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By L. F. Heising

The Bureau of Mines evaluated 191 composites from the central Mesabi Range, Minn., chiefly by reductive roasting and magnetic separation. After reductive roasting and magnetic separation at minus 325 mesh, 28 composites produced concentrates that contained an average of 66.0 percent iron with less than 10 percent silica. Recovery of contained iron was over 90 percent. Natural magnetic material in excess of 5 percent was present in 142 composites. Trial flotation tests were used to evaluate three samples unresponsive to reductive roasting and magnetic separation procedures, and satisfactory concentrates having low silica contents (averaging 6.6 percent) were achieved.

Jan 1, 1965

By Jack I. Paige

The devitrification of lithium silicate glasses was studied to determine the effect of annealing temperature, composition, and additives on nucleation and crystallization. High-purity glasses, prepared from reagent-grade chemicals, had close to optical quality when prepared by a vacuum induction melting method developed during this research, The progress of devitrification was traced by differential thermal analysis and thermal expansion for those lithium metasilicate-silica compositions containing 80 to 90 percent silica. Microscopic studies of glasses partially devitrified at various temperatures and annealing times indicated that the primary initial mode of formation of individual crystals ,vas from densely crystalline zones that filled in as crystallization advanced Of the additives tested, calcium, potassium, and sodium helped promote devitrification with the least cracking or surface deformation. Tin oxide was most effective in reducing volume contrast ion during devitrification, but was not ClS effective in preventing cracking as calcium or potassium additions.

Jan 1, 1965

By Joseph A. Cavallaro

This report describes the timed release analysis technique that was developed to serve as a tool for assessing the froth flotation cleaning potentials of fine-size coals. Using this developed technique, 16 coals from 10 different coalbeds were tested. All of the coals included in this study were quite amenable to froth flotation with float coal yields ranging from 80.7 to 99.5 percentage points. Float-and-sink analyses of the coals tested are shown to be of limited value in predicting froth flotation cleaning potential. Generally the float-and-sink analyses indicated a better product could be obtained than froth flotation could provide; although, in four of the coals tested froth flotation results were superior to those expected from the gravimetric analysis. The fixed carbon content of the samples collected was found to correlate with the floatability of the coals. The higher rank coals were the most readily floatable coals while the lower rank coals did not respond quite as well to flotation.

Jan 1, 1965

By Stephen Utter

Stresses induced by block-caving mining were estimated from in-place measurements of strain or deformation in rock and concrete around mine openings. The four types of gages used for measurements in the Climax Molybdenum mine during 1959-61 were Whittemore gage, Carlson strain meter,2 Valore strain cell, and Climax extensometer. Gage performance in the laboratory was evaluated by stressing instrumented rock and concrete specimens in a universal testing machine and by comparing measurements taken by the gages and a standard gage. Gage performance in the mine was evaluated by comparing measurements taken during an 18-month test. The Whittemore gage, Carlson strain meter, and the Climax extensometer proved suitable for the investigation; the Valore strain cell, effective in the laboratory tests, gave erratic measurements in the mine.

Jan 1, 1965

By J. M. Kuchta

Experimental data are presented on the autoignition temperature (AIT) characteristics of the hydrocarbon jet fuel, JP-6, in various oxygen-nitrogen atmospheres under conditions of constant volume and constant pressure. AIT's of this fuel in air varied little with fuel injection pressure but increased greatly with decreasing fuel content at low fuel-air-ratios. They also increased with decreasing oxygen content of the fuel vapor-oxidant atmosphere. Consistent with thermal ignition theory, the ignition temperatures increased with decreasing initial pressure, ignition delay, and vessel radius; expressions are given which define the observed variation of AIT with these variables for JP-6 fuel vapor-air mixtures. The significance of autoignition temperature data obtained using various ignition criteria is discussed to show the usefulness of such data in evaluating fire and explosion hazards. In addition, data are presented on the extent of oxidation that occurs prior to autoignition of this fuel in air at various temperatures.

