Energy-dispersive X-ray Spectroscopy for the Quantitative Analysis of Pyrite Thin Specimens

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.

Quantitative energy-dispersive X-ray fluorescence analysis for unknown samples using full-spectrum least-squares regression

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.

Observation and Analysis of VLF Nocturnal Multimode Interference Phenomenon based on Waveguide Mode Theory

Very low frequency(VLF)signals are propagated between the ground-ionosphere.Multimode interference will cause the phase to show oscillatory changes with distance while propagating at night,leading to abnormalities in the received VLF signal.This study uses the VLF signal received in Qingdao City,Shandong Province,from the Russian Alpha navigation system to explore the multimode interference problem of VLF signal propagation.The characteristics of the effect of multimode interference phenomena on the phase are analyzed according to the variation of the phase of the VLF signal.However,the phase of VLF signals will also be affected by the X-ray and energetic particles that are released during the eruption of solar flares,therefore the two phenomena are studied in this work.It is concluded that the X-ray will not affect the phase of VLF signals at night,but the energetic particles will affect the phase change,and the influence of energetic particles should be excluded in the study of multimode interference phenomena.Using VLF signals for navigation positioning in degraded or unavailable GPS conditions is of great practical significance for VLF navigation systems as it can avoid the influence of multimode interference and improve positioning accuracy.

Numerical analysis of matrix swelling and its effect on microstructure of digital coal and its associated permeability during CO_(2)-ECBM process based on X-ray CT data

Matrix swelling effect will cause the change of microstructure of coal reservoir and its permeability,which is the key factor affecting the engineering effect of CO_(2)-ECBM technology.The Sihe and Yuwu collieries are taken as research objects.Firstly,visualization reconstruction of coal reservoir is realized.Secondly,the evolution of the pore/fracture structures under different swelling contents is discussed.Then,the influence of matrix phase with different swelling contents on permeability is discussed.Finally,the mechanism of swelling effect during the CO_(2)-ECBM process is further discussed.The results show that the intra-matrix pores and matrix-edge fractures are the focus of this study,and the contacting area between matrix and pore/fracture is the core area of matrix swelling.The number of matrix particles decreases with the increase of size,and the distribution of which is isolated with small size and interconnected with large size.The swelling effect of matrix particles with larger size has a great influence on the pore/fracture structures.The number of connected pores/fractures is limited and only interconnected in a certain direction.With the increase of matrix swelling content,the number,porosity,width,fractal dimension,surface area and volume of pores/fractures decrease,and their negative contribution to absolute permeability increases from 0.368% to 0.633% and 0.868%-1.404%,respectively.With the increase of swelling content,the number of intra-matrix pores gradually decreases and the pore radius becomes shorter during the CO_(2)-ECBM process.The matrix continuously expands to the connected fractures,and the width of connected fractures gradually shorten.Under the influence of matrix swelling,the bending degree of fluid flow increases gradually,so the resistance of fluid migration increases and the permeability gradually decreases.This study shows that the matrix swelling effect is the key factor affecting CBM recovery,and the application of this effect in CO_(2)-ECBM process can be discussed.

Elemental composition x-ray fluorescence analysis with a TES-based high-resolution x-ray spectrometer

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.

X-ray Manifestations of Pneumoconiosis Patients and Differential Analysis with Pulmonary Tuberculosis

[Objectives]This study was conducted to explore the X-ray manifestations of pneumoconiosis patients and differentiation from pulmonary tuberculosis.[Methods]Retrospective analysis was conducted on 103 patients who underwent lung examinations,including 47 cases of pneumoconiosis and 56 cases of pulmonary tuberculosis.The differences in nodule characteristics and accompanying cavity sign between pneumoconiosis and pulmonary tuberculosis were compared.[Results]The X-ray manifestations of pneumoconiosis patients mainly included various forms of lung images,which were uneven in density,and had blurry edges,and sometimes thickening of lung markings and reduction of lung volume could be observed.The acinar nodules observed in X-ray films of patients with hematogenous disseminated pulmonary tuberculosis appeared petal like.The uniformity of nodule appearance such as nodule distribution,nodule density,and nodule size was significantly lower in pneumoconiosis than in hematogenous disseminated pulmonary tuberculosis,showing a statistical significance(P<0.05).The diameter of cavities in patients with pneumoconiosis accompanied by cavity sign[(0.64±0.13 vs 3.37±0.95)cm]was lower than that in patients with secondary pulmonary tuberculosis accompanied by cavity sign.There was a significant difference in the thickness of the cavity wall between the two diseases,and patients with pneumoconiosis accompanied by cavity sign had a higher rate of thick wall cavities(>3 mm).The X-ray manifestations of pneumoconiosis and tuberculosis were relatively similar,but the distribution,density and size of nodules in pneumoconiosis were relatively uneven,and the patients accompanied by cavity sign had smaller cavity diameter and higher rate of thick-walled cavities.[Conclusions]This study provides a reference for the clinical differential diagnosis of pneumoconiosis and pulmonary tuberculosis.

