Fused silica capillary deactivation with D4 in the presence of oxygen

A new, simple procedure to deactivate fused silica capillaries without hydrothermal treatment is proposed. Based on high temperature reactions of octamethylcyclotetrasiloxane (D₄) in the presence of oxygen, this procedure results, upon coating with dimethylsilicone (SE-30), in columns which give almost symmetric peaks for as little as 150 pg of critical compounds, such as decylamine, thereby demonstrating very high inertness. A mechanism of the deactivation procedure, which, in contrast to previously developed procedures, is based on thermal reactions under aerobic conditions, is proposed.     

Syntheses of Two Potential Ligands for Tc-99m Labeling as Diagnosis Agents of Alzheimer''''s Disease

Two types of ligands-biphenyl and stilbene derivatives, whichcan be labeled with Tc-99m for the diagnosis of Alzheimer'sdisease (AD) have been synthesized successfully. The key stepsin these two syntheses involved Suzuki reaction and Wittig reac-tion respectively. The new discovered debromination reactionmay be expanded to the compounds with double or triple bondadjacent to the carbon atom bearing the bromine atoms. Thesetypes of syntheses provide a route to a series of biphenyl andstilbene derivatives that will benefit the search of new imagingagents for AD.     

Dynamic optimization problems with bounded terminal conditions

Bounded terminal conditions of nonlinear optimization problems are converted to equality terminal conditions via the Valentine's device. In so doing, additional unknown parameters are introduced into the problem. The transformed problems can still be easily solved using the sequential gradient-restoration algorithm (SGRA) via a simple augmentation of the unknown parameter vector . Three example problems with bounded terminal conditions are solved to verify this technique.This research was supported in part by the National Aeronautics and Space Administration under NASA Grant No. NCC 2-106.     

Sufficient conditions for a strong relative minimum in an optimal control problem

In this paper, on the basis of Young's method (Ref. 1), sufficient conditions for a strong relative minimum in an optimal control problem are given. Young's method generalizes geodesic coverings and the simplest Hilbert integral from the standard variational calculus. This paper carries Young's method over to nonparametric problems.     

Quantitative surface analysis by Auger and x-ray photoelectron spectroscopy

Recent developments in quantitative surface analysis by Auger (AES) and x-ray photoelectron (XPS) spectroscopies are reviewed and problems relating to a more accurate quantitative interpretation of AES/XPS experimental data are discussed. Special attention is paid to consideration of elementary physical processes involved and influence of multiple scattering effects on signal line intensities. In particular, the major features of core-shell ionization by electron impact, Auger transitions and photoionization are considered qualitatively and rigorous approaches used to calculate the respective transition probabilities are analysed. It is shown that, in amorphous and polycrystalline targets, incoherent scattering of primary and signal Auger and photoelectrons can be described by solving analytically a kinetic equation with appropriate boundary conditions. The analytical results for the angular and energy distribution, the mean escape depth, and the escape probability as a function of depth of origin of signal electrons as well as that for the backscattering factor in AES are in good agreement with the corresponding Mote Carlo simulation data. Methods for inelastic background subtraction, surface composition determination and depth-profile reconstructions by angle-resolved AES/XPS are discussed. Examples of novel techniques based on x-ray induced photoemission are considered.     

Isoperichoric focusing field-flow fractionation and thin layer isoperichoric focusing based on coupling of gradient generated by primary field with secondary field action: general principles and performances

The primary field forces can generate spatially oriented gradient of the effective property of a continuum or pseudo-continuum fluid (carrier liquid). When this gradient is coupled with the action of a secondary field of identical or different nature the isoperichoric focused zones of the dispersed species can appear. Consequently, they can be separated according to differences responding to the property gradient of the carrier liquid. This concept can be applied under static (non-flow) conditions in thin layer focusing as well as under dynamic conditions with the elution due to the carrier liquid flow in focusing field-flow fractionation. The gradient established by the action of the primary field and the concentration distribution of the isoperichoric focused zone formed by the coupled effect of the gradient and of the primary or secondary field are described theoretically. The rigorous relationship describing the shape of the focused zone is compared with the approximate solutions. The performances of the proposed principle were evaluated by model calculations. Potential experimental configurations considering the implementation of the static and dynamic conditions are discussed. The generalized isoperichoric focusing theory can be applied to describe the particular processes operating in analytical and preparative focusing separations of the particles of various, but especially of biological origin.     

Electromagnetic interference shielding and radiation absorption in thin polypyrrole films

Results of permittivity measurements, electromagnetic interference shielding effectiveness, and heat generation due to microwave absorption in conducting polymer coated textiles are reported and discussed. The intrinsically conducting polymer, polypyrrole, doped with anthraquinone-2-sulfonic acid (AQSA) or para-toluene-2-sulfonic acid (pTSA) was applied on textile substrates and the resulting materials were investigated in the frequency range 1-18 GHz. The 0.54 mm thick conducting textile/polypyrrole composites absorbed up to 49.5% of the incident 30-35 W microwave radiation. A thermography station was used to monitor the temperature of these composites during the irradiation process, where absorption was confirmed via visible heat losses. Samples with lower conductivity showed larger temperature increases caused by microwave absorption compared to samples with higher conductivity. A sample with an average sheet resistivity of 150 Ω/sq. showed a maximum temperature increase of 5.27 °C, whilst a sample with a lower resistivity (105 Ω/sq.) rose by 3.85 °C.     

Inductively coupled plasma atomic emission spectrometry — Optimization of the operating conditions in the determination of trace of elements in line-rich emission matrices

Radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometer was used in the determination of Y, Sc and rare earth elements in Eu₂O₃ or Lu₂O₃ as pure rare earth matrices. The Mg II 280.270 nm/Mg I 285.213 nm line intensity ratio was measured to evaluate the robustness of the operating conditions. The operating conditions were affected by varying the incident power and sheathing gas flow rate. The carrier gas flow rate remained a constant value. The relationship between the Mg II 280.270 nm/Mg I 285.213 nm ratio and the excitation temperature was obtained. A dependence of the magnesium ratio in the pure solvent and the corresponding values in the presence of the above matrices was established.     

Selective cleavage of acetals with ZnBr2 in dichloromethane

A selective cleavage of acetals of 1,2- and 1,3-diols has been achieved under mild conditions using ZnBr₂ in dichloromethane at room temperature. Acetal types cleavable by this procedure include benzylidene, isopropylidene and cyclohexylidene acetals. This method is compatible with several other types of hydroxyl protecting groups such as Bn, Bz, TBDPS, TIPS and TBDMS.     

Characterization of CNS disorders and evaluation of therapy using structural and functional MRI

Modern drug development requires technologies that allow rapid translation from the preclinical to the clinical stage. It is obvious that non-invasive imaging modalities such as magnetic resonance imaging (MRI) will play a central role in this regard. This article reviews the use of structural and functional MRI readouts for characterization of central nervous system (CNS) disorders and evaluation of the efficacy of potential CNS drugs. Examples comprise dementia of Alzheimer's type, cerebral ischemia, and neuroinflammation covering both clinical and preclinical aspects. In these examples MRI has been used to obtain relevant structural information on brain atrophy, on the location and extent of ischemic brain areas, and on the number and distribution of demyelinated plaques. These structural data are complemented by readouts assessing the functional consequences associated with the pathomorphological changes. In the last decade, MRI has evolved into a standard tool for the development of CNS drugs. With regard to target-specific/molecular imaging applications MRI is limited by its inherently low sensitivity; complementary imaging modalities utilizing optical and radionuclear reporter systems will thus be required.