Slope-Ratio Technique for the Determination of Trace Elements by X-Ray Spectroscopy: A New Approach to Matrix Problems

1968 ◽  
Vol 22 (4) ◽  
pp. 321-324 ◽  
Author(s):  
Frank Cuttitta ◽  
Harry J. Rose

A new approach to solving matrix problems in x-ray fluorescence analysis of trace elements has been applied to the determination of bromine in saline waters and zinc in silicates. The method requires no prior knowledge of the chemical composition of the sample. Marked matrix effects are minimized by dilution, and the problem of variable backgrounds due to residual matrix effects is solved by using a slope-ratio technique. In this proposed technique, the slope of a standard curve prepared from pure solutions is compared with that of spiked samples. The ratio of the slopes of these two curves permits the calculation of an adjusted background which does not significantly differ from that of an absorbent impregnated with the sample matrix free of the element sought. Experimental parameters concerning the technique are presented. The excellent agreement of the zinc and bromine data with analytical results obtained by more conventional methods suggests that the technique can be used for the determination of other trace constituents in geologic materials. Application of the slope-ratio technique to other modes of instrumental analysis appears feasible.

1987 ◽  
Vol 41 (3) ◽  
pp. 509-512 ◽  
Author(s):  
A. M. E. Balaes ◽  
K. Dixon ◽  
G. J. Wall

This paper describes the development of an accurate, precise, and rapid analytical procedure using x-ray-fluorescence spectrometry for the determination of Nb, Ta, Mg, Al, Si, P, K, Ca, Ti, Mn, Fe, Zr, and Sn in a wide variety of materials resulting from the processing of Ta-Nb-Sn slags to produce Ta-Nb oxides. The method involves evaporation of all the liquids to dryness, a 1:8 fusion of the solid materials with a flux consisting of Na-Li tetraborate and Na2CO3, and the addition of La oxide as a heavy absorber. With the use of a computer program, residual matrix effects are corrected for by influence-factor calculations.


2009 ◽  
Vol 58 (12) ◽  
pp. 1011-1022 ◽  
Author(s):  
Akiko Otaka ◽  
Yoko Yanada ◽  
Akiko Hokura ◽  
Kenji Matsuda ◽  
Izumi Nakai

1976 ◽  
Vol 20 ◽  
pp. 431-436
Author(s):  
J. A. Cooper ◽  
B. D. Wheeler ◽  
G. J. Wolfe ◽  
D. M. Bartell ◽  
D. B. Schlafke

A procedure using tube excited energy dispersive x-ray fluorescence analysis with interelement corrections has been developed for multielement analysis of major and trace elements and ash content of coal, coke, and fly ash. The procedure uses pressed pellets and an exponential correction for interelement effects. The average deviations ranged from about 0.0003% for V at an average concentration of about .003% to 0.1% for S at an average concentration of 4%. About 25 elements were measured and 100 second minimum detectable concentrations ranged from about one part per million for elements near arsenic to about one tenth of one percent for sodium.


1984 ◽  
Vol 28 ◽  
pp. 53-60
Author(s):  
R. D. Giauque ◽  
J. M. Jaklevic ◽  
A. C. Thompson

The potential advantages of synchrotron sources for x-ray fluorescence analysis have been discussed by several authors. These advantages include high incident flux, tunable excitation energies using crystal monochromators, and reduction of scattered background due to polarization effects. Minimum detectable limits have both been calculated and measured, and have demonstrated the improvements that can be achieved vising synchrotron sources. In this paper we present results obtained using tunable, monochromatic excitation and a high resolution lithium-drifted silicon, Si(Li), spectrometer for the quantitative analysis of a variety of sample types. Our experiments were designed to investigate the advantages and limitations of tunable monochromatic excitation with respect to optimum sensitivity, accuracy, and elemental selectivity in energy dispersive x-ray fluorescence analysis.


1975 ◽  
Vol 19 ◽  
pp. 273-292
Author(s):  
B. P. Fabbi ◽  
H. N. Elsheimer ◽  
L. F. Espos

Upgrading a manual X-ray spectrograph, interfacing with an 8K computer, and employment of interelement correction programs have resulted in a several-fold increase in productivity for routine quantitative analysis and an accompanying decrease in operator bias both in measurement procedures and in calculations. Factors such as dead time and self-absorption also are now computer corrected, resulting in improved accuracy. All conditions of analysis except for the X-ray tube voltage are controlled by the computer, which enhances precision of analysis. Elemental intensities are corrected for matrix effects, and from these the percent concentrations are calculated and printed via teletype.Interelement correction programs utilizing multiple linear regression are employed for the determination of the following minor and trace elements; K, S, Rb, Sr, Y, and Zr in silicate rocks, and Ba, As, Sb, and Zn in both silicate and carbonate rock samples. The last named elements use the same regression curves for both rock types. All these elements are determined in concentrations generally ranging from 0.0025% to 4.00%, The sensitivities obtainable range from 0.0001% for barium to 0.001% for antimony. The accuracy, as measured by the percent relative error for a variety of silicate and carbonate rocks, is on the order of 1-7%. The exception is yttrium (13.8%).


1981 ◽  
Vol 25 ◽  
pp. 117-120
Author(s):  
Randall H. Dow

AbstractThe analysis of geological samples by x-ray fluorescence analysis is complicated by matrix effects and sample variability. Diluting the sample in a suitable matrix such as lithium tetraborate and then fusing it helps to reduce problems associated with sample inhomogeneities and reduces matrix effects considerably.Unfortunately, many of the trace elements in the sample can be diluted below their detection limits by this technique. Pressing the ground powder into a hard disk avoids this problem and is less time consuming. Matrix effects can be very serious however, but can be calculated and compensated for by fundamental parameters programs.


Sign in / Sign up

Export Citation Format

Share Document