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By Robert W. Freedman

As part of a continuing effort to reduce the weight and bulk of equipment that mining personnel must carry underground, the Bureau of Mines and the Mining Enforcement and Safety Administration (MESA) investigated accurate and convenient gas samplers for use by mine inspectors in sampling mine atmospheres. The samplers are septum-stoppered glass vials commonly used for routine blood sampling. These lightweight, compact samplers yield results comparable with those obtained with conventional bottle samplers of 250-ml nominal capacity.

Jan 1, 1975

By M. E. Poad

Structural properties of steel-fiber-reinforced shotcrete and polymer-impregnated shotcrete, both plain and fiber-reinforced, were investigated by the Federal Bureau of Mines, Spokane Mining Research Center. The research center has found that flexural strengths can be increased by as much as 106 percent, and splitting-tensile strength by 50 percent, by introducing randomly oriented steel fibers. A slight decrease of compressive strength was found in the fiber-reinforced shotcrete. Polymer-impregnated shotcrete exhibited a threefold to fourfold increase in compressive and splitting-tensile strength. The techniques of preparing shotcrete with the dry process, using both fast-set agents and regulated-set cement, are described, along with the results of physical-property testing. Physical properties include compressive and splitting-tensile strengths, tangent and secant moduli, and stress-strain curves for plain shotcrete, fiber-reinforced shotcrete, and polymer-impregnated plain and fiber-reinforced shotcrete. Flexural strengths for plain and fiber-reinforced shotcrete are also reported. Steel-fiber shotcrete is the more promising of the new structural materials for ground support, and additional research is recommended.

Jan 1, 1975

By A. Landsberg

Chlorination of sulfide minerals and several prepared metal sulfides was studied. The resulting data were analyzed with respect to kinetics of the reactions and application to nonpolluting methods of winning metals from sulfide ores. Sulfides of iron, copper-iron, nickel, lead, zinc, silver, bismuth, arsenic, rhenium, molybdenum, and tungsten were investigated at temperatures up to 600° C. Copper-iron, lead, and zinc sulfides showed at least some product-controlled (parabolic) kinetics at the lower temperatures within the temperature ranges studied, but only nickel and silver sulfides had chlorination rates controlled by parabolic reaction kinetics in the commercially important temperature range of 450° to 600° C.

Jan 1, 1975

By J. E. Tress

The Bureau of Mines has developed a process to utilize waste heat from electric arc steelmaking furnace gases to preheat the ferrous material charged to the furnace. Four heat exchangers were designed, tested, and operated successfully on 1-ton electric arc furnaces. Briquets and pellets were charged continuously, both countercurrent to the hot furnace offgasses and at ambient temperatures. A comparison of the electrical energy consumed in each situation showed that preheating can lower energy requirements as much as 15.6 percent.

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 M. C. Irani

The Bureau of Mines, in cooperation with the Mine Safety Appliances Co., has developed a new methane analyzer system for underground applications. Methane enters coal mine ventilation air from the breakup of coal at the active face, from the collapse of roof rock during retreat mining, and from the ribs abutting virgin coal. Each source contributes varying amounts to the total emission, depending upon rate of mining, type of mining, and the character of the coalbed and adjacent strata. The evaluation of individual parameters of methane emission requires the continuous monitoring of individual mine sections over a long period of time. The methane analyzer system was developed to meet this need. The system has been installed and operated in an active mine in the Pittsburgh coalbed. The system and details of its installation and calibration are described. Data are presented to substantiate its reliability.

Jan 1, 1975

By H. B. Carroll

The performance of commercially available portable instrumentation for detecting nitrogen dioxide, sulfur dioxide, and hydrogen sulfide was evaluated. Length-of-stain detector tubes from several manufacturers were included in the study. The instruments were evaluated in atmospheres with 50-and 80-percent relative humidities at 75° F and containing test gas concentrations of 0.1, 0.25, 0.50, 1.0, 1.5, and 2.0 times the threshold limit values. The results from the gas analyzers were correlated with the known contaminant concentration by calculating and plotting an estimated line of regression, confidence limits, and correlation coefficient for each detector system. An increase in the relative humidity from 50 to 80 percent at /5° F changed the instrument response to the contaminants. The uncertainties in detection precision reported are for the observer-instrument system. The main difference or inconsistency in toxic gas concentrations determined with length-of-stain tubes resulted from the observer's interpretation of the results rather than from a predominant difference in the tubes.

