Abstract:A novel approach to detecting gold in tin dioxide advanced nanomaterials via total reflection X ray fluorescence analysis (TRXF) is proposed. Data of gold and tin detection acquired via the nonstandard method for powders and with the use of an internal standard technique in aqueous suspensions are compared. Accuracy of the gold detection in powder nanomaterials via TRXF without sample decomposition is shown.
“…According to [180,181], gold clusters are distributed on the surface of SnO 2 ; therefore, the use of the TXRF method for sample suspensions significantly simplifies the analysis of the Au concentration in SnO 2 . In this case, it is possible to directly determine the total Au content at the level of 1-2 wt.% using gallium as an internal standard with s r = 0.12 [212]. Interestingly, the results of the analysis of suspensions by the TXRF method, in contrast to ICP MS, can be used to assess the uniformity of the additive distribution over the surface by evaluating the results of determination in individual aliquots taken from the volume of suspensions [213].…”
Section: Distribution Of Additives Between the Volume And The Surface...mentioning
Tin dioxide has huge potential and is widely studied and used in different fields, including as a sensitive material in semiconductor gas sensors. The specificity of the chemical activity of tin dioxide in its interaction with the gas phase is achieved via the immobilization of various modifiers on the SnO2 surface. The type of additive, its concentration, and the distribution between the surface and the volume of SnO2 crystallites have a significant effect on semiconductor gas sensor characteristics, namely sensitivity and selectivity. This review discusses the recent approaches to analyzing the composition of SnO2-based nanocomposites (the gross quantitative elemental composition, phase composition, surface composition, electronic state of additives, and mutual distribution of the components) and systematizes experimental data obtained using a set of analytical methods for studying the concentration of additives on the surface and in the volume of SnO2 nanocrystals. The benefits and drawbacks of new approaches to the high-accuracy analysis of SnO2-based nanocomposites by ICP MS and TXRF methods are discussed.
“…According to [180,181], gold clusters are distributed on the surface of SnO 2 ; therefore, the use of the TXRF method for sample suspensions significantly simplifies the analysis of the Au concentration in SnO 2 . In this case, it is possible to directly determine the total Au content at the level of 1-2 wt.% using gallium as an internal standard with s r = 0.12 [212]. Interestingly, the results of the analysis of suspensions by the TXRF method, in contrast to ICP MS, can be used to assess the uniformity of the additive distribution over the surface by evaluating the results of determination in individual aliquots taken from the volume of suspensions [213].…”
Section: Distribution Of Additives Between the Volume And The Surface...mentioning
Tin dioxide has huge potential and is widely studied and used in different fields, including as a sensitive material in semiconductor gas sensors. The specificity of the chemical activity of tin dioxide in its interaction with the gas phase is achieved via the immobilization of various modifiers on the SnO2 surface. The type of additive, its concentration, and the distribution between the surface and the volume of SnO2 crystallites have a significant effect on semiconductor gas sensor characteristics, namely sensitivity and selectivity. This review discusses the recent approaches to analyzing the composition of SnO2-based nanocomposites (the gross quantitative elemental composition, phase composition, surface composition, electronic state of additives, and mutual distribution of the components) and systematizes experimental data obtained using a set of analytical methods for studying the concentration of additives on the surface and in the volume of SnO2 nanocrystals. The benefits and drawbacks of new approaches to the high-accuracy analysis of SnO2-based nanocomposites by ICP MS and TXRF methods are discussed.
Inductively coupled plasma mass spectrometry (ICP-MS) is used for separate determination of platinum and palladium on the surface and in the bulk of tin dioxide based nanocomposites. Synthesis of SnO2 matrices was conducted using deposition from the solution and flame spray pyrolysis (FSP). The modifiers were injected by impregnation via the dispersion of the matrix powders in the solutions of precursors in volatile solvents and subsequent evaporation of the solvent. It is shown that palladium is present on the surface of the nanocomposites regardless of the synthesis procedure. As the losses of the modifier after impregnation of SnO2synthesized by FSP method were obserbed, we concluded that the properties of the SnO2surface depend on the method of obtaining matrix. It was also shown that for the materials obtained by the method of deposition from the solutions 30 - 50% Pt are present on the surface and other 50 - 70% are distributed in the bulk of SnO2. The use of pyrolysis in the flames makes it possible to increase the content of Pt on the surface up to 80%. The loss of Pt observed in both cases and attributed to the differences in the microstructure of SnO2results in the etherification of thin layers of phases of complex composition which affect the processes of superficial diffusion and evaporation. Reproducibility of the results of Pt and Pd determination indicates to a high degree of heterogeneity of the studied materials.
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