Accuracy analysis of iron content of galvanized coating using an X-ray fluorescence spectrometer with an L-spectrum

The accuracy(repeatability and reproducibility) of the iron content analysis of galvanized coating using an X-ray fluorescence spectrometer with an L-spectrum is not better than that of flame atomic absorption spectrometry, sometimes it exceeds the quality control limit.Influences, such as current, voltage, equipment(internal circulating water, 10%CH4+90%Ar, and vacuum) checking, instrument monitoring, sample cleaning, and oper-ators, were investigated by means of 6-sigma and lean operations to improve accuracy.

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.

Optimized online filter stack spectrometer for ultrashort X-ray pulses

Currently,with the advent of high-repetition-rate laser-plasma experiments,the demand for online diagnosis for the X-ray spectrum is increasing because the laser-plasma-generated X-ray spectrum is very important for characterizing electron dynamics and applications.In this study,scintillators and silicon PIN(P-type–intrinsic-N-type semiconductor)diodes were used to construct a wideband online filter stack spectrometer.The X-ray sensor and filter arrangement was optimized using a genetic algorithm to minimize the condition number of the response matrix.Consequently,the unfolding error was significantly reduced based on numerical experiments.The detector responses were quantitatively calibrated by irradiating the scintillator and PIN diode with various nuclides and comparing the measuredγ-ray peaks.A prototype 15-channel spectrometer was developed by integrating an X-ray detector with front-and back-end electronics.The prototype spectrometer could record X-ray pulse signals at a repetition rate of 1 kHz.Furthermore,an optimized spectrometer was employed to record the real-time spectra of laser-driven bremsstrahlung sources.This optimized spectrometer offers a compact solution for spectrum diagnostics of ultrashort X-ray pulses,exhibiting improved accuracy in terms of spectrum measurements and repetition rates,and could be widely used in next-generation high-repetition-rate high-power laser facilities.

Glancing incidence x-ray fluorescence spectrometry based on a single-bounce parabolic capillary

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.

Quantitative analysis results of CE-1 X-ray fluorescence spectrometer ground base experiment

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.

L-shell x-ray fluorescence relative intensities for elements with 62≤Z≤83 at 18 keV and 23 keV by synchrotron radiation

The relative intensities of L-subshell x-ray fluorescence(XRF)for elements with atomic numbers 62≤Z≤83 were measured at two excitation energies,18 keV and 23 keV,using a synchrotron radiation source at a beamline of the Synchrotron Light Center for Experimental Science and Applications in the Middle East(SESAME),Jordan.The experimentally measured results of the relative intensities were compared with the calculated results using the subshell fluorescence yield and the Coster-Kronig transition probabilities recommended by Campbell and the values based on the Dirac-Hartree-Slater model by Puri.The experimental and theoretical results are in agreement.In this work,L XRF relative intensities for the elements Sm,Gd,Tb,Er,Ta,W,Re,Hg,Pb and Bi at energies of 18 keV and 23 keV were measured.

Design and calibration of an elliptical crystal spectrometer for the diagnosis of proton-induced x-ray emission(PIXE)

Laser-driven proton-induced x-ray emission(laser-PIXE) is a nuclear analysis method based on the compact laser ion accelerator. Due to the transient process of ion acceleration, the laser-PIXE signals are usually spurted within nanoseconds and accompanied by strong electromagnetic pulses(EMP), so traditional multi-channel detectors are no longer applicable.In this work, we designed a reflective elliptical crystal spectrometer for the diagnosis of laser-PIXE. The device can detect the energy range of 1 keV–11 ke V with a high resolution. A calibration experiment was completed on the electrostatic accelerator of Peking University using samples of Al, Ti, Cu, and ceramic artifacts. The detection efficiency of the elliptical crystal spectrometer was obtained in the order of 10-9.

Determination of Content of Eight Elements in Metal Coating Smeared on Waste Plastics by X-ray Fluorescence Spectrometry

X-ray fluorescence spectrometry was used to detect the content of eight elements in metal coating smeared on waste plastics,and effects of sample cups,elements in plastic substrate,and interaction of elements in metal coating on detection results were analyzed. The results show that the RSD of the method used to detect element content in the metal coating smeared on the waste plastics ranged from 0.008% to 0.044%; the determination range of the eight elements was 0.002%-52.0%,and their detection limit ranged from 0.0002% to 0.0008%. The determination results of X-ray fluorescence spectrometry were consistent with that of ICP-AES. The method can provide technical support for the determination of damage and pollution caused by metal coating smeared on waste plastics.

