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By Rex D. Thomas

Concentration of the kerogen (organic material) in oil shale was accomplished by centrifuging after pretreating the oil shale with carbonic acid to remove the carbonates and pretreatment with sodium hydroxide (pH 11.5) to remove the claylike minerals. Analysis of the materials obtained showed that the concentrations of organic sulfur and organic nitrogen compounds were not affected by centrifuging. These compounds are evenly distributed in the kerogen and are not strongly bound to the mineral constituents. Organic oxygen compounds, however, were concentrated in the light fraction. These compounds are more closely associated with the kerogen and are not bound to the mineral constituents. Iron compounds other than pyrite apparently are closely associated with the organic material.

Jan 1, 1970

By R. B. Tippin

To study continuous operation of the heavy liquid separation (HLS) of minerals, the Bureau of Mines concentrated spodumene from a typical ore. The studies included heavy liquid concentration, removal of the heavy liquid from the mineral products, and recovery of the heavy liquid for reuse. The research program examined the influence of feed moisture, steam consumption, stripping time, and condition of steam. Operation of multiple cyclones in series resulted in spodumene concentrates assaying 92 to 95 percent spodumene and indicated mineral recoveries of 86 to 89 percent. Continuous filtration and steam stripping produced mineral products containing less than I pound of heavy liquid tetrabromoethane (TBE) per ton of material. Problems unique to this process are discussed, including heavy liquid properties and viscosity, toxicity, material handling hazards, and safety precautions.

Jan 1, 1970

By C. F. Swab

A relatively innocuous halocarbon was investigated as a substitute for the highly toxic carbon tetrachloride in the approval testing of chemical cartridges. The vapor effluent of 1,1,2-trichloro-1,2,2-trifluoroethane from chemical cartridges is continuously monitored by a nondispersive infrared analyzer. Breakthrough times for the cartridges, using the halocarbon, can be equated to those of carbon tetrachloride, if multiplied by the factor, 1.49.

Jan 1, 1970

By James C. Patterson

Sintered fly ash was shown to have promise as a modifier for poorly drained soils. Turf grown in mixtures of sintered fly ash and soil benefited from increased water-infiltration rates, greater total pore space, and higher moisture availability, The result was an improved turf stand with increased grass yield and root density.

Jan 1, 1970

By Larman J. Heath

Wellbore enlargement was tested using hydrazine hydrate in a gas-storage well in Ohio to increase the well productivity. The wellbore was to be enlarged by chemical disaggregation of the sandstone adjacent to the wellbore. Productivity immediately declined 49.1 percent and gradually declined to zero in 7 months. A down-hole camera survey showed a white-to-gray precipitate covering the entire wellbore surface. The precipitate was chemically analyzed and identified as mostly carbazic acid, a hydrazine derivative of carbonic acid. Formation of this precipitate was not anticipated; this viscous sub-stance caused the gradual loss in productivity of the well. The wellbore was not enlarged. Laboratory tests were run to determine what clay stabilization measures could be taken in sandstone cores to prevent clay swelling and particle migration caused by hydrazine hydrate. Normal clay stabilization methods did not prevent the virtually complete loss in permeability to hydrazine hydrate. Other laboratory tests using natural gas diluted with small amounts of carbon dioxide confirmed the ease with which carbazic acid could be formed in a hydrazine hydrate-saturated environment within and adjacent to the wellbore.

Jan 1, 1970

By George S. Koch

The distribution of gold in part of the Getchell mine, Humboldt County, Nev., is presented through the statistical analysis of 956 assays of rock cuttings from wagon-drill holes. Two methods to predict grade in undeveloped parts of the ore body are evaluated, and the possibility of sampling bias is tested. The distribution of gold is compared with that in three other Nevada gold deposits of the same type characterized by gold particles mostly of submicron size associated with carbonaceous rocks, and also with that in deposits with coarse-grained gold. Usually, fewer samples of a given type are required to make a satisfactory grade estimate for submicron deposits than for coarse-grained deposits. The economic consequence is that submicron gold deposits are likely to be less expensive to sample and evaluate than coarse-grained deposits.

