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By J. B. Janus

This report continues a series of analyses of coal samples made by the Bureau of Mines in connection with the yearly purchase of several million tons of coal for various Government agencies. Listed are the analytical data on the composition and quality of tipple and de livered samples of coal collected during fiscal year 1974.

Jan 1, 1975

By D. H. Desy

The Bureau of Mines has conducted research on the ignition of methane-air mixtures by sparks caused by frictional impact of aluminum alloys on rusted steel at typical coal mine fan speeds. The objectives were to establish the incendivity of aluminum alloys under these conditions, to investigate differences between aluminum alloys, and to evaluate substitute materials for the aluminum-steel combination. With a specially designed apparatus, three commercial aluminum casting alloys and a number of experimental aluminum alloys were tested for incendivity of the frictional impact against rusted steel in flammable methane-air mixtures. All aluminum alloys tested produced some ignitions. Of the experimental alloys, the harder alloys and those containing silicon tended to be more incendive than the others. With the normal experimental conditions, constructional steel, stainless steel, brass, and plastic did not cause ignition of methane-air mixtures in frictional impact against rusted steel. Some ignitions occurred with constructional steel at high speed in more flammable gas mixtures enriched with oxygen. From these findings, it is suggested that constructional material combinations other than the aluminum-steel combustion would minimize this inc endive hazard. A detailed description is given of previous research, and comparison is made with present results where appropriate.

Jan 1, 1975

By F. P. Haver

Because State and Federal agencies have limited the amount of sulfur oxides that can be discharged to the atmosphere, most copper smelters plan to convert the S02 in offgases to sulfuric acid. In some cases, however, it might be preferable to use a nonsmelting method to fix the sulfur in the form of a discardable product. Research by the Federal Bureau of Mines has shown that sulfur in copper concentrate can be converted into insoluble anhydrite (CaS04) by roasting the concentrate with lime (CaO). After leaching the calcine to recover metal values, the residue may be discarded without harm to the environment. The process can use a rougher flotation product, thus reducing separation costs and saving valuable minerals (for example, molybdenite) that are now lost in making cleaner concentrate. In tests, rougher concentrate was pelletized with the theoretical amount of lime and roasted for 1 hour in a 6-1/2-inch-ID by 11-foot-long rotary kiln at 700° C. Sulfur retention was about 97 percent. Leaching the calcine with 20 percent RCI extracted approximately 99 percent of the copper, 73 percent of the iron, and 91 percent of the molybdenum. After the molybdenum was removed from the leach solution by adsorption on activated carbon, copper with a purity in excess of 99 percent was obtained by cementation on sponge iron. The strip solution then could be spray-roasted at 500° C to recover the RCI for recycle and obtain F2O3 as a byproduct.

Jan 1, 1975

By F. P. Haver

A method to recover copper and elemental sulfur from chalcopyrite concen¬trate, using a ferric chloride leach, CuFeS2 + 3FeCl3 ? CuCl + 4FeCl2 + 2S, was reported by the Federal Bureau of Mines in 1971 (Report of Investigations 7474). Since that time, additional work has been done to improve certain steps in the procedure; that is, the recovery of sulfur from the leach residue, the recovery of copper and iron from the leach solution, and the regeneration of the leach solution. It was determined that over 99 pct of the elemental sulfur in the leach residue could be extracted at ambient temperature with an ammonium sulfide solution. Heating the pregnant solution precipitated crystals of rhombic sulfur (99.5 pct purity) and liberated ammonia and hydrogen sulfide for recycle. Copper with a purity in excess of 99 pct was obtained from the leach solution by electrolysis, using a diaphragm cell, with an energy requirement of less than 0.7 kW-hr/lb. Metal was deposited as a weakly adherent powder that could be easily dislodged from the cathode and withdrawn continuously from the cell in the form of a slurry. During electrolysis, part of the Fe(II) was oxidized to Fe (III) at the anode so there was no chlorine evolution. The leach solution was regenerated by direct oxidation of the spent electrolyte with air or oxygen in a turboaerator at 80° C. This precipitated the iron dissolved during leaching in an easily filterable form, Fe203.xH20, and converted the remaining Fe(II) to Fe(III).

