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By Albert W. Deurbrouck

This Bureau of Mines report describes the washability characteristics of 13 coalbed samples collected in Colorado. Such data are needed to evaluate the quality of the coals of the West, where most of our low-sulfur-content coal reserves are found. Of the 13 samples included in this report, 11 had a total sulfur content of 1 percent or less. All of the samples contained low percentages of ash or could be readily washed to a desirable ash level with minimal loss of yield. The coals ranged in rank from high-volatile A bituminous to subbituminous B; nine of the samples were high-volatile C bituminous. The coalbeds ranged in thickness from 6 to 26 feet; the average was about 8 feet.

Jan 1, 1970

By B. J. Dalton

The Bureau of Mines Helium Research Center has developed a computer program for solving two-phase equilibria data for binary mixtures and for evaluating thermodynamic functions of interest, including all critical points. This computer program was used to calculate equilibrium points on the PVTu surface for the helium-nitrogen system as predicted by the Van der Waals equation of state. Numerical values are tabulated and illustrations are presented for 1,279 equilibrium points and for quantities needed to construct Ponchon diagrams. Equilibrium ratios as a function of pressure at constant temperature and of temperature at constant pressure-are also shown graphically. In addition, saturated partial molal volume and partial molal enthalpy data are given. It is shown that the Van der Waals helium-nitrogen system exhibits retro-grade condensation of the second type for liquid helium concentrations of about 0.07 mole fraction or less and pressures below about 45 atm. It is also shown that the critical point is at a -maximum value of pressure (at constant temperature) and of temperature (at constant pressure).

Jan 1, 1971

By Paul Biggs

This Bureau of Mines report provides information on 138 waterflood projects in Wyoming. Injection was in 25 producing zones and 65 fields. Specific data presented include field location, discovery and development, water supply and injection, oil and water production, estimates of oil in place, and oil recoveries by primary and secondary methods. The 138 projects studied will, if successful, recover about 800 million barrels of secondary oil. Almost all of the injection water is from deep water wells.

Jan 1, 1970

By Raymond M. Stateham

Microseismic noise rates and slope movements were measured in an unstable area along the north wall of the Tripp-Veteran pit, Kennecott Copper Corp., Ruth, Nev. Low-noise, wide-band microseismic geophones were located at various points in the wall, and the change in distance across open fractures, resulting from instability, was determined by repeated measurements between fixed points set on each side of the fractures. The microseismic noise rate increased and decreased with corresponding increases and decreases in the rate at which the fractures opened. The microseismic noise rates and changes in width of the fractures show excellent agreement, and the two types of measurements complement each other in monitoring the progress of pit wall failure.

Jan 1, 1971

By J. R. Ross

Recovery of uranium from slightly alkaline mine water, available in the Ambrosia Lake district of New Mexico, was studied using countercurrent ion exchange columns developed by the Bureau of Mines. Approximately 5 million gallons of mine water containing 9 to 12 ppm U308 was treated by ion exchange using a 14-inch-diameter absorption column composed of five or six compartments each 4 feet deep. Uranium recoveries averaged in excess of 98 percent at solution flows ranging from 15 to 25 gallons per square foot per minute and resin loadings up to 3.6 pounds of U.08 per cubic foot. In subsequent tests, loaded resin was continuously eluted in a countercurrent elution column with a diameter of 4 inches and containing a bed of resin 9 feet deep. The resin was eluted to a residual loading of less than 0.06 pound of U305 per cubic foot, at a resin-retention time of 224 minutes, using only 1.9 volumes of 1.1 M NaCl-0.05 M NaHCO3 solution per volume of resin. Compared with existing ion exchange practices for recovering uranium from mine waters in the Ambrosia Lake district of New Mexico, use of these improved ion exchange contactors would reduce ion exchange resin requirements at least 70 percent and allow further substantial reductions in capital and operating costs.

Jan 1, 1971

By E. E. Remmenga

Often a collection of analytical data, which should reasonably be expected to follow the normal distribution, contains too many extreme values, which the experimenter is inclined to eliminate according to some arbitrary procedure. The stepwise computer procedure described for this purpose is similar to many other truncation procedures; however, because truncation of a basically normal distribution causes a downward bias in the estimated variance, this procedure provides a graphical method to compensate for the bias.

