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
To explore ways to improve the accuracy of quantitative analysis of samples in the micrometer to nanometer range of magnitudes,we adopted analytical transmission electron microscopy(AEM/EDS)for qualitative and quantit...To explore ways to improve the accuracy of quantitative analysis of samples in the micrometer to nanometer range of magnitudes,we adopted analytical transmission electron microscopy(AEM/EDS)for qualitative and quantitative analysis of pyrite materials.Additionally,the k factor of pyrite is calculated experimentally.To develop an appropriate non-standard quantitative analysis model for pyrite materials,the experimentally calculated k factor is compared with that estimated from the non-standard quantitative analytical model of the instrument software.The experimental findings demonstrate that the EDS attached to a TEM can be employed for precise quantitative analysis of micro-and nanoscale regions of pyrite materials.Furthermore,it serves as a reference for improving the results of the EDS quantitative analysis of other sulfides.展开更多
A kind of excellent CdZnTe crystal has been grown in Yinnel Tech, Inc. in recent years. Based on these CdZnTe crystals and some new techniques, a portable energy-dispersive spectrometer has been constructed which has ...A kind of excellent CdZnTe crystal has been grown in Yinnel Tech, Inc. in recent years. Based on these CdZnTe crystals and some new techniques, a portable energy-dispersive spectrometer has been constructed which has yielded good results. CdZnTe detector has a 3% relative resolution in high-energy field and can detect gamma rays at room temperature. An integrated circuit based on preamplifier and shaping amplifier chips is connected to the detector. Voltage pulses are transformed into digital signals in MCA (multichannel analyzer) and are then transmitted to com- puter via USB bus. Data process algorithms are improved in this spectrometer. Fast Fourier transform (FFT) and nu- merical differentiation (ND) are used in energy peak’s searching program. Sampling-based correction technique is used in X-ray energy calibration. Modified Gaussian-Newton algorithm is a classical method to solve nonlinear curve fitting problems, and it is used to compute absolute intensity of each detected characteristic line.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Funded by the International Science&Technology Cooperation Program of Hubei Province of China(No.2022EHB024)。
文摘To explore ways to improve the accuracy of quantitative analysis of samples in the micrometer to nanometer range of magnitudes,we adopted analytical transmission electron microscopy(AEM/EDS)for qualitative and quantitative analysis of pyrite materials.Additionally,the k factor of pyrite is calculated experimentally.To develop an appropriate non-standard quantitative analysis model for pyrite materials,the experimentally calculated k factor is compared with that estimated from the non-standard quantitative analytical model of the instrument software.The experimental findings demonstrate that the EDS attached to a TEM can be employed for precise quantitative analysis of micro-and nanoscale regions of pyrite materials.Furthermore,it serves as a reference for improving the results of the EDS quantitative analysis of other sulfides.
文摘A kind of excellent CdZnTe crystal has been grown in Yinnel Tech, Inc. in recent years. Based on these CdZnTe crystals and some new techniques, a portable energy-dispersive spectrometer has been constructed which has yielded good results. CdZnTe detector has a 3% relative resolution in high-energy field and can detect gamma rays at room temperature. An integrated circuit based on preamplifier and shaping amplifier chips is connected to the detector. Voltage pulses are transformed into digital signals in MCA (multichannel analyzer) and are then transmitted to com- puter via USB bus. Data process algorithms are improved in this spectrometer. Fast Fourier transform (FFT) and nu- merical differentiation (ND) are used in energy peak’s searching program. Sampling-based correction technique is used in X-ray energy calibration. Modified Gaussian-Newton algorithm is a classical method to solve nonlinear curve fitting problems, and it is used to compute absolute intensity of each detected characteristic line.
