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By C. I. Pierce

This report describes and presents results of a phase of a laboratory study conducted at the Morgantown Petroleum Research Laboratory, Federal Bureau of Mines, Morgantown, W. Va., to determine the response of shielded electrodes of different dimensions in thin, noninvaded beds and to stimulate interest in the use of focused-type logging devices in the Appalachian oilfields. A blotter model was used to obtain plots of the potential field in the vicinity of a model shielded electrode. Three plots are presented. The difference in curvature of equipotential lines and the variation in measured resistance values for different blotter-model conditions suggest that the shielded electrode will give resistivities higher than normal when measurements are taken in a thin conductive bed located between resistive beds, and resistivities lower than normal when measurements are taken in a thin resistive bed located between conductive beds.

Jan 1, 1961

By A. L. Engel

This report describes results of laboratory-scale experimental treatment of nine ores containing gold and silver, including samples of products of previous plant treatment, from ore deposits in California and Nevada. The samples treated were taken by engineers of the Bureau of Mines during investigations of these ore deposits. The information reported is of interest for development of the mining districts represented or in future Investigations of similar ores from other sources. The treatment methods were as simple as possible. More complicated treatments were tried when required, The applicability of the methods and their limitations in treating the ores are shown by the data in this report. The following treatment methods were employed in the experiments described: Screen analyses were made to determine distribution of values in various screened-sized portions of crushed ore, or to determine optimum size to which a particular ore should be crushed or ground to liberate values, and some-times to determine residual values in various-sized portions of treated material.

Jan 1, 1961

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1961

By H. F. Yancey

Traditionally the Pacific Northwest has relied on hydroelectric power, which has been both abundant and cheap. However, comparatively few hydroelectric sites capable of providing low-cost power remain, therefore the need for supplemental thermal generation, perhaps within the next decade, is generally recognized. Based on the present cost and availability of competing fuels, coal seems to be the logical choice for projected thermal power plants. Power companies and public utilities have become interested in establishing reserves of coal for future use. One deposit explored in 1958-59 lies in southern Thurston and northern Lewis Counties, Wash., near Centralia. Drilling, totaling 22,700 feet, proved the existence of 70 million tons of strippable coal--an ample reserve for the projected power plant. The coal, like most others and particularly those of Washington and Oregon, when mined in full seam section by mechanical methods, would require cleaning to make it suitable for use. The amount and nature of the impurities in this coal dictated a thorough investigation of its cleaning characteristics to establish economic factors and to insure proper preparation-plant design. Therefore, arrangements were made through a cooperative agreement to conduct such work at the Seattle Coal Research Laboratory of the Bureau of Mines. This report describes that investigation. The results are of interest primarily in connection with the utilization of this particular deposit, but some of the information developed is applicable to other deposits of low-rank coals in the West, because the impurities in these coals differ greatly in behavior from those generally associated with the higher rank coals of the Appalachian field.

Jan 1, 1961

By H. J. Heinen

This report summarizes preliminary research studies by the Bureau of Mines in electrowinning molybdenum directly from pure or impure molybdenum trioxide (MoO3) by fused-bath electrolysis in an open graphite cell without need of a protective inert atmosphere. A formulated electrolyte of the tertiary system containing 41.6 percent sodium pyrophosphate, 16.7 percent sodium tetraborat, 33.3 percent sodium chloride, and 8,4 percent molybdenum trioxide, by weight, electrolyzed at 1,000° C,, gave excellent results. Current density studies were made over a range from 20 to 260 amperes per square decimeter. Current efficiencies of 80 to 90 percent were obtained over the entire range. Yields up to 500 grams of molybdenum per kilowatt-hour were obtained. Higher current densities, however, reduced yields and produced a finer grained metal. The two most important facets in electrowinning molybdenum from MoO3, in an open cell, are temperature and electrode spacing to minimize or eliminate the formation of the suboxide MoO2, the major source of oxygen contamination. At temperatures of 1,000° C. and higher, together with the proper spacing of the electrodes, formation of oxides are practically eliminated. Molybdenum metal electrowon from pure MoO3 was 99.9 percent pure and contained 0,056 percent oxygen and 0,007 percent carbon. This metal, when arc-melted, had a Vickers hardness number of 175 and contained 50 parts per million oxygen and less than 10 parts per million carbon. Molybdenum metal electrowon directly from an impure MoO3 containing 90 percent MoO3 resulted in a metal of 99.8 percent purity.

