Simultaneous Preconcentration and Separation of Chromium(III) and Chromium(VI) at the Low-Temperature Directed Crystallization of Natural Water

It was shown that low-temperature directed crystallization of natural water can be used for separating chromium(III) and chromium(VI). At a moderate crystallization rate (6–10 mm/h), the final part of the ingot (concentrate) is a suspension containing chromium(III) and chromium(VI) in the solid and liquid phases, respectively. It is proposed to separately determine these chromium species by atomic absorption spectrometry after separating the phases by centrifugation and dissolving the precipitate in acids.     

Analytical Chemistry at the Institute of Single Crystals of the National Academy of Sciences of Ukraine

The paper describes the history and main lines of inquiry of the Analytical Laboratory at the Institute of Single Crystals (Kharkov, Ukraine) organized in 1955.     

Canonical representations of the Lie superalgebraosp(1,4)

The method for constructing infinite-dimensional representations of Lie superalgebras proposed by the authors recently is applied to the superalgebraosp (1, 4). Explicit formulae for its generators in terms of two or three pairs of operators fulfilling the canonical commutation relations, at most one pair of operators fulfilling the canonical anticommutation relations and at most one real parameter are obtained. The generators of the Lie subalgebrasp (4, ) osp (1,4) are represented skew-symmetrically and both the Casimir operators are equal to multiples of the unity operator.Dedicated to Professor Ivan Úlehla on the occasion of his sixtieth birthday.     

Pulsed Electron-Nuclear Double Resonance in the Fourier Regime

Nuclear magnetic resonance (NMR) spectroscopy provides atomic-level molecular structural information. However, in molecules containing unpaired electron spins, NMR signals are difficult to measure directly. In such cases, data is obtained using the electron-nuclear double resonance (ENDOR) method, where nuclei are detected through their interaction with nearby unpaired electron spins. Unfortunately, electron spins spread the ENDOR signals, which challenges current acquisition techniques, often resulting in low spectral resolution that provides limited structural details. Here, we show that by using miniature microwave resonators to detect a small number of electron spins, integrated with miniature NMR coils, one can excite and detect a wide bandwidth of ENDOR data in a single pulse. This facilitates the measurement of ENDOR spectra with narrow lines spread over a large frequency range at much better spectral resolution than conventional approaches, which helps reveal details of the paramagnetic molecules’ chemical structure that were not accessible before.     

Liquid chromatographic methods for biotransformation studies of ochratoxin A

Liquid chromatographic methods were used for the detection of ochratoxin A (OTA) and its metabolites ochratoxin alpha (OTalpha), 10-hydroxy OTA (10-OHOTA), 4R-hydroxy OTA (4R-OHOTA) and the ethyl ester of OTA (OTC) in in vitro samples, obtained with Caco-2 cell culture experiments and in in vivo urine samples from sheep. A high-performance liquid chromatography method with fluorescence detection (HPLC-FLD) and a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method were developed and validated for the detection of OTA and its metabolites OTalpha, 10-OHOTA, 4R-OHOTA and OTC, which was used as internal standard. The LOD/LOQ values for OTalpha, 4R-OHOTA and OTA were 0.63/2.11, 0.99/3.31 and 0.84/2.81 microg/L, respectively, for the HPLC-FLD method and 0.98/3.28, 1.11/3.72 and 0.88/2.96 microg/L, respectively for the LC-MS/MS method. Within-day and between-day precision were both <12% for the HPLC-FLD method, and <10% for the LC-MS/MS method. The recovery of OTA and its metabolites ranged between 71 and 111% for the HPLC-FLD method and between 79 and 110 % for the LC-MS/MS method. In the first experiment only OTA was added to the Caco-2 cells while in the second experiment 3-methylcholanthrene (3MC) was also present in the cell culture systems. Besides OTA, which was recovered in all the samples, an unknown compound was also observed in the second experiment. When 3MC was added, the results showed that the OTA concentration in the basolateral samples was decreased by 50%. The methods were also implemented for the analysis of urine samples of sheep, fed increasing amounts of OTA. With the HPLC-FLD method it could be concluded that the concentration of OTA and OTalpha increased according to ingested amounts of OTA, with OTalpha being the most abundant compound. The results obtained with the LC-MS/MS method confirmed these results. Copyright (c) 2008 John Wiley & Sons, Ltd.     

Admixtures to d-wave gap symmetry in untwinned YBa2Cu3O7 superconducting films measured by angle-resolved electron tunneling

We report on an ab anisotropy of Jc parallel b/Jc parallel a approximately/= 1.8 IcRn parallelb/IcRn parallel a approximately/= 1.2 and in ramp-edge junctions between untwinned YBa2Cu3O7 and s-wave Nb. For these junctions, the angle theta with the YBa2Cu3O7 crystal b axis is varied as a single parameter. The RnA(theta) dependence presents twofold symmetry. The minima in IcRn at theta approximately/= 50 degrees suggest a real s-wave subdominant component and negligible d(xy)-wave or imaginary s-wave admixtures. The IcRn(theta) dependence is well fitted by 83% dx2-y2-, 15% isotropic s-, and 2% anisotropic s-wave order parameter symmetry, consistent with deltab/deltaa approximately/= 1.5.     

Phase-sensitive order parameter symmetry test experiments utilizing Nd(2-x)Ce(x)CuO(4-y)/Nb zigzag junctions

Phase-sensitive order parameter symmetry test experiments are presented on the electron-doped high-T(c) cuprate Nd(2-x)Ce(x)CuO(4-y). These experiments have been conducted using zigzag-shaped thin film Josephson structures, in which the Nd(2-x)Ce(x)CuO(4-y) is connected to the low-T(c) superconductor Nb via an Au barrier layer. For the optimally doped as well as for the overdoped Nd(2-x)Ce(x)CuO(4-y), a clear predominant d(x2-y2)-wave behavior is observed at T=4.2 K. Both compounds were also investigated at T=1.6 K, presenting no indications for a change to a predominant s-wave symmetry with decreasing temperature.     

A novel class of naturally occurring halogenated pyrroles, 1,1′-dimethyl-3,3′,4,4′,5,5′-hexabromo-2,2′-bipyrrole, 5,5′-dichloro-1,1′-dimethyl-3,3′,4,4′-tetrabromo-2,2′-bipyrrole, and 1,1′-dimethyl-3,3′,4,4′,5,5′-hexachloro-2,2′-bipyrrole

Crystal structure determinations of the three title hexahalogenated bipyrroles, (I) C₁₀H₆Br₆N₂, (II) C₁₀H₆Br₄Cl₂N₂, and (III) C₁₀H₆Cl₆N₂, reveal essentially planar pyrrole rings having dihedral angles of 64.7, 65.1, and 64.2° between the least-squares planes, favoring in each case a closer methyl–halogen conformation. All three complexes crystallize in the orthorhombic space group Pbcn with the following cell dimensions: (I) a = 12.654(3) Å, b = 8.853(2) Å, c = 13.753(3) Å, = = = 90°, Z = 4; (II) a = 12.438(6) Å, b = 8.753(6) Å, c = 13.696(3) Å, = = = 90°, Z = 4; (III) a = 12.088(6) Å, b = 8.566(4) Å, c = 13.486(8) Å, = = = 90°, Z = 4.