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By R. B. Schluter

The Bureau of Mines investigated the flotation responses of two copper-nickel ore samples from the Duluth Complex with the objective of recovering bulk sulfide concentrates. One of the ores studied was taken from a test pit; the other was taken from a test shaft. The samples were quite similar except that the pit sample analyzed 0.35 pct Cu and 0.11 pct Ni and the shaft sample analyzed 0.69 pct Cu and 0.14 pct Ni. Flotation responses were studied in both laboratory and pilot plant tests. Pilot plant flotation responses were similar for both samples resulting in grades of 12.2 pct Cu and 2.5 pct Ni for the pit sample and 12.2 pct Cu and 2.1 pct Ni for the shaft sample. Weight recoveries were 2.5 pct for the pit sample and 5.2 pct for the shaft sample. Copper and nickel recoveries for the pit sample were 87 and 62 pct, respectively, and 92 and 73 pct for the shaft sample. Both concentrates contained small but significant values of cobalt and precious metals. Cobalt recoveries were low--less than 40 pct for both concentrates. Precious metals contents of the concentrates were 1.59 oz/ton for the pit sample and 0.99 oz/ton for the shaft sample. Silver was the predominant precious metal by weight, but platinum and palladium represented the highest values.

Jan 1, 1980

By K. R. Farley

A simplified method for the atomic absorption determination of antimony is described. Samples are dissolved in hydrobromic acid and diluted to volume with water. Solutions can be ready for analysis in about 10 minutes and are stable for at least 24 hours. The spectral line at 231 nanometers is used, and there is no effect on absorption resulting .from the presence of any concentration of HBr. Absorbance is linear with antimony concentrations up to 120 micrograms per milliliter. Sensitivity is 1.48 micrograms per milliliter per 0.0044 absorbance. Relative errors on National Bureau of Standards Standard Reference Materials were 3 percent or less, and relative standard deviations on 12 determinations of each of three flue dust samples were 4 percent or less (95-percent confidence limit).

Jan 1, 1980

By R. H. Nafziger

The Bureau of Mines evaluated 18 domestic titaniferous materials with widely varying compositions, mineralogy, and physical properties in electric-arc furnaces, Techniques were devised to recover both the titanium and iron values contained in these materials so that the reliance of the United States on foreign sources of higher grade ilmenites and rutile might be decreased. Most of the tested titaniferous materials responded well to lower grade or byproduct reductants, such as bituminous coals, charcoal, and coke breeze. Sufficient slag fluidity was realized by maintaining from 8 to 12 wt-pct iron in the slags; no contaminating fluidizers were required. Fluid slags containing up to 79, 70, and 54 wt-pct Ti02 were realized from east coast ilmenites, a rock ilmenite, and a titaniferous magnetite ore, respectively. A carbon-lined furnace shell is recommended for minimum slag contamination. Good results also were obtained during extended submerged-arc furnace tests.

Jan 1, 1980

By Steven J. Page

Responding to the increasing concern for dust control in metal and nonmetal mining, the Bureau of Mines investigated typical dust reduction efficiencies of wet bar cutter machines as they are presently being used in salt mines. Wet bar techniques have previously been used in coal mines, achieving dust reduction efficiencies ranging from 11 to 60 pct. Two different wet bar techniques, namely, the front spray and the water trickle, have been studied as they are currently being used in two salt mines. Preliminary results show that the dust reduction efficiencies have a large variation (0 to 66 pct), as is the case for wet bars used in coal. However, whereas wet bars in coal required 3 to 4 gpm water consumption, wet bars in salt obtained similar efficiencies with only 0.1 to 0.4 gpm. The most reliable data obtained during this study show that the front spray system consistently performs at efficiencies between 41 and 66 pct, with an average of 54 pct. The results indicate that, although wet bar cutter techniques in salt mines are a relatively simple and inexpensive means of dust control with a minimum of water consumption, further investigation should be performed to fully evaluate and optimize wet bar cutter dust reduction efficiencies.