Quantitative Analysis of FeMo Alloys by X-Ray Fluorescence Spectrometry

A quantitative analysis method of molybdenum in FeMo alloys by X-ray spectrometry using borate fusion technique was compared with that with pressed pellet. The complete pre-oxidation of FeMo alloys for the preparation of homogeneous fused discs was achieved by employing an automated fusion machine equipped with specially designed O2-blowing nozzles, which used lithium tetra-borate as flux with the addition of lithium nitrate (LiNO3) as oxidizer. The calibration curves of Mo and Fe were used in the quantitative analysis of standard materials and unknown plant samples with satisfactory accuracy and precision, utilizing the corrections of the matrix effects and line overlap. It was confirmed that the newly proposed method of preparing fused glass discs of FeMo alloys can replace the conventional wet chemical analyses requiring the labor intensive and time consuming procedure.

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.

Spectrometer of hard X-ray imager payload onboard the ASO-S mission

A spaceborne hard X-ray spectrometer, composed of an array of 99 scintillation detectors and associated readout electronics, has been developed for the hard X-ray imager(HXI). The HXI is one of the three payloads onboard the advanced space-based solar observatory(ASO-S), which is scheduled to be launched in early 2022 as the first Chinese solar satellite. LaBr3 scintillators and photomultiplier tubes with a super bialkali cathode are used to achieve an energy resolution better than 20% at 30 keV.Further, a new multi-channel charge-sensitive readout application-specific integrated circuit guarantees high-frequency data acquisition with low power consumption. This paper presents a detailed design of the spectrometer for the engineering model of the HXI and discusses its noise and linearity performance.

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.

Test of a High Throughput Detector on the X-ray Crystal Spectrometer of the EAST

An attempt was made to improve the spatio-temporal resolution of the tangen- tial X-ray crystal spectrometer （XCS） on the Experimental Advanced Superconducting Tokamak （EAST） by evaluating experimentally the applicability of a novel X-ray photon detection tech- nology for measuring the satellite spectra of Ar XVII with a high counting rate. High-resolution experimental data on the profiles of ion temperature and plasma rotation velocity facilitate the studies of the mechanisms underlining important physical phenomena, such as plasma heating, L-H transition and momentum transport. Based on silicon diode array and single-photon counting technology, a relatively small area （83.8 x 33.5 mm~） two-dimensional detector was successfully in- stalled and tested in the recent EAST campaign. X-ray photon counting rate higher than 20 MHz was observed for the first time, and high quality satellite spectra were recorded for ion temperature and plasma rotation measurement, indicating that the new technology is suitable for the next-step high-resolution XCS on EAST, and the deployment of a detector array with a much larger X-ray sensing area is planned for better plasma coverage.

Use of portable X-ray fluorescence in the analysis of surficial sediments in the exploration of hydrothermal vents on the Southwest Indian Ridge

Hydrothermal plumes released from the eruption of sea floor hydrothermal fluids contain large amounts of oreforming materials. They precipitate within certain distances from the hydrothermal vent. Six surficial sediment samples from the Southwest Indian Ridge（SWIR） were analyzed by a portable X-ray fluorescence（PXRF） analyzer on board to find a favorable method fast and efficient enough for sea floor sulfide sediment geochemical exploration. These sediments were sampled near, at a moderate distance from, or far away from hydrothermal vents. The results demonstrate that the PXRF is effective in determining the enrichment characteristics of the oreforming elements in the calcareous sediments from the mid-ocean ridge. Sediment samples（〉40 mesh） have high levels of elemental copper, zinc, iron, and manganese, and levels of these elements in sediments finer than 40 mesh are lower and relatively stable. This may be due to relatively high levels of basalt debris/glass in the coarse sediments, which are consistent with the results obtained by microscopic observation. The results also show clear zoning of elements copper, zinc, arsenic, iron, and manganese in the surficial sediments around the hydrothermal vent. Sediments near the vent show relatively high content of the ore-forming elements and either high ratios of copper to iron content and zinc to iron content or high ratios of copper to manganese content and zinc to manganese content. These findings show that the content of the ore-forming elements in the sediments around hydrothermal vents are mainly influenced by the distance of sediments to the vent, rather than grain size. In this way, the PXRF analysis of surface sediment geochemistry is found to satisfy the requirements of recognition geochemical anomaly in mid-ocean ridge sediments. Sediments with diameters finer than 40 mesh should be used as analytical samples in the geochemical exploration for hydrothermal vents on mid-oceanic ridges. The results concerning copper, zinc, arsenic, iron, and manganese and their ratio features can be used as indicators in sediment geochemical exploration of seafloor sulfides.

Design of Time-Resolved Shifted Dual Transmission Grating Spectrometer for the X-Ray Spectrum Diagnostics

A new time-resolved shifted dual transmission grating spectrometer （SDTGS） is designed and fabricated in this work. This SDTGS uses a new shifted dual transmission grating （SDTG） as its dispersive component, which has two sub transmission gratings with different line densities, of 2000 lines/mm and 5000 lines/mm. The axes of the two sub transmission gratings in SDTG are horizontally and vertically shifted a certain distance to measure a broad range of 0.1-5 keV time-resolved X-ray spectra. The SDTG has been calibrated with a soft X-ray beam of the synchrotron radiation facility and its diffraction efficiency is also measured. The designed SDTGS can take full use of the space on a record panel and improve the precision for measuring spatial and temporal spectrum simultaneously. It will be a promising application for accurate diagnosis of the soft X-ray spectrum in inertial confinement fusion.