Use of high-resolution X-ray computed tomography and 3D image analysis to quantify mineral dissemination and pore space in oxide copper ore particles

Mineral dissemination and pore space distribution in ore particles are important features that influence heap leaching performance. To quantify the mineral dissemination and pore space distribution of an ore particle, a cylindrical copper oxide ore sample (I center dot 4.6 mm x 5.6 mm) was scanned using high-resolution X-ray computed tomography (HRXCT), a nondestructive imaging technology, at a spatial resolution of 4.85 mu m. Combined with three-dimensional (3D) image analysis techniques, the main mineral phases and pore space were segmented and the volume fraction of each phase was calculated. In addition, the mass fraction of each mineral phase was estimated and the result was validated with that obtained using traditional techniques. Furthermore, the pore phase features, including the pore size distribution, pore surface area, pore fractal dimension, pore centerline, and the pore connectivity, were investigated quantitatively. The pore space analysis results indicate that the pore size distribution closely fits a log-normal distribution and that the pore space morphology is complicated, with a large surface area and low connectivity. This study demonstrates that the combination of HRXCT and 3D image analysis is an effective tool for acquiring 3D mineralogical and pore structural data.

MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTI-TATIVE X-RAY DIFFRACTION PHASE ANALYSIS

A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.

Comparative Analysis of the Multi-Frequency Bio-impedance and Dual-energy X-ray Absorptiometry on Body Composition in Obese Subjects

To examine accuracy of body composition predicted by the Multi-Frequency Bioelectric Impedance Analysis （MF-BIA） compared with the Dual-energy X-ray Absorptiometry （DXA） in adults with obese. We measured body composition of 749 adults with obese both by the MF-BIA and DXA. The Lin＇s concordance correlation and the Bland-Altman plots were used to examine the consistency. The concordance correlation coefficient of %BF between the MF-BIA and DXA in men and women was 0.560, and 0.669, respectively. Compared with the DXA, the MF-BIA significantly underestimated %BF by 4.33% in men （P 〈 0.001）, however overestimated %BF by 0.50% in women （P 〈 0.001）. After corrected by the correction equations established in this study, the differences were significantly decreased. Therefore, the MF-BIA （TANITA MC-180） may need to be corrected in estimating body composition for adults with obese.

Chemical Analysis of Hydroxyapatite Artificial Bone Powders by Energy Dispersive X-Ray Fluorescence Spectrometry(EDXRF)

Stoichiometric hydroxyapatite(HA)nanoparticles were synthesized by a wet chemical method.Calcium nitrate tetra hydrate used as calcium source and dibasic ammonium phosphate used as phosphorous source.Calcium nitrate tetra hydrate and dibasic ammonium phosphate solutions were prepared by dissolving the salts in distilled water.Stoichiometric hydroxyapatite nanoparticles used by artificial bone powders and synthesized by a wet chemical method were analyzed using EDXRF method.The concentrations of K,Ca,Ti,V,Cr,Fe,Ni,Cu,Sr and Pb for artificial bone powders have been determined.Besides,Calcium contents were evaluated according to the agitation time and temperature in the production process.

Elemental and proximate analysis of coal by x-ray fluorescence assisted laser-induced breakdown spectroscopy

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.

Impact of Different Grinding Aids on Standard Deviation in X-Ray Fluorescence Analysis of Cement Raw Meal

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.

High-Throughput Powder Diffraction Using White X-Ray Beam and a Simulated Energy-Dispersive Array Detector

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.

Application of methods of X-ray diffraction analysis and acoustic emission on research of plastic deformation in steels

Results of researches on plastic deformation of steels were obtained by acoustic emission and X-ray methods.The new numerical-analytical method of the thin structure parameter determination on one diffraction line was offered.It is supposed that with a growth of the deformation the cubic lattice will be transformed in the orthorhombic lattice.It is shown that changes of a condition of crystal structure of austenitic steel occur in four stages and of carbonaceous steel occur in six stages.Existence of two types of acoustic emission sources in carbonaceous steel and one type of acoustic emission source in austenitic steel was proposed.

AN INCREMENTAL METHOD OF X-RAY DIFFRACTION QUANTITATIVE PHASE ANALYSIS OF SAMPLESCONTAINING AMORPHOUS MATERIAL

A new method for quantitative X-ray diffraction phase analysis of a powder misture has been developed according to Popovic's doping method. The weight fraction of amorphous material in the analysed sample is obtained. For a multicomponent system in which (n-2) pure phases are added into an n-phase compnent sample and theweight fractions of all n phases can be determined by the method. The test results of confirmation agree well with the theory.

