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By D. W. Mitchell

This Bureau of Mines report summarizes experience and past research on methods for sealing abandoned areas of a coal mine and areas from which the pillars have been wholly or partially extracted. The Federal Coal Mine Health and Safety Act of 1969 requires that such areas be ventilated or sealed with explosion-proof bulkheads, but the present study indicates that bulkheads alone cannot isolate areas in a coal mine in which methane and other dangerous gases have accumulated. Gas-air exchanges between sealed and open areas must be controlled.

Jan 1, 1971

By James H. Russell

Several solid sorbents were compared for their effectiveness in removing sulfur dioxide from flue gases. The materials were tested for the rate of sorption and capacity at about 300° C, and rate of regeneration around 700° C in thin beds and in 4-inch-diameter fluidized beds. Rates of material loss were also estimated. The sorbents tested included three samples of alkalized alumina, two samples of sodium carbonate-impregnated alumina, and one proprietary sample of porous silica impregnated with copper and iron compounds. The results showed that all the alkalized aluminas had good sorption capacities and rates, required high temperature regeneration, and suffered excessive material loss; the sodium carbonate-impregnated aluminas (1) had high sorption rates but barely adequate capacities, (2) required high temperature regeneration, and (3) suffered excessive material losses; and the copper-iron impregnated silica suffered only slight material loss and could be regenerated at a relatively low temperature, but the sorption rate and capacity were too small. None of the sorbents met all the arbitrary performance criteria that follow: sorption rate constant of 1 min-1, sorption capacity of 0.1 g sulfur per g sorbent, regeneration rate constant of about 0.075 min-1 at a reasonable temperature, less than 0.07 pct per hour material loss during operation, and a chemical life of 500 cycles.

Jan 1, 1971

By L. C. Headley

Surface areas of two synthetic and three natural consolidated porous samples were obtained by the Orr low-pressure permeametry technique. The results suggest that the Orr technique is a useful substitute for the low-temperature gas adsorption (BET) method for determining the surface area of rock samples. It was more rapid than the BET method, and the surface-area values obtained were larger but agreed better with BET values than values calculated from the Kozeny-Carman equation. Efforts were unsuccessful to demonstrate the influence of channel-size distribution on pressure-flow rate curves by means of experimental data and a parallel channel model.

Jan 1, 1971

By Benton L. Tibbetts

Comprehensive geophysical measurements were made in the Tertiary Channel gravel deposits of Badger Hill, Calif., with the refraction seismograph, gravimeter, and well logging equipment, to develop a three-dimensional physical model of the gold-bearing gravels. Tests were also made of the applicability of magnetometer and electrical resistivity techniques. Results of 14 seismic profiles revealed four distinct layers with velocities of 1,600 ft/sec for loose gravel, 5,900 ft/sec for compact gravel, 8,600 ft/sec for cemented, blue gravel, and 15,500 ft/sec for bedrock. The depth to bedrock along the middle of the channel varied from a minimum of 100 feet in the hydraulically mined pit area to a maximum of about 300 feet in the upper bench area immediately south of the pit. These geophysical methods revealed that 40 percent of the drill holes necessary to delineate the deposit could be eliminated, at a cost saving of at least 30 percent.

Jan 1, 1971

By L. B. Pankratz

Low-temperature heat capacities, high-temperature enthalpy increments, and the enthalpy of formation at 298° K were determined calorimetrically for vanadium subnitride (VN0.465). The low-temperature investigation gave S°298.15 = 6.379 ±0.005 cal/deg mole, and a combustion calorimeter investiga¬tion provided ?Hf°298.15 = -31.80 ±0.60 kcal/mole. The two quantities were combined with the high-temperature data to give standard values of enthalpies of formation and free energies of formation above 298° K. These and related thermodynamic functions were tabulated to 1,800° K. Similar data are included in the range of 298° to 1,600° K for the mononitride, VN.

Jan 1, 1971

By Larman J. Heath

Liquid incendiaries were burned within the interstices of several different types of sandstone cores to determine the technical feasibility of increasing sandstone permeability by this method. Fuel-oxidant mixtures were tested in 186 cores; six cores exploded when ignited. In virtually all instances, the explosion completely pulverized the sandstone cores. In addition n those cores damaged by explosions, 24 cores were fractured so severely that permeability tests were impossible. Although combustion gener¬ally increased the permeability, specific mixtures at given pressures were inconsistent in their ignition and burning behavior. Tests indicated that the heat of burning incendiaries significantly increased sandstone permeability. The improved permeability ratios were usually less than 2, but one was 10.3. Permeability alteration by other in situ methods was not as effective as that by flame propagation.