Jan 1, 1971

By P. T. Brooks

Mineral nodules from the ocean floor represent a vast potential source of manganese, nickel, cobalt, and copper. Process development studies to devise methods for recovering these metals were conducted by the Bureau of Mines using two types of nodules--relatively low-grade calcareous nodules from the Atlantic Ocean and higher grade siliceous nodules from the Pacific Ocean. Ammoniacal carbonate leaching of reduced nodules appeared to have the best potential for processing the calcareous nodules, but the method proved to be impractical for recovering manganese. Extraction of 90 percent or better of the nickel, cobalt, and copper showed the technique to be attractive for recovery of these metals. The siliceous nodules appeared amenable to a process that starts with either a sulfur dioxide leach or a sulfation roast followed by a water leach to dissolve the soluble sulfates.

Jan 1, 1971

By F. P. Haver

Because of increasing concern with air pollution, the Bureau of Mines has developed a hydrometallurgical procedure to obtain elemental sulfur from chalcopyrite (CuFeS2) by means of the following reaction: CuFeS2 + 3FeCl3 ? CuCl + 4FeCl2 + 2S. Under optimum conditions, 99.6 percent of the copper and 71.6 percent of the iron were extracted in 2 hours from a typical mill concentrate containing 75 percent CuFeS2 and 15 percent pyrite (FeS2). At the same time, 68.2 percent of the sulfur in the concentrate was oxidized to the elemental form. The leach was highly selective; gangue minerals, including pyrite, were not attacked, thus accounting for the relatively low recoveries of iron and sulfur. To obtain these results, the concentrate was ground to 98.9 percent minus 325 mesh, and 300 grams was treated with 1 liter of boiling ferric chloride (FeCl3) solution. The FeC13/CuFeS2 ratio was 2.7. Cement copper containing 99.9 percent copper was recovered from the leach solution by cementation on sponge iron. Excess iron, dissolved during leaching and cementation, was removed from the stripped solution by crystallization. Ferrous chloride (FeCl2?4H2O), obtained as a byproduct, was converted to high-purity ferric oxide (Fe203) and HCI by an oxidizing roast. The hydrochloric acid was then electrolyzed to obtain chlorine, which was used to regenerate the leach solution. The leach residue, which contained ~50 weight-percent elemental sulfur, was treated with an organic solvent to recover the sulfur and cyanided to reclaim gold and silver.

Jan 1, 1971

By F. E. Joyce

The Bureau of Mines studied copper-nickel minerals (mainly sulfides) of the Duluth Gabbro Complex in north-eastern Minnesota to determine their response to selective high-temperature sulfatization techniques. The gabbro, containing 0.44 percent copper and 0.13 percent nickel, was ground to minus 325 mesh and sulfatized in a heated, rotating, stainless steel bench-scale retort. Tests demonstrated that over 95 percent of the copper and 80 percent of the nickel can be converted to water-soluble sulfates, depending upon the roasting conditions employed. Yield equations were developed using regression analysis for predicting the extraction of copper and nickel between the temperature limits of 520° to 670° C, the roasting time limits of 3 to 7 hours, and S02 limits of 10 to 40 percent in S02-air mixtures.

Jan 1, 1971

By Hillary W. St. Clair

This report describes an experimental method for determining parameters for the rate of reaction of CO2 with solid carbon. The method involves the simulation of a flow reactor by a mathematical model based on a hypothetical multistage reactor which permits calculation of the analyses of effluent gas and carbon consumed as functions of the flow rate and duration of the reaction. The method is applied to experimental data on the reaction of coke with CO2 in fluidized-bed and fixed-bed flow reactors. A method is described whereby two parameters may be determined simultaneously. The method involves a reiterative procedure that finds the values of the parameters that minimize the sum of squares of deviation between calculated and observed analyses of the effluent gas.

