Crystallography Reports - A coordination polymer [Hg(L)Cl2]n consisting of HgCl2 and Schiff base bidentate ligand (4-methoxyphenyl) pyridine-2yl methyleneamine (L) was prepared and structurally... 相似文献
The growth morphology of crystals of zinc tris(thiourea) sulphate (ZTS) is investigated experimentally, and computed using
the Hartman-Perdok approach. Attachment energies of the observed habit faces are calculated for determining their relative
morphological importance. A computer code is developed for carrying out these calculations. A special procedure is adopted
for computing the cohesive energy of a slice of the structure parallel to any rational crystallographic plane. For estimating
the cohesive energies, formal charges on the experimentally determined atomic positions in the molecules of ZTS are calculated
by ab initio molecular-orbital computations, with wave functions obtained by the Hartree-Fock procedure. Fairly good agreement with the
observed crystal morphology is obtained for a model of growth mechanism in which ZTS is assumed to exist in solution sa szinc
tris(thiourea) ions and sulphate ions. 相似文献
A new and efficient method was described for an easy synthesis of functionalized mesoporous silica (MCM-41) using thiophene-2-carbaldehyde. This new chemically bonded analytical reagent was used as an effective sorbent for the solid phase extraction of palladium(II) ion from aqueous solutions. Conditions for effective adsorption of trace levels of palladium concentration were optimized with respect to different experimental parameters in batch process. Thiourea solution could efficiently elute adsorbed palladium(II) ion from the surface of the sorbent which then was determined by inductively coupled plasma atomic emission spectrometer (ICP-AES).Common coexisting ions did not interfere with the separation and determination. The preconcentration factor was 100 (1 ml elution volume) for a 100 ml sample volume. The limit of detection of the proposed method is 0.2 ng ml−1. The maximum sorption capacity of sorbent under optimum conditions has been found to be 5 mg of palladium per gram of sorbent. The relative standard deviation under optimum conditions was 3.2% (n = 10). Accuracy and application of the method was estimated by using test samples of natural and synthetic water spiked with different amounts of palladium(II) ion. 相似文献
A sensitive high-performance liquid chromatographic technique is described for the separation of R- and S-acebutolol in human plasma and urine. The procedure involves derivatization with the chiral reagent S-(+)-1-(1-naphthyl)ethyl isocyanate. The resulting diastereoisomers are quantified using normal-phase high-performance liquid chromatography with fluorescence detection (220/389 nm). Virtual baseline separation, free from interference, with achieved (resolution factor = 1.45). Excellent linearity (r greater than 0.998) was observed throughout the range 10-500 ng/l and 2-100 mg/l in plasma and urine, respectively. Inter-assay variability was less than 5% for each enantiomer at concentrations of 10 ng/ml. This method is applicable for the determination of the pharmacokinetics, in man, of acebutolol enantiomers in plasma and urine. 相似文献
Reaction of the ligand 2, 2′‐diamino‐4, 4′‐bithiazole (DABTZ) with Zn(ClO4)2, CdCl2, and Hg(SCN)2 gives complexes with composition [Zn(DABTZ)2](ClO4)2, [Cd(DABTZ)2Cl2], and [Hg(DABTZ)(SCN)2]. The complexes were characterized by elemental analyses and infrared spectroscopy. The crystal structure of the [Hg(DABTZ)(SCN)2] was determined by X‐ray crystallography. The complex is built up of a monomeric Hg(SCN)2 unit with one 2, 2′‐diamino‐4, 4′‐bithiazole ligand coordinated to the Hg atom via the two N atoms giving rise to a five‐member chelate ring in a distorted tetrahedral environment. There is π‐π stacking interaction between the parallel aromatic rings belonging to adjacent chain as planar species in which the mean molecular planes are close to parallel and separated by a distance of ~ 3.5Å, close to that of the planes in graphite. The coordinated 2, 2′‐diamino‐4, 4′‐bithiazole molecule is involved in hydrogen bonding acting as hydrogen‐bond donors with N atoms from the SCN ligand as potential hydrogen‐bond acceptors. The hydrogen bonding yields infinite chains parallel to the crystallographic vectors a and b. Each molecule is bonded to three neighbours. Both amine H atoms are hydrogen bonded to N atoms. 相似文献
A simple and useful method employing cloud point extraction is proposed for the preconcentration and separation of silver
in water samples. The silver cation reacts with bis(2-mercaptoanil) acetylacetone (BMAA) at pH 6. The resulting compound is
subsequently entrapped in the Triton X-114 micelles. After optimization of the complexation and extraction conditions, a preconcentration
factor of 50 was obtained (volume of initial sample was 10 mL). As an analytical example, trace amounts of Ag were determined,
after preconcentration, in a complex aqueous matrix such as seawater using flame atomic absorption spectrometry. The calibration
curve was linear in the range 2–200 ng/mL and the limit of detection was 0.43 ng/mL. The relative standard deviation was lower
than 2.4%.
