No abstract

Um procedimento simples e rápido de microextração líquido-líquido com líquido iônico e agitação vortex (VALLME) foi usado na determinação de quantidades traço de cádmio por espectrometria de absorção atômica com chama (FAAS). O líquido iônico (IL), hexafluorato de 1-hexil-3-metilimidazólio ([Hmim][PF 6 ]), foi usado como solvente extractor. Os íons Cd 2+ foram complexados com pirrolidina ditiocarbamato de amônia (APDC), e então confinados em pequenas gotas de IL pela intervenção do sistema de agitação vortex. Alguns fatores que influenciam na extração tais como pH, concentração de ligante, quantidade de líquido iônico, tempo de extração e efeito da força iônica foram completamente investigados e otimizados. Sob condições ideais, o limite de detecção foi de 1,1 ng mL -1 . O desvio padrão relativo (RSD) foi 4,3% para 20 ng mL -1 de cádmio (n = 10), e o gráfico de calibração usando o método de preconcentração foi linear de 5 a 150 µg L -1 , com um coeficiente de correlação de 0,998. O método proposto foi aplicado com sucesso na determinação de cádmio em amostras de água e folhas de espinafre.A simple and rapid vortex-assisted ionic liquid based liquid-liquid microextraction (VALLME) procedure was used for the determination of trace amounts of cadmium by flame atomic absorption spectrometry (FAAS). Ionic liquid (IL), 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF 6 ]), was used as an extractant solvent. Cd 2+ was complexed with ammonium pyrrolidinedithiocarbamate (APDC) and then entered into the fine IL droplets by the assistance of vortex agitator system. Some effective factors that influence the extraction efficiency such as pH, ligand concentration, amount of ionic liquid, extraction time and ionic strength effect were completely investigated and optimized. Under the optimum conditions, the limit of detection (LOD) was 1.1 ng mL -1 . The relative standard deviation (RSD) was 4.3% for 20 ng mL -1 of cadmium (n = 10), and the calibration graph using the preconcentration method was linear from 5 to 150 µg L -1 , with a correlation coefficient of 0.998. The proposed method was successfully applied for determination of cadmium in water samples and spinach leaves.

For [C(O)NH](N)2P(O)-based structures, the magnitude of the differences in the N—H...O, H...O=P and H...O=C angles has been evaluated when the N—H bond lengths, determined by X-ray diffraction, were compared to the neutron normalized values and the maximum percentage difference was obtained, i.e. about 3% for the angle even if the N—H bond lengths have a difference of about 30% (0.7 Å for the X-ray and 1.03 Å for the neutron-normalized value). The symmetries of the crystals are discussed with respect to the symmetry of the molecules, as well as to the symmetry of hydrogen-bonded motifs, and the role of the most directional hydrogen bond in raising the probability of obtaining centrosymmetric crystal structures is investigated. The work was performed by considering nine new X-ray crystal structures and 204 analogous structures retrieved from the Cambridge Structural Database.