FPT: An Integrated Fundamental Parameters Program for Broadband EDXRF Analysis without a Set of Similar Standards

1982 ◽  
Vol 26 ◽  
pp. 355-368 ◽  
Author(s):  
D. A. Gedcke ◽  
L. G. Byars ◽  
N. C. Jacobus

The x-ray fluorescence (XRF) method is well known for its capability to perform fast and accurate quantitative analysis for all elements with atomic numbers greater than ten. Energy dispersive x-ray fluorescence (EDXRF) adds to this capability the benefit of quick qualitative analysis, due to its simultaneous sensitivity to all the elements. The method has the potential for rapid and complete chemical analysis of any sample which arrives on the analytical chemist's doorstep. Although the method has been a productive tool for fast and accurate repetitive analysis of similar samples, its applicability to unique unknowns has been rather limited. The limitation arises from the usual need to calibrate the instrument's response with a set of 6 to 12 standards, whose compositions must be similar to the unknown sample. Anyone who has struggled to develop and maintain such a suite of accurately certified standards knows that a great deal of effort and expense is involved. This effort is well justified when the analyst expects to analyze the same type of material frequently over an extended tine period. However, for a unique sample analysis, the task of developing a suite of similar standards simply makes the analysis impractical. What is needed is a method that requires minimal standards, or uses no standards at all.

Author(s):  
V. V. Damiano ◽  
R. P. Daniele ◽  
H. T. Tucker ◽  
J. H. Dauber

An important example of intracellular particles is encountered in silicosis where alveolar macrophages ingest inspired silica particles. The quantitation of the silica uptake by these cells may be a potentially useful method for monitoring silica exposure. Accurate quantitative analysis of ingested silica by phagocytic cells is difficult because the particles are frequently small, irregularly shaped and cannot be visualized within the cells. Semiquantitative methods which make use of particles of known size, shape and composition as calibration standards may be the most direct and simplest approach to undertake. The present paper describes an empirical method in which glass microspheres were used as a model to show how the ratio of the silicon Kα peak X-ray intensity from the microspheres to that of a bulk sample of the same composition correlated to the mass of the microsphere contained within the cell. Irregular shaped silica particles were also analyzed and a calibration curve was generated from these data.


2014 ◽  
Vol 633 ◽  
pp. 443-446
Author(s):  
Kai Li ◽  
Hai Jian Li ◽  
Ping Wu

This paper studied the problems met in the quantitative analysis of synthetic Mullite phase,which was based on the analysis of various typical Mullite composite scheme. A method of quantitative analysis of Mullite phase (excluding amorphous phase SiO2) by use X-ray diffraction was discussed. The error of the analysis can be verified by chemical analysis of Al2O3 content. The method can effectively improve the accuracy of quantitative analysis of the Mullite phase, the error analysis is less than 3%. The error range can meet the accuracy requirement of Mullite content in the production.Studies show that this method is preliminarily solved how to quantitative the content of mullite phase by X-ray diffraction method .


1991 ◽  
Vol 35 (B) ◽  
pp. 727-736 ◽  
Author(s):  
T. He ◽  
R. P. Gardner ◽  
K. Verghese

EDXRF analysis is conveniently split into two parts: (1) the determination of X-ray intensities and (2) the determination of elemental amounts from X-ray intensities. For the first, most EDXRF analysis has been done by some method of integrating the essentially Gaussian distribution of observed full energy pulse heights. This might be done, for example, by least-square fitting of Gaussian distributions superimposed on a straight line or a quadratic background. Recently more elaborate shapes of the energy peaks also have been considered (Kennedy, 1990). After the X-ray intensities have been determined, interelement effects between the analyte element and other elements must be corrected for in order to obtain the elemental amounts from X-ray intensities. This correction can be done either by an empirical correction procedure as in the influence coefficient method which requires measurements on a number of standard samples to determine the required coefficients, or by theoretical calculation as in the fundamental parameters method which does not require standard samples.


1996 ◽  
Vol 06 (01n02) ◽  
pp. 367-373
Author(s):  
HUIYING YAO ◽  
CHENGZHI JIN ◽  
JINGXIA ZHANG ◽  
BENJIE WU

Application of PiXE On biology, medicine and environment has been successful in the last twenty years. However, with the development of science and technique, lower detectable limit, sub-ppm sensitivity, more accurate quantitative analysis and the element chemical state information were presented which can not be achieved by PIXE. The synchrotron radiation as an excitation source to induce X-ray emission (SXRF) is a very powerful method with all the above requirements. In this paper the advantages of SXRF were discussed and compared with PIXE. The article shows our work on biological field by PIXE and SXRF also.


1979 ◽  
Vol 23 ◽  
pp. 313-316 ◽  
Author(s):  
W. Parrish ◽  
G. L. Ayers ◽  
T. C. Huang

AbstractThis paper outlines the use of an IBM Series/1 small computer for instrument automation and data reduction for X-ray polycrystalline diffractometry and wavelength dispersive X-ray fluorescence spectrometry. The profile fitting method is used to determine 2θ, d and relative peak and integrated intensities in diffraction, and the fundamental parameters method (LAMA program) is used for quantitative analysis of bulk and thin film samples. The methods are precise and rapid.


1986 ◽  
Vol 30 ◽  
pp. 97-104 ◽  
Author(s):  
Michael Mantler

The fundamental-parameter technique is an important tool for quantitative x-ray chemical analysis and is routinely applied for the quantification of bulk specimens and single layer films. A method extending it to multiple film layers has recently been introduced by Mantler and results from such applications have been reported by Huang and Parrish. In addition, fundamental-parameter methods can be employed to predict intensity ratios of fluorescent lines as well as the spectral distribution of radiation scattered by the specimen (shape of the background in the vicinity of emission, lines). This is useful for accurate quantitative analysis in the case of a poor peak-to-background ratio, where the precise determination of net intensities is difficult.


2004 ◽  
Vol 12 (4) ◽  
pp. 20-23 ◽  
Author(s):  
Brian J. Cross ◽  
Kenny C. Witherspoon

Energy-Dispersive X-Ray Spectroscopy (ED-XRS or EDS) is a powerful and easy-to-use technique for the elemental analysis of a wide variety of materials. Most commonly, this technique is called X-Ray Fluorescence (XRF), which classically uses x-ray photon sources to excite the sample. A Scanning Electron Microscope (SEM), of course, uses electrons as the excitation source for microbeam x-ray spectroscopy together with sample imaging using characteristic x-rays and/or secondary electrons. These two XRS techniques are used independently, although often the same sample is analysed by both, to provide complementary information.The advantages of both techniques have been reviewed several times [e.g. 1,2], SEM-EDS being more suited to imaging and microbeam quantitative compositional analysis and maps, and XRF more suited to accurate quantitative analysis, especially for trace elements, while analyzing a much larger area.


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