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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 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 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 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 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 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 K. E. Stanfield

Oil-yield results are presented for 65 oil-shale sections in Piceance Creek Basin, Colorado, sampled during the period 1957 through 1963. Including previously published data, oil-yield results for 203 sampled sections have now been released by the Bureau of Mines to aid in appraising the shale oil potential of the basin. Oil yields of core samples (135 sets) were regarded as reliable bases for appraising the Mahogany-zone interval, but only 5 sets of cores sampled the deeper, lower-zone oil shales. Drill cuttings (68 sets) sampled the lower-zone oil shales, but their oil yields are principally indicative and should be confirmed by analyses of cores. More complete core sampling of the lower-zone oil shales is needed.

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 Dean E. Bluman

The Bureau of Mines investigated the convective heat transfer coefficients for recirculated suspensions of 30-micron glass beads in inert gas. Coefficients for the suspensions were not significantly higher than coefficients for the pure gas. Reynolds numbers of the suspensions were 20,000 to 35,000; solids loadings ranged from 0.0 to 0.7 pound per pound of gas. Comparison of the results with published data showed the direction of heat flow to have no effect at the test conditions.

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 Elton L. Litchfield

The Bureau of Mines determined minimum energies for direct initiation of expanding gaseous detonation waves in acetylene-oxygen mixtures. Composition limit ranges for the initiation of detonation with fixed energies have been compared to data in the literature. Assuming that the stored electrical energy is completely converted to thermal energy, the agreement between the energy of primary explosive initiators and the energy of electrical discharge initiators was good. Minimum energies for initiation of detonation in the most sensitive composition (40 percent C20 plus 60 percent 0 2) were: 0.64 joule at an initial pressure of 1/4 atmosphere, 5.0X10-2 joule at 1/2 atmos¬phere, and 3.7X10-3 joule at I atmosphere. Fuel concentrations in mixtures initiated to detonation by 4.9X102 joules ranged from 10 to 65 percent C2H2 at 1/4 atmosphere, 10 to 67 percent C2H2 at 1/2 atmosphere, and 9 to 68 percent C2H2 at 1 atmosphere.

Jan 1, 1967

By C. Gary Reiness

A safety glass eyepiece which had been repeatedly exposed to mine environment over a number of years was studied to determine some of its optical properties. In the regions from 385 to 400 mµ and from 625 to 760 mµ, the transmittance was less than the 89 percent required by the American Standard Safety Code for Head, Eye, and Respiratory Protection. From 200 to 320 mµ the relative transmittance of two parts of the eyepiece was found to vary widely, having a maximum of 38 percent difference at 315 mµ. Irradiation of the glass by ultraviolet light caused enhanced absorption in the range from 200 to 1,200 mµ. There was a time-dependent increase of 1016 color centers per cubic centimeter throughout this range after 36.5 hours of irradiation. The rate-of-growth curve for the optical density, at 243.5 mµ and 23° C, was resolved into linear and saturable components, indicating zero order and first order

Jan 1, 1968

By R. K. Koch

The vapor pressures of liquid molybdenum and liquid zirconium were determined by the Langmuir free-evaporation method. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. The vapor-pressure data led to the following equations: [log p (atm) = 5.429 - 28,380 T for liquid molybdenum in the range 2,890° to 2,990° K, and log p (atm) = 6.521 - 30,940 T for liquid zirconium in the range 2,229° to 2,795° K.] Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 157.6 ± 1.8 kcal/mole and 148.4 ± 2.4 kcal/mole for molybdenum and zirconium, respectively, where the uncertainties are two standard devia¬tions. Second-law standard heats of sublimation determined from sigma plots and tabulated enthalpies were 143.5 ± 2.7 kcal/mole and 149.2 ± 3.8 kcal/mole for molybdenum and zirconium, respectively. The better agreement in heats of sublimation for zirconium is attributed to the 566° K temperature range studied which permitted a more accurate definition of the vapor pressure curve than could be obtained from the 100° K span for molybdenum. This supposition was verified by making a sigma-prime plot which utilized solid vapor pressure data for molybdenum to extend the evaluation range by 800° K. This gave a standard heat of sublimation of 155.2 ± 1.6 kcal/mole which is in good agree¬ment with the third-law value. The plot also gave a standard entropy of sublimation (298.15° K) of 35.73 ± 0.48 eu.

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 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