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By Robert C. Ellman

Stockpiles containing 2.3 million tons of lignite constructed in the period 1948-56 in conjunction with the construction of Garrison Dam on the Missouri River demonstrate successful stable long-term storage of lignite. Uniform and thorough compaction of each of the I-foot-thick layers by which the piles were constructed produced a bulk density of 70 Ib/cu ft. Air penetration into the stockpiles was restricted to a degree that prevents spontaneous heating or deterioration of the stored lignite, A continuing record of observations beginning with stockpiling operations in 1948 has been accumulated, This includes periodic fuel analysis, analysis of pile gases, and measurement of pile temperatures on the first large stock-pile, pile 5. This report describes the stockpiling method, the changes in heating value, pile gas composition, and pile temperature and summarizes observations from 1953 to 1964, Data accumulated attest to the stability of the stored lignite. The variation of the average heating value of periodic pile-depth samples is only 160 Btu/lb (11,990 to 11,830) on the moisture" and ash-free (maf) basis during almost 10 years of storage. Temperature levels of the pile interior are progressively decreasing. At pile surface, cyclic variations occur with the season. The only problem encountered with the large stockpiles is wind and water erosion of the pile surface. The partially successful control measures used are described.

Jan 1, 1967

By D. R. Corson

The Bureau of Mines instrumented an operating stope in a deep vein mine to determine the amount of wall closure and the magnitude of loads imposed on a backfilled stope. Hydraulic pressure cells used to monitor pressures in the fill) with bolt closure points to measure vein-wall movement and the procedure for their installation) are described) and the results of the laboratory calibration analysis of the reliability of these cells are given. An attempt to monitor density and moisture changes in the backfill with a nuclear density-moisture device was only partly successful) owing to either deformation of access tubing or relative displacements of the vertical vein walls relative to the emplaced tubes. Data from the instrumentation indicate vein-wall closure in excess of 20 inches and pressures within the fill approaching 600 psi. Analysis) incorporating field data with results of laboratory tests of the compressibility of timber and tests defining the constrained moduli of the fill) points out the limited restraint to vein closure offered by timber sets. Ground movement induced by mining activity could be more effectively con-trolled by the use of densely compacted backfill.

Jan 1, 1967

By E. K. Kleespies

The Bureau of Mines determined the kinetics of the reaction of titanium-iron alloys with titanium trichloride dissolved in sodium chloride to provide a basis for understanding the reactions occurring in metallurgical processes involving reduction of the metal halides or alloy refining in fused salts. The rate of the heterogeneous reaction was determined between titanium-iron alloys and titanium trichloride to elucidate the effects of alloy composition on the rate. Measurements were made in an inert atmosphere with a high-temperature thermobalance using high-purity reactants. The rates of the reactions were about 1 x 10-5 g Ti/cm2-sec, and the reaction was phase-boundary controlled. Titanium alloys of the body-centered cubic beta structure reacted faster than those with the hexagonal close-packed alpha structure. The inter-metallic compound, TiFe, reacted very slowly, whereas TiFe2 was inert. Alloys containing above 89 atomic percent iron gained weight by reacting with titanium species in the salt solution and depositing titanium in the alloy. The effect of TiCl3 concentration on the reaction rate was determined from 2 to 12 weight-percent TiC13 and at various alloy compositions. At high iron contents, above 50 atomic percent, the TiC13 concentration effect was small. At lower iron contents, the TiC13 concentration effect was greater for beta-crystalline alloys than for alpha-crystalline alloys. The temperature dependence of the reaction between titanium alloy containing 8.7 atomic percent iron and titanium trichloride was measured over the temperature range 1,062° to 1,220° K, and the energy of activation was 7.7 kilocalories for the reaction.

Jan 1, 1967

By T. Estelle Gardner

The Bureau of Mines made enthalpy measurements on sodium bromide and sodium iodide in the temperature range 400° to 1,200° K using an ice calorimeter. Equations representing enthalpy as a function of temperature were derived from the data by the method of least squares. These equations were used to calculate smooth values of heat capacity, enthalpy, and entropy at 50° K intervals from the ice point to 1,200° K. The melting point determined for sodium bromide was 1,020° K; the melting point of sodium iodide was 934° K. The heats of fusion of sodium bromide and sodium iodide were calculated to be 6,270 and 5,680 cal/mole, respectively.

