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By J. E. Murphy

Purification of samarium metal by sublimation and by vaporization from a low-melting metal flux, at the same temperature, were compared. Vaporization proved more effective for removing impurities such as magnesium, calcium, and manganese. Recovery of samarium, however, is more rapid by sublimation because of its constant rate of distillation.

Jan 1, 1970

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 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 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

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 W. F. Marshall

This report describes exhaust-emission data from 10 diesel engines: six 4-cycle, direct-injection, naturally aspirated engines; two 4-cycle, direct-injection, turbocharged engines; one 4-cycle, precombustion-chamber, turbo-charged engine; and one 2-cycle, direct-injection engine. These engines were tested over a 3-year period (1968-70). Lowest emissions were obtained with a precombustion-chamber engine. Emissions from the 2-cycle, direct-injection engine fell within the range of emission rates for the 4-cycle, naturally aspirated, direct-injection engines. Excluding the precombustion-chamber engine and excepting one of the 4-cycle, naturally aspirated engines, carbon monoxide emission rates were about the same for all engines tested. Test data on smoke, odor, and emissions of hydrocarbons, oxides of nitro-gen, carbon monoxide, and aldehydes are given.

Jan 1, 1971

By R. F. Abernethy

A small-scale method was developed for determining the free-swelling index of coal samples of limited quantity, especially the macerals. Results of a series of tests using a 0.3-gram sample correlated well with those by the standard method using a 1-gram sample. The standard and small-scale methods are modified to give unrestricted swelling for those coals having swelling index numbers above 7.

Jan 1, 1971

By J. M. Stuve

Calorimetric determinations of the low-temperature heat capacities, standard enthalpy of formation, and high-temperature enthalpies were made of (Na20)4 ?Fe20,(c). The resulting values of entropy (S°), enthalpy of formation (?Hf°), and free energy of formation (?Gf°) at 298.15° K are 104.676 cal/deg mole, -656.2 ±.kcal/mole, and -603.4 A kcal/mole, respectively. Tabulations of Cp°, S°, - (G°-H°298)/T, H°-H°298, ?Hf°, ?Gf°, and log Kf are given to 1,200° K.

Jan 1, 1971

By Lester J. Crow

A preliminary survey was performed to investigate the impregnation of relatively weak, porous volcanic tuff and a relatively strong, dense sandstone with five different monomers. Increases in compressive strengths by factors of 2 to 5, and elastic moduli by factors of 2 to 3.5, are reported for natural rocks (tuff., sandstone, dacite), which were impregnated with five monomers (methyl methacrylate; chlorostyrene; 40 percent TMPTMA-60 percent styrene; 40 percent TMPTMA-60 percent chlorostyrene; 60 percent polyester-40 percent styrene); polymerization took place after monomers were forced into the rock. Impregnation was performed (1) by pressurizing rock specimens from one end, or (2) by a vacuum-soak operation. Polymerization was accomplished by either radiation or chemical initiation techniques. Strength improvement is dependent on (1) the type of monomer used, (2) the amount of polymer incorporated into the rock, and (3) the degree of water saturation of the rock. Water saturation strongly reduced the effectiveness of the method for the polymer systems tested. The more viscous monomers (for example, 60 percent polyester-40 percent styrene) were more effective in displacing the water from the rock, and compressive strengths of wet rock were doubled with these systems. Water saturations ranging from 25 to 100 percent of maximum saturation gave essentially identical results. Further tests on other types of mine rock; including shale and coal, are planned. Water-compatible polymer systems should be developed, or present systems should be suitably modified. For application to tunnel stabilization, design studies evaluating the improvement in rock strength and its influence on the support system are also recommended.

