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By Manuel Gomez

Published experimental coke data from a pilot plant slot-type oven were examined by statistical regression analysis. Quantitative relationships were found to exist between the coking rate, bulk density, and fine grinding of the coal, sole-oven expansion, volatile matter, moisture, ash, and carbon con-tent of the coal and coke parameters indicative of size and strength. Regression equations developed from coke data were shown to yield computed values that were in good agreement with experimental results for 11 coke properties. Prediction equations developed were evaluated with an independent set of data. Present results indicate that the variables cited undergo much interaction and the sum of these interactions determines coke size and strength.

Jan 1, 1967

By Jr. Driscoll

The thermoelectric properties of yttrium monoarsenide, yttrium monoanti-monide) and ternary materials from the Y-As-Se and Y-Sb-Te systems were investigated by the Bureau of Mines from room temperature to 1,000° C. The maximum calculated figure of merit for yttrium monoarsenide and yttrium monoantimonide was 2 x 10-5 ° C-1. YAs and YSb were semimetallic conductors with low Seebeck coefficients and electrical resistivities. The values of the Seebeck coefficient and electrical resistivity of the Y-As-Se and Y-Sb-Te materials were between those of the yttrium selenides and tellurides and of YAs and YSb, respectively. The maximum power factor calculated for the Y-As-Se materials was 2 X 10-5 watt/cm ° C2 which yielded an estimated figure of merit of 6 X 10-4 0 C-1. Most of the Y-As-Se compounds had high Seebeck coefficients and moderately low electrical resistivities. The Y-Sb-Te materials were degenerate semiconductors with power factors of 6 X 10-8 watt/cm ° C2.

Jan 1, 1967

By Alla D. Mah

Heat content and entropy data at high temperatures were obtained for cuprous oxide (Cu2O) and cupric oxide (CuO). Experimental results and smooth values are reported. Equations are given for heat content increments and heat capacities above 2980 K. Low-temperature heat capacity data were obtained for cuprous oxide. Evaluation of the 2980 K entropy gave, S°298.15(Cu2O) = 22.08 ± 0.10 cal/deg mole. Heat of formation values were determined for cuprous and cupric oxides. The values are: AH°298.15(Cu2O) = -40,830 ± 300 cal/mole, and AH°298.15(CuO) = -37,230 ± 150 cal/mole.

Jan 1, 1967

By Theodore Kessler

The purpose of this Bureau of Mines investigation was to determine what new organic compounds or high concentrations of a particular organic species can be formed by exposure of coal derivatives to ultrasonic energy. Tetralin, l-methylnaphthalene, and pyridine were used as model compounds. Gaseous and solid reaction products resulting from the ultrasonic irradiation of these coal derivatives were determined using mass spectrometry. Products from the irradiation of tetralin were studied as a function of time, atmosphere, and sample size. The sonolysis (chemical reactions produced by ultrasonic energy) of tetralin and l-methylnaphthalene produced C2H2, HCN, CH4, H2, CO, and CO2, depending upon the experimental conditions. The ultrasonic irradiation of tetralin also produced diacetylene under certain experimental conditions. The cleavage of organic chemical bonds by ultrasonic cavitation in the absence of water was also observed in this study.

Jan 1, 1967

By James H. Russell

The Bureau of Mines used a statistical approach to evaluate the effects of temperature, current density, and composition of the electrolyte on the purity of boron prepared by electrolysis of a fused mixture of boric oxide in potassium fluoborate. The quadratic equation which best fits the data was calculated for a temperature of 650° to 850° C, a cathode current density of 40 to 1,150 amp/ft2,and a boric oxide content of 0.3 to 7.1 molal. The best products, better than 95 percent boron, were obtained when the current density was less than 2 amp/ft2 and the boric oxide content was less than 2 molal.

Jan 1, 1967

By Webster S. Anderson

The design, development, and testing of hydraulic props to provide a lightweight, high strength, recoverable unit is described. Modifications in design incorporating threaded components resulted in the development of a lightweight hydraulic prop fabricated from aluminum alloy tubing. This new design facilitates interchange and replacement of component parts, and the physical properties of the material are not changed as they are when welding is required. The new prop is 65,000 pounds and has a maximum load capacity of a lower weight-to-load capacity ratio than the hydraulic props now available.

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 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 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