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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 Benjamin W. Haynes

This research was conducted as part of the U.S. Department of the Interior, Bureau of Mines program to recover metals, glass, and a combustible fraction from municipal solid waste (MSW). The objective of this analytical study was to determine the concentration of antimony, arsenic, and mercury in samples taken from various sampling areas in the Bureau of Mines raw refuse recycling plant and to compare these values with those for coals used in the generation of electricity. To provide the necessary analytical data, sensitive reproducible ashing-chemical digestion-atomic absorption procedures were adapted from published procedures. It was determined that antimony and mercury concentrations in the combustible fraction of MSW are approximately an order of magnitude higher than those found in coals presently used for power generation;' the arsenic concentration is similar in both fuels.

Jan 1, 1978

By V. R. Miller

The Bureau of Mines developed and evaluated a detecting and sorting device to separate the copper-bearing portion from the barren portion of Michigan native copper ore in the minus 4- plus 1-inch size range. Small-scale sorting tests were also conducted on minus 1- plus 1/2-inch material from the Centennial No. 6 mine, using a previously developed system that was modified to increase sensitivity. Results showed that, with the added sensitivity, 85 to 90 pct of the copper in the minus 1- plus 1/2-inch material could be recovered in about 50 to 60 pct of the fraction. Sorting tests on minus 4- plus 2-inch and minus 2- plus 1-inch fractions from the Centennial mine were conducted with the large sorting system. Results showed that 86 to 93 pct of the copper was recovered in 43 to 64 wt-pct of the sorted fractions. Combining of concentrates from the two fractions resulted in a recovery of 90 pct of the Popper in 55 pct of the weight. The composite concentrate contained 2.40 pct copper, and the tailing analyzed 0.33 pct Cu; the head sample assayed 1.46 pct Cu.

Jan 1, 1978

By Calvin K. Lee

This Bureau of Mines report describes a simple fire-retardant treatment for wood. The treatment involves preheating the wood surface at high heat flux (~0.6 cal/cm2 sec) to form an in situ surface char layer (~3 mm thick) on the wood. Laboratory-scale fire tests show that the precharring technique improves the fire-resistance of virgin wood by decreasing and delaying generation of volatile gases through thermal insulation effect of the surface prechar layer.

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. J. Ferrante

Low-temperature heat capacities and high-temperature enthalpies for syn¬thetic Cu2S and CuS were measured. This investigation is part of the Bureau of Mines goals to provide thermodynamic data essential to the more efficient processing of copper ores, and thereby minimize the current dislocations in energy, environment, and mineral supply. Heat capacities were measured with an adiabatic calorimeter from 5 to 310 K, and resulted in S°298 = 27.76 for Cu2S(c) and S°298 = 16.05 cal/deg mole for CuS(c). Low-temperature values are tabulated for Cp°, S°, -(G°-Ho°)/T, and H°-Ho°. Enthalpies were measured with a copper block calorimeter from 298.15 to 1,600 K for Cu2S(c,1) and 298.15 to 780 K for CuS(c). The thermal behavior of CuS showed no transitions or other significant anomalies for the low- or high-temperature investigations. Cu2S showed reversible transitions at 376 K with an isothermal heat absorption of 0.865 kcal/mole, 720 K with an isothermal absorption of 0.280 kcal/mole, and approximately 1,400 K (congruent melting point) with a heat of fusion of 3.070 kcal/mole. High-temperature data are tabulated for H°-H°298, Cp°, S°, and -(G°-H°298)/T. Enthalpies are also expressed in equation form. The low¬and high-temperature data were combined with data from the literature to cal¬culate and tabulate ?Hf°, ?Gf°, and log Kf as a function of temperature.

Jan 1, 1978

By P. B. Altringer

The Bureau of Mines conducted laboratory tests to devise a procedure for recovering a marketable grade of tungsten from the brine of Searles Lake, Calif. The brine contains only 56 parts per million of tungsten (70 parts per million of W03). Using ion exchange resins synthesized by Bureau chemists, 98 percent of the tungsten was extracted from the brine and 92 percent of the tungsten was recovered as a marketable iron-tungsten concentrate containing 44 percent tungstic oxide. Although major technical problems have largely been resolved, research is progressing to escalate testing in a process-development unit to provide more reliable data for an economic appraisal.

