Rapid X-ray fluorescence analysis of intercalation compounds for molybdenum and cobalt content

2021 ◽  
Vol 87 (8) ◽  
pp. 12-18
Author(s):  
V. N. Talanova ◽  
O. L. Lependina ◽  
D. Kh. Kitaeva ◽  
N. M. Kabaeva ◽  
R. U. Takazova ◽  
...  
Keyword(s):  
Molybdenum Disulfide ◽  
Cobalt Content ◽  
Fluorescence Analysis ◽  
Dilution Method ◽  
Metal Compounds ◽  
X Ray ◽  
Determination Error ◽  
Coupling Equations ◽  
Comparison Of The Results

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.

A Rapid and Accurate X-Ray Determination of the Rare Earths Elements in Solid or Liquid Materials using the Double Dilution Method

1968 ◽  
Vol 12 ◽  
pp. 546-562
Author(s):  
R. Tertian
Keyword(s):  
Rare Earth ◽  
Rare Earth Elements ◽  
Accurate Determination ◽  
Fluorescence Analysis ◽  
Dilution Method ◽  
Practical Advantage ◽  
X Ray ◽  
The Matrix

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.

scholarly journals Determination of Optimum Conditions for X-Ray Fluorescence Analysis Using Coupling Equations

2012 ◽  
Vol 02 (02) ◽  
pp. 81-86
Author(s):  
Antonina Nikonovna Smagunova ◽  
Oyuntsetseg Bolormaa ◽  
Sergei Dimitrovich Pan’kov
Keyword(s):  
Fluorescence Analysis ◽  
Optimum Conditions ◽  
X Ray ◽  
Coupling Equations

Sorption of Se (IV) from aqueous solutions with subsequent determination by X-ray fluorescence analysis

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 ◽  
...  
Keyword(s):  
Inductively Coupled Plasma ◽  
Fluorescence Analysis ◽  
Standard Samples ◽  
Phase Contact Time ◽  
Sorbent Phase ◽  
X Ray ◽  
Fundamental Parameters ◽  
Inductively Coupled ◽  
Subsequent Determination

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.

Determination of the composition of binary chalcogenide glasses by X-ray fluorescence analysis

2010 ◽  
Vol 44 (1) ◽  
pp. 24-27 ◽  
Author(s):  
G. A. Bordovsky ◽  
A. V. Marchenko ◽  
P. P. Seregin ◽  
N. N. Smirnova ◽  
E. I. Terukov
Keyword(s):  
Chalcogenide Glasses ◽  
Fluorescence Analysis ◽  
X Ray

Measurement Of Relative X-Ray Intensity Ratios for Elements With Z=14 to 92 Using EDXRF Spectrometer

1993 ◽  
Vol 37 ◽  
pp. 697-709 ◽  
Author(s):  
Krassimir N. Stoev ◽  
Joseph F. Dlouhy
Keyword(s):  
Fluorescence Analysis ◽  
Radiative Transition ◽  
Published Data ◽  
Emission Rates ◽  
Experimental Physics ◽  
X Ray ◽  
Overlapped Peaks ◽  
Intensity Ratios ◽  
Atomic Structure Calculations

Nowadays x-ray fluorescence analysis is one of the major techniques for determination of trace elements. Vacuum operated Si (Li) .energy-dispersive x-ray spectrometers can analyze simultaneously up to 50 elements from Na (Z=11) to U (Z = 92) . Proper interpretation of the accumulated spectra requires correct solution of x-ray line overlap problems. In many cases knowledge of x-ray intensity ratios can make the procedure for resolving the overlapped peaks more reliable and reproducible. Measurements of radiative transition rates can also provide fundamental tests of theoretical atomic structure calculations. There are many other useful applications of x-ray emission rates in theoretical and experimental physics. On the other hand, there are differences in the published data, which suggests that x-ray intensity ratios are still not known with the necessary accuracy, and new measurements are useful and necessary.

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