Jan 1, 1967

By C. C. Shale

Electrical resistivities for various coal ashes in air and in a nitrogen atmosphere are given over the range 100° to 1,500° F. Resistivity of low-carbon ash in air is very high at low temperature, rises to a maximum at about 250° F, decreases very rapidly with increasing temperature to about 800° F, then decreases gradually to approach an asymptote at 1,500° F. Resistivity of high-carbon ash in air follows this same general trend at values which are much lower and are proportional to the carbon content. After the carbon has been burned off, resistivity of the remaining ash approaches the high values corresponding to low-carbon ash of similar chemistry. Two factorial experiments show the effects of temperature, particle size, chemical content, and compressibility on the resistivities of four fly ashes of widely different chemical composition in the temperature range proposed for coal-fired turbines. Resistivities of all low-carbon ashes tested fall in the range 106 to 107 ohm cm at 1,500° F and should be removable by electrostatic precipitators. Ashes containing carbon in excess of about 8 percent, however, have low resistivity (as determined in nitrogen), especially at high temperatures. Therefore, high-carbon materials may not be collectable in precipitators because the resistivity is below the minimum value necessary for precipitation. Consequently, high carbon residues from partial combustion of coal probably could not be removed effectively at high temperatures.

Jan 1, 1968

By D. A. Wilson

A process was developed on a laboratory scale in which a solid waste byproduct from refining of secondary lead was converted into three valuable products. Roasted lead blast furnace matte was leached with water to recover copper. This was followed by brine leaching to recover lead. Residues were finally smelted to yield pig iron. Copper was precipitated as cement copper and the lead product obtained was a mixture of pure 3PbO.PbC12.xH20 and Pb(OH)C1. Copper recovery was 89 percent and lead recovery was 96 percent.

Jan 1, 1967

By M. L. Odenbaugh

The viscosity reduction effect of varied concentrations of leonardite (a naturally oxidized form of lignite) and leonardite-caustic on the rheological properties of a standard bentonite drilling fluid was studied and evaluated. The minimum plastic viscosity was found to occur at application rates of 4 lb of leonardite and 1.33 lb of caustic per barrel of drilling fluid. Leonardite-caustic treatment was not beneficial in treatment of salt-contaminated drilling fluids. Although filter loss rate was reduced; both yield values and gel strength were increased. Compared with other viscosity control agents) including quebracho) ligno-sulfonate) humic acids extracted from leonardite) as well as other reaction products of lignite) leonardite is less effective at low application rates but is an effective treating agent at rates of 2 Ib/bbl or more. Considering the comparable merits of the substance tested) the major factor in determining which agent to use should be based on cost consideration.

Jan 1, 1967

By T. E. Sterner

A laboratory investigation was conducted to determine the applicability of the thermal oil-recovery method as a means of increasing ultimate oil recovery in the Appalachian region. The primary objective was to establish self-sustained combustion in consolidated and unconsolidated sand test assemblies saturated with various amounts of Pennsylvania Grade crude oil and synthetic brine. Tests using blocks of sandstone were unsuccessful because of sealing problems and fracturing of the rock due to thermal stresses. A combustion wave of about 700° F was propagated through the sand-oil-water packs in the linear tube tests. The high air flux used resulted in high oil consumption and rapid movement of the combustion wave through the tubes. Analytical tests on the sand pack showed that sufficient fuel was deposited during the linear tube experiments for a self-sustained combustion wave.

Jan 1, 1967

By Thornton L. Neathery

Geologic investigation of a mineralized zone in eastern Alabama indicates that large quantities of talc and soapstone are scattered over a wide area close to the surface. Laboratory experiments show that this material may be upgraded to a high-quality talc. A market survey indicates that the talc deposits may be of current and long-range interest. The anthophyllite asbestos which is associated with the talc does not appear to occur in sufficient quantities to be considered as a primary commercial source.