The text was submitted by the authors in English. 相似文献
In this study, a simple, rapid and efficient method, dispersive liquid-liquid microextraction (DLLME) combined gas chromatography-electron capture detection (GC-ECD), for the determination of chlorobenzenes (CBs) in water samples, has been described. This method involves the use of an appropriate mixture of extraction solvent (9.5 μl chlorobenzene) and disperser solvent (0.50 ml acetone) for the formation of cloudy solution in 5.00 ml aqueous sample containing analytes. After extraction, phase separation was performed by centrifugation and the enriched analytes in sedimented phase were determined by gas chromatography-electron capture detection (GC-ECD). Our simple conditions were conducted at room temperature with no stiring and no salt addition in order to minimize sample preparation steps. Parameters such as the kind and volume of extraction solvent, the kind and volume of disperser solvent, extraction time and salt effect, were studied and optimized. The method exhibited enrichment factors and recoveries ranging from 711 to 813 and 71.1 to 81.3%, respectively, within very short extraction time. The linearity of the method ranged from 0.05 to 100 μg l−1 for dichlorobenzene isomers (DCB), 0.002-20 μg l−1 for trichlorobenzene (TCB) and tetrachlorobenzene (TeCB) isomers and from 0.001 to 4 μg l−1 for pentachlorobenzene (PeCB) and hexachlorobenzene (HCB). The limit of detection was in the low μg l−1 level, ranging between 0.0005 and 0.05 μg l−1. The relative standard deviations (R.S.D.s) for the concentration of DCB isomers, 5.00 μg l−1, TCB and TeCB isomers, 0.500 μg l−1, PeCB and HCB 0.100 μg l−1 in water by using the internal standard were in the range of 0.52-2.8% (n = 5) and without the internal standard were in the range of 4.6-6.0% (n = 5). The relative recoveries of spiked CBs at different levels of chlorobenzene isomers in tap, well and river water samples were 109-121%, 105-113% and 87-120%, respectively. It is concluded that this method can be successfully applied for the determination of CBs in tap, river and well water samples. 相似文献
A rapid, sensitive, stereospecific reversed-phase high-performance liquid chromatographic method was developed for simultaneous quantitation of ketoprofen enantiomers, probenecid and their conjugates in biological fluids. Following addition of the internal standard, indoprofen, the constituents were extracted into isooctane-isopropanol (95:5), water-washed, extracted with chloroform, then evaporated and the residue sequentially derivatized with ethyl chloroformate and L-leucinamide hydrochloride. The formed diastereomers were chromatographed on a reversed-phase column with a mobile phase of 0.06 M KH2PO4-acetonitrile-triethylamine (65:35:0.1) at a flow-rate of 1 ml/min and a detection wavelength of 275 nm. The minimum quantifiable concentration was 0.5 micrograms/ml in 100 microliters of rat plasma and urine samples. The intra- and inter-day coefficients of variation for this method are less than 10%. The assay is successfully applied to a pharmacokinetic study. The simultaneous analysis of probenecid with several other non-steroidal anti-inflammatory drugs was also successful. 相似文献
In this paper, a novel pipette tip micro-solid phase extraction based on molecularly imprinted polymer as a selective sorbent was developed and applied for extraction, pre-concentration and high-performance liquid chromatographic determination of trace amounts of malachite green (MG), rhodamine B (RB), methyl orange (MO) and acid red 18 (AR) dyes in seawater samples. Different parameters affecting the extraction efficiency such as type and volume of eluent solvent, sample volume, number of cycles of extraction and desorption, amount of sorbent and pH of the sample solution were evaluated using one-variable-at-a-time and response surface methodology. In order to optimize dyes extraction, seven factors in three levels were used for Box–Behnken experimental design. Under optimum extraction condition, pH of sample solution was 3.1 for MG, 3.0 for RB, 7.1 for MO and 6.1 for AR; volume of eluent solvent (HCl, 0.5 mol L−1) was 200 µL; volume of the sample solution was 10 mL (for MG) and 4 mL (for RB, MO and AR); the concentration of triton X-114 was 0.085 (MG), 0.10 (RB), 0.08 (MO) and 0.075 (AR) % v/v; the number of extraction cycles was 10 (MG), 6 (RB), 5 (MO) and 7 (AR); the number of elution cycles was 10, 6, 5 and 9, respectively, for MG, RB, MO and AR; NaCl concentration was 0.4 mol L−1; and amount of MIP was 2.0 mg for all dyes. The linear range of calibration curves was 0.5–250.0 µg L−1 for malachite green and methyl orange and 0.5–150.0 µg L−1 for both rhodamine B and acid red 18. The detection limits calculated to be 0.083, 0.10, 0.12 and 0.17 µg L−1 for MG, RB, MO and AR, respectively. The developed protocol was successfully used for determination of dyes in seawater of Chabahar Bay. The mean recoveries were ranged between 76.1 and 97.3% by mean relative standard deviations of 1.2–7.1%.