Jan 1, 1975

By Fred N. Kissell

Air recirculation caused by dust scrubbers at coal mine working faces was examined by the Federal Bureau of Mines with regard to the potential hazards caused by a possible buildup of methane gas. A theoretical analysis indicated that there was no apriori way to predict the effect of scrubber recirculation on methane concentration levels. Experiments conducted in a full-scale model of a working face area indicated that methane levels were dependent to a great extent on the location of the scrubber exhaust, but that the scrubber recirculation did not substantially increase the methane concentration above those levels that would have prevailed were the scrubber not in operation. An analysis of two underground scrubber trials showed that the scrubbers had no significant effect on methane levels, and a review of explosions attributed to recirculation showed that these were characterized by a lack of fresh air as well as recirculation. It was concluded that high methane levels are due more to a lack of fresh air than to recirculation.

Jan 1, 1975

By R. E. Siemens

A process is being developed by the Bureau of Mines to selectively recover nickel and cobalt from low-grade domestic laterites. In laboratory evaluation of the process, the oxides in the laterite were selectively reduced with carbon monoxide at temperatures from 350° to 600° C. For material containing more than about 5 percent magnesia, pyrite additions or post-reduction heat treatments were necessary to achieve satisfactory nickel and cobalt extraction for this range of reduction temperatures. Multistage leaching of the reduced material at ambient temperature and pressure in the presence of oxygen, ammonium sulfate, and ammonium hydroxide extracted up to about 90 and 85 percent of the contained nickel and cobalt, respectively. The nickel was selectively recovered from the leach solution by solvent extraction and was then stripped from the loaded organic with dilute sulfuric acid to provide a nickel-rich electrolyte. Treatment of the raffinate with hydrogen sulfide resulted in the recovery of cobalt as a sulfide. The only contaminant in solution was magnesium which was removed by ion exchange or precipitation. In this process the energy requirements are relatively low and except for minor operation losses, only coke and oxygen are consumed.

Jan 1, 1975

By G. L. Gates

The waters used to waterflood the Wilmington oilfield were studied by the Bureau of Mines, in cooperation with the city of Long Beach, Calif. Increases in the pressure of the injection wells indicated that they were being plugged by materials suspended in the waters. This study was made to identify the suspended materials, determine their origin, and find methods of preventing their formation. The suspended oil-coated materials were iron sulfide, barium sulfate, calcium carbonate, clay, and sand (or silica). Results indicated that the sulfide, which was as high as 90 milligrams per liter, was the product of sulfate-reducing bacteria. The injection of ocean water increased the sulfate content of the waters in the petroleum reservoirs from 3 to 250 milligrams per liter, thereby furnishing sulfate for growth of the bacteria. The waters were supersaturated with barium sulfate. Laboratory tests showed that sulfide could be removed from the waters by adding iron at a cost of 1 to 2 mills per barrel. The solubility of iron sulfide and calcium orthophosphate in the injection waters was also determined.

Jan 1, 1975

By C. M. McCulloch

The methane content of virgin bituminous coalbed can now be measured accurately in the field with exploration core samples from vertical boreholes. The gas content of the coal per unit weight can be used either to design a mine ventilation system or to determine if degasification of the coalbed will be necessary before mining, and to determine the gas resources in the coalbed. The equipment necessary to conduct the test costs less than $50. The gas con-tent of the coal in place in the ground is determined by summing the gas lost from coring, gas measured during desorption, and the residual gas in the coal. Upon removal from the borehole, the core sample is placed in an airtight container and des orbed for several weeks until the desorption rate is below 0.05 cm3/g for 5 consecutive days. The gas lost from the core while it was being cored and the residual gas are estimated by a new graphical method. The amount of gas remaining depends upon whether the coal is friable or blocky. Friability appears to relate to the depth of the sample below the surface, fixed carbon percentage, Hardgrove grindability index, and proximity to tectonic disturbance. Friable coals emit nearly 96 pct of the total gas during desorption whereas a blocky coal emits only 60 pct of its total gas. Coalbeds that are ill defined as to their blocky or friable nature must be tested in the laboratory for unambiguous analysis.

