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Description: The purpose of this study was to determine the effect of gamma radiation on the direct sulfochlorination of hydrocarbons and nitrobenzene. The radiation source consisted of spent uranium fuel elements, providing a gamma radiation intensity up to 2.5 x 10/sup 6/ roentgen/ hour. The sulfochloriuation studies were carried out either with SO/sub 2/Cl/sub 2/ or with gaseous mixtures of SO/ sub 2/ aud Cl/sub 2/. Attempts to sulfuochlorinate nitrobenzene and benzene were unsuccessful. There was no detectable reaction in the case of nitrobenzene, while the reaction with benzene produced only chlorinated products, up to the full addition product 1,2,3,4,5,6-hexachlorocyclohexane. Liquid cyclohexane reacted with SO/sub 2/ and Cl/sub 2/ in the presence of gamma radiation to give very high yields of cyclohexanesullonyl chloride, and to a smaller extent chlorocyclohexane and cyclohexanedisulfonyl chloride. The leugth of the chemical chain reaction induced by gamma radiation was estimated at over 2 x 10/sup 5/, and the radiochemical yield G was greater than 10/sup 6/. Sulfochlorination was the predominant reaction but at lower radiation intensities and for SO/sub 2/Cl/ sub 2/ ratios lower than unity, chlorination was found to exceed sulfochlorinatiou. Within a temperature range of 11.5 to 40.0 deg C, the selectivity of the reaction was independent of temperature. For a total gas flow rate of 1.9 l/min per liter C/sub 6/H/sub 12/ and SO/sub 2/Cl/sub 2/ ratios of 2/ 1, the rate of conver sion to C/sub 6/H/sub 11/SO/sub 2/Cl was proportional to the square root of the absorbed radiation dose up to a dose rate of 40 rad/min, but became independent of dose rate above 400 rad/min. Under these conditions, the conversion rate was 0.025 g-moles C/sub 6/H/sub 11/SO/sub 2/Cl/ (l) (min). A basic plant design was developed for the contiuuous sulfo chlorination of cyclohexame initiated by gamma radiation. Tbe economics of ...
Date: June 1, 1958
Creator: Schneider, A.
Partner: UNT Libraries Government Documents Department

Hexone Extraction-Coulometric Titration of Uranium

Description: Samples containing 5 to 10 mg of uranium were extracted with hexone (methyl isobutyl ketone) and titrated coulometrically in sulfate media. Relative standard deviations of 0.43% for samples containing 5 mg and 0.56% for 10 mg were determined by precision studies. (auth)
Date: June 22, 1959
Creator: Blevins, E. L.
Partner: UNT Libraries Government Documents Department

Solution Effects on Cesium Complexation with Calixarene - Crown Ethers from Liquid to Supercritical Fluids

Description: Supercritical fluid CO2 is an alternative solvent for extraction of metals. The solubility parameter of supercritical CO2 varies with density resembling that of liquid hexane at moderate pressures in the supercritical region to those of chlorinated solvents at very high pressures. By changing density of supercritical CO2, the solvation environment of a metal chelate system can vary continuously and resembles over a wide range of solvents. Thus, supercritical CO2 provides a unique system for studying solvation effects on metal chelation. This project is designed to investigate the solvation effects on cesium complexation with macrocyclic compounds including crown ethers and calixarene-crown ethers in CO2 from liquid to supercritical region at high pressures. A powerful spectroscopic technique for studying cesium chelation is nuclear magnetic resonance (NMR). Cesium has only one isotope, 133Cs, with a nuclear spin I = 7/2. Popov et al. used NMR to study cesium complexation with crown ethers and cryptand.
Date: June 1, 1999
Creator: Wai, Chien M. & Yonker, Clem
Partner: UNT Libraries Government Documents Department

Separation of Fischer-Tropsch wax from catalyst using supercritical fluid extraction. Quarterly technical progress report, 1 October 1995--31 December 1995

