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By Raymond M. Stateham

Climatic conditions are compared with roof fall occurrence from April 1, 1972, to December 31, 1975, by the Bureau of Mines. These comparisons indicate that humidity has a strong influence on roof fall occurrence rates. Cubic regression techniques are used to develop best fit curves. Statistical analysis of these curves indicate that both are sinusoidal and exhibit positive correlation with each other. The sine waves have a period of 1 year with maximum and minimum inflection points in August and February.

Jan 1, 1978

By H. W. Kilau

The Bureau of Mines used a high-temperature rotational viscometer to test basic oxygen furnace slags to determine fluorspar requirements and to evaluate colemanite and fused boric acid as substitute fluidizers. A continuous technique of viscosity measurement was adapted to better determine the viscosity-temperature profiles of volatile fluorspar slags. Criteria used for estimating slag fluidizer effectiveness were (1) the apparent solidification temperature, and (2) the temperature range of slag crystallization. Colemanite and fused boric acid in high-basicity slag were superior fluidizers to fluorspar when compared on the basis of boron versus fluorine concentration. Fused boric acid was nearly equivalent to ceramic-grade fluorspar when compared on a simple weight basis, while colemanite was inferior to fluorspar. Fluorspar slags volatilized fluorine during viscosity testing. Colemanite and fused boric acid slags were stable, no boron losses being detected. A fluidizing limit was found for fluorspar at 2.9 percent fluorine concentration; higher concentrations impaired viscosity and caused foaming and crusting of slag. Concentrations of boron up to 4.4 percent resulted in very fluid slags with no fluidizing limit.

Jan 1, 1978

By Frank G. Horino

Drill cores from 18 exploratory holes that were drilled into the unleached saline beds were tested for mechanical properties by the Bureau of Mines. Test cores were primarily selected from zones L4B, R4B, L3, and R3A in the Piceance Creek Basin, Rio Blanco County, Colo. Regression analysis techniques were tried in an attempt to relate kerogen yield or apparent specific gravity to the parameters compressive strength, Young's modulus, and Poisson's ratio. Correlation coefficients were very poor, indicating that this type of analysis was not amenable to these data. Analysis of variance techniques were tried using a division of either greater than or less than 10% nahcolite together with the requirement of less than 3% dawsonite. Results showed that a larger percentage of nahcolite tended to lower the compressive strength and to increase Young's modulus. A second analysis was made using a division of less than 3% dawsonite and greater than 3% dawsonite together with the requirement of less than 1% nahcolite. For this analysis, a larger per-centage of dawsonite tended to increase compressive strength, Young's modulus, and Poisson's ratio. Mean compressive strength values were determined for the mining horizons of interest. Average physical properties for design purposes were also determined for the horizons of interest and for a proposed adit based only on logged geologic depths to these horizons. No consideration was given to percentages of nahcolite and dawsonite. Creep data obtained from nahcolite-and dawsonite-rich oil shales provides a best fit to a modified power equation.

Jan 1, 1978

By Seth C. Schaefer

As part of the Bureau of Mines, U.S. Department of the Interior, effort to provide thermodynamic data for the advancement of minerals technology, the Gibbs energy of formation of sphalerite (zinc sulfide) was investigated with a high-temperature galvanic cell employing stabilized zirconia as the electrolyte. In the temperature range 948 to 1,210 K, potential measurements were obtained for the cell Pt, ZnS + ZnO, S02 = 1 atm // Zr02 // Cu20 + Cu, Pt, with the overall cell reaction ZnS(c) + 3 Cu20(c) = ZnO(c) + 6 Cu(c) + S02(g). (1) These results, combined with the best available values of ?Gf° for ZnO, S02, and Cu20 from the literature, give the Gibbs energy of formation of zinc sulfide for the reaction Zn(l,v) + 1/2 S2(g) = ZnS© (2) ?Gf° = -64.223 + 24.02 X 10-3T ± 0.650 kcal/mole (3) (948-1,180 K; standard states - pure liquid zinc and S2 gas at 1 atm), and ?Gf° = -92.720 + 48.17 X 10-3 ± 0.650 kcal/mole (1,180-1,210 K; standard states - pure zinc vapor and S2 gas at 1 atm). A third law analysis yields for the formation reaction Zn(1) + 1/2 S2(g) = ZnS(c), (5) a standard enthalpy of formation as follows: ?Hf298.15 = -63.64 ± 0.700 kcal/mole.