Jan 1, 1975

By J. M. Stuve

Low-temperature heat capacities and the enthalpy of formation were deter-mined calorimetrically by the Bureau of Mines for CuO?CuS04. The derived standard entropy (S°298.15) was 40.36±0.04 cal/deg-mole, and the enthalpy of formation (?H°f) was -219.l±0.3 kcal/g-mole. A large thermal anomaly was observed in the heat capacity of CuO?CuS04 at 20±0.1 K. Gibbs energy of formation data are tabulated up to 1,200 K. Construction details of a precision low-temperature adiabatic calorimeter capable of determining heat capacities of solids in the temperature range 5 to 320 K are given. A calibrated miniature germanium resistance thermometer was incorporated into the calorimeter to extend the range of accurate measurements below 15 K. High-resistance dc heater windings were used throughout the cryostat to reduce heat conduction of inner connecting wires.

Jan 1, 1975

By Donald I. Kurth

The Bureau of Mines conducted experimental work on comminuting coal. The size distributions of coarse fragments and fine particles were obtained under different modes of energy application--drop, impact crushing, wedge impact, compression, and shear tests. Four levels of energy application were used in the impact crushing and wedge impact tests. Airborne dust and respirable air-borne dust distributions were obtained for the impact crushing and wedge impact tests. Analyses of nonairborne dust and coarse fragment-fine particle distributions were carried out on impact, wedge, compression, and shear tests. The experimental size data on nonairborne dust were fitted to normal, log-normal, power law, Weibull, log-Weibull, and exponential distribution functions. Both the nonairborne dust and the coarse fragment-fine particle size distributions are best described by Weibull distributions. For the impact crushing tests, mean product size was found to be inversely related to specific crushing energy. The particle counts in a given size range of airborne and nonairborne dust were found to increase with increased input energy and specific crushing energy. However, in another sense the particle distributions were independent of energy level; that is, the percent-ages in a given size range were approximately constant regardless of energy level. Respirable airborne dust was related to respirable-size nonairborne dust by a power law.

Jan 1, 1975

By Robert Lee Stahl

Comprehensive field tests were made by the Federal Bureau of Hines at the Conda open pit mine near Soda Springs, Idaho, to determine whether surface geophysical techniques could be used to detect and delineate faults in phosphate deposits. The tests included seismic refraction, magnetometry, electrical resistivity, and airborne photography. Of the several geophysical techniques tested in the field, horizontal resistivity profiling was the most effective method for diagnosing faults. The method is quick, inexpensive, accurate, and can be easily used by mining company personnel to detect and delineate faults.

Jan 1, 1975

By Sathit Tandanand

This Bureau of Mines report describes the method of obtaining a strength index for rock drillability, particularly for percussion drills. The original Protodyakonov method has been slightly modified, essentially to eliminate uncertainties in the measurement of the volume of fines, and to avoid conjecture in selecting the representative value as the strength coefficient. A theoretical consideration of the relevant parameters in the method was extended from a comminution theory, and hence the meaningful value was obtained experimentally by plotting the ratio of the number of drops and the volume of fines against the number of drops. The minimum ratio of the number of drops to the volume of fines in the plot was selected as the coefficient of rock strength. The modified method of obtaining the strength coefficient preserves the original Protodyakonov test apparatus and the merit of simplicity of the test procedure. The modified coefficient of rock strength shows its usefulness in predicting penetration rates with greater reliability than other mechanical properties. Consequently, the drillability curves were drawn using the modified coefficient of rock strength as the parameter for penetration rate prediction in the field.