Jan 1, 1980

By Nicholas Kyriazi

It is of interest to know how to obtain as high an absorption efficiency as possible from a CO2-absorption canister used in closed-circuit breathing apparatus. In this study the Bureau of Mines found that varying the bed depth and the cross-sectional area of a canister changes its absorption characteristics. In tests using four ,1 rectangular, variable-depth canisters with different cross-sectional areas, the Bureau found that, given a constant weight of the chemical absorbent, LiOH, and a constant COa input, the canisters with a greater cross-sectional area reached C02 levels of 0.5 volume-percent in the effluent gas sooner than did the canisters with a greater bed depth. However, resistance to flow through the canister increases with bed depth, and a trade-off is inevitable. It was anticipated that the efficiency of a canister would increase with increasing intergranular air space approaching the tidal volume of the breathing waveform and then level off at some point under 100 percent. This postulation was partially substantiated. Cylindrical and radial canisters were also tested and compared. It appears that shape is not as important a factor in absorption efficiency as bed depth, since neither canister differed significantly from the rectangular canisters with regard to absorption efficiency values.

Jan 1, 1980

By J. E. Pahlman

As part of its effort to reduce the need for strategic minerals through conservation and to reduce the capital and energy requirements of mineral processing, the Bureau of Mines has investigated a method for preparing ferrochromium alloys containing less than 2 percent carbon. This method will conserve chromium and should reduce the capital and energy requirements for chromite reduction. Reduced products containing less than 2 wt-pct C and as low as 0.01 wt-pct C were obtained by reacting pellets of chromite and carbonaceous reductant mixtures at pressures of 0.1 to 1 torr and temperatures of 1,230° to 1,320° C. The extent of reduction increased with increased temperature and decreased pressure; however, operating conditions were limited due to the onset of significant chromium vaporization at higher temperatures and lower pressures. Foundry coke, anthracite, and carbon black were found to be supe¬rior to graphite as reductants. The reduction of chromite to metallics was found to proceed via the carbide intermediates (Fe,Cr)7C3 and (Fe,Cr)23C6, No evidence of carbide intermediates Fe3C or Cr3C2 was found. Buttons of ferrochrome alloys were made by melting a mixture of reduced products with CaO and Si02 at 1,700° C for 20 minutes in an induction furnace,

Jan 1, 1980

By W. P. Diamond, J. R. Levine

The explosion hazard of methane-air mixtures has become an increasingly serious mine planning problem, and an advance assessment of methane gas potential can therefore be essential for a safe and economic mine development pro- gram. As part of its coal mine health and safety program, the Bureau of Mines has developed a simple, inexpensive test to measure the methane content of coal samples obtained from exploration cores. The gas content of coal per unit weight as determined by the direct method test can be used as a basis for a preliminary estimate of mine ventilation requirements, and to determine if degasification of the coalbed in advance of mining should be considered. Since the Bureau began measuring the gas content of coal samples in 1972, experience has led to equipment and procedural changes, the most significant of which has been the development of a ball mill for crushing the coal sample to release the residual gas at the end of the desorption test period. This revised procedure replaces the crushing box and graphical methods described in earlier Bureau publications. The results of 583 direct method tests are summarized in tabular form. These results include data on the gas content of 125 coalbeds in 15 States.

Jan 1, 1980

By W. P. Diamond

The explosion hazard of methane-air mixtures has become an increasingly serious mine planning problem, and an advance assessment of methane gas potential can therefore be essential for a safe and economic mine development program. As part of its coal mine health and safety program, the Bureau of Mines has developed a simple, inexpensive test to measure the methane content of coal samples obtained from exploration cores. The gas content of coal per unit weight as determined by the direct method test can be used as a basis for a preliminary estimate of mine ventilation requirements, and to determine if degasification of the coalbed in advance of mining should be considered. Since the Bureau began measuring the gas content of coal samples in 1972, experience has led to equipment and procedural changes, the most significant of which has been the development of a ball mill for crushing the coal sample to release the residual gas at the end of the desorption test period. This revised procedure replaces the crushing box and graphical methods described in earlier Bureau publications. The results of 583 direct method tests are summarized in tabular form. These results include data on the gas content of 125 coalbeds in 15 States.

