Chemical shifts in the Kα1,2 and Kβ1,3 X-ray emission spectra for halogen compounds of elements with atomic numbers ranging from 22 to 29 were measured using a wavelength-dispersive X-ray fluorescence spectrometer

This study focuses on the validation of a wavelength dispersive X-ray fluorescence (WD-XRF) spectrometer for the rapid determination of iron (Fe) and zinc (Zn) concentrations in certified reference materials (CRMs). Five CRMs were used to establish calibration curves. The results were analyzed in terms of accuracy, precision, repeatability and linearity to assess the performance of the WD-XRF method. Accuracy was evaluated by comparing measured values to certified values, with relative accuracy calculated for each sample. Precision was determined through repeatability, where samples were measured in at least 7 replicates across different days, and relative standard deviation (RSD) was calculated. Linearity was assessed by plotting measured intensities and concentrations against certified concentrations, with the correlation coefficient (R2) values close to 1, indicating a strong linear relationship. Additionally, the WD-XRF method demonstrated high repeatability, with low RSD values across multiple measurements. The study concluded that WD-XRF is a reliable method for the rapid analysis of elemental composition, providing strong accuracy, precision and linearity for Fe and Zn determination in CRMs and can be applied as a valuable method for rapid and non-destructive analysis in various agricultural and food-related applications. HIGHLIGHTS The effectiveness of wavelength dispersive X-ray fluorescence (WD-XRF) method was evaluated to confirm its reliability for determining the elemental composition, specifically iron (Fe) and zinc (Zn), in plant-based certified reference materials (CRMs). Five CRMs were used for calibration and 2 known samples were used as the test samples to determine the analytical performance of WD-XRF. The linearity and correlation with the certified values of WD-XRF results revealed strong correlation with R-square being greater than 0.95 and the recovery percentage of 2 known samples were range from 98.75 - 109.66 for Fe and Zn concentration. WD-XRF spectrometer can be used as a rapid method for determination of Fe and Zn concentrations in rice seeds. GRAPHICAL ABSTRACT

The particle size and heterogeneity effects on the analyte line were investigated for the analysis of powdered samples by X-ray fluorescence technique. In the analysis of samples utilizing the powder method, these effects caused serious errors with variations in particle size for the emitted intensity. The fluorescence intensities of some elements in pellet samples of cement (the range of particle sizes, < 32 µm, 32–38 µm, 38–45 µm, 45–63 µm, 45–75 µm, 75–106 µm, and 106–150 µm and, at press pressure 3.50 and 1.41 × 107 kg/m2), are measured using a wavelength dispersive X-ray fluorescence (WDXRF) spectrometer for 14 pellets prepared according to the powder method. The results show that the K α X-ray fluorescence intensities from samples can effect about 17% maximum differences in normalized intensities within selected particle sizes. These experimental results were interpreted by comparing with the other experimental results in the literature.

The emergence of the integrated wavelength-dispersive and energy-dispersive Zetium X-ray fluorescence spectrometer technique offered new chances to analyze elemental distribution with minimal sample preparation in complex matrix geological samples-northern Hainan island soils. Wavelength-dispersive X-ray fluorescence was applied for the measurement of bromine in the northern Hainan island soil. To reduce the fluctuations of the low-bromine-content measurement results, a two-channel measurement of bromine was designed, and the average value of the two-channel measurements was used as the final result. The soil samples in northern Hainan Island were rich in iodine, with a content range of a few µg/g to more than 100 µg/g, and these were particularly suitable to be analyzed by energy-dispersive X-ray fluorescence spectrometer. The geological samples in northern Hainan Island were brown, purple, and brown-red soil containing kaolinite, ilmenite, rutile, anatase, and goethite. These soil samples were rich in titanium, aluminum, and iron. The titanium concentration in the northern Hainan Island soil was anomalously high (up to 15.05%), far exceeding the content range of the calibration curve. Owing to the empirical coefficient matrix correction method, unreliable or even unreasonable results were obtained for some elements. By systematically mitigating matrix effects through the development of custom reference materials and building matrix-matched measurement and calibration routines, the quantification of Vanadium, Barium, and major components in northern Hainan Island soil samples was optimized. The efficacy of the X-ray fluorescence spectrometer method was confirmed by comparison with inductively coupled plasma–optical emission spectroscopy analysis. This work demonstrates the capability of the integrated wavelength-dispersive and energy-dispersive Zetium X-ray fluorescence spectrometer technique for reliable quantitative elemental analysis of complex matrix geological samples.