Jan 1, 1975

By R. A. Guidotti

The Federal Bureau of Mines has studied the reaction of oxides of columbium, vanadium, and tantalum with ammonia in vertical, gas-solids reactors at temperatures ranging from 300° to 1,300° C with the goal of preparing nitride intermediates for subsequent preparation of the metals by a thermal-decomposition step. The best nitride conversions were obtained in nonmetal reactors. With Cb205, V2O3, and V205 , low-temperature maxima in reaction rates occurred at 800°,800°, and 450° C, respectively, during oxynitride formation (in A1203) at 1 atm of pure ammonia. Conversion of the oxynitride, in a second step, to the mononitride was optimum at 1,200° C for columbium and 1,050° C for vanadium. In the case of Ta205, the rate of reaction to form Ta3N5 (in a single step) was highest at 900° C, where the presence of up to 5 percent methane was found to be beneficial; improved results were obtained by conducting the nitriding in a rotary kiln. Optimum space velocities (in the vertical Al203 reactor) ranged from 5,280 hr-1 for Cba205 to 7,950 hr-1 for V203. Oxide particle size had little effect upon reaction rates. Under fully optimized conditions, products containing less than 1 percent oxygen were readily obtained in under 6 hours.

Jan 1, 1975

By T. A. Sullivan

The use of sulfur combined with either sand or waste copper tailings was investigated by the Bureau of Mines as a substitute for a good graded aggregate in asphalt paving materials. The research was part of a utilization program to develop meaningful uses for a projected oversupply of sulfur. Many sections of the country lack good aggregate for paving but do have available sources of sands and sulfur. The development of paving mixtures of desert sands or tailings with sulfur and asphalt was accomplished in the laboratory and tested by laying small paving test sections. Three types of material were studied for use with the sulfur and asphalt. They were (1) a concrete sand similar in gradation to river or beach sands, (2) desert blow sand, and (3) waste copper tailings. Desert blow sand and waste copper tailings are much finer than concrete sand. Mix designs were established for the three types of materials, sulfur, and asphalt used in the paving materials. The best mix designs were as follows, in weight-percent: 80.5 concrete sand, 13.5 sulfur, and 6 asphalt; and 77 either blow sand or tailings, 17 sulfur, and 6 asphalt. Small-scale testing showed that these mixtures were suitable paving materials but would require specialized equipment for transporting and laying. The chemical modification of sulfur to obtain properties that would allow placement of these materials with normal asphalt paving equipment was studied. Results indicate that reacting sulfur with dicyclopentadiene before adding it to the paving mixture was effective in modifying the sand-sulfur-asphalt paving so it could be placed and rolled with conventional equipment.

Jan 1, 1975

By W. E. Lamont

The Federal Bureau of Mines, in cooperation with phosphate companies in the Florida land-pebble area, made a comprehensive study of the waste clays, or "phosphate slimes," produced in the mining of phosphate rock in Florida. These slimes represent a significant ecological problem and a major deterrent to effective land recovery in the phosphate-mining areas. Physical, chemical, and mineralogical studies were made of slime samples submitted by 15 of the 16 plants in Florida in an effort to identify factors that prevent successful consolidation of the slimes and subsequent recovery of the mined lands. Results of these studies indicated that the clay mineral attapulgite, a hydrated magnesium silicate, was primarily responsible for the very poor settling characteristics of the slimes, and that the quantity of attapulgite in the slimes effectively controlled the settling rate, pulp density of terminal solids, viscosity, percent solids of filter cake, and flocculant requirements.

Jan 1, 1975

By W. P. Diamond, B. M. Bench, C. M. McCulloch, Maurice Deul

As part of the Bureau of Mines methane control program, the Pittsburgh coalbed was studied in Washington and Green Counties, Pa., and in Marion and Monongalia Counties, W. Va., where this coalbed is now being mined at its greatest depth. The coalbed thickness appeared to be structurally controlled; the bed was generally thinner near the axes of anticlines and thicker near the axes of synclines. The overburden isopach shows a similar relationship. Most of the clay veins in coal occur in the synclinal troughs, generally under sandstone roof. Cleat orientations measured in 18 underground mines showed that face cleats are perpendicular to the axial trends of the folds, and the butt cleats are parallel to the axial trends, indicating structural control of the cleat. Measurement and analysis of surface joint orientations provide a method for predicting the cleat orientations of the coalbed, but linears measured from infrared photographs and photoindex sheets helped only to determine regional trends. The results of these investigations provide a geologic framework for rational planning for underground mine development to use the best available technology to cope with methane emissions, coalbed discontinuities, and related ground support problems.

