A study of aluminum recovery from power plant fly ash by high temperature chlorination was undertaken to demonstrate that fly ash could be a potential source of aluminum, iron and possibly silicon. Magnetic separation of the iron oxide served as a first step to alleviate the iron contamination problem. However, the agglomeration of some iron oxide with alumina and silica made it difficult to completely separate the iron from the fly ash. Further iron separation was achieved by chlorinating the nonmagnetic ash fraction at 550/sup 0/C for 30 minutes. This reduced the iron oxide content to less than 4 percent by weight. Chlorine flow rates affected the reaction rate much more drastically than temperatures. This suggested that diffusion was the major rate-controlling step. Besides Fe/sub 2/O/sub 3/, Al/sub 2/O/sub 3/ and SiO/sub 2/, other oxides such as CaO, K/sub 2/O, Na/sub 2/O and MgO might have complicated the alumina recovery by forming individual chlorides or complexes. Investigating methods for separating more Fe/sub 2/O/sub 3/, and possibly CaO, K/sub 2/O, Na/sub 2/O and MgO from the nonmagnetic ash fraction before chlorinating it is highly recommended.

The heat capacity of high purity electrotransport refined lutetium was measured between 1 and 20/sup 0/K. Results for theta/sub D/ were in excellent agreement with theta values determined from elastic constant measurements. The heat capacity of a series of lutetium-hydrogen solid solution alloys was determined and results showed an increase in ..gamma.. from 8.2 to about 11.3 mJ/g-atom-K/sup 2/ for hydrogen content increasing from zero to about one atomic percent. Above one percent hydrogen ..gamma.. decreased with increasing hydrogen contents. The C/T data showed an increase with temperature decreasing below about 2.5/sup 0/K for samples with 0.1 to 1.5 atomic percent hydrogen. This accounts for a large amount of scatter in theta/sub D/ versus hydrogen content in this range. The heat capacity of a bulk sample of lutetium dihydride was measured between 1 and 20/sup 0/K and showed a large increase in theta/sub D/ and a large decrease in ..gamma.. compared to pure lutetium.

The experimental verification of the two-step nature of energy dissipation of photon energy by a crystal is the subject of this dissertation. The ..cap alpha..(O,O) Davydov component of the lowest energy singlet transition in pure strain-free napthalene single crystals is shown to exhibit an increase in absorption with increasing temperature, due to an increase in polariton damping via polariton-phonon scattering processes. (GHT)

A chelating ion-exchange resin with N-(2-hydroxyethyl)ethylene-diaminetriacetic acid (HEDTA) used as the ligand chemically bonded to XAD-4 by an ester linkage, HEDTA-4, was synthesized. It is stable under normal experimental conditions with the liquid chromatograph. The structure of the resin was confirmed by an infrared spectrum, and by potentiometric titrations. The capacity of the resin was also obtained by potentiometric titration and by a nitrogen analysis. The resin was used to pack a column of 5 mm internal diameter and 5 cm long. The effect of pH on the retention of different metal ions on the resin was studied. It was found that the resin was most selective for chromium(III), copper(II), lead(II), mercury(II), uranium(VI), zirconium(IV) and zinc(II) at a pH of less than 3. Furthermore, the resin proves to be functioning with a chelating mechanism rather than ion-exchange, and it can concentrate trace metal ions in the presence of a large excess of calcium and magnesium. This makes the resin potentially useful for purifying and analyzing drinking water.

The critical stress for the reorientation of vanadium hydride was determined for the temperature range 180/sup 0/ to 280/sup 0/K using flat tensile samples containing 50 to 500 ppM hydrogen by weight. The critical stress was observed to vary from a half to a third of the macroscopic yield stress of pure vanadium over the temperature range. The vanadium hydride could not be stress induced to precipitate above its stress-free precipitation temperature by uniaxial tensile stresses or triaxial tensile stresses induced by a notch.