Jan 1, 1978

By H. Kenneth Sacks

The Bureau of Mines has developed hardware for electromagnetic (EM) detection and location of miners trapped in underground coal mines. This report describes a technique for using the developed equipment for locating uncased boreholes underground. Results of several field and laboratory experiments are described.

Jan 1, 1978

By M. M. Tilman

The Bureau of Mines conducted research to determine whether it is possible to substantially improve the fatigue resistance of lead sheet by means of surface coatings. Five types of coatings were applied to unalloyed chemical lead sheet. Flexural tests revealed that the best fatigue resistance was obtained with coatings of vacuum grease. Vacuum-grease coatings on unalloyed lead sheet resulted in fatigue resistance at least as good as that of the fatigue-resistant alloy Pb-0.04 Ca. Coated lead sheet was also tested in short-time tensile tests and in tensile creep tests. Tensile and yield strengths were increased by several of the coatings with only moderate loss of ductility. Creep resistance was also improved in varying degrees by most of the coatings. The Bureau also conducted research on the effectiveness of noise barriers by using sheet lead in combination with other materials. Noise barriers consisting of continuous-cast sheet lead with gypsum board were found to be effective and relatively inexpensive barriers.

Jan 1, 1978

By W. R. McDonald

The Bureau of Mines, U.S. Department of the Interior, conducted small-scale field tests on acidic copper tailings as part of its effort to develop, improve, and demonstrate technology for stabilizing mining and mineral-processing wastes. Two successful demonstration revegetation plots were established on an abandoned copper-tailings pond located on public land adjacent to Holden Village, Wash. The tailings were neutralized with treatments of either dolomitic lime or limerock and fertilized with processed sewage sludge and/or commercial fertilizer. Excellent plant growths covering 70 and 24 percent of the surface were achieved on 1/8-and 1-1/2-acre test plots planted in 1973 and 1974, respectively. Regar brame, Tegmar intermediate wheatgrass, and tall wheatgrass provided the best plant growth and surface coverage. The target pH of tailings neutralization was 6.8; however, good plant growth occurred in areas where the soil pH ranged from 2.9 to 5.8.

Jan 1, 1978

By Richard G. Sandberg

Sphalerite concentrates prepared during processing of Missouri lead ores contain small percentages of cobalt and nickel which adversely affect zinc electrolysis. The Bureau of Mines has evaluated solvent extraction and precipitation techniques to remove and recover cobalt and nickel from zinc sulfate solution prior to zinc electrolysis. Prepared zinc sulfate solutions containing about 190 gpl of zinc and 50 ppm of both cobalt and nickel were treated using various combinations of complexing reagents, solvent, pH, concentration, time, and temperature. The following complexing reagents gave the best results: a-nitroso-ß-naphthol, ß-nitroso-a-naphthol, 1,2 cyclohexane dione dioxime (nioxime), di-2-pyridyl ketone oxime, and dimethylglyoxime. These reagents in suitable solvents lowered the cobalt and nickel levels to <0.1 ppm. Stripping the complexed reagents from the solvents was not possible except for nioxime. Direct addition of the appropriate reagent to the prepared zinc sulfate solution resulted in the precipitation of cobalt and nickel. Several possible flowsheets are presented for the removal and recovery of cobalt and nickel. Good zinc deposits were successfully electrowon from zinc sulfate solutions purified by solvent extraction and precipitation.

