Preparative isolation of (+)-beta-eudesmol fromAmyris balsamifera

Summary Optically pure (+)-beta-eudesmol is a possible starting material for the synthesis of several termite defense compounds. A two step procedure for the isolation of gram quantities of (+)-beta-eudesmol from commercially availableAmyris balsamifera oil (syn. West Indian sandalwood oil), containing 8% beta-eudesmol, was developed. Step one consisted of an efficient vacuum distillation of the total oil. Step two was a medium pressure LC separation with an AgNO₃ impregnated silica gel stationary phase. Several other separation procedures failed due to the presence of many closely related sesquiterpene alcohols (75% of the oil).     

A compact permanent magnet array with a remote homogeneous field

We present the design and construction of a single sided magnet array generating a homogeneous field in a remote volume. The compact array measures 11.5 cm by 10 cm by 6 cm and weights approximately 5 kg. It produces a B(0) field with a 'sweet spot' at a point 1cm above its surface, where its first and second spatial derivatives are approximately zero. Unlike other sweet spot magnets of this general type, our array has B(0) oriented parallel to its surface. This allows an ordinary surface coil to be used for unilateral measurements, giving the potential for dramatic SNR improvement.     

Distortion-free single point imaging of multi-layered composite sandwich panel structures

The results of a magnetic resonance imaging (MRI) investigation concerning the effects of an aluminum honeycomb sandwich panel on the B1 and B0 fields and on subsequent image quality are presented. Although the sandwich panel structure, representative of an aircraft composite material, distorts B0 and attenuates B1, distortion-free imaging is possible using single point (constant time) imaging techniques. A new expression is derived for the error caused by gradient field distortion due to the heterogeneous magnetic susceptibility within a sample and this error is shown not to cause geometric distortion in the image. The origin of the B0 distortion in the sample under investigation was also examined. The graphite-epoxy 'skin' of the panel is the principal source of the B0 distortion. Successful imaging of these structures sets the stage for the development of methods for detecting moisture ingress and degradation within composite sandwich structures.     

Acoustic disturbance from gas non-uniformities convected through a nozzle

The non-steady flow generated by convection of gas containing non-uniform temperature regions or “entropy spots” through a nozzle is examined analytically as a source of acoustic disturbance. The first portion of the investigation treats the “compact nozzle”, the case where all wave lengths are much longer than the nozzle. Strengths of transmitted and reflected one-dimensional waves are given for supersonic and subsonic nozzles and for one configuration of supersonic nozzle with normal shock at the outlet. In addition to a wave reflected from the nozzle inlet, the supersonic nozzle discharges two waves, one facing upstream and the other facing downstream. For reasonable values of the nozzle inlet Mach number, the pressure amplitude of each wave increases directly as the discharge Mach number.The acoustic perturbations from a supercritical nozzle of finite length, in which the undisturbed gas velocity increases linearly through the nozzle, are analyzed for several inlet and discharge Mach number values and over a wide frequency range. The results which agree with the compact analysis for low frequency, deviate considerably as the frequency rises, achieving pressure fluctuation levels of several times the compact values. It is shown that this result originates in a phase shift between the two waves emitted downstream and that the pressure fluctuations for moderate frequencies may be approximated from the compact analysis with an appropriate phase shift.In all cases, the pressure fluctuations caused by a 2% fluctuation in absolute inlet temperature are large enough to require consideration in acoustic analysis of nozzles or turbine blade channels.     

Numerical simulations of high-speed chemically reacting flow

The essentially nonoscillatory (ENO) shock-capturing scheme for the solution of hyperbolic equations is extended to solve a system of coupled conservation equations governing two-dimensional, time-dependent, compressible chemically reacing flow with full chemistry. The thermodynamic properties of the mixture are modeled accurately, and stiff kinetic terms are separated from the fluid motion by a fractional step algorithm. The methodology is used to study the concept of shock-induced mixing and combustion, a process by which the interaction of a shock wave with a jet of low-density hydrogen fuel enhances mixing through streamwise vorticity generation. Test cases with and without chemical reaction are explored here. Our results indicate that, in the temperature range examined, vorticity generation as well as the distribution of atomic species do not change significantly with the introduction of a chemical reaction and subsequent heat release. The actual diffusion of hydrogen is also relatively unaffected by the reaction process. This suggests that the fluid mechanics of this problem may be successfully decoupled from the combustion processes, and that computation of the mixing problem (without combustion chemistry) can elucidate much of the important physical features of the flow.This work has been supported by the Aerospace Corporation through a Corporate Fellowship, by NASA Dryden Flight Research Center under Grant NCC 2-374, by ONR Grant N00014-86-K-0691, by NSF Grant DMS 88-11863, and by a DARPA Grant in the ACMP Program.     

