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By Albert J. Rambosek

The results obtained in a study of the stress conditions existing in a drill bit-point area and in the underlying rock, when the bit was in full but nonpenetrative contact with the rock, are presented. This investigation by the Bureau of Mines was the preliminary exploratory phase of a long-range program of research on rock drilling to establish criteria for the maximum economically feasible rate of rock penetration. The photoelastic technique of experimental stress analysis was the principal method used to obtain the data. Transparent models and transmitted light were employed to investigate patterns in drill-bit models and isotropic materials under the bit when subjected to a concentrated static load. Comparative stress data for anisotropic rock were obtained by the reflective photoelastic technique. Brittle lacquer and an extensometer were used obtain supplementary information wherever substantiating data were desired to check photoelastic results. The zone of maximum shear occurs along an arc near the contact face of the bit. The stress distribution pattern in an isotropic model rock near the area contacted by the bit was nearly a mirror image of that exhibited within a similar areal zone of the bit. The stress pattern in granodiorite specimens was similar, though not symmetric, to the pattern in the isotropic model rock. The asymmetry of the stress pattern in the granodiorite was attributed to the anisotropic characteristics of the constituent minerals of various sizes.

Jan 1, 1963

By Vernon F. Swanson

Several laboratory flotation tests were conducted by the Bureau of Mines on a sample of unweathered diorite from the B. F. Camden property, Amherst County, Va. Results showed that an ilmenite concentrate analyzing 45.5 percent Ti02 (titania), 0.07 percent P205 (phosphorus pentoxide), and 2.21 percent Si02 (silicon dioxide) could be produced from a feed containing 7.72 percent Ti02 and 3.94 percent P205. Ti02 recovery in the concentrate was 47.6 percent in a batch test. The weathered saprolite material overlying the diorite required scrubbing and desliming to remove argillaceous material and preliminary flotation of apatite followed by flotation of ilmenite. The resulting concentrate analyzed 47.3 percent Ti02, 0.19 percent P205, and 0.99 percent Si02 from a starting feed of 8.99 percent Ti02 and 3.37 percent P205; TiO2 recovery was 54.5 percent.

Jan 1, 1963

By Laird Crocker

This report describes a study of beryllium recovery from sulfate leach liquor by di-2-ethylhexyl phosphate (EHPA) solvent extraction in conjunction with caustic stripping. The work was one phase of Bureau of Mines research on process development for Spor Mountain, Utah, ores. Solution for the solvent extraction studies was prepared by sulfuric acid leaching of ore containing 0.6 pet BeO, Before solvent extraction of beryllium, the leach liquor was treated to prevent coextraetion of iron by either (1) removal of ferric iron by amine solvent extraction or (2) reduction of ferric iron to nonextractable ferrous iron by treatment with sulfur dioxide. Beryllim was extracted from the aqueous leach liquor by countercurrent multistage contacting with a kerosine solution of EHPA. The loaded organic solution was stripped with sodim hydroxide solution. Subsequently, beryllium hydroxide was precipitated by boiling the sodium beryllate strip solution and converted to beryllium oxide of 98 pct BeO-grade by calcining. Material of this grade can be directly processed into beryllium-copper alloy or be used as starting material for further refining to produce high-purity, nuclear-grade beryllium. Over 90 pct of the beryllium contained in the leach liquor was recovered as beryllia.

Jan 1, 1963

By Sara Jane Boles

The purpose of this Bureau of Mines investigation was primarily to isolate and examine the effect of liquid content upon the apparent porosity and bulk density of compacts pressed from high-purity, fused aluminum oxide, and, secondarily, to study the actual mechanism by which the liquid content affects the bulk density. No attempt was made to approach the theoretical maximum density of the oxide by introducing additives, particle packings, or similar variables; instead this study is an intercomparison of the bulk densities obtained as functions of the water contents of the compacting mixtures. Water content was varied from 7 percent to 25 percent, on a total-weight basis. The data gathered indicated a well-defined optimum water content for obtaining minimum apparent porosity and maximum bulk density, under the conditions of the experiment. During the course of this study, a number of additional variables in the forming process were discovered and are introduced in this report, although a thorough evaluation was found to be beyond the scope of this present investigation.