Jan 1, 1965

By C. O. Hawk

Distillable oils derived from coal were desulfurized and hydrogenated at 2,500 psig in a two-step vapor-phase catalytic operation to give a product rich in saturated cyclic hydrocarbons. The first step was mainly a desulfurization at 400 C, the second a saturation at 300 C. One of the oils used as feed stock was from low-temperature carbonization of a bituminous coal, the other was from the liquid-phase hydrogenation of coal in the Bureau's pilot plant. The product from the saturation step was distilled to remove the light ends and high-boiling residue and to recover a fraction having acceptable properties with respect to heating value, density, freezing point, viscosity, and boiling range according to specifications suggested by the Air Force for ultra-high-speed aircraft fuel. Quantities of the fuel fraction available were too small for the thermal stability test approved by the Air Force. The experiments, performed on laboratory scale, comprised mostly a study of the effect of varying the oil feed rate (at constant oil-to-hydrogen ratio) on the yield of the desired fuel fraction. The yield of the fuel fraction made from low-temperature carbonization oil was a little more than 1 percent of the weight of coal carbonized; that from coal-hydrogenation oil was about 12 percent of the weight of coal hydrogenated. A few attempts to do both desulfurization and saturation in one operation with sulfur resistant catalysts, developed for vapor-phase hydrogenation or hydroforming, were unsuccessful. By leaving the low-boiling ends in both feed stocks to desulfurization, another product was obtained: a low-sulfur aromatic cut boiling below 200 C. This material would be suitable as a solvent or a chemical raw material.

Jan 1, 1965

By K. C. Dean

This report is the first of a series concerned with processes for producing magnesium. These reports will evaluate metallothermic, carbothermic , and electrolytic production methods, and will furnish a cost basis for comparing the processes. Areas deemed most promising for future research will be delineated for each procedure. This report presents briefly the history of the metallothermic process, and describes the operations of the Defense Plant Corp. (DPC) plants that employed the process. A hypothetical plant designed to produce 12,000 tons of magnesium per year, using ferrosilicon as a reductant, is described, and raw materials, energy, and major equipment requirements are estimated. Several process modifications are suggested for future research.

Jan 1, 1965

By Jerry W. Ramsey

The Bureau of Mines examined a low-, a medium-, and a high-volatile Pennsylvania anthracite by densimetric methods using four mesh si.s of each anthracite. Using high-pressure mercury the macropore volumes and distributions of these pore volumes determined, densities in mercury were calculated, and specific pore vo1.r. ware obtained from these mercury densities in conjunction with helium densities. The helium densities were also used with the ultimate analyses of these anthracites in calculating structural parameters by statistical densimetric methods. The effect of 106 or 108 rads of gamma irradiation in the presence of air and in vacuum upon the properties studied with two mesh sizes of each anthracite. Results of the statistical densimetric method seem to show some breakdown of condensed ring structural units at the lower irradiation level, with subsequent polymerization at the longer period of gamma irradiation. The structural parameters obtained also indicated that in going from high- to low-volatile anthracite, either the number of condensed rings per structural unit increased, or the degree of polymerization increased.

Jan 1, 1965

By G. L. Gates

The Bureau of Mines studied the scales formed in producing wells in the Wilmington field, California. The scales were primarily barium sulfate and resulted from the mixing of injected sea water and formation waters; there was excess sulfate in the injection water and the formation waters contained appreciable barium. After breakthrough, the produced brines were supersaturated with barium sulfate. Laboratory tests indicated that barium sulfate precipitated quickly When the supersaturated brines were agitated with crystals of barium sulfate and fairly rapidly when more sulfate solution was added. Precipitation occurred slowly on standing or under nonturbulent conditions. Both the apparent and equilibrium solubilities of barium sulfate in these brines were determined and compared with equilibrium solubilities in distilled water and sodium chloride solutions.