Jan 1, 1970

By R. L. Blake

The crystal structure of hematite, a-Fe203, has been refined as part of a continuing study of the behavior of phases in the Fe-O system during reduction and oxidation. Three-dimensional diffraction intensities were collected on two spherical single crystals of hematite with a semiautomated Buerger single-crystal diffractometer. The first crystal refined was a natural Elba hematite with minor impurities. The other, a synthetic crystal, was refined at the request of Mossbauer spectroscopy investigators concerned with impurities in the natural crystal. The structure has been refined with a least-squares program and the final structure for the natural crystal irradiated with CuKa-radiation gave a discrepancy factor (R) of 3.65 percent using 49 unrejected reflections of the 51 measured. For the synthetic crystal, using MoKa-radiation, the discrepancy factor converged to 2.8 percent using 95 unrejected reflections and was 3.3 percent for all 109 reflections. The structure model of Pauling and Hendricks has been confirmed with essentially no change in the iron coordinates and approximately a 5-percent change in the oxygen coordinates. Selected interatomic distances and angles were calculated as were anisotropic temperature factors.

Jan 1, 1970

By G. H. Keith

Electrowon tungsten powders were investigated with respect to consolidation, fabrication, and mechanical properties. Sheet, 0.03 inch thick, was produced and its tensile strength measured between 250° and 1,935° C. The large particle size of electrowon tungsten effectively precluded sintering to a density sufficient to allow hot working to sheet or bar. The powders were consolidated by die pressing to 70-percent density, sheathing in molybdenum, and high-energy-rate extruding to either round or sheet bar of 100-percent density. The material was then rolled conventionally to sheet. The mechanical properties of the sheet prepared from the electrowon powders compared favorably with those reported in the literature for sheet prepared from commercially produced hydrogen-reduced powder.

Jan 1, 1970

By Daniel C. Boteler

Five lignites from the northern Great Plains province were carbonized at temperatures from 500° to 1,000° C in a bench-scale unit. A replicated Greco-Latin square experimental design was employed to allow testing of four independent variables at five levels. Independent variables investigated were temperature, source of lignite (mine), weight of charge, and moisture content of charge. Dependent variables were char yield, tar yield, light-oil yield, tar plus light-oil yield, carbonization gas yield, and carbonization gas heat yield. An analysis of variance indicated that, at the 99-percent confidence level, the independent variables of carbonization temperature, source of lignite, and weight of charge were significant for yields of char, tar plus light oil, and carbonization gas, whereas moisture content was only significant for carbonization gas yields. At the 95-percent confidence level, moisture content significantly influenced the carbonization gas heat yield per pound of lignite charge and the yields of dry tar plus light oil. All dependent variables were determined on a moisture- and ash-free basis. Multiple regression equations for predicting seven different factors of carbonization yields as functions of carbonization temperature and initial composition were developed using computer techniques. Equations for yields of char, tar plus light oil, and carbonization gas were compared with equations previously developed by others at the 500° C level.

Jan 1, 1970

By Joseph L. Condon

Fifteen shots of three explosives with charge weights of 0.52, 1.1, 3.1, and 5.1 kilograms were fired in a pond to study the seismic effects of detonating explosives in water. Shock pressures and bubble periods were measured with pressure transducers in the water. Vibrations were measured on land in three orthogonal directions with particle velocity gages. Statistical tests indicated that a charge weight exponent of 0.43 best scaled the data. While shock pressures and bubble periods showed considerable differences in explosive performances, the amplitudes of ground vibrations showed less difference, and one prediction equation was therefore derived to estimate vibration amplitudes from all the explosives.