Description: The objective of this research project is to evaluate the potential of supercritical fluid (SCF) extraction for separating the catalyst slurry of a Fischer-Tropsch slurry bubble column (SBC) reactor into two fractions: (1) a catalyst-free wax containing less than 10 ppm particulate matter and (2) a concentrated catalyst slurry that is ready for recycle or regeneration. The wax will be extracted with a hydrocarbon solvent that has a critical temperature near the operating temperature of the SBC reactor, i.e., 200-300{degrees}C. Initial work is being performed using n-hexane as the solvent. During the reporting period, work on the small-scale, continuous-flow apparatus continued. Initial experiments have been performed on a binary mixture of n-hexane (solvent) and squalane (model compound) at 200{degrees}C. A total of fifteen samples were collected at 135, 160, and 208 psig, with pressures being controlled to within {plus_minus}2 psi. Results indicate that the equilibrium phase compositions can in principle be measured to a reproducibility of {plus_minus}0.5% in the squalane-rich bottomphase and {plus_minus}2% in the hexane-rich top phase, with respect to the minor component. However, other data measured at these same conditions at another time exhibited scatter that was as much as 5 times greater. We believe that improvements in (1) the method of preheating the feed to the view cell/phase separator and to (2) the sample collection technique are required before data of high accuracy can consistently be generated. The apparatus modifications required to effect these improvements are currently underway and should be completed by the middle of February.
Date: June 1, 1996
Creator: Thies, M.C. & Joyce, P.C.
Partner: UNT Libraries Government Documents Department

Fischer Tropsch synthesis in supercritical fluids. Quarterly technical progress report, October 1--December 31, 1995

Description: Objectives for this quarter were to attempt to develop a model to predict the molecular diffusion coefficients to a high degree of accuracy so the authors may be able to predict both the molecular diffusion coefficient and thus the effective diffusivity a priori. They are working on a semi-empirical equation based on the rough hard sphere theory to predict diffusion coefficients in supercritical fluids. In addition, they planned to take additional data in order to extend the database available for development of the predictive equation. The paper discusses accomplishments and problems related to the diffusion coefficients of F-T products in supercritical fluids. Data are presented on the diffusion coefficients of 1-octene in ethane, propane, and hexane.
Date: June 1, 1996
Creator: Akgerman, A. & Bukur, D.B.
Partner: UNT Libraries Government Documents Department

Autoignition chemistry of the hexane isomers: An experimental and kinetic modeling study

Description: Autoignition of the five distinct isomers of hexane is studied experimentally under motored engine conditions and computationally using a detailed chemical kinetic reaction mechanism. Computed and experimental results are compared and used to help understand the chemical factors leading to engine knock in spark-ignited engines and the molecular structure factors contributing to octane rating for hydrocarbon fuels. The kinetic model reproduces observed variations in critical compression ratio with fuel structure, and it also provides intermediate and final product species concentrations in very dose agreement with observed results. In addition, the computed results provide insights into the kinetic origins of fuel octane sensitive.
Date: June 1, 1995
Creator: Curran, H.J.; Gaffuri, P.; Pitz, W.J.; Westbrook, C.K. & Leppard, W.R.
Partner: UNT Libraries Government Documents Department

A study of stability of tungstophosphoric acid, H{sub 3}PW{sub 12}O{sub 40}, using synchrotron XPS, XANES, Hexane cracking, XRD and IR spectroscopy

Description: Tungstophosphoric Acid (HPW) has been investigated using different spectroscopic and chemical techniques. Bulk sensitive techniques such as x-ray diffract ion (XRD) and infrared (IR) spectroscopy indicate that the acid is stable at temperatures as high as 300 degrees C or higher. However, our work suggests that HPW starts loosing stability at temperature as low as 200 degrees C. For instance, P 2p peak was not detected in the XPS spectrum of HPW preheated at 100 degrees C, but was clearly observed after preheating the acid at 200 degrees C and 400 degrees C. This suggests the destruction of the molecules of the surface leading to the enrichment of surface with phosphorus. These results may explain why HPW deactivates very fast, e.g., 8 min at 200 degrees C, in hexane cracking experiments. This could limit the use of HPW in surface reactions that even require moderate temperatures. Detailed infrared spectroscopic investigation of the HPW as a function of temperature showed a gradual in crease in absorbance of the W-O-W corner shared vibration relative to the absorbance of the other bands. This indicates that the symmetry, and hence the stability, of the molecule was decreased upon heating.
Date: June 7, 2002
Creator: Jalil, Pasl A.; Faiz, M.; Tabet, N.; Hamdan, N.M. & Hussain, Z.
Partner: UNT Libraries Government Documents Department

Sensing liquid properties with shear-mode resonator sensors

Description: Liquid properties are measured from the changes they induce in the resonant frequency and damping of thicknessshear mode quartz resonators. A smooth-surfaced resonator viscously entrains the contacting fluid and responds to the density-viscosity product. Separation of density and viscosity is accomplished using two devices: one with a smooth surface and one with a corrugated surface that traps fluid. By observing the difference in stored and dissipated energies in the contacting fluid, its non-Newtonian characteristics can also be determined.
Date: June 1, 1995
Creator: Martin, S.J.; Cernosek, R.W. & Spates, J.J.
Partner: UNT Libraries Government Documents Department