Jan 1, 1963

By L. B. Pankratz

The heat contents of the sesquioxides of erbium, holmium, thulium, and ytterbium (Er203, Ho203, Tm203, and Yb203) in the cubic crystalline form were measured over the temperature range from 298° to 1,800° K. The erbium and holmium sesquioxides gave regular heat content-temperature curves. Thulium sesquioxide had a minor thermal anomaly near 1,680° K, with a heat absorption of 310 cal/mole; similarly, ytterbium sesquioxide had a minor anomaly near 1,365° K, with a heat absorption of 150 cal/mole. The heat content results are presented in both tabular form (at 100° intervals) and in algebraic form. Entropy increments, corresponding to the tabulated heat content results, also are listed.

Jan 1, 1963

By Richard F. Hewlett

Computing average grade and tonnage either for an entire ore deposit or for individual blocks of ore is a continuing problem in mining. As part of a research program, investigating application of statistical techniques to mine sampling, Bureau of Mines engineers at the Denver Mining Research Center have made extensive use of an electronic digital computer for developing mine sampling theory, simulation of ore deposits, and analysis of mine sample and assay data. This report is one of a series describing use of the digital computer for rapid solution of computing problems in the mining industry.3 4 Development of a computer program to compute ore reserves by the commonly used triangular method was necessary so that results could be made available for analysis within hours.

Jan 1, 1963

By Alla D. Mah

Energies of combustion of vanadium nitride (VN) and vanadium carbide (VC) were measured. Correcting to vanadium tetroxide (V204) as the final state, the heats of combustion were ?H298.15=-118,700±100 cal/mole of vanadium nitride and ?H298.15=-240,270±360 cal/mole of vanadium carbide. With vanadium pentoxide (V205) as the final state, the heats of combustion were ?H298.15= -133.440±100 cal/mole of vanadium nitride and ?H298.15=-255,020±360 cal/mole of vanadium carbide. Combining these results with vanadium oxide data, the heats of formation obtained were ?298.15=-51,880±200 cal/mole of vanadium nitride and ?H298.15=-24,350±400 cal/mole of vanadium carbide. Heats and free energies of formation of vanadium nitride and carbide were calculated to 2,000° K.

Jan 1, 1963

By W. J. Boone

Experimental determinations were made of vapor-liquid equilibria data for a helium-nitrogen-methane system. A mixture composition was chosen to approximate the crude helium to be produced Or conservation that will eventually be further refined to obtain pure helium. Although there are publications of studies of the vapor-liquid equilibria of helium-nitrogen, helium-methane, and nitrogen-methane binary systems, there is little indication of work done on the ternary system of helium-nitrogen-methane. The experimental data presented in this report supplement the information available for the binary systems. The equilibrium vapor-liquid data and equilibrium vaporization coefficients are presented in tabular form. Graphs are employed to show an extensive amount of the data.

Jan 1, 1963

By Walter Kawa

The hydrogenation of phenyl ether, benzyl ether, and phenyl sulfide in the presence of iron catalysts was studied by the Bureau of Mines to gain a better understanding of the role of iron catalysts in the hydrogenation of coal. The carbon-oxygen and carbon-sulfur bonds in these compounds may be similar to some of the carbon-oxygen and carbon-sulfur bonds in coal which react during the early stages of liquefaction by hydrogenation. Experiments were made in batch autoclaves for 4 hours; hydrogen was at a pressure of about 540 atmospheres. In the hydrogenation of phenyl ether at 400° C, metallic iron catalyzed both hydrogenolysis (splitting-hydrogenation) and nuclear hydrogenation (addition of hydrogen to aromatic rings) reactions, Products were principally benzene and cyclohexane. The activity of metallic iron was decreased by adding carbon monoxide or a reactive sulfur-containing organic compound. Ferrous sulfide catalyzed the conversion of phenyl ether to benzene, phenol, and small amounts of cyclohexane. Hydrogenolysis of benzyl ether was catalyzed by metallic iron and to a lesser extent, by ferrous sulfide at 250° C. No nuclear hydrogenation was observed with either catalyst. Conversion of phenyl sulfide to benzene was nearly quantitative in experiments made at 250° C with equimolar quantities of phenyl sulfide and metallic iron or iron as ferric oxide. Conversions of metallic iron and ferric oxide to ferrous sulfide were nearly stoichiometric. No reaction of phenyl sulfide occurred in the presence of ferric oxide and water, and very little occurred in the presence of metallic iron and water. Ferrous sulfide also catalyzed the hydrogenolysis of phenyl sulfide to benzene, but conversion was lower than in experiments with metallic iron or ferric oxide. The activity of ferrous sulfide was increased by adding water and decreased by adding hydrogen sulfide. The results of this study suggest that ferrous sulfide is an active form of iron when iron is used as a catalyst for the hydrogenation of coal.

