Mass spectra of substituted pyrazolo[1,5-a]-1,3,5-triazines

High resolution electron impact mass spectrometric measurements have been made on twelve pyrazolo[1,5-a]-1,3,5-triazines. Substituents attached to carbon atoms 2, 4, 7, and 8 were used to label the various fragments. Three major ions were observed (a) the molecular ion, (b) an ion corresponding to M-RCN where R is the substituent attached to C-4 and (c) an aryl cyclopropenyl cation which was observed in 7-aryl derivatives. Intensities and accurate mass-measurements are given for all ions having intensities exceeding 2% of the base peak. Nine of the twelve pyrazolo-[1,5-a]-1,3,5-triazines included in this study are described here for the first time.     

Exploiting C3-symmetry in the dynamic coordination of a chiral trisoxazoline to copper(II): improved enantioselectivity, and catalyst stability in asymmetric lewis acid catalysis

Chiral C3-symmetric trisoxazolines are highly efficient stereodirecting ligands in enantioselective Cu(II) Lewis acid catalysis which is based on the concept of a stereoelectronic hemilability of the divalent copper; in direct comparison with the analogous bisoxazoline systems they are more efficient in the enantioselective alpha-amination as well as the enantioselective Mannich reaction of prochiral beta-ketoesters.     

Chromatographic and mass spectrometric methods for determination of lysergic acid diethylamide (LSD) and metabolites in body fluids.

Continued illicit use of the potent psychedelic drug lysergic acid diethylamide (LSD) has stimulated efforts to develop effective analytical methods for detection of the drug and its metabolites in body fluids from suspected LSD users. Recently reported methods based on gas and liquid chromatography, combined with single- and multiple-stage mass spectral analysis, now permit accurate detection and quantitation of LSD at sub-nanogram/milliliter concentrations.     

Modeling β-γ coincidence spectra of <Superscript>131m</Superscript>Xe, <Superscript>133</Superscript>Xe, <Superscript>133m</Superscript>Xe,and <Superscript>135</Superscript>Xe

In support of the Comprehensive Nuclear-Test-Ban Treaty (CTBT), improvements have been made to the model of the Automated Radioxenon Sampler/Analyzer (ARSA) β-γ coincidence detector for radioxenon monitoring. MCNPX is used to simulate the detector response for all the electrons and photons emitted from ^131mXe, ¹³³Xe, ^133mXe, ¹³⁵Xe, and ¹³⁷Cs signals. A MatLab code was written to incorporate the MCNPX results in the calculation of β-γ coincidence spectra. These will aid in the development of the Spectral Deconvolution Analysis Tool (SDAT)¹ and to calibrate β-γ coincidence systems. The models developed for this work include improvements over previous models in their ability to address Compton scattering in the β-cell, and the β-distribution offset in the 31 keV γ-ray region for ¹³³Xe.     

An experiment to measure the pressure dependence of the zero-shear-rate viscosity

A simple experimental method, based on Stokes' law for falling spheres, has been devised and used to measure the pressure-dependence of the zero-shear-rate viscosity of a polypropylene melt. The experiment was performed by maintaining three thick-walled test cylinders containing the polymer melt and the falling sphere at the same elevated temperature but different pressures for periods of time ranging from 20 to 48 hours.When compared with experiments using high-pressure capillary or rotational viscometers, this experimental method has the advantages that viscous heating is non-existent and the apparatus and data analysis are relatively simple. The principal disadvantage encountered here, thermal degradation at high temperatures, could probably be reduced by molding specimens under vacuum and by shortening the exposure time. Since the falling-sphere experiment provides data at very low shear rates and the capillary and rotational viscometers generate data at high shear rates, the two experimental methods are complementary.The pressure coefficient b [=d(In η₀/dp] was determined for Hercules Pro-fax 6523 polypropylene in two series of experiments at different temperatures. For seven experiments at 218.3°C and pressures up to 97.9 $\text{MN}\text{m}{}^2$ (14,200 psi), the average value of b ± 95% confidence limits was found to be 14.8 ($\text{GN}\text{m}{}^2$)^?1 ± 2.9.The average b was 12.6 ($\text{GN}\text{m}{}^2$)^?1 ± 1.4 in a series of eight experiments at 232.2°C and pressures up to 123 $\text{MN}\text{m}{}^2$ (17,800 psi).