Jan 1, 1961

By Thomas C. Atchison

The experimental work described in this report is part of a continuing study by the Federal Bureau of Mines of the fundamental physical processes involved in breaking rock with explosives. Six explosives were tested for their strain-producing abilities in a dolomitic marble. The explosives selected for testing had a tenfold variation in detonation pressure and a fivefold variation in characteristic impedance (product of loading density and rate of detonation). Strain pulses produced by the detonation of small charges of the explosives were recorded at distances of 5 to 130 feet. Peak strain, ?, was found to decrease with distance, R, in accordance with an exponential propagation law previously determined for other rock types, namely ? = (K/R)e ?aR The absorption constant, a, did not vary significantly with the explosive and was of the same order of magnitude as that for other rock types. The different explosives produced a fivefold variation in the value of the intercept constant, K.

Jan 1, 1961

By J. W. Davis

The storage stability characteristics of a diesel type fuel were determined to evaluate the effect of the polar compounds in the fuel. These compounds, comprising most of the nitrogen and oxygen containing compounds and many sulfur containing compounds, were separated from the fuel with a chromatographic column. This fraction was further separated into three polar extracts by graded elution through the column. Each extract was characterized. A storage program using the depolarized fuel, the fuel as received, and blends of the extracts with both fuels, was conducted. Results showed that the removal of the more polar components stabilized the fuel. Blending the polar extracts with the original fuel and with the depolarized fuel in the same ratio as they existed originally and at two and three times the original ratio increased the amount of gum present before storage, but had little effect on the formation of additional gum during storage. Distillate fuels produced by commercial refining of petroleum contain traces of organic nitrogen, sulfur, and oxygen compounds that are more polar4 than the remainder of the fuel. Recent laboratory studies by the Federal Bureau of Mines (1),6 in which these compounds were removed from a fuel, have shown that they influence its storage stability. The objective of this work was to determine the amount of these compounds present in a fuel and their effect upon its stability in storage. To evaluate the role of these polar compounds, it is necessary to remove them from the distillate fuel. Many can be removed by chemical treatment (2), but such treatment precludes reblending the polar components to approximate the original fuel composition. Solvent extraction is free of some of the criticism of chemical treatment, but it is more difficult because of the complex mixture from which compounds must be removed.

Jan 1, 1961

By E. G. King

Many of the existing thermodynamic values for the titanium halides are estimates, including all the entropies and high-temperature heat contents of their crystalline and liquid phases. This report contains the results of low-temperature heat capacity measurents (which lead to entropy values at 298.15° K,) and high-temperature heat-content measurements of four halides - trichloride, tribromide, tetrabromide, and tetraiodide. The new data are combined with selected heat-of-formation values at 298.15° K. to obtain improved values of the heats and free energies of formation of these halides at high temperatures, thus supplementing the previous data of Kelley and Mah.5/ ACKNOWLEDGEMENTS This investigation was conducted under a cooperative arrangement between the Federal Bureau of Mines and the Department of the Navy, Office of Naval Research. The work was done by Bureau of Mines personnel using Bureau of Mines calorimetric equipment. The Office-of Naval Research supplied the supporting funds and arranged for procuring the samples of the titanium halides. The samples were prepared and analyzed by the Inorganic Chemistry Section, Division of Chemistry, National Bureau of Standards.

Jan 1, 1961

By Frank Parrish

THIS REPORT by the Federal Bureau of Mines presents data on water-supply wells used by waterflood operators in North Texas and shows the distribution of permeable source sediments. Averages of well characteristics, including static fluid levels, working fluid levels, net thicknesses, producing rates, and depths, are presented and discussed. Essentially all water used in waterflooding is mineralized water from consolidated sediments. This study is concerned with the geology and distribution of these mineralized source sediments, whereas previous work in this area was predominantly a study of shallow sources of potable water. Tables, isopachous maps, and electric-log cross sections are included to describe the several source aquifers. In general, water-producing capacity increases with depth of the sediments. Wells completed in Cretaceous sediments 82 to 600 feet deep yield 50 to 600 barrels of water daily, whereas those completed in Pennsylvanian sediments 360 to 4,110 feet deep yield 100 to 7,000 barrels daily. Although deeper formations are used where oil and water are produced conjunctively and where large withdrawal rates are required, insufficient well data prevented mapping of deeper formations.

