Surface Tension of Calcium Aluminosilicate Glass Using Computerized Drop Shape Analysis

Numerical analysis is used in this study to derive surface tension from the shape of a liquid silicate sessile drop. The speed afforded by the drop shape analysis package facilitates analysis of experimentally derived drop profiles. Drop symmetry, contact angles, and local shape variations can be readily determined, thereby permitting the detection of experimental errors. The experimental and analytical technique was first validated by determining the surface tension of high-purity gallium and aluminum under carefully controlled furnace atmospheres. Results for a calcium aluminosilicate melt are compared to pendant drop and maximum-bubble pressure measurements reported in the literature. The use of an internal scaling factor and the effect of substrate interactions are discussed.     

Suitability of commercial cottonseed for producing edible high protein flours by liquid classification

The 1976 and 1977 crops of glanded cottonseed from oil mills located in 7 major U.S. cottonbelt growing areas were evaluated as to their suitability for processing into edible, high-protein flours. Both the physical and chemical characteristics of fuzzy seed samples were studied. Ginned seed samples were hulled, dried, comminuted, slurried with hexane and liquid classified by both a laboratory differential settling test (DST) and pilot plant liquid cyclone process (LCP). Liquid cyclone operating data and extensive analytical data of the kernels, flour and meals produced are shown. A free gossypol level of 1.10% or less in full fat kernels was the determining factor for producing edible flours from glanded seed by the LCP. The Lower Rio Grande Valley area was the only area from which liquid classified cottonseed flour consistently exceeded the current maximal free gossypol standard of 450 ppm. Ca. 94% of the total U.S. cottonseed production is suitable for producing edible, high-protein flours by liquid classification.     

High-Thermal-Conductivity Aluminum Nitride Ceramics: The Effect of Thermodynamic, Kinetic, and Microstructural Factors

Improvement in the thermal conductivity of aluminum nitride (AlN) can be realized by additives that have a high thermodynamic affinity toward alumina (Al₂O₃), as is clearly demonstrated in the aluminum nitride-yttria (AlN-Y₂O₃) system. A wide variety of lanthanide dopants are compared at equimolar lanthanide oxide:alumina (Ln₂O₃: Al₂O₃, where Ln is a lanthanide element) ratios, with samaria (Sm₂O₃) and lutetia (Lu₂O₃) being the dopants that give the highest- and lowest-thermal-conductivity AlN composites, respectively. The choice of the sintering aid and the dopant level is much more important than the microstructure that evolves during sintering. A contiguous AlN phase provides rapid heat conduction paths, even at short sintering times. AlN contiguity decreases slightly as the annealing times increase in the range of 1–1000 min at 1850°C. However, a substantial increase in thermal conductivity results, because of purification of AlN grains by dissolution-reprecipitation and bulk diffusion. Removal of grain-boundary phases, with a concurrent increase in AlN contiguity, occurs at high annealing temperatures or at long times and is a natural consequence of high dihedral angles (poor wetting) in liquidphase-sintered AlN ceramics.     

Alumina-, niobia-, and niobia/alumina-supported NiMoS catalysts: Surface properties and activities in the hydrodesulfurization of thiophene and hydrodenitrogenation of 2,6-dimethylaniline

The activity of NiMoS catalysts supported on niobia, alumina, and niobia/alumina was compared for the thiophene hydrodesulfurization (HDS) and 2,6-dimethylaniline (2,6-DMA) hydrodenitrogenation (HDN) reactions. To evaluate the acidity of the supports and identify the nature of the sulfide sites, adsorption of 2,6-dimethylpyridine, pyridine, and CO was performed and followed by IR spectroscopy. This study has shown that with niobia as a support, the activity of NiMoS catalysts in thiophene HDS and in HDN of 2,6-DMA was no longer promoted by the synergy between Ni and Mo. The absence of synergy between molybdenum and nickel on niobia can be explained by the strong interaction of each metal with niobia at the expense of interaction with each other. Moreover, it has been shown that on a niobia/alumina support, the formation of the NiMoS phase can be directly linked to the presence of alumina not covered by niobia. However, niobia is an interesting support for the HDN of 2,6-DMA, because it favors the formation of xylene through direct ammonia elimination involving low H₂ consumption. The activity for xylene formation on niobia is linked to the electron-deficient nature of the Mo sulfide site, as demonstrated by CO adsorption followed by IR.     

Quantitative preparation of long chain thioethers from an oxo-trans-2-enoic ester and a 9,12-dioxo-trans-10-enoic acid

Branched-chain thioethers have been prepared from methyl 4-oxo-trans-2-hexadecenoate and 9,12-dioxo-trans-10-octadecenoic acid. The reagents involved in these preparations were mercaptoacetic and mercaptopropionic acids. The yields of these thioethers are almost quantitative.     

