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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 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 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 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 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 Vance G. Leak

Leaching of manganese from low-grade Minnesota ores was studied over the temperature range 25° to 225° C at atmospheric and elevated pressures to demonstrate that good recoveries of manganese could be achieved from unroasted ores using reagents available nearby. Various combinations of ore, pyrite, lignite derivatives, and sulfuric acid were tested on a small scale. Pyrite alone required the highest temperature to effect a good extraction, but the combination of pyrite, lignite char, and sulfuric acid solubilized 99 percent of the manganese after 30 minutes of reaction at 75° C.

Jan 1, 1971

By Galen G. Waddell

This report describes a method of measuring and analyzing the initial deformation which occurs in the medium surrounding a mine accessway as the opening is created. Discussed are (1) the hypothesis upon which the research is based; (2) the in situ rock-deformation measuring equipment developed; (3) the field tests, consisting of measuring the deformation of the medium around two 4-foot-diameter raise bores as the boring progressed; and (4) a finite-element technique to correlate theoretical with experimental results, using elastic theory. Described also are the raise-bore operation and performance. The instrumentation developed proved to have the sensitivity and resolution necessary to measure rock deformation around a full-scale raise bore during excavation. Tests show the relationships of rock deformation to progress of the raise boring and to time. The initial deformation of the opening appeared to be elastic. Using the deformation records and an estimated field stress, the modulus of elasticity was determined for the rock mass. In addition, the importance of this type of measurement in assessing support-problem areas is discussed.

Jan 1, 1971

By Murray Jacobson

A method for determining airborne trona dust concentrations using a midget impinger was developed. During sampling, the trona dust, composed of sodium carbonate and bicarbonate, dissolves in the collecting medium (water). Resulting solutions are then titrated using 0.1 [N] hydrochloric acid solution. The mass concentration of the trona sample is determined from a calibration curve relating the volume of acid required for neutralizing a collected sample to the mass of the dust. Test results obtained using this method are equivalent to those obtained using a gravimetric sampling method.

Jan 1, 1971

By George S. Koch

Several methods of calculating ore grades by diamond-drill sampling in the Homestake mine, Lead, S. Dak., have been evaluated by statistical analyses of assay data. The natural distribution of gold particles, partly masked through sampling and assaying procedures, is probably lognormal. As a consequence of the gold particles being clustered rather than randomly distributed within the ore bodies, (1) more mine samples are needed to obtain a specified precision of mean grade than the number predicted by the standard-error-of-the-mean law; (2) the variance of gold values is not inversely proportional to sample volume, and, therefore, small-diameter drill core yields samples nearly as good as larger diameter core; and (3) sampling at 5-foot intervals provides nearly as good results as sampling at shorter intervals.

Jan 1, 1971

By E. G. Davis

This report summarizes an investigation to determine the occurrence and recoverability of heavy minerals in sand and gravel operations in the Southeastern United States. A total of 61 samples from 34 sand and gravel operations in Alabama, Georgia, South Carolina, and North Carolina were studied. Heavy minerals, in amounts ranging from 3 to 400 pounds per ton, were found in all of the samples. Eighty percent of the samples contained 20 to 40 pounds per ton of heavy min¬eral. Valuable heavy minerals, in order of decreasing amounts, were ilmenite, kyanite, zircon, rutile, and monazite. Large-scale concentration tests were made on five samples from four major producers. Gravity concentration by Humphreys spirals and tables resulted in bulk heavy mineral concentrates that graded from 82 to 98 percent total heavy minerals. Mineral recoveries ranged, in percent, as follows: Ilmenite 60 to 95; zircon 96 to 100; kyanite 37 to 77; rutile 89 to 100; and monazite 96 to 100. Separation studies on the gravity concentrates showed they would respond to high-tension and high-intensity magnetic separation techniques to produce individual mineral concentrates. The recovery of each individual mineral from fractionation of the heavy mineral gravity concentrates, in percent, was: Ilmenite 77 to 94; rutile 41 to 68; kyanite 62 to 79; zircon 49 to 83; and rare-earth products, monazite and xenotime, 42 to 96. The grade of each mineral concentrate was: Ilmenite 51.1 to 68.7 percent Ti02; rutile 93.7 to 94.3 percent Ti02; kyanite 55 percent A1203; zircon 58 to 61 percent Zr02; and rare-earth products containing 73.8 to 90.8 percent monazite and 4.8 to 12.7 percent xenotime.

