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By G. L. Gates

The waters used to waterflood the Wilmington oilfield were studied by the Bureau of Mines, in cooperation with the city of Long Beach, Calif. Increases in the pressure of the injection wells indicated that they were being plugged by materials suspended in the waters. This study was made to identify the suspended materials, determine their origin, and find methods of preventing their formation. The suspended oil-coated materials were iron sulfide, barium sulfate, calcium carbonate, clay, and sand (or silica). Results indicated that the sulfide, which was as high as 90 milligrams per liter, was the product of sulfate-reducing bacteria. The injection of ocean water increased the sulfate content of the waters in the petroleum reservoirs from 3 to 250 milligrams per liter, thereby furnishing sulfate for growth of the bacteria. The waters were supersaturated with barium sulfate. Laboratory tests showed that sulfide could be removed from the waters by adding iron at a cost of 1 to 2 mills per barrel. The solubility of iron sulfide and calcium orthophosphate in the injection waters was also determined.

Jan 1, 1975

By C. M. McCulloch

The methane content of virgin bituminous coalbed can now be measured accurately in the field with exploration core samples from vertical boreholes. The gas content of the coal per unit weight can be used either to design a mine ventilation system or to determine if degasification of the coalbed will be necessary before mining, and to determine the gas resources in the coalbed. The equipment necessary to conduct the test costs less than $50. The gas con-tent of the coal in place in the ground is determined by summing the gas lost from coring, gas measured during desorption, and the residual gas in the coal. Upon removal from the borehole, the core sample is placed in an airtight container and des orbed for several weeks until the desorption rate is below 0.05 cm3/g for 5 consecutive days. The gas lost from the core while it was being cored and the residual gas are estimated by a new graphical method. The amount of gas remaining depends upon whether the coal is friable or blocky. Friability appears to relate to the depth of the sample below the surface, fixed carbon percentage, Hardgrove grindability index, and proximity to tectonic disturbance. Friable coals emit nearly 96 pct of the total gas during desorption whereas a blocky coal emits only 60 pct of its total gas. Coalbeds that are ill defined as to their blocky or friable nature must be tested in the laboratory for unambiguous analysis.

Jan 1, 1975

By D. G. Kuehn

Studies were conducted by the Bureau of Mines to determine the positive ions and neutral species produced in glow discharges of gas streams containing 1.0 percent NO in helium, 29 percent dry air in helium, and 1.06 percent NO in N2, Mass spectrographic measurements were conducted for gas pressures from 2.3 to 10.0 torr and dc currents from 10 to 20 mAo Ion species observed included NO+, N2 +, O2 +, N+, and 0+ with lesser amounts of He+, He2+, and N02+. Variations in various ionic and neutral species with discharge duration were interpreted to be consistent with an electrically induced dissociation of NO to produce N2 and O2. No nitrogen oxides were observed to form in glow discharges of the helium-air mixture.

Jan 1, 1975

By Donald I. Kurth

The Bureau of Mines conducted experimental work on comminuting coal. The size distributions of coarse fragments and fine particles were obtained under different modes of energy application--drop, impact crushing, wedge impact, compression, and shear tests. Four levels of energy application were used in the impact crushing and wedge impact tests. Airborne dust and respirable air-borne dust distributions were obtained for the impact crushing and wedge impact tests. Analyses of nonairborne dust and coarse fragment-fine particle distributions were carried out on impact, wedge, compression, and shear tests. The experimental size data on nonairborne dust were fitted to normal, log-normal, power law, Weibull, log-Weibull, and exponential distribution functions. Both the nonairborne dust and the coarse fragment-fine particle size distributions are best described by Weibull distributions. For the impact crushing tests, mean product size was found to be inversely related to specific crushing energy. The particle counts in a given size range of airborne and nonairborne dust were found to increase with increased input energy and specific crushing energy. However, in another sense the particle distributions were independent of energy level; that is, the percent-ages in a given size range were approximately constant regardless of energy level. Respirable airborne dust was related to respirable-size nonairborne dust by a power law.

Jan 1, 1975

By Robert Lee Stahl

Comprehensive field tests were made by the Federal Bureau of Hines at the Conda open pit mine near Soda Springs, Idaho, to determine whether surface geophysical techniques could be used to detect and delineate faults in phosphate deposits. The tests included seismic refraction, magnetometry, electrical resistivity, and airborne photography. Of the several geophysical techniques tested in the field, horizontal resistivity profiling was the most effective method for diagnosing faults. The method is quick, inexpensive, accurate, and can be easily used by mining company personnel to detect and delineate faults.

