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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 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 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 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

By H. R. Appell

The Bureau of Mines is experimentally converting cellulose, the chief constituent of organic solid waste, to a low-sulfur oil, All types of cellulosic wastes, including urban refuse, agricultural wastes, sewage sludge, wood, lignin, and bovine manure, have been converted to oil by reaction with carbon monoxide and water at temperatures of 350° to 400° C and pressures near 4,000 psig, and in the presence of various catalysts and solvents, Cellulose conversions of 90 percent and better (corresponding to oil yields of 40 to 50 percent) have been obtained. A continuous reactor for use at maximum conditions up to 500° C and 5,000 psig has been operated successfully, Using sucrose as a feedstock, operation in this system has permitted a simplified and preliminary chemical study of the conversion process. Oil yields of over 30 percent have been obtained with this unit.

Jan 1, 1971

By D. A. Wilson

A cyclic leaching process was developed for selectively leaching and recovering cadmium from nickel-cadmium scrap battery waste. The six major steps in the process are the following: (1) washing the plates to remove KOH electrolyte, (2) roasting at 550° to 600° C to oxidize metallic cadmium and decompose cadmium and nickel salts, (3) leaching with an ammonium nitrate solution, (4) precipitation of the leached cadmium from solution as cadmium carbonate using CO2 gas, (5) removal of CO2 from the lixiviator by adjusting to pH 4.5, heating, and evacuating the system, and (6) removal of small amounts of leached nickel from the lixiviator using a solvent extraction technique. The regenerated lixiviator is then recycled to leach additional plates. Cadmium extraction was 94 percent and the cadmium carbonate product contained 0.14 percent nickel and 0.12 percent cobalt impurity. The leached plates were smelted to a high nickel-low iron alloy with no detectable amounts of cadmium.

Jan 1, 1971

By R. A. Vik

The influence of thermal treatments on the grindability of low-grade hematitic iron ores from Michigan and Minnesota was examined in bench-scale tests. Treatment factors were roasting temperature, roasting atmosphere, and ore cooling conditions. Bond ball mill grindability and work indices were used as response indicators in evaluating the condition of the ore. Of the three treatment factors evaluated, roasting atmosphere, which brought about the con version of iron oxides to magnetite, had the most significant effect; roasting temperature had the next most important effect; and cooling condition had the least effect. Optimum grindability was obtained with reduced-quenched products of both ores at 650° C, near the alpha-beta phase transformation of quartz.

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 R. L. Rough

Photoelastic, wire resistance, and borehole-deformation gages were used to measure the in situ strains when an outcropping Black Hand Sandstone Formation in Hocking State Forest, Hocking County, Ohio, was overcored to stress-relieve the surrounding sandstone. Strains transmitted to the photo-elastic gage did not produce isochromatic patterns suitable for quantitative analysis. Strain readings from the wire resistance gage indicated tensile-strain loading during overcoring; readings from the strain-gage bridges in the borehole-deformation gage indicated compressive-strain relaxation during overcoring. The magnitude and orientation of the computed stress fields obtained from both gages were comparable when the corresponding tensile and compressive elastic moduli were applied. Stresses computed from deformation and resistance gages at depths to 5 feet showed the maximum stresses to range from 1.042 to 2.121 times greater than the minimum stresses. The bearings of principal stresses calculated from the deformation gage readings varied between N 61° E and N 83° E; the wire resistance strain gage bearing computations varied between N 68° E and N 82° E. Measurements of in situ strain in sandstone were shown to have promise but to require further development in field technique that could likely be achieved through experience.

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 Verne E. Hooker

Near-surface temperature measurements in two granite quarries show that diurnal temperature variations are significant to a depth of 1 or 2 feet, and annual temperature variations are significant to a depth of at least 25 feet. As a result, ground stress anomalies due to temperature exist near the surface, and their magnitude depends upon the time of day and the time of year. Rock stress and corresponding temperature measurements were made in one granite quarry over a rock temperature range of 33° to 81° F. Measured rock temperatures show good agreement with values predicted from one-dimensional heat flow theory. Calculated and measured stress-temperature coefficients for the two granites in this study are given. Thermally induced stress variations in near-surface rocks tested were as large as 1,690 psi from combined daily and seasonal temperature changes.

Jan 1, 1971

By J. M. Kuchta

Bench-scale test methods were developed by the Bureau of Mines for use by the Department of Transportation in the classification of solid and liquid oxidizers. A burning rate test is recommended for evaluating the fire hazard of solid inorganic oxidizers when mixed with a red oak sawdust as the reference combustible. A spontaneous ignition test is proposed for evaluating liquid and solid inorganic oxidizers which may decompose violently or ignite spontaneously when unmixed or mixed with the wood sawdust under unconfined conditions. Test results are compared for various representative oxidizers and a classification system is proposed for use in the government transportation regulations.

Jan 1, 1972

By H. E. Thomas

[The Bureau of Mines has conducted a field hydraulic fracturing experiment to determine the preferential orientation of induced fractures in oil shale at a depth of about 400 feet in the Green River Basin of Wyoming. The hydraulic fracturing treatment was performed by injecting extremely viscous water-base gel and 8- to 12-mesh sand into the oil shale through straddle packers set in an impermeable section of smooth-walled, 6-1/4-inch-diameter open hole. An impression packer proved that a horizontal fracture, which has an average width of about 1/2 inch at the borehole, was induced. A corehole drilled 100 feet from the fractured well intersected the fracture and confirmed its horizontal orientation. Because a horizontal fracture was successfully initi¬ated, it is inferred that the creation of multiple, closely spaced horizontal fractures may be feasible in Green River Basin oil shale.]

