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1.
Environ Pollut ; 289: 117831, 2021 Nov 15.
Artículo en Inglés | MEDLINE | ID: mdl-34358874

RESUMEN

Microbial-mediated Sb volatilization is a poorly understood part of the Sb biogeochemical cycle. This is mostly due to a lack of laboratory and field-deployable methods that are capable of quantifying low-level emissions of Sb from diffuse sources. In this study, we validated two methods using a H2O2 -HNO3 liquid chemotrap and an activated coconut shell charcoal solid-phase trap, achieving an absolute limit of detection of 4.6 ng and below 2.0 ng Sb, respectively. The activated charcoal solid-phase trapping method, the most easily operated method, was then applied to contaminated shooting range soils. Four treatments were tested: 1) flooded, 2) manure amended + flooded, 3) 70 % water holding capacity, and 4) manure amendment +70 % water holding capacity, since agricultural practices and flooding events may contribute to Sb volatilization. Volatile Sb was only produced from flooded microcosms and manure amendment greatly influenced the onset and amount of volatile Sb produced. The highest amount of volatile Sb produced, up to 62.1 ng kg-1 d-1, was from the flooded manure amended soil. This suggests that anaerobic microorganisms may potentially be drivers of Sb volatilization. Our results show that polluted shooting range soils are a source of volatile Sb under flooded conditions, which may lead to an increase in the mobility of Sb. Some of these volatile Sb species are toxic and genotoxic, highlighting the role of Sb volatilization on environmental health, especially for individuals living in contaminated areas exposed to wetlands or flooded conditions (e.g., rice paddy agriculture surrounding mining areas). This work paves way for research on Sb volatilization in the environment.


Asunto(s)
Antimonio , Contaminantes del Suelo , Antimonio/análisis , Humanos , Peróxido de Hidrógeno , Estiércol , Suelo , Contaminantes del Suelo/análisis
2.
Food Chem ; 294: 405-413, 2019 Oct 01.
Artículo en Inglés | MEDLINE | ID: mdl-31126481

RESUMEN

In the present paper, a new analytical preconcentration/speciation method for antimony species determination in bottled mineral water samples using the SiO2/Al2O3/SnO2 adsorbent was developed. The method is based on selective adsorption of Sb(III) ions by SiO2/Al2O3/SnO2 under a wide pH range (2.5-7.5). Total antimony was determined with previous sample treatment using 0.1% (w/v) l-cysteine and the concentration of Sb(V) species was determined by the difference between total and Sb(III). The proposed method provided an analytical curve ranging from 0.50 to 5.00 µg L-1 (r = 0.999), limit of detection (LD) of 0.17 µg L-1 and preconcentration factor (PF) of 136-fold. The method exhibited tolerance to different metal ions and the accuracy was attested from addition and recovery tests (95.2-106.0%) in bottled mineral water samples using 2.0% (w/v) l-cysteine, as well as by analysis of certified material. Only Sb(III) species were determined in mineral water (0.54-1.04 µg L-1).


Asunto(s)
Antimonio/análisis , Agua Potable/análisis , Aguas Minerales/análisis , Espectrofotometría Atómica/métodos , Óxido de Aluminio/química , Antimonio/química , Cisteína/química , Análisis de Inyección de Flujo , Límite de Detección , Oxidación-Reducción , Dióxido de Silicio/química , Compuestos de Estaño/química
3.
Angew Chem Int Ed Engl ; 56(2): 632-636, 2017 01 09.
Artículo en Inglés | MEDLINE | ID: mdl-27930850

RESUMEN

One-electron oxidation of the stibines Aryl3 Sb (1, Aryl=2,6-i Pr2 -4-OMe-C6 H2 ; 2, Aryl=2,4,6-i Pr3 -C6 H2 ) with AgSbF6 and NaBArylF4 (ArylF =3,5-(CF3 )2 C6 H3 ) afforded the first structurally characterized examples of antimony-centered radical cations 1.+ [BArylF4 ]- and 2.+ [BArylF4 ]- . Their molecular and electronic structures were investigated by single-crystal X-ray diffraction, electron paramagnetic resonance spectroscopy (EPR) and UV/Vis absorption spectroscopy, in conjunction with theoretical calculations. Moreover, their reactivity was investigated. The reaction of 2.+ [BArylF4 ]- and p-benzoquinone afforded a dinuclear antimony dication salt 32+ [BArylF4 ]2- , which was characterized by NMR spectroscopy and X-ray diffraction analysis. The formation of the dication 32+ further confirms that the isolated stibine radical cations are antimony-centered.