Jan 1, 1967

By J. M. Stuve

The standard heats of formation (?Hf°) of holmium trichloride and terbium trichloride were measured by solution calorimetry. Heats of solution of holmium and terbium metals and their anhydrous chlorides were measured in 4.360 molal HCI at 298.15° K. From these measurements ?Hf° for HoC13 (c) was calculated as -240,290 ±1,700 cal/mo1e, and ?Hf° for TbC13 (c) was calculated as -238,330 ±1,500 cal/mole at 298.15° K.

Jan 1, 1967

By J. P. Morris

The Bureau of Mines investigated the mechanics of fuming of iron-carbon melts during top-blowing with oxygen. Melts weighing 45 lb were prepared in an induction furnace and blown with oxygen by means of water-cooled lances. The rate of fuming was measured and correlated with the operating variables. The data showed that the primary cause of fuming was a boil at the bath surface in the impingement zone of the oxygen jet. Nucleation of the carbon monoxide bubbles producing the boil was apparently brought about by the precipitation of an oxide phase. The actual fuming mechanism involved partial oxidation and vaporization of bubble films and fine metal spray generated by the bursting of the bubbles. Bubbles that formed outside the impingement zone produced little fume. The distribution of trace elements between the metal and fume strongly indicated that the fume contained fine spray particles as well as particles that had condensed from vapor. The rate of fuming was found to be proportional to the carbon content of the metal) the concentration of oxygen in the jet) and the bath temperature) provided that a continuous boil occurred. In the absence of a boil) very little fume was produced.

Jan 1, 1967

By W. H. Engelmann

The electrokinetic (zeta) potentials of a charcoal granite in an aluminum chloride (AlCl3) solution and in an oleylanunonium acetate (C18H35NH3+ -OCOCH3) solution have been correlated with the specific damping values as measured by the pendulum sclerometer. This investigation shows that the pendulum specific damping attains a minimum at the isoelectric point for the charcoal granite-aluminum chloride and charcoal granite-oleylammonium acetate systems, and thus indicates that the penetration of the diamond points is a maximum at the isoelectric point.

Jan 1, 1967

By James A. Wasson

This report analyzes the petroleum-production potential of the basal Greenbrier dolomite zone, Sycamore-Millstone field, Sherman District, Calhoun County, W. Va., through the application of certain secondary-recovery methods. The well logs obtained and the core recovered from a well in this formation permitted an evaluation of the productive capability of the reservoir, Approximately 120,000 stb of oil may be produced from a 20-acre five-spot unit at breakthrough if the property is waterflooded. At an assumed limiting producing gas-oil ratio of 20)000 sef/stb, approximately 69,000 stb of oil should be recovered by low-pressure gas drive.

Jan 1, 1967

By M. J. Kovalik

The effects of the process variables on the production of chemical coke on a chain grate stoker, a type of traveling grate, were studied. Six bituminous coals, ranging in volatile matter from 16.7 to 43.8 percent, were successfully carbonized, yielding chemical coke with acceptable physical properties. The coke yields were dependent on the volatile-matter content of the coal. The air fuel ratio had the most marked effect on the yield and characteristics of the resultant coke, and the general furnace performance. Results can only be predicted; the actual yield and quality of coke obtained from any given coal can only be determined by actual tests using the optimum processing variables to obtain a coke with minimum volatile-matter content and to retain as much of the fixed carbon in the original coal as possible.

Jan 1, 1967

By K. E. Stanfield

Oil-yield results are presented for 65 oil-shale sections in Piceance Creek Basin, Colorado, sampled during the period 1957 through 1963. Including previously published data, oil-yield results for 203 sampled sections have now been released by the Bureau of Mines to aid in appraising the shale oil potential of the basin. Oil yields of core samples (135 sets) were regarded as reliable bases for appraising the Mahogany-zone interval, but only 5 sets of cores sampled the deeper, lower-zone oil shales. Drill cuttings (68 sets) sampled the lower-zone oil shales, but their oil yields are principally indicative and should be confirmed by analyses of cores. More complete core sampling of the lower-zone oil shales is needed.

