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.

ANALYSIS OF COBALT AND NICKEL BASES CATHODES BY X-RAY FLUORESCENCE SPECTROSCOPY

2021 ◽  
pp. 103-111
Author(s):  
A.V. Alekseev ◽  
◽  
G.V. Orlov ◽  
P.S. Petrov ◽  
◽  
...  
Keyword(s):  
Fluorescence Spectroscopy ◽  
Emission Spectroscopy ◽  
High Resolution Mass Spectrometry ◽  
Analytical Signal ◽  
Atomic Emission ◽  
X Ray ◽  
Fundamental Parameters ◽  
The Matrix ◽  
Resolution Mass ◽  
Cobalt And Nickel

In this work, Al, Cr, Cu, Fe, Ni, Si and Y were determined in SDP-6 cathodes based on cobalt and SDP-1 and AZh8 nickel-based cathodes by x-ray fluorescence spectroscopy. 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. A standard-free analysis was carried out using the method of fundamental parameters. The correctness of the results obtained was confirmed by a comparative analysis by atomic emission spectroscopy and high-resolution mass spectrometry with a glow discharge.

Dc arc emission analysis of rare earth metals and their oxides with sorption preconcentration of impurities

2018 ◽  
Vol 84 (11) ◽  
pp. 9-14
Author(s):  
E. S. Koshel ◽  
V. B. Baranovskaya ◽  
M. S. Doronina
Keyword(s):  
Rare Earth ◽  
Rare Earth Metals ◽  
Analytical Signal ◽  
Graphite Powder ◽  
Atomic Emission ◽  
Standard Samples ◽  
Emission Analysis ◽  
Sorption Preconcentration ◽  
Sample Shape

The analytical capabilities of arc atomic emission determination of As, Bi, Sb, Cu, Te in rare earth metals (REM) and their oxides after preparatory group concentration using S,N-containing heterochain polymer sorbent are studied on a high-resolution spectrometer “Grand- Extra” (“WMC-Optoelectron-ics” company, Russia). Sorption kinetics and dependence of the degree of the impurity extraction on the solution acidity are analyzed to specify conditions of sorption concentration. To optimize the procedure of arc atomic emission determination of As, Bi, Sb, Cu, and Te various schemes of their sorption preconcentration and subsequent processing of the resulted concentrate with the addition of a collector at different stages of the sorption process have been considered. Graphite powder is used as a collector in analysis of rare earth oxides due to universality and relative simplicity of the emission spectrum. Conditions of analysis and parameters of the spectrometer that affect the analytical signal (mass and composition of the sample, shape and size of the electrodes, current intensity and generator operation mode, interelectrode spacing, wavelengths of the analytical lines) are chosen. The evaporation curves of the determinable impurities were studied and the exposure time of As, Bi, Sb, Cu, and Te in the resulted sorption concentrate was determined. Correctness of the obtained results was evaluated using standard samples of the composition and in comparisons between methods. The results of the study are used to develop a method of arc chemical-atomic emission analysis of yttrium, gadolinium, neodymium, europium, scandium and their oxides in a concentration range of n x (10-2 - 10-5) wt.%.

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.

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.

Fluorescence staining of salicylaldehyde azine, and applications in the determination of potassium tert-butoxide

RSC Advances ◽  
2016 ◽  
Vol 6 (36) ◽  
pp. 30636-30641 ◽  
Author(s):  
Jinlai Yang ◽  
Jian Rui ◽  
Xu Xu ◽  
Yiqin Yang ◽  
Jun Su ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Fluorescence Staining ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Resolution Mass

Salicylaldehyde azine (1), with an aggregation-induced emission (AIE) function, was synthesized from salicylaldehyde and characterized by nuclear magnetic resonance, high resolution mass spectrometry, and X-ray single crystal diffraction.

Lateral resolution of the electron microbeam analysis

1978 ◽  
Vol 36 (1) ◽  
pp. 542-543
Author(s):  
H.J. Dudek
Keyword(s):  
Quantitative Analysis ◽  
Depth Resolution ◽  
Lateral Resolution ◽  
Cylindrical Particle ◽  
Correction Procedure ◽  
X Ray ◽  
Element Concentrations ◽  
Microbeam Analysis ◽  
The Matrix

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S

Determination of quaternary ammonium compounds in food products by the method of ultra-performance liquid chromatography/high resolution mass-spectrometry

2020 ◽  
Vol 86 (8) ◽  
pp. 23-31
Author(s):  
V. G. Amelin ◽  
D. S. Bolshakov
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Quaternary Ammonium ◽  
High Resolution Mass Spectrometry ◽  
Food Products ◽  
Quaternary Ammonium Compounds ◽  
High Resolution Mass ◽  
Ammonium Compounds ◽  
Resolution Mass

The goal of the study is developing a methodology for determination of the residual amounts of quaternary ammonium compounds (QAC) in food products by UHPLC/high-resolution mass spectrometry after water-acetonitrile extraction of the determined components from the analyzed samples. The identification and determination of QAC was carried out on an «UltiMate 3000» ultra-high-performance liquid chromatograph (Thermo Scientific, USA) equipped with a «maXis 4G» high-resolution quadrupole-time-of-flight mass spectrometric detector and an ion spray «ionBooster» source (Bruker Daltonics, Germany). Samples of milk, cheese (upper cortical layer), dumplings, pork, chicken skin and ground beef were used as working samples. Optimal conditions are specified for chromatographic separation of the mixture of five QAC, two of them being a mixture of homologues with a linear structure (including isomeric forms). The identification of QAC is carried out by the retention time, exact mass of the ions, and coincidence of the mSigma isotopic distribution. The limits for QAC detection are 0.1 – 0.5 ng/ml, the determination limits are 1 ng/ml for aqueous standard solutions. The determinable content of QAC in food products ranges within 1 – 100 ng/g. The results of analysis revealed the residual amount of QAC present in all samples, which confirms data of numerous sources of information about active use of QAC-based disinfectants in the meat and dairy industry. The correctness of the obtained results is verified by introduction of the additives in food products at a level of 10 ng/g for each QAC. The relative standard deviation of the analysis results does not exceed 0.18. The duration of the analysis is 30 – 40 min.

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