Jan 1, 1978

By R. K. Clifford

Chalcopyrite (CuFeSz) concentrates produced on the Lead Belt of Missouri typically contain 28 pct Cu and from 0.5 to 1.5 pct each of nickel and cobalt. Most of the nickel and cobalt are present as the mineral siegenite, (Ni,Co)3S4, almost none of which is recovered presently. The Bureau of Mines, U.S. Department of the Interior, has been conducting research on the chalcopyrite to produce a marketable fraction enriched in cobalt and nickel. Ferric chloride leaching of various chalcopyrite (copper) concentrates has yielded residues containing from 10.2 to 16.2 pct Ni and 8.3 to 11.4 pct Co with recoveries of approximately 79 pct. In another approach, laboratory froth-flotation tests have been conducted to investigate the effects of regrinding, roasting, baking, and steaming prior to flotation, with a variety of reagents. The best laboratory results were obtained after regrinding the copper concentrate to 94 pct minus 400 mesh and floating the chalcopyrite at natural pH (6.5) with 0.48 pound of sodium diethyldithiophosphate and 0.01 pound of sodium cyanide per ton of concentrate. This procedure yielded a tailings assaying 20.4 pct Cu, 5.2 pct Ni, and 3.45 pct Co. The tailings contained 67.2 pct of the nickel and cobalt and 15.9 pct of the copper originally in the copper concentrate; the remainder of the values reported to the flotation concentrate, which analyzed 29.6 pct Cu. To verify the laboratory flotation results, a 60 kg/hr process demonstration unit (PDU) was constructed in the Cominco American Magmont mill, Bixby, Mo.

Jan 1, 1978

By David R. Flinn

This Bureau of Mines report describes methods to electrodeposit erosion-resistant titanium diboride coatings from molten alkali metal borate baths at 900° C. These coatings have been shown to be highly resistant to material loss during impingement with high-velocity alumina and silicon carbide powders, and they show promise as protective coatings to reduce metal loss in erosive chemical environments, such as coal gasification systems. The most erosion-resistant coatings were prepared on nickel, Inconel, and molybdenum from an electrolyte containing LiBO2, NaBO2, Na2Ti03, and TiO2. The best coatings were deposited at current densities of [~]20 ma/cm2, using titanium or titanium diboride anodes. Erosion-resistant coatings were shown to exhibit (1) a high degree of crystallographic orientation along the (100) or (110) planes, (2) a chromium impurity level of less than 3 pct, and (3) a uniform, smooth, consolidated surface appearance when viewed under a microscope or by scanning electron microscopy. Optical spectroscopic studies of the molten electrolyte suggest that the lower valent (+3) titanium ion predominates in the baths.

Jan 1, 1979

By J. S. Hansen

In support of its objective to conserve mineral resources by minimizing premature failure of materials, the Bureau of Mines conducted a cooperative study with the U.S. Department of Energy on the erosion and abrasion resistance of hard materials for valves in coal conversion systems. This report describes a newly developed erosion-testing apparatus and presents data on the erosion resistance of over 200 materials. Erosion resistance of most metals was comparatively low. In contrast, ceramics and cermets such as B4C, WC, SiC, Si3N4, and TiB2, when fabricated to minimize porosity, displayed greater than five times the erosion resistance of metals. Coatings such as boron diffused into Mo and WC, chemical-vapor-deposited TiCN, and electrodeposited TiB2 were highly erosion resistant if applied in thicknesses ranging from 60 to 75 µm. Erosion resistance of cemented carbides was inversely related to metal binder content.

Jan 1, 1979

By P. C. Good

This Bureau of Mines report describes the preparation of phosphoric acid directly from phosphate ore, without prior beneficiation, in a small-scale, continuous process research unit, as part of an effort to improve minerals and metals recovery from domestic resources while minimizing environmental effects. Three phosphate-matrix samples, ranging in grade from 18.2 pct P20S5to 11.9 pct P205, were dry-fed at a rate of 1.82 kg/hr (4 lb/hr) to a continuous-circuit, 12-liter, single-tank digester to yield phosphoric acid and byproduct gypsum filter cake. Comparison with earlier data shows that a significantly improved filtration rate was attained in a single-tank reactor compared with that attained in a five-tank reactor train processing the same ore. Iron and aluminum impurities in the product phosphoric acid averaged about 60 pct higher than amounts reported in commercially prepared, concentrate-derived acid. All gypsum filter cakes prepared had a firm, sandy texture, rendering them physically suitable for stacking or landfill use. Introduction of dry attritioning and air classification approximately doubled the attainable filtration rate when the dry-beneficiated product was digested. In air classification, there was a 12-to 14-pct P205 loss. Depending on the technique used and the matrix grade, overall P205 recovery ranged from about 72 to 89 pct.