4.
ACS Appl Mater Interfaces ; 8(36): 23810-9, 2016 Sep 14.
Artículo en Inglés | MEDLINE | ID: mdl-27538719

RESUMEN

The nonconventional deuterated stibine (SbD3) compound has been used for the first time in combination with trigermane (Ge3H8) to produce hyper-doped Ge-on-Si films with carrier concentrations n > 10(20) cm(-3) and record-low resistivities ρ = 1.8 × 10(-4) Ω cm. The growth takes place on Ge and Ge1-xSix buffered Si(100) wafers at ultralow temperatures (∼330 °C) at which Sb diffusion is negligible, leading to extremely flat atomic profiles of the constituents. The Sb substitution in the Ge lattice is determined by RBS channeling and corroborated by high-resolution XRD, which also reveal a systematic increase in lattice constant vs concentration, as expected due to the incorporation of the larger Sb. High-resolution TEM illustrates defect-free monocrystalline structures with device-quality morphologies. The electrical characteristics of the samples are measured using Hall effect and resistivity measurements combined with contactless infrared ellipsometry and are found to be consistent with an extrapolation of the bulk Ge:Sb properties to the high carrier concentrations achieved in our films. The Sb/Ge ratio in the doped layers is approximately the same as that in the precursor reaction mixture, indicating a highly efficient Sb incorporation afforded by the compatible reactivity of the molecules employed in this study. The resultant films are attractive for next generation germanium technologies that require low-resistance n+ junctions or a Fermi level that approaches the direct gap minimum in the conduction band, which drastically enhances the optical emission efficiency of n-type Ge.

5.
Talanta ; 141: 259-66, 2015 Aug 15.
Artículo en Inglés | MEDLINE | ID: mdl-25966412

RESUMEN

The electrochemical generation of antimony volatile species (stibine) using Au and Ag mercury amalgamated cathodes is described. Compared with some other cathode materials commonly used for electrochemical hydride generation, performance of the amalgamated cathodes is substantially better in the following aspects: higher interference tolerance, higher erosion resistance and longer useful working time. Using the amalgamated cathodes, it could be shown that interferences from major constituents at high concentrations, especially from transition metals, affecting stibine generation are not as significant as they are using other cathode types in regards to sensitivity and useful working time. Results obtained using the Ag/Hg amalgamated cathode showed a slightly higher sensitivity than the corresponding results obtained using the Au/Hg cathode. The Au/Hg cathode, which to our knowledge has not previously been used to generate stibine, showed considerably longer useful working time than the Ag/Hg one. The optimum catholytes for electrolytic generation of stibine (SbH3) from Sb(III) and Sb(V) using the Au/Hg electrode were aqueous solutions containing 0.5mol L(-1) H2SO4 and 0.5mol L(-1)HCl, respectively. Under optimized conditions, using the Au/Hg cathode and comparing to aqueous standards calibration curves, detection limits (3σ) of 0.027µg L(-1) for Sb(III) and 0.056µg L(-1) for Sb(V), were obtained. To check accuracy a marine sediment reference material (PACS-2, NRC) was analyzed using a method purportedly developed for this task. Good agreement, 95% confidence, was found between the certified and the experimental values for Sb. The proposed method was also applied to the determination of Sb in aqueous solutions of marine sediments samples from Comuna de Bajo Alto Provincia de El Oro-Ecuador. Recoveries of five replicate determinations of these samples were in the range of 98-103% thus showing acceptable accuracy in the analysis of real samples.

6.
Acta Crystallogr Sect E Struct Rep Online ; 70(Pt 10): m351, 2014 Oct 01.
Artículo en Inglés | MEDLINE | ID: mdl-25484676

RESUMEN

In the title compound, [SbBr(C10H7)2], the Sb(III) atom has a distorted trigonal-pyramidal coordination geometry and the planes of the two naphthalene ring systems make a dihedral angle of 80.26 (18)°. An intra-molecular C-H⋯Br hydrogen bond forms an S(5) ring motif. In the crystal, weak C-H⋯Br inter-actions link the mol-ecules into helical chains along the b-axis direction.

7.
Mem. Inst. Oswaldo Cruz ; 103(2): 130-137, Mar. 2008. graf, tab
Artículo en Inglés | LILACS | ID: lil-480643

RESUMEN

The pentavalent antimonies, mainly the meglumine antimoniate, are recommends as first-choice medicines for leishmaniasis therapy. In this work we described the development of formulations of meglumine antimoniate injectable medication, as well as the analytical methodology used in the selective determination of Sb(III) and Sb(Total) by hydride generation - inductively coupled plasma atomic emission spectrometry (HG-ICP-AES) and ICP-AES, respectively. On that purpose the analytical methodology was developed focusing on the HG-ICP-AES technique. The formulations using propylene glycol/water as vehicles in a 20:80 proportion were more appropriate for subsequent use in industrial scale. These formulations also showed a lower variation on Sb(III) percentage, no need of buffer solution to stabilize the formulation and no influence of the autoclaving in the quality of the product. The results of the development of the analytical methodology point out the proposed method as an efficient alternative for the determination of Sb(III) in the presence of large quantities of Sb(V) in injectable solutions of meglumine antimoniate, in a selective, linear, accurate and precise manner. In addition, the method showed a low limit of quantification, less interference of the matrix, and more resilience than batch techniques proposed in the Brazilian Pharmacopeia.


Asunto(s)
Antimonio/análisis , Antiprotozoarios/química , Análisis de Inyección de Flujo/métodos , Meglumina/química , Compuestos Organometálicos/química , Espectrofotometría Atómica/métodos , Antiprotozoarios/normas , Química Farmacéutica/normas , Meglumina/normas , Compuestos Organometálicos/normas , Control de Calidad
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