The accurate analysis of the elemental composition plays a crucial role in the research of functional materials.The emitting characteristic x-ray fluorescence(XRF)photons can be used for precisely discriminating the s...The accurate analysis of the elemental composition plays a crucial role in the research of functional materials.The emitting characteristic x-ray fluorescence(XRF)photons can be used for precisely discriminating the specified element.The detection accuracy of conventional XRF methodology using semiconductor detector is limited by the energy resolution,thus posing a challenge in accurately scaling the actual energy of each XRF photon.We adopt a novel high-resolution x-ray spectrometer based on the superconducting transition-edge sensor(TES)for the XRF spectroscopy measurement of different elements.Properties including high energy resolution,high detection efficiency and precise linearity of the new spectrometer will bring significant benefits in analyzing elemental composition via XRF.In this paper,we study the Ledge emission line profiles of three adjacent rare earth elements with the evenly mixed sample of their oxide components:terbium,dysprosium and holmium.Two orders of magnitude better energy resolution are obtained compared to a commercial silicon drift detector.With this TES-based spectrometer,the spectral lines overlapped or interfered by background can be clearly distinguished,thus making the chemical component analysis more accurate and quantitative.A database of coefficient values for the line strength of the spectrum can then be constructed thereafter.Equipped with the novel XRF spectrometer and an established coefficient database,a direct analysis of the composition proportion of a certain element in an unknown sample can be achieved with high accuracy.展开更多
Glancing incidence x-ray fluorescence spectrometry using a single-bounce parabolic capillary is proposed for the analysis of layered samples.The divergence of the x-ray beam was 0.33 mrad.In this paper,we used this in...Glancing incidence x-ray fluorescence spectrometry using a single-bounce parabolic capillary is proposed for the analysis of layered samples.The divergence of the x-ray beam was 0.33 mrad.In this paper,we used this instrumental setup to analyze a Si single crystal and a 50 nm HfO_(2) single-layer film deposited on a Si substrate.展开更多
The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectr...The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectrum evaluation method is able to obtain the background-corrected and interference-free net peaks, which is significant for quantization analyses. A variety of analytical parameters and functions to describe the features of the fluorescence spectra of pure elements are used and established, such as the mass absorption coefficient, the Gi factor, and fundamental fluorescence formulas. The FSLS iterative program was compiled in the C language. The content of each component should reach the convergence criterion at the end of the calculations. After a basic theory analysis and experimental preparation, 13 national standard soil samples were detected using a spectrometer to test the feasibility of using the algorithm. The results show that the calculated contents of Ti, Fe, Ni, Cu, and Zn have the same changing tendency as the corresponding standard content in the 13 reference samples. Accuracies of 0.35% and 14.03% are obtained, respectively, for Fe and Ti, whose standard concentrations are 8.82% and 0.578%, respectively. However, the calculated results of trace elements (only tens of lg/g) deviate from the standard values. This may be because of measurement accuracy and mutual effects between the elements.展开更多
Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in therm...Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in thermal power plants,the measurement repeatability of LIBS needs to be further improved due to the difficulty in controlling the stability of the generated plasmas at present.In this paper,we propose a novel x-ray fluorescence(XRF) assisted LIBS method for high repeatability analysis of coal quality,which not only inherits the ability of LIBS to directly analyze organic elements such as C and H in coal,but also uses XRF to make up for the lack of stability of LIBS in determining other inorganic ash-forming elements.With the combination of elemental lines in LIBS and XRF spectra,the principal component analysis and the partial least squares are used to establish the prediction model and perform multi-elemental and proximate analysis of coal.Quantitative analysis results show that the relative standard deviation(RSD) of C is 0.15%,the RSDs of other elements are less than 4%,and the standard deviations of calorific value,ash content,sulfur content and volatile matter are 0.11 MJ kg,0.17%,0.79% and 0.41%respectively,indicating that the method has good repeatability in determination of coal quality.This work is helpful to accelerate the development of LIBS in the field of rapid measurement of coal entering the power plant and on-line monitoring of coal entering the furnace.展开更多