Jan 1, 1961

By Marvin L. Whisman

Several parameters controlling the reproducibility of tritium determina¬tion in organic compounds by liquid scintillation counting were evaluated by the Federal Bureau of Mines. These included optimum volume of scintillator solution for maximum counting efficiency, reproducibility of counting a sealed commercial standard and comparison with duplicate counts on laboratory-prepared samples. The error introduced by using microliter pipets, optical differences in counting vials, reproducibility of counting organic samples where quenching is a factor, reproducibility of counting laboratory-prepared samples with an added internal standard, optimum ratio of internal standard activity to sample activity, effect of sample volume upon counting efficiency, count rate at which coincidence losses become apparent, and reproducibility of organic compound radioassay by the standard addition technique are outlined. From the evaluation of these parameters, a technique that can be applied routinely to organic compounds containing tritium has been established, and details are included in this report.

Jan 1, 1961

By R. G. Dressler

The Federal Bureau of Mines designed, constructed, and operated a demonstration plant at Louisiana, Mo., to produce gasoline, liquid fuels, and organic compounds from coal by a modified Fischer-Tropsch gas-synthesis process. Satisfactory equipment was developed to produce and purify synthesis gas and convert it into the desired products. Coal or coke was gasified with oxygen and steam to make a gas consisting essentially of carbon monoxide, hydrogen, and carbon dioxide. Dust in the raw gas was removed by cyclone separation, water scrubbing, and electrostatic precipitation. Carbon dioxide, hydrogen sulfide, and organic sulfur were removed with diethanolamine, iron oxide, and activated carbon. The gas was passed over iron catalyst and was converted into synthetic liquids, which were then separated and fractionated into gasoline, diesel oil, other liquid fuels, and oxygenated organic compounds. A 39-day continuous run demonstrated the feasibility of the process. Addition of 3 milliliters of tetraethylead per gallon of upgraded (or finished) gasoline gave a product with an octane rating up to 90 by the research method. After a caustic wash, the diesel oil was of a superior quality; its cetane number was 60 or above.

Jan 1, 1961

By R. B. Porter

Bench-scale tests were performed by the Federal Bureau of Mines on lignite and subbituminous coal at pressures to 1,000 p.s.i.g. (pounds per square inch gage) in atmospheres of hydrogen or nitrogen to obtain information concerning the influence of pressure on carbonization of normally noncaking coals. The distribution of gaseous, liquid, and solid products as a function of processing pressure was determined. Except for special experiments, the carbonization was at 940° F. In a hydrogen atmosphere above 400 p.s.i.g., agglomeration of the solid residue (especially with lignite) became noticeable and increased directly with the processing pressure. Although in some instances the solid particles fused together, the mechanical strength of the agglomerate was always low. On the basis of visual inspection, the coals agglomerated in the following order of decreasing intensity: (1) Steam-dried lignite; (2) lignite; and (3) subbituminous coal. Addition of lignite tar in quantities to 25 percent by weight of charge did not increase agglomeration or change the carbonization characteristics of the coal.

