Report on Standard Samples and Related Materials for Spectrochemical Analysis

Abstract. Previous research has supported the use of Amazon’s Mechanical Turk (MTurk) for online data collection in individual differences research. Although MTurk Masters have reached an elite status because of strong approval ratings on previous tasks (and therefore gain higher payment for their work) no research has empirically examined whether researchers actually obtain higher quality data when they require that their MTurk Workers have Master status. In two different online survey studies (one using a personality test and one using a cognitive abilities test), the psychometric reliability of MTurk data was compared between a sample that required a Master qualification type and a sample that placed no status-level qualification requirement. In both studies, the Master samples failed to outperform the standard samples.

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Silicate analysis of carbonated rocks using ICP-AES with calibration by the concentration ratio

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2020-86-5-16-21 ◽

2020 ◽

Vol 86 (5) ◽

pp. 16-21

Author(s):

T. A. Karimova ◽

G. L. Buchbinder ◽

S. V. Kachin

Keyword(s):

Inductively Coupled Plasma ◽

Concentration Ratio ◽

Total Error ◽

Atomic Emission ◽

Emission Spectrometry ◽

Calibration Error ◽

Plasma Atomic Emission Spectrometry ◽

Standard Samples ◽

Inductively Coupled ◽

Carbonate Materials

Calibration by the concentration ratio provides better metrological characteristics compared to other calibration modes when using the inductively coupled plasma atomic emission spectrometry (ICP-AES) for analysis of geological samples and technical materials on their base. The main reasons for the observed improvement are: i) elimination of the calibration error of measuring vessels and the error of weighing samples of the analyzed materials from the total error of the analysis; ii) high intensity of the lines of base element; and iii) higher accuracy of measuring the ratio of intensities compared to that of measuring the absolute intensities. Calcium oxide is better suited as a base when using calibration by the concentration ratio in analysis of carbonate rocks, technical materials, slags containing less than 20% SiO2 and more than 20% CaO. An equation is derived to calculate the content of components determined in carbonate materials when using calibration by the concentration ratio. A method of ICP-AES with calibration by the concentration ratio is developed for determination of CaO (in the range of contents 20 – 100%), SiO2 (2.0 – 35%), Al2O3 (0.1 – 30%), MgO (0.1 – 20%), Fe2O3 (0.5 – 40%), Na2O (0.1 – 15%), K2O (0.1 – 5%), P2O5 (0.001 – 2%), MnO (0.01 – 2%), TiO2 (0.01 – 2.0%) in various carbonate materials. Acid decomposition of the samples in closed vessels heated in a HotBlock 200 system is proposed. Correctness of the procedure is confirmed in analysis of standard samples of rocks. The developed procedure was used during the interlaboratory analysis of the standard sample of slag SH17 produced by ZAO ISO (Yekaterinburg, Russia).

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

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2018-84-11-9-14 ◽

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.%.

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

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2020-86-10-5-9 ◽

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.

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