X-ray fluorescence (XRF) analysis utilizes particle size which is resulted from milling of a material. The milling ensures uniform and fine grained powder. The finer and more uniform the particle size is, the better t...X-ray fluorescence (XRF) analysis utilizes particle size which is resulted from milling of a material. The milling ensures uniform and fine grained powder. The finer and more uniform the particle size is, the better the result and easier it is for material quality control. To ensure uniformity in particle size and finer powder, a comparative analysis was conducted with different grinding aids and pressed pellet method was used in obtaining analysis results. Pressed pellets of cement raw meal sample milled with different grinding aids (graphite, aspirin and lithium borate) were subjected to XRF. Graphite produced better particle size uniformity with a corresponding standard deviation that made quality control of raw meal easier and better than aspirin and lithium borate.展开更多
The structure around Ti^(4+) in Bao-SiO_2 -B_2O_3-TiO_2 had been studied by X-ray fluorescence spectra. The results show that the Ti^(4+) mainly exists in the [TiO_4] and enters the network of [SiO_4]. [TiO_4] has the...The structure around Ti^(4+) in Bao-SiO_2 -B_2O_3-TiO_2 had been studied by X-ray fluorescence spectra. The results show that the Ti^(4+) mainly exists in the [TiO_4] and enters the network of [SiO_4]. [TiO_4] has the tendency to change to [TiO_6] with the increase of TiO_2 con-tent. When the TiO_2 content increases to about 20mol% the tendency reaches its maximum.展开更多
Coupling equations used to calculate the chemical composition of substances by X-ray fluorescence analysis can be classified as empirical, theoretical or semi-empirical based on the method for determining the coeffici...Coupling equations used to calculate the chemical composition of substances by X-ray fluorescence analysis can be classified as empirical, theoretical or semi-empirical based on the method for determining the coefficients of the calibration function. The advantages and disadvantages of each class of equations are discussed. Recommendations for the selecting the optimum conditions for determining empirical correction coefficients and their control during analysis are provided.展开更多
Synchrotron X-ray fluorescence analyses of crystal and amorphous clinopyroxene were compared. The results showed that using the synchrotron X-ray as a source of energy, the diffraction X-ray of crystal materials will ...Synchrotron X-ray fluorescence analyses of crystal and amorphous clinopyroxene were compared. The results showed that using the synchrotron X-ray as a source of energy, the diffraction X-ray of crystal materials will seriously affect the X-ray fluorescence analysis. In order to avoid the influence of diffraction, the best way to solve it is to use the monochromatic source, or to have a collimating slit between sample and Si(Li) detector.展开更多
A method using synchrotron radiation X-ray fluorescence analysis to in situ determine trace elements during protein electrophoretically separating process was established. The distribution of elements in protein bands...A method using synchrotron radiation X-ray fluorescence analysis to in situ determine trace elements during protein electrophoretically separating process was established. The distribution of elements in protein bands for human liver cytosolic sample separated by SDS-PAGE was analyzed a-long polyacrylamide gel. The results showed that the protein fraction of peak III in cvtosol was mainly composed of metal ion Zn-associated proteins, being in agreement with that given by atomic absorption spectrometry. Thus, it demonstrated the feasibility of this novel technique for in situ analysis of trace elements in protein bands.展开更多
