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91.
92.
研究了多接收器电感耦合等离子体质谱仪(MC-ICP MS)测定铅同位素比值时,影响测试结果准确度和精密度的主要因素及其优化过程。在优化条件下,10 h内连续30次测定4 ng/mL NIST SRM 981同位素标准溶液铅同位素比值,获得208Pb/206Pb、207Pb/206Pb和206Pb/204Pb相对标准偏差(RSDs)分别为0.005%、0.004%和0.054%。长期监测208Pb/206Pb、207Pb/206Pb和206Pb/204Pb,标准偏差(2SDs)分别为0.000 06、0.000 05和0.006 7。采用NEPTUNE MC-ICP MS法测定了低铅海洋碳酸盐样品中稳定铅的同位素比值,并对南海橙黄滨珊瑚(Porites lutea)和库氏砗磲(Tridacna gigas)进行了分析,得到全流程空白为8~10 pg,重复样误差优于0.1%。经0.50 mol/L HNO3洗脱之后,得到海南珊瑚样品中208Pb/206Pb、207Pb/206Pb的比值分别为2.086 2±0.001 5、0.849 90±0.001 47(n=16);海南砗磲样品中208Pb/206Pb、207Pb/206Pb的比值分别为2.116 9±0.004 2、0.864 81±0.001 62(n=9)。进一步考察了南海海洋碳酸盐中204Pb的同位素比值。分析结果表明,南海海洋碳酸盐中稳定铅同位素比值与中国气溶胶、珠江三角洲大气沉降、黄土及南海海底玄武岩等具有很好的相关性。方法适用于复杂基体高钙低铅的海洋碳酸盐样品中铅同位素比值的分析。 相似文献
93.
In the later stages of drug design projects, accurately predicting relative binding affinities of chemically similar compounds to a biomolecular target is of utmost importance for making decisions based on the ranking of such compounds. So far, the extensive application of binding free energy approaches has been hampered by the complex and time‐consuming setup of such calculations. We introduce the free energy workflow (FEW) tool that facilitates setup and execution of binding free energy calculations with the AMBER suite for multiple ligands. FEW allows performing free energy calculations according to the implicit solvent molecular mechanics (MM‐PB(GB)SA), the linear interaction energy, and the thermodynamic integration approaches. We describe the tool's architecture and functionality and demonstrate in a show case study on Factor Xa inhibitors that the time needed for the preparation and analysis of free energy calculations is considerably reduced with FEW compared to a fully manual procedure. © 2013 Wiley Periodicals, Inc. 相似文献
94.
Syntheses,Structures, Luminescent Properties and Photocatalytic Activities of Two Lead(II) Compounds
CONG Yao MA Cai-Lian CHE Guang-Bo BAI Hong-Ye SUN He-Yi REN Ao LIU Chun-Bo 《结构化学》2013,(11):1673-1679
Two lead(ll) compounds, [Pb(qlc)(phen)2(NO3)]e-H20 (1) and [Pb(qlc)z(phen)]-3H20 (2) (Hqlc = quinoline-3-carboxylic acid, phen = 1,10-phenanthroline), were synthesized and charac- terized by elemental analysis, single-crystal X-ray diffraction, IR and thermogravimetric analysis. Crystal 1 is of monoclinic, space group C2/c with a = 25.246(5), b = 12.543(3), c = 18.917(4) A, β = 105.77(3)°, V= 5765(2) A3, Z = 4, C68H46N12OllPb2, Mr = 1621.53, Dc = 1.886 g.cm-3,/.t(MoKa) = 5.912 mm-1, F(000) = 3152, GOOF = 1.080, the final R = 0.022 and wR = 0.0571 for 4822 observed reflections (1 〉 2a(/)). Crystal 2 is oftriclinic, space group Pi with a = 8.7883(10), b = 11.7031 (13), c = 15.9320(17) A, a = 69.9400(10), fl = 78.9780(10), 7 = 79.1650(10)°, V = 1497.4(3) A3, Z = 2, C32H26NaO7Pb, Mr. = 785.71, Dc = 1.729 g.cm-s, p(MoKa) = 5.688 mm-1, F(000) = 756, GOOF = 1.106, the final R = 0.0313 and wR = 0.088 for 59i5 observed reflections (1 〉 2σ(I)). Single-crystal X-ray diffraction analysis reveals that 1 exhibits a two-dimensional (2D) layer based on π-π stacking interactions between phen. Simultaneously, the adjacent 2D layers are assembled via π-π stacking interactions between phen and quinoline tings into a 3D supramolecular structure. The zero- dimensional structure of 2 is also further extended by π-π interactions to form a 2D supramolecular layer. Furthermore, these two compounds exhibit photoluminescence at room temperature in the solid state and their photocatalytic activities have been studied by degradation methylene blue. 相似文献
95.