Jan 1, 1978

By Ann G. Kim

The Bureau of Mines investigated factors that influence the formation of methane and other hydrocarbon gases in coal, which is an integral part of the coalification process. Coalification begins with a biogenetic stage in which plant debris decomposes and peat is formed; methane and CO2 are the predominant gases produced during this stage. During the diagenetic stage of coalification hydrogen and the hydrocarbon gases methane, ethane, ethylene, propane, propylene, butene, iso- and normal butane, and pentane are formed by dissociation of the organic material. Methane may also be produced by a secondary reaction of hydrogen with unsaturates or by the reduction of CO2. The gas contained in coalbeds is a mixture of methane, C2 through C5 alkanes, CO2, 02, N2, H2, and H2; its heating value is equivalent to that of natural gas. The gas content of coal depends on many variables, but an empirical relationship between adsorptive capacity, rank, and depth has been observed.

Jan 1, 1978

By Ann G. Kim

The Bureau of Mines investigated factors that influence the formation of methane and other hydrocarbon gases in coal, which is an integral part of the coalification process. Coalification begins with a biogenetic stage in which plant debris decomposes and peat is formed; methane and CO2 are the predominant gases produced during this stage. During the diagenetic stage of coalification hydrogen and the hydrocarbon gases methane, ethane, ethylene, propane, propylene, butene, iso-and normal butane, and pentane are formed by dissociation of the organic material. Methane may also be produced by a secondary reaction of hydrogen with unsaturates or by the reduction of CO2. The gas contained in coalbeds is a mixture of methane, C2 through C5 alkanes, CO2, O2, N2, H2, and He; its heating value is equivalent to that of natural gas. The gas content of coal depends on many variables, but an empirical relationship between adsorptive capacity, rank, and depth has been observed.

Jan 1, 1978

By S. E. Khalafalla

The ability of potentiometric, gas-sensing electrodes to reliably monitor free gaseous molecules in solution has been recently demonstrated. A gas such as sulfur dioxide from a dilute sample solution diffuses through a hydrophobic, gas-permeable membrane to an internal filling solution. The latter solution contains a sufficiently large excess of sodium bisulfite, the concentration of which can be considered constant regardless of the quantity of sulfur dioxide entering by diffusion. The electrode response is essentially due to the liberated hydrogen ions from the bisulfite-sulfur dioxide equilibrium. This Bureau of Mines report describes a new technique used to detect the formation, and to estimate the stability constant, of gas-molecule and gas-ion complexes in solution, as part of an effort to minimize the undesirable environmental impacts associated with mining and mineral processing. Although the unknown activity coefficients of the neutral and ionic species in the external solution complicate the quantitation of results, methods to circumvent these difficulties are presented. The technique is based on the isometric shift of the Nernst diagram of ion-selective electrodes to higher concentrations relative to the standard aqueous calibration curve. The method is applied to detect and estimate the formation constant of a sulfitocitrate complex, and agrees well with an independently determined stability constant of the disulfitomercu-rate complex.

Jan 1, 1978

By Benjamin W. Haynes

The Bureau of Mines conducted research to devise technology for increasing the Nation's mineral supply by recovering valuable constituents from currently discarded waste materials. Municipal solid waste (MSW), presently a major disposal problem, represents a significant source of metals, glass, and a combustible fraction that can be used to supplement coal in generating heat and electricity. As part of the total metallurgical system to treat MSW, this study evaluates the combustible fraction of MSW to characterize the various combustible components and to identify the principal sources of elements that eventually may be objectionable from corrosive or environmental considerations. Several possible sources for cadmium, chromium, cobalt, copper, lead, nickel, and zinc have been tentatively identified. These sources are pigments, inks, paper stock, and additives to plastics. A correlation between industry consumption values and measured concentrations in MSW was found for several elements.

Jan 1, 1978

By R. P. Beyer

Low-temperature heat capacities and standard enthalpy of formation of copper difluoride (CuF2) were determined by the Bureau of Mines. The low-temperature heat capacities were determined from 11 to 302 K by adiabatic calorimetry. The enthalpy of formation was determined by HC1 solution calorimetry. The standard values of entropy (S°) and enthalpy of formation (?Hf°) at 298.15 K are l8.65±0.03 cal/deg mole and -129.02±0.29 kcal/mole, respectively.