Jan 1, 1967

By O. C. Baptist

The gravitational pressure gradient (GPG) in porous sandstone containing free gas was determined to define the proper GPG to use when calculating the rate of downdip flow of oil in the Sub-Scalez No, 1 sand, Elk Hills field, Naval Petroleum Reserve 1. The GPG was determined at several gas saturations using long, artificially consolidated sandstone models that were mounted vertically in some tests and horizontally, with rotation, in others. Also determined by laboratory and field tests were relative permeabilities, capillary pressure relations; critical gas saturation, water sensitivity, and depletion drive performance. The critical gas saturation in the models having an absolute permeability of 1 to 2 darcys was about 2 percent of pore volume. The GPG with the critcal gas saturation was that due to the weight of the gas-saturated oil. The GPG in the upper part of the models was reduced as gas saturation increased to a value considerably larger than the critical. The exact gas saturation at which the GPG became less than that due to the weight of the oil could not be determined but was estimated to be of the order of 10 percent of pore volume. Tests indicate that the rate of oil production is not permanently reduced by exposure of the sand to fresh water but that the rate of injection of fresh water will be considerably less than that to brine, Methods for determining the factors mentioned above are discussed.

Jan 1, 1967

By Donald W. Mitchell

The fire hazard of neoprene, polyvinyl chloride, and rubber conveyor belts was studied at the Federal Bureau of Mines Experimental Coal Mine. The effects of intensity of ignition source, velocity of the ventilating air, and type of belt were investigated at three levels in small-scale gallery experiments. Studies were made in the mine on the effects on ignition and flame propagation of belt-entry dimensions, belt widths, and belt configuration. Methods for extinguishing belt fires were also investigated under simulated mining conditions, and during these trials coal dust and grease were placed on the belt. The research showed that conveyor belts will burn. Neoprene, polyvinyl chloride, and rubber belts, with and without carcass, ignited and propagated flame. The highest rate of flame propagation was obtained on rubber belt. The fire hazard increased with increase in intensity of ignition source and air velocity. Flame propagated only when air was forced through the test zone; propagation was not obtained when forced ventilation was not used, as would exist in a neutral entry in a mine. Automatic water sprays and high-expansion foam effectively arrested flame propagation; direct application of water and bicarbonate dusts was ineffective.

Jan 1, 1967

By R. F. Abernethy

The work discussed in this report was done by the Bureau of Mines to develop a method for determining trace amounts of fluorine in coal. Samples of coal mixed with calcium oxide as a fixative agent for fluorine were ashed at 600° C and the residue was fused with sodium carbonate. The melt was dissolved in phosphoric and sulfuric acids and distilled to separate the fluorine) which was determined in the distillate by a SPADNS-zirconium spectrophotometric method. Fluorine determinations of 83 commercial coals ranged from 0,001 to 0.019 percent.

Jan 1, 1967

By James H. Aase

Shales from 10 locations in Michigan were sampled, tested, and evaluated to determine their suitability as raw materials for producing lightweight aggregate by rotary-kiln methods. Sampling procedures and the geology of the shale units tested are discussed. Preliminary testing in a muffle furnace preceded extensive testing in a l6-inch by 14-foot rotary-kiln. Rotary-kiln products from these shales ranged in weight from 35.5 to 61.2 pounds per cubic foot (pcf). Concrete test specimens made pith selected aggregates were evaluated to determine the qualities of the concrete. Compressive strengths of the concrete ranged from 2,830 to 4,240 psi after 28 days of curing. Unit weight of the concrete ranged from 94.8 to 101.5 pcf. Lightweight aggregate suitable for use in structural concrete meeting ASTM standards was produced by the rotary-kiln method using shale samples from two locations.

Jan 1, 1967

By Joseph N. Harstead

This Bureau of Mines report provides information on the first 49 water-flood projects (or units) in Nebraska. All injection was in the ?D? or "J" Cretaceous sands of western Nebraska. Specific data presented include location, map, discovery and development, water supply and injection, oil and water production, estimates of oil in place, primary and secondary recoveries. The 49 projects studied) including four dual-zone projects, should recover about 126.5 million barrels of oil. Eighty-six percent of the estimated oil had been recovered by the end of 1966. Abundant water was found near most projects.

Jan 1, 1967