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By R. A. Guidotti

The Federal Bureau of Mines studied the thermal decomposition of the nitrides of the Group V A metals (CbN, Ta3N5, and VN) with the goal of preparing high-purity metals. Solid-state purification and arc and electron-beam melting were examined. Electron-beam melting proved to be the most efficient means of nitrogen and oxygen removal. Columbium and tantalum of 99.9-pct purity were prepared by this technique; in the case of vanadium, however, nitrogen could not be reduced below the solid-solution level.

Jan 1, 1976

By Arthur M. Hartstein

The Federal Bureau of Mines, under a contract with Ultrasystems, Inc., investigated the thermal oxidative degradation characteristics of conveyor belts used in underground mines. This included the determination of smoke evolution, glow characteristics, char yields, and the identification and quantification of all volatile decomposition products in the form of gram of specific product formed per gram of belt sample tested. In addition to these investigations, degradation studies were conducted on some pure ingredients used in conveyor-belt formulations. Three basic classes of belts were investigated: neoprene, polyvinyl chloride, and styrene-butadiene rubber compositions. The studies indicate that styrene-butadiene-based belts exhibit good flame resistance and are the least hazardous in regard to overall formation of toxic decomposition products. Under this program, thermogravimetric analysis was definitely established as a method of material differentiation.

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 P. T. Brooks

Electrochemical machining sludge, a troublesome fluid waste product, was dewatered on a bench-scale basis by three alternative methods tested by the Federal Bureau of Mines. These methods would enable recycling 89 percent or more of the liquid content of the sludge and allow the dewatered solids to be dumped as landfill or processed further to recover contained nickel. Dewatering by vacuum precoat filtration was estimated to be the least expensive. Based on treating 20,000 gallons per day of sludge, precoat filtration costs were estimated as totaling 1.96 cents per gallon of sludge. Two options of an alternative method, comprised of acidification, reprecipitation, thickening, and filtration, were estimated to cost either 3.41 or 3.60 cents per gallon of sludge.

Jan 1, 1976

By J. B. Janus

This report, the 25th in a series, lists analytical data of coal samples collected by the Bureau of Mines in connection with the purchase of several million tons of coal for various Government agencies during fiscal year 1975. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. Ultimate analyses are given for these coalbeds only. The delivered coal was sampled at destination in accordance with instructions furnished by the Bureau of Mines, and all samples were analyzed in the Bureau laboratory at Pittsburgh.

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 W. P. Diamond

Coalbeds exhibit a directional permeability, with the maximum permeability oriented parallel to the face cleat. Thus, the most efficient pattern of vertical degasification holes for a coalbed is dependent upon cleat orientation. Surface joints, infrared photolinears, and Ronchi grating photolinears were investigated as potential estimators of subsurface cleat orientation. Cleat orientations were measured in 18 mines, in the Pittsburgh coalbed in southwestern Pennsylvania and northern West Virginia to be used as a standard against which prediction techniques would be evaluated. Two cleat systems with a strong geographic segregation were measured in the study area: N 670 W -N 280 E (950 separation) for the north, and N 76° W -N 17° E (930 separation) for the south. Directional data obtained from the three techniques investigated yielded satisfactory regional predictions of cleat orientation. Analysis of surface joints was the only technique considered sufficiently reliable on a local basis. Prediction of cleat orientation is based on the pairing of the principal directional sets into all reasonable combinations of fundamental systems. The system or systems composed of the most dominant sets nearest to 90° separation are likely to be a reliable prediction of cleat orientation. The most dominant set of the system selected is likely to be the face cleat.

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 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 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 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 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 Willard L. Hunter

A series of steel heats, one low-alloy and nine carbon, was made by the Bureau of Mines in a 1-ton arc furnace from ferrous scrap from incinerated refuse, steel cans, and detinned steel cans, both alone and blended with heavy-melting scrap. Two additional control heats, one of carbon steel and one of low-alloy steel, were made from electric furnace heavy-melting scrap to pro-vide comparative data. The steel products were cast into two 4-by 4-inch nominal 50-pound ingots; in most heats, an 8-by 8-inch nominal 7S0-pound ingot was also obtained. Tests of these ingots indicated that reinforcing bars of acceptable quality can be made from urban refuse components such as steel cans.

Jan 1, 1976

By Jack E. Fraley

Magnesium oxysulfate cement has been specially formulated as a sealant in underground coal mines for reducing sloughing of shale roofs and coal ribs, for reducing air losses through block stoppings, for constructing sprayed stop-pings over approved jute cloth or metal lath, and for reducing combustibility of polyurethane foam. A standard spray machine (Mining Enforcement and Safety Administration (MESA) approved) was used for the underground testing. Our research shows that a 1/2-inch coating reduces shale and coal sloughing, reduces air losses through block stoppings, and prevents fire propagation through a metal tunnel lined with polyurethane foam. During the underground tests, excess mixing water was used to improve pumping the slurry to the spray nozzle. This was later found to increase shrinkage cracks in the cured coatings. Controlling excess water is important to an acceptable coating.

Jan 1, 1976

By Charles M. McCulloch

This Bureau of Mines report discusses the principles of using computers to draw maps and plot geologic data of mining areas. The types of maps that can be drawn by a computer are reviewed, using as examples two separate areas where poor roof and gas emissions caused mining problems. Such maps can be used not only to help identify problem areas, but also to predict areas where problems could occur, thus giving mine operators time to work out solutions prior to mining. The average cost of a computer-drawn map for a mine property is less than $100, including computer time and man-hours for data preparation.

Jan 1, 1976