Jan 1, 1965

By J. L. Eakin

The Bureau of Mines determined agents that are effective in foaming heavy brines and oil from gas wells in severe concentrations of sodium chloride, in severe concentrations of calcium chloride, or in moderate oil-brine mixtures. Dynamic foam tests were designed to select the more effective foaming agents. Numerous foaming agents were tested in concentrated simulated brines, in oilfield brines having varied concentrations of ions, in heavy natural brines, and in a commercial brine generally used as a reservoir pressure-balancing fluid. Several agents were detected that could perform efficiently in the field under the most severe saline conditions. Agents that promote foaming in oil-brine mixtures were also determined.

Jan 1, 1965

By A. R. Taylor Jr.

The heat capacities of a-quartz form beryllium fluoride were measured at approximately 3° intervals from 8° to 300° K., using an adiabatic calorimeter. At 298.15° K the heat capacity and entropy were 12.39 cal/deg mole and 12.75 ±0.04 eu respectively. Enthalpy measurements were made with an ice calorimeter at approximately 30° intervals on the quartz and glassy forms of beryllium fluoride between 300° and 1,200° K. A melting point of 825° K and an 0,-8 type transition at 500° K with a heat effect of 75 ca1/mole were deter-mined from the enthalpy data for the quartz-type sample. Beryllium fluoride glass crystallized spontaneously into the quartz modification at 500° K. The heat of the reaction BeF2 (a-quartz) .... BeF2 (glass) was found to be 1,125 ±16 cal/mole at 298° K by solution calorimetry. This value, when corrected to 273° K, was used to correct for the heat absorbed by the formation of glassy BeF2 when the sample was dropped into the ice calorimeter from temperatures above the melting point. Using corrected enthalpy measurements, the heat of fusion was determined to be 1.13 kcal/mole at 825° K.

Jan 1, 1965

By Albert W. Deurbrouck

This report describes the preparation characteristics of 23 coal samples collected from nine of the more significant coalbeds of Fayette County, W. Va. In 1963 almost 5.4 million tons of medium to high volatile B coals of excellent quality for metallurgical and steam markets were produced in Fayette County. Of the 23 coal samples collected 11 would require some upgrading to pro-vide metallurgical quality products, 11 were acceptable as received, and 1 was a noncaking coal. Cleaning these coals to metallurgical standards would require only the removal of the sink 1.58 specific gravity material which would be quite easy as very little near-separating-gravity material was present at this gravity.

Jan 1, 1965

By R. L. Solmer

During 1959-61, the Bureau of Mines investigated the strain and deformation induced in rock and concrete linings around mine openings by retreat panel caving at the Climax Molybdenum mine. Two concrete-lined slusher drifts on the Phillipson level of the mine were instrumented with both electrical strain gages and extensometers. Changes in strain and deformation were recorded over an 18-month period during the undercutting and caving of the mining panel. General agreement was found between the strain and deformation measurements and the hypothesis that the vertical component of the stress field on the openings is almost completely removed by undercutting. This phenomenon is a possible explanation for the structural failures that occur in the slusher drifts during the undercutting cycle.

Jan 1, 1965

By Robert C. Johnson

Single crystal whiskers of ZrO2 and TiO2 were grown by solution and crystallization of these oxides in molten baths. Mixtures of Na2B407 and LiC1 were the most suitable growth media for zirconia. Sodium borate alone and Na2CO3 plus SiO2 were best suited for titania. The solubilities of zirconia and titania in molten sodium borate were determined, Whether zirconia whiskers were dendritic or nondendritic depended on the temperature used. The best single crystal whiskers were grown below 1,100° C. Titania whiskers always grew as single crystals. The tensile strengths of zirconia and titania whiskers were about 15,000 psi and 50,000 psi, respectively. Modulus of rupture was about 49,000 psi for zirconia whiskers and 75,000 psi for titania whiskers. Chemical analyses showed the zirconia and titania whiskers to be pure. The zirconia and titania whiskers were shown by X-ray analysis to be, respectively, baddeleyite and rutile.

