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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 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 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 F. N. Kissell, C. M. McCulloch, Maurice Deul, J. R. Levine

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 content 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 desorbed 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 Alexander May

The Bureau of Mines, in cooperation with the Florida phosphate mining industry, investigated the dewatering of waste phosphatic slimes. Part of this investigation was to determine the electrophoretic mobilities and cation exchange capacities of the slimes. The mobilities and exchange capacities are reported for samples of slimes taken from 15 plants operating in the Florida land-pebble phosphate district that includes Polk,Hillsborough, Manatee, Hardee, and DeSoto Counties. The electrophoretic mobilities determined were all negative, ranging from -0.24 to -1.93 (micrometers per second) per (volt per centimeter). Also reported are frequency distributions of electrophoretic mobilities, electrophoretic mobilities of slime diluted with distilled water and electrophoretic mobilities of sand-slime mixtures. The cation exchange capacities ranged from 17 to 45 milliequivalents per 100 grams of slime solids.

Jan 1, 1975

By K. Thirumalai

The feasibility of breaking hard rock by thermal weakening and subsequent mechanical impacting was tested, Field tests at a basalt quarry in Dresser, Wis., demonstrated that large hard-rock blocks (5 by 5 by 5 ft) could be effectively reduced in size by this method. A series of secondary breakage tests, using air-propane heating, resulted in an average heating cost of $0.36 per ton. This combination energy approach provides an alternate means of size reduction of large hard-rock boulders for quarry and for underground are chute and grizzly operations where mechanical methods, used alone, are ineffective.

Jan 1, 1975

By W. M. Dressel

In producing feed for a lead blast furnace, concentrates analyzing 70 to 80 pct Pb are sintered to produce a physically acceptable low-sulfur product which contains only about 50 pct Pb. Mixtures of PbS with varying amounts of SiO2, CaO, Fe 20., and ZnS were heated in an oxidizing atmosphere at 1,000° C; the products were cooled and examined to determine the problems involved in producing sinter with substantially higher lead levels. Microscopic and electron microprobe studies of the above products as well as experimental and commercial sinters indicate that sinters consist essentially of lead silicates, lead-zinc silicate, calcium zinc silicate, and spinel (ferrite). Lead oxide and lead sulfate areas appear to result from insufficient mixing of the materials prior to sintering. The data give an insight into the process and show that sintering results from a complex interaction of all constituents and that sintering is not simply a matter of diluting the mixture to control the oxidation of lead sulfide.

Jan 1, 1975

By R. H. Sprute

Hydraulic backfill consisting of siliceous mill tailings was successfully dewatered and consolidated by electrokinetics in a field test conducted by the Bureau of Mines at the Star mine, Burke, Idaho. A stope at the 2,000-foot level was filled in such a way that slimes and coarse sand were retained in the scope. Following settlement of solids and decant of surface water, direct current applied between buried electrodes created a firm, dense material in approximately 3 hours. This rapid densification of fine-grained material demonstrated the utility of this method and suggests other applications, particularly in the control of slime deposits that cause serious problems in many deep mines.

Jan 1, 1975

By E. S. Shedd

Amenability studies were conducted by the Federal Bureau of Mines on an electrooxidation technique for the extraction of mercury from cinnabar ores, particularly those that are too low in grade to be furnaced or retorted economically. Oxidation was accomplished by electrolysis of the ore while slurried with brine. Mercury was dissolved through the formation of the soluble tetrachloro mercury complex, HgC142-. Mercury extractions ranged from 90 to 98 percent in 4 to 6 hours of processing time when tests were made on eight different types of cinnabar ores containing from 0.7 to 18 pounds mercury per ton ore. Salt concentration was varied from 4 to 10 weight-percent depending on whether Pb02 anodes and iron cathodes were used or whether graphite was used for both electrodes. Power consumption ranged from 17 to 64 kilowatt-hours per ton of ore treated. Ninety-nine percent of the mercury was recovered from pregnant solutions by precipitation on an active metal such as zinc, followed by distillation of the resulting amalgam at 600° C.

