , Kwai Chung, N.T., Hong Kong ,Tel.+852********,**************************Fischer Instrumentation (S) Pte Ltd , Singapore 658065, Singapore ,Tel.+6562766776,***************************Nantong Fischer Instrumentation Ltd, Shanghai 200333, P.R. China ,Tel.+862132513131,***********************Fischer Measurement Technologies (India) Pvt. Ltd , Pune 411036, India ,Tel.+912026822065,***********************FISCHERSCOPE ®; XDL ®; WinFTM ® are registered trademarks of Helmut Fischer GmbH Institut für Elektronik und Messtechnik, Sindelfingen - Germany.951-062 12/09 05-09。

物理专业 词汇X-Z

物理专业 词汇X-Z
zurich classification 苏里世分类
zwitterion 两性离子
yukawa interaction 汤川相互酌
yukawa potential 汤川势
z axis z轴
z model z模型
zboson z玻色子
zeeman atomic absorption analysis 塞曼原子吸收光分析
zeeman effect 塞曼效应
x ray telescope x 射线望远镜
x ray term x 射线能级
x ray topography x 射线形貌学
x ray tube x 射线管
x rays x 射线
x unit x 单位
x y recorder x y 记录仪
xenon 氙
xenon lamp 氙灯
x ray photoelectron spectroscopy x 射线光电子能谱学
x ray photoemission diffraction x 射线光电发射衍射
x ray refraction x 射线折射
x ray scattering x 射线散射
x ray small angle scattering x 射线小角度散射
物理专业英语词汇(X-Z)
x axis 横座标
x cut x 切割
x radiation 伦琴辐射
x ray absorption x 射线吸收
x ray analysis x 射线分析
x ray apparatus x 射线装置
x ray astronomy x 射线天文学
xi particle 粒子

X-ray

X-ray

实验一:X射线系列实验I布拉格衍射测定X射线的波长和晶格常数通过本实验了解X射线的特点、产生和应用;理解X射线管产生连续X射线谱和特征X射线谱的基本原理;掌握测定X射线的波长和测定样品晶格常数的原理及方法;了解X射线实验仪的基本原理和使用。

训练实验技能和实验素养。

一.引言X射线是德国科学家伦琴(W.C.Röntgen)于1895年在研究阴极射线管时发现的,是人类揭开研究微观世界序幕的“三大发现”之一,给医学和物质结构的研究带来了新的希望。

就在伦琴宣布发现X射线的第四天,一位美国医生就用X射线照相发现了伤员脚上的子弹。

从此,对于医学来说,X射线就成了神奇的医疗手段。

因为这一具有划时代意义的重大发现,伦琴于1901年被授予第一届诺贝尔物理学奖。

X射线可用来帮助人们进行医学诊断和治疗;也可用于工业上的非破坏性材料的检查;在基础科学和应用科学领域内,则被广泛用于晶体结构分析、化学分析和原子结构的研究。

有关X射线的实验非常丰富,其内容十分广泛而深刻。

X射线波长约为10nm到10–2nm之间,与晶体中原子间的距离为同一数量级,是研究晶体结构的有力工具。

本实验是利用德国莱宝公司的X射线实验仪及附件,来测量X射线的波长和晶格常数,从而对X射线的产生、特点和应用有初步的认识。

二.实验目的1、利用钼靶的特征X-ray研究NaCl晶体的布拉格散射;2、确定Kα与KβX-ray的波长;3、验证布拉格定律。

三.实验原理1.X射线的基本性质X射线(X-ray),又被称伦琴射线或X光,X射线和可见光线一样,也是电磁波的一种,不同的是较之可见光,它的波长更短,介于紫外线和γ射线之间,约10 nm ~ 0.01 nm (注:1 nm = 10-9 m)。