Jan 1, 1979

By D. E. Shanks

As part of its goal to help maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines, U.S. Department of the Interior, is investigating a fused-salt electrolytic procedure for producing zinc metal. A previous report described preliminary, small-scale work on the fused-salt electrolysis of ZnC12. The present report covers a more detailed investigation of the properties of ZnC12-alkali metal chloride electrolyte systems in relation to the production of zinc metal and also discusses electrolysis in largescale, internally heated cells. The effect of composition on bath stability, current efficiency, cell voltage, and liquidus temperature was determined for the ZnCla-NaC1-KC1, ZnC12-NaC1-LiC1, and ZnC12-KC1-LiC1 electrolyte systems. An electrolyte com-posed of 38 mole-pct ZnC12, 31 mole-pct NaC1, and 31 mole-pct KC1 gave the best overall results. Sludge (ZnO) formation in the ZnC12-NaC1-KC1, ZnC12-KC1-LiC1, and ZnC12-KC1 systems was investigated during prolonged electrolysis. The ZnC12-KC1-NaC1 electrolyte showed the least sludge formation. A 1,500-amp cell was operated using the ZnC12-NaC1-KC1 electrolyte at 500° C. Zinc metal was produced at the rate of 4.0 lb/hr with a current efficiency of 95 pct.

Jan 1, 1979

By William C. McBee

Specialized sulfur concretes were developed by the Federal Bureau of Mines as a result of research for the beneficial utilization of sulfur in construction materials. Materials were developed for use in acid and salt corrosive environments where portland cement concrete has been found to deteriorate. Because the mineral aggregates also come into contact with the corrosive media, concretes were developed utilizing both limestone and quartz aggregates. The sulfur binder used with both aggregates was modified by reaction with 5 pct dicyclopentadiene to improve product durability. Sulfur quartz aggregate concrete was found to have moderately high strength characteristics (6,000 psi compressive) and was extremely resistant to chemical attack by both acid and salt solutions. Sulfur limestone aggregate concrete exhibited very high strength characteristics (9,000 psi compressive) and was extremely resistant to chemical attack of salt solutions. Both types of concretes maintained their strength and integrity after long-term testing in acid and salt solutions and exhibited considerable resistance to damage by the action of freezing and thawing. Potential uses include leach tanks, electrolytic cells, thickeners, bridge decking, industrial flooring, pipe, and tile.

Jan 1, 1979

By J. B. Stephenson

The Bureau of Mines, under an interagency agreement with the Department of Energy (DOE), investigated the feasibility of hardfacing the critical surfaces of valves and similar devices by chemical vapor deposition. The purpose of this research was to increase the wear resistance of these components for use in the abrasive and erosive environment of coal gasification units. Tungsten and molybdenum coatings were produced on nickel-plated carbon steels and stain-less steels by hydrogen reduction of the metal hexafluoride at 325° to 600° C. Titanium nitride coatings were produced on low-carbon steels by the reaction of titanium tetrachloride, hydrogen, and nitrogen at 1,000° C. Titanium carbonitride coatings were produced on low-carbon steels by the reaction of nitrogen, hydrogen, and methane at 900° C. Tungsten, molybdenum and titanium nitride coatings were formed on 6-, 10-, and l2-inch (0.15-, 0.25-, and 0.30-meter) ball valve seats for evaluation in the low-Btu coal gasification pilot plant at the Morgantown Energy Research Center, Morgantown, W. Va.

Jan 1, 1979

By Max L. Glenn

As part of its goal to minimize requirements for mineral commodities through conservation and substitution, the Bureau of Mines conducted research to develop molybdenum as a potential substitute for superalloys containing the strategic and critical materials, nickel, chromium, and cobalt. Since molybdenum requires protection from oxidation at high temperatures, several complex oxides of the spinel and perovskite structure were investigated to determine which possessed the greatest potential for use as oxidation-barrier coatings. Two spinels (MgCr204 and MgA1204) and five perovskites (BaHfO3, YCrO3, NdCrO3, BaZrO3, and LaCrO3) were selected for testing. Various high-temperature prop¬erties that are important for oxidation-resistant coatings were examined, including diffusion rates of oxygen and molybdenum, recession (vaporization) rates, hardness, erosion resistance, sinterability, reactivity with molybdenum, and ease of application. From the evaluation of high-temperature properties, two spinels (MgCr204 and MgA1204) stand above the other oxides as possible coatings for molybdenum. However, laboratory coatings of MgCr204 at 1,360° C (2,480° F) are equivalent or inferior to currently available MoSi2 coatings; laboratory coatings of MgA1204 may be comparable under limited conditions to currently available MoSi2 coatings at the same temperature.