Jan 1, 1971

By D. G. Kesterke

Research was conducted to determine the feasibility of extracting elemental oxygen from silicate-bearing melts by high-temperature electrolysis. The method was based on a modification of existing processes for electrowinning metals from their oxides dissolved in molten halide systems. Electrolyses were performed at temperatures ranging from 1,050° to 1,250° C in boron nitride cells that incorporated a silicon carbide cathode and an iridium anode. The electrolytes contained volcanic scoria as the oxygen source, plus mixtures of BaF2 and LiF as fluxing agents. Cell gases containing almost 14 volume-percent oxygen were obtained. The average anode current efficiency for several experiments of extended duration was calculated to be 55 percent. Cell design and operating conditions are described, and some of the problems associated with the process are discussed.

Jan 1, 1971

The Bureau of Mines has long been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts, the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions1 issued by the Bureau of Mines, and the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. The Government, with the exception of the Tennessee Valley Authority, purchased approximately 5.5 million tons of coal in fiscal year 1971. In connection with these purchases, the Bureau analyzed 4,366 samples. These are published (table 1) for the use of Government officials and the public. Such analyses of delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1972

By Verne E. Hooker

Near-surface temperature measurements in two granite quarries show that diurnal temperature variations are significant to a depth of 1 or 2 feet, and annual temperature variations are significant to a depth of at least 25 feet. As a result, ground stress anomalies due to temperature exist near the surface, and their magnitude depends upon the time of day and the time of year. Rock stress and corresponding temperature measurements were made in one granite quarry over a rock temperature range of 33° to 81° F. Measured rock temperatures show good agreement with values predicted from one-dimensional heat flow theory. Calculated and measured stress-temperature coefficients for the two granites in this study are given. Thermally induced stress variations in near-surface rocks tested were as large as 1,690 psi from combined daily and seasonal temperature changes.

Jan 1, 1971

By D. G. Kuehn

Positive ion sampling studies have been conducted on do discharges containing 0.33 percent sulfur dioxide in helium. Measurements were made for normalized gas pressures from 0.45 to 6.8 torr and discharge currents from 5 to 40 ma. Ion species observed included SO+, S+, SO2+, SO3+; O+, and 0+, 02+. Studies were conducted on the functional dependence of the various ion species with respect to axial distance, pressure, current, and gas flow rate. Interpretation of these results is consistent with the assumption of SO2 dissociation. Deposition of sulfur compounds was observed in the plasma container during these studies. The present results are compared with previous studies which have been conducted in SO2.

Jan 1, 1971

By Charles Findlay, Stephen Krickovic

A methane emission rate study was conducted in 1969 on a longwall section of a Lower Kittanning coalbed mine in central Pennsylvania. The longwall face was mined with a drum shearer between developed headings on the head end and headings on the tail end that were driven with a ripper-type continuous miner as needed. The study was conducted over 22 consecutive shifts (7-1/3 days). The average methane emission rate from the Lower Kittanning coalbed during mining at the face and developing the headings at the tail end of the face was 34 cfm. Caving of the gassy overlying strata as the result of mining at the face increased the methane emission to rates ranging from 702 to 1,049 cfm.

Jan 1, 1971

By Stephen Krickovic

A methane emission rate study was conducted in 1969 on a longwall section of a Lower Kittanning coalbed mine in central Pennsylvania. The longwall face was mined with a drum shearer between developed headings on the head end and headings on the tail end that were driven with a ripper-type continuous miner as needed. The study was conducted over 22 consecutive shifts (7-1/3 days). The average methane emission rate from the Lower Kittanning coalbed during mining at the face and developing the headings at the tail end of the face was 34 Am. Caving of the gassy overlying strata as the result of mining at the face increased the methane emission to rates ranging from 702 to 1,049 cfm.

Jan 1, 1971

By Thomas E. Green

A gas volumetric method was developed for determining metallic aluminum at the 0.01-to 0.3-percent level in 100-gram samples of recycled glass. The method is based on the measurement of the change in gas volume produced by the reaction 2 Al + 2 NaOH + 2 H2O ? 2 NaAl02 + 3 H2 using a simple apparatus assembled from readily available glassware. Apart from sampling errors, the precision of the method is within ±5 percent. A minor modification of the apparatus would extend the method to larger samples or samples of higher metallic aluminum content. Metallic iron and metallic zinc do not interfere at the concentrations found in recycled glass recovered from incinerator residues.

Jan 1, 1971

By J. M. Kuchta

Ignition and flammability test methods were developed by the Bureau of Mines for use in the classification of flammable solids by the Department of Transportation. A rotating disk ignition apparatus and a flame-spread-rate apparatus are proposed for determining the ignitability and flammability, respectively, of most flammable solids. Extremely flammable solids, such as pyrophoric materials, are evaluated by determining their ease of spontaneous ignition in an environmental chamber at high-humidity conditions. Data are presented for various representative solids to show the reliability of the test methods for classifying the materials. A classification system is also proposed for use in government transportation regulations.