Jan 1, 1975

By C. M. McCulloch

As part of the Bureau of Mines methane control program, the Pittsburgh coalbed was studied in Washington and Green Counties, Pa., and in Marion and Monongalia Counties, W. Va., where this coalbed is now being mined at its greatest depth. The coalbed thickness appeared to be structurally controlled; the bed was generally thinner near the axes of anticlines and thicker near the axes of synclines. The overburden isopach shows a similar relationship. Most of the clay veins in coal occur in the synclinal troughs, generally under sandstone roof. Cleat orientations measured in 18 underground mines showed that face cleats are perpendicular to the axial trends of the folds, and the butt cleats are parallel to the axial trends, indicating structural control of the cleat. Measurement and analysis of surface joint orientations provide a method for predicting the cleat orientations of the coalbed, but linears measured from infrared photographs and photoindex sheets helped only to determine regional trends. The results of these investigations provide a geologic framework for rational planning for underground mine development to use the best available technology to cope with methane emissions, coalbed discontinuities, and related ground support problems.

Jan 1, 1975

By H. H. Fields, Joseph Cervik, G. N. Aul

Coal is a soft and brittle material. Drilling rates in the Pittsburgh coalbed using a drag bit exceed 3 ft/min at 2,500-pound thrust. However, maintaining the bit on a horizontal trajectory or parallel to bedding planes to attain lengths of 1,000 feet is difficult. This Bureau of Mines report presents a drill string configuration that can be guided through the coalbed. The angle of the borehole is measured periodically and by proper combinations of bit thrust and rotational speed (r/min), bit trajectory can be lifted or dropped to keep the bit in the coalbed. An example of a hole drilled to 2,126 feet is presented to show levels of thrust and rotational speed used to lift or drop the bit, the seemingly unexplainable events that occur, and the strategy used during drilling. Thrust levels during drilling range from 600 to 2,500 pounds. Hydraulic motors powered by a 30-hp, 440-volt motor provide ample power for drilling horizontal holes 2,000 feet long.

Jan 1, 1975

By Joseph Cervik

Coal is a soft and brittle material. Drilling rates in the Pittsburgh coalbed using a drag bit exceed 3 ft/min at 2,500-pound thrust. However, maintaining the bit on a horizontal trajectory or parallel to bedding planes to attain lengths of 1,000 feet is difficult. This Bureau of Mines report presents a drill string configuration that can be guided through the coalbed. The angle of the borehole is measured periodically and by proper combinations of bit thrust and rotational speed (r/min), bit trajectory can be lifted or dropped to keep the bit in the coalbed. An example of a hole drilled to 2,126 feet is presented to show levels of thrust and rotational speed used to lift or drop the bit, the seemingly unexplainable events that occur, and the strategy used during drilling. Thrust levels during drilling range from 600 to 2,500 pounds. Hydraulic motors powered by a 30-hp, 440-volt motor provide ample power for drilling horizontal holes 2,000 feet long.

Jan 1, 1975

By S. R. Borrowman

Mill tailings from conventional uranium extraction processes contain nearly all of the radium originally in the ore. Such tailings require controlled storage in perpetuity to safeguard the surrounding environment from radioactive contamination. Alternatives to controlled storage of the tailings are (1) removal of the radium from the tailings for separate storage or use or (2) removal of the radium when processing the uranium ore. In laboratory tests conducted by the Federal Bureau of Mines, radium was leached from tailings using either hydrochloric acid or ethylenediamine tetraacetic acid. A hydrochloric acid leaching method was used to extract both radium and uranium from the ore to yield tailings containing less radium than those produced by either conventional sulfuric acid or alkaline leaching processes. From 77 to 94 percent of the radium in mill tailings was concentrated by sedimentation in slime fractions representing nearly 25 weight-percent of the original sample.

Jan 1, 1975