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By Hillary W. St. Clair

The effective coefficient for rate of reduction of a sample of granular iron ore may be determined by passing the reducing gas through a bed of the are at constant flow rate and periodically analyzing the effluent gas, The method of analyzing the data is based on a mathematical model that takes into account the variation in composition of the gas and solids with time and position in the bed. A method is described for determining the value of the rate coefficient that gives best agreement between the observed and calculated analyses of the effluent gas.

Jan 1, 1967

By Charles E. Whieldon

This report presents the results of a study on part of the Smithfield oilfield, Wetzel County, W. Va. The primary purpose of the investigation was to determine the original and the present volume of stock-tank oil in the formations and to investigate the feasibility of waterflooding the Gordon Stray, Gordon, and Fourth sands underlying the I. D. Morgan lease. The study was based on laboratory core analyses, geophysical well logs, geologic considerations, and various field prediction data from the I. D. Morgan lease. The Bureau found that, of the three sands cored, the Gordon Sand was the best prospect for waterflooding, and that a properly engineered water flood should recover 136 to 230 barrels of oil per acre-foot from this formation.

Jan 1, 1967

By J. J. Demeter

A tube-wall reactor with a Raney nickel catalyst deposited on the outer wall of the tube by flame spraying is effective in the practically complete conversion of 3H2+1CO synthesis gas to a high-Btu gas (methane) at an hourly space velocity of 7,000 volumes of gas (NTP) per hour per volume of annular volume. Partially reacted synthesis gas containing an appreciable amount of methane can also be treated in this reactor to increase the heating value to over 900 Btu per cubic foot. Excellent heat removal through the metal wall to a coolant and temperature control were obtained. The heat transfer co-efficient from the catalyst to the coolant was about 275 Btu per hour per square foot per ° F. Synthesis tests were conducted with tubes 1.2 inches in ad by 6 inches long, and 1.3 inches in od by 36 inches long. When operating at a synthesis gas rate of 100 to 120 scfh per square foot of catalyst-coated tube, catalyst life was long enough to realize a catalyst cost for the raw Raney nickel alloy of about 0.3 cent per 1,000 cubic feet of pipeline gas (900 to 950 Btu per scf). Gas recycling at ratios of 1:1 to 3:1 was effective in increasing conversion and in extending the life of the catalyst to about 16 weeks. In cost and in operating characteristics the tube-wall reactor compares favorably with the fluidized-bed and hot-gas-recycle reactor systems for the synthesis of high-Btu gas from H2+CO.

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 P. G. Clites

This study was conducted to determine the patterns of heat transfer to water-cooled copper crucibles during vacuum arc melting. Values of heat flux from the ingot to the crucible were determined during nonconsumable electrode vacuum arc melting of zirconium and during consumable electrode vacuum arc melting of titanium) zirconium) and steel. The results of these studies con-firm the existence of a high thermal resistance between the ingot and the crucible wall which results from the shrinkage of the ingot as the metal solidifies. Maximum heat flux occurs near the top of the ingot where maximum values of heat flux of 1.4 X 106 Btu/ft2 hr were observed during small-scale consumable electrode arc melting of zirconium and titanium. The maximum heat flux for consumable electrode arc melting of 8-inch-diameter ingots was 0.5 X 106 Btu/ft2 hr. The effects of electrode material) electrode diameter) arc current) and arc potential on heat flux from the ingot to the crucible were studied. Data were also obtained on crucible wall temperatures and on the effect of very narrow annular water jackets.

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 E. K. Kleespies

The Bureau of Mines determined the kinetics of the reaction of titanium-iron alloys with titanium trichloride dissolved in sodium chloride to provide a basis for understanding the reactions occurring in metallurgical processes involving reduction of the metal halides or alloy refining in fused salts. The rate of the heterogeneous reaction was determined between titanium-iron alloys and titanium trichloride to elucidate the effects of alloy composition on the rate. Measurements were made in an inert atmosphere with a high-temperature thermobalance using high-purity reactants. The rates of the reactions were about 1 x 10-5 g Ti/cm2-sec, and the reaction was phase-boundary controlled. Titanium alloys of the body-centered cubic beta structure reacted faster than those with the hexagonal close-packed alpha structure. The inter-metallic compound, TiFe, reacted very slowly, whereas TiFe2 was inert. Alloys containing above 89 atomic percent iron gained weight by reacting with titanium species in the salt solution and depositing titanium in the alloy. The effect of TiCl3 concentration on the reaction rate was determined from 2 to 12 weight-percent TiC13 and at various alloy compositions. At high iron contents, above 50 atomic percent, the TiC13 concentration effect was small. At lower iron contents, the TiC13 concentration effect was greater for beta-crystalline alloys than for alpha-crystalline alloys. The temperature dependence of the reaction between titanium alloy containing 8.7 atomic percent iron and titanium trichloride was measured over the temperature range 1,062° to 1,220° K, and the energy of activation was 7.7 kilocalories for the reaction.

Jan 1, 1967

By T. Estelle Gardner

The Bureau of Mines made enthalpy measurements on sodium bromide and sodium iodide in the temperature range 400° to 1,200° K using an ice calorimeter. Equations representing enthalpy as a function of temperature were derived from the data by the method of least squares. These equations were used to calculate smooth values of heat capacity, enthalpy, and entropy at 50° K intervals from the ice point to 1,200° K. The melting point determined for sodium bromide was 1,020° K; the melting point of sodium iodide was 934° K. The heats of fusion of sodium bromide and sodium iodide were calculated to be 6,270 and 5,680 cal/mole, respectively.

