Development and Applications of a Laboratory Micro X-ray Fluorescence (μXRF) Spectrometer Using Monochromatic Excitation for Quantitative Elemental Analysis

Abstract

The analytical characterization and an application example of a novel laboratory X-ray fluorescence (μXRF) microprobe is presented, which combines monochromatic, focused X-ray beam excitation with a high-performance silicon drift detector (SDD) and two-dimensional/three-dimensional (2D/3D) scanning capability. Because of the monochromatic excitation, below the (multiple) Compton/Rayleigh scattering peak region, the XRF spectra obtained by this laboratory spectrometer has similarly high peak-to-background ratios as those which can be obtained at synchrotron sources. However, the flux density difference between the proposed laboratory instrument and current synchrotron end stations is on the order of several orders of magnitude. As a result, sub-ppm minimum detection limits (MDL) for transition metals are obtained for a variety of sample matrices. The monochromatic excitation also allows for the efficient use of an iterative Monte Carlo simulation algorithm to obtain quantitative information on the analyzed samples. The analytical characteristics of this instrument and quantitative results, in combination with an iterative reverse Monte Carlo simulation algorithm, will be demonstrated using measurements conducted on an iron-containing meteorite.

Seasonal Cyclicity in Trace Elements and Stable Isotopes of Modern Horse Enamel

“…Various new methods of fast, high-resolution and non-destructive elemental analyses are now widely available (e.g. [29] [30] [31]), enabling the measurement of trace elements in fossil material without altering the samples. The application of trace element proxies for paleo-environmental reconstructions from tooth enamel using these new methods opens up a whole range of opportunities to reconstruct paleo-seasonality, most noteworthy in terrestrial ecosystems where data for seasonality reconstruction is sparse.…”

Luminescent thermometer based on Eu3+/Tb3+‐organic‐functionalized mesoporous silica

“…The pore size distributions were obtained by analysis of the desorption branch of the isotherms using the Barrett–Joyner–Halenda (BJH) method. Energy dispersive XRF measurements were performed using an in‐house developed μXRF instrument (at Ghent University Analytical Chemistry department) . The instrument has a monochromatic microfocus source (XOS, East Greenbush, NY, USA) and an SDD detector (e2v, Chelmsford, UK).…”

“…Powder X-ray diffraction (PXRD) patterns were recorded on a Thermo Scientific ARL X'TRA diffractometer equipped with a Cu Kα Energy dispersive XRF measurements were performed using an inhouse developed μXRF instrument (at Ghent University Analytical Chemistry department). [26] The instrument has a monochromatic microfocus source (XOS, East Greenbush, NY, USA) and an SDD detector (e2v, Chelmsford, UK). The XRF spectra were analyzed using an AXIL software package.…”

The energy dispersive scheme of X‐ray fluorescence analysis with a crystal polarizer and polycapillary optics

“…As it has been recently shown in, multiple suppression of the background level in the spectral bandwidth of about 1 keV can be obtained by the band‐reject HOPG filter exploiting diffraction extinction. For further sensitivity enhancement, various measurement schemes are applied with polarization or monochromatization of the primary beam . As for X‐ray polarization are commonly used different scattering targets, it is necessary to apply rather powerful X‐ray sources to obtain the required intensity of radiation at the scattering angle near π/2 or a long time exposure.…”

“…For further sensitivity enhancement, various measurement schemes are applied with polarization or monochromatization of the primary beam. [4][5][6][7] As for Xray polarization are commonly used different scattering targets, [5] it is necessary to apply rather powerful X-ray sources to obtain the required intensity of radiation at the scattering angle near π/2 or a long time exposure. In general, in energy range E < 10 keV the polarization scheme with a scattering target provides 3-10 times increase of S/N ratio depending on analyzed material.…”