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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 E. G. King

This report contains experimentally determined heat-content values for cerium dioxide and Columbium (niobium) dioxide in the temperature range from 298° to 1,800° K. There are no previous similar data for Columbium dioxide, and those for cerium dioxide have an upper limit of 373° K. The heat-content and corresponding entropy-increment data are presented in tabular form. Equations were derived to represent the heat contents and heat capacities. The data for cerium dioxide are entirely regular, but those for columbium dioxide show two previously unreported anomalies at 1,090° and 1,200° K.

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 E. G. King

In continuation of the study of thermodynamic properties of the common interoxidic compounds of ferroalloy elements, this report gives the results of low-termperature heat-capacity measurements and entropy evaluations of the monotungstates of sodium, magnesium, and calcium. Previous reports4 5/ of this laboratory dealt with low-temperature heat capacities, entropies, and heats of formation of the sodium vanadates. Heat-capacity measurements of the monotungstates of sodium, magnesium, and calcium (Na2W04, MgW04, and CaW04) were conducted throughout the temperature range 51° to 298° K. The entropies at 298° K. were evaluated and then combined with entropy data for the elements and oxides to obtain entropies of formation. This information is an essential part of the data needed for thermodynamic appraisals of chemical reactions of these substances. No similar data for any tungstate are to be found in the literature.

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 John E. Shelton

Flotation tests were conducted on two samples of copper-nickel-bearing ore from the Harriman area near Rockport, Maine. The samples were taken by Roland F. Beers, Inc., for tests in cooperation with the Federal Bureau of Mines. One sample, analyzing 0.38 percent copper and 0.71 percent nickel, was essentially a disseminated pyrrhotite in hypersthene. Pentlandite, chalcopyrite, pyrite, and millerite were intimately associated with the pyrrhotite. Locked series flotation tests on this sample showed that 87.4 and 73.4 percent of the copper and nickel, respectively, could be recovered in a bulk concentrate that analyzed 3.47 percent copper and 5.34 percent nickel. The copper-and nickel-bearing minerals were collected with sulfhydric collectors in an alkaline circuit. Cleaning the concentrate three times with the addition of pH regulators was sufficient to attain the previously stated grades. The second sample had analyses of 0.31 percent copper and 0.85 percent nickel; talc and hypersthene were the main gangue minerals. Bulk sulfide flotation, made while depressing the talc, resulted in a concentrate that analyzed 2.33 percent copper and 4.70 percent nickel at recoveries of 70.0 and 54.4 percent, respectively. Flotation of the talc followed by bulk sulfide flotation resulted in a nickel content greater than 5 percent. A locked-series test showed that 60.7 percent of the copper and 73.7 percent of the nickel could be recovered at grades of 1.29 and 4.85 percent, respectively.

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 J. G. Croeni

The high thermal-neutron cross section of gadolinium and the good mechanical and corrosion properties of titanium suggest that alloys of these two metals might be useful as control rod material. To aid in establishing the feasibility of this combination, the Federal Bureau of Mines investigated the titanium-gadolinium system. The results indicate that the system is composed of a single eutectic reaction and a peritectoid reaction involving the alpha-beta transformation of titanium. The eutectic isotherm extends from 1 to 99 pct, gadolinium at 1,240° C. The established eutectic composition is about 95 pct, gadolinium. The peritectoid reaction occurs at 885° C. and extends almost over the entire composition range. Hardness increases slightly with additions of gadolinium, and little change is obtained by heat treatment. Alloys containing less than 10 pct. gadolinium are amenable to extensive cold-working, but alloys having higher percentage of gadolinium content are only moderately cold-workable. All alloys can be hot-worked in iron sheathing at 750° C. Observation indicates that all compositions possess good machinability. Corrosion resistance to water at room temperature is apparently poor, especially in the gadolinium-rich alloys. INTRODUCTION A combination of the good mechanical and corrosion properties of titanium and the variety of thermal-neutron cross sections characteristic of the rare-earth metals suggests that alloys of these metals may be used for control rod materials. For this reason the Bureau of Mines proposed a study of the titanium-gadolinium alloy system, and the Atomic Energy Commission sponsored the investigation.

