Catalytic asymmetric synthesis of glutamate analogues

Utilizing our lateral metalation coupled with Jacobsen's catalytic asymmetric amino nitrile synthesis, we have demonstrated the ability to synthesize isoxazole-containing amino acid glutamate analogues in high yield and high enantiomeric excesses. Chiral centers alpha or beta at the C-5 position do not detract from diastereoselectivity of the Jacobsen-Strecker reaction. [reaction: see text]     

Direct Observation of the Molten State of Nanometer-sized Particles With an Atomic Force Microscope: A Feasibility Study

An atomic force microscope (AFM) was used to directly examine the physical state of nanometer-sized particles. The critical diameter of indium particles, where evidence of melting at room temperature was observed, was 7.8 ± 1.2nm. This conclusion is based on a method relying on the manipulation of particles in ambient air and at constant temperature. This method involves a simple set-up that permits a combination of both manipulation and imaging of individual particles. To determine whether a particle is molten, three criteria are used: the merging of particles to form bigger spherical particles, a tip-induced shape change, and the formation of nanofibers. All three criteria have been checked using other particle materials. An attempt at 56°C revealed oxidation of the indium particles as the major problem for melting investigation. Manipulations under high-purity nitrogen atmosphere support the validity of the findings. The use of the AFM to determine whether a nanoparticle is molten is, however, complicated by the oxidation issue.     

Resonant Brewster filters with absentee layers

A method for lowering the sideband levels associated with the spectral response of resonant waveguide-grating filters is presented. With a TM-polarized incident wave near the Brewster angle, the filter sidebands are suppressed by application of a half-wavelength absentee waveguide layer and an arbitrary-thickness grating layer. Adjusting the thickness of the grating layer permits control of the filter linewidth without appreciably affecting the sideband features. To verify the theoretical prediction, we fabricated and tested a double-layer waveguide-grating filter. It exhibited a peak efficiency of 82.4%, with sideband reflection levels below 0.6%, over a 95-nm spectral range.     

Microstructure and dynamics in lyotropic liquid crystals. Principles and applications of nuclear spin relaxation

Abstract

Nuclear spin relaxation of quadrupolar nuclei provides access to a wide range of properties of lyotropic liquid crystals, ranging from the molecular ordering and dynamics at the interface to the macroscopic viscoelastic behaviour. We emphasize here the unique capability of the spin relaxation method to provide detailed geometric and dynamic information relating to the microstructure of lyotropic liquid crystals, i.e. the metric, curvature, and fluctuations of the dividing interface that separates polar and non-polar regions. This information is conveyed to the spin system via the translational diffusion of surfactants or counterions over the interface. The general principles of the spin relaxation method, as applied to lyotropic liquid crystals, are described, with emphasis on the model-independent information content of the relaxation observables and on the relation to microstructure. Specific results for lamellar, hexagonal, cubic, and nematic phases are also described.     

Uncertainty of standard addition experiments: a novel approach to include the uncertainty associated with the standard in the model equation

A new model equation for determining the measurement result in standard addition experiments was derived and successfully applied to the quantitative determination of rhodium in automotive catalysts. Existing equations for standard addition experiments with gravimetric preparation were changed in order to integrate the novel idea of including the uncertainty associated with the standard into the model equation. Using this novel equation combined with the ordinary least squares algorithm for the regression line also yielded a new formula for the associated measurement uncertainty. This uncertainty accounts for the first time for the uncertainty associated with the standard. The derivation for the model equation and the resulting associated measurement uncertainty is shown for gravimetric standard addition experiments both with and without an internal standard.     

Antiferroelectric siloxane liquid crystal dimers with large molecular tilt under an applied electric field

The scope of the present study is the response of a series of antiferroelectric dimeric or bi‐mesogenic siloxanes to an applied electric field with focus on their pretransitional behaviour and the field‐induced antiferro–ferroelectric (AF–F) transition. Most of these compounds possess a molecular tilt close to 45° and spontaneous polarization in the field‐induced ferroelectric (F) phase in the range of 250–300 nC cm^?2. In the dimers with a spacer length exceeding five carbons, a transformation from first to second order of the field‐induced AF–F transition is found with temperature. Several different indications for this transformation are identified and their characteristics are discussed in the framework of the existing theoretical models. A large field‐induced in‐plane deviation of the sample optic axis was observed in the pretransitional region of several of the siloxane dimers and is likely due to the flexibility of the linking chains. The potential of the antiferroelectric bimesogenic siloxanes for displaying high contrast images and grey scale capability is shortly discussed. The large molecular tilt close to 45° in combination with the field‐induced AF–F transition of second order seems to be the most attractive features of these materials.     

Estimation of optimal backward perturbation bounds for the linear least squares problem

In this paper a method of estimating the optimal backward perturbation bound for the linear least squares problem is presented. In contrast with the optimal bound, which requires a singular value decomposition, this method is better suited for practical use on large problems since it requiresO(mn) operations. The method presented involves the computation of a strict lower bound for the spectral norm and a strict upper bound for the Frobenius norm which gives a gap in which the optimal bounds for the spectral and the Frobenius norm must be. Numerical tests are performed showing that this method produces an efficient estimate of the optimal backward perturbation bound.     

Solvent extraction procedures combined with back-extraction for trace metal determinations by atomic absorption spectrometry

Metal dithiocarbamate extractions with three different organic solvents (chloroform, freon and 4-methylpentan-2-one) followed by back-extraction with nitric acid are described. The back-extraction is studied in detail and simple rapid procedures are described for each solvent. The dilute nitric acid solution obtained is suitable for use with both flame and electrothermal atomic absorption spectrometry. Quantitative recoveries were obtained for Cd, Cu, Fe, Ni, Pb and Zn. Cobalt could be rapidly back-extracted only from chloroform and freon.     

Annoyance caused by noise from shooting ranges

This paper reports results from a study of annoyance due to noise from shooting ranges. The results show that annoyance is low up to a certain threshold after which it increases relatively quickly. This threshold varies with the choice of exposure measurement, but the covariation between exposure and annoyance is relatively similar and shows by and large the same tendency. An increase in number of shots fired does not increase the extent of annoyance. When the exposure is measured in dB(A) Fast the threshold for annoyance seems to be about 60–65 dB(A).     

Implementation of a protein profiling platform developed as an academic-pharmaceutical industry collaborative effort

As much attention has devoted to the proteome research during the last few years, biomarker discovery has become an increasingly hot area, potentially enabling the development of new assays for diagnosis and prognosis of severe diseases. This is the field of research interest where efforts originating from both academic and industrial groups should jointly work on solutions. In this paper, we would like to demonstrate the fruitful combination of both research domains where the scientific crossroads sprout fresh ideas from the basic research domain and how these are refined and tethered to industrial standards. We will present an approach that is based on novel microfluidic devices, utilizing their benefits in processing small-volume samples. Our biomarker discovery strategy, built around this platform, involves optimized samples processing (based on SPE and sample enrichment) and fast MALDI-MS readout. The identification of novel biomarkers at low-abundance level has been achieved by the utilization of a miniaturized sample handling platform, which offers clean-up and enrichment of proteins in one step. Complete automation has been realized in the form of a unique robotic instrumentation that is able to extract and transfer 96 samples onto standard MALDI target plates with high throughput. The developed platform was operated with a 60 sample turnaround per hour allowing sensitivities in femtomol regions of medium- and low-abundant target proteins from clinical studies on samples of multiple sclerosis and gastroesophageal reflux disease. Several proteins have been identified as new biomarkers from cerebrospinal fluid and esophagus epithelial cells.