Jan 1, 1971

By C. Daniel Kealy

Finite-element,, mathematical models that solve LaPlace's and Richard's equations numerically were used to locate the phreatic surface within tailings pond embankments and to define the subsurface flow of water from the pond. Both must be known to design structurally and environmentally safe tailings dams. The permeability distribution within and beneath the embankment, the fluid potential values upgradient and downgradient from the embankment, and the geometry and elevation of an approximately impermeable layer at some depth beneath the embankment were used as computer inputs in analyzing over a dozen finite-element models of tailings dams varying structurally from simple to complex. Results predicted with the finite-element model were confirmed with measurements in a laboratory model of a tailings pond and in the field. Of particular importance to the design of safe slopes, all data indicated that the phreatic surface within a tailings dam is concave upward, a configuration opposite that in most earth dams. The close correlation between predicted and experimental values confirmed the practicability of using the finite-element technique to design safe tailings dams.

Jan 1, 1971

By J. W. Town

The Bureau of Mines studied the effects of reducing gas composition, tem-perature, and superficial gas velocity on the regeneration rate of alkalized alumina. Regeneration was assumed to follow the simple first order reaction for removal of sorbed S02: dµ/dt = -Kµ. An Arrhenius relationship can be plotted, which shows an activation energy of about 75 kcal/mole for simulated reformed propane. The general effects of the individual gases can be described as follows: (1) CO and H2 produced rates proportional to their con-centrations, up to about 5 percent for each; (2) addition of CO2 had no effects on the regeneration rate by CO; (3) the regeneration rate by H2 was lowered by the addition of H2O while the regeneration rate by CO was increased by 0 addition; (4) H2S showed a positive effect up to concentration levels of about 2 percent and then produced a rapid negative effect; (5) carbonyl sulfate (COS) increased the sulfur content; and (6) propane was as effective in regenerating the loaded pellets as was simulated reformed propane.

Jan 1, 1971

By Gene Asai

Properties obtained for columbium carbide-carbon castings ranging in car-bon content from 12 to 17 weight-percent were compared with those of hot-pressed composites of similar composition. The properties were oxidation resistance in static air between 500° and 700° C, linear thermal expansion between 20° and 2,400° C, electrical resistivity between 20° and 1,500° C; microhardness between 20° and 1,500° C, and modulus of rupture between 1,300° and 1,800° C. CbC-C castings differed markedly from hot-pressed material with respect to microstructure, electrical resistivity, and modulus of rupture, but behaved quite similarly with respect to oxidation resistance, thermal expansion, and hot hardness. In oxidation resistance, thermal expansion, and hot hardness both materials were independent of carbon content. Both castings and hot-pressed composites oxidize rapidly in air above 600° C, have thermal expansion coefficients very similar to columbium metal, and the logarithm of the hardness decreases linearly with increasing temperature. The microstructures of hot-pressed composites contained varying amounts of graphite in a CbC matrix but did not contain significant amounts of a eutectic structure present in all castings, nor did they contain graphite needles which were present in the hypereutectic castings. The higher electrical resistivity of hypereutectic castings over hypereutectic hot pressings was attributed to the presence of highly oriented graphite needles in the castings. The modulus of rupture of castings was 1-1/2 to 2 times that of hot-pressed composites. Both materials displayed bend ductility above 1,800° C.

Jan 1, 1971

By J. D. Marchant

Solid-state electrotransport of impurities in cerium, lanthanum, and praseodymium, using a pulsed current, was investigated. The results were compared with those of using a steady current. Impurities that showed appreciable movement with the pulsed current, but not with the steady current, were as follows: Molybdenum and oxygen in cerium, aluminum, iron, and molybdenum in lanthanum. The use of a pulsed current enhances the practical application of solid-state electrotransport to remove a wider variety of impurities from the host metals.

Jan 1, 1971

By Thomas O. Llewellyn

Laboratory semicontinuous and continuous heavy liquid cyclone separation pilot plant tests were made to determine the feasibility of producing a high-grade kyanite concentrate from a kyanite-quartz rock sample from Graves Mountain, Ga. Use of a three-stage heavy liquid cyclone circuit demonstrated that a 96.4-to 99.0-percent kyanite concentrate could be obtained with recoveries of 95.5 to 96.7 percent. The test work showed that by steam stripping with 6.9 tons of steam per ton of ore and two stages of detergent scrubbing the residual TBE content of kyanite cyclone products was 0.22 pound per ton of ore.

Jan 1, 1971

By R. L. Wise

Heat content studies were conducted on burned shale, spent shale, and three grades of raw oil shale from the Green River Formation. Corrections were made for product enthalpies. The results were compared with previous work, indicating good agreement below retorting temperatures, but some differences at retorting temperatures. A general equation was developed relating heat content to oil-shale grade and temperature.

