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By Renpei Yoda

An investigation was conducted to develop columbium alloys with e1evated-temperature strengths higher than those exhibited by more common commercial columbium alloys, and attention was given to improving the oxidation resistance and ease of fabrication. Additions of carbon, aluminum, and chromium were made to some columbium-base alloys, and their effects on workability, recrystallization, oxidation resistance, and mechanical properties at elevated temperatures were explored. The additions were made to take advantage of (1) solid solution strengthening, and (2) precipitation hardening. Three alloys displayed good high-temperature properties with relatively good oxidation resistance at 1,000° C, and tensile strengths from 26,000 to 32,200 psi at 1,400° C. When the properties of these alloys were compared with those of commercial alloys, B-66 and FS-85 (1),4 the outcome was favor-able for the alloys studied in this investigation.

Jan 1, 1967

By Karl-Heinz Frohne

This report presents the findings of a study of a portion of the Clover-Rush Run oilfield located in Roane County, W. Va. The study was made to investigate the possibilities of secondary oil recovery in the Big Injun sandstone underlying the William Kaufman lease. Reservoir properties, original reserves, and primary oil recovery are also presented. The investigation is based on a core analysis and related laboratory tests, well records, field production data, and subsurface information from the Kaufman property. A theoretical primary oil recovery of 9.7 percent of original oil in place is predicted for the reservoir. A waterflood performance prediction of a hypothetical pilot area was made by use of a computer. The prediction showed that, based on laboratory oil water relative permeability curves, the water-injection time needed to initiate oil production is excessive and that the stabilized water-injection and corresponding oil-production rates are very low. This precludes waterflooding the reservoir on an economic basis. A prediction for secondary oil recovery by gas injection was attempted but could not be completed because essential reservoir data were not available. In July 1965, the lease operator initiated, and is currently conducting, a gas-injection program, but there had been no increase in oil production up to November 1966.

Jan 1, 1967

By R. V. Higgins

The Bureau of Mines investigated the use of electronic computers for obtaining more information about relative permeabilities of reservoir rock to oil and water. It was found that there are many possible combinations of relative permeability curves that will result in virtually the same recovery versus injection) but they require different times and rates to recover the oil even with different mobility ratios. Permeability curves obtained by the use of non-viscous oil and employed for calculating the waterfloods of viscous oils can lead to serious inaccuracies. For viscous oils) the wettability characteristics in the middle portion of the permeability curve affect recovery nearly as much as other portions of the curve; this) however) is not true for non-viscous oils in water-wet reservoir rock.

Jan 1, 1967

By James A. Wasson

The Mitchell and Berea sands were cored and logged in Fred Link well K-l, Lower Newport field, Washington County, Ohio. Core and reservoir fluid analyses and available field data were studied to determine if these sands could be successfully waterflooded. The results of the study indicate that there is insufficient oil in place to form an oilbank in either the western Mitchell pool or the Berea sand, and that no commercial recovery of oil by waterflooding can be obtained in these reservoirs.

Jan 1, 1967

By W. E. Anable

The Bureau of Mines studied the purification of commercially available vanadium in the 100-kw electron-beam furnace. Purification studies were conducted on a 100-gram button scale by melting and holding the liquid vanadium at temperatures ranging from 2,060° to 2,080° C at pressure of 5(10)-5 torr for periods ranging from 5 to 20 minutes. The effect of doping vanadium with carbon and metallic additions was determined. This study demonstrated that hydrogen was readily removed to 3 ppm or less, oxygen and carbon were reduced to less than 100 ppm each, and the metallic impurities were reduced Co the range of 10 to 500 ppm. The nitrogen content was not reduced in any of the buttons; rather, the nitrogen concentration generally increased as samples were held for successively longer periods. Oxygen was removed much faster and more completely when vanadium was doped with small carbon additions or one of several dopes prior to melting.

Jan 1, 1967

By Heinz W. Sternberg

A method for the electrochemical reduction of the benzene ring was developed and applied to the electrochemical reduction of coal. Successive electrochemical reductions of a vitrain from low-volatile bituminous coal in ethylenediamine saturated with lithium chloride resulted in the addition of 53 hydrogens per 100 carbon atoms. Ultimate analyses and pyridine solubility of the vitrain recovered after each reduction showed that hydrogen added at the beginning has a much greater effect on solubility than hydrogen added at a later stage. Surprisingly, the removal of sulfur from the vitrain takes place only after the more reactive aromatic rings are reduced. Nuclear magnetic resonance analysis and average molecular weight determination of the extracts of the reduced vitrain samples, representing about 18 percent of the vitrain, showed that these fractions had 95 percent of their hydrogen content on saturated carbon atoms and an average molecular weight of 800 to 900. A study of the effect of operating variables on current efficiency showed that current efficiency is highest with aluminum as cathode material and with lithium chloride as electrolyte. A substantial increase in current efficiency of difficulty reducible olefinic double bonds was achieved by adding a proton donor. This result is significant in connection with the electrochemical reduction of coal which proceeds from readily reducible aromatic double bonds to difficultly reducible isolated double bonds. It is proposed that reduction is achieved by electrolytically generated and subsequently solvated electrons and hence does not require prior adsorption of the substrate at the electrode surface. This offers a distinct advantage for electrolytic reduction of sparingly or insoluble substrates such as coal.

