Environmental monitoring of Central Kazakhstan territories where heavy space booster rockets land requires fast, efficient, and inexpensive analytical methods. The goal of this study was to develop a method for quantitation of the most stable transformation product of rocket fuel, i.e., highly toxic unsymmetrical dimethylhydrazine - 1-methyl-1H-1,2,4-triazole (MTA) in soils using solid-phase microextraction (SPME) in combination with gas chromatography-mass spectrometry. Quantitation of organic compounds in soil samples by SPME is complicated by a matrix effect. Thus, an isotope dilution method was chosen using deuterated analyte (1-(trideuteromethyl)-1H-1,2,4-triazole; MTA-d3) for matrix effect control. The work included study of the matrix effect, optimization of a sample equilibration stage (time and temperature) after spiking MTA-d3 and validation of the developed method. Soils of different type and water content showed an order of magnitude difference in SPME effectiveness of the analyte. Isotope dilution minimized matrix effects. However, proper equilibration of MTA-d3 in soil was required. Complete MTA-d3 equilibration at temperatures below 40°C was not observed. Increase of temperature to 60°C and 80°C enhanced equilibration reaching theoretical MTA/MTA-d3 response ratios after 13 and 3h, respectively. Recoveries of MTA depended on concentrations of spiked MTA-d3 during method validation. Lowest spiked MTA-d3 concentration (0.24 mg kg(-1)) provided best MTA recoveries (91-121%). Addition of excess water to soil sample prior to SPME increased equilibration rate, but it also decreased method sensitivity. Method detection limit depended on soil type, water content, and was always below 1 mg kg(-1). The newly developed method is fully automated, and requires much lower time, labor and financial resources compared to known methods.
<p>Electrode materials were prepared from activated carbonizates of walnut shell, apricot pits and shungite rock from “Bakyrchik” deposit, East Kazakhstan. Physicochemical characteristics of the obtained samples were studied by the Brunauer-Emett-Taylor method, scanning electron microscopy, Raman spectroscopy and other methods. Electrochemical properties of the obtained materials were studied by the method of cyclic voltammetry. It was found that the samples have an amorphous structure. Samples based on plant raw materials after hydrothermal carbonization at 240 °С during 24 h, have more homogeneous and developed surface. Specific surface area of carbon containing materials based on apricot pits is 1300 m<sup>2</sup>/g, for those on the based on mineral raw material, it is 153 m<sup>2</sup>/g. It was shown that materials after hydrothermal carbonization can be used for catalytic purposes and electrodes after thermal carbonization for analytical and electrocatalytic purposes. Electrode obtained by HTC have electrocatalytic activity. CSC 240 has high background current (slope i/Е is 43 mА V<sup>–1</sup> cm<sup>–2</sup>), low potential of the hydrogen electroreduction (more positive by ~ 0.5 V than samples based on plant raw materials). The reaction of DA determination is more pronounced on the electrodes obtained by HTC 240 °C, 24 h, due to the nature, carbon structure and high specific surface area of obtained samples.</p>
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