Jan 1, 1978

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 Raymond F. Farrell

A goal of the U.S. Department of the Interior, Bureau of Mines, is the advancement of minerals technology through the development of improved metals and minerals processing. In support of this goal, the Albany Metallurgy Research Center has developed atomic absorption spectrographic methods for the rapid analysis of A1203, CaO, Fe203, MgO, MnO, and Si02 in steelmaking slags. The application of these methods is discussed using an inexpensive pressure dissolution system. The overall coefficient of variation is 5 pct. The accuracy is the same as the reproducibility.

Jan 1, 1979

By A. Visnapuu

The Bureau of Mines, as a part of its goal to minimize occupational hazards associated with mining and mineral processing operations, has developed and field tested a compact exhaust air muffler for mechanized, jumbo-mounted pneumatic rock drills. The muffler is constructed of 1/8-inch sheet steel and has nominal dimensions of 1-3/4 by 9 by 13 inches. A directed air passage, flexible neoprene baffles, and an expandable slit-type outlet are incorporated to reduce drill exhaust air noise and eliminate muffler icing. Field tests in actual mining operations showed a l5-dbA reduction in exhaust noise and an 8-to 12-dbA reduction in overall drilling noise with no icing problems or decrease in drill performance. Data are presented on muffler construction, laboratory, and field test results.

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 L. A. Haas

The U.S. Department of the Interior, Bureau of Mines, is conducting laboratory-scale research to determine the leaching conditions required with sulfuric acid for extracting base metal from a matte with a copper-to-nicke1 ratio of 6 to 1. The matte (61.2 pct Cu, 9.7 pct Ni, 3.3 pct Fe, 21 pct S, and about 5 oz of precious metals per ton) was prepared from Duluth Complex (Minnesota) ore by smelting a bulk sulfide flotation concentrate. The matte was pre leached at atmospheric pressure to selectively extract 20 pct of the nickel, and the undissolved solids were referred to as the matte residue. Autoclave leaching of the matte residue extracted over 95 pct of the nickel, copper, and iron. The remaining leach residue in the autoclave contained over 100 oz of precious metals per ton. The leaching conditions required were matte grind of greater than 98 pct minus 325 mesh, pulp concentration of 50 g/1, total pressure of 100 psig with oxygen at 150° C or 400 psig with air at 180° C, 50 g/1 H2S04, 700 rpm agitator speed, and 6 hours of leaching time. The leaching time was decreased to 2 hours by increasing the agitator speed to 1,300 rpm. Sulfuric acid concentration greater than 50 g/1 did not appreciably enhance the base metal extraction, but with less acid, residues with higher iron concentrations were obtained. Supersaturation of the liquor was prevented at 150° C by using a 1ixiviant that contained 30 g/l Ni and 20 g/1 Cu.

Jan 1, 1979

By W. N. Cathey

Many materials including carbides, silicides, phosphides, borides, nitrides, oxides, and metals were studied by the Bureau of Mines as potential fuel cell catalysts for electroreduction of oxygen in a 1[N]H2S04 electrolyte. The objective of this study was to assess the potential of abundant, low-cost materials as substitutes for platinum or to increase the catalytic efficiency of platinum. Several compounds were rejected because of their reaction in the corrosive environment of the oxygen electrode. However, some of the remaining were the most active catalysts. Activity of carbides such as tungsten carbide could be improved by doping with platinum-group metals, by varying stoichiometry, or by sputtering on a layer of platinum. While no catalysts were found with activity as high as platinum, some compounds were shown to be deserving of further investigation.

Jan 1, 1979

By T. E. Bernard

The CO2-absorbent canisters used in four approved rescue breathing apparatus were investigated. A breathing machine was used to simulate human expiration with gas flow rates of 26, 37, and 48 1/min of 3.5% CO2 in air. The exit gas CO2 concentration, the pressure drop across the canister, and the exit-gas temperature were monitored. The absorbent capacities of the packed-bed canister designs were found to be dependent on flow rate within the range studied, while the capacities of the other designs were less affected. The radial canister had the least resistance to breathing while the complex bed design proved to be the most effective in utilization of the chemical. The overall results indicated that LiOH (lithium hydroxide) has the highest capacity for CO2 absorption among the absorbents tested. It can be used in a simple packed-bed design while maintaining acceptable levels of resistance and exit-gas temperature. Examination of oxygen supply with respect to CO2-absorption capacity suggested that it is desirable to closely match CO2-absorption capacity with the avail-able O2 supply to minimize the size and weight of rescue breathing apparatus.

Jan 1, 1979