Dispersive X-ray Fluorescence Research Articles

Areas for Improvement in XRF Analysis of Low Atomic Number Elements

Accurate analysis of the light elements has been, from the early applications of X-ray fluorescence spectrometry a struggle compared to the determination of heavy elements in the same matrices. In contrast, there has been virtually no upper limit to the atomic number of the element that could be determined. The lower limit, however, has been continuously adjusted downward through the years. Clearly, the sensitivity as well as the lower limit of detection for the heavy elements have also been improved, but the effect is Jess striking than the advances made in the region of tight element performance. This paper deals specifically with wavelength dispersive sequential x-ray fluorescence spectrometry, although some of the observations made are equally applicable to energy dispersive spectrometry.

Backscatter/Fundamental-Parameters Analysis of Unweighed Samples using Multi-Target, Multi-Crystal Regions of Interest from WDXRF and EDXRF

AbstractA method has been developed to simultaneously compute matrix corrections from a composite spectrum of multi-target energy-dispersive (EDXRF) and multicrystal wavelength—dispersive (WDXRF) x-ray fluorescence systems, A serial line installed between the WDXRF and EDXRF spectrometers via a PDF 11/34a computer allows acquired wavelength data to be digitally transformed into an energy spectrum. The low-energy x-ray information from the WDXRF unit is then coupled with the backscatter coherent/incoherent information from the EDXRF unit, enabling enhanced quantitative analysis for low-atomic-number (low-Z) elements. The peak resolution obtainable from the WDXRF spectra often removes the necessity for peak-overlap corrections.Backscatter intensities obtained from the EDXRF unit are used to provide information on total sample mass and to correct for matrix effects. The resulting backscatter fundamental-parameter (BFP) calculations generally provide an accurate analysis of samples without prior knowledge of the sample matrix. Such an approach is particularly useful for samples in which quantities of carbon, oxygen, and other low-Z constituents cannot be explicitly determined.Regions of interest (ROI) are created by the computer code “PREP” and processed by the BFP code "MSAP" an extension of the “SAP3” computer program for quantitative multielement analysis by energy-dispersive x-ray fluorescence,

Trace Element Analysis of Solutions at the PPB Level

We have developed a technique to determine the dissolved solid components of water and other liquids by Energy- Dispersive X-Ray Fluorescence (EDXRF) spectrometry. The liquid samples are presented to the spectrometer as small dried spots of the residue remaining after evaporation of the liquid. The dried residues are mounted on thin plastic films cemented to 35 mm plastic slide mounts. Elements from sodium through uranium are detected with detection limits less than one nanogram in favorable cases. Precision of the measurement is better than 2 % relative in favorable cases for secondary-target excitation, and is typically 5 to 10 % for direct excitation given the geometry of the instrument. Detection limits are as low as a part per billion relative to the original liquid for solutions whose total dissolved solid content is 1000 part per million or less.

Phosphorus Determination in Borophosphosilicate or Phosphosilicate Glass Films on a Si Wafer by Wavelength Dispersive X-ray Spectroscopy

Films of borophosphosilicate glass (BPSG) or phosphosilicate glass (PSG) are deposited on single crystal Si (100) wafers (typically 4 to 6 inches in diameter) by chemical vapor deposition processes during the fabrication of radiation-hardened microcircuits. These films act as insulator and as passivation layers. Since the P content of the glass layer is critical because of fluidity and corrosion problems, careful certification is required. The certification analysis has been accomplished here previously by empirical energy dispersive (ED) X-ray fluorescence (XRF) methods which use a set of expensive and fragile PSG wafer calibration standards. The results obtained were uncertain and the standards were sometimes broken.

Evidence for mineral matter forms in coal liquefaction extracts

High- and low-temperature ashes from feed coal, coal extract solution and filter cake from a two-stage coal liquefaction process have been studied by X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive X-ray fluorescence (SEM/EDX). Hydrocracking experiments using alumina support only, in place of the active Ni Mo catalyst on alumina, were also carried out, with trace metal analysis of the coal extract solution feed and hydrocracked extracts using atomic absorption and emission spectroscopy. The major mineral transformations occurring were of pyrite to pyrrhotite and the fixation of organic sulphur by calcium carbonate. Mineral particles were not observed in the coal extract solution ashes, even under high magnification, and the study indicated that size alone was not a determining factor as to whether a coal mineral was to be found in a coal-derived liquid. None of the trace metals was deposited on the alumina support under hydrocracking conditions, in marked contrast to the results obtained with the normal Ni Mo catalyst. These results lead to the conclusion that for the deposition of trace elements to occur a reaction must take place and hence the trace elements must be chemically bound in some form.

A Rapid and Precise Computer Method for Qualitative X-Ray Fluorescence Analysis

AbstractThis paper describes a computer method for wavelength dispersive (WD) qualitative X-ray fluorescence (XRF) analysis. It determines the elements, spectral lines, wavelengths, reflection angles and peak intensities of the first and second order reflections in less than half a minute of time using an IBM Series/1 minicomputer. The resolution and precision are significantly better than the energy dispersive (ED) method and when combined with high speed computer recording the speed is comparable.

Energy dispersive X-ray fluorescence analysis in ion-exchange studies

The combination of rapid, semi-quantitative energy dispersive fluorescence X-ray analysis techniques with standard ion-exchange experiments provides a simple, interesting, and educational introduction to this new method of analysis.