Jan 1, 1971

By Robert Blickensderfer

Tungsten alloys with high-temperature strength properties, comparable to the best of alloys recently developed by others, were produced by a new process called here the oxyreaction process. The process involved additions of a powder of a reactive metal compound, ZrN, ZrW2, or HfW2, to a base metal powder, tungsten, which contained some oxygen. The powders were blended, compacted, sintered, and extruded. During sintering, diffusion and internal oxidation occurred to produce reactive-metal oxide particles and solid solutions. A dispersion of oxide particles could be precipitated by heat treating. The oxyreaction process circumvents many of the agglomerating and coarsening problems encountered in the current methods for dispersing a stable oxide in a metal. Oxyreaction strengthening results from solid-solution strengthening and from dispersion strengthening produced by the reactive metal and its oxides. At a test temperature of 1,650° C, the alloys prepared from WW, had tensile strengths up to 70,000 psi and stress-rupture lives up to 142 hr at 10,000 psi stress; the alloys prepared from ZrN powders had tensile strengths up to 80,000 psi and stress-rupture lives up to 27 hr at 10,000 psi stress. Tensile strengthening in the alloys was attributed to Zr in solid solution or to Zr-O-W structures too small to be observed in an electron microscope replica. Stress-rupture life was attributed to a dispersion of submicron Zr02 particles which precipitated and grew to 0.05-to 0.2-micron size during the test. Tensile strengthening and stress-rupture life were dependent upon both the zirconium and oxygen contents with the maximum occurring at roughly 0.9 atomic pot Zr and 0.9 atomic pot 0. Studies of the details of the oxyreaction process were made on the W-ZrW2 alloys and three general steps were determined: (1) The reaction of 0 in tungsten powder with ZrW2 to form relatively large Zr02 particles; (2) the dissolution of remaining ZrW2 into the W matrix and partial internal oxidation to form ultrafine but sparse zirconium oxide particles and possibly to establish Zr-O-W structures; (3) the development of ultrafine Zr02 particles during high-temperature aging.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated the properties and anisotropy in properties of rolled Zn-Ti and Zn-1.0 wt pct Cu-Ti alloys containing up to 0.36 wt pct Ti. Finish rolling was at varied temperatures to total reductions as high as 92 pct. Alloy properties are very sensitive to various combinations of composition, rolling temperature, and reduction. Properly rolled Zn-1.0 Cu-Ti alloys are superior in strength to Zn-Ti alloys. Conditions are described that lead to best tensile properties. Creep resistance for Zn-Ti alloys decreases with increased rolling temperature when finish rolled to 92-pct total reduction: but not when finish rolled to 33- or 67-pct reduction. Creep resistance for 7n-1.0 Cu-Ti alloys improves with increased rolling temperature to about 480° F. Heavily cold-rolled Zn-1.0 Cu-Ti alloys have fine grain sizes and poor hardness, tensile, and creep properties, but high ductility. Thermal expansivity is markedly affected by the copper addition. Data show the anisotropy of tensile, creep, and thermal expansivity properties. Large idiomorphic crystallites of TiZn15 appear in both Zn-Ti and Zn-Cu-Ti alloys when more than about 0.2 pct Ti is present. A new Zn-Cu-Ti intermediate phase was also identified. Empirical equations are presented relating creep rates with major process variables.

Jan 1, 1971

By J. D. Dixon

The Bureau of Mines investigated the principles of support-rock interaction, based on structural matrix methods which permit mathematical formulation of the problem and computer solution. The principles are given under two main sections: the first discusses the idealization of the tunnel support structural system for matrix analysis; the latter discusses the analysis procedures necessary for carrying out the solution. A general frame matrix computer program and a medium-size computer should be sufficient for carrying out the procedures involved. The example problem consists of a circular tunnel support which is subjected to a uniformly distributed vertical load, Three wall thickness-radius ratios are studied in combination with four support-rock modulus ratios. This problem illustrates the main procedures of the support-rock interaction analysis involved, and examination of the results reveals the influence of the relative rigidities of the support and the rock.

Jan 1, 1971

By P. G. Pigott

This Bureau of Mines laboratory research demonstrated that building bricks meeting ASTM specification C62-66 for grades SW and MW of FBS-type bricks can be produced from waste copper mill tailings. Waste tailings from accumulations at Magna, Utah, Anaconda, Mont., and Hayden, Miami, and San Manuel, Ariz., were dry-pressed into bricks, and the products were tested in accordance with ASTM Designation C67-66 on sampling, and testing of brick. An evaluation derived from pilot-plant production of similar brick at the Coal Research Bureau of West Virginia University indicated the production cost to be about $34 per 1,000 bricks. Utilization of such mill tailings on a commercial scale would eliminate the need for digging new pits for brick raw material production, conserve natural resources, and simultaneously remove potential sources of air pollution.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated creep and other properties of extruded Zn-30 pct-AI alloys containing 0 to 0.7 pct Mg. The alloys were extruded both above and below the Zn-Al eutectoid temperature of 275° C. Creep behavior is defined for the alloys as extruded and after various heat treatments. Tensile properties, hardness, thermal expansivity, impact resistance, and microstructures are given. The alloys, either with or without magnesium, required substantially less pressure for extrusion near 275° C than at higher or lower temperatures. The alloys containing magnesium exhibited significantly greater hardness, tensile strength, and creep resistance, but much lower ductility than the 2n-30 pct Al alloy. The properties were very sensitive to the processing conditions.

