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
High-throughput powder X-ray diffraction(XRD)with white X-ray beam and an energy-dispersive detector array is demonstrated in this work on a CeO;powder sample on a bending magnet synchrotron beamline at the Shanghai S...High-throughput powder X-ray diffraction(XRD)with white X-ray beam and an energy-dispersive detector array is demonstrated in this work on a CeO;powder sample on a bending magnet synchrotron beamline at the Shanghai Synchrotron Radiation Facility(SSRF),using a simulated energy-dispersive array detector consisting of a spatially scanning silicon-drift detector(SDD).Careful analysis and corrections are applied to account for various experimental hardware-related and diffraction angle-related factors.The resulting diffraction patterns show that the relative strength between different diffraction peaks from energy-dispersive XRD(EDXRD)spectra is consistent with that from angle-resolved XRD(ARXRD),which is necessary for analyzing crystal structures for unknown samples.The X-ray fluorescence(XRF)signal is collected simultaneously.XRF counts from all pixels are integrated directly by energy,while the diffraction spectra are integrated by d-spacing,resulting in a much improved peak strength and signal-to-noise(S/N)ratio for the array detector.In comparison with ARXRD,the diffraction signal generated by a white X-ray beam over monochromic light under the experimental conditions is about 104 times higher.The full width at half maximum(FWHM)of the peaks in q-space is found to be dependent on the energy resolution of the detector,the angle span of the detector,and the diffraction angle.It is possible for EDXRD to achieve the same or even smaller FWHM as ARXRD under the energy resolution of the current detector if the experimental parameters are properly chosen.展开更多
Microwave heating contributes to coal fracturing and gas desorption. However, problems of low penetration depth, local overheating and fracture closure exist. Coal demineralisation by acids has advantages in coal unbl...Microwave heating contributes to coal fracturing and gas desorption. However, problems of low penetration depth, local overheating and fracture closure exist. Coal demineralisation by acids has advantages in coal unblocking and permeability improvement, while it is difficult for acid to enter microcracks.Microwave-asisted acidification may offer an alternative. In this work, XRD,^(1)H-NMR, and SEM were used to evaluate the effect of microwave-assisted acidification on the microstructure of coal. Results show that kaolinite, calcite, and dolomite can be dissolved by acid. After microwave irradiation, the graphitization of microcrystalline structure of carbon improves. Microwave-assisted acidification erodes minerals in coal and enhances the graphitization degree of microcrystalline structure. Compared to individual microwave irradiation or acidification, the pore volume and pore connectivity can be greatly enhanced by microwave-assisted acidification. The NMR permeability of coal increased by 28.05%. This study demonstrates the potential of microwave-assisted acidification for coalbed methane recovery.展开更多
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 the National Key Research and Development Program of China,China(2017YFB0701900)High-Level Special Funds(G02256401 and G02256301)+1 种基金supported by the fund of the Guangdong Provincial Key Laboratory(2018B030322001)the Guangdong-Hong Kong-Macao Joint Laboratory(2019B121205001)。
文摘High-throughput powder X-ray diffraction(XRD)with white X-ray beam and an energy-dispersive detector array is demonstrated in this work on a CeO;powder sample on a bending magnet synchrotron beamline at the Shanghai Synchrotron Radiation Facility(SSRF),using a simulated energy-dispersive array detector consisting of a spatially scanning silicon-drift detector(SDD).Careful analysis and corrections are applied to account for various experimental hardware-related and diffraction angle-related factors.The resulting diffraction patterns show that the relative strength between different diffraction peaks from energy-dispersive XRD(EDXRD)spectra is consistent with that from angle-resolved XRD(ARXRD),which is necessary for analyzing crystal structures for unknown samples.The X-ray fluorescence(XRF)signal is collected simultaneously.XRF counts from all pixels are integrated directly by energy,while the diffraction spectra are integrated by d-spacing,resulting in a much improved peak strength and signal-to-noise(S/N)ratio for the array detector.In comparison with ARXRD,the diffraction signal generated by a white X-ray beam over monochromic light under the experimental conditions is about 104 times higher.The full width at half maximum(FWHM)of the peaks in q-space is found to be dependent on the energy resolution of the detector,the angle span of the detector,and the diffraction angle.It is possible for EDXRD to achieve the same or even smaller FWHM as ARXRD under the energy resolution of the current detector if the experimental parameters are properly chosen.
基金supported by the National Natural Science Foundation of China (Nos. 52274195, 52274196, 51904103, and 52174180)the Science and Technology Innovation Program of Hunan Province (No. 2022RC1178)+1 种基金Hunan Provincial Natural Science Foundation of China (Nos. 2022JJ20024, and 2021JJ30254)Scientific Research Foundation of Hunan Provincial Education Department (No. 21B0465)。
文摘Microwave heating contributes to coal fracturing and gas desorption. However, problems of low penetration depth, local overheating and fracture closure exist. Coal demineralisation by acids has advantages in coal unblocking and permeability improvement, while it is difficult for acid to enter microcracks.Microwave-asisted acidification may offer an alternative. In this work, XRD,^(1)H-NMR, and SEM were used to evaluate the effect of microwave-assisted acidification on the microstructure of coal. Results show that kaolinite, calcite, and dolomite can be dissolved by acid. After microwave irradiation, the graphitization of microcrystalline structure of carbon improves. Microwave-assisted acidification erodes minerals in coal and enhances the graphitization degree of microcrystalline structure. Compared to individual microwave irradiation or acidification, the pore volume and pore connectivity can be greatly enhanced by microwave-assisted acidification. The NMR permeability of coal increased by 28.05%. This study demonstrates the potential of microwave-assisted acidification for coalbed methane recovery.