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By Robert E. Barieau

This report describes a method for treating pressure-volume-temperature (PVT) data obtained with a Burnett compressibility apparatus. The method makes use of a general nonlinear least-squares technique developed at the Bureau of Mines Helium Research Center. It is assumed that an adequate functional form is available for the expression of the compressibility factor as a function of either the molal density or the pressure. The functional form of the compressibility factor can be either linear or nonlinear in the parameters to be evaluated. Formulas are given for calculating variances and covariances of all parameters evaluated and for calculating the variance of calculated quantities of interest.

Jan 1, 1967

By D. Bienstock

The use of alkalized alumina in removing sulfur dioxide from a coal-combustion flue gas at 625° F was investigated on a pilot plant scale. The absorber was 26 feet long and 1.6 inches ED. Counter-current gas-solids flow at gas velocities of 8 to 15 ft/sec in the presence and absence of baffles, as well as solids entrainment at gas velocities of 20 to 23 ft/sec with solids recycle, were employed. The spent absorbent as regenerated as fixed bed with the reducing gases--reformed natural .7.7d hydrogen. Of absorption-regeneration were successful completed using the alkalized alumina rolled into spherical granules 10 to 16 mesh. There was no loss in activity of absorbent toward SO2 with a modest attrition equivalent to 0.l percent of the solids feed. Supporting studies were conducted on the effect of the sodium content in the absorbent, the composition of the reducing gas, thermal treatment to increase absorbent hardness, and removal of absorbed chlorine from the absorbent. A mathematical model was formulated to describe the removal of SO2 by alkalized aluminum from fixed and falling beds.

Jan 1, 1967

By L. C. George

The Bureau of Mines measured vapor pressures of selected mixtures in the binary system SnCla-ZnC12 by the static pressure method. Equations expressing the vapor pressure) and the heat and free energy of vaporization) as functions of temperature were developed by numerical analysis based on the sigma-plot method. It was found that the vapor pressure of any SnCl2-ZnCl2 mixture) at any temperature within the range of this investigation) could be accurately calculated from the derived values for the heat and free energy of vaporization for the mixture, with a probable error of 0.01 cm Hg or less.

Jan 1, 1967

By R. L. Andrews

The Bureau of Mines investigated means of electrodepositing iridium to form thick coatings suitable for the protection of such metals as tungsten and molybdenum, which oxidize rapidly at high temperatures. Using a fused sodium cyanide bath, thick, adherent, and coherent deposits of iridium up to 15 mils thick were plated on tungsten and molybdenum substrates at 600° C and current densities of 10 to 100 ma/cm2. Limited oxidation testing of molybdenum encapsulated with pure iridium indicates that the coating may offer protection to approximately l,000° C in flowing air, but that at higher temperatures, the volatility of its oxide limits use of pure iridium. Alloy coatings of iridium with platinum, palladium, and rhodium up to 4 mils thick were formed from a fused sodium cyanide electrolyte; because their oxides are less volatile, these alloys may protect substrates at higher temperatures. Deposits made from aqueous electrolytes either had very low rates of deposition or were highly stressed and cracked when heavy deposits were made.

Jan 1, 1967

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 Wilbur I. Duvall

In this report, the Bureau of Mines presents a theoretical solution for the stresses and displacements in an infinite elastic plate containing a circular hole the boundary of which is loaded by applied radial stresses over four separated arcs. The problem solved is a two-dimensional approximation of the stresses and displacements developed by a large tunnel-boring machine anchored in a circular tunnel. Analysis of the solution shows that the tangential tensile stresses induced on the boundary of the circular opening can be minimized in the roof and maximized in the floor of the opening by proper spacing and loading of the four arcs.

Jan 1, 1967

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