Jan 1, 1980

By Philip Thompson

The Bureau of Mines investigated a selective flocculation-flotation technique to remove insoluble slimes from low-grade potash ore in a continous 45-kilogram-per-hour (100-pound-per-hour) process investigation unit (PIU). This research is part of the Bureau's program to improve resource recovery from low-grade ores. Results showed that 84 percent of the insoluble slimes were removed from an ore containing 5.5 percent water-insolubles and 14 percent K20 using a Bureau-developed, cationic flocculant-glycol ester-diesel oil reagent. Subsequent potash flotation recovered 75 percent of the potash in a cleaner concentrate assaying 56 percent K20. Concentrate leaching upgraded the product to market specifications of 60 percent K2O. An economic evaluation by the Bureau suggested that the rate of return on investment, after taxes, should be about 20 percent for such an enterprise.

Jan 1, 1980

By Theodore Christos

The Bureau of Mines sponsored an investigation of the thermal oxidative degradation characteristics of certain solvents and hydraulic fluids used in underground mining operations. The following halogenated solvents were studied in view of their usefulness and their flame retardant property: tetrachloroethylene, C12C = CC12; 1, 1, 2-trichloroethane, CIH2CCHC12: and trichloroethylene, C12C = CHC1. The hydraulic fluids studied were representative of five groups approved by the Mine Safety and Health Administration for underground operation, namely: glycol-water solutions, mineral oil-water emulsions, synthetics other than phosphate esters, synthetic phosphate esters, and mixtures of phosphate esters with mineral oils and other ingredients. It was observed that the partially halogenated solvents present a greater potential toxic hazard than the fully halogenated materials, due not only to the easy production of hydrogen chloride but also to their ease of oxidation leading to the formation of phosgene and carbon monoxide. The pure phosphate esters exhibited the best thermal oxidative stability of the five groups of hydraulic fluids tested. A fluid containing phosphate esters mixed with mineral oils and other unidentified ingredients appeared to be the most hazardous On the basis that it produced very toxic acrolein and phosphine.

Jan 1, 1980

By S. E. Khalafalla

In support of its goal to maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines has investigated a novel hydrometallurgical system with sulfur dioxide. Differential leaching with dissolved SO2 of manganese, nickel, and cobalt from their hydrous oxides was found to be very rapid and efficient--almost instantaneous and quantitative. In this method a given weight of mixed oxides previously ground to minus 200-mesh is slurried with a leach solution containing a specified quantity of dissolved SO2 for 10 minutes at room temperature and ambient pressure. An empirical leaching parameter, R, is defined as the ratio of the number of SO2 moles in the leaching solution to the weight of the metal oxide charge. Plots of the variation of metal extraction with the ratio R generate a series of sigmoidal-shaped curves, each of which is characteristic of a specific metal extraction. A threshold value of R is required to initiate the leaching of a given metal from the mixed oxides. Once this threshold is reached, the metal recovery can increase to more than 95 pct in very short times. For increasing values of R, the extractability of various metals by SO2 follows the order: Mn > Ni > Co >> Fe, Al, Cu. Differences in the threshold R values permit a variety of metal separations to be made simply by adjusting the quantity of SO2 in the contacting solution. Success in this leaching system depends upon comminuting the sea nodules to less than 0.149 mm (100-mesh). Above this critical size, leaching is slowed due to the inaccessibility of inner particle reacting groups to the SO2 leaching agent. This results in nonselective extraction and less extraction of preferred metal values. At or below 0.149 mm, leaching by SO, is possible with all its attributes of selectivity, sensitivity, and rapidity. Leaching with HC1 solutions of the same pH level as dissolved SO2 yielded mixed, slow, and incomplete metal extractions. This observation rules out any interpretation based on hydrogen ion as the leaching agent. The leaching curves resemble the complexometric titration curves of heavy metals with specific coordination species.