Jan 1, 1975

By Lawrence K. Barker

Crude shale oil produced by underground retorting of Green River Formation oil shale was hydrogasified over a cobalt-molybdate-on-alumina catalyst at operating temperatures ranging from 800° to 1,300° F, pressures of 500, 1,000, and 1,500 psig, and a liquid hourly space velocity of 1.02 volumes of oil per volume of catalyst per hour (Vo/Vc/hr). At a temperature of 1,300° F and pressure of 1,500 psig, 94 weight-percent of the liquid feed was converted to gas containing 72 volume-percent methane. With two reactors in series at a temperature of 1,170° F in reactor 1 and 1,260° F in reactor 2 and a pressure of 1,500 psig, 97 weight-percent of the liquid feed was converted to gas with a methane content of 75 volume-percent. Liquefied petroleum gas (LPG) was hydrogasified at operating temperatures ranging from 500° to 1,400° F at a pressure of 500 psig over a cobalt-molybdate-on-alumina catalyst. Similar experiments were made with an empty tubular reactor. The data indicate that gasification reactions in the presence of a cobalt-molybdate catalyst change from predominantly a catalytic (carbonium ion) reaction to predominantly a thermal (free radical) reaction at temperatures greater than 1,100° F. The data also indicate that a reaction temperature of 1,350° F is necessary at the space velocities used in this investigation to make a synthetic natural gas (methane content of 90 volume-percent) from in situ crude shale oil.

Jan 1, 1975

By B. W. Madsen

Research by the Bureau of Mines has shown that treatment of open pit waste by crushing and sizing followed by flotation of the fines and leaching the coarse fraction results in greater metal recoveries than obtained by leaching only. Tests with a chalcocite-bearing quartz monzonite mine waste sample that had been crushed to minus 6 inches and screened on 1/2 inch yielded copper and silver recoveries of 71 and 22 percent, respectively, by the combined flotation-leaching process, compared with 48 percent of the copper and no silver recovered leaching the run-of-mine material. Copper was more readily leached from the coarse material with the minus 1/2-inch fines removed than from material with the fines included. The improved leaching was attributed to improved permeability and the associated improved circulation of air to the interior of the ore column. Cost estimates showed that the proposed intensive treatment of mine waste will require a greater capital investment and higher annual operating costs than conventional milling and dump leaching process. However, the income from the additional metal production offsets the increase in capital investment and operating costs, resulting in additional profit.

Jan 1, 1975

By H. R. Appell

The Bureau of Mines studied the conversion of a variety of cellulosic wastes, for example, sawdust, bovine manure, sewage sludge, urban refuse (free of metal and ceramics), etc., to heavy oils. The objective of the investigation was to determine the scope of the reaction and elucidate the chemistry involved. The reactions took place in the presence of synthesis gas and water or carbon monoxide and water under conditions of elevated temperatures and pressures. Waste conversions above 90 pct, often near 99 pct, with oil yields in the range of 40 to 60 pct, were obtained in the temperature range of 250° to 425° C and pressure range of 1,500 to 4,000 psig. Because mild conditions were sought, most of the experiments were conducted at temperatures of 250° to 350° C and pressures of 1,500 to 3,000 psig. In general, lower viscosity products were obtained at higher reaction temperatures. Conversions and oil yields were significantly increased by operating in the presence of a high-boiling oil; either anthracene oil or oil recycled from the process was satisfactory. Synthesis gas containing 50 pct carbon monoxide gave satisfactory results as a replacement for carbon monoxide. Cobalt molybdate on alumina catalyst, used with sodium carbonate, gave a product of lower viscosity and lower oxygen content than sodium carbonate used as the sole catalyst. The waste-to-oil process has been successfully investigated in continuous flow equipment as well as in batch autoclaves.

Jan 1, 1975

By Peter D. Lohn

The Bureau of Mines conducted both laboratory and field investigations to study the effectiveness of medium-pressure (up to 30,000 psi) water jets in controlling the generation of airborne respirable dust during the hydraulic fragmentation of coal. Laboratory studies were conducted at the Farmington High Energy Test Site of the Twin Cities Mining Research Center, and field studies were carried out at the Humphrey No. 7 mine, Mount Morris, Pa., in the Pittsburgh coalbed. The water jets were produced by commercially available triplex pumps. The dust samples were collected by midget impinger samplers, and analyzed by electronic and optical counting techniques. Respirable dust concentration for a full-scale production model was projected at below 2 mg/m3, the maximum exposure allowed by the Federal Coal Mine Health and Safety Act of 1969.

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 W. E. Robinson

Differences in the composition or chemical structure of the organic material in samples of Uinta Basin (Utah) oil shale were studied relative to stratigraphic position within the Green River Formation. This involved a systematic study of the soluble organic material and the insoluble organic material (kerogen) present in the samples. Emphasis was placed upon the distribution of the alkanes (normal and isoprenoid compounds) in the soluble extracts and upon the aromaticity of the kerogen. Significant differences exist in the chemical composition of the organic material from various strata within the Uinta Basin, some of which were related to burial depth but most were related to source material variations, environmental differences, or other factors. The Uinta Basin samples differed significantly from Piceance Creek Basin and Green River Basin samples in the large amount of soluble extract they contained.