Jan 1, 1972

By Charles C. Boley

High-volatile A bituminous coal from the Allen mine, Las Animas County, Colo., blended with char produced from the same coal yielded accept-able metallurgical coke in a 500-lb movable-wall test oven. Nineteen experimental runs were carried out using several concentration levels of two different chars, 5.6 and 19.6 percent volatile matter, produced by entrainment carbonization of the base coal. With the higher-volatile char, an acceptable coke was produced at a 22.5-percent concentration; the lower-volatile char did not produce an acceptable coke at the concentrations investigated.

Jan 1, 1972

By E. L. Singleton

The Bureau of Mines investigated extraction of aluminum from aluminum-silicon alloys as a means of utilizing domestic aluminum silicate ores for aluminum production. Aluminum was extracted from aluminum-silicon alloys by electrolysis in molten electrolytes of NaCl-KCI-AIC13 and NaCl-KCI-AIF3 in a laboratory-scale cell. Six alloys with aluminum contents ranging from 20 to 87 percent aluminum were tested, and aluminum products of primary grade or better were obtained. More than 80 percent of the aluminum was recovered with current efficiencies as high as 91 percent. Recovery of a metallurgical-grade silicon product from the anode residue by an acid leaching procedure was possible with the 50-50 and 65-35 Al-Si alloys.

Jan 1, 1972

By G. L. Fitzpatrick

Preliminary results of an experiment in seismic holography indicate that the techniques of acoustical holography may be successfully used with seismic waves to determine the size and general shape of underground objects. This experiment was carried out under field conditions on a moderately large scale compared with the typical laboratory experiments in acoustical holography. The object to be mapped was a 100-foot-diameter, spherical, low-velocity zone of explosively fractured rock in oil shale at an average depth of 80 feet. The seismic wavelength of the Fourier component wave used in making the seismic holograms was 50 feet at a frequency of 140 cps. The hologram sampling aperture was 226 feet square and was sampled by 441 geophones in a 21 by 21 rectangular array. One novel aspect of the experiment was the use of a wide-band polychromatic explosive source of seismic waves rather than a narrow-band quasi-monochromatic vibrator source. A successful laser reconstruction of the object image from a lensless Fourier-transform hologram in the form of a 5/l6-inch-square photographic transparency is illustrated. The size of the underground object measured from the laser reconstruction of the object and the size inferred from a knowledge of the amount of explosives used to fracture the site and the tensile strength of the oil shale are found to agree.

Jan 1, 1972

By R. B. Schluter

Drying and preheating (partial induration) the green, unfired iron ore pellets is a means of reducing the energy required to produce metallized pellets. The Bureau of Mines processed three magnetite and two hematite concentrates through the unit operations of pelletizing, preheating in air, and reduction to metal to determine the effects of preheating upon the properties of the metallized pellets. The pellets were prepared in a 16-inch-diameter laboratory balling drum. Preheating and metallization were carried out in an externally heated 4-inch-ID by 4-inch-long stainless steel drum using air for the preheating atmosphere and lignite char as a reductant. The results 'varied considerably: two of the magnetites spalled when preheated in air at temperatures of 900° C and above, and the third magnetite and the hematite flotation concentrate required complete induration at 1,300° C to produce satisfactory pellets. The earthy hematite ore yielded excellent pellets at all preheat temperatures.

Jan 1, 1972

By T. A. Sullivan

The processing of sweated aluminum electronic scrap was investigated to develop methods for recovering the aluminum and concentrating the other metals, including copper, lead, gold, and silver, into a product that can be separated by known methods. Two molten-salt electrorefining processes were developed and tested. The first process utilized a three-layer refining cell with a BaCI2-NaF-AIF3 electrolyte, which operated at 750° to 850° C. The second process used an all-chloride electrolyte of NaCI-KCI-AICI3 at 750° to 800° C, with separate anode and cathode compartments. High-quality aluminum was recovered that averaged 99.8-percent pure in the three-layer cell and 99.6-percent pure in the compartment cell. Over 94 percent of the aluminum was recovered with cathode current efficiencies of approximately 90 percent in both methods. The copper, lead, tin, silver, gold, and other metals were concentrated threefold in an anode product. Separation of lead and part of the tin by liquation from this product seemed feasible. The anode product was smelted to prepare a 96-percent copper bullion that contained 690 ounces of silver and 65 ounces of gold per ton, with 98 percent recovery of these values.

Jan 1, 1972

By E. G. Davis

The Bureau of Mines investigated gaseous direct reduction of low-grade iron ore concentrates in a continuous fluid-bed reactor. These studies were made in a 4-inch diameter fluid-bed reactor using hydrogen alone, and oxygen-or air-reformed natural gas as the reductants. The percent reduction is directly dependent on the mole ratio of hydrogen in the reducing gas to the oxygen associated with the iron oxide in the ore. Two-and three-stage fluid bed tests were simulated by repeated continuous tests. The results showed that percent reduction of the final product was dependent on the mole ratio of the quantity of hydrogen in the gas of each stage to oxygen in the iron oxide of the initial ore feed. Reduction as high as 87 percent in the single stages and as high as 94 percent in the multistages was obtained when either hydrogen or reformed natural gas was used as the reducing gas. Magnetic separation and concentration of the highly reduced fluid-bed product yielded a high metallic iron concentrate analyzing 85 percent total iron and 80 percent metallic iron with total iron recovery as great as 90 percent. Agglomeration of the high-grade metallized concentrate produced hard pellets analyzing 85 percent total iron and 78 percent metallic iron. Green pellets, with good strength, were made without any binder in a drum pelletizer. Direct melting of the high-metallic fluid-bed product in a basic lined arc furnace produced a nearly pure iron which contained 0.09 C and 0.01 P with 95 percent recovery of the metallic iron in the metal.

Jan 1, 1972