Jan 1, 1981

A preliminary study was conducted by the Bureau of Mines to determine the effect of humidity on salt mine airborne dust levels. Results showed less dust where the humidity was elevated. Dust reductions appeared to be dependent on the equilibrium between humidity and salt.

Jan 1, 1980

The Bureau of Mines conducted large-scale laboratory copper ore leaching tests to enable improving copper recovery from large dump-leaching operations. This was done by comparing leaching progress when copper was recovered from recycled leach liquor either by cementation or by solvent extraction. Copper was leached from 7-ton ore samples at room temperature using pH 2 ferric sulfate solutions. With are samples containing 11 percent minus 0.5-inch fines, no marked advantage in using either of the copper recovery methods was evident after 416 days of leaching. With ore containing 32 percent minus 0.5-inch fines, solvent extraction of copper was advantageous in that 60 percent of the copper was extracted after 568 days, whereas only 48 percent of the copper was extracted when cementation was used. Less acid was consumed during leaching when solvent extraction, rather than cementation, was used for copper recovery. Iron, contributed by cementation with scrap iron, plugged the ore bed containing 32 percent fines.

Jan 1, 1981

By M. J. Sapko

A moderately scaled apparatus was developed by the Bureau of Mines to determine the fire resistance characteristics of mine conveyor belts and similar type materials. The design of the apparatus was based upon data obtained in full-scale fire tests and features a radiant panel to preheat the belt and a methane-oxygen ribbon burner to ignite the sample under ventilating condi¬tions in a rectangular duct. The test method overcomes the limitations of existing laboratory-scale methods and provides a measure of both ignitability and flammability in quantitative terms. Flame propagation depended upon such variables as air velocity, ignitor heat flux, and belt width and height in the test chamber. Data are presented for nine belt materials and fire resistance ratings are proposed in terms of the flame spread rate, heat release rate, and the critical ignitor heat flux. The ratings discriminate between the fire hazard posed by different fire-resistant belts and tend to be in reasonable agreement with those obtained in full-scale fire tests.

Jan 1, 1981

By L. A. Haas

The Bureau of Mines conducted bench-scale leaching tests with recycled spent copper electrolytes and copper-nickel mattes produced from the Minnesota Duluth Complex concentrates. This report describes the first stage of an overall two-stage leach operation. The objective of this research was to determine the matte-leach technology required to convert spent copper electrolyte into an enriched nickel liquor suitable for a nickel refinery and there-fore essentially free of copper, iron, and sulfuric acid. The experimental variables investigated were matte composition, particle size, spent electrolyte content, pulp concentration, oxygenation, temperature, and time. The time required to produce an enriched purified nickel liquor decreased with increasing pulp concentration, temperature, and oxygenation, but increased with increasing particle size and electrolyte copper and acid content. Nickel-rich (about 50 g/l) liquors at a pH of about 4 and containing less than 1 g/l of copper and iron were produced at 70° C by leaching minus 325-mesh low-iron (less than 5 pct) matte for 8 hours with spent electrolyte containing 22.4 g/l Cu, 28.9 g/l Ni, less than 0.1 g/l Fe, and 50 g/l H2S04 at a pulp concentration of 1 kg of matte per liter of spent electrolyteo Varying the nickel content of the spent electrolyte from 11 to 101 g/l appeared to have no appreciable influence on the matte leaching characteristics.

Jan 1, 1981

By C. F. Davidson

The Bureau of Mines studied the extraction of lithium from lithium-containing clays by chlorination with hydrogen chloride (HC1). In bench-scale laboratory investigations, HC1-H20 mixtures were used to selectively chlorinate lithium, but not calcium or magnesium, in lithium-containing clays. The addition of calcium carbonate to the clay was found to improve the lithium recovery. Reaction conditions found to affect the lithium recovery were ratio of clay to carbonate, reaction temperature, and HC1 concentration. The best conditions for selective chlorination of the lithium were 2:1 clay-carbonate, 750° C, and 20 wt-pct HC1. The experimental results and trends in lithium extraction are explained using thermodynamic relationships.