Jan 1, 1971

By D. R. Corson

The Bureau of Mines instrumented two similarly backfilled stopes--one filled in the normal manner and the other with the fill densified using vibratory compactors--to evaluate the effect of fill compaction on subsequent vein-wall closure proposed as a adjunct process for strengthening cemented fill. Hydraulic pressure cells to monitor pressures within the fill and mechanical closure devices to measure vein-wall movement and the procedure for their installation are described. The field compaction work was generally performed manually by utilizing small commercial concrete vibrators. A prototype immersible vibrator using slusher cables to propel the vibrator in the stope was used on several lifts of fill. Although compaction efforts were less effective than anticipated in increasing the final density of fill, analysis of the field data does indicate somewhat improved strain characteristics and an increased pressure buildup for the densified fill. The effects of a prolonged period of inactivity and of rock burst occurrences in the immediate area are also reflected in plots of strain and pressure within the two instrumented stopes.

Jan 1, 1971

By S. C. Schaefer

Thermodynamic properties of indium oxide (In203) have been studied with a high-temperature galvanic cell employing stabilized zirconia electrolytes. In the temperature range 790° to 1,230° K the free-energy change for the cell reaction 21n(1) + 3Cu20(c) = In203(c) + 6Cu(c) together with the standard free energy of formation of cuprous oxide gives the standard free energy of formation of indium oxide from the elements as ?Gf° = -218.78 + 75.34 X 10-3T ±0.7 kcal/mole. A third-law analysis yields the standard enthalpy of formation: ?Hf°298.15 = -221.5 kcal/mole.

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 L. B. Pankratz

Enthalpies above 298° K were investigated for four crystalline sodium borates by copper-block drop calorimetry. Determinations were made to 1,200° K for NaB02, 1,003° K for Na2B407, 1,005° K for NaB305, and 1,046° K for Na2Be013. No phase transitions or other thermal anomalies were found. The enthalpy determinations, when combined with known heats of formation at 298° K and other supplementary data, enabled the calculation of the heats and free energies of formation of the compounds to their melting points. Values of relative enthalpies, entropies, heat capacities, free energy functions, enthalpies of formation, free energies of formation, and equilibrium constants of formation were tabulated at even temperatures.

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

By V. E. Edlund

Laboratory batch flotation tests were conducted on copper converter slags to evaluate the relative merits of recovering copper from slow-cooled versus water-quenched slags. Three slags containing 1.6, 5.0, and 6.6 percent copper were used. More than 90 percent of the copper was recovered in a rougher concentrate leaving a 0.2- to 0.3-percent copper tailings when treating slow-cooled slag. Lower recoveries and higher copper tailings ranging from 0,5 to 0.6 percent copper were obtained from quenched slag. Grindability studies were made on the respective heat-treated slags. Quenched slags proved more difficult to grind than slow-cooled slags. Cost studies showed that (1) the cost of slow cooling and crushing off-sets any advantages of higher copper recoveries from slow-cooled slag, and (2) water-quenched slag, which requires no crushing preparatory to grinding, could be treated more economically. Costs based on processing 1,000 tons of slag per day would be $1.85 per ton for quenched slag versus $2.37 per ton for slow-cooled slag.

Jan 1, 1971

By V. E. Edlund

Laboratory batch flotation tests were conducted on copper converter slags to evaluate the relative merits of recovering copper from slow-cooled versus water-quenched slags. Three slags containing 1.6, 5.0, and 6.6 percent copper were used. More than 90 percent of the copper was recovered in a rougher concentrate leaving a 0.2- to 0.3-percent copper tailings when treating slow-cooled slag. Lower recoveries and higher copper tailings ranging from 0.5 to 0.6 percent copper were obtained from quenched slag. Grindability studies were made on the respective heat-treated slags. Quenched slags proved more difficult to grind than slow-cooled slags. Cost studies showed that quenched slags can be treated at slightly lower cost than slow-cooled slags. However, the cost advantage of processing quenched slags is more than offset by the higher copper recoveries obtained from slow-cooled slags.