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 F. W. Wessel

Manganiferous carbonate slates of the Cuyuna range, which are part of the unoxidized thin-budded iron formation, represent a large potential source of manganese. This report details recent bench-scale research by the Federal Bureau of Mines in applying mineral-dressing techniques to these materials in order to investigate their potential uses. Work outlined in the report was directed toward the production of concentrates usable as iron-blast furnace feed, but an equally important objective might have been to furnish an enriched feed for extractive processes for recovering manganese. Flotation concentrates were prepared that contained 11.1 percent manganese, 27.8 percent iron, and 12.2 percent silica, with recoveries of 73 percent of the manganese and 48 percent of the iron. Calculated analysis for a simulated sinter suggests a product containing 16.0 percent manganese, 40.2 percent iron, and 17.6 percent silica, with 31 percent recovery of the dry weight of the ore. The silica in the flotation concentrates was due to quartz and iron silicates. Substantial quantities of the iron silicates (stilpnomelane and smaller amounts of minnesotaite) were present in the slate, and the need to reject these minerals limited the recovery of iron. The sintered flotation concentrate would be usable as ferruginous manganese ore for iron blast-furnace feed because of its favorable manganese silica ratio. The unsintered flotation concentrates, representing 45 percent of the feed weight and containing manganese enriched in the ratio of 1.6 : 1, also could be used as feed to processes for extracting manganese.

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 F. P. Haver

The Federal Bureau of Mines developed a 10,000-ampere cell to determine the economic feasibility of producing high-purity electrolytic titanium from mill scrap or offgrade sponge. Operating variables were investigated, matetial handling procedures were established, and the cost of electrorefining titanium was determined. The prototype cell produced premium-grade metal (<100 Brinell hardness number (B.h.n.)) from very impure Kroll sponge at a processing cost of less than $0.60 per pound. Refined metal was deposited at the cathode in the form of coarse (85 percent plus 34-mesh), hexagonal crystals of a titanium when the cell was operated an 850° C. A cathode current density of 1,000 amperes per square foot and a molten sodium chloride electrolyte containing approximately 5 percent by weight of soluble titanium were used. In continuous operation, at the optimum number of ampere-hours, (40,000), the current efficiency averaged slightly less than 60 percent. It was possible to supply large enough amounts of electric current for electrolysis to maintain the temperature of the bath, thus reducing overall power consumption to less than 5 kilowatt-hours per pound of metal refined.

Jan 1, 1961

By W. Beckering

In characterizing tars obtained by the low-temperature carbonization of North Dakota lignite, infrared spectra have been an invaluable aid in both qualitative and quantitative examination. Quite, early in the tar-research program of the Federal Bureau of Mines it became evident that the small number of published spectra available for hydroxy-aromatics would be inadequate for comparative purposes when dealing with the wide range of compounds present in coal tar; therefore, compiling a catalog of spectra was begun as a continuing part of the tar program. Because these spectra should be valuable to other investigators in this and related fields, they are being presented in these reports. This supplement to the original publications presents the spectra (figs, I to 32), representing 32 compounds, largely phenolic materials. The major problem of this project has been the availability of materials for examination. Most of the compounds included in this supplement were synthesized at the Bureau of Mines Lignite Research Laboratory. Some were obtained from commercial sources, whereas the compound 2&apos;-hydroxy-l-phenylnaphthalene was synthesized at the Bureau of Mines laboratory in Bruceton, Pa. The spectrum of 2-ethyl-4-methylphenol, figure 32, is a correction of the spectrum presented as figure 26 in the original reports

Jan 1, 1961

By J. B. Gayle

Coke-pushing difficulties have been the subject of much controversy but relatively little scientific investigation. Nevertheless, continuing pushing difficulties can greatly decrease the life of a coke oven and should therefore be considered in the selection of the blend and operating conditions used for coke production. The present Federal Bureau of Mines investigation was undertaken to correlate results of previous investigators and to supplement these results to the limited extent practical by us of an experimental slot-type oven. To this end, pushing pressures have been determined routinely for Tuscaloosa oven tests conducted during the past 10 years. Nevertheless, the accumulated information remains incomplete in many respects, and in view of the recognized inadequacies of the data, publication is now undertaken only because of the scarcity of published information on this important problem and the discontinuation of carbonization studies with this oven.

Jan 1, 1961