Measurement and prediction of aromatic solute distribution coefficients for aqueous-organic solvent systems. Final report

Description: Experimental and modeling activities were performed to assess techniques for measurement and prediction of distribution coefficients for aromatic solutes between water and immiscible organic solvents. Experiments were performed to measure distribution coefficients in both clean water and wastewater systems, and to assess treatment of a wastewater by solvent extraction. The theoretical portions of this investigation were directed towards development of techniques for prediction of solute-solvent/water distribution coefficients. Experiments were performed to assess treatment of a phenolic-laden coal conversion wastewater by solvent extraction. The results showed that solvent extraction for recovery of phenolic material offered several wastewater processing advantages. Distribution coefficients were measured in clean water and wastewater systems for aromatic solutes of varying functionality with different solvent types. It was found that distribution coefficients for these compounds in clean water systems were not statistically different from distribution coefficients determined in a complex coal conversion process wastewater. These and other aromatic solute distribution coefficient data were employed for evaluation of modeling techniques for prediction of solute-solvent/water distribution coefficients. Eight solvents were selected in order to represent various chemical classes: toluene and benzene (aromatics), hexane and heptane (alkanes), n-octanol (alcohols), n-butyl acetate (esters), diisopropyl ether (ethers), and methylisobutyl ketone (ketones). The aromatic solutes included: nonpolar compounds such as benzene, toluene and naphthalene, phenolic compounds such as phenol, cresol and catechol, nitrogenous aromatics such as aniline, pyridine and aminonaphthalene, and other aromatic solutes such as naphthol, quinolinol and halogenated compounds. 100 references, 20 figures, 34 tables.
Date: June 1, 1984
Creator: Campbell, J.R. & Luthy, R.G.
Partner: UNT Libraries Government Documents Department

Geothermal direct-contact heat exchange. Final report

Description: A glass direct contact heat exchange column was operated in the laboratory at atmospheric pressure using hot water and normal hexane. Column internals tested included an empty column, sieve trays, disk-and-doughnut trays, and two types of packing. Operation was very smooth in all cases and the minimum temperature approaches varied from less than 1{sup 0}C for packing to 13{sup 0}C for the empty column. High heat transfer rates were obtained in all cases, however, columns should be sized on the basis of liquid and vapor traffic. The solubilities of hydrocarbons were determined for normal hexane, pentane and butane in water and sodium chloride and calcium chloride brines at various temperatures. The values seem to be internally consistent and salt content was found to depress hydrocabon solubility. Laboratory stripping tests showed that gas stripping can be used to remove hydrocarbon from reject hot water from the direct contact heat exchange column. Although the gas volumes required are small, stripping gas requirements cannot be accurately predicted without testing. A computer program was used to study the effect of operating variables on thermodynamic cycle efficiencies. Optimum efficiencies for the moderate brine conditions studied were obtained with isopentane as working fluid and relatively low operating pressure. A preliminary design for a 50 MWe plant was prepared and plant capital cost and operating cost were estimated. These costs were combined with previously developed brine production and power transmission costs to provide an estimate of the cost of delivered power for a geothermal field at Heber, California. A pilot plant program is described that would be suitable for continuing the investigation of the direct contact process in the field. The program includes a suggested schedule and the estimated cost.
Date: June 10, 1976
Creator: Sims, A.V.
Partner: UNT Libraries Government Documents Department

NMR studies of molecules in liquid crystals and graphite

Description: NMR experiments to measure proton dipole couplings were performed on a series of n-alkanes (n-hexane through n-decane) dissolved in nematic liquid crystals. Computer modeling of the experimental NMR-spectra was done using several different models for intermolecular interactions in these systems. The model of Photinos et al. was found to be best in describing the intermolecular interactions in these systems and can provide a statistical picture of the conformation and orientation of the alkane molecules in their partially-oriented environment. Order parameters and conformational distributions for the alkanes can be calculated from the modeling. The alkanes are found to have conformational distributions very much like those found in liquid alkanes. Proton NMR spectra of tetrahydrofuran (THF) intercalated in two graphite intercalation compounds were also measured. Computer simulations of these spectra provide a picture of THF in the constrained environment between the graphene layers where the THF is oriented at a particular angle, can translate and rotate freely, but does not appear to pseudorotate.
Date: June 1, 1992
Creator: Rosen, M. E.
Partner: UNT Libraries Government Documents Department