Jan 1, 1975

By Michael L. Boucher

Copper and nickel sulfides occurring in the Duluth Complex of northern Minnesota were examined at the Bureau of Mines, A microscopic study was undertaken to determine the mineralogy and paragenesis of the ore minerals. Eighty-two samples were taken from one deep diamond drill core located near Babbitt, Minn. Modal analyses are presented for the Duluth Complex rocks and for the are minerals in the major mineralized zone. The major sulfide minerals are chalcopyrite, cubanite, pyrrhotite, troilite, and pentlandite. Results of this investigation suggest that the mineralization is related to the structural features of the enclosing rocks: pores, open fractures, and cavities. The pyrrhotite-troilite-pentlandite assemblage is believed to have formed from an immiscible sulfide melt, probably associated with the troctolitic rocks. Most of it settled to the very porous base of the Duluth Complex, and to the other porous zones near xenoliths; small portions were trapped higher in the section. A later introduction of a copper-rich sulfide melt replaced some of the pyrrhotite-troilite and oxides, and filled in the remaining open spaces and fractures in the Duluth Complex and those of the adjacent footwall rock.

Jan 1, 1975

By Karl R. Becker

A variety of commercial detonators (fuse type and electric instantaneous and delay types) were subjected to impact and thermal stimuli to determine initiation stimulus levels and the dominant parameters in resistance to initiation. In the impact trials the detonators were impacted along their length to find the most sensitive region; threshold initiation limits obtained for these regions ranged from 3.47 to 20.82 joules (2.6 to 15.4 ft-lb). The friction sensitivity of the explosive component was an important parameter in determining sensitivity; various construction features of nonexplosive components played a role as well. In the thermal sensitivity trials, the detonators were heated from ambient to 100° C at an average rate of about 1.0° C/min, and thereafter at 0.5° C/min until they exploded; the explosion temperatures observed ranged from 121° to 188° C. These temperatures correlated quite well with the reaction temperatures of certain characteristic explosive components used by different manufacturers. The data also indicated an effect of confinement on explosion temperatures of detonators.

Jan 1, 1975

By J. R. Cobble

The Federal Bureau of Mines conducted static tests at 2,500° F on 39 refractory compositions, and dynamic tests at [2,825°35° F] on 31 commercial refractory brick specimens to determine their resistance to corrosion and erosion by a slag similar in composition to that used in producing insulating mineral wool. The static tests showed fireclay, low-alumina compositions (<70 percent A1203), zircon, zirconia, SiC, and clay-bonded graphite refractories to be unsuitable. Dynamic test results indicated that magnesia and chromia compositions were superior to high-alumina compositions (=70 percent A1203) as a furnace lining for melting mineral wool. Data from these tests indicated that magnesia and chromia compositions with low RO/R203 mole ratios were more resis tant to attack by mineral wool slags than ones with high RO/R203 mole ratios.

Jan 1, 1975

By George A. Savanick

An experimental hydraulic jetting device intended to operate in a 16-in-diam borehole was designed, fabricated, and used to cut coal and simulated coal samples. This device consisted of two 0.107-in-diam nozzles that rotated in a plane perpendicuIar to a 50-inch length of high-pressure tubing. Experi¬ments were also conducted with stationary jets issuing from a single 0.142-in-diam nozzle. Numerous experiments were performed using systematic variations of jet parameters coupled with assessments of cutting rates. These Bureau of Mines tests showed that when operated at 4,000 psi pressure and a 40-gpm flow rate (1) the device can fragment coal up to a distance of 8 feet from the nozzle, (2) 4,000-psi jets cut more effectively than lower pressure jets with the same nozzle diameter, (3) stationary jets do not cut as effectively as moving jets, (4) interkerf breaking occurs when the kerf spacing is less than 2 inches, and (5) if the kerfs are spaced <1/2 inch, the jet is deflected and thereby reduces cutting effectiveness.

Jan 1, 1975

By J. C. Franklin

A data-acquisition system was designed by the Bureau of Mines to monitor five detectors with radon continuously flowing through each. These detectors could be monitored up to 12 times an hour, but were only monitored according to a preset time, thus allowing radon to be monitored continuously in a uranium mine. The counter can be set to monitor each detector for any period of time up to 16.5 minutes. This allows very low concentrations to be monitored longer to reduce statistical error. There would be no upper limit in radon concentration that could be monitored, but there would be a lower limit of 50 picocuries per liter (pCi/l). Each detector was cylibrated in the laboratory by the Lucas flask method. Multiple samples were taken at two different concentrations, and the correction factor for each detector was determined by a least squares fit of the data. To verify the calibrations, a series of measurements at several concentrations were made against a constant source. Our agreement at low radon concentrations (300 pCi/i) with the two-filter method as within 3 percent; thus, the total error would be this difference plus the two-filter error. At high concentrations the coefficient of variation ranged between 2.1 and 9.8 percent for the five different detector units.