G. Rauret R. Rubio M. Llaurado 《International journal of environmental analytical chemistry》2013,93(1-2):59-68
Abstract The destruction of the filter for metal determination in atmospheric aerosols is an important step in the analysis. Nowadays the decomposition of this kind of sample has not been completely solved, so it is interesting to study new methods for filter sample attack. In the present work the application of the combustion method in a closed flask for mixed cellulose esters filter decomposition for lead determination is proposed. For this purpose optimum operating conditions as stopper flask design, sample size, flask volume, shaking time and volume and concentration of absorbing solution are established, and accuracy and precision of the proposed method using AAS for the measurements is given. The results obtained by the closed flask combustion are compared with those found by wet attack with HNO3. The method proposed is rapid, has low reagent contamination and no loss of lead by volatilization or by amalgamation occurs. This method shows an accuracy and a precision in good agreement with the standard method. 相似文献
96.
The solution-phase photodecomposition of l, l-dichloro-2,2-bis(5′-chloro-2′-methoxy-phenyl)ethylene (MPE) has been studied at an excitation wavelength of 313 nm in the presence of O2 as well as in vacuum-degassed solutions. Only two non-volatile compounds are produced: 2,5-dichloro-3-(5′-chloro-2′-methoxyphenyl)benzofuran (BFD) and a minor product which was not identified. The BFD represents approximately 90% of the total non-volatiles. The volatile products were identified as CH3Cl, CH4 and HC1, with CH3C1 being approximately 99.9 % of the total volatiles. Photolyses were carried out in C6H12 and CCI4 solvents, the same products being observed in both solvents. Variation of MPE concentration has little or no effect on the relative quantum yield of decomposition. The photodecomposition of MPE does not follow the same pathway as the photodecomposition of DDE. 相似文献
97.
Walter N. L. dos Santos Dannuza D. Cavalcante Hadla S. Ferreira Cesário F. das Virgens Aline R. Borges Marcia M. Silva 《International journal of environmental analytical chemistry》2013,93(15):1447-1452
A cloud point extraction procedure for pre-concentration and determination of cadmium and lead in drinking water using sequential multi-element flame atomic absorption spectrometry is described. 4-(2-thiazolylazo)-orcinol (TAO) has been used as complexing agent and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The conditions for reaction and extraction (surfactant concentration, reagent concentration, effect of incubation time, etc) were studied and the analytical characteristics of the method were determined. The method allows the determination of cadmium and lead with quantification limits of 0.30?µg?L?1 and 2.6?µg?L?1, respectively. A precision expressed as relative standard deviation (RSD, n?=?10) of 2.3% and 2.6% has been obtained for cadmium concentrations of 10?µg?L?1 and 30?µg?L?1, respectively, and RSD of 1.3% and 1.7% for lead concentrations of 10?µg?L?1 and 30?µg?L?1, respectively. The accuracy was confirmed by analysis of a natural water certified reference material. The method has been applied for the determination of cadmium and lead in drinking water samples collected in the cities of Ilhéus and Itabuna, Brazil. Recovery tests have also been performed for some samples, and results varied from 96 to 105% for cadmium and 97 to 106% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by World Health Organization and the Brazilian Government. 相似文献
98.