Separation and identification of phenolic acids and related compounds by gas chromatography and fourier transform infrared spectroscopy

Phenolic acids and related compounds were separated by gas chromatography using three separate columns. One of these columns was coupled to a Fourier transform infrared spectrometer. The trimethylsilyl derivatives could be separated and identified by comparing the relative retention times of the three different columns. However, where there was overlap, the accompanying infrared data clearly distinguished between the questionable derivatives, thus enabling characterization of all derivatives.The use of trade, firm, or corporation names in this article is for the information and convenience of the reader. Such use does not constitute an official endorsement or approval by the U.S. Department of Agriculture or the Forest Service of any product or service to the exclusion of others that may be suitable.     

Mixed-Mode Fracture in Soda-Lime Glass Using Indentation Flaws

Mixed-mode failure of soda-lime glass under inert and fatigue test conditions was studied using Knoop indentation flaws. For annealed cracks (residual stress-free) crack extension (catastrophic or subcritical) is by an abrupt transition from the initial crack plane to a noncoplanar crack plane followed by a reorientation of the crack normal to the applied stress. Although fatigue strength of these inclined flaws increased linearly with respect to orientation of the flaws to the applied stress up to an angle of 60°, this increase was considerably less than what was predicted by existing theories. It is believed that subcritical crack growth causes the crack to be realigned perpendicular to the applied stress before failure for all orientations; hence, fatigue strength does not show the dramatic increase at orientation angles as predicted by theory. For as-indented cracks the contact residual stress causes the crack extension to be less inclined to the initial crack plane than for annealed cracks, but in this case also, the crack realigns itself perpendicular to the applied stress. Again, fatigue strength is relatively insensitive to the orientation angle as predicted by theory and subcritical crack growth is believed to play a primary role in determining this strength dependency.     

Synthesis and Microstructure of Highly Oriented Lead Titanate Thin Films Prepared by a Sol-Gel Method

Thin films of PbTiO₃ were deposited on fused silica, resistor-grade alumina, and single-crystal (100) MgO by a sol–gel processing method. Whereas the films deposited on silica and alumina substrates were randomly oriented and polycrystalline, highly {100} oriented PbTiO₃ films were grown on the MgO single crystals. The perovskite-type structure was observed with films deposited on the single-crystal MgO and annealed at temperatures as low as 470°C, whereas a pyrochlore-type strcuture was observed with films on fused silica and alumina processed in a similar manner. All films heat-treated at temperatures in excess of 570°C showed significant formation of a second PbTi₃O₇ phase. The films were characterized by electron microscopy and glancing-incidence-angle X-ray diffraction.     

The Thermodynamic Properties of Silicon Oxynitride

A critical assessment of thermal and equilibrium data for silicon oxynitride (Si₂N₂O) is presented. Selected values for the heat of formation of Si₂N₂O from the elements and the absolute entropy of Si₂N₂O at 298.15 K are ΔH⁰_f,298=−947.7 ± 5.4 kJ/mol and S⁰₂₉₈= 45.35 ± 0.4 J/mol·K, respectively. A table of thermodynamic functions for Si₂N₂Ofrom 298 to 2500 K, which has been calculated from the analysis of the literature data, is also presented.     

Production of human normal adult and fetal hemoglobins in Escherichia coli

A hemoglobin expression system in Escherichia coli is described. In order to produce authentic human hemoglobin, we need to co-express both methionine aminopeptidase and globin genes under the control of a strong promoter. We have constructed three plasmids, pHE2, pHE4 and pHE7, for the expression of human normal adult hemoglobin and a plasmid, pHE9, for the expression of human fetal hemoglobin, in high yields. The globin genes can be derived from either synthetic genes or human globin cDNAs. The extra amino-terminal methionine residues of the expressed globins can be removed by the co-expressed methionine aminopeptidase. The heme is inserted correctly into the expressed alpha- globin from our expression plasmids. A fraction (approximately 25%) of the heme is not inserted correctly into the expressed beta- or gamma- globin. However, the incorrectly inserted hemes can be converted into the correct conformation by carrying out a simple oxidation-reduction process on the purified hemoglobin molecule. We have investigated the functional properties of the expressed hemoglobins by measuring their oxygen-binding properties and their structural features by obtaining their 1H-NMR spectra. Our results show that authentic human normal adult and fetal hemoglobins can be produced from our expression plasmids in E. coli and in high yields. Our expression system allows us to design and to produce any recombinant hemoglobins needed for our research on the structure-function relationship in hemoglobin.