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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

By C. Kenneth Eilerts

A method is described for controlling instability in finite-difference computations of liquid saturation near the borehole of a recovery well. Differences of pressure-and saturation-dependent variables are indexed offcenter, upstream and downstream alternately, to provide a stabilizing average. It was found that size of the time step could be increased by a factor of 4 without loss of numerical stability. Finite differences of the variables occur in a variety of relative numerical sizes and combinations. Those relationships of the differences that contribute to instability may be identified by the computing program in which they occur and modified to assist convergence of the computations and execution of the partial differential equations of liquid and gas flow.

Jan 1, 1971

By Ralph B. Adair

The Bureau of Mines conducted laboratory batch and small-scale continuous tests on samples of silt from the Nolichucky Reservoir near Greeneville, Tenn., to develop a process for the recovery of commercial-grade muscovite concentrates. Using a combination of Humphreys spirals for preconcentration followed by cationic flotation, 94.5 percent of the muscovite was recovered in a product containing 96.5 percent muscovite.

Jan 1, 1971

By Judith A. Eisele

The possibility of improving the volatilization of gold through the formation of a metal-gold chloride vapor complex was investigated. Gold-silica mixtures, containing ferrous and nonferrous minerals and salts as additives, were treated in a laboratory tube furnace with a flow of chlorine gas at various temperatures. The addition of pyrite (FeS2) to a charge of gold-silica increased the volatility of the gold from 3, 20, and 62 percent of the total gold to 62, 93, and 100 percent at 200°, 300°, and 400° C, respectively. Chemical analyses of the condensate indicated the volatile species to be FeAuCl6.

Jan 1, 1971

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions2 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made, Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated the properties of zinc alloys containing 25 to 40 wt pet Al and 0 to 0.7 pet Mg. Microstructures, hardness, and tensile properties were evaluated for material as extruded at 285° C, solution treated at 300° to 400° C, and subsequently aged at 100° to 200° C. The alloys without magnesium are characterized by low hardness and strength with high tensile elongation and reduction in area. It was verified that magnesium effectively retards the Zn-Al eutectoid transformation below 275° C and markedly increases hardness and strength with decreases in ductility. Solution treating at 350° C results in large grain sizes and gross embrittlement. Subsequent aging of the Zn-Al-Mg alloys at 200° C restores ductility substantially and stabilizes the structures, but strengths are considerably reduced. Combined strength and ductility properties are better for the as-extruded condition than for any heat-treated condition. There is usually little advantage in overall tensile properties from increasing magnesium above 0.1 pct.

Jan 1, 1971

By W. E. Robinson

Sixty samples, selected from a 2,300-foot core of the Green River Formation in Colorado, were studied to ascertain differences in the structure of the organic material present in the oil shale samples. Emphasis was placed upon relating differences in the aromatic content of the insoluble kerogen and the alkane content of the extractable material obtained from the selected samples. The methods used in determining these differences consisted of fractionation of the soluble material, carbon and hydrogen analysis, volatile material determination, carbon residue determination, oxidation rate determination, and infrared analysis. In general, it was concluded that the organic material in this core does vary in chemical structure and that same of these variations resulted from factors related to depth of burial. Other observed changes in structure of the organic material were not depth-dependent and resulted from other factors such as source material variations, biological alterations, or ecological differences.

Jan 1, 1971

By M. L. Whisman

The Bureau of Mines developed a radiotracer method for detecting the contribution of selected components and additives to thermally induce deposits of turbine aircraft fuels. Fuels were examined before and after 52 weeks of storage at 130° F. Of particular concern was the influence of aromatic hydrocarbon fuel constituents on thermal-stability quality of jet fuels during storage. A microfuel coker test apparatus was used to thermally stress the test fuels and blends, and the resultant contribution to deposits of selected fuel components, labeled with carbon-14, was determined by radioactive-counting techniques. Ninety-one blends of five test fuels with carbon-14-labeled fuel additives or components were prepared, tested, stored for 52 weeks at 130° F, and reanalyzed for deposit-forming tendency. These additives included two anti-oxidants, a metal deactivator, and a corrosion inhibitor. Of the labeled hydrocarbon fuel systems studied, the greatest reaction was observed in blends containing methyl-and ethyl-substituted indenes. Other aromatic types also showed some contribution to the deposits. Three of the additives showed a marked tendency to degrade and react during storage and thermal stress. A cresol antioxidant, however, barely contributed to deposit formation. Oleic acid interacted with cadmium present in aircraft fuel systems and produced deleterious effects upon the thermal-stability quality of the fuel.

Jan 1, 1971

By K. C. Strebig

The effect of some organic additives in diamond drilling of quartzite was investigated in the laboratory with a drill instrumented to measure the rate of penetration, the thrust, and the torque and to record each as a function of the distance drilled. A statistical plan was followed throughout the investigation, and an equation representing the bit performance was derived from the mathematical theory of reliability. The coefficient of friction in drilling increased with the use of additives, although the wear coefficient decreased. The decrease in wear associated with an increase in energy per unit volume consumed and the increase in penetration rate resulted in a net decrease in the cost per foot of drilling. A hypothesis explaining the effects achieved with the additives is given.

