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By George L. Gates

The Bureau of Mines studied pressure-buildup data from a number of California gas wells to determine if the reservoir properties calculated from these data correlated with field-observed reservoir properties. Pressure-buildup curves from 24 wells showed distinct changes in slope, indicating changes in permeability of the reservoir rock. Calculated distances from the wells to indicated permeability changes were in fair agreement with distances deter-mined in the field. Pressure-buildup curves from three wells had more than one distinct change in slope, indicating multiple permeability changes. Thus field data supported the theoretical relations used to calculate reservoir properties from pressure-time relations measured in gas wells.

Jan 1, 1967

By Heinz W. Sternberg

A method for the electrochemical reduction of the benzene ring was developed and applied to the electrochemical reduction of coal. Successive electrochemical reductions of a vitrain from low-volatile bituminous coal in ethylenediamine saturated with lithium chloride resulted in the addition of 53 hydrogens per 100 carbon atoms. Ultimate analyses and pyridine solubility of the vitrain recovered after each reduction showed that hydrogen added at the beginning has a much greater effect on solubility than hydrogen added at a later stage. Surprisingly, the removal of sulfur from the vitrain takes place only after the more reactive aromatic rings are reduced. Nuclear magnetic resonance analysis and average molecular weight determination of the extracts of the reduced vitrain samples, representing about 18 percent of the vitrain, showed that these fractions had 95 percent of their hydrogen content on saturated carbon atoms and an average molecular weight of 800 to 900. A study of the effect of operating variables on current efficiency showed that current efficiency is highest with aluminum as cathode material and with lithium chloride as electrolyte. A substantial increase in current efficiency of difficulty reducible olefinic double bonds was achieved by adding a proton donor. This result is significant in connection with the electrochemical reduction of coal which proceeds from readily reducible aromatic double bonds to difficultly reducible isolated double bonds. It is proposed that reduction is achieved by electrolytically generated and subsequently solvated electrons and hence does not require prior adsorption of the substrate at the electrode surface. This offers a distinct advantage for electrolytic reduction of sparingly or insoluble substrates such as coal.

Jan 1, 1967

By Robert C. Bates

Variations in water percolation rates through saturated cohesionless hydraulic backfill (mill tailings) have been studied in relation to the many physical aspects of the system to determine the most important factors in causing these variations. A multivariable least-squares regression analysis of 135 separate tests shows that a reliable estimate of the water percolation rate through typical hydraulic backfill can be made if the bulk density (unit weight), specific gravity, and grain-size distribution are known or can be estimated. Equations for predicting percolation rate, coefficient of permeability, and seepage velocity are developed both for the range of data analyzed and for extrapolation. The prediction equations for use within the range of data studied are quite accurate, while the ones developed for extrapolation are less accurate but still give reasonable approximations of flow rates. The equations given are valid for cohesionless materials that are free of clays and micas, exemplified by classified mill tailings. The equation developed for predicting percolation rates is as follows: 1nP20 = 11.39147 + 2.853422 1n(VR X D10) + 0.1747436 VR X Cu -178.8039 D10 X D50 + 311.7034 (DSO )3, (1) where P20 = percolation rate, inches per hour at 20° C; correction factors for other temperatures are given in the text, VR = void ratio, dimensionless, D10 = effective size (diameter in millimeters of the 10-percent-finer grain size), Cu = coefficient of uniformity (ratio of the diameter of the 60-percent-finer grain size over D10), D50 = average size (diameter in millimeters of the 50-percent-finer grain size), and In = natural logarithm (log to the base e). The prediction equation for percolation rate is rather complicated, so for practical use a nomograph that simplifies the solution of the prediction equation was developed.

Jan 1, 1967

By K. P. V. Lei

The Bureau of Mines investigated molten-salt electrorefining as a practical method for reclaiming vanadium from vanadium scrap. An electrolytic process utilizing a KC1-LiC1-VC12 electrolyte at 615° C was developed for producing ductile vanadium with a purity over 99.9 percent. The recovery of the vanadium in the cell feed ranged from 88 to 93 percent with a current efficiency from 83 to 95 percent.

