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.

Sorption of As (III) and Se (IV) from aqueous solutions for subsequent determination by total reflection X-ray fluorescence

2021 ◽  
Vol 87 (8) ◽  
pp. 19-22
Author(s):  
D. G. Filatova ◽  
A. A. Arkhipenko ◽  
M. A. Statkus ◽  
I. V. Mikheev ◽  
V. B. Baranovskaya ◽  
...  
Keyword(s):  
Raw Materials ◽  
Total Reflection ◽  
Phase Contact Time ◽  
Sorbent Phase ◽  
X Ray ◽  
Icp Ms ◽  
Subsequent Determination ◽  
Processed Products ◽  
Branched Structure

An approach to the simultaneous isolation of As (III) and Se (IV) from solutions on a new S,N-containing sorbent followed by determination of the analyte in the sorbent phase using total reflection X-ray fluorescence (TXRF) has been proposed. To match the goal, a sorbent with a branched structure was synthesized on the base of polyacrylamide modified with formaldehyde and hydrogen sulfide. This is a heteroatomic copolymer containing sulfide bridges in the chain and crosslinking by a tertiary amine. Conditions for the quantitative co-extraction of As (III) and Se (IV), i.e., sorption in solutions of 1 M HNO3 with calcium ions present, heating to 60°C and phase contact time of 1 h were determined. The mechanism of sorption interaction of the analytes under specified conditions is discussed. It is shown that a 100-fold excess of iron, zinc and copper does not interfere with the extraction of analytes, thus providing the possibility of As (III) and Se (IV) isolation from different types of raw materials and processed products using the synthesized sorbent. A method for the direct XRF quantification of arsenic and selenium with sr 0.09 and 0.08, respectively, in the sorbent phase has been developed. The correctness of the results was confirmed by the ICP-MS method in analysis of aqueous reference solution after dissolution of the sorbate in HNO3 (1:1).

scholarly journals Methodical features of multielement analysis of rocks by inductively coupled plasma mass spectrometry

2016 ◽  
pp. 56-63
Author(s):  
Ya. V. Bychkova ◽  
M. Yu. Sinitsyn ◽  
D. B. Petrenko ◽  
I. Yu. Nikolaeva ◽  
I. A. Bugaev ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Inductively Coupled Plasma ◽  
High Resolution Mass Spectrometry ◽  
Sample Collection ◽  
Standard Samples ◽  
Medical Products ◽  
Inductively Coupled ◽  
Subsequent Determination ◽  
Plasma Mass Spectrometry

A methodic of destruction of objects with hardly dissolvable matrix (earth materials, tableted medical products) for subsequent determination of microelements by high-resolution mass- spectrometry with inductively coupled plasma is developed. Analytical and methodical problems, appearing during of a sample collection and preparation at investigated objects, are described, the ways of their overcoming are proposed. The opportunity of carrying out of quantitative analysis of investigated objects after dissolution by means of using multielemental standard solutions is shown. Accuracy of a developed methodic of sample preparation was checked by analysis of standard samples of earth materials.

ANALYSIS OF SOLDERS ON TIN AND LEAD BASES BY X-RAY FLOORESCENT SPECTROSCOPY

2021 ◽  
pp. 124-131
Author(s):  
A.V. Alekseev ◽  
◽  
G.V. Orlov ◽  
P.S. Petrov ◽  
A.V. Slavin ◽  
...  
Keyword(s):  
Emission Spectroscopy ◽  
High Resolution Mass Spectrometry ◽  
Analytical Signal ◽  
Atomic Emission ◽  
Standard Samples ◽  
X Ray ◽  
Fundamental Parameters ◽  
The Matrix ◽  
Resolution Mass

The determination of the elements Cu, Ni, Sb, Bi, Pb, Zn and Fe in the tin-based solder VPr35, as well as the elements Sn, Ni, Sb, Bi and In in the lead-based VPr40 solder by the method of х-ray fluorescence spectroscopy has been carried out. The calibration dependences are corrected taking into account the superposition of signals from interfering elements on the analytical signal and changes in intensity caused by inter-element influences in the matrix. The analysis was carried out by the method of fundamental parameters without using standard samples. The correctness of the results obtained was confirmed by their comparative analysis by atomic emission spectroscopy and high-resolution mass spectrometry with a glow discharge.

NCSXRF: A General Geometry Monte Carlo Simulation Code for EDXRF Analysis

1991 ◽  
Vol 35 (B) ◽  
pp. 727-736 ◽  
Author(s):  
T. He ◽  
R. P. Gardner ◽  
K. Verghese
Keyword(s):  
Least Square ◽  
Influence Coefficient ◽  
Standard Samples ◽  
Simulation Code ◽  
X Ray ◽  
Fundamental Parameters ◽  
Edxrf Analysis ◽  
Influence Coefficient Method ◽  
Energy Pulse

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.

X-Ray Fluorescence Analysis of Oxide Magnetic Tape Using Thin Layer Fundamental Parameter Analysis

1991 ◽  
Vol 35 (B) ◽  
pp. 1133-1138
Author(s):  
Ko Kimura ◽  
Hideaki Wakamatsu ◽  
Takeshi Kitamura ◽  
Ryozo Maeda ◽  
Kunthiro Fujiwara
Keyword(s):  
Thin Layer ◽  
Magnetic Tape ◽  
Inductively Coupled Plasma ◽  
Rapid Determination ◽  
Fluorescence Analysis ◽  
Parameter Analysis ◽  
Elemental Content ◽  
Fundamental Parameter ◽  
Standard Samples ◽  
X Ray

In recent years, for the development of magnetic tape, it has become increasingly important that the elemental content be determined accurately and rapidly. In the past, the elemental content of magnetic tape was determined by calibration analysis using a wavelength dispersive X-ray fluorescence spectrometer(WDXRF). For calibration analysis many standard samples and large amount of sample were needed. Preparation of sample for calibration analysis, as well as for inductively coupled plasma emission spectral analysis(ICP) was difficult. On the other hand, for thin layer fundamental parameter analysis(we call TLFP) using a WDXRF, a few standard samples and l.pss sample are needed and preparation of the sample is easy. The superiority of TLFP analysis can be seen In comparison with calibration analysis and IOP analysis in Table 1. For this reason, this study has established a method for accurate and rapid determination of the elemental composition of oxide magnetic tape by TLFP analysis using a WDXRF.

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