Reaction of metallo S-alkyl N-cyanodithioiminocarbonates and alkyl N-cyanocarbamates with hydrazine. A novel preparation of 5-amino-3-mercapto-1,2,4-triazole

Metal salts of S-alkyl-N-cyanodithioiminocarbonates 7 react as electrophiles with hydrazine hydrate to form 5-amino-3-mercapto-1H-1,2,4-triazole 1 . The novel 4-cyanothiosemicarbazide 9 is proposed as the intermediate which cyclizes to the aromatic triazole. The rate determining step is addition of hydrazine to the iminocarbonate and is second order. Other nucleophiles such as substituted hydrazines and amines failed to react. Exchange of either or both sulfurs with oxygen leads to decomposition or mixtures of products.     

Radionuclide dating and trace element analysis by accelerator mass spectrometry

Accelerator Mass Spectcrometry (AMS) is being used for both radionuclide dating and stable isotope trace element determination with limits of high sensitivity. The areas of applications of radionuclide AMS include oceanography, terrestrial studies, glaciology, hydrology, environmental studies, meteorology, archaeology, anthropology, analysis of crude oils, biomedical and materials sciences, etc. The techniques and applications of radionuclide AMS are reviewed. The applications of stable element AMS include the measurements of trace impurities in electronic and other materials. The techniques and applications of stable element AMS are discussed with particular emphasis on electronic materials such as Si, GaAs, and HgCdTe. The design of the University of North Texas stable element AMS facility built in collaboration with Texas Instruments Incorporated is discussed.Work supported in part by the National Science Foundation Grants No. DMR-8812331 and ECD-9003099, the Office of Naval Research Grants No. N00014-89-J-1309, N00014-89-J-1344, N00014-90-J-1691, and N00014-91-J-1785, Texas Instruments Incorporated, Texas Utilities Electric Inc. International Digital Modeling Corp., North Texas Research Institute, Combustion Engineering Inc., LTV Corporation, the State of Texas Higher Education Coordinating Board — Texas Advanced Technology Research Program, the Robert A. Welch Foundation, and the University of North Texas Organized Research Fund.     

An analytical methodology for magnetic field control in unilateral NMR

Traditionally, unilateral NMR systems such as the NMR-MOUSE have used the fringe field between two bar magnets joined with a yoke in a 'U' geometry. This allows NMR signals to be acquired from a sensitive volume displaced from the magnets, permitting large samples to be investigated. The drawback of this approach is that the static field (B0) generated in this configuration is inhomogeneous, and has a large, nonlinear, gradient. As a consequence, the sensitive volume of the instrument is both small and ill defined. Empirical redesign of the permanent magnet array producing the B0 field has yielded instruments with magnetic field topologies acceptable for varying applications. The drawback of current approaches is the lack of formalism in the control of B0. Rather than tailoring the magnet geometry to NMR investigations, measurements must be tailored to the available magnet geometry. In this work, we present a design procedure whereby the size, shape, field strength, homogeneity, and gradients in the sensitive spot of a unilateral NMR sensor can be controlled. Our design uses high permeability pole pieces, shaped according to the contours of an analytical expression, to control B0, allowing unilateral NMR instruments to be designed to generate a controlled static field topology. We discuss the approach in the context of previously published design techniques, and explain the advantages inherent in our strategy as compared to other optimization methods. We detail the design, simulation, and construction of a unilateral magnet array using our approach. It is shown that the fabricated array exhibits a B0 topology consistent with the design. The utility of the design is demonstrated in a sample nondestructive testing application. Our design methodology is general, and defines a class of unilateral permanent magnet arrays in which the strength and shape of B0 within the sensitive volume can be controlled.