Guillermo J. Copello Rocío Martínez Vivot Florencia Varela 《International journal of environmental analytical chemistry》2013,93(9):828-843
In this work, an all the way green analytical procedure based on a silicon oxide film-solid phase extraction system is proposed for lead traces determination. From the synthesis of a solid phase extraction (SPE) system and throughout the metal preconcentration and determination only aqueous media were employed. Characterisation of the film was carried out by Scanning Electron Microscopy and Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy. Preconcentration conditions, prior to Pb(II) Electrothermal Atomic Absorption Spectrometry (ETAAS) determination, such as adsorption and desorption time, pH and temperature, were optimised. Langmuir, Freundlich and Dubinin-Radushkevich isotherm models were analysed along with the evaluation of adsorption energy and standard free energy (ΔG 0). The greatest adsorption was obtained with incubation at pH 7 and 37°C. By using a small volume of 0.5?mol?L?1 HNO3 (0.5?mL) lead was desorbed from the silicon oxide film after 2?h incubation, generating low amount of waste. The films showed better adjustment for the Langmuir model (R2 ?=?0.989). The detection limit (3.29σ) for Pb(II) was 0.228?µg?L?1. The developed procedure is 10-fold more sensitive in comparison to direct ETAAS determination. Recovery values from soft tap-water and soft well-water were above 95%. When hard water was analysed, Pb(II) adsorption was found to be interfered by Mg2+ and Ca2+. After five preconcentration cycles relative recovery was found not to decay below 90%, indicating that the silicon oxide film could be used for multiple lead determinations. 相似文献
99.
Mohammad Mazloum-Ardakani Javad Safari Parvin Pourhakkak Mohammad Ali Sheikh-Mohseni 《International journal of environmental analytical chemistry》2013,93(14):1638-1649
A PVC (poly vinyl chloride) membrane electrode for lead ion based on 2-(((E)-2-((E)-1-(2-hydroxyphenyl)methyliden)hydrazono)metyl)phenol (HMHMP) as a membrane carrier was prepared. This electrode exhibited linear response with Nernstian slope of 29.2?±?0.2?mV per decade within the concentration range of 2.0?×?10?7–1.0?×?10?1?M lead ion. The limit of detection, as determined from the intersection of the extrapolated linear segments of the calibration plot, was 8.0?×?10?8 M. The electrode exhibited high selectivity for Pb (II). The response time of the electrode was about 5–10?s for different concentrations. The electrode is suitable for use in aqueous solutions in a pH range of 5.0–7.5. It was used as an indicator electrode in a titration of Pb (II) with chromate at constant pH. This electrode was used for the determination of lead in ore samples, and the results were in agreement with those obtained with an atomic absorption spectroscopy (AAS) method. Also lead selective electrode was used for monitoring of lead in spiked samples of the Zayanderud River and waste water by the potentiometry technique. 相似文献
100.
Dr. Goutam Kumar Kole Dr. Abdul Malik Puthan Peedikakkal Belinda Mei Fang Toh Prof. Dr. Jagadese J. Vittal 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(12):3962-3968
An attempt has been made to design double‐stranded ladder‐like coordination polymers (CPs) of hemidirected PbII. Four CPs, [Pb(μ‐bpe)(O2C‐C6H5)2] ? 2H2O ( 1 ), [Pb2(μ‐bpe)2(μ‐O2C‐C6H5)2(O2C‐C6H5)2] ( 2 ), [Pb2(μ‐bpe)2(μ‐O2C‐p‐Tol)2(O2C‐p‐Tol)2] ? 1.5 H2O ( 3 ) and [Pb2(μ‐bpe)2(μ‐O2C‐m‐Tol)2(O2C‐m‐Tol)2] ( 4 ) (bpe=1,2‐bis(4′‐pyridyl)ethylene), have been synthesised and investigated for their solid‐state photoreactivity. CPs 2 – 4 , having a parallel orientation of bpe molecules in their ladder structures and being bridged by carboxylates, were found to be photoreactive, whereas CP 1 is a linear one‐dimensional (1D) CP with guest water molecules aggregating to form a hydrogen‐bonded 1D structure. The linear strands of 1 were found to pair up upon eliminating lattice water molecules by heating, which led to the solid‐state structural transformation of photostable linear 1D CP 1 into photoreactive ladder CP 2 . In the construction of the double‐stranded ladder‐like structures, the parallel alignment of C?C bonds in 2 – 4 is dictated by the chelating and μ2‐η2:η1 bridging modes of the benzoate and toluate ligands. The role of solvents in the formation of such double‐stranded ladder‐like structures has also been investigated. A single‐crystal‐to‐single‐crystal transformation occurred when 4 was irradiated under UV light to form [Pb2(rctt‐tpcb)(μ‐O2C‐m‐Tol)2(O2C‐m‐Tol)2] ( 5 ). 相似文献