As the nearest celestial body to the earth, the moon has become a hot spot again in astronomy field recently. The element analysis is a much important subject in many lunar projects. Remote X-ray spectrometry plays an...As the nearest celestial body to the earth, the moon has become a hot spot again in astronomy field recently. The element analysis is a much important subject in many lunar projects. Remote X-ray spectrometry plays an important role in the geochemical exploration of the solar bodies. Because of the quasi-vacuum atmosphere on the moon, which has no absorption of X-ray, the X-ray fluorescence analysis is an effective way to determine the elemental abundance of lunar surface. The CE-1 X-ray fluorescence spectrometer (CE-1/XFS) aims to map the major elemental compositions on the lunar surface. This paper describes a method for quantitative analysis of elemental compositions. A series of ground base experiments are done to examine the capability of XFS. The obtained results, which show a reasonable agreement with the certified values at a 30% uncertainty level for major elements, are presented.展开更多
Determining the contents of F,S(total),and Cl in the studied samples of the limestone and marbles with high calcite contents was carried out by the nondestructive method of WDXRFS(Wavelength Dispersive X-ray Fluoresce...Determining the contents of F,S(total),and Cl in the studied samples of the limestone and marbles with high calcite contents was carried out by the nondestructive method of WDXRFS(Wavelength Dispersive X-ray Fluorescence Spectrometry).All measurements were performed in a vacuum condition using a WDXRF spectrometer S8 TIGER(Bruker AXS,Germany).The studied samples have wide ranges of F,S(total),and Cl contents,and high concentration of calcite(89.5%-99%).Main objective of this research is to develop WDXRF(WD X-ray fluorescence)technique for the determination of F,S(total),and Cl.The calculated values of the ILD(instrumental limit of the detection)were within the interval from 3 for S(total)to 37 for F mg/kg.The repeatability was found to be satisfactory with the relative standard deviations lower than 7%.展开更多
In order to further understand the sources of PM2.5 in Shanghai air, the synchrotron X-ray fluores- cence microprobe at the BL-4A Beamline of Photon Factory of High Energy Accelerator Research Organization, Japan, was...In order to further understand the sources of PM2.5 in Shanghai air, the synchrotron X-ray fluores- cence microprobe at the BL-4A Beamline of Photon Factory of High Energy Accelerator Research Organization, Japan, was applied to analyze the individual PM2.5 particles collected from Shanghai air in the winter of 2007. Eight categories of emission sources were recognized in these individual particles. The source identification shows that most of the analyzed PM2.5 particles are derived from vehicle exhaust and metallurgical emissions. This suggests that the important emission sources of PM2.5 in Shanghai air would be vehicle exhaust and metallurgical activities.展开更多
基金the National Major Scientific Research Instrument Development Project(Grant No.11927805)the National Key Research and Development Program of China(Grant No.2022YFF0608303)+2 种基金the NSFC Young Scientists Fund(Grant No.12005134)the Shanghai-XFEL Beamline Project(SBP)(Grant No.31011505505885920161A2101001)the Shanghai Municipal Science and Technology Major Project(Grant No.2017SHZDZX02)。
文摘The accurate analysis of the elemental composition plays a crucial role in the research of functional materials.The emitting characteristic x-ray fluorescence(XRF)photons can be used for precisely discriminating the specified element.The detection accuracy of conventional XRF methodology using semiconductor detector is limited by the energy resolution,thus posing a challenge in accurately scaling the actual energy of each XRF photon.We adopt a novel high-resolution x-ray spectrometer based on the superconducting transition-edge sensor(TES)for the XRF spectroscopy measurement of different elements.Properties including high energy resolution,high detection efficiency and precise linearity of the new spectrometer will bring significant benefits in analyzing elemental composition via XRF.In this paper,we study the Ledge emission line profiles of three adjacent rare earth elements with the evenly mixed sample of their oxide components:terbium,dysprosium and holmium.Two orders of magnitude better energy resolution are obtained compared to a commercial silicon drift detector.With this TES-based spectrometer,the spectral lines overlapped or interfered by background can be clearly distinguished,thus making the chemical component analysis more accurate and quantitative.A database of coefficient values for the line strength of the spectrum can then be constructed thereafter.Equipped with the novel XRF spectrometer and an established coefficient database,a direct analysis of the composition proportion of a certain element in an unknown sample can be achieved with high accuracy.