Jan 1, 1972

By J. M. Kuchta

Bench-scale test methods were developed by the Bureau of Mines for use by the Department of Transportation in the classification of solid and liquid oxidizers. A burning rate test is recommended for evaluating the fire hazard of solid inorganic oxidizers when mixed with a red oak sawdust as the reference combustible. A spontaneous ignition test is proposed for evaluating liquid and solid inorganic oxidizers which may decompose violently or ignite spontaneously when unmixed or mixed with the wood sawdust under unconfined conditions. Test results are compared for various representative oxidizers and a classification system is proposed for use in the government transportation regulations.

Jan 1, 1972

By James H. Scott

A technique of seismic refraction data analysis has been developed in which a digital computer is used to generate a two-dimensional model representing a layered-earth depth interpretation. Travel times are picked on seismic records by the human interpreter. These times, together with shot point and geophone locations and refraction layer control information, are submitted to the computer on punched cards. A first approximation delineation of each refraction horizon is obtained by a computer adaptation of the delay-time method. The approximation is then tested and improved by the computer through the use of a ray-tracing procedure in which ray travel times computed for the model are compared against field-measured travel times. The model is subsequently adjusted in an iterative manner so as to minimize the discrepancy between computed and measured travel times. The Fortran program is listed in the appendix of the report together with instructions for preparing data cards and examples of results.

Jan 1, 1972

By H. E. Thomas

[The Bureau of Mines has conducted a field hydraulic fracturing experiment to determine the preferential orientation of induced fractures in oil shale at a depth of about 400 feet in the Green River Basin of Wyoming. The hydraulic fracturing treatment was performed by injecting extremely viscous water-base gel and 8- to 12-mesh sand into the oil shale through straddle packers set in an impermeable section of smooth-walled, 6-1/4-inch-diameter open hole. An impression packer proved that a horizontal fracture, which has an average width of about 1/2 inch at the borehole, was induced. A corehole drilled 100 feet from the fractured well intersected the fracture and confirmed its horizontal orientation. Because a horizontal fracture was successfully initi¬ated, it is inferred that the creation of multiple, closely spaced horizontal fractures may be feasible in Green River Basin oil shale.]

Jan 1, 1972

By B. J. Scheiner

Oxidation procedures based on the chlorine-hypochlorite system were investigated for improving gold recovery from carbonaceous gold ores. The oxidation pretreatment prior to cyanidation was accomplished by (1) addition of sodium hypochlorite to ore pulp, (2) by addition of chlorine to ore pulp, and (3) by generation of hypochlorite in situ by electrolysis of a brine solution used to pulp the ore. Gold extraction of 90 pct was achieved by cyanidation of carbonaceous ore that had been pretreated with 20 Ib per ton sodium hypochlorite at 50° C for 4 hours. Similarly, pretreatment of the ore pulp with 35 1b chlorine per ton at 24° to 30° C and 15 hours reaction time resulted in 89-pct gold extraction by subsequent cyanidation. Concomitant studies showed that electrolyzing the pulp prepared with a brine solution was equally as effective as electrolyzing hypochlorite and chlorine for oxidizing carbonaceous ore constituents that are deleterious to cyanidation. Gold extraction of 90 pct was obtained by electrolysis when 275 lb of are was treated at 200 amp for 7 hours in an 8-to 10-pct salt solution. Power consumption was in the range of 60 kwhr per ton.

Jan 1, 1972

By Harold L. Rhodes

Vapor-liquid equilibria data for 65-34-1 and 25-27-48 mole percent helium-nitrogen-methane mixtures are presented for 12 temperatures from 76.5° to 164° K and pressures from 100 to 1,200 psia. These data were obtained in a windowed phase equilibria cell equipped with a vapor recirculating pump. Isobaric and isothermal K-values are plotted for both mixtures. Two isometric plots are included.

Jan 1, 1972

By Charles C. Boley

High-volatile A bituminous coal from the Allen mine, Las Animas County, Colo., blended with char produced from the same coal yielded accept-able metallurgical coke in a 500-lb movable-wall test oven. Nineteen experimental runs were carried out using several concentration levels of two different chars, 5.6 and 19.6 percent volatile matter, produced by entrainment carbonization of the base coal. With the higher-volatile char, an acceptable coke was produced at a 22.5-percent concentration; the lower-volatile char did not produce an acceptable coke at the concentrations investigated.

Jan 1, 1972