Jan 1, 1967

By C. C. Shale

Electrical resistivities for various coal ashes in air and in a nitrogen atmosphere are given over the range 100° to 1,500° F. Resistivity of low-carbon ash in air is very high at low temperature, rises to a maximum at about 250° F, decreases very rapidly with increasing temperature to about 800° F, then decreases gradually to approach an asymptote at 1,500° F. Resistivity of high-carbon ash in air follows this same general trend at values which are much lower and are proportional to the carbon content. After the carbon has been burned off, resistivity of the remaining ash approaches the high values corresponding to low-carbon ash of similar chemistry. Two factorial experiments show the effects of temperature, particle size, chemical content, and compressibility on the resistivities of four fly ashes of widely different chemical composition in the temperature range proposed for coal-fired turbines. Resistivities of all low-carbon ashes tested fall in the range 106 to 107 ohm cm at 1,500° F and should be removable by electrostatic precipitators. Ashes containing carbon in excess of about 8 percent, however, have low resistivity (as determined in nitrogen), especially at high temperatures. Therefore, high-carbon materials may not be collectable in precipitators because the resistivity is below the minimum value necessary for precipitation. Consequently, high carbon residues from partial combustion of coal probably could not be removed effectively at high temperatures.

Jan 1, 1968

By D. A. Wilson

A process was developed on a laboratory scale in which a solid waste byproduct from refining of secondary lead was converted into three valuable products. Roasted lead blast furnace matte was leached with water to recover copper. This was followed by brine leaching to recover lead. Residues were finally smelted to yield pig iron. Copper was precipitated as cement copper and the lead product obtained was a mixture of pure 3PbO.PbC12.xH20 and Pb(OH)C1. Copper recovery was 89 percent and lead recovery was 96 percent.

Jan 1, 1967

By M. L. Odenbaugh

The viscosity reduction effect of varied concentrations of leonardite (a naturally oxidized form of lignite) and leonardite-caustic on the rheological properties of a standard bentonite drilling fluid was studied and evaluated. The minimum plastic viscosity was found to occur at application rates of 4 lb of leonardite and 1.33 lb of caustic per barrel of drilling fluid. Leonardite-caustic treatment was not beneficial in treatment of salt-contaminated drilling fluids. Although filter loss rate was reduced; both yield values and gel strength were increased. Compared with other viscosity control agents) including quebracho) ligno-sulfonate) humic acids extracted from leonardite) as well as other reaction products of lignite) leonardite is less effective at low application rates but is an effective treating agent at rates of 2 Ib/bbl or more. Considering the comparable merits of the substance tested) the major factor in determining which agent to use should be based on cost consideration.

Jan 1, 1967

By T. E. Sterner

A laboratory investigation was conducted to determine the applicability of the thermal oil-recovery method as a means of increasing ultimate oil recovery in the Appalachian region. The primary objective was to establish self-sustained combustion in consolidated and unconsolidated sand test assemblies saturated with various amounts of Pennsylvania Grade crude oil and synthetic brine. Tests using blocks of sandstone were unsuccessful because of sealing problems and fracturing of the rock due to thermal stresses. A combustion wave of about 700° F was propagated through the sand-oil-water packs in the linear tube tests. The high air flux used resulted in high oil consumption and rapid movement of the combustion wave through the tubes. Analytical tests on the sand pack showed that sufficient fuel was deposited during the linear tube experiments for a self-sustained combustion wave.

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. M. Stuve

The standard heats of formation (?Hf°) of holmium trichloride and terbium trichloride were measured by solution calorimetry. Heats of solution of holmium and terbium metals and their anhydrous chlorides were measured in 4.360 molal HCI at 298.15° K. From these measurements ?Hf° for HoC13 (c) was calculated as -240,290 ±1,700 cal/mo1e, and ?Hf° for TbC13 (c) was calculated as -238,330 ±1,500 cal/mole at 298.15° K.

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 W. H. Engelmann

The electrokinetic (zeta) potentials of a charcoal granite in an aluminum chloride (AlCl3) solution and in an oleylanunonium acetate (C18H35NH3+ -OCOCH3) solution have been correlated with the specific damping values as measured by the pendulum sclerometer. This investigation shows that the pendulum specific damping attains a minimum at the isoelectric point for the charcoal granite-aluminum chloride and charcoal granite-oleylammonium acetate systems, and thus indicates that the penetration of the diamond points is a maximum at the isoelectric point.

Jan 1, 1967

By James A. Wasson

This report analyzes the petroleum-production potential of the basal Greenbrier dolomite zone, Sycamore-Millstone field, Sherman District, Calhoun County, W. Va., through the application of certain secondary-recovery methods. The well logs obtained and the core recovered from a well in this formation permitted an evaluation of the productive capability of the reservoir, Approximately 120,000 stb of oil may be produced from a 20-acre five-spot unit at breakthrough if the property is waterflooded. At an assumed limiting producing gas-oil ratio of 20)000 sef/stb, approximately 69,000 stb of oil should be recovered by low-pressure gas drive.

Jan 1, 1967

By M. J. Kovalik

The effects of the process variables on the production of chemical coke on a chain grate stoker, a type of traveling grate, were studied. Six bituminous coals, ranging in volatile matter from 16.7 to 43.8 percent, were successfully carbonized, yielding chemical coke with acceptable physical properties. The coke yields were dependent on the volatile-matter content of the coal. The air fuel ratio had the most marked effect on the yield and characteristics of the resultant coke, and the general furnace performance. Results can only be predicted; the actual yield and quality of coke obtained from any given coal can only be determined by actual tests using the optimum processing variables to obtain a coke with minimum volatile-matter content and to retain as much of the fixed carbon in the original coal as possible.

Jan 1, 1967