Wavelength dispersive and energy dispersive x-ray fluorescence spectrometers are compared. Separate sections are devoted to principles of operation, sample excitation, spectral resolution, and x-ray detection. Tabulated data from the literature are cited in the comparison of accuracy, precision, and detection limits. Spectral interferences and distortions are discussed. Advantages and limitations are listed for simultaneous wavelength dispersive spectrometers, sequential wavelength dispersive spectrometers, and Si(Li) energy dispersive spectrometers. Accuracy, precision, and detection limits are generally superior for wavelength dispersive spectrometers.

Chemical shifts and full widths at half maximum intensity (FWHM) of Kα and Kβ1,3 X-ray emission lines and differences of full widths at half maximum intensity (ΔFHWM) using metallic element as reference for these emission lines were measured for oxygen compounds of elements in the range 22≤Z≤29 with a Wavelength-Dispersive X-Ray Fluorescence Spectrometer (WDXRF). It was also found larger chemical shifts and FWHM for Kβ1,3 lines than those of Kα ones. It should be noted that the magnitude of the chemical shifts increases with increasing number of ligand atom.

ABSTRACTThe effective atomic numbers of compounds of the first row transition elements were determined experimentally by a scattering method using wavelength dispersive X-ray fluorescence spectrometer. A calibration curve was created by using the intensity ratios of coherent to Compton scattered peaks of pure elements from atomic number 13–48. This relationship was employed to determine the effective atomic numbers of the compounds. The effective atomic numbers were also calculated by using empirical formulas from the literature. Mass attenuation coefficients were calculated using software. The experimentally measured values of the effective atomic numbers with the calculated values by empirical formulas were comparable.

Chemical shift in Lα, Lβ, Lβ, Lβ, Lγ and Lγ emission lines of 47Ag, 48Cd and 50Sn compounds

Rapid quantitative determination of major and trace elements in silicate rocks and soils employing fused glass discs using wavelength dispersive X-ray fluorescence spectrometry

A simple analytical method was developed for the determination of total bromine in fruits and grain products by means of wavelength dispersive X-ray fluorescence spectrometry (WDXRF).Five gram samples of fresh fruits, frozen fruits, dried fruits and grain products were extracted with distilled water twice and diluted to 25 mL with distilled water. The sample solution (0.5 mL) was dripped onto the filter paper, which was dried and analyzed by WDXRF. The working curve was linear in the range of 0 to 10 microg/mL. Recoveries at the level of 5 microg/g were 76-104%. The detection limit was 0.5 microg/g and the determination limit was 1.5 microg/g in foods. Compared to the GC-ECD method, this method gave equivalent results for fresh fruits, frozen fruits and grain products. In addition, some dried fruits, in which a slightly high level was detected, gave almost the same results with the GC-ECD method. Therefore, this method is considered to be available as an alternative to the GC-ECD method.

Wavelength dispersive X-ray fluorescence (WD-XRF) spectroscopy is a widely used instrumental spectroscopy method for a variety of samples.

A precise and accurate compositional characterization methodology using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry for mixed oxide nuclear fuels is reported. The methodology involves pelletization of standards and samples. The calibration plots were made by plotting the percent intensity of analyte X-ray lines against their amount percent. The relative standard deviation were 0.4% and 0.25%, respectively for uranium and thorium, having U ranging from 2.85 to 4.2 (wt%). The analytical results were compared with chemical analysis method and were in good agreement. The developed WDXRF method is non-destructive, fast and better in comparison to chemical analysis methods.

