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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 Donald N. H. Chi

This Bureau of Mines report is concerned with a theoretical study of the aerodynamic response of a single mine entry to flame-induced disturbance. The unsteady, one/dimensional, compressible flow equations were solved using the method of characteristics. This study was primarily undertaken to determine the feasibility of extending the method of characteristics to study the aero-dynamic response of complex mine networks. It was demonstrated that although the technique has merit in studying the complex wave interaction in single entries, it appears to be too unwieldly and too expensive for network analysis. Effort was also directed at a further study of the dispersion and filtering characteristic of aerodynamic disturbances in mine passageways.

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 Larry P. Jackson

As part of the current research effort in shale-oil chemistry conducted by the Federal Bureau of Mines, reduced chlorophyllins were prepared and pyrolyzed in an effort to identify the role of plant pigments and their decomposition products in the nitrogenous compounds found in the product of oil-shale pyrolysis. The properties of the chlorophyllin pyrolysates were related to the composition of the reduced chlorophyllins with particular emphasis on the amount and types of nitrogen compounds formed. A comparison based on the types of nitrogen compounds present was made betvJeen shale oil and the chlorophyll in pyrolsates. In order to make this comparison, a sample of shale-oil light distillate was separated into polar and nonpolar fractions, and a careful examination of the polar fraction was conducted to obtain an accurate picture of the types of nitrogen compounds present. The information gathered from these studies was used to evaluate reduced chlorophyllin as a model of oil-shale kerogen insofar as the production of nitrogen compounds was concerned. The results indicate that the reduced chlorophyllin does yield nitrogen products which are directly related to the nitrogenous compounds in shale oil, and it therefore represents a good model of shale-oil kerogen.

Jan 1, 1975

By John F. Papp

The Bureau of Mines has sampled microstructure of low-pressure flat flames by mass spectrometer for normal methane-oxygen-argon and for methane-oxygen-argon-bromotrifluoromethane flames. The physical and chemical phenomena, and the method of analysis of mole fraction data to evaluate net reaction rates are here considered in detail. Included is a computer program listing with output on one flame. Chemical species considered are CH4 , CO, CO2, H, H20, OH, Ar, H2, O2 , O, H2CO, CH3 , CF3Br, HF, HBr, Br, CH3Br, HCO, F2CO, CH2 CF2 , H02.

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 P. W. Jeran, C. D. Sullivan, 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 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

By Maurice Deul, Herbert H. Fields, John H. Perry

The Bureau of Mines has been promoting health and safety in mining since its establishment in 1910. One area of research covers methane control in coalbeds; this report describes a multipurpose borehole used for both degasification and the production of commercial-quality gas. The multipurpose borehole was drilled into a barrier pillar, and seven horizontal degasification holes and one pressure point hole were drilled radially out from its perimeter. On January 28, 1974, after 505 days of degasification, a compressor was installed to the exhaust stack of the multipurpose borehole (2), and pipeline--quality gas was introduced into a commercial pipeline. As of February 4, 1975, over 171 million cubic feet of gas had been purchased by the gas company. The in situ pressure at a depth of 200 feet into the coalbed and the average gas flow and water flow from the degasification holes as they were completed and closed off were 203 psig, 1,200,000 cfd, and 6.8 gpm, respectively. Twenty-four hours after the seven holes were connected through individual pipes to the atmosphere, the total gas and water flows and the in situ pressure dropped, respectively, to 971,000 cfd, 1.3 gpm, and 18 psig. Five hundred days later, the corresponding values were 620,000 cfd, 0.15 gpm, and 10.5 psig. Daily flows have been as high as 800,000 cfd, and as low as 360,000 cfd, during the last 500 days. On February 4, 1975, after 882 days of degasification, 576 million cubic feet of gas had been removed from the Pittsburgh coalbed; apparently a much larger area of virgin coal is being degasified than is defined by the holes. This study indicates that horizontal boreholes drilled into a coalbed from the bottom of any shaft will effectively remove gas from the Pittsburgh coalbed.

Jan 1, 1975

By Herbert H. Fields

The Bureau of Mines has been promoting health and safety in mining since its establishment in 1910. One area of research covers methane control in coalbeds; this report describes a multipurpose borehole used for both degasification and the production of commercial-quality gas. The multipurpose borehole was drilled into a barrier pillar, and seven horizontal degasification holes and one pressure point hole were drilled radially out from its perimeter. On January 28, 1974, after 505 days of degasification, a compressor was installed to the exhaust stack of the multipurpose borehole (1), and pipeline--quality gas was introduced into a commercial pipe-line. As of February 4, 1975, over 171 million cubic feet of gas had been purchased by the gas company. The in situ pressure at a depth of 200 feet into the coalbed and the average gas flow and water flow from the degasification holes as they were completed and closed off were 203 psig, 1,200,000 cfd, and 6.8 gpm, respectively. Twenty-four hours after the seven holes were connected through individual pipes to the atmosphere, the total gas and water flows and the in situ pressure dropped, respectively, to 971,000 cfd, 1.3 gpm, and 18 psig. Five hundred days later, the corresponding values were 620,000 cfd, 0.15 gpm, and 10.5 psig. Daily flows have been as high as 800,000 cfd, and as low as 360,000 cfd, during the last 500 days. On February 4, 1975, after 882 days of degasification, 576 million cubic feet of gas had been removed from the Pittsburgh coalbed; apparently a much larger area of virgin coal is being degasified than is defined by the holes. This study indicates that horizontal boreholes drilled into a coalbed from the bottom of any shaft will effectively remove gas from the Pittsburgh coalbed,

Jan 1, 1975

By Ann G. Kim

Methane in coal constitutes a serious hazard in coal mining. Draining the methane in advance of mining can mitigate this hazard, conserve energy, and offer economic benefits. This Bureau of Mines report evaluates the Pittsburgh coalbed in Greene County, Pa., to determine if advance drainage is feasible. The gas content of virgin reserves in Greene County is estimated at 100 to 200 ft3/ton, a total of over 370 billion ft3 of gas in an area approximately 310 mi2. Because of the similarity to natural gas, drained coalbed gas could be recovered and added to pipeline supplies of natural gas. The value of conserved gas would offset the cost of drainage and extend energy resources.

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