基金Project supported by the National Key Research and Development Program of China(Grant No.2021YFF0701202)the National Natural Science Foundation of China(Grant No.11875087)。
文摘Glancing incidence x-ray fluorescence spectrometry using a single-bounce parabolic capillary is proposed for the analysis of layered samples.The divergence of the x-ray beam was 0.33 mrad.In this paper,we used this instrumental setup to analyze a Si single crystal and a 50 nm HfO_(2) single-layer film deposited on a Si substrate.
基金supported by the National Key R&D Project of China(No.2017YFC0602100)the National Natural Science Foundation of China(No.41774147)Sichuan Science and Technology Support Program(No.2015GZ0272)
文摘The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectrum evaluation method is able to obtain the background-corrected and interference-free net peaks, which is significant for quantization analyses. A variety of analytical parameters and functions to describe the features of the fluorescence spectra of pure elements are used and established, such as the mass absorption coefficient, the Gi factor, and fundamental fluorescence formulas. The FSLS iterative program was compiled in the C language. The content of each component should reach the convergence criterion at the end of the calculations. After a basic theory analysis and experimental preparation, 13 national standard soil samples were detected using a spectrometer to test the feasibility of using the algorithm. The results show that the calculated contents of Ti, Fe, Ni, Cu, and Zn have the same changing tendency as the corresponding standard content in the 13 reference samples. Accuracies of 0.35% and 14.03% are obtained, respectively, for Fe and Ti, whose standard concentrations are 8.82% and 0.578%, respectively. However, the calculated results of trace elements (only tens of lg/g) deviate from the standard values. This may be because of measurement accuracy and mutual effects between the elements.
基金supported by National Energy R&D Center of Petroleum Refining Technology of China(RIPP,SINOPEC)National Key Research and Development Program of China(No.2017YFA0304203)+5 种基金Changjiang Scholars and Innovative Research Team in University of Ministry of Education of China(No.IRT_17R70)National Natural Science Foundation of China(Nos.61975103,61875108,61775125 and 11434007)Industrial Application Innovation Project(No.627010407)Scientific and Technological Innovation Project of Shanxi Gemeng US-China Clean Energy R&D Center Co.,Ltd111 Project(D18001)Fund for Shanxi‘1331KSC’。
文摘Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in thermal power plants,the measurement repeatability of LIBS needs to be further improved due to the difficulty in controlling the stability of the generated plasmas at present.In this paper,we propose a novel x-ray fluorescence(XRF) assisted LIBS method for high repeatability analysis of coal quality,which not only inherits the ability of LIBS to directly analyze organic elements such as C and H in coal,but also uses XRF to make up for the lack of stability of LIBS in determining other inorganic ash-forming elements.With the combination of elemental lines in LIBS and XRF spectra,the principal component analysis and the partial least squares are used to establish the prediction model and perform multi-elemental and proximate analysis of coal.Quantitative analysis results show that the relative standard deviation(RSD) of C is 0.15%,the RSDs of other elements are less than 4%,and the standard deviations of calorific value,ash content,sulfur content and volatile matter are 0.11 MJ kg,0.17%,0.79% and 0.41%respectively,indicating that the method has good repeatability in determination of coal quality.This work is helpful to accelerate the development of LIBS in the field of rapid measurement of coal entering the power plant and on-line monitoring of coal entering the furnace.
文摘X-ray fluorescence (XRF) analysis utilizes particle size which is resulted from milling of a material. The milling ensures uniform and fine grained powder. The finer and more uniform the particle size is, the better the result and easier it is for material quality control. To ensure uniformity in particle size and finer powder, a comparative analysis was conducted with different grinding aids and pressed pellet method was used in obtaining analysis results. Pressed pellets of cement raw meal sample milled with different grinding aids (graphite, aspirin and lithium borate) were subjected to XRF. Graphite produced better particle size uniformity with a corresponding standard deviation that made quality control of raw meal easier and better than aspirin and lithium borate.