Silicon K X-ray fluorescence spectra of soil samples in a volcano island are measured using a commercially available wavelength dispersive X-ray fluorescence spectrometer for elemental analysis. EXEFS (extended X-ray emission fine structure) are found at the low energy side of the K X-ray fluorescence diagram lines. Synchrotron radiation XANES (X-ray absorption near edge structure) spectra are measured for the same samples and for aerosols collected in the same island. The EXEFS spectra are compared with the XANES spectra. The EXEFS method becomes an easy-to-perform alternative of XANES measurements using a similarity between EXEFS and XANES. We analyze the chemical state of Si in the soil samples.

The handheld X-ray fluorescence spectrometer (hXRF) was applied to major element analysis in the geological samples and the results were compared with the results of the wavelength dispersive X-ray fluorescence spectrometer (WDXRF). In addition, the analytical compositions were confirmed by X-ray diffractometer (XRD) and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX). In the case of pXRF analysis, eight geological reference materials were used to calibrate the analytical method and four known concentration samples were used to prove the method. In research, ten geological samples from Phuket province, Thailand were collected with different depths corresponding to O horizon (0-0.1 m), A horizon (0.1-0.3 m), B1 horizon (0.3-1.0 m), B2 horizon (1.0-2.0 m), C1 horizon (2.0-3.0 m), C2A horizon (3.0-5.0 m), C2B horizon (5.0-8.0 m), C3 horizon (8.0-12.0 m), D horizon (12.0-20.0 m) and RK horizon (> 20.0 m). The elemental analysis results showed that the pXRF results were matched well with that WDXRF results. The concentration range in ten samples were Si (18-22 wt%), Al (12-15 wt%), Fe (1-4 wt%), K (0.4-3.2 wt%) and Ti (0.2-0.4 wt%). The concentration of some elements such as Ca and Mg on those ten samples are low and they are unable to analysed by hXRF. The XRD patterns revealed that all samples consisted of quartz, kaolinite, halloysite, illite, vermiculite and biotite.

Silicon and phosphorus contents in polished and unpolished rice planted in a district of high incidence of amyotrophic lateral sclerosis (ALS) have been determined by neutron activation and X-ray fluorescence methods, and compared with those from control areas. In the neutron activation analysis, beta-ray spectra of 32P produced by the 31P(n, gamma)32P reaction on polished and unpolished rice were measured with a low background beta-ray spectrometer. In the X-ray fluorescence analysis, characteristic X-rays were analyzed with a wavelength dispersive X-ray fluorescence spectrometer. Silicon contents in polished and unpolished rice from the ALS area are 42 micrograms.g-1 and 370 micrograms.g-1, respectively, and the corresponding phosphorus contents are 1,210 micrograms.g-1, and 3,370 micrograms.g-1, respectively. The data for ALS area are equal to those for the control area within standard deviation.

This paper reports the development of a simple method for measuring titanium dioxide in cosmetic products using X-ray fluorescence. A sample is prepared by stirring in a dispersion medium and then filtering with a 0.1 μm pore size membrane filter. The titanium dioxide particles trapped on the dried membrane filter are then measured with a wave-length dispersive X-ray fluorescence spectrometer. This sample preparation procedure was investigated using scanning electron microscopy (SEM), energy dispersive X-ray fluorescence (EDX) mapping, inductively coupled plasma atomic emission spectrometry (ICP-AES) and turbidimetry. Interferences can be separated from the titanium dioxide layer on the membrane filter with this preparation procedure. The relative standard deviation for the analysis is less than 0.4%, the recovery is more than 99.0%, and the calibration curve gives a correlation coefficient of R = 1.000. The detection limit for titanium dioxide using this procedure is 0.02% by weight in product. This method is applicable to various cosmetic products containing powdered titanium dioxide.