Jan 1, 1967

By Robert C. Ellman

Stockpiles containing 2.3 million tons of lignite constructed in the period 1948-56 in conjunction with the construction of Garrison Dam on the Missouri River demonstrate successful stable long-term storage of lignite. Uniform and thorough compaction of each of the I-foot-thick layers by which the piles were constructed produced a bulk density of 70 Ib/cu ft. Air penetration into the stockpiles was restricted to a degree that prevents spontaneous heating or deterioration of the stored lignite, A continuing record of observations beginning with stockpiling operations in 1948 has been accumulated, This includes periodic fuel analysis, analysis of pile gases, and measurement of pile temperatures on the first large stock-pile, pile 5. This report describes the stockpiling method, the changes in heating value, pile gas composition, and pile temperature and summarizes observations from 1953 to 1964, Data accumulated attest to the stability of the stored lignite. The variation of the average heating value of periodic pile-depth samples is only 160 Btu/lb (11,990 to 11,830) on the moisture" and ash-free (maf) basis during almost 10 years of storage. Temperature levels of the pile interior are progressively decreasing. At pile surface, cyclic variations occur with the season. The only problem encountered with the large stockpiles is wind and water erosion of the pile surface. The partially successful control measures used are described.

Jan 1, 1967

By D. R. Corson

The Bureau of Mines instrumented an operating stope in a deep vein mine to determine the amount of wall closure and the magnitude of loads imposed on a backfilled stope. Hydraulic pressure cells used to monitor pressures in the fill) with bolt closure points to measure vein-wall movement and the procedure for their installation) are described) and the results of the laboratory calibration analysis of the reliability of these cells are given. An attempt to monitor density and moisture changes in the backfill with a nuclear density-moisture device was only partly successful) owing to either deformation of access tubing or relative displacements of the vertical vein walls relative to the emplaced tubes. Data from the instrumentation indicate vein-wall closure in excess of 20 inches and pressures within the fill approaching 600 psi. Analysis) incorporating field data with results of laboratory tests of the compressibility of timber and tests defining the constrained moduli of the fill) points out the limited restraint to vein closure offered by timber sets. Ground movement induced by mining activity could be more effectively con-trolled by the use of densely compacted backfill.

Jan 1, 1967

By Thornton L. Neathery

Geologic investigation of a mineralized zone in eastern Alabama indicates that large quantities of talc and soapstone are scattered over a wide area close to the surface. Laboratory experiments show that this material may be upgraded to a high-quality talc. A market survey indicates that the talc deposits may be of current and long-range interest. The anthophyllite asbestos which is associated with the talc does not appear to occur in sufficient quantities to be considered as a primary commercial source.

Jan 1, 1967

By J. P. Morris

The Bureau of Mines investigated the mechanics of fuming of iron-carbon melts during top-blowing with oxygen. Melts weighing 45 lb were prepared in an induction furnace and blown with oxygen by means of water-cooled lances. The rate of fuming was measured and correlated with the operating variables. The data showed that the primary cause of fuming was a boil at the bath surface in the impingement zone of the oxygen jet. Nucleation of the carbon monoxide bubbles producing the boil was apparently brought about by the precipitation of an oxide phase. The actual fuming mechanism involved partial oxidation and vaporization of bubble films and fine metal spray generated by the bursting of the bubbles. Bubbles that formed outside the impingement zone produced little fume. The distribution of trace elements between the metal and fume strongly indicated that the fume contained fine spray particles as well as particles that had condensed from vapor. The rate of fuming was found to be proportional to the carbon content of the metal) the concentration of oxygen in the jet) and the bath temperature) provided that a continuous boil occurred. In the absence of a boil) very little fume was produced.

Jan 1, 1967

By James H. Aase

Shales from 10 locations in Michigan were sampled, tested, and evaluated to determine their suitability as raw materials for producing lightweight aggregate by rotary-kiln methods. Sampling procedures and the geology of the shale units tested are discussed. Preliminary testing in a muffle furnace preceded extensive testing in a l6-inch by 14-foot rotary-kiln. Rotary-kiln products from these shales ranged in weight from 35.5 to 61.2 pounds per cubic foot (pcf). Concrete test specimens made pith selected aggregates were evaluated to determine the qualities of the concrete. Compressive strengths of the concrete ranged from 2,830 to 4,240 psi after 28 days of curing. Unit weight of the concrete ranged from 94.8 to 101.5 pcf. Lightweight aggregate suitable for use in structural concrete meeting ASTM standards was produced by the rotary-kiln method using shale samples from two locations.