Jan 1, 1971

By T. T. Campbell

Studies were conducted by the Bureau of Mines to develop a process for preparing thorium-magnesium master alloys or pure thorium metal by magnesium reduction of thorium tetrachloride in a semicontinuous reactor. Thorium tetrachloride was prepared in a fluidized-bed reactor by chlorination of thorium oxide or thorium oxalate. Conditions were established for producing a suitable thorium oxide feed for a fluidized-bed reactor. Thorium tetra-chloride was purified by vacuum sublimation and subsequently reduced by magnesium in a semicontinuous reactor to form thorium-magnesium alloys. Relatively pure thorium was produced by removing magnesium from the alloys by vacuum sublimation. Close to 100 percent of the thorium fed into the reactor was recovered either as metal (~93 percent) or as thorium oxide (~7 percent). The oxide can be recycled directly into the process.

Jan 1, 1971

By James J. Olson

The Bureau of Mines recorded and analyzed overpressure levels for three production blasts at the White Pine copper mine, Upper Michigan, to obtain representative data from single-heading blasts in a long, straight haulageway and to estimate the damage potential inherent in production blasts fired in close proximity to underground structures. Commercial pressure gages with a flat response to 1 kHz were used with an FM tape recorder to record the overpressures from one dynamite and two AN-FO (ammonium nitrate-fuel oil), 500-msec production blasts having zero-delay charge weights of about 75 lb (34 kg). The recorded waveforms from the underground blasts (1) were more complex than the typical free-air wave, (2) were of longer duration, and (3) had numerous secondary arrivals due to reflections from the ribs and roof. The waveforms showed that the zero-delay charges produced the only high overpressures. First pulse peak overpressures from the blasts ranged from 0.10 lb/in2 (6.9 X 102 N/m2) at a distance of 471.1 ft (144 m) to a maximum of 1.76 lb/in2 (121.3 X 102 N/m2) at 191,7 ft (58.4m) from the blasts. An analysis of variance of the first pulse overpressures from the three White Pine blasts showed that no statistically significant difference existed among the overpressure levels from the dynamite and AN-FO blasts and that a single equation P = 4.9 x 103 (D /W1 / 3) 2 .15, where P = overpressure in pounds/inch2, D = d-stance from the blast in feet, and W = zero-delay charge weight in pounds, could be used to describe the falloff of overpressure with distance.

Jan 1, 1971

By P. R. Tisot

Structural response and/or deformation was determined for each of four different grade Green River oil shales (27.0-, 34.5-, 45.5-, and 63.5-gal/ton) as they were heated in an inert atmosphere, under constant compressive stress, from ambient to subretorting temperatures; that is, below those required for rapid pyrolysis of the organic matter. Small cores and small columns of confined fragments comprised the test specimens, which were heated, in a specially designed microunit, at a uniform rate either to 725° or to 825° F under three different stress levels, 80, 200, and 325 psi. Structural response of some cores was observed as they were heated in a stress-free environment. The obtained stress-strain-time-temperature relationships provide information regarding the oil shale's yield temperature, yield stress, rate of compressive strain, loss of mechanical strength, and nature of structural deformation. Effects of structural deformation on induced permeability in small columns of fragments are presented. Results indicate that underground retorting of Green River oil shale may be seriously impaired through loss of induced permeability brought about by structural deformation of rich oil shale under the influence of heat and compressive stress.

Jan 1, 1971

By William G. Pariseau

A small displacement-small strain finite element technique utilizing the constant strain triangle and incremental constitutive equations for elastic-plastic media that are nonhardening and obey a Coulomb yield condition has been applied to the analysis of gravity flow initiation in a V-shaped hopper containing a powder under lunar environmental conditions. Three methods of loading were examined. Of the three, the method of computing the initial state of stress in a filled hopper prior to drawdown by adding material to the hopper layer-by-layer is superior (as expected). Results of the analysis of a typical hopper problem show that the initial state of stress, the elastic moduli, and the strength parameters have an important influence on material response subsequent to the opening of the hopper outlet.

Jan 1, 1971