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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 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 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 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 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 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 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