Crystal structure of Al(tBu)3(NH2CH2CH2Ph): A molecular “slinky”

The molecular structure of Al(^tBu)₃(NH₂CH₂CH₂Ph) is determined by the crystal packing of the phenyl rings and the pseudo spherical Al(^tBu)₃ units, and may be viewed as a layered structure consisting of double sheets of the phenyl rings and the Al(^tBu)₃ units. The Al–N–C–C linkage shows severe disorder as a result of its flexibility. The structure of Al(^tBu)₃ (NH₂CH₂CH₂Ph) can be likened to a molecular slinky, in which the rigid ends are fixed in space by molecular packing forces, leaving the interior link to adopt multiple orientations. Crystal data: orthorhombic, Cmca,a=13.282(9),b=25.01(1),c=13.210(9), Å,V=4388(10) ų,Z=4,R=0.0957,R _w=0.0957.     

Radiation-induced trapping centers in thin silicon dioxide films

In this paper the technological and scientific aspects of radiation-related charge trapping in thin SiO₂ films are reviewed. These films are amorphous in nature and are thermally grown on single crystal silicon substrates serving as the insulating layer in metal-oxide-semiconductor (MOS) capacitors and transistors. The structure and operation of these devices are reviewed with special emphasis on the effect of charges trapped in the oxide. The technical importance of understanding the interaction of ionizing radiation with thin SiO₂ films is illustrated with two practical examples. The first involves the operation of MOS transistors in environments where ionizing radiation is present, leading to an accumulation of positive space charge in the oxide. The second deals with process-induced defects generated by radiation encountered during the fabrication of devices by processes such as electron beam lithography or electron gun metallization. Unannealed traps of this type capture hot electrons producedin the substrate during the operation of the MOS transistor. In both these examples, the charging of the oxide results in instabilities which degrade operation.

Its sensitivity to charge trapped in the insulator makes the MOS system an ideal vehicle for scientific study of these phenomena. The basic techniques for characterizing the density, capture cross-sections, and location are briefly discussed and applied to the problem of radiation-induced defects in thin SiO₂ films. Ionizing radiation is shown to interact with the SiO₂ in two modes. In the first it supplies carriers to fill pre-existing hole traps at the interfaces. In the second it creates electron and hole traps in the bulk of the thin film. These latter defects are in a neutral state after irradiation and are detectable only when either electrons or holes are subsequently injected into the oxide. The capture cross-sections, trap densities and location of these centers in the film are presented. The annealing treatments required to remove these traps from aluminium and polysilicon gate devices are also discussed. The number traps produced by an incident 25 KV electron beam is found to depend weakly on the dosage. A dipolar defect, produced by the ionizing radiation, seems to explain the behavior of the neutral centers.     

Routine analysis by high precision gas chromatography/mass selective detector/isotope ratio mass spectrometry to 0.1 parts per mil

Stable isotope methods are potentially quite useful for validating natural or enhanced mineral degradation of contaminants. For this reason, a continuous flow gas chromatograph (GC), isotope ratio mass spectrometer (IRMS) has been coupled with a quadrupole mass selective detector (MSD) to allow simultaneous mass spectral and stable carbon isotope ratio data to be obtained from a single chromatographic analysis. This allows the target contaminant and any extra-cellular degradation intermediates to be both qualified and quantified. Previously acceptable limits of precision (0.3 parts per mil) are undesirable given the small fractionation observed during aerobic degradation. To further understand the fate of organic contaminants and to gain information about the metabolic degradative pathway employed by a microorganism, routine isotopic analyses on a range of analytes have been performed. Quantities of sample producing mass-44 ion beam signal (I(44)) of 2 x 10(-10) to 1 x 10(-8) A were analysed. When the IRMS was tuned for high sensitivity, ion source nonlinearities were overcome by peak height correction from an algorithm that was produced using known isotopic standards of varying concentrations. This led to sample accuracy of <0.01 per thousand and sample precision of 0.1 per thousand. Copyright 1999 John Wiley & Sons, Ltd.     

