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By James H. Gary

Data regarding the composition and physical properties of Florida land-pebble phosphate-waste slime are presented, and the feasibility of dewatering and beneficiating the slime by several different methods is discussed. Chemical analyses, electron micrographs, and X-ray diffraction data showed that principal constituents of the slime included quartz, attapulgite, and flaorapatite. Viscosity of the slime changed with pH; thixotropic, Newtonian, and rheopectic states were observed as the pH increased. Use of various flocculating agents was not effective in improving thickening properties of the slime. Dewatering tests using pressure filtration showed that temperature influenced the filtration rate more than pressure; the filtration rate at 165° C was tenfold that at room temperature. Selective flotation of the slime, using two different processes, gave promising results. About 25 pct of the phosphate was recovered in a concentrate assaying 31 pct P205, Other tests demonstrated that the slime could be successfully fractionated at 20-microns using a hydrocyclone. In hydrometallurgical tests about 80 pct of the phosphorus and alumina were chemically extracted from the slime using sulfuric acid. Limited bacteriological studies made of the slime showed that several types of microorganisms were present and grew in the material despite the presence of fluorine-bearing minerals.

Jan 1, 1963

By G. T. Krempasky

In an attempt to develop a suitable precast concrete support for underground use, two different models (1955 and 1958) of a five-piece concrete set were designed, fabricated, and tested under adverse loading conditions. Model 1955 was designed to withstand an ultimate, uniformly distributed, vertical load equivalent to what a three-piece, 12- by 12-inch wood set of intermediate-grade Douglas fir would withstand. A design figure of 138,000 pounds for the vertical load was used on both the 1955 and 1958 models. In addition, the 1958 model was designed to withstand a uniform horizontal load of 7,000 pounds per foot and additional concentrated-point loading. The step- by-step design of each model is presented in the appendixes. A series of five destruction tests was conducted underground on the 1955 model, and results of the tests showed that the type and method of blocking were of major significance.

Jan 1, 1963

By William C. Miller

This report describes investigations by the Bureau of Mines designed to establish the noise level and spectrum of various types of pneumatic rock drills and to furnish information that would be useful in conducting sound measurements in mining environments and in reducing the noise generated in pneumatic drilling. These investigations show that (1) the noise generated by the drills in the frequencies below 100 cps is caused by the impact of the piston and drill steel, in the frequency range between 100 and 2,000 cps by the exhausting of air from the ports, and in the frequencies above 2,000 cps by the resonant frequencies of steel drill parts and of drill steel; (2) satisfactory instruments and instrumentation systems are available for field and laboratory measurements; (3) reliable sound measurements can be made in mining environments; and (4) devices can be developed that will abate the noise.

Jan 1, 1963

By W. E. Robinson

Samples of raw oil shale and kerogen concentrates were oxidized by alkaline potassium permanganate, air, nitric acid, oxygen, and ozone to obtain information about the chemical structure of organic kerogen in oil shale. In one test, oil shale and oil-shale products were oxidized exhaustively with alkaline potassium permanganate, and the distribution of the organic carbon in the final oxidation products was determined. Comparing results of this oxidation with those obtained from other carbonaceous materials and known compounds gave information about the structure of kerogen. Alkaline potassium permanganate oxidation also was used partly to degrade kerogen into soluble products for characterization purposes. Structures present in these degradation products were indicative of type structures originally present in the kerogen. Nitric acid, oxygen, and ozone were used also for partly degrading kerogen to soluble oxidation products. Carbon-balance oxidation tests using alkaline potassium permanganate showed that Colorado oil-shale kerogen differs from many other carbonaceous materials such as coal and kerogens from other areas. Composition of the degradation products indicated that Colorado oil-shale kerogen is predominantly cycloparaffinic and saturated heterocyclic structures with some long-chain paraffinic and aromatic structures present. The ring systems may be connected through short carbon chains or bridges containing oxygen, nitrogen, and sulfur.

Jan 1, 1963

By M. E. Hawkins

Mineral analyses and electrical resistivity measurements of 324 representative samples of oilfield brines from 24 oil-productive counties in Mississippi and Alabama are presented in tabular form. Results of the mineral analyses, which include calcium, magnesium, carbonates, bicarbonates, sulfates, chlorides, sodium, and barium (with strontium if present), are reported in milligrams per liter. Electrical resistivity measurements in ohm-meter2 per meter at 75° F are reported in ohm-meters in the tables. Chemical analyses of formation waters are helpful to operators having water problems associated with petroleum recovery; electrical resistivity values are helpful in making interpretations from electric logs.

Jan 1, 1963

By David J. Kusler

A gravimetric method for the determination of carbon dioxide, carbon monoxide, hydrogen, methane, and oxygen in blast furnace top gas is described. Nitrogen may be determined directly by volume measurement or by difference. The method is direct, permits continuous as sampling, and provides an averaged analysis over a selected range of sampling intervals from 1/2 to 24 hr or more. Neither expensive equipment nor specialized personnel are required. The method is suitable for routine analysis, and the results compare favorably with those obtained by established methods.

Jan 1, 1963

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