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By Cavallaro. J. A.

This report presents the results of a washability study of 455 raw coal channel samples with special emphasis on sulfur reduction. These raw coals contained on the average 14.0 percent ash, 1.91 percent pyritic sulfur, and 3.02 percent total sulfur. The complete washability data are presented for each sample processed. A statistical evaluation is included for the coalbeds from which more than 10 samples were collected and for the geographical coal producing regions. A graphical summation is presented for the coal producing regions and selected coalbeds. Finally a similar statistical evaluation is included showing composited data interpolated at Btu recovery levels of 50, 60, 70, 80, 90, and 100 percent. Graphical summations are presented for the various coal producing regions. Generally, significant sulfur reduction is achieved if the coals are crushed to a finer size and the higher specific gravity increments are removed. If a 50-percent Btu recovery was acceptable, then 32 percent of the samples tested could be upgraded to meet the current Environmental Protection Agency (EPA) standard of 1.2 pounds of S02 emission per million (MM) Btu when crushed to 14-mesh top size and separated gravimetrically.

Jan 1, 1976

By David E. Emerson

The Bureau of Mines has developed a mass spectrometer method for deter-mining the helium-3 content of high-purity helium. The work was performed to evaluate experimental methods for removing helium-3 from high-purity helium and to better determine the composition of pure helium used in research. This was accomplished by increasing the inlet sample pressure, ionizing current, and amplification of the current produced by the ions collected on a conventional mass spectrometer that had been modified. With these modifications, the helium-3 content was determined in the parts-per-million and parts-per-billion range in helium-4.

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 G. M. Martinez

A cell concept adaptable to large-scale electrowinning of zirconium metal from zirconium tetrachloride was investigated by the Federal Bureau of Mines. Tests were made in twin cells, each 12 inches in diameter by 33 inches long. Electrowinning was performed in one chamber from which the electrolyte was transferred after electrolysis to the other chamber where it was renewed by the introduction of ZrC14 by direct sublimation. The formation of a salt plug in the connecting pipe provided a seal between the chambers. Optimum electrolyte composition, with respect to quality of the metal product (91 pct meeting ASTM standards except for the oxygen content) and current-carrying capability (about 350 amp) was determined to be 16.7 wt-pct NaF-83.3 wt-pct NaCl mixture plus ZrC14 equal to about 3 wt-pct zirconium. A twin-cell design incorporating the unit operations covered by this investigation is proposed.

Jan 1, 1976

By Lewis M. McNay

The strength characteristics of hydraulic sandfill modified by varying quantities of type III portland cement and two flocculants were investigated by the Bureau of Mines. Three different sand-cement ratios were examined using different percentages of flocculant. Two other experimental variables were curing time and weight-percent solids for hydraulic mixture. Results of unconfined compression tests with strain are discussed. Maximum strength was achieved with 0.5 weight-percent of ferric sulfate per ton of solids when the slurry mixture was 75 weight-percent solids. The bearing capacity of hydraulic sandfill is reduced by increasing the water content and decreasing the amount of cement mixed with sandfill.

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 M. J. Ferrante

The standard enthalpy of formation, low-temperature heat capacities, and enthalpy increments above 298 K were determined by the Federal Bureau of Mines for synthetic dawsonite [NaA1C03(OH)21. The enthalpy of formation was determined by hydrochloric acid solution calorimetry, with the result ?Hf°298 = -469.4±0.7 kcal/mole. The low-temperature heat capacities were determined from 6 to 307 K by adiabatic calorimetry. Tabulated are low-temperature values of Cp°, S°, and H.-Ho° from 3 to 298 K. The derived entropy at 298 K is S298 = 31.55±0.3 cal/deg mole. Enthalpy increments above 298 K were obtained by copper-block drop calorimetry. Tabular data of Cp°, S°, H°-H°298, -(G°-H°298)/T, ?Hf°, ?Gf°, and log Kf are given from 298 to 477 K. Enthalpies and Gibbs energies of decomposition are also reported.

Jan 1, 1976

By J. M. Singer

In this Bureau of Mines study coal and rock dust beds were entrained by airblasts generated by gas explosions at the closed end of a 0.61-m-diameter explosion tunnel, 49.7 m long. The system was designed to simulate entrainment of mine dust deposits by accidental gas explosion at the coal face of nonintersecting mine passageways. Full-scale mine explosion trials confirmed many of the results of the explosion tunnel experiments and indicated several new features of dust entrainment. Dispersal of 20.3-cm-long stepped dust beds located 35 m from the closed end always began during the early portion of the ascending gradient of the first transient airflow (and pressure) wave, and was usually completed before the end of the first quarter-wave period. Bulk quantities of dust were entrained simultaneously by longitudinal regression from the leading edge of the dust bed and by surface lifting of the top layer. Instantaneous threshold air velocities for bulk quantities of coal and rock dust beds in separate, mixed, and layered configurations were in the same range (5 to 30 m/sec) as previously found under steady-state velocity conditions. Selective lifting of coal dust layers from rock dust occurred when the threshold dispersal velocity of coal dust but not of the underlying rock dust was exceeded.