Jan 1, 1967

By J. L. Reuss

The Bureau of Mines derived information on the softening characteristics of both unfired and indurated iron ore pellets as measured by hot compression strength in a laboratory study. A surprisingly high hot strength (240 1b per ½ -inch spheroid) was developed by unfired magnetite pellets near 900° C; lesser maxima were developed by pellets made from hematite and specularite concentrates near 1,000° C. Those from goethite remained weak throughout the pre induration heating. Fully indurated commercial pellets retain a high resistance to softening when heated in air. On the contrary, in a hot reduing atmosphere their high cold crushing strength dissipates rapidly. At 1,000° C, for example, the average compression strength of seven different commercial pellets was 110 lb; at 1,100° C, the hot strength was only 60 lb. After a rather sharp initial drop, the loss of strength with increase of temperature was gradual. There was no sudden collapse, nor any significant difference, in behavior of commercial pellets whether made from magnetite or hematite concentrates.

Jan 1, 1968

By L. A. Haas

A kinetic study of the carbon deposition reaction was undertaken by the Bureau of Mines as part of a broad investigation of metallurgical reactions in the iron ore blast furnace. The disproportionation of carbon monoxide on iron pellets was investigated at carbon monoxide pressures between 0.5 and 2 atmospheres (absolute) and temperatures from 400° to 1,075° C. Gas flow in the range from 0.25 to 0.85 standard liter per minute was found to have little effect on the reaction velocity. The addition of nitrogen and helium to caron monoxide exerted only a dilution effect on the rate of carbon deposition. However, an addition of 1 percent hydrogen increased the rate about 100 times. Small amounts of carbon dioxide in the inlet gas exerted little effect on the rate of carbon deposition. The maximum rate for carbon deposition in the first 2 hours occurred at 550° C. The apparent molar activation energies at various stages of the reaction were found to vary from 13 kcal initially to 36 kcal during the latter stages of the reaction. The reaction rate behavior was tentatively explained by an adsorption step followed by the diffusion of iron through a shell of inactive iron carbide.

Jan 1, 1968

By Francis X. Cannaday

Equipment and techniques were developed with Bureau of Mines facilities for measurement in the laboratory of sonic shear wave velocity in variously shaped rock specimens in a wide range of sizes. A variety of rock types was tested. The shear wave front is produced by electronically excited, piezo-electric ceramic) disk-shaped transducers. Transmitter and receiver are interchangeable. Special equipment components were Bureau produced; other components were commercially available. The equipment permits quick measurement of shear wave velocity on variously shaped specimens with a minimum of specimen preparation. The technique, under favorable conditions, allows for determination of the moment of arrival of the shear wave when it is superimposed on a weak longitudinal wave.

Jan 1, 1968

By R. B. Schluter

Magnetite pellets were simultaneously reduced and indurated on a laboratory scale in order to determine the effects of temperature, induration time, degree of metallization, and sulfur content upon the physical and chemical properties of prereduced pellets. The reductants were commercially-pure tank gases. Among the findings were these: 1,100° C is the minimum temperature that will produce acceptably hard pellets using carbon monoxide as the reduc-ing gas. Prolonged treatment time improves the pellets' crushing strength, but the rate of improvement falls off sharply after 2 hours' induration. At 1,120° C, 75-percent metallization produces the maximum crushing strength; there was no corresponding peak at 900° or 1,050° C. Sulfur in the furnace atmosphere lowers the required induration temperature. A few tenths of 1 percent sulfur in the pellet increases the sintering rate of metallic iron in pellets by forming a liquid FeS phase that facilitates iron transfer.

Jan 1, 1968

By William R. Barton

Sampling to determine development potential of beryllium deposits was conducted at 31 New England localities. A total of 54 additional areas where the geochemical environment appeared favorable were sampled to determine if economically interesting percentages of beryllia (BeO) might occur. Newry Hill-Plumbago Mountain, Maine, Iron Mountain, N.H., and Long Island, Maine, were investigated in some detail to determine the size and grade of deposits. The mineralized pegmatites at Newry Hill-Phunbago Mountain are extensive but very low grade; at Iron Mountain the ore bodies are very rich but of small volume; at Long Island beryl occurs with molybdenite, wolframite, and scheelite, but the tonnage of ore was not determined.