Jan 1, 1971

By F. D. Sutterfield

This study was conducted to provide experimental evidence on the effect of modifications of gasoline front-end composition on the photochemical specific reactivities of automotive emissions. Evaporative and evaporative-plus-exhaust emissions from an automobile operated with four fuels of different volatility and varying levels of C.-C5 olefins were irradiated in a 10040 environmental chamber at three sets of initial hydrocarbon-nitrogen oxides concentrations. Reactivity was measured and expressed in terms of rate-of-NO2 formation and dosages of oxidant, peroxyacetyl nitrate, and formaldehyde. The compositional changes that were necessary in reducing fuel volatility were found to have no significant effect on the reactivity of the emissions. However, replacing C4-C5 olefins with saturated components resulted in sharp decreases in all reactivity manifestations observed for the evaporative emission samples. A lesser influence (of C4-C5 olefin replacement) was found with the composite exhaust-plus-evaporative samples; the effect that was observed could be attributed to the evaporative emission portion of the sample. The data therefore suggest that saturation of front-end fuel olefins had no large effect on exhaust emission reactivity.

Jan 1, 1971

By Robert E. Wood

[The temperature dependency of the low-density thermal conductivity coefficients, ?°T, of nitrogen, 100° to 1,200° K, is correlated with the Keyes' equation, ?T ½ -1 -12/T) WT = aT+ bT 10 The equation ?T,P = ?°T +a[ ]ß represented 509 experimental higher V pressure thermal conductivities in the temperature range 131.2° to 973.15° K for pressures to 500 atmospheres, with a mean absolute deviation of 2.35 percent. This equation was used to compute thermal conductivities of gaseous nitrogen for 47 pressures, 1 to 240 atmospheres, and 110 temperatures, 133° to 740° K, which are common to conditions encountered in Bureau of Mines helium purification processes. Isobaric heat capacities, CP, and viscosities, ?T,P, from previous work were combined with the present thermal conductivities, ?T,P, to compute Prandl1 numbers, C?T P / ?T ,P, of nitrogen. Tabular values of Prandtl num¬bers are presented for 49 pressures, 1 to 240 atmospheres, and 75 temperatures, 133° to 740° K. Estimated uncertainties are ±5 percent in the tabulated thermal conductivities and ±15 percent for the computed Prandtl numbers. However, the uncertainty may rise to ±10 percent for thermal conductivities and to ±30 percent for Prandtl numbers as the critical conditions of nitrogen are approached.]

Jan 1, 1971

By J. A. Lamonica

The Bureau of Mines conducted an environmental noise survey to determine the noise levels to which underground coal mine employees are exposed, to evaluate noise survey techniques and equipment, and to compare noise exposures using two criteria, Walsh-Healey and CHABA, for determining allowable exposures that were under consideration for the Federal Coal Mine Health and Safety Act of 1969- Time study techniques and Bureau-approved standard sound level meters were employed. The shift exposures of 20 percent of the miners studied were in excess of the safe standards established by both criteria. The shift exposures calculated using the Walsh-Healey criteria were greater than those calculated using the CHABA criteria owing to the intermittent nature of the exposure. Ultimately the CHABA criteria were rejected, and the Walsh-Healey criteria were adopted.

Jan 1, 1971

By I. L. Nichols

The inplace cyanidation leaching of gold from placer deposits is a potential method for treating gravels too deeply buried and too low in gold content to be processed economically by conventional dredging methods. Laboratory experiments were made to evaluate those placer cyanidation factors adaptable to small-scale studies. The variables investigated included gold particle size and location in sand beds, cyanide solution flow rate, and cyanide solution strength as factors affecting gold solubility rates. The solution flow rate, in turn, was influenced by variables such as bed slope, solution head pressure, and sand size, and the effects of these factors were studied. Free gold, minus 150-mesh and finer in size, is rapidly dissolved by dilute cyanide solutions from mixtures of gold and silica sand prepared to simulate placer deposits. About 94 percent of minus 325-mesh free gold was extracted in 5 hours from silica sand mixtures, and 94 percent extraction of minus 150-mesh gold was obtained in 21 hours with 0.1 percent NaCN solutions. Moving solutions were almost twice as effective in leaching free gold from silica sand mixtures than stagnant solutions.

Jan 1, 1971