Jan 1, 1970

By H. R. Babitzke

As part of a continuing project to develop refractory metal alloys for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation strengthening techniques to improve the properties of columbium alloys. The purpose was to investigate the effects of hafnium, tungsten, and boron on the formability, strength, and oxidation resistance of columbium. The experiment was of factorial design with two replications which called for 72 ingots of 36 basic compositions, weighing 150 grams each. Hafnium, tungsten, and boron were evaluated at 3, 3, and 4 levels, respectively. Values of alloy content are all in atomic percent. The highest strength observed was 29,000 psi at 1,200° C for alloys Cb-15Hf (No. 3), Cb-7.5Hf-5W-2B (No. 14), and Cb-15Hf-5W-2B (No. 15). At 1,200° C, the ternary alloy Cb-15Hf-5W (No. 6) which has shown good properties in previous Bureau of Mines investigations was the most resistant to oxidation For boron additions, the alloys oxidized more readily with increasing amounts of this element. The fabricability of the alloys high in boron became increasingly difficult, resulting in an inadequate number of alloys required for a complete statistical analysis for all the tests. As a result of the decrease in ductility, an insufficient quantity of tensile samples were available for a proper analysis for the high-temperature strength data.

Jan 1, 1970

By Charles Prasky

This report describes bench-scale studies and pilot-plant development of the Bureau of Mines process for roasting iron ores with a ferrous scrap reductant, such as discarded automobile hulks, to yield artificial magnetite. Quality magnetic concentrates containing about 66 percent iron and 6 percent silica with iron recoveries of over 90 percent were obtained after roasting fine-grained oxidized or nonmagnetic taconite with unburned, sheared automobile hulks in a rotary kiln. The relatively complete oxidation of the lighter gage metal in the automobile during roasting resulted in a metallic byproduct consisting of the unconsumed heavier gage metal scrap. This residual or tailored scrap is potentially useful as heavy melting stock and has more value than the original automobile hulk.

Jan 1, 1970

By B. H. Eccleston

The effect upon automobile emissions in changing from leaded to lead-free gasolines was studied in experiments by the Bureau of Mines in cooperation with the American Petroleum Institute. Typical U.S. leaded gasolines and prototype lead-free gasolines of comparable octane quality were used in eight vehicles operated to simulate city driving. The experiments were run at 70° and 95° F. Exhaust and evaporative emissions were measured and the photochemical effect of the emissions was experimentally observed in an artificial smog chamber. Results of the study reveal the manner and degree in which the changes in fuel composition alter the amount and characteristics of both exhaust and evaporative emissions. Briefly, it is shown that the compositional differences between leaded and prototype lead-free fuels resulted in higher photo-chemical pollution potential of the emissions from the lead-free fuels. The effect is attributed to the photochemical characteristics of high-octane fuel components that are used in greater quantity in the lead-free fuels.

Jan 1, 1970

By W. R. Hardwick

Nuclear explosive fracturing has been suggested as a method to make hard rock amenable to extraction by a modified block-caving method. To evaluate this possibility, conventional and nuclear blasting practices are discussed, underground mining methods for large deposits and their costs are described, and the cost of fracturing ore with a nuclear explosive and subsequent mining by a modified caving system is estimated and compared with both open-stope and block-caving mining costs. While the direct cost of fracturing the ore in hard rock with a nuclear explosive is less than with conventional explosives, additional costs imposed by the use of nuclear explosives may make their use unattractive for deep mining.

Jan 1, 1970

By K. Robert Dorman

Spray-applied polyurethane foam was used to insulate the walls of heated rooms excavated in permafrost. The experiment was designed to determine whether polyurethane foam can be sprayed successfully on frozen ground under freezing conditions and to measure the effectiveness of the insulation in maintaining--at elevated temperatures for an extended period--a room excavated in frozen ground. Two manufacturers' foams were investigated in the laboratory. Subsequently, one of the foams was employed to insulate two small rooms, one in frozen gravel and one in frozen silt, in an experimental tunnel belonging to the U.S. Army Cold Regions Research and Engineering Laboratory (USACRREL) near Fairbanks, Alaska. Following insulation, heat was introduced into the two rooms. Heat migration across the insulating barrier into the walls, in addition to wall closures, was monitored over an 8-month period. The results show that polyurethane foam can be successfully sprayed on frozen ground in below-freezing temperatures. Given this type of insulation, together with winter cold to supercool the surrounding ground, it should be possible to maintain a shaft or heated room in permafrost for several years.