Jan 1, 1963

By Charles W. Huggins

Knoop hardness indentations were studied and measured with the electron microscope on TiB2, HfC, and A1B12 crystals. A detailed description of replicating the indentations using collodion and Faxfilm is made. A John Hopkins grating having 28,800 lines per inch was used to accurately determine the magnification used on the electron microscope. The primary objectives were to prepare carbon replicas of hardness indentations, to measure the indenations accurately, and to compare the results with those obtained with the light microscope. The resulting data showed excellent agreement between the measurements made on the replicas with the electron microscope and those made with the optical microscope. The replicas made from collodion showed slightly better agreement with the light optical values than did the replicas made from Faxfilm.

Jan 1, 1963

By Lloyd Carpenter

Eighteen elements were determined spectrochemically in vanadium metal and its compounds in the general range of 1 to 1,000 ppm by means of spark-ignited unidirectional arc excitation. The samples were converted to vanadium pentoxide and combined with a mixture of graphite, lithium carbonate, and gallium oxide. For the molybdenum determination, the oxidized samples were mixed with sodium chloride and packed in copper electrodes. Average precision of the method was 15.6 percent relative standard deviation and relative error was 4.4 percent.

Jan 1, 1963

By P. R. Tisot

Knowledge acquired from this research contributes to a better understanding of the physical structure of Green River oil shale and provides fundamental data and concepts that may serve to improve oil-shale technology. This study by the Bureau of Mines indicates that oil shale is a highly consolidated organic-inorganic system with no significant micropore structure, pore volume, or internal surface. This system is a form of physical structure that precludes rapid diffusion of either gases or liquids. The mineral matter consists essentially of nonspherical particles that tend to follow a log-normal size distribution. An excess of 99 weight-percent of these particles have equivalent spherical diameters of less than 44 microns--75 weight-percent are from 2 to 20 microns, and 15 weight-percent are less than 2 microns. The surface area (3 to 5 square meters per gram) of these mineral constituents is mainly external surface. The mineral constituents contain some micropore structure--pore radii ranging from 10 to 100 Angstrom--with the pore sizes randomly distributed. Distribution of the organic matter within the inorganic matrix is essentially interparticle and not intraparticle. The organic matter within the micropores of the mineral constituents is less than 4 percent of the total. Estimates made from surface area data suggest that perhaps only a small amount of the organic matter is bonded either physically or chemically to the mineral constituents.

Jan 1, 1963

By Aldo L. Furno

Sufficient quantities of combustible vapors are released by some sulfurs to produce flammable atmospheres under prolonged storage. Hydrogen sulfide and carbon disulfide appear to be the principal flammable constituents in the vapor space above molten sulfur. If sufficient carbon disulfide is present, ignition of the vapor-air mixtures can occur spontaneously on contact with the heated surfaces found within storage tanks.

Jan 1, 1963

By Arden D. Fugate

This work was conducted to determine a feasible process for converting siliceous fluoride offgases to a commercially usable product. The offgases were generated by pyrohydrolytic defluorination of low-grade fluorspar in a gas-fired rotary kiln, and fluorine was collected as a hydrofluoric-fluosilicic acid. A silicon-free fluoride solution for further processing was then produced by neutralizing the acidic scrubber solution with anhydrous ammonia, silicon being separated as orthosilicic acid. Ninety to ninety-nine percent of the fluorine originally present remained in solution as ammonium fluoride. Silicon was also separated from synthetic fluosilicic acids, having F-to-Si weight ratios ranging from 3.50 to 14.3. The solutions below a ratio of 4.06, the F-to-Si ratio of H2SiF6, containing dissolved silicon were desiliconized as completely as those containing less than the stoichiometric quantity of silicon. An electrolytic-grade cryolite was recovered from the ammonium fluoride solution by reacting with either sodium aluminate or alumina trihydrate and sodium hydroxide. A product containing 97 to 100 percent of the fluorine, represented by Na3A1F6, was recovered, and 94 to 99 percent of the theoretical yield was realized.

