Energy dispersive X-ray fluorescence analysis of gallstones

The elemental analysis of south Indian gallstones has been carried out using energy dispersive X-ray fluorescence (EDXRF) spectroscopy. A number of important elements including Fe, Cu, Zn, Br, and Pb were estimated from the EDXRF spectra. The results are presented and discussed.     

Energy dispersive X-ray fluorescence analysis of marine pollution indicators

The present work shows a methodology for the application of EDXRF with a X-ray tube, in the analysis of elements in the following matrices: microalgae, marine algae, marine sediments and corals. Various methods were applied: one using a relative external standard, a fundamental parameters method, an absolute method based on elemental sensitivity, a method which used X-ray fluorescence excitation measured in the back side of the sample for low contents heavy elements determination and a TRXRF method. The thin layer samples were prepared using a plastic resin. The analyzed samples of marine algae, marine sediments and corals belong to a marine ecosystem from the North of Havana City, the most affected area by natural metereological phenomena and human impact.     

Energy dispersive X-ray fluorescence analysis of airborne particulate matter

Positron annihilation lifetime technique was applied to study the electric field dependence of size, intensity and size distribution of free volumes in various liquid crystals negative nematic MBBA(N-(4-methoxybenzylidene)-4-n-butylaniline), positive nematic 5CB (4-cyano-4-n-pentylbiphenyl) and cholesteric mixture of MBBA and cholesteryl oleate. Positron annihilation decay curves were obtained in the direct and alternate electric field range from 0 to 120 V/mm, and annihilation curves were resolved into four lifetime components. The relation between the free volume parameters and the variation of molecular alignment is discussed for nematic and cholesteric liquid crystals.     

Energy dispersive X-ray fluorescence analysis of chloride in reforming catalysts

A relatively less expensive Phillips PV 9500/SY 585 automatic energy dispersive X-ray fluorescence (EDXFR) spectrometer with rhodium target, was modified using a commercial kitchen aluminium wrapping foil filter, for the determination of chloride in bifunctional reforming catalysts. Quantitation of chloride was carried out by the Claisse-Quintin method with a catalyst sample of known chloride content as an external standard. The results of EDXRF chloride analysis of different catalyst samples, containing varying amounts of percent carbon and chloride, compared well (p>0.75) with those obtained by silver chloride precipitation method. The small values of percent relative standard deviations at 0.4 to 4.5% showed a good reproducibility of the method. With the total analysis time of a few minutes combined with no sample preparation, the present method seems to be superior as compared to presently employed methods of chloride analysis in reforming catalysts.     

Determination of tungsten in ores by energy dispersive X-ray fluorescence analysis

The possible determination of tungsten in low grade ores from Northern India, Rajasthan State has been explored by energy dispersive X-ray fluorescence analysis /EDXRF/ technique using radioisotope based excitation of W L X-rays and high resolution Si/Li/ detector system. Finely powdered ore has been diluted with optimal quantity of cellulose and converted into pellets to make it suitable for X-ray analysis after homogenization. The experiments have shown the minimum detectable limit of 33 ppm in diluted matrix. The results are compared with the spectrophotometric stannous chloride-thiocyanate method. EDXRF appears to be encouraging for routine and precise analysis of tungsten in low grade ores.     

Chemometric methods in energy dispersive X-ray fluorescence

Chemometric methods like principal component regression (PCR) are an excellent tool for the determination of matrix parameters from scattered radiation. PCR is used for the determination of carbon, hydrogen and oxygen from water and oil-based samples. This information is used in combination with fundamental parameters to determine zink in liquid samples. The method allows an accurate prediction of element concentrations in strong varying matrices.     

Development of a method for direct determination of solids as thin films by energy dispersive X-ray fluorescence analysis

Solid samples can be analysed as without a prior decomposition step, if they are pulverized and then embedded in a thin layer of a cold-setting polymer. This method is very appropriate for materials which are difficult to decompose or which can be easily contaminated. The sample components are evenly distributed in a thin layer, which improves considerably the signal-tonoise-ratio, and this leads to a decrease of the limits of detection. The reproducibility of the method was tested with cobalt oxide and yttrium oxide and also a mixture of these with silver oxide and manganese dioxide. Between 20 and 60 ng of these elements can be determined without difficulty, with a precision of ± 2–4%. The correlation coefficients found for the calibration graphs were between 0.994 and 0.999.     