Spatial resolution and image processing for pinhole camera-based X-ray fluorescence imaging: a simulation study

Spatial resolution and image-processing methods for full-field X-ray fluorescence(FF-XRF)imaging using X-ray pinhole cameras were studied using Geant4simulations with different geometries and algorithms for image reconstruction.The main objectives were:(1)calculating the quantum efficiency curves of specific cameras,(2)studying the relationships between the spatial resolution and the pinhole diameter,magnification,and camera binning value,and(3)comparing image-processing methods for pinhole camera systems.Several results were obtained using a point and plane source as the X-ray fluorescence emitter and an array of 100×100 silicon pixel detectors as the X-ray camera.The quantum efficiency of a back-illuminated deep depletion(BI-DD)structure was above 30%for the XRF energies in the 0.8–9 keV range,with the maximum of 93.7%at 4 keV.The best spatial resolution of the pinhole camera was 24.7μm and 31.3 lp/mm when measured using the profile function of the point source,with the diameter of 20μm,magnification of 3.16,and camera bin of 1.A blind deconvolution algorithm with Gaussian filtering performed better than the Wiener filter and Richardson iterative methods on FF-XRF images,with the signal-to-noise ratio of 7.81 dB and improved signalto-noise ratio of 7.24 dB at the diameter of 120μm,magnification of 1.0,and camera bin of 1.

Simulation Study of Quantitative X-Ray Fluorescence Analysis of Ore Slurry Using Partial Least-Squares Regression

X-ray fluorescence （XRF） in combination with partial least-squares （PLS） regression was employed to analyze the ore slurry grade. Using the Monte Carlo simulation code PENELOPE, X-ray fluorescence spectra of ore samples were obtained. Good accuracy was achieved when this method was used to analyze elements with concentrations of several percent or above. It was demonstrated that the more the number of X-ray fluorescence spectra used to calibrate, the better the obtained accuracy. In this method detector resolution was found to have little or no effect on the results of quantitative analysis. The effect of the concentration of water was investigated as well, and it was found to have little influence on the results.

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.

Potential Applications of X-ray Fluorescence Core Scanner in Elemental Analyses of the Muddy Sediments on the Coastal Shelves of China and in Ecological Study

Large areas of muddy sediments on the coastal shelves of China provide important samples for studying climate and ecological changes.Analysis of a large number of such samples,which is essential for systematic study on environmental information recorded in mud areas because of complicated sedimentary environment and variable sedimentary rate,requires a fast and economical method.In this study,we investigated the potential of X-ray fluorescence core scanner(XRFS),a fast analytical instrument for measuring the elemental concentrations of muddy sediments,and observed a significant correlation between the element concentrations of muddy sediments determined by regular X-ray fluorescence spectrometer(XRF)and XRFS,respectively.The correlations are mainly determined by excitation energy of elements,but also influenced by solubility of element ions.Furthermore,we found a striking link between Al concentrations and marine-originated organic carbon(MOC),a proxy of marine primary productivity.This indicates that MOC is partly controlled by sedimentary characteristics.Therefore,XRFS method has a good potential in fast analysis of a large number of muddy sediment samples,and it can also be used to calibrate MOC in ecological study of coastal seas.

Analysis of Heavy Metals in Human Scalp Hair Using Energy Dispersive X-Ray Fluorescence Technique

Analysis of six heavy metals (Cr, Mn, Ni, Cu, Zn and Mo) in human scalp hair was carried out among various occupational distributions to ascertain their heavy metal burden, using energy dispersive x-ray fluorescence technique (ED-XRF). The result of the analysis shows that mean concentrations (mg/kg) of heavy metals obtained were as follows: Cr = 17.1 ± 12.7;Mn = 3.11 ± 0.50;Ni = 11.3 ± 9.3;Zn = 451 ± 128;Cu = 83.3 ± 35.8 and Mo is 9.16 ± 9.1.While the mean concentrations of Cr, Cu, and Mo were higher in the females, that of Mn, Ni and Zn were more in the males. Statistical analysis of the results for both genders at 0.05 probably shows significant difference for Ni, Zn and Mo while Cr, Mn and Cu showed no significant difference. The relationships between age, body mass, height, and heavy metal concentrations were also investigated. Statistical analysis of the results indicates that there was no correlation between the body mass (R2 ≤ 0.048), height (R2 ≤ 0.002) and heavy metal concentration in hair. Zn showed the highest deviation among other elements in the individual samples for both genders which reflect the individual variation in the concentration of Zn.