Jan 1, 1963

By James S. Browning

The Bureau of Mines conducted laboratory batch and small-scale continuous selective flotation tests of barite-fluorspar ores from two deposits near Marion, Ky., to determine the technical feasibility of recovering commercial grade fluorspar and barite concentrates. The lignin sulfonate-sodium fluoride method of floating the fluorspar successfully produced acid-grade fluorspar concentrates. Flotation of the barite from the fluorspar tailing using petroleum sulfonate collector yielded concentrates suitable for use in compounding oil-well drilling mud. The fluorspar and barite recoveries were about 82 and 85 percent, respectively.

Jan 1, 1963

By J. Burlin Johnson

This report describes an investigation of the relationship between crater dimensions formed in laboratory blasting experiments and the mechanical properties of the material cratered. Scaled field data have been included when available. The results show that tensile strength and possibly other mechanical properties may be useful in predicting maximum crater dimensions.

Jan 1, 1963

By W. W. Agey

Past investigations on waterborne impurities in the flotation process have been concerned primarily with the treatment of specific ores with particular local waters. Although some anions and cations present in water are known to react with flotation reagents, a definitive study has not been made on the effect of such common ions upon the flotation process. This report describes the fundamental research undertaken to define and measure the adverse and/or beneficial effects of different concentrations and combinations of several common anions and cations when oleic acid is used to froth-float limestone from a pulp of quartz and limestone. Research on the effect of waterborne impurities upon the flotation process was composed of two equally important phases. The first phase comprised development of a procedure for floating limestone from quartz that would give the same results in test after test. Some difficulty was encountered, but once such a procedure was developed, the second phase, comprising study and measurement of the effect of various ions c on to natural water upon the flotation of limestone, was quickly completed.

Jan 1, 1963

By John E. Miller

Supercompressibility factors, Fpv, were derived from experimental compressibility data for five helium-nitrogen mixtures containing from 50 to 100 pct helium. These Fpv values are required as volumetric correction factors for or if ice meter measurement of "crude helium" (helium-nitrogen) purchased by the Government in a program of helium conservation. Although compressibility measurements were made by the Burnett method (2)3 - for pressures from 100 to 3,400 psia and temperatures from 40° to 100° F, Fpv values were needed only for pressures from 400 to 2,000 psia. Consequently, values at increments of 2° F, 2 pct helium, and 10 psia were tabulated only for the required pressure range. Values for pressures outside this range can be calculated from information shown in the tables. Values for the second, third, and fourth coefficients in the equation Z = 1 + BP + CP2 + DP3 are also included.

Jan 1, 1963

By Martin H. Stanczyk

Acid leaching of selected copper sulfide minerals, impure copper sulfide flotation concentrates, and a cement copper precipitate at elevated temperatures and pressures was investigated. Copper extractions of 97 to 99 pct were obtained by leaching chalcopyrite and the flotation concentrates with water under oxidizing conditions at 200° C for 30 to 60 min. In tests with bornite, chalcocite,and cement copper, addition of sulfuric acid or pyrite to the autoclave was required to obtain similar copper extractions. The chemistry of leaching copper minerals was studied. It was determined that different copper sulfides altered to covellite as one step in their dissolution.

Jan 1, 1963

By D. Bienstock

To develop a rugged catalyst capable of withstanding hydraulic attrition resulting from the oil-circulation process for synthesizing liquid fuels, use of an iron catalyst containing an active coating surrounding an inert solid core of metal was investigated. This massive-iron catalyst in the form of steel shot and lathe turnings was activated by partial oxidation with steam at 600° C, impregnated with alkali, and reduced with hydrogen at 450° 6. The massive-iron catalysts were resistant to oxidation and spalling, and a 6-month catalyst life was attained. Higher operating temperatures could be employed than with fused iron oxide catalysts, resulting in greater gasoline yields. Because the lathe turnings pack with void volumes of 70 to 90 percent, it has become possible to employ a fixed bed without the danger of cementation that occurs with fused iron oxides.

Jan 1, 1963