The electric mobility and effective valence of hydrogen and deuterium in vanadium, niobium, tantalum and three niobium-tantalum alloys were measured. A resistance technique was used to directly determine the electric mobility of hydrogen and deuterium at 30/sup 0/C while a steady-state method was used to measure the effective valence. The use of mass spectrographic techniques on a single specimen which contained both hydrogen and deuterium greatly increased the precision with which the isotope effect in the effective valence could be measured.

Off-line experiments indicated that fluorides of As, Se, Br, Kr, Zr, Nb, Mo, Tc, Ru, Sb, Te, I and Xe could be volatilized, but except for Br, Kr, I and Xe, none of these elements were observed after mass separation in the on-line experiments. The results of the on-line experiments indicated a very low level of hydride contamination at ambient temperature and consequently, uranium tetrafluoride replaced uranyl stearate as the primary gaseous fission product target. Possible reasons for the failure of the heated target system to yield non-rare gas activities are discussed and suggestions for designing a new heated target system are presented.

The feasibility of calculating Wagner self-interaction parameters from binary phase diagrams was examined. The self-interaction parameters of 22 non-ferrous liquid solutions were calculated utilizing an equation based on the equality of the chemical potentials of a component in two equilibrium phases. Utilization of the equation requires the evaluation of the first and second derivatives of various liquidus and solidus data at infinite dilution of the solute component. Several numerical methods for evaluating the derivatives of tabular data were examined. A method involving power series curve fitting and subsequent differentiation of the power series was found to be the most suitable for the interaction parameter calculations. Comparison of the calculated self-interaction parameters with values obtained from thermodynamic measurements indicates that the Wagner self-interaction parameter can be successfully calculated from binary phase diagrams.

The crystal and molecular structures of the following organophosphorus (OP) insecticides have been determined by three-dimensional X-ray analysis: ronnel (0,0-dimethyl 0-2,4,5 trichlorophenyl phosphorothioate), ronnel oxon (0,0-dimethyl 0-2,4,5 trichlorophenyl phosphate), bomophos (0-(4-bromo-2,5-dichlorophenyl) 0,0-dimethyl phosphorothioate), Ruelene (0-(4-tert-Butyl-2-chlorophenyl)-0-methyl-N-methyl phosphoroamidate), fospirate (0,0-dimethyl 0-3,5,6-trichloro-2-pyridyl phosphate) and chlorpyrifos (0,0-diethyl 0-3,5,6-trichloro-2-pyridyl phosphorothioate). Phosphorus to meta hydrogen distances for the respective compounds are: 5.51, 5.49, 5.42, (5.68, 5.13), 5.79 and 5.78 A. All of these distances fall well within the range of literature values cited for the intramolecular active site-separation distance for insect acetylcholinesterase (AChE), yet are well outside that for mammalian AChE. In addition the crystal structure of ronnel displays a hydrogen-sulfur intermolecular interaction in the b direction and a phosphorus which is readily accessible for phosphorylation of AChE. The structure of ronnel oxon is quite similar to that of ronnel. CNDO 11 molecular orbital calculations are presented to show the charge distribution in the compound. A likely intramolecular hydrogen bond in bromophos restricts rotation about the phenolic C-O bond. The configuration of Ruelene is substantiated by CNDO 11 molecular orbital calculations and van der Waals arguments and features a possible weak intramolecular hydrogen bond which somewhat restricts rotation about the phenolic C-O bond. Charge density information …

The proton NMR in powdered samples of H/sub 2/O(s), H/sub 2/S(s), and C/sub 6/H/sub 6/(s) have been studied by multiple pulse line narrowing techniques. The resultant spectra provide nuclear magnetic shielding tensors that are (at least approximately) axially symmetric. The anisotropy is 34.2 +- 1.0 ppM for ice, 11.1 +- 1.0 ppM for the highest-temperature phase of solid hydrogen sulfide, and -5.3 +- 0.3 for benzene. Comparisons are made with previous experimental and theoretical work.