Jan 1, 1979

By L. E. Schultze

As part of the Bureau of Mines research program on recovering alumina from domestic resources, methods for extracting iron from aluminum sulfate solutions (obtained by leaching kaolinitic clay with dilute sulfuric ,acid) were investigated. In countercurrent extraction experiments at a l-gal/hr flow rate of aluminum sulfate leach liquor, the iron concentration &apos;was decreased from 1.4 g/l to 0.01 g/l after four stages of using a primary amine extractant. The iron-loaded amine solution was regenerated in five stages using 3[N] sulfuric acid or in four stages using 6[N] sulfuric acid. The aluminum sulfate solution obtained was suitable for the preparation of alumina meeting cell-grade standards of less than 0.01 pct iron.

Jan 1, 1979

By A. T. Iannacchione, D. G. Puglio

The Bureau of Mines established geologic factors affecting the mining of the Lower Kittanning coalbed to aid in coalbed minability studies and examined the occurrence of "wants" (places where coal is missing) and types of unstable roof rock strata. Trends established from mapping, including prediction of areas of high methane emissions, were extrapolated to unmined areas. "Wants" in the coalbed are of two types: Erosional and depositional. Erosional features occur where north-south-trending sand-filled channels cut into the coalbed. Variations in depositional environments have caused the coalbed to "split" into several thinner units. Slickensides, commonly indicative of unstable roof, are adjacent to and on the underside of sandstone channels; they were caused by differential compaction and by soft sediment sliding along the contact between the sandstone and adjacent shale. The frequency of unstable roof also increases where the interval between the Middle and Lower Kittanning coalbed is less than 30 feet. The zones of weakness at the contacts above and below the Middle Kittanning coalbed are the controlling factors for unstable roof in these strata. Methane emissions from the coalbed are controlled primarily by depth, fracture permeability, and rank of coal. Local geologic factors are coalbed thickness, associated rock strata, structure, and proximity to outcrop.

Jan 1, 1979

By A. T. Iannacchione

The Bureau of Mines established geologic factors affecting the mining of the Lower Kittanning coalbed to aid in coalbed minability studies and examined the occurrence of "wants" (places where coal is missing) and types of unstable roof rock strata. Trends established from mapping, including prediction of areas of high methane emissions, were extrapolated to unmined areas. &apos;Wants&apos; in the coalbed are of two types: Erosional and depositional. Erosional features occur where north-south-trending sand-filled channels cut into the coalbed. Variations in depositional environments have caused the coalbed to "split" into several thinner units. Slickensides, commonly indicative of unstable roof, are adjacent to and on the underside of sandstone channels; they were caused by differential compaction and by soft sediment sliding along the contact between the sandstone and adjacent shale. The frequency of unstable roof also increases where the interval between the Middle and Lower Kittanning coalbed is less than 30 feet. The zones of weakness at the contacts above and below the Middle Kittanning coalbed are the controlling factors for unstable roof in these strata. Methane emissions from the coalbed are controlled primarily by depth, fracture permeability, and rank of coal. Local geologic factors are coalbed thickness, associated rock strata, structure, and proximity to outcrop.

Jan 1, 1979

By Martin Hertzberg

A comprehensive study of the flammability behavior of air-dispersed coal dust was made using an 8-liter Bureau of Mines system which included the following: (1) An optical probe to continuously monitor the dust concentration; (2) measurements of ignition energy requirements; (3) the use of several narrow size distributions ranging from 3 to 65 µm in average diameter; (4) measurements of the extent of flame propagation based on pressure attained at constant volume, residual O2 content after combustion, and flame and dust surface temperatures. The measured lean limit for near-horizontal propagation of Pittsburgh coal dust was about 135 mg/l (milligrams per liter), virtually independent of particle size. Required ignition energies were hundreds of joules and measured limit flame temperatures were 1,450 to 1,600° K. Data on inerting? requirements with KHC03, rock dust, and NaC1 gave approximately the same results as full-scale explosion tests. The good agreement suggests that the cause of earlier discrepancies between small-scale laboratory data and full-scale mine experiments may not have been the difference in size, but were rather a problem of proper care in isolating and controlling the significant experimental variables and in consistently defining the extent of flame propagation at the limits.

Jan 1, 1979