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.

Geochemical analysis of marine sediments using fused glass disc by X-ray fluorescence spectrometry

一个方法为 Na 的内容决心被开发， Mg ，艾尔， Si ， P ， S ， Cl ， K ， Ca ， Ti ， V ， Cr ， Mn ， Fe ， Ni ， Cu ， Zn ， Ga ， Nb ， Zr ， Y ， Sr ， Rb ， Ba ，在使用的海洋的沉积样品盖住 26 专业，未成年者，和踪迹元素的 La 和 Ce 等等由X光检查荧光 spectrometry 熔化了玻璃圆盘。刻度用海洋的沉积被成为证明引用材料和样品由在不同比例与流沉积和碳酸盐标准样品混合几海洋的沉积准备了的合成标准。矩阵效果用理论高山被改正哈象内部标准的系数，经验系数和散布放射(为踪迹元素) 。方法的精确性被证明参考材料 GBW07314， GBW07334 和 GSMS6 的分析评估。结果在与 RSD 的对标准的证明价值的好同意不到 2.60% 除了 Y，有 RSD 的 Cr， Ga， Ce， La， Nb， Rb，和 V 不到 9.0%(n=12 ) 。

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.

X-ray fluorescence spectrometry determination of open-hearth furnace slag by pressed powder briquetting

A rapid analysis method of determining content of eight compounds of open-hearth furnace slag was developed using X-ray fluorescence spectrometry and pressed powder briquettes. Matrix effect was corrected using theoretical alpha coefficient. Grains-size effect was eliminated by optimized sample preparation technique parameters. Mineral effect was corrected with standard curve of specially made standard samples. The analysis results of TiO2, TFe, SiO2, MgO, Al2O3, CaO, MnO and P2O5 in slag samples showed that both precision and accuracy are comparable with that of chemical method.

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.

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.

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 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.

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.

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.

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.

Speciation Analysis of Arsenic Compounds in Seafood by Ion Chromatography-Atomic Fluorescence Spectrometry

Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L^(-1) CH_3COONH_4 and 15 mmol L^(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L^(-1) for As B, 0.4261 μg L^(-1) for As(III), 0.216 μg L^(-1) for DMA, 0.211 μg L^(-1) for MMA, and 0.709 μg L^(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.

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.

Preliminary determination of calcium,phosphorus,and the calcium/phosphorus ratio in cortical bone of Chinstrap penguin using synchrotron X-ray fluorescence analysis

Synchrotron radiation X-ray fluorescence （SR-XRF） approach was applied to analyzing of Chinstrap penguin （ Pygoscelis Antarctica） cortical bone. The method enabled the in situ determination of Ca and P concentrations and the Ca/P ratio in cortical bone. The preliminary results show that ： （ 1 ） there is the bone site-related difference for Ca and P concentrations. The mean values for the investigated parameters （ on a dry-weight basis） are： 30.7% （Ca） and 14.9% （P） for the femoral cortical bone, 21.4% （Ca） and 11.5% （P） for wing cortical bone. （2） The variation for the Ca/P ratio in cortical bone is lower than those for Ca and P separately. This is in agreement with the previous report that the specificity of the Ca/P ratio is better than that of Ca and P concentrations and is more reliable for the diagnosis of bone disorders. The authors suggest that further studies be conducted to establish norreal values of Ca, P and Ca/P ratio for polar animals and provide a basis for the diagnosis of bone disorders.

Determination of Element Levels of Lagoon from Townships near Cocody City Abidjan Côte D’Ivoire Using Energy Dispersive X-Ray Fluorescence

Eight water bottles from Ebrie lagoon with pollution potency were studied using nuclear chemistry technique and Energy dispersive X-ray fluorescence. This pollution is characterized by pH and conductivity parameters, concentrations average in mg/L of metals such Fe (0.731), Mn (0.345), Cr (0.070), Cu (0.014) and concentrations of nutrients known to be pollutants and toxic for living or-ganisms. These heavy metals are dangerous to the lives, the local inhabitants and also a threat to aquatic life since this water is essential for the economical town, Abidjan. According to the Manganese concentration average (0.345 mg) values that higher than WHO (0.05 mg) value, the main likely source of pollu-tants is anthropogenic, industrial and agricultural. This study also shows the use of materials and lubricants near the lagoon that pollute this water.

Determination of Trace Germanium in Marine Sediments by Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS)

A method for the analysis of trace germanium in marine sediments by HG-AFS has been investigated. The experimental conditions such as the acidity of reduction reaction, the amount of sodium boro-hydride, the carrier gas flow rate, etc., were tested and optimized by using a kind of orthogonal design. The detection limit of the presented method is 0.95 μg L -1 for germanium. The calibration curve shows a satisfactory line in the concentration range 0-320 μg L -1 Ge with a variation coefficient of ±2.1%.

Evaluation of Atomic Fluorescence Spectrometry for Determination of Mercury Using a Low-Powered Argon Microwave Plasma Torch (MPT)

The Microwave-Induced Plasma (MIP) has received considerable attention during the past decade since theintroduction of the Becnakker Cavity. It has been commonly used as an atomization cell for atomic emission spectrometry (AES) and atomic absorption spectrometry (AAS), and a great success was achieved for both techniques. More