Jan 1, 1961

By J. P. Capp

The Federal Bureau of Mines and the Alabama Power Company conducted an experiment in underground gasification of coal at Gorgas, Ala. involving the use of hydraulic fracturing to increase the air acceptance of a coalbed for the introduction of combustion air and removal of product gases. Air acceptance is defined as the flow rate of air which can be injected into the coalbed at 65 p.s.i.g. This was the second time the hydraulic-fracturing technique was used at Gorgas. Sand suspended in a heavy oil served as the fracturing fluid in the first experiment; in the second the sand was two to six times larger and was suspended in a water-starch gel. In addition to providing further tests of the underground-gasification process, the purpose of the second experiment was to determine the effects of the larger sand and greater volumes of a water-base fluid on (1) the extent of the fractured area, (2) the air acceptance of the coal, and (3) the rate at which a gasification path could be carbonized (linked) through the coal, and to compare these results with those of the first experiment. The coal was fractured by injecting 11,000 lb. of sand and 33,580 gal. of water and water-gel at 200 to 600 g.p.m. and 900 to 1,000 p.s.i. The fluid fractured the coal and the sand served as a propping agent to hold the cracks and crevices open. Pressures during the fracturing operation at test boreholes indicated that the fracturing fluid extended only about 150 ft. from borehole H, the point of application of the fracture. Injection of air revealed that the air acceptance of the coalbed within this e t was materially increased. On the other hand, increased air acceptance also was noted at boreholes up to 280 ft. from borehole H and at the electrolinking area 300 to 400 ft. away, indicating that the fracture effects extended considerably farther than was evident from observation. Similar effects were noted at approximately the same distances after the first hydraulic fracture.

Jan 1, 1961

By Arden D. Fugate

The Federal Bureau of Mines conducted extensive studies on solid-state defluorination (laboratory scale) and tests on molten defluorination (intermediate scale) of siliceous fluorspars. The studies were made to develop a pyrohydrolytic process for liberating fluorine from offgrade fluorspars. Test results showed that more than 90 percent of the fluorine can be evolved by solid-state defluorination at 1,300° C., and more than 97 percent can be liberated by molten-state defluorination at 1,420° C. Solid-state defluorination conditions were established by conducting tests on mixtures of ceramic-grade fluorspars and high-purity silica flour. Pelletized mixtures were defluorinated under varying conditions of time, temperature, and relative concentrations of silica, calcium fluoride, and water. The effects of adding various amounts and combinations of aluminum oxide and iron oxide on defluorination were also studied. Investigations of solid-state defluorination indicates that the following two reactions are involved: 2CaF2 + 3SiO2 = 2CaSiO3 + SiF4, and CaF2 + Sio2 + H20 = CaSiO3 + 2HF, The second reaction is dominant, although significant defluorination can be achieved by the first reaction.

Jan 1, 1961

By E. G. King

Thermodynamic data for the hydrated varieties of alumina are sparse, and those for the common clay minerals are virtually nil. This paper partly fills the vacuum by reporting low-temperature heat-capacity measurements and entropy evaluations of diaspore (A10(OH)) and three clay minerals of the composition A12Si207?2H20 - kaolinite, dickite, and halloysite. The heat-capacity measurements were made in the temperature range 510 to 298.15° K., and the entropies were evaluated at 298.15° K. Diaspore has an unusually low heat capacity and entropy compared with boehmite (another mineral of the same chemical composition). The entropies of the three clay minerals differ too little for entropy to be the important factor relating to differences in the thermal stability of these substances.

Jan 1, 1961

By K. K. Kershner

The purpose of this research by the Federal Bureau of Mines was to investigate the recovery of tin from mine-run ores and low-grade concentrates. Over 95 percent of the total tin in such materials was volatilized to tin chlorides at temperatures ranging from 520° to 565° C. Gaseous mixtures of hydrogen and hydrogen chloride were used for reducing cassiterite to stannous oxide and for converting this compound to tin chlorides. The chlorides were swept from the reaction zone of an oscillating kiln by a rapid flow of reactant gases and collected in a condensing system. Losses of tin that occur in current metallurgical processing were prevented. Approximately the same time of treatment was required for minus 35-mesh mine-run ores and low-grade concentrates. In a continuous process, the circulating gases would require some enrichment.

Jan 1, 1961

By T. A. Henrie

One objective of Project Gnome is to study the feasibility of a phase of the Plowshare program recovering thermal energy from an underground nuclear explosion. The test will be conducted in an underground salt deposit. It is anticipated that some of the energy thus released will be stored as thermal energy in molten salt. This report describes the pre-Gnome experiments conducted at the Federal Bureau of Mines Metallurgy Research Laboratory, Boulder City, Nev. The objectives of this study were to determine the problems involved in the recovery of thermal energy from molten salts to assist in planning the experimental program for the Gnome project.