Jan 1, 1965

By James S. Browning

The Bureau of Mines conducted laboratory batch and pilot plant flotation tests to determine the technical feasibility of recovering commercial-grade mica from a California micaceous schist. Best results in the laboratory batch tests were obtained using sodium carbonate and sodium silicate for pH control and quartz depression, and a combination of fatty acid and cationic reagents as the mica collector. In continuous pilot plant flotation tests, an alkaline fatty acid-cationic method recovered about 70 percent of the mica in a concentrate analyzing 95.6 percent mica.

Jan 1, 1965

By W. W. Weller

Heat capacity measurements of anhydrous cobalt sulfate (CoSO4), copper sulfate (CuSO4), nickel sulfate (NiSO4), and zinc sulfate (ZnSO4) were conducted over the temperature range 51° to 298° K. The results were used to evaluate the following entropies at 298.15° K (cal/deg mole): CoSO4, 28.1; CuSO4, 26.8; NiSO4, 24.8; and ZnSO4, 26.4. Entropies were combined with heats of formation to give free energies of formation.

Jan 1, 1965

By G. E. Rennick

A siphon-type laboratory airlift well was designed and operated by the Bureau of Mines to study the concurrent flow of air and oil in small-diameter pipes. Glass flowstrings ranging from to 1 inch in diameter and from L4 to 64 feet in length were equipped with various-sized air-entry jets. Liquid holdup volumes were used to correlate vertical-flow data, and empirical equations for computing gas requirements were derived. The effect of flowstring length on flow efficiency, oil- and gas-production rates, and gas-oil ratios was relatively minor at all flowing pressures. Air-jet sizes and flowstring diameters, however, had a marked effect on flow efficiency and oil- and gas-production rates. The small air-jet sizes increased maximum flow efficiency and its associated flowing pressures but decreased oil- and gas-production rates. An increase in flowstring diameter increased maximum flow efficiency with its associated flowing pressure and also increased the production rates of oil and gas.

Jan 1, 1965

By Norman G. Foster

The mass spectra of 14 previously unreported alkylthiophenes are pre-sented. Low ionization voltage data of selected compounds from these 14 and 23 previously reported alkylthiophenes are presented and discussed for their value in supporting fragmentation mechanisms analytical correlations. A comparison with and corroboration of earlier correlations is made. Additional correlations concerning detection of side chain branching and the detection of ethyl-alkyl and propyl-alkylthiophenes are made. A discussion of the possible fragmentation routes and mechanism of fragmentation is given. Speculative structures are inferred s out some of the ions and hence this work provides a basis for suggesting fation mechanisms for the alkylthiophenes according to modern theories ass spectrometry. Verification of these mechanisms must await the availability of isotopically labeled molecules which are labeled in specific lotions that permit the definition of the paths of frag-mentation. Some suggestions for further work to generalize on the correlations and studies made to this point are presented.

Jan 1, 1965

By Jr. Smith

The equilibrium compositions of product gases for mixtures of air with methane, propane, or ethylene at and around flame temperatures are reported. For each hydrocarbon, compositions are given for five fuel-to-air ratios--two lean, two rich, and one stoichiometric--at five pressures, from 1 to 20 atmospheres, and at an ambient temperature of 25° C.

Jan 1, 1965

By R. L. Crosby

A part of the liquidus of the magnesium-zirconium system was determined by chemical analysis of suction samples taken from the melt in the approximate temperature range of 850° to 1,450° C. The melt was prepared in a furnace pressurized with an inert gas. The average zirconium value in weight-percent of the liquidus composition at each sampling temperature was 0.96 at 867° C, 1.40 at 1,062° C, 2.05 at 1,262° C, and 2.96 at 1,402° C. The equilibrium solid phase was zirconium.

Jan 1, 1965