V. B. Baranovskaya

Determination of selenium and cadmium dopants in nanocomposites based on zinc and indium oxides by high resolution continuous source electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

An approach is proposed to the determination of selenium and cadmium dopants in new nanocomposites based on zinc and indium oxides. The approach is based on a combination of highly efficient high resolution continuous source electrothermal atomic absorption spectrometry (ETAAS) for the analysis of suspensions and inductively coupled plasma mass spectrometry for the analysis of solutions. A procedure is developed for the determination of Se and Cd dopants and matrix components based on Zn and In in nanocomposite solutions by inductively coupled plasma mass spectrometry. Stabilizing agents for the preparation of suspensions are studied for the ETAAS analysis of powders without their decomposition. The results of determination of CdSe dopants by high resolution ETAAS are validated by inductively coupled plasma mass spectrometry.

Analysis of incinerator waste emissions containing toxic elements by sorption–continuum source electrothermal atomic absorption spectrometry

Possibilities of the determination of toxic elements, As, Cd, Co, Cr, Cu, Ni, Pb, Se, Sn, and Te, in emissions from a waste incineration plant are studied by high-resolution electrothermal atomic absorption spectrometry of with a continuum spectral source. A procedure is developed for the preparation of samples of solid domestic waste by the sorption of toxic elements on an S,N-containing sorbent. The analytical conditions of work on an atomic absorption spectrometer with a continuum spectral source are chosen. An improvement of performance characteristics in comparison to the known procedures is shown. A procedure of the determination of the chosen toxic elements in emissions from an incineration plant by electrothermal atomic absorption spectrometry with improved performance characteristics is developed and passed through metrological certification.

Determination of arsenic, cadmium, selenium, and tellurium in technogenic raw materials after sorption concentration on hydroxides using inductively coupled plasma atomic emission spectrometry

A method of group extraction of As, Se, Te, and Cd using hydroxides of iron, lanthanum, and magnesium in analysis of technogenic raw materials which makes it possible to simplify determination of the listed elements and to consider and reduce possible interferences is proposed. On the basis of the performed studies, an ICP-AES express method of determination of toxic elements in technogenic copper-containing raw material is developed. The relative standard deviation of the results of analysis performed using the developed method is 9–2.5% at concentrations of the determined elements from n × 10−4 to n × 10−1 wt %.

Analysis of high-purity materials by inductively coupled plasma mass spectrometry (Review)

A review of the works dedicated to the application of the method of inductively coupled plasma mass spectrometry (ICP-MS) to the analysis of high-purity materials (semiconductors, metals, and their oxides) and published after 2004 is presented. The limitations of this method in the analysis of such objects are discussed. Advantages and disadvantages are demonstrated for three principal ways of the application of the ICP-MS method to the analysis of high-purity materials: direct analysis of a solid sample (laser ablation and injection of a sample in the form of a suspension); preliminary dissolution of an analyte sample; utilization of the approach separating analytes and matrix.

Determination of admixtures of high-melting metals in rare-earth metals and their compounds

The study considers the possibility of using inductively coupled plasma mass spectrometry (ICP MS) for the determination of admixtures of Zr, Nb, Mo, Hf, Ta, W, and Te in rare-earth metals and their compounds using preliminary extraction or extraction-chromatographic preconcentration. The admixture elements have been separated by extraction with trioctylphosphine oxide in dichloroethane from hydrochloric acid media and back extraction with oxalic acid. Chemical separation provided a 1–4-order reduction of the lower quantification limit for these elements using ICP MS.

Combined Methods of Analysis of Metal-Containing Raw Material (Review)

Methods of analysis of reusable metal-containing material (RMR) are considered in the review: X-ray fluorescence, atomic absorption spectrophotometry, and atomic emission and mass spectrometry with inductively coupled plasma. Peculiarities of the applied methods are shown, and a method of analysis with consideration of the specificity of RMR should be developed for every object. In the most cases, the methods of sample processing harmonized with the applied method of analysis and sample content.

Sorption atomic emission determination of As, Bi, Sb, Se, and Te in recyclable metal-containing raw material

The possibility of group concentration of As, Bi, Sb, Se, and Te using sulfur- and nitrogen-containing sorbents with the subsequent determination by ICP-AES and DCA-AES with MAES in analysis of metal-containing recyclable raw material is studied. Conditions of ICP-AES and DCA-AES with MAES analysis of sorption concentrate from solutions or from solid phase are selected. The developed method makes it possible to determine the listed toxic elements in the range of mass fraction of n × 105−n × 103% (RSD = 15-7 rel %). Accuracy of the results was controlled by varying weighed samples of analytes and by comparison of the results with the known values.

Analysis of pure nonferrous and rare metals by atomic emission spectroscopy with photodiode detection

Analytic possibilities of direct determination of impurities in pure nonferrous and rare metals (Ga, In, Cd, Al, Cu, Ni, and Sn) by the arc atomic emission method with application of multichannel atomic emission spectroscopy are studied. The conditions for the performance of the analysis are established. The limits of detection and determination of impurities in studied materials are estimated. The possibility to determine elements at a level of 10−4–10−5 wt % is demonstrated. The accuracy is checked by comparing the obtained results with values of the determined impurities proved by use of state standard reference samples or departmental standard specimens. Improved techniques of arc atomic emission analysis of high purity nonferrous and rare metals are developed. The techniques possess amended metrological characteristics and permit one to considerably reduce the time of carrying out the analysis.

Detection of Sodium in Highly Pure Graphite via High-Resolution Electrothermal Atomic Absorption Spectrometry with a Continuous Spectrum Source

This study is dedicated to elucidating the analytical abilities of electrothermal atomic absorption spectrometry with a continuous spectrum source (ETAAS-CSS) to detect the presence of sodium in highly pure graphite powder. In order to plot the calibration dependence for sodium detection, a special technique based on argon dilution of the atomic vapor obtained by introducing the aqueous reference solution in the atomizer is applied. The conditions for thermal pretreatment of highly pure graphite powder and atomization of sodium are established, and the sodium detection threshold is evaluated via ETAAS-CSS (2.6 × 10–4 ng) as well. The validity of the results is confirmed via the sample variation method.

Advanced Techniques for Sample Processing of the Reusable Metal-Containing Raw Material (Review)

A review of the sample processing of different types of reusable metal-containing material (catalytic agents, e-wastes, cuttings, etc.) is given in the article; the purpose of the sample processing is the further analysis in the form of solutions: dilution in the mineral acid mix, alloying with different fluxes, leaching, etc. Increase in the temperature and pressure, ultrasonic impact, and microwave radiation are applied for the purpose of sample processing intensification. Methods of sample processing with application of sorbate concentration for the further definition of not only the noble, nonferrous, and rare metals but also the toxic elements are described. The review shows that the stage of sample processing is very important for achieving the potential of the applied analytical methods.