Mathematical techniques for quantitative elemental analysis by energy dispersive X-ray fluorescence

Recent interest in the use of automated or semi-automated energy dispersive X-ray fluorescence analysis has created the need for improved mathematical techniques and computer software for use with this type of analysis. The present paper reviews the efforts to date to develop the mathematical techniques necessary for implementing: (1) the library least-squares method for the determination of characteristic elemental X-ray intensities and (2) the use of the Monte Carlo method for extending the fundamental parameters approach to radioisotope and X-ray machine exciting sources for the determination of elemental amounts.     

Micro energy dispersive X-ray fluorescence analysis of polychrome lead-glazed Portuguese faiences

Several glazed ceramic pieces, originally produced in Coimbra (Portugal), were submitted to elemental analysis, having as premise the pigment manufacture production recognition. Although having been produced in Coimbra, their location changed as time passed due to historical reasons. A recent exhibition in Coimbra brought together a great number of these pieces and in situ micro Energy Dispersive X-ray Fluorescence (µ-EDXRF) analyses were performed in order to achieve some chemical and physical data on the manufacture of faiences in Coimbra.     

Biomedical applications of energy dispersive X-ray fluorescence

An X-ray fluorescence method for in vitro analysis of trace elements in biological samples is presented. The method is characterised by the use of an X-ray tube with secondary targets as a monoenergetic radiation source, and by thin specimens. The method has been applied to the analysis of blood serum samples, gunshot residue and urinary calculi.     

Wavelength dispersive X-ray fluorescence imaging using a high-sensitivity imaging sensor

A new wavelength-dispersive X-ray fluorescence (WD-XRF) imaging spectrometer equipped with a high-sensitivity imaging sensor was developed in our laboratory. In this instrument, a straight polycapillary optic was applied instead of a Soller slit as well as a 2D imaging X-ray detector instead of X-ray counters, which are used in conventional WD-XRF spectrometers. Therefore, images of elemental distribution were available after a short exposure time. Ni Kα images and Cu Kα images were clearly obtained at corresponding diffraction angles for a short exposure time of 10 s. By optimizing the spectrometer, the time required for imaging is reduced, leading to XRF image movies. It is difficult to distinguish two peaks (Ti Kα (4.508 keV) and Ba Lα (4.465 keV)) due to the poor energy resolution of EDXRS. However, Ti and Ba images could be successfully observed by the WD-XRF imaging spectrometer. The energy resolution of the developed spectrometer was 25 eV at the Ti Kα peak.     

Improved digital filtering for automated spectral deconvolution in energy dispersive X-ray fluorescence analysis

For the quantitation of overlapping peaks in energy dispersive X-ray fluorescence analysis, a computer program has been developped. It is based on a linear least-squares deconvolution of digitally filtered spectra. The performance of five different filters was studied on simulated spectra with respect to systematic and random errors. It is concluded that a symmetric, zero-weighted filter consisting of a Gauss-shape central lobe and a negative constant involving an energy range of 280 eV gives optimal results. The random error introduced by the filtering procedure is very moderate, so that the total error is only slightly above the value predicted from theory. A series of difficult analytical situations (S/Mo; S/Pb; Ti/V/Ba) are treated satisfactorily. Explantations for problems experienced in the literature are suggested.     

Temperature resolved X-ray diffraction as a tool of thermal analysis

Time and temperature resolved X-ray diffraction was used for thermal analysis. Series of diffraction patterns were measured, while the samples are heated/cooled stepwise or isothermally with freely selectable temperature programs.The method was applied for the investigation of the phase transitions of ammonium nitrate and HMX (1,3,5,7-tetranitro-1,3,5,7-tetraaza-cyclooctane), when the identification of phases was required. Its capability in the field of kinetics is demonstrated with the isothermal investigation of the solid state reaction of ammonium nitrate with copper oxide and the non-isothermal investigation of the high temperature corrosion of nickel, which was performed by means of a difference procedure. For obtaining structural details peak fitting and Rietveld refinement were applied for the investigation of ammonium nitrate and HMX.We are indebted to Mr. K. O. Hartmann, Mr. H. Fietzek and Mr. H. G. Farr for their assistance during the measurements and for the maintenance of the measuring systems.     

