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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

By R. A. Welsh

The Bureau of Mines has developed a photoelectric concentrator apparatus which is capable of collecting incremental products from the discharge of wet concentrating tables. The instrument uses photoelectric cells as sensors to differentiate between two products which have differences in color or reflectivity. The photocells provide a signal that controls a mobile splitting device that separates the products. Tests conducted on a wet table demonstrated the ability of the apparatus to separate a product containing 81.5 percent pyrite from a lower-grade product containing only 68.8 percent pyrite. The photoelectric concentrator should have a broad application for collecting concentrates with visible color or reflectivity differences from wet concentrating tables.

Jan 1, 1972

By F. G. Horino

This report presents the theory and design of a stiff loading machine used by the Bureau of Mines. The machine incorporates three high-strength steel columns as the restraining member in parallel with the specimen. The theory presented gives the basis of design and the dimensions of component parts of the machine. Laboratory verification of the theoretical stiffness is described using three different setups involving a hydraulic jack and spacers and confirms the stiffness calculations to within 1 percent. Experimental techniques, testing procedures, and special equipment designed for determining the complete stress-strain behavior of NX cores of both hard and soft rock are described. Typical test data are presented as force-displacement curves for two rock types, a marble and a granite.

Jan 1, 1972

By E. M. Murphy

Comparative data from ASTM method of test E-162 and large-scale trials in the Experimental Mine show that the flame-spread quality of brattice cloth and other ventilation control materials can effectively be evaluated by either method. Materials having a flame spread index of 25 or less, as determined by the simpler and more economical laboratory test ASTM E-162, do not present a serious fire hazard when used in coal mines.

Jan 1, 1972

By William J. Campbell

Three types of X-ray analytical instrumentation were compared for applications in the secondary brass and bronze industry. The instruments were a conventional X-ray spectrograph, a portable X-ray spectrograph, and a radioiso-topic X-ray analyzer using balanced filters. The following two general applications were considered: Rapid identification for sorting scrap metals and quantitative analyses to provide guidance in the melting and casting of alloys. Twenty-three analyzed copper-base alloys were used as standards. Although the alloys varied widely in composition, matrix correction procedures were not necessary except for copper. The conventional X-ray spectrograph provides positive identification of the alloys and quantitative values for the six elements investigated--aluminum, copper, iron, lead, tin, and zinc. Equivalent results were obtained with the portable X-ray spectrograph for those elements whose characteristic X-rays are in the wavelength range of the instrument. The radioisotopic X-ray analyzer distinguishes certain groups of alloys and provides quantitative determinations for copper, lead, tin, and zinc. The sensitivity of the analyzer was marginal for the determination of small concentrations of elements of atomic number 26 or lower.

Jan 1, 1972

By Abdurrahman Cetinbas

The effect of water infusion on the flow of methane and on the production of dust was investigated at an active face in the Pittsburgh coalbed. The average total flow of methane at the face decreased by approximately 79 percent, whereas the flow from the ribs increased about 24 percent after infusion. On the day after infusion, dust concentrations appear to have been reduced; however, the presence of large quantities of rock dust obscured the results on the following days.

Jan 1, 1972