Jan 1, 1967

By D. Bienstock

The use of alkalized alumina in removing sulfur dioxide from a coal-combustion flue gas at 625° F was investigated on a pilot plant scale. The absorber was 26 feet long and 1.6 inches ED. Counter-current gas-solids flow at gas velocities of 8 to 15 ft/sec in the presence and absence of baffles, as well as solids entrainment at gas velocities of 20 to 23 ft/sec with solids recycle, were employed. The spent absorbent as regenerated as fixed bed with the reducing gases--reformed natural .7.7d hydrogen. Of absorption-regeneration were successful completed using the alkalized alumina rolled into spherical granules 10 to 16 mesh. There was no loss in activity of absorbent toward SO2 with a modest attrition equivalent to 0.l percent of the solids feed. Supporting studies were conducted on the effect of the sodium content in the absorbent, the composition of the reducing gas, thermal treatment to increase absorbent hardness, and removal of absorbed chlorine from the absorbent. A mathematical model was formulated to describe the removal of SO2 by alkalized aluminum from fixed and falling beds.

Jan 1, 1967

By Theodore Kessler

The purpose of this Bureau of Mines investigation was to determine what new organic compounds or high concentrations of a particular organic species can be formed by exposure of coal derivatives to ultrasonic energy. Tetralin, l-methylnaphthalene, and pyridine were used as model compounds. Gaseous and solid reaction products resulting from the ultrasonic irradiation of these coal derivatives were determined using mass spectrometry. Products from the irradiation of tetralin were studied as a function of time, atmosphere, and sample size. The sonolysis (chemical reactions produced by ultrasonic energy) of tetralin and l-methylnaphthalene produced C2H2, HCN, CH4, H2, CO, and CO2, depending upon the experimental conditions. The ultrasonic irradiation of tetralin also produced diacetylene under certain experimental conditions. The cleavage of organic chemical bonds by ultrasonic cavitation in the absence of water was also observed in this study.

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 J. L. Reuss

The Bureau of Mines derived information on the softening characteristics of both unfired and indurated iron ore pellets as measured by hot compression strength in a laboratory study. A surprisingly high hot strength (240 1b per ½ -inch spheroid) was developed by unfired magnetite pellets near 900° C; lesser maxima were developed by pellets made from hematite and specularite concentrates near 1,000° C. Those from goethite remained weak throughout the pre induration heating. Fully indurated commercial pellets retain a high resistance to softening when heated in air. On the contrary, in a hot reduing atmosphere their high cold crushing strength dissipates rapidly. At 1,000° C, for example, the average compression strength of seven different commercial pellets was 110 lb; at 1,100° C, the hot strength was only 60 lb. After a rather sharp initial drop, the loss of strength with increase of temperature was gradual. There was no sudden collapse, nor any significant difference, in behavior of commercial pellets whether made from magnetite or hematite concentrates.

Jan 1, 1968

By L. A. Haas

A kinetic study of the carbon deposition reaction was undertaken by the Bureau of Mines as part of a broad investigation of metallurgical reactions in the iron ore blast furnace. The disproportionation of carbon monoxide on iron pellets was investigated at carbon monoxide pressures between 0.5 and 2 atmospheres (absolute) and temperatures from 400° to 1,075° C. Gas flow in the range from 0.25 to 0.85 standard liter per minute was found to have little effect on the reaction velocity. The addition of nitrogen and helium to caron monoxide exerted only a dilution effect on the rate of carbon deposition. However, an addition of 1 percent hydrogen increased the rate about 100 times. Small amounts of carbon dioxide in the inlet gas exerted little effect on the rate of carbon deposition. The maximum rate for carbon deposition in the first 2 hours occurred at 550° C. The apparent molar activation energies at various stages of the reaction were found to vary from 13 kcal initially to 36 kcal during the latter stages of the reaction. The reaction rate behavior was tentatively explained by an adsorption step followed by the diffusion of iron through a shell of inactive iron carbide.

Jan 1, 1968

By Israel Liebman

The Bureau of Mines conducted an investigation to determine those factors that are significant in affecting the velocity of flames propagating along the boundary separating gaseous fuel and air. In addition the aerodynamic motion of the gases in the vicinity of such interfacial flames was delineated. Parameters in the study included flammable zone thickness, flammable zone concentration of gradient, fuel type, and position of the flame relative to various environmental surfaces. Of all these factors, the flammable zone thickness and burning velocity of the stoichiometric mixture were found to have the most significant effect on the flame speed. Notion of the gases in the vicinity of the interfacial flames was examined by particle track and interferometric techniques. The relative velocity of the interfacial flame with respect to the unburned gas on the central