X-Ray Fluorescence Analysis of Stainless Steels and Low Alloy Steels Using Secondary Targets and the Exact Program

1978 ◽  
Vol 22 ◽  
pp. 325-335 ◽  
Author(s):  
J. C. Harmon ◽  
G.E.A. Wyld ◽  
T. C. Yao ◽  
J. W. Otvos

Exact is a mini-computer based fundamental parameters program which is utilized for matrix corrections in energy-dispersive X-ray analyses. We have previously shown this technique to work well with radioactive sources. However, due to the limited selection of isotopic sources available and their inherent low X-ray flux, we have investigated the use of Fe, Sn, and Dy secondary-targets as sources of monochromatic X-rays. Results to date indicate that the secondary-targets provide X-ray radiation which has sufficient monochromaticity for our technique to remain valid.

1967 ◽  
Vol 11 ◽  
pp. 63-94 ◽  
Author(s):  
Toshio Shiraiwa ◽  
Nobukatsu Fujino

AbstractWith fluorescent X-ray analysis as routine work, the correction term for the coexistent element can be expressed as linear terms of the weight fraction of the element because the compositions of samples are limited to a small range. Usually those correction factors which require a great deal of work are obtained experimentally. The authors have obtained theoretical equations of fluorescent X-ray intensity which are in good agreement with experimental values. The linear correction factors are obtained from derivatives of those equations, and their values can be easily calculated with a computer. The experimental X-ray intensity versus the weight fractions is usually expressed as a line. However, the linear approximation is not correct over a wide range of the composition. The second derivative of the theoretical equation explains the deviation from the linear approximation and gives the range where the linear approximation is allowed. The calculations are applied to the analysis of stainless steels, several low-alloy steels, and iron ores, and experimental results are corrected by the calculated results. Correction factors for Ni Kα, Fe Kα, Cr Kα, Mn Kα, and Cu Kα in stainless steels and Cr Kα and Mn Kα in low-alloy steels are calculated for coexistent elements such as carbon, silicon, titanium, chromium, manganese, copper, niobium, and molybdenum. For example, standard deviations of chromium and manganese analyzed results in lowalloy steels decrease from 0.169 and 0.044% to0.030 and0.023%, respectively, with theoretical corrections. In the analysis of iron ore, the fluorescent X-ray intensity of iron is affected by combined oxygen, which is different for the various compounds of iron oxides, and other impurities such as alumina, silica, and lime. The correction factors of these are obtained by calculation, and the standard deviation decreases from 1.70 to 0.44% for 55.1 to 68.5% iron. It is found by experiment that the theoretical values have about 1 or 2% of relative errors, and their derivatives also have relative errors of the same order of magnitude. But the ranges of coexistent elements are usually small, a few percent at most in routine work, and the theoretical values can be used in practical analyses.


Author(s):  
D. A. Carpenter ◽  
M. A. Taylor

The development of intense sources of x rays has led to renewed interest in the use of microbeams of x rays in x-ray fluorescence analysis. Sparks pointed out that the use of x rays as a probe offered the advantages of high sensitivity, low detection limits, low beam damage, and large penetration depths with minimal specimen preparation or perturbation. In addition, the option of air operation provided special advantages for examination of hydrated systems or for nondestructive microanalysis of large specimens.The disadvantages of synchrotron sources prompted the development of laboratory-based instrumentation with various schemes to maximize the beam flux while maintaining small point-to-point resolution. Nichols and Ryon developed a microprobe using a rotating anode source and a modified microdiffractometer. Cross and Wherry showed that by close-coupling the x-ray source, specimen, and detector, good intensities could be obtained for beam sizes between 30 and 100μm. More importantly, both groups combined specimen scanning with modern imaging techniques for rapid element mapping.


Author(s):  
D. A. Carpenter ◽  
Ning Gao ◽  
G. J. Havrilla

A monolithic, polycapillary, x-ray optic was adapted to a laboratory-based x-ray microprobe to evaluate the potential of the optic for x-ray micro fluorescence analysis. The polycapillary was capable of collecting x-rays over a 6 degree angle from a point source and focusing them to a spot approximately 40 µm diameter. The high intensities expected from this capillary should be useful for determining and mapping minor to trace elements in materials. Fig. 1 shows a sketch of the capillary with important dimensions.The microprobe had previously been used with straight and with tapered monocapillaries. Alignment of the monocapillaries with the focal spot was accomplished by electromagnetically scanning the focal spot over the beveled anode. With the polycapillary it was also necessary to manually adjust the distance between the focal spot and the polycapillary.The focal distance and focal spot diameter of the polycapillary were determined from a series of edge scans.


2020 ◽  
Vol 86 (10) ◽  
pp. 5-9
Author(s):  
D. G. Filatova ◽  
A. A. Arkhipenko ◽  
M. A. Statkus ◽  
V. V. Es’kina ◽  
V. B. Baranovskaya ◽  
...  

An approach to sorptive separation of Se (IV) from solutions on a novel S,N-containing sorbent with subsequent determination of the analyte in the sorbent phase by micro-x-ray fluorescence method is presented. The sorbent copolymethylenesulfide-N-alkyl-methylenamine (CMA) was synthesized using «snake in the cage» procedure and proven to be stable in acid solutions. Conditions for quantitative extraction of Se (IV) were determined: sorption in 5 M HCl or 0.05 M HNO3 solutions when heated to 60°C, phase contact time being 1 h. The residual selenium content in the solution was determined by inductively coupled plasma mass spectrometry (ICP-MS) using 82Se isotope. The absence of selenium losses is proved and the mechanism of sorption interaction under specified conditions is proposed. The method of micro-x-ray fluorescence analysis (micro-RFA) with mapping revealed a uniform distribution of selenium on the sorbent surface. The possibility of determining selenium in the sorbent phase by micro-RFA is shown. When comparing the obtained results with the results of calculations by the method of fundamental parameters, it is shown the necessity of using standard samples of sorbates to obtain correct results of RFA determination of selenium in the sorbent phase.


1988 ◽  
Vol 32 ◽  
pp. 105-114 ◽  
Author(s):  
H. Schwenke ◽  
W. Berneike ◽  
J. Knoth ◽  
U. Weisbrod

AbstractThe total reflection of X-rays is mainly determined by three parameters , that is the orltical angle, the reflectivity and the penetration depth. For X-ray fluorescence analysis the respective characteristic features can be exploited in two rather different fields of application. In the analysis of trace elements in samples placed as thin films on optical flats, detection limits as low as 2 pg or 0.05 ppb, respectively, have been obtained. In addition, a penetration depth in the nanometer regime renders Total Reflection XRF an inherently sensitive method for the elemental analysis of surfaces. This paper outlines the main physical and constructional parameters for instrumental design and quantitation in both branches of TXRF.


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