Jan 1, 1968

By Israel Liebman

The Bureau of Mines conducted an investigation to determine those factors that are significant in affecting the velocity of flames propagating along the boundary separating gaseous fuel and air. In addition the aerodynamic motion of the gases in the vicinity of such interfacial flames was delineated. Parameters in the study included flammable zone thickness, flammable zone concentration of gradient, fuel type, and position of the flame relative to various environmental surfaces. Of all these factors, the flammable zone thickness and burning velocity of the stoichiometric mixture were found to have the most significant effect on the flame speed. Notion of the gases in the vicinity of the interfacial flames was examined by particle track and interferometric techniques. The relative velocity of the interfacial flame with respect to the unburned gas on the central streamline was found to equal the burning velocity of a stoichiometric homogeneous fuel-air mixture. In addition, it was observed that the composition of the lean fuel-air mixture at the boundary of the combustion zone appears to be less than that defined as the fuel's lower flammable limit.

Jan 1, 1968

By Oliver C. Fursman

The Bureau of Mines undertook this investigation in order to determine the feasibility of producing commercially acceptable alumina and iron by application of the Pedersen process to high-silica, high-titania, ferruginous bauxites of the Pacific Northwest. Calcium aluminate slags were produced by smelting bauxite with coke and lime in an electric-arc furnace. Over 90 percent of the total alumina can be extracted by sodium carbonate solution from slags of properly controlled ternary-phase composition (CaO-Al203-SiO2) that are cooled slowly enough to permit adequate crystallization of the 2CaO-SiO2 and the calcium aluminate compounds. Most of the iron charged was recovered in the regulus; the slag contained about 2 percent iron (as iron oxide), regardless of smelting time.

Jan 1, 1968

By T. N. Rushton

Rate minima are encountered in the reduction of magnetite with hydrogen. In a certain temperature zone, the reaction rate decreases with rise in temperature. This is inexplicable by classical kinetic theories; neither is a transition in reduction mechanism suitable for interpreting the observed behavior, This anomaly can be fully explained by hypothesizing two species of chemisorbed hydrogen with different adsorption coefficients and activation energies for adsorption. Competition between two energetic states of adsorption occurs with temperature rise, with the low energy state predominating below the anomalous temperature zone and the high energy state above it. The presence of two possible adsorption sites appears to be characteristic for oxidic adsorbents.

Jan 1, 1968

By Wesley T. Holmes

This report describes the first phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected slag compositions in the titania-alumina-silica-calcia-magnesia system. Both the melting-holding-quenching method and the hot-stage microscope method were used in the tests. Liquidus temperatures of slags studied ranged from 1,217° to 1,667° C. The lowest liquidus temperature of the slags occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. Liquidus temperatures were also lowered when Si02 was substituted for Ti02 plus Al2O3 when CaO and MgO levels were held constant. Improved methods for the measurement of liquidus temperatures on very small samples are described.

Jan 1, 1968

By T. A. Sullivan

Refining in a molten salt electrolyte was investigated as a means of recovering nickel containing less than 1 percent and preferably less than 0.2 percent cobalt from nickel products containing up to 5 percent cobalt. Electrolytic separation of nick and cobalt was accomplished in a molten KCl-LiCl-NiCl2 electrolyte. Nickel containing less than 0.10 percent cobalt was routinely prepared. Factors that influenced the transfer of cobalt to the refined product were the nickel concentration of the electrolyte, the cobalt concentration of the electrolyte, the ratio of nickel to cobalt in the electrolyte, and cathode current densities. A method of recovering the cobalt from the electrolyte was developed. The possibility of preparing high-purity nickel by this process was shown, as well as the preparation of various cobalt-nickel-tungsten alloys.

Jan 1, 1968

By Wesley T. Holmes

This report describes the second phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected synthetic slag compositions in the Ti02 -A1203 -FeO-Si02 -CaO-MgO system. Both the hot-stage microscope and the strip furnace (melting-holding-quenching technique) were used during test procedure to determine the effects of CaO, MgO, and SiO2 on the liquidus temperature of slags. The liquidus temperatures of slags studied ranged from 1,241° to 1,900° C. The lowest liquidus temperature for each Ti02 plus A1203 plus FeO weight-percent generally occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. In this investigation substitution of either CaO or MgO for SiO2 and MgO for CaO raised the liquidus temperature of more than 50 percent of the reported base slags when Ti02, A1203, and FeO contents were held constant. The results of this investigation may serve as guidelines for determining flux requirements in smelting a wide variety of titaniferous magnetite concentrates or ores.

Jan 1, 1968