波长小于0.01 nm的称为超硬X射线,在0.01 ~ 0.1 nm范围内的称为硬X射线,0.1 ~ 1 nm范围内的称为软X射线。

其中,波长较短的硬X射线能量较高,穿透性较强,适用于金属部件的无损探伤及金属物相分析;波长较长的软X射线能量较低,穿透性弱,可用于非金属的分析。

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Chandra Fellow Current address: Department of Physics and Astronomy; Ohio University; Athens, OH 45701
–3– understanding of the relevant radiation mechanisms responsible for the high-energy emission of blazars and the underlying particle acceleration mechanisms. The low-energy component of blazar SEDs is well understood as synchrotron emission from ultrarelativistic electrons in a relativistic jet directed at a small angle with respect to the line of sight. In the framework of leptonic models (for a review of the alternative class of hadronic jet models, see, e.g., Rachen (2000)), high-energy emission will result from Compton scattering of lower-frequency photons off the relativistic electrons. Possible target photon fields for Compton scattering are the synchrotron photons produced within the jet (the SSC process; Marscher & Gear (1985); Maraschi, Ghisellini, & Celotti (1992); Bloom & Marscher (1996)), or external photons (the EC process). Sources of external seed photons include the UV – soft X-ray emission from the disk — either entering the jet directly (Dermer, Schlickeiser, & Mastichiadis 1992; Dermer & Schlickeiser 1993) or after reprocessing in the broad line region (BLR) or other circumnuclear material (Sikora, Begelman, & Rees 1994; Blandford & Levinson 1995; Dermer, Sturner, & Schlickeiser 1997) —, jet synchrotron radiation reflected at the BLR (Ghisellini & Madau 1996; Bednarek 1998; B¨ ottcher & Dermer 1998), or the infrared emission from circumnuclear dust (Bla˙ zejowski et al. 2000; Arbeiter, Pohl, & Schlickeiser 2002). According to the now well-established AGN unification scheme (Urry & Padovani 1995), blazars can be unified with other classes of AGN, in particular radio galaxies, through orientation effects. However, Sambruna, Maraschi, & Urry (1996) have pointed out that such orientation effects can not explain the differences between different blazar sub-classes. Instead, it has been suggested that the sequence of spectral properties of blazars from HBLs via LBLs to FSRQs can be interpreted in terms of an increasing total power input into nonthermal electrons in the jet, accompanied by an increasing contribution of external photons to the seed photon field for Compton upscattering (Madejski 1998; Ghisellini et al. 1998). It has been suggested that this may be related to an evolutionary effect due to the gradual depletion of the circumnuclear material being accreted onto the central black hole (D’Elia & Cavaliere 2000; Cavaliere & D’Elia 2002; B¨ ottcher & Dermer 2002). Detailed modeling of blazars in the different sub-classes (FSRQs, LBLs and HBLs) seems to confirm this conjecture (for a recent review, see, e.g., B¨ ottcher (2002)). As mentioned earlier, blazars tend to exhibit rapid flux and spectral variability. The variability is most dramatic and occurs on the shortest time scales at the high-energy ends of the two nonthermal spectral components of their broadband SEDs. Particularly interesting variability patterns could be observed at X-ray energies for those blazars whose X-ray emission is dominated by synchrotron emission. Observational studies of X-ray variability in blazars have so far focused on HBLs and, in particular, on the attempt to identify clear pat-
Department of Physics and Astronomy, Rice University, 6100 Main Street, Houston, TX 77005-1892 mboett@ and James Chiang NASA Goddard Space Flight Center, Code 661, Greenbelt, MD 20771 Joint Center for Astrophysics and Physics Department, University of Maryland, Baltimore, MD 21250 jchiang@ ABSTRACT We are presenting a detailed parameter study of the time-dependent electron injection and kinematics and the self-consistent radiation transport in jets of intermediate and low-frequency peaked BL Lac objects. Using a time-dependent, combined synchrotron-self-Compton and external-Compton jet model, we study the influence of variations of several essential model parameters, such as the electron injection compactness, the relative contribution of synchrotron to external soft photons to the soft photon compactness, the electron-injection spectral index, and the details of the time profiles of the electron injection episodes giving rise to flaring activity. In the analysis of our results, we focus on the expected X-ray spectral variability signatures in a region of parameter space particularly well suited to reproduce the broadband spectral energy distributions of intermediate and low-frequency peaked BL Lac objects. We demonstrate that SSCand external-Compton dominated models for the γ -ray emission from blazars are producing significantly different signatures in the X-ray variability, in particular in the soft X-ray light curves and the spectral hysteresis at soft X-ray energies, which can be used as a powerful diagnostic to unveil the nature of the high-energy emission from BL Lac objects.
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