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 P. W. Jerant

The methane emissions from an advancing coal mine section were continuously monitored for 120 days. During this time, the section advanced 2,000 feet into virgin Pittsburgh coalbed producing 54,565 tons of coal with a total methane emission of 91 million ft3. Analysis of the data gathered showed that daily methane emissions did not correlate with overburden thickness and daily coal production. A good correlation was found between the daily methane emission and the average length of rib exposed to virgin coal.

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 John A. Breslin

Size distributions and concentrations of particulates emitted from diesel engine exhausts were measured with cascade impactors. Samples were taken from the exhaust of two types of engines using three types of fuel and operating under five different engine speed and load conditions. The measured mass median diameters of the diesel particulates were typically about 0.3 um. There was no significant difference in mass median diameter between engines or fuels and only a slight dependence on operating mode. Concentration measurements ranged from 14.2 to 250.9 mg/cu m, and calculated mass outputs, from 64 to 10,000 mg/min. Significant differences in mass output were found between engines, fuels, and especially between different operating modes. The quantity of clean dilution air that would be required to reduce the particulate mass concentration below the 2.0 mg/cu m respirable dust standard for coal mines was greater than the dilution air required to meet the standards for noxious gases for both engines tested.

Jan 1, 1976

By John A. Breslin

Size distributions and concentrations of particulates emitted from diesel engine exhausts were measured with cascade impactors. Samples were taken from the exhaust of two types of engines using three types of fuel and operating under five different engine speed and load conditions. The measured mass median diameters of the diesel particulates were typically about 0.3 um. There was no significant difference in mass median diameter between engines or fuels and only a slight dependence on operating mode. Concentration measurements ranged from 14.2 to 250.9 mg/cu m, and calculated mass outputs, from 52 to 3,443 mg/min. Significant differences in mass output were found between engines, fuels, and especially between different operating modes. The quantity of clean dilution air that would be required to reduce the particulate mass concentration below the 2.0 mg/cu m respirable dust standard for coal mines was greater than the dilution air required to meet the standards for noxious gases for both engines tested.

Jan 1, 1976

By Robert P. Vinson

This report describes three coal mine ventilation studies by the Bureau of Mines in which sulfur hexafluoride (SF6) was used as a tracer gas. One of these studies was conducted to determine air movement and leakage in a sealed area. Another was run to determine the ventilation efficiency of a bleeder system. Finally, a study was made of air leakage across permanent stoppings of parallel intake airways. These studies proved sulfur hexafluoride to be a useful addition to the equipment commonly used in coal mine ventilation analysis.

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 D. L. Paulson

The Bureau of Mines studied the feasibility of producing copper matte in an electric furnace from blends of copper concentrate similar to those currently smelted in a gas-fired reverberatory system at an installation in Tacoma, Wash. A 800-kva electric-arc furnace was used to determine the distribution of constituents when arseniferous concentrates are being smelted in an electric-arc furnace. Test results from smelting 40 tons of materials indicated that electric smelting is more like a conventional gas-fired system than originally expected. Although gas composition over the molten bath is much different in an electric furnace, the secondary constituents such as arsenic, lead, zinc, and antimony behaved the same as in a reverberatory furnace. The results established that an electric furnace would be compatible with sulfur and particulate recovery facilities that are being used.

Jan 1, 1976

By B. J. Scheiner

The Federal Bureau of Mines has successfully demonstrated an electrooxidation-solvent extraction-carbon adsorption process for recovering molybdenum and rhenium from offgrade concentrates. The flow sequence consists of dissolution of metal values by electrooxidation, liquid-solid separation by thickening, acidification and chlorate ion removal by sulfur dioxide treatment, solvent extraction to concentrate the molybdenum and rhenium, separation of molybdenum and rhenium by carbon adsorption, and metal recovery by crystallization. Molybdenum and rhenium were recovered as ammonium paramolybdate and ammonium perrhenate. Electrolysis of brine-concentrate pulps to generate a hypochlorite oxidizing agent in situ resulted in the dissolution of 98.9 and 99.1 pct of the molybdenum and rhenium, respectively, at an energy consumption of 13.7 kwhr/lb of molybdenum extracted.

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