Limit dilution method: determination of correction factors for resolving matrix effects in X-ray fluorescence analysis

1988 ◽  
Vol 43 (6-7) ◽  
pp. 811-818 ◽  
Author(s):  
F.Bosch Reig ◽  
T.Domenech Carbó ◽  
V. Peris Martinez ◽  
J.V.Gimeno Adelantado
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.


1968 ◽  
Vol 12 ◽  
pp. 546-562
Author(s):  
R. Tertian

AbstractThe double dilution method has many important advantages. For any element to be determined, let us say A, It enables us to control or calculate the matrix factor (sum of the absorption end enhancement effects) for the sample being Investigated towards A radiation, and it furnishes corrected Intensities which are strictly proportional to A concentration. Thus the results are exact, whatever the general composition of the sample, their accuracy depending only on the quality of measurement and preparation. Another major practical advantage is that the method does not require systematic calibration but only a few permanent standards consisting of a pure compound or of an accurately known sample.The procedure has been tested successfully for accurate determination of rare earth elements using, for solid materials such as ores and oxide mixtures, the borax fusion technique. It also can be readily applied to liquids. All the rare earth elements can be titrated by that method, as well as yttrium, thorium and, if necessary, all the elements relevant to X-ray fluorescence analysis. The concentration range considered for solids is of one comprised between 0.5 and 100 % and, with a lesser accuracy, between 0.1 and 0-5 % Examples are given relative to the analysis of various ores. Finally it rcust be pointed out that the method is universal and applies to the analysis of every solid, especially ores, provided that they can be converted to solid or liquid solutions. It appears that most industrial analyses can be worked on In this way.


1977 ◽  
Vol 21 ◽  
pp. 75-88
Author(s):  
B. S. King ◽  
L. F. Espos ◽  
B. P. Fabbi

An X-ray fluorescence (XRF) method has been devised for the rapid quantitative determination of 16 minor and trace elements in geological materials. This method, a modification of a direct dilution method (1, 2, 3), uses a sample-to-binder ratio of 85:15 for sample preparation. Pellets prepared by this method are durable and do not deteriorate rapidly when exposed to high X-ray irradiation. Interferences and matrix effects are successfully corrected in actual analyses by employment of multiple linear regression equations.Accuracy and precision have been improved over the method previously used in this laboratory. Detection limits have been lowered for Zn, Rb, Y and Zn approximately by the factor of 2. When interelement corrections are made, the XRF values are found to be in good agreement with the preferred chemical values for the 19 international silicate-rock standards.


1992 ◽  
Vol 344 (1-2) ◽  
pp. 16-21 ◽  
Author(s):  
F. Bosch Reig ◽  
V. Peris Martinez ◽  
F. Bosch Mossi ◽  
J. V. Gimeno Adelantado

1973 ◽  
Vol 17 ◽  
pp. 214-224
Author(s):  
C. H. Anderson ◽  
J. E. Mander ◽  
J. W. Leitner

AbstractCorrection factors, termed α-factors, similar to those defined by LaChance and Traill have been generated by the addition of variable, known amounts of individual oxides, or other compounds, to a base cement sample and measuring the x-ray intensities of the elements of interest. The effects of all common constituents of cement on the determination of CaO, SiO2 and Al2O3 were found. Factors for rhodium and chromium primary radiation were determined and, in general, showed small but significant differences. The factors for rhodium at 50kV and 30kV were substantia11y identical. The correction factors were tested through the use of the NBS 1011- 1016 cements as reference standards to analyze the new proposed NBS cement series. The correction factors not only furnished improved calibration curves, but also allowed the determination of CaO, Al2O3 and SiO2 with an average deviation of less than 0.2% (absolute) from the provisional values furnished with the standard samples.


1992 ◽  
Vol 344 (1-2) ◽  
pp. 22-26 ◽  
Author(s):  
F. Bosch Reig ◽  
F. Bosch Mossi ◽  
V. Peris Martinez ◽  
J. V. Gimeno Adelantado

2021 ◽  
Vol 87 (8) ◽  
pp. 12-18
Author(s):  
V. N. Talanova ◽  
O. L. Lependina ◽  
D. Kh. Kitaeva ◽  
N. M. Kabaeva ◽  
R. U. Takazova ◽  
...  

Synthesizing and studying the properties of nanomaterials based on layered molybdenum disulfide, often face a need for rapid elemental analysis and prompt return of the material to the customer. Sometimes, nanoparticles of molybdenum disulfide are to be modified with metal compounds to improve the catalytic or magnetic properties of the material. We propose a method for rapid X-ray fluorescence determination of molybdenum and cobalt in the range of 10 – 50% in such compounds using a bulk method without dilution. Analytical signals were measured at the wavelengths of MoKα and CoKα lines using a VRA-30 spectrometer (Carl Zeiss, Germany; X-ray tube with Rh anode). The metal content was calculated using the derived coupling equations. The determination error ranges within ±2.7% (abs.) and 1.4% (abs.) for Mo and Co, respectively. Correctness of the method was confirmed for a batch of synthesized compounds by comparison of the results obtained with the data of XRF analysis using the dilution method traditionally used in the laboratory. The proposed rapid method provides simplification of the procedure and more than 4-fold shortening of analysis in time, the sample being preserved and can be used for further research.


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.


2010 ◽  
Vol 44 (1) ◽  
pp. 24-27 ◽  
Author(s):  
G. A. Bordovsky ◽  
A. V. Marchenko ◽  
P. P. Seregin ◽  
N. N. Smirnova ◽  
E. I. Terukov

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