Investigation of the quantitative properties of the quadrupole orthogonal acceleration time-of-flight mass spectrometer with electrospray ionisation using 3,4-methylenedioxymethamphetamine

This paper describes the investigation of the potential of a quadrupole orthogonal acceleration time-of-flight mass spectrometer (Q-TOF) equipped with an atmospheric pressure ionisation interface for quantitative measurements of small molecules separated by reversed phase liquid chromatography. To this end, the detection limits and linear dynamic range in particular were studied in an LC/MS/MS experiment using 3,4-methylenedioxymethamphetamine standards and 3,4-methylenedioxyethylamphetamine for internal standardisation. In a second phase, the experiment was repeated with real biological extracts (whole blood, serum, and vitreous humour). A calibration for 3,4-methylenedioxymethamphetamine and its metabolite 3,4-methylenedioxyamphetamine was prepared in each of these matrices again using 3,4-methylenedioxyethylamphetamine as internal standard. The resulting quantitative data were compared with those obtained by liquid chromatography with fluorescence detection for the same extracts. The Q-TOF results revealed excellent sensitivity and a linear dynamic range of nearly four decades (2-10 000 pg on-column, r(2) = 0.9998, 1/x weighting). Furthermore, all the calibration curves prepared in biological material were superimposable, LC/MS/MS and LC-fluorescence, and the quantitative results for actual samples compared very favourably. It was concluded that the Q-TOF achieves a linear dynamic range for quantitative LC/MS/MS work exceeding that of fluorescence detection and at much better absolute sensitivity. Copyright 1999 John Wiley & Sons, Ltd.     

Synthesis,thermal reactivity,and kinetics of stabilized phosphorus ylides,part 2: [(Arylcarbamoyl)(cyano)methylene]triphenylphosphoranes and their thiocarbamoyl analogues

A series of five cyano(arylcarbamoyl) phosphorus ylides 2 and five cyano(arylthiocarbamoyl) phosphorus ylides 3 are prepared and fully characterized. Pyrolytic reaction products of a representative example of each type obtained by flash vacuum pyrolysis technique show that they undergo thermal extrusion of Ph₃PO or Ph₃PS. Kinetic study of the gas‐phase pyrolysis of each ylide by static method shows that these reactions are unimolecular and first order with no significant substituent effect, but the thiocarbamoyl ylides 3 react 40–65 times more rapidly than their carbamoyl analogues 2 . © 2006 Wiley Periodicals, Inc. Int J Chem Kinet 38: 496–502, 2006     

Spin-glass-like distribution of interaction fields in a nearly ferromagnetic Ni-Cu alloy

The magnetic specific heat (C_m) of a Ni-Cu alloy of 40 at% Ni was determined from low-temperature heat capacity measurements in various magnetic fields and is shown to derive from a dilute concentration of giant-moment clusters, consistent with previous magnetization measurements. From the field and temperature dependences of C_m, it is also deduced that the distribution of interaction (exchange and anisotropy) fields experienced by the clusters extends continuously from large positive fields to large negative fields, relative to the applied field.     

Restoration of atmospherically degraded images using complex spectral ratios

A method for reconstructing atmospherically degraded stellar images from measured spectral ratios is described. An advantage of the ratio method is that an auxillary measurement to establish the OTF of the atmosphere is not required in most cases of interest.     

Structure of 72,74Se at high spin

Lifetimes of high spin states up to { }=22⁺ in the yrast positive parity bands have been measured to investigate the shape evolution with increasing spin in ^{72, 74}Se. The Q _t values derived from these measurements indicate that prolate shape stabilizes for ⁷²Se, while a triaxial shape develops for ⁷⁴Se at higher spins. Comparison of the observed trend in Q _t with spin for ^{72, 74}Se with that of the corresponding kryptones isotones emphasizes the stability provided by N=38 prolate shell gap even at high rotational frequency.