Jan 1, 1971

By Richard F. Link

The principal procedures for the statistical analysis of gold assay and other trace-element data depend on applying either the normal frequency distribution or the lognormal frequency distribution. The consequences of applying both methods are examined through reference to example data from United States and South African gold mines. It is concluded that for estimation of average grades, except for certain data with a very high coefficient of variation (ratio of standard deviation to mean), use of the lognormal distribution is ordinarily undesirable because bias may be introduced and little efficiency can be gained. However, if biased average grades can be tolerated, as in the examination of data from surveys in exploration geochemistry, use of the log-normal distribution may be desirable. Various statistical analyses are detailed, and the tables presented to implement the analyses are more complete than those previously published.

Jan 1, 1971

By Robert M. Doerr

The research objective was to determine the effect of aluminum alloy additions on the oxidation behavior of cobalt-nickel alloys. Thirty high-purity alloys were reacted with 02 at 0.5 atm at 1,351°, 1,389°, and 1,429° K in a volumetric apparatus for about 300 min. The alloy compositions consisted of Co-Ni master alloys (0, 22, 50, 70, 91, and 100 wt pct Ni) with aluminum additions of about 0, 1, 2, 4, and 8 wt pet. Large early deviations from, or changes in, the parabolic rate constant were encountered, but in most cases, the reaction rate declined approximately in accordance with the parabolic rate law. A sharp peak in the parabolic oxidation rate constant was observed for specimens containing a to 22 percent nickel and 1 to 2 percent aluminum at 1,351° K, and the rate constants for these compositions were lower at the higher temperatures. Specimens containing 8 percent aluminum reacted far more slowly than did any of the others.

Jan 1, 1971

By E. J. White

Data from oil well logs and core analyses were used to quantitatively evaluate formation porosity and water saturation of heterogeneous carbonates and to study the pore geometry and performance characteristics of cores from these formations. Logs and cores from the Madison limestone from 233 wells in three fields in the Williston basin were used in the investigation. A comparison of log and core analyses shows that log porosities are consistently larger than core porosities, and the differences are correlatable with core porosity ranges. Water saturations from logs are usually smaller than the corresponding core saturations by summation of fluids, but the difference is attributable to mud filtrate invasion into the cores during drilling. Petrophysical studies show that the low permeabilities and high residual water saturations in these reservoir rocks are due to their fine crystalline texture and complex pore geometry (heterogeneity). It is concluded that both log and core analyses must be used for reliable evaluation of these carbonate formations.

Jan 1, 1971

By Jack C. White

Studies were made to determine the character and distribution of the copper lost in copper mill tailings. Acid soluble (oxide) and acid insoluble (sulfide) copper were determined for heavy-liquid sink and float products of screen-sized fractions from 12 copper mill tailings. In most of the tailings studied, the coarse-size fractions are higher in copper grade than the respective bulk tailings, high in sulfide copper, and low in oxide copper. Oxide copper occurs predominantly in the minus 325-mesh "slimes." Microscopic examination of heavy-liquid sink products indicated that recovery of liberated copper sulfide minerals is complete in most mills, and that copper minerals not being recovered are locked with gangue particles. Additional copper could probably be recovered from most tailings by size classification, scavenger froth flotation of the coarse fraction, and regrinding of the concentrate to achieve liberation of the locked sulfides.

Jan 1, 1971

By A. R. Taylor

Using solution calorimetry, the following heats of reaction were determined: (1) NaCN(c) + 1/Cu20(c) + 129H20(l) ? CuCN(c) + NaOH?128.5H2O ?H = -13.44±0.10 kcal/mole, (2) HCN(2) + NaOH?128.5H20 ? NaCN(c) + 129.5H20(l) ? = -2.52±0.02 kcal/mole. From these reactions, the heats of formation for CuCN(c) and HCN(2) were calculated to be 22.7±0.4 kcal/mole and 24.9±0.4 kcal/mole, respectively. Reaction 2 was made to check the consistency of literature values for heats of formation of HCN and NaCN. Adiabatic calorimetric measurements between 10° and 400° K showed the entropy and heat capacity of CuCN(c) to be 21.51±0.06 eu and 14.58±0.04 cal/mole deg, respectively, at 298° K. A broad anomaly in the heat capacity was found in the temperature range 285°-320° K. The heat of transition associated with this anomaly was less than 1 cal/mole, the sensitivity of the measurements.

Jan 1, 1971

By W. K. Overbey

Knowledge of fracture systems in oil or gas reservoirs is essential to the efficiency of both primary and secondary production operations. A relationship was established between structural features of the surface and both natural and induced fractures in oil and gas reservoirs, thus providing a method of predicting the direction of rock fracture prior to field development and well completion. Correlations between the surface features and under-ground fractures resulted from analysis of joint strike measurements, bottom-hole impression packer surveys, photographs of hydraulically fractured wells, fracture data from oriented cores, in situ strain measurements from formation outcrops, and lineament analyses from aerial photographs. The mean orientation of surface fractures, lineaments, and stress field directions ranged from N 53° E to N 73° E, compared with an average orientation of N 63° E for the hydraulically induced fractures. Tectonic stress field was shown to influence the direction of hydraulically induced fractures. This report presents the details and application of techniques to obtain the orientation of the principal horizontal compressive stress field component and thus the direction of induced fractures.

Jan 1, 1971