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Abstract  

For the determination of arsenic compounds in terrestrial plant samples, a crucial step is the efficient extraction of arsenic from the solid plant matrix. However, the use of methanol-water extraction often resulted in low extraction efficiencies of less than 50%. In this study, eight solid-liquid extraction procedures (mainly based on mechanical mixing and sonication) were evaluated for the recovery of arsenic species from a submerged freshwater plant, coontail (Ceratophyllum demersum), collected in Moira River, Ontario, Canada. Speciation of As in the extracts was carried out with both anion-, and cation-exchange HPLC with sector-field inductively coupled plasma mass spectrometric (SF-ICP-MS) detection. The results obtained depended critically on the extraction solvents used in different extraction procedures. Extraction with methanol-water led only to 9%–44% recoveries of As. A high extraction yield (approximately 82%) was obtained by water extraction. Alkaline hydrolysis also resulted in high extraction efficiencies (86%–98%), but severe oxidation of As(III) to As(V) was observed. A protease enzymatic extraction led to a recovery of 48%. Approximately 0.5% of the total As in the plant sample was lipid-soluble. It was found that the extraction of inorganic arsenic species was suppressed by the presence of methanol in the extraction solvents, while high content of methanol in the extraction solvents was effective for the extraction of organic arsenic species. Therefore, it is recommended to perform the extraction both with water alone and with methanol-water (9+1, v/v), in order to obtain the complete As species profile in terrestrial plants.

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Journal of Thermal Analysis and Calorimetry
Authors: J. Yao, F. Wang, L. Tian, Y. Zhou, H. Chen, K. Chen, N. Gai, R. Zhuang, T. Maskow, B. Ceccanti, and G. Zaray

Abstract  

Using TAM III multi-channel calorimetry combined with direct microorganism counting (bacteria, actinomycetes and fungi) under laboratory conditions, we determined the microbial population count, resistance and activity toward cadmium (Cd(II)) and hexavalent chromium (Cr(VI)) toxicity in soil. The thermokinetic parameters, which can represent soil microbial activity, were calculated from power-time curves of soil microbial activity obtained by microcalorimetric measurement. Simultaneous application of the two methods showed that growth rate constant (k), peak-heat output power (P max) and the number of living microorganisms decreased with increasing concentration of Cd and Cr. The accumulation of Cr on E. coli was conducted by HPLC-ICP-MS. Cr6+ accumulation by Escherichia coli was increased steadily with increasing Cr6+ concentration. The results revealed that the change in some thermo-kinetic parameters could have good corresponding relationship with metal accumulation. Our work also suggests that microcalorimetry is a fast, simple, more sensitive, on-line and in vitro method that can be easily performed to study the toxicity of different species of heavy metals on microorganism compared to other biological methods, and can combine with other analytic methods to study the interaction mechanism between environmental toxicants and microbes.

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Summary  

We have used inductively coupled plasma mass spectrometry (ICP-MS) as the primary tool for determining concentrations of a suite of nuclides in samples excised from high-burnup spent nuclear fuel rods taken from light water nuclear reactors. The complete analysis included the determination of 95Mo, 99Tc, 101Ru, 103Rh, 109Ag, 137Cs, 143Nd, 145Nd,148Nd,147Sm, 149Sm, 150Sm, 151Sm, 152Sm, 151Eu, 153Eu, 155Eu, 155Gd, 237Np, 234U, 235U, 236U, 238U, 238Pu, 239Pu, 240Pu, 241Pu, 242Pu, 241Am, 242mAm, and 243Am. The isotopic composition of fissiogenic lanthanide elements was determined using high-performance liquid chromatography (HPLC) with ICP-MS detection. These analytical results allow the determination of fuel burn-up based on 148Nd, Pu, and U content, as well as provide input for storage and disposal criticality calculations. Results show that ICP-MS along with HPLC-ICP-MS are suitable of performing routine determinations of most of these nuclides, with an uncertainty of ±10% at the 95% confidence level.

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two-dimensional gel electrophoresis-LA-ICP-MS followed by capillary HPLC-ICP-MS and ES-LTQuadrupole Orbitrap MS . Anal. Chem. , 85 , 2037 – 2043 . B óna , L. , A dányi , N. , F arkas , R

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