Alpha-actinin expression at different differentiating time points from temporal lobe cerebral cortex neural stem cells to neuron-like cells using energy dispersive X-ray analysis

BACKGROUND： Alpha-actinin （ a -actinin） plays a key role in neuronal growth cone migration during directional differentiation from neural stem cells （NSCs） to neurons. OBJECTIVE： To detect in situ microdistribution and quantitative expression of a -actinin during directional differentiation of NSCs to neurons in the temporal lobe cerebral cortex of neonatal rats. DESIGN, TIME AND SETTING： Between January 2006 and December 2008, culture and directional differentiation of NSCs were performed at Department of Histology and Embryology, Preclinical Medical College, China Medical University. Immune electron microscopy was performed at Department of Histology and Embryology and Department of Electron Micrology, Preclinical Medical College, China Medical University. Spectrum analysis was performed at Laboratory of Electron Microscopy, Mental Research Institute, Chinese Academy of Sciences. MATERIALS： Basic fibroblast growth factor, epidermal growth factor, brain-derived nerve growth factor, type-1 insulin like growth factor, and a -actinin antibody were provided by Gibco BRL, USA; rabbit-anti-rat nestin monoclonal antibody, rabbit-anti-rat neuron specific enolase polyclonal antibody, and EDAX-9100 energy dispersive X-ray analysis were provided by PHILIPS Company, Netherlands. METHODS： NSCs, following primary and passage culture, were differentiated with serum culture medium （DMEM/F12 ＋ 10% fetal bovine serum ＋ 2 ng/mL brain-derived nerve growth factor ＋ 2 ng/mL type-1 insulin like growth factor）. MAIN OUTCOME MEASURES： Expression of a -actinin in neuron-like cells was quantitatively and qualitatively detected with immunocytochemistry using energy dispersive X-ray analysis. RESULTS： Immunocytochemistry, combined with electron microscopy, indicated that positive α -actinin expression was like a spheroid particle with high electron density. In addition, the expression was gradually concentrated from the nuclear edge to the cytoplasm and expanded into developing neurites, during differentiation of neural stem cells to neurons. Conversely, energy dispersive X-ray analysis indicated that the more mature the neural differentiation was, and the greater the expression of α -actinin. CONCLUSION： The gradual increase of α -actinin expression is related to growth, development, and maturity of differentiated neuron-like cells, in neonatal rat frontal lobe cortex, at different differentiating time points of NSCs to neurons.

A SOLUTION OF MINIMUM NORM FOR QUANTITATIVE PHASE ANALYSIS BY STANDARDLESS X-RAY DIFFRACTION

A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus.The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.

A SOLUTION OF MINIMUM NORM FOR QUANTITATIVE PHASE ANALYSIS BY STANDARDLESS X-RAY DIFFRACTION

A new expression of quantitative phase analysis by standardless X-ray diffraction has been derived using intensity matrix of vector modulus,The criterion of standardless X-ray diffraction analysis was suggested,so as to separate the diffraction pattern of every phase from that of sample.The optimal solution could be obtained by the least squares regression.

DATA PROCESSING OF UNIVERSAL QUANTITATIVE METHOD IN STANDARDLESS X-RAY PHASE ANALYSIS

Accuracy of coeffcient A_(isp) is related to the reference phase chosen during analysis. The cri- terion of choosing reference phase which may minimize the error of A_(isp) was deduced. The optimum results could be obtained by using the method of least squares if the number of sam- pies for analysis is more than the phase in samples. The procedure presented here is satisfacto- ryfor ordinary phase analysis.

Subunit Arrangement of a 2-Ketoisovalerate Ferredoxin Oxidoreductase from Thermococcus profundus Revealed by a Low Resolution X-Ray Analysis

2-ketoisovalerate ferredoxin oxidoreductase (VOR) is a key enzyme in hyperthermophiles catalyzing the coenzyme A-dependent oxidative decarboxylation of aliphatic amino acid-derived 2-keto acids. The enzyme purified under anaerobic conditions from a hyperthermophilic archaeon, Thermococcus profundus, is a hetero-octamer (αβγδ)2 consisting of four different subunits, α = 45 kDa, β = 31 kDa, γ = 22 kDa and δ = 13 kDa, respectively, and it has three [4Fe-4S] clusters per αβγδ-protomer, similar to other ferredoxin oxidoreductases. In the present study, the native enzyme was purified from this strain and crystallized to give rod-like crystals that were suitable for X-ray diffraction experiments. The crystals belonged to space group P41212, with unit-cell parameters a = b = 136.20 ?, c = 221.07 ?. Diffraction images were processed to a resolution of 3.0 ?. The data collected so far indicate the approximate molecular boundaries and a partial main-chain trace of the enzyme.