Jan 1, 1975

By Sathit Tandanand

This Bureau of Mines report describes the method of obtaining a strength index for rock drillability, particularly for percussion drills. The original Protodyakonov method has been slightly modified, essentially to eliminate uncertainties in the measurement of the volume of fines, and to avoid conjecture in selecting the representative value as the strength coefficient. A theoretical consideration of the relevant parameters in the method was extended from a comminution theory, and hence the meaningful value was obtained experimentally by plotting the ratio of the number of drops and the volume of fines against the number of drops. The minimum ratio of the number of drops to the volume of fines in the plot was selected as the coefficient of rock strength. The modified method of obtaining the strength coefficient preserves the original Protodyakonov test apparatus and the merit of simplicity of the test procedure. The modified coefficient of rock strength shows its usefulness in predicting penetration rates with greater reliability than other mechanical properties. Consequently, the drillability curves were drawn using the modified coefficient of rock strength as the parameter for penetration rate prediction in the field.

Jan 1, 1975

By W. E. Lamont

The Federal Bureau of Mines, in cooperation with phosphate companies in the Florida land-pebble area, made a comprehensive study of the waste clays, or "phosphate slimes," produced in the mining of phosphate rock in Florida. These slimes represent a significant ecological problem and a major deterrent to effective land recovery in the phosphate-mining areas. Physical, chemical, and mineralogical studies were made of slime samples submitted by 15 of the 16 plants in Florida in an effort to identify factors that prevent successful consolidation of the slimes and subsequent recovery of the mined lands. Results of these studies indicated that the clay mineral attapulgite, a hydrated magnesium silicate, was primarily responsible for the very poor settling characteristics of the slimes, and that the quantity of attapulgite in the slimes effectively controlled the settling rate, pulp density of terminal solids, viscosity, percent solids of filter cake, and flocculant requirements.

Jan 1, 1975

By R. L. Stein

For the past several years, the Bureau of Mines has been actively engaged in developing two new oxygen self-rescuers through research contracts with private industry. These new oxygen self-rescuers are designed to be carried by a miner while he is at work and are used during emergency escape, supplying high-purity oxygen to the user and, at the same time, absorbing carbon dioxide (C02), The first of the two new self-rescue breathing devices is a 10-minute, self-contained apparatus developed by the Mine Safety Appliance Co, Size and weight of the unit are comparable to the currently used self-rescue devices. The second device, designed and developed by Lockheed Missiles and Space Corp., is 8. 4.5-lb package which supplies 1 hour of oxygen to the miner. Both devices have a canister which contains the oxygen-producing and CO2-absorbing potassium superoxide chemical, a breathing bag, a bite-type mouthpiece, noseclip, goggles, and hoses connecting the canister and mouthpiece. When needed in an emergency, the miner removes the outer protective cover and dons the unit. For both devices oxygen is immediately available once the mouthpiece is placed in the mouth. These two new units have received prototype approval from the National Institute for Occupation and Safety Health (NIOSH) and the Mining Enforcement and Safety Administration (MESA).

Jan 1, 1976

By Carl F. Wingquist

Electrical resistance heating to effect thermal fragmentation of semiconductive rock was examined by the Bureau of Mines. Tests were carried out on copper-bearing ores of the Nonesuch Shale Formation in the laboratory and in the the field at White Pine, Mich. Fieldwork included primary and secondary breakage tests. Heating tests on in situ rock failed to produce thermal dam-age to an extent considered useful; however, boulders up to 30 ft3 were effectively broken by the method. Power input to the test rock was taken from a 50-kV, 5-amp dc power supply.

Jan 1, 1976

By E. E. Maust

The literature on the activation of sphalerite for flotation by short¬chain xanthates leaves unanswered the question of whether a compact surface film of activator sulfide is necessary or merely sufficient for high flotation recoveries. Studies by Guarnaschelli and Plaksin indicate that xanthate adsorption and flotation of sphalerite are increased with increasing hole/ electron ratio. These results, and the known acceptorlike behavior of many heavy-metal impurities in zinc sulfide, suggest that activation may result from a traditional semiconductor doping effect at the surface. Using the theory of chemisorption states on ionic crystals as developed by Levine and Mark, the Bureau of Mines has carried out A calculation to estimate the surface-state energies of various metals when they are substituted at zinc sites on (110) sphalerite surfaces. Based on a simple Madelung-Born treatment of ionic solids, the calculation indicates that many of the metals known to activate sphalerite for subsequent flotation have lower surface-state energies than nonactivators. The results of these calculations are discussed from the standpoint of consistency with the proposed activation mechanism and observed flotation results. The satisfactory agreement obtained is taken to be support for the proposed mechanism, and further elaboration of a surface-doping model is attempted.