Jan 1, 1961

By W. W. Fowkes

The Federal Bureau of Mines examined a low-temperature tar obtained from a small-scale commercial unit for carbonizing North Dakota lignite for products that might be important to the economic processing of the tar. Tie tar may be divided into three distinct parts: (1) Tar acids, 45 volume-percent; (2) tar bases, 1 volume percent; and (3) neutral compounds, 54 volume-percent. It has a boiling range of approximately 150° to 380° C. (the decomposition temperature) and yields 18 weight-percent as hard pitch. The tar distillate up to 365° C. may be separated as: (1) Tar acids, 48 volume-percent; (2) tar bases, 1 volume-percent; and (3) hydrocarbons, 51 volume-percent. The tar-acid distillate, boiling to approximately 265° C., was characterized in some detail; the neutral fractions and the tar bases were less thoroughly examined. In general, as might be expected of a primary low-temperature tar, the lower boiling fractions are less in quantity compared with the usual high-temperature tar. The homologous series of each major class appears to be rather complete, although some components are present in very small amounts. The tar is quite unstable thermally, and might be more conveniently processed by extraction methods rather than by distillation procedures. The neutral fraction of the tar is highly aromatic, and might be considered as base stock for the production of liquid fuels.

Jan 1, 1961

By John Nagy

The effect of low percentages of methane (0 to 5 pet.) in an air atmosphere on spark initiated explosions of coal dust was investigated. With low dust concentrations (0.1 to 0.4 oz./cu, ft.), small amounts of methane increase the explosion pressure; with larger dust concentrations (0.5 to 2.0 oz./cu. ft.), small amounts of methane decrease the explosion pressure. The rate of pressure rise of a coal dust explosion increases with increase in methane concentration; about 3 to 4 pct. further addition of methane yields a decrease in the rate of pressure rise. Convection currents created by the air or gas blast used to disperse dust produce an increase in explosion pressure and rate of pressure rise. The minimum explosive concentration of the coal dust decreases about linearly as the concentration of methane increases from 0 to 5 pct. The explosion pressure increases linearly as the initial pressure within the chamber increases. Similarities between coal dust and methane explosions are indicated, INTRODUCTION During coal mining, methane occluded in coal or adjoining strata is liberated into the mine atmosphere,4 Normally, the methane is diluted and swept away by the ventilating air. Under some conditions, through accidental disruption of the ventilation system, sudden outburst, or because insufficient fresh air is supplied to a working place, low percentages of methane may be present during mining operations. If it is permitted to accumulate, methane itself presents an explosion hazard; its limits of explosibility arc approximately 5 and 15 pct. The effect of low percentages of methane on the explosibility of coal dust was studied to provide a broader understanding of the hazards of ignition and explosion and thus to facilitate development of control

Jan 1, 1961

By Nick Derick

The continued growth of steel production in the Western States is contingent upon the development of new iron ore sources. Recent development of economical techniques for concentrating and agglomerating taconites has focused attention on the low-grade magnetite deposits near Atlantic City, Wyo., as potentially important sources of iron ore for blast furnace smelting. Therefore, the Federal Bureau of Mines has made comparative evaluations of blast furnace burdens that incorporate pellets produced from Atlantic City concentrates. The Bureau also has evaluated the relative effect of Utah coke on blast furnace performance, using a high-quality Eastern coke as a basis for comparison. This work was done in the Bureau's experimental blast furnace at Bruceton, Pa. Tests determined the maximum wind rate that could be used while a continuous stock movement was maintained in the furnace. The furnace was operated at wind rates ranging from 800 to 1,400 std. c.f.m., them maximum limit of the blowers for the 1.75 in.-diameter tuyeres used. Using a normal Utah ore burden and Utah coke, the furnace went into a tight hanging condition with a wind rate above 950 std, c.f.m. Using the experimental pellet burden again with Utah coke, the wind rate could be increased to 1,000 std, c.f.m. and probably to 1,050 std. c.f.m, before tight hanging occurs. This represents an increase of 5 to 10 pct. in the wind rate. The experimental results indicate an accompanying increase of iron production, as much as 8 pct.

Jan 1, 1961