Jan 1, 1976

By K. J. Liles

Research was undertaken by the Bureau of Mines to determine the technical feasibility of producing lightweight aggregate from the waste glass fraction of municipal incinerator residues. Tests were conducted to determine the amount and optimum size of glass, the amount of sodium silicate, and the method used to form the material to be expanded. The most suitable mixture, 78 percent glass, 20 percent clay, and 2 percent sodium silicate, was pelletized and then expanded by exposure to a temperature of 1,550° F for 15 minutes The resulting lightweight material had a bulk density of 38 lb/cu ft and exhibited excellent pore structure. Concrete test cylinders made from the light weight aggregate had a unit weight of 104 lb/cu ft and a compressive strength of 2,550 lb/sq in after a 28-day steam cure.

Jan 1, 1976

By F. P. Haver

Primary lead is produced in the United States by the pyrometallurgical smelting of lead sulfide (galena, PbS) concentrates, which poses sulfur dioxide and lead air pollution control problems. The Federal Bureau of Mines has investigated an alternative hydrometallurgy procedure that does not generate gaseous sulfur oxides and diminishes the potential for the escape of lead into the atmosphere. The procedure involves leaching galena flotation concentrates with ferric chloride (FeC13) solution to obtain lead chloride (PbC12) and elemental sulfur as expressed by the following chemical reaction: PbS + 2FeC13 ? PbC12 + 2FeCl2 + S°. At 100° C, over 99 pct of the PbS in the concentrate is converted to PbCl2 in less than 15 min. The leach solution, composed of brine (NaCl) containing slightly more than the theoretical required amount of FeC13, dissolves the PbC12 as it is formed, leaving a residue of elemental sulfur plus gangue. High-purity PbC12 (>99.9 pct) crystallizes from the leach filtrate on cooling and is electrolyzed in a low-temperature, fused-salt cell to obtain corroding-grade metal (>99.94 pct Pb). Spent leach solution (FeC12) is regenerated for further use by reaction with the chlorine obtained in the electrolysis of lead chloride. Other values, such as Ag, Cu, Zn, and S°, are recovered by additional treatment of either the leach solution or leach residue.

Jan 1, 1976

By Carl F. Wingquist

Electrical resistance heating to effect thermal fragmentation of semiconductive rock was examined by the Bureau of Mines. Tests were carried out on copper-bearing ores of the Nonesuch Shale Formation in the laboratory and in the the field at White Pine, Mich. Fieldwork included primary and secondary breakage tests. Heating tests on in situ rock failed to produce thermal dam-age to an extent considered useful; however, boulders up to 30 ft3 were effectively broken by the method. Power input to the test rock was taken from a 50-kV, 5-amp dc power supply.

Jan 1, 1976

By Arthur M. Hartstein

The Federal Bureau of Mines, under a contract with Ultrasystems, Inc., investigated the thermal oxidative degradation characteristics of conveyor belts used in underground mines. This included the determination of smoke evolution, glow characteristics, char yields, and the identification and quantification of all volatile decomposition products in the form of gram of specific product formed per gram of belt sample tested. In addition to these investigations, degradation studies were conducted on some pure ingredients used in conveyor-belt formulations. Three basic classes of belts were investigated: neoprene, polyvinyl chloride, and styrene-butadiene rubber compositions. The studies indicate that styrene-butadiene-based belts exhibit good flame resistance and are the least hazardous in regard to overall formation of toxic decomposition products. Under this program, thermogravimetric analysis was definitely established as a method of material differentiation.

Jan 1, 1976

By Joan T. May

The Bureau of Mines conducted laboratory tests to evaluate the production of high-purity H3P04 by HCl digestion and solvent extraction. Both batch and bench-scale continuous tests were made. Western phosphate rock concentrates were acidulated with HCI, and the digestion liquors were processed by solvent extraction. Phosphoric acid was extracted with isoamyl alcohol and recovered from the organic extract by contact with an NH4F solution. This solution was fractionally distilled to yield high-purity H3P04. The raffinate from solvent extraction was treated with lime to precipitate CaF2, which was subjected to steam pyrolysis to generate HF. This method was successful in recovering 95 pet of the phosphate and 80 pct of the fluoride contained in the concentrates.

Jan 1, 1976