文摘The structure around Ti^(4+) in Bao-SiO_2 -B_2O_3-TiO_2 had been studied by X-ray fluorescence spectra. The results show that the Ti^(4+) mainly exists in the [TiO_4] and enters the network of [SiO_4]. [TiO_4] has the tendency to change to [TiO_6] with the increase of TiO_2 con-tent. When the TiO_2 content increases to about 20mol% the tendency reaches its maximum.
文摘Coupling equations used to calculate the chemical composition of substances by X-ray fluorescence analysis can be classified as empirical, theoretical or semi-empirical based on the method for determining the coefficients of the calibration function. The advantages and disadvantages of each class of equations are discussed. Recommendations for the selecting the optimum conditions for determining empirical correction coefficients and their control during analysis are provided.
文摘Synchrotron X-ray fluorescence analyses of crystal and amorphous clinopyroxene were compared. The results showed that using the synchrotron X-ray as a source of energy, the diffraction X-ray of crystal materials will seriously affect the X-ray fluorescence analysis. In order to avoid the influence of diffraction, the best way to solve it is to use the monochromatic source, or to have a collimating slit between sample and Si(Li) detector.
文摘A method using synchrotron radiation X-ray fluorescence analysis to in situ determine trace elements during protein electrophoretically separating process was established. The distribution of elements in protein bands for human liver cytosolic sample separated by SDS-PAGE was analyzed a-long polyacrylamide gel. The results showed that the protein fraction of peak III in cvtosol was mainly composed of metal ion Zn-associated proteins, being in agreement with that given by atomic absorption spectrometry. Thus, it demonstrated the feasibility of this novel technique for in situ analysis of trace elements in protein bands.
文摘As the nearest celestial body to the earth, the moon has become a hot spot again in astronomy field recently. The element analysis is a much important subject in many lunar projects. Remote X-ray spectrometry plays an important role in the geochemical exploration of the solar bodies. Because of the quasi-vacuum atmosphere on the moon, which has no absorption of X-ray, the X-ray fluorescence analysis is an effective way to determine the elemental abundance of lunar surface. The CE-1 X-ray fluorescence spectrometer (CE-1/XFS) aims to map the major elemental compositions on the lunar surface. This paper describes a method for quantitative analysis of elemental compositions. A series of ground base experiments are done to examine the capability of XFS. The obtained results, which show a reasonable agreement with the certified values at a 30% uncertainty level for major elements, are presented.
文摘Determining the contents of F,S(total),and Cl in the studied samples of the limestone and marbles with high calcite contents was carried out by the nondestructive method of WDXRFS(Wavelength Dispersive X-ray Fluorescence Spectrometry).All measurements were performed in a vacuum condition using a WDXRF spectrometer S8 TIGER(Bruker AXS,Germany).The studied samples have wide ranges of F,S(total),and Cl contents,and high concentration of calcite(89.5%-99%).Main objective of this research is to develop WDXRF(WD X-ray fluorescence)technique for the determination of F,S(total),and Cl.The calculated values of the ILD(instrumental limit of the detection)were within the interval from 3 for S(total)to 37 for F mg/kg.The repeatability was found to be satisfactory with the relative standard deviations lower than 7%.
基金Supported by Knowledge Innovation Project of Chinese Academy of Sciences (KJCX3.SYW.N3) National Natural Science Foundation of China (10775172, 10675159)performance under approval of Photon Factory (PF) Program Advisory Committee(Proposal No.2007G502)
文摘In order to further understand the sources of PM2.5 in Shanghai air, the synchrotron X-ray fluores- cence microprobe at the BL-4A Beamline of Photon Factory of High Energy Accelerator Research Organization, Japan, was applied to analyze the individual PM2.5 particles collected from Shanghai air in the winter of 2007. Eight categories of emission sources were recognized in these individual particles. The source identification shows that most of the analyzed PM2.5 particles are derived from vehicle exhaust and metallurgical emissions. This suggests that the important emission sources of PM2.5 in Shanghai air would be vehicle exhaust and metallurgical activities.