Jan 1, 1975

By Patrick J. Cain

The fatigue-failure characteristics under high-frequency (10 KHz) cyclic loading were determined for a marble, granite, and quartzite. The rock speci-mens were cyclicly loaded (using a high-power piezoelectric sonic transducer) at a constant strain amplitude generated by forming a longitudinal standing stress (strain) wave in the cylindrical test specimen. The number of load cycles required to fail each rock type at a given strain amplitude was deter-mined. The fatigue fractures were tensile in nature and the fracture load amplitudes were as low as 30 pct of the static tensile strength. Also the internal heating of the rock caused by the material damping (internal friction) was measured. The damping and internal heat generation in the specimens was analyzed to show that nearly all of the power input can be accounted for as a change in enthalpy in the specimen. Using these results the thermal strain in the rock was calculated to evaluate its contribution to fatigue failure. The thermal strain was found to range up to 30 pct of the dynamic strain amplitude depending on the load amplitude and the number of load cycles. The specific energy required for failure was determined and possible applications of the high-frequency fatigue fragmentation process are discussed.

Jan 1, 1975

By P. R. Tisot

The structural response of propped oil shale fractures was determined for each of two different grades of Green River oil shales (38.0 and 29.0 gpt) as they were heated in an inert atmosphere from ambient to subretorting temperatures (below those required for rapid pyrolysis of the organic matter). Small oil shale cores were propped apart by 3-mm glass beads to simulate a small cross section of a propped oil shale fracture between an injection and a producing well. These specimens were then heated at a uniform bate up to 800° F in a specially designed test cell under stress levels from 100 to 1,000 psi in biaxial and in triaxial confinement. Under the conditions of heat and compressive stress utilized in this study, all of the propped fractures in the two oil shales underwent structural deformation ranging from partial to complete collapse, as evidenced by proppant embedment. Structural collapse of induced fractures would in turn result in serious impairment or complete loss of the fracture flow capacities of the specimens. Results from this Bureau of Mines study indicate that underground retorting of Green River oil shale may be seriously impaired by loss of permeability when utilizing propped fractures in oil shales assaying more than 28 gpt.

Jan 1, 1975

By C. M. McCulloch

A series of geological surveys were completed in six coal mines in connection with a Bureau of Mines research program on methane control. The aim of these surveys was twofold: First, to study the overall geology of the coalbed, and second to use the resulting data to evaluate the influence of the geological characteristics of the coalbed on safe and efficient coal extraction. This report explains the advantages of geologic maps and fence diagrams in coal mining, and how the knowledge gained from such geologic investigations of mines can help control many underground problems.

Jan 1, 1975

By B. Dimitriades

The Bureau of Mines measured the reactivities of 19 hydrocarbons known to be prominently present in automotive exhaust and ambient air in a smog chamber. Results agreed well with those obtained using two other smog chambers. Reactivity scales were developed for hydrocarbons and aldehydes using the results of this work and those of a previous study. Application of the reactivity scales to automotive exhaust samples gave fair agreement between predicted and observed rate-of-N02-formation values; however, predicted and observed ozone yields were neither in agreement nor did they correlate well. This lack of correlation for ozone yield was attributed to the inappropriateness of (1) the individual component reactivity data, (2) the reactivity classification scheme used, and (3) the linear summation method. In seeking to understand this problem and to develop more appropriate reactivity scales, the data were examined from a reaction mechanism standpoint, and further studies were suggested.

Jan 1, 1975

By C. A. Wilson

The Bureau of Mines started a continuing program to investigate and evaluate analytical techniques to assist governmental agencies to select simple, rapid, reliable methods for crude oil spill identification. Six crude oil samples were analyzed to evaluate gas-liquid chromatography, atomic absorption spectrophotometry, infrared spectoscopy, sulfur and nitrogren determinations, mass spectrometry, nuclear magnetic resonance spectroscopy, and ultraviolet spectrophotometry. Samples were studied from the following selected fields: El Morgan, Egypt; Duri, Indonesia; Minagish, Kuwait; Bachaquero, Venezuela; Gach Saran, Iran; and Prudhoe Bay, Alaska. These samples were chosen to represent high-production fields that are likely to be involved in oceanic transport. Over 50 years of Bureau of Mines analytical research on petroleum served as the basis for evaluation of the experimental results to determine which of the methods are effective techniques to identify crude oil spills. Gas-liquid chromatographic analysis, atomic absorption spectrophotometric analysis, and sulfur-nitrogen determinations are recommended as the most useful of the techniques investigated.

Jan 1, 1975