Jan 1, 1971

By L. A. Haas

The feasibility of removing sulfur dioxide by carbon monoxide reduction in a fixed-bed catalytic reactor was investigated by the Bureau of Mines. The reduction rate of sulfur dioxide with carbon monoxide was significantly dependent upon the iron and alumina content of the mixed catalyst. Maximum catalytic activity was obtained with about 40 percent iron-alumina mixture with a nominal gas mixture of 10 percent carbon monoxide, 5 percent sulfur dioxide, and the balance nitrogen. The synergistic effect of this catalyst mixture was explained by a dual reaction site mechanism, with both iron and alumina augmenting their specific sites at their interparticle contacts. The catalytic activity also increased with decreasing catalyst pellet size. With O.7-mm pellets, the entire pellet appeared to be catalytically active in a 2-gram catalyst bed. The apparent activation energy of the reaction was 18.3 kcal per mole in the temperature range of 350° to 600° C. Carbonyl sulfide (COS) was produced by the interaction of carbon monoxide and sulfur. The amount decreased with decreasing CO concentration. The ratio of COS formed per SO2 removed reached a maximum at about 400° C. The reaction rate appeared to be independent of S02 concentration in the range of 0.2 to 16 percent. The rate, however, increased directly with the CO concentration in the range of 5 to 20 percent. The presence of CO2 (<15 percent) had no appreciable effect on the rate. However, not over 0.5 percent oxygen could be tolerated. This method appears feasible for removing S02 from waste gas if the oxygen is removed prior to the catalytic S02 reduction process.

Jan 1, 1971

By K. P. V. Lei

An electrochemical process was developed for the preparation of vanadium from vanadium carbide. Commercially available vanadium carbide (V2C) was used as the starting material. Vanadium was obtained by electrolysis of the V2C in a BaCl2-KCl-NaCI-VCl2 electrolyte at 670° C using a helium-atmosphere, molten-salt electrolytic cell. Vanadium products were recovered with purities high as 99.6 percent. Current efficiencies of 87 percent and vanadium recoveries of 84 percent were attained. The cathode products were amenable to electrorefining to high-purity vanadium of 99.96-percent purity.

Jan 1, 1971

By M. J. Ferrante

The Bureau of Mines investigated the applicability of the freeze-drying technique for preparing dispersion-strengthened tungsten powders suitable for conversion by powder metallurgy into materials which might have improved high-temperature strength. Extruded rods from compacts of tungsten-5 vol pct thoria had at 1,650° C a tensile strength of 30,300 psi and a 10-hour stress-rupture strength of 12,700 psi, These are slightly below those measured for swaged rods of commercial tungsten-3.7 vol pct thoria. Only those tungsten-thoria dispersions containing a stoichiometric deficiency of oxygen yielded a significant strengthening effect. A low-melting eutectic formed in extruded tungsten dispersions containing either zirconia or yttria, which caused a lowering of the tensile strengths. These tensile strengths were only slightly higher than strengths of elemental tungsten made from commercial powder having a particle size of 2.4 microns (Fisher subsieve). Sheet made from this commercial tungsten had a slightly higher tensile strength than tungsten made by freeze drying, but the freeze-dried tungsten sheet had a lower recrystallization temperature, a lower ductile-to-brittle transition temperature, and a higher purity.

Jan 1, 1971

By George S. Koch

A statistical analysis of silver assay data from rotary-drill-hole cut-tings and diamond-drill-hole cores from the Round Mountain prospect, Custer County, Colo., demonstrates several useful methods for estimating grades and tonnages of ore from the drilling of wide-spaced holes in disseminated deposits of precious metals. A new method of are appraisal is introduced which estimates grade and tonnage of are by calculating convex hulls (smallest convex polygons) for sample points with assay values above specified cutoff grades. Analyses of variance compare the consistency of data from rotary-and diamond-drill holes, from rotary-drill holes sampled at 2-and 4-foot intervals, from two methods of sample preparation, and from atomic-absorption and fire assaying. Evidently, data from the two types of drill holes, from holes sampled at the two intervals, and from different methods of preparation are in agreement. Atomic-absorption silver values are consistently lower than fire-assay silver values.

Jan 1, 1971