Jan 1, 1981

By S. D. Hill

To help insure the continued viability of the minerals and materials sector of the U.S. economy, the Bureau of Mines is conducting research and disseminating technology that will result in more efficient minerals extraction. As part of this effort, a process is being investigated that involves an aqueous chlorine-oxygen leaching procedure to treat complex sulfide concentrates to produce ZnCl2. Subsequent fused-salt electrolysis of the ZnCI2 produces high-purity zinc metal. Previous reports described preliminary, small-scale research on the chlorine-oxygen leaching system and fused-salt electrolysis of ZnCl2. This report discusses the details of design, construction, and longterm, continuous operation of both monopolar and bipolar fused-salt cells. The effects of temperature, electrode gap, current density, electrolyte composition, and electrode configuration on current efficiency and energy consumption were determined for a ZnCl2-KC1-NaCl electrolyte system. Zinc metal was produced at the rate of about 50 lb/day in a monopolar cell which was operated continuously for 60 days with current efficiencies from 85.8 to 98.6 pct and an average power consumption of 2.1 kwhr/lb. Bipolar cells with several different electrode configurations were operated for 90 days. A current efficiency of about 70 pct and power consumption of about 1.7 kwhr/lb of zinc were achieved using a three-electrode-pair, bipolar assembly with a chlorine gas lift pump to circulate electrolyte.

Jan 1, 1981

By Joseph E. Matta, John C. LaScola, Fred N. Kissell

The Bureau of Mines investigated coal storage silos to determine how gassy coal must be for methane accumulations in a silo to become hazardous and where such accumulations are likely to occur. Methane concentrations were measured in the open space above the stored coal pile, in the pile, and in the reclaiming area. No methane layering was found in closed-top silos. Reclaiming areas were as gassy as the top part of the silos. Coal samples were collected from the conveyors entering the silos in order to assess the gassiness of the coal. No simple correlation was found between the gassiness of the coal stored and the measured methane concentrations. However, at mines where the average 24-hour gas emission from the conveyor belt samples was 14 ft3/ton or more, fans or open tops were used. It appears that a large fraction of the methane released during storage remains in the void space between the coal particles.

Jan 1, 1981

By M. J. Ferrante

High-temperature enthalpy and X-ray powder diffraction studies were con-ducted on aluminum sulfide (Al2S3) as part of the Bureau of Mines effort to provide new data for the advancement of mineral technology consistent with environmental preservation and energy conservation. Relative enthalpies were measured with a copper-block calorimeter from 298.15 to 879 K. Tabulated values are listed for heat capacity, entropy, Gibbs energy functions, and relative enthalpies between 298.15 and 900 K. Enthalpies were also given in the form of an equation and combined with published data to calculate standard enthalpies of formation and Gibbs energies of formation for reactions of crystalline aluminum with crystalline, liquid, and gaseous diatomic sulfur. The hexagonal, rhombohedral, and cubic phases of Al2S3 were identified by X-ray powder diffraction studies, and the indexed powder diffraction patterns of these phases are given. The hexagonal phase was stable to about 852 K and was partially converted to the rhombohedral form at 879 K.

Jan 1, 1981

By Robert P. Vinson

This Bureau of Mines report presents the results of tracer gas studies conducted at three facilities where bagger hoods had been installed several years ago to remove airborne silica dust from the vicinity of the bagging operator. The studies indicated that for optimum benefits makeup air must be evenly dispersed, the hood enclosures and duct systems must be as airtight as possible, the average intake air velocity of each hood should be at least 200 fpm, and the hoods and duct systems must be properly maintained.

Jan 1, 1981