High field magnetization of Pr1-xGdxNi single crystals

Magnetization measurements were carried out on Pr_1−xGd_xNi single crystals for x=0.1, 0.2, 0.3 and 0.4 using pulsed magnetic fields up to 55 T and at 4.2 K. For the data observed along the c-axis there are clear indications of transitions, of the combined system of Pr and Gd moments, from a ferrimagnetic to a ferromagnetic state. The observed saturation magnetizations at 55 T and intermediate magnetizations at 1 T were well modeled assuming ferro- and ferri-magnetic structures, respectively.     

Indirect detection of the 183W and 57Fe nuclei using 119Sn‐relayed 1H,X correlation spectroscopy

Recently reported triple‐resonance Y‐relayed ¹H,X correlation experiments have been utilized to characterize ¹⁸³W and ⁵⁷Fe chemical shifts using ¹¹⁹Sn as the Y‐relaying nucleus instead of the previously used ³¹P. Application of an adaptation of Gudat's original INEPT/HMQC sequence results in a significant enhancement of the signal‐to‐noise (S/N) ratio for two‐dimensional ¹¹⁹Sn‐relayed ¹H,¹⁸³W and ¹H, ⁵⁷Fe correlation spectra with efficient detection of the transition metal nucleus in tungsten and iron complexes lacking an observable direct scalar coupling between the transition metal and any hydrogen nuclei. Strengths and shortcomings of the novel sequence and the original sequences reported by Gudat are discussed in the context of ¹¹⁹Sn‐relayed proton detection of very low frequency transition metal nuclei. Copyright © 2010 John Wiley & Sons, Ltd.     

Oxidation activity of Au nanoparticles on aerogel supports

We have prepared titania aerogel and titania-coated silica aerogel incorporating thiol-capped Au nanoparticles. Both composite materials showed high CO oxidation activity after they were calcined at 673 K. Compositional and morphological changes driven by calcination were evaluated with thermogravimetry and X-ray diffractometry. From the results, it was suggested that the nanoparticles transformed from a faulted to a near-regular FCC structure presumably in concert with the formation of firm contacts between the nanoparticles and the gel substrates. While the diameters of the Au particles in the titania aerogel considerably increased upon calcination, those in the titania-coated silica aerogel were almost unchanged. As a consequence, the latter composite aerogel showed higher activity for oxidation of CO.     

Crystal structure of [1,4-bis[1-(3,5-dichlorophenolato-2-ylmethyl)-ylpropylamino-kappa2N,O]piperazine-kappa2N,N']cobalt(II).

The X-ray crystal structure of the title complex, Co(Cl2bprpi) is described. In this complex the Co(II) center displays a distorted octahedral coordination geometry. The piperazine ring exhibits boat conformation, forming chelate rings and capping the Co atom. The N2-Col-N3 angle is 69.41(15) degrees, extremely smaller than 90 degrees. Because the small angle causes a large steric hindrance, the piperazine ring can be effective as an ion size-recognition site. The molecular structure is stabilized by intramolecular N-H...O hydrogen bonds and Cl...H contacts.     

Pseudo soliton in fluidized beds and its perturbed treatment

The author summarize the recent analysis of a two-fluid model which describes fluidized beds of granular particles. It has been found that near the transition point from stable fluidized beds to unstable ones the two-fluid model is reduced to the KdV equation with small dissipation. The amplitude and the propagating velocity of a pulse of the reduced equation is obtained.Department of Physics, Tohoku University, Sendai 980, Japan. E-mail: hisao@cmpt01.phys.tohoku.ac.jp. Translated from Teoreticheskaya i Matematicheskaya Fizika, Vol. 99, No. 2, pp. 309–314, May, 1994.     

Enantioselective addition of allyltin reagents to amino aldehydes catalyzed with bis(oxazolinyl)phenylrhodium(III) aqua complexes

Bis(oxazolinyl)phenylrhodium(III) aqua complexes, (Phebox)RhX?(H?O) [X = Cl, Br], were found to be efficient Lewis acid catalysts for the enantioselective addition of allyl- and methallyltributyltin reagents to amino aldehydes. The reactions proceed smoothly in the presence of 5-10 mol % of (Phebox)RhX?(H?O) complex at ambient temperature to give the corresponding amino alcohols with modest to good enantioselectivity (up to 94% ee).     

Preparative purification of gentamicin components using high-speed counter-current chromatography coupled with electrospray mass spectrometry

We developed a useful and preparative method based on high-speed counter-current chromatography with mass spectrometry (HSCCC/MS) to purify gentamicin C1a, C2/2a and C1 from standard powder. The analytes were purified on the HSCCC model CCC-1000 (multi-layer coil planet centrifuge) with a volatile two-phase solvent system composed of n-butanol/10% aqueous ammonia solution (50:50, v/v) and detected on an LCMS-2020EV quadrupole mass spectrometer fitted with an electrospray ionization (ESI) source system in positive ionization following scan mode (m/z 100-500). The HSCCC/ESI-MS peaks indicated that gentamicin C1a (m/z 450: [M+H](+)), C2/2a (m/z 464: [M+H](+)) and C1 (m/z 478: [M+H](+)) have the peak resolution values of 1.3 and 1.7 from 30 mg of loaded gentamicin powder. The HSCCC yielded 3.9 mg of gentamicin C1a, 12.6 mg of gentamicin C2/2a and 12.0 mg of gentamicin C1. These purified substances were analyzed by LC/MS with scan positive-mode. Based on the LC/MS chromatograms and spectra of the fractions, analytes were estimated to be over 95% pure. These gentamicin isomers of C1a, C2/2a and C1 were evaluated for their antibacterial activities. The overall results indicate that this approach of HSCCC/MS is a powerful technique for the purification of gentamicin components.