Jan 1, 1970

By G. H. Keith

A vanadium-base alloy consisting of the following elements in weight-percent--molybdenum, 20; titanium, 10; carbon, 0.1; silicon, 0.5; and yttrium, 0.5--had exceptionally high strength at temperatures up to 1,200° C. This alloy was capable of fabrication to sheet of ~ 1 mm thickness by a combination of hot swaging and hot and warm rolling. In the warm-rolled condition at ambient temperature, its ultimate tensile strength was 1,205 MN/m2. The strength at 1,200° C was 150 MN/m2. Within the temperature range of 25° to 1,200° C, the ductility of the alloy as measured by elongation increased from 4 to >90 percent. Strengthening was achieved by both solid-solution and dispersed-phase mechanisms. Alloys of 20 percent molybdenum and 10 percent titanium were stronger than the other molybdenum-titanium alloy compositions tested. Strength was increased 15 percent in the temperature range of 25° to 800° C, with no accompanying loss in ductility, by the addition of 0.5 percent silicon. Workability was improved by additions of 0.25 and 0.5 percent yttrium.

Jan 1, 1970

By W. R. K. Wu

This Bureau of Mines report presents a statistical study of the repeat abilities of coal-plasticity parameters obtained in the tests with the Gieseler plastometer and the Audibert-Arnu and Hoffmann dilatometers. Repeatability is expressed in terms of one or two standard deviations for the differences between duplicates. The statistical method employed here is summarized. Results are tabulated for the temperature and nontemperature parameters of the three tests.

Jan 1, 1970

By Ivan L. Nichols

Tailings dumps at Mercur, Utah, contain about $7 million worth of gold in 3.5 million tons of mill tailings assaying about 0.07 ounce of gold per ton. Commercial mining and milling at Mercur ceased in 1942. To determine whether improved technology was now available that might permit economic reprocessing of the Mercur dumps, the Bureau of Mines probed for a low-cost method that would be applicable to these tailings. A composite sample prepared for laboratory studies assayed 0.062 ounce gold per ton. About 10 percent of the gold occurred as a water-soluble cyanide. Conventional cyanide leaching dissolved 32 percent of the gold, and hot, strong cyanide solution dissolved 42 percent. Results were not improved by pretreatment with acids, bases, or oxidants. After expensive preroasting, gold recovery by cyanidation was increased to 65 percent. The simple procedures were ineffective, and more effective procedures were too costly for economical processing of Mercur tailings.

Jan 1, 1970

By A. Aly Selim

This report describes the feasibility of predicting percussive drilling rates by equations derived from statistical regression analysis. The least squares statistical method was used and the analysis was performed both by direct and by stepwise linear regression analysis. The predicted penetration rate is a function of the drill power and the physical properties of the rocks penetrated. The results show promise that the technique may be of value in providing a mathematical model by which percussive drill manufacturers and users can predict the performance of a given drill. Experimental work involved two mining type percussive drills. Penetration data for these drills were determined from nine rocks drilled in the laboratory. Drill work rates (power) were determined in a separate series of experiments. Rock physical properties were measured from diamond-drill core samples taken from the same blocks used for percussive drilling.

Jan 1, 1970

By G. G. Campbell

Bureau of Mines research to develop an in situ retorting recovery method for oil shale has involved field testing of fracturing techniques for creating fluid-flow paths in impermeable oil shale. Electrolinking, hydraulic fracturing without and with sand propping, and explosive fracturing with a liquid explosive were tested in a 25-ft-square, five-spot pattern. These wells were drilled into oil shale at 50-to 88-ft depths near Rock Springs, Wyo. Results of the fracturing tests were evaluated by injecting air into a test well and measuring flow rates and flow profiles in adjacent test wells before and after each test. To identify points of air entry (location of fractures) in wells, flow profiles were determined by use of inflatable packers and by continuous logging with an airflow probe developed during the fracturing program. Electrolinking and hydraulic fracturing without sand propping were relatively ineffective; hydraulic fracturing with sand propping created horizontal fractures with desirable flow capacity; and fracture flow capacity was significantly increased by detonation of nitro-glycerin displaced in the natural and hydraulically induced fracture systems.

Jan 1, 1970