Interpretation system for automated wavelength dispersive X-ray fluorescence spectrometry

A prototype expert system for automated interpretation of wavelength dispersive X-ray fluorescence spectra is described. The system consists of two main components: a pre-processor (PREXRF) written in BASIC and a knowledge handling part (INFERXRF) that contains the knowledge base and the inference engine implemented in PROLOG. Both systems rely heavily on the theory of fuzzy sets in an attempt to deal with incomplete and uncertain information. The performance of the interpretation system for automated analysis of simulated and measured samples is demonstrated.     

Analysis of uranium ores by energy dispersive X-ray fluorescence

Summary The determination of uranium in ores by energy-dispersive X-ray fluorescence (XFA) is demonstrated for uranium ore samples of known content. For calibration silica gel standards are used. Matrix effects are corrected by measuring the Compton scattering peaks. The radionuclide ¹⁰⁹Cd as well as a X-ray tube in combination with Mo or Sn as secondary targets are suited as X-ray sources. The mean relative deviation of the values found from the given values is 5%

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Analyse von Uranerzen mit Hilfe der energiedispersiven Röntgenfluorescenz

Zusammenfassung Die Anwendbarkeit der energiedispersen Röntgenfluorescenzanalyse zur Bestimmung des Urangehaltes in Erzen wird am Beispiel von Uranerzproben bekannten Gehaltes demonstriert. Für die Eichung werden Kieselgel-Standards verwendet. Die Matrixeffekte werden mit Hilfe der ComptonStreupeaks korrigiert. Als Röntgenquellen eignen sich sowohl eine ¹⁰⁹Cd-Radionuklidquelle als auch eine Röntgenröhre mit Mo oder Sn als Sekundärtarget. Die mittlere relative Abweichung der Analysenwerte von den gegebenen Werten beträgt 5 %.

     

能量色散X射线荧光光谱背景扣除方法的探讨

能量色散X射线荧光分析使得特征X射线的全能峰叠加在背景之上,针对能量色散X射线荧光谱线背景扣除算法的研究,简述了剥峰法和小波变换法扣除背景的原理,并将这两种方法用于对实际谱线的处理,取得了良好的效果.同时对两种方法的算法和处理效果进行了对比研究,表明剥峰法相对简单,而小波变换法需要考虑小波基和分解层次等的影响,但是对整个谱线的综合处理效果相对要好一些.     

Determination of nickel in lateritic ore by various techniques of energy dispersive X-ray fluorescence analysis

Radiometric techniques of determining the nickel content in lateritic ore samples are described. In some of the methods proposed a semiconductor detector and a multichannel pulse height analyzer are required. In another technique simple portable equipment with a proportional counter was used. Calculation methods of correction for matrix effects were applied, in combination with measurements of the fluorescence to scatter ratio and the use of edge filters.     

Soil characterization by energy dispersive X-ray fluorescence: sampling strategy for in situ analysis.

This work describes a sampling strategy that will allow the use of portable EDXRF (energy dispersive X-ray fluorescence) instruments for "in situ" soil analysis. The methodology covers a general approach to planning field investigations for any type of environmental studies and it was applied for a soil characterization study in the zone of Campana, Argentina, by evaluating data coming from an EDXRF spectrometer with a radioisotope excitation source. Simulating non-treated sampled as "in situ" samples and a soil characterization for Campana area was intended. "In situ" EDXRF methodology is a powerful analytical modality with the advantage of providing data immediately, allowing a fast general screening of the soil composition.     

Energy dispersive transmission X-ray scanning micro-imaging with an X-ray guide tube

A scanning micro-imaging instrument using an energy dispersive transmission X-ray spectrometry is developed. This instrument consists of micro X-ray source, X-ray guide tube, x–y scanning stage, and an SDD (Silicon Drift Detector), which is an energy dispersive X-ray spectrometer with a high throughput signal processor for measuring transmission X-ray spectrum. Using this instrument, (1) two-dimensional imaging of an intermediate product of multi-layer ceramic capacitor, and (2) thickness distribution imaging of an aluminum can-tab top, are performed nondestructively.