Jan 1, 1976

By J. R. White, S. W. Lambert, C. M. McCulloch

Examination of several coalbeds in Walker County, Ala., Cambria, Greene, and Fayette Counties, Pa., and Raleigh and Wyoming Counties, W. Va., indicates that cleat orientations are similar throughout a vertical sequence of strata. Studies of cleat orientation were carried out in underground mines that are operating in separate coalbeds vertically above one another. The data show that over a vertical separation of 100 to 400 feet, the average difference in coal cleat orientation between mines is 04° for the face and 08" for the butt cleat. Variations of coal cleat direction between coalbeds examined in strip-mined areas show similar values. Cleat orientations measured at outcrops agree well with the directions measured underground, suggesting that the amount of vertical separation between coalbeds has little effect on the resulting differences in cleat directions. The largest variation of cleat directions between adjacent coalbeds occurs where a large horizontal distance separates two sample locations. Cleat orientations for deeper coalbeds are most reliable where the data are taken from directly above.

Jan 1, 1976

By D. A. Wilson

A laboratory method for processing lead battery scrap has been developed that eliminates virtually all of the S02 emission that normally is produced when a reverberatory or blast furnace is used. The method employs a hydrometallurgical step to convert the PbS04 to PbO and CaS04 by mixing the battery scrap with a slurry of Ca(OH)2. The reaction is exothermic and goes to completion in 2 to 5 minutes at room temperature. The dried product is mixed with a KC1-NaC1 flux and carbon and reduced at 6500 C. A minimum charge ratio of 3 parts of carbon to 100 parts of battery scrap is required for reduction. The process produces lead reductions and recoveries as high as 97.0 and 94.9 percent, respectively. The KCI-NaCl flux is recovered using a standard counter-current water leach followed by evaporation.

Jan 1, 1976

By Martin Hertzberg

The concept of limit burning velocities is used to formulate a quantitative theory of flammability limits. Competing processes dissipate power from a combustion wave and quench propagation at some characteristically low limit velocity. There are four competing processes and one complication: (a) Free, buoyant convection, (b) conductive-convective wall losses, (c) radiation, (d) selective, diffusional demixing (the complication), and (e) flow gradient effects (flame stretch). These complexities are unraveled by creating an idealization that is initially freed from these competing processes. The ideal serves as a standard, and its burning velocity (Su), ideal is a unique function of the initial thermodynamic variables of state. By adding each process individually, it is possible to evaluate their significance, quantitatively, in terms of a limit velocity (Su)a , b , c , or e , and to explore the nature of their cooperative interactions. The larger the limit velocity, the more significant the process. The apparently diverse observations of flammability behavior are readily unified within this simple, conceptual framework.

Jan 1, 1976

By Daryl R. Tweeton

The Bureau of Mines conducted experiments to measure the influence of environment on the friction and wear of a steel-quartz system at several speeds and loads. In each test a quartz block was pressed against a rotating ring of low-carbon steel. Environments used were moist air, dry air, dry nitrogen, water, aqueous oleylarnmonium acetate (ClsH35NH3+-OCOCH3), and aqueous aluminum chloride (A1C13). The sliding speeds were 2.2, 13, and 33, cm/sec, and the loads were 6.8 and 13.6 kg. The coefficient of friction, the wear, and the roughness of the surfaces were measured, and the wear debris was examined. The coefficient of friction was significantly lower in moist air at 2.2 cm/sec than for any other combination of environment and speed employed, and was generally an inverse function of the oxidizing ability of the environment. The coefficient of friction increased somewhat with increasing load. The wear of the steel rings was greatest in dry air at all speeds and loads. The wear of the quartz blocks at 180 rpm was greatest in dry air, but at 12 rpm it was greatest in nitrogen. Friction and wear in aqueous oleylarnmonium acetate and in aqueous aluminum chloride were similar to effect in water alone.

Jan 1, 1976

By F. P. Haver

The Bureau of Mines is developing a leach-electrolysis procedure to produce Special High Grade (SHG) zinc from sulfide concentrate without the generation of sulfur oxide gases. Chlorine-oxygen leaching of the concentrate yields zinc chloride (ZnCI2) which, after purification, is electrolyzed in a fused-salt cell to obtain molten zinc metal and chlorine gas for recycle. This paper describes a laboratory-scale investigation made to develop a procedure for electrowinning zinc metal from ZnC12. Zinc chloride by itself is not a suitable electrolyte because it fumes badly above its melting point and is a poor conductor of electricity. Other salts therefore must be added to prevent fuming and improve the conductivity. Optimum results were obtained with a KC1-LiCl-ZnCl2 bath at 500° C, using a current density of 5 amp/in2 and an electrode spacing of 0.5 inch. Under these conditions, SHG zinc was produced at a current efficiency of 94.3 pct and an energy requirement of 1.16 kwhr/lb. Fused-salt electrowinning eliminates the need to handle and melt cathodes and increases the production of metal per unit cell volume through the use of higher current densities than are possible with aqueous electrolysis.

Jan 1, 1976

By William C. McLaughlin

In the deep vein mines of the Coeur d'Alene mining district, rock bursts are a potential hazard to the mine structure and underground personnel. Damage repair costs are estimated by one company to exceed $1 per ton of ore mined. The Bureau of Mines, in cooperation with the mining companies, has conducted research intermittently over the past 10 years to help reduce bursts. Onsite inspections of major rock bursts were conducted, and reports were submitted to mine management; these included the geology and geometry of the affected area. The paper discusses the development and improvement of microseismic and surface monitoring equipment. The underground microseismic network, when operated on a regular basis and the results plotted daily, is capable of detecting stress concentration in certain areas. The surface seismographs record rock bursts, blasts, earthquakes, etc., throughout the district and show approximate location, time, and relative intensity of the event.

Jan 1, 1976

By G. W. Elger

This report describes pilot-plant studies and an economic evaluation of a process developed by the Federal Bureau of Mines, Albany Metallurgy Research Center, to produce synthetic rutile from a rock-type ilmenite concentrate. In this process, ilmenite blended with coke and lime is smelted in an electric arc furnace to separate most of the iron as salable pig iron and to form a titania-enriched slag of low iron content, which is treated with oxygen and titanium pyrophosphate. The titanium oxides are converted to crystalline rutile; the phosphate glass contains most of the associated impurities. The treated slag is ground and leached with sulfuric acid to liberate rutile crystals, which are concentrated by physical methods. In pilot testing conducted to obtain data for a cost estimation, a synthesized product containing about 88 wt-pct TiO2 and less than 2 pct FeO was extracted from a rock-type ilmenite concentrate containing about 45 wt-pct TiO2. The estimated fixed capital cost (on a mid-1975 basis) of a plant producing 500 tpd of synthetic rutile is $28,290,100. Based on 330 operating days per year, the estimated operating cost for this process is $351 per ton of synthetic rutile. The estimated selling price of synthetic rutile made from rock-type ilmenite is $344 per ton, based on a credit of $160 per ton of pig iron and a 20 pct interest rate of return on investment after taxes.

Jan 1, 1976

By E. E. Maust

The present work is part of an ongoing Bureau of Mines effort to provide a better understanding of the fundamental phenomena involved in sulfide flotation, the role of oxygen in xanthate adsorption being one essential issue. Galena was chosen as the material around which to develop a conceptual model, partly because of its demonstrated oxygen sensitivity and partly because information on its properties and flotation behavior constitutes the largest part of the fundamental information available on sulfides of commercial importance. The model is formulated primarily in terms of surface electronic energy levels produced by oxygen and xanthate and is further developed using existing experimental evidence and its implications. Four major functions of oxygen are elucidated, and the relationship of these to the formation of lead xanthate, dixanthogen, and a surface compound is discussed. Though yet incomplete, the model provides a useful framework within which the results of diverse experiments can be related to one another in their proper perspective, as shown by a brief discussion and resolution of some apparently discordant results reported in the literature.

Jan 1, 1976

By David Schlain

This Bureau of Mines report describes a method for electrodepositing titanium diboride from a molten salt bath. Initially, the electrolyte is a mixture of LiBO2, NaB02, Na2 Ti03 , Li2Ti03, and Ti02? The cell is operated at 900° C in a dry, inert atmosphere with consumable anodes of titanium or hot-pressed titanium diboride (TiB2) powder. Agitation of the electrolyte is essential. Current densities may be 6 to 9 amperes per square decimeter (amp/dm2) with titanium anodes and 9 to 30 amp/dm2 with titanium diboride anodes. A current density of 6 amp/dm2 is equivalent to a plating rate of about 35 micrometers per hour. The adherence of the TiB2 deposit varies with the substrate material. It is most adherent on molybdenum and on 4130 steel that has been preplated with copper and nickel, less adherent on nickel, and still less adherent on Inconel and on 4130 steel without the preplate. Cathode and anode reactions are suggested.

Jan 1, 1976

By James J. Snodgrass

The Bureau of Mines designed and constructed a series of calibration models for geophysical borehole logging. A nominal hole diameter of 3 inches was selected as representative of typical core holes drilled for mining and engineering purposes, although additional hole diameters of 2, 5, and 8 inches are provided in one of the models for determination of empirical correction factors for variations in hole diameter. The physical properties of the models were determined by laboratory analyses of drill core samples and evaluated statistically for reliability. This report outlines the location of the models, elements of design and construction, and results of the laboratory tests. The models are available at the Denver Federal Center, Denver, Colo., for use by Government agencies and private industry to calibrate logging equipment for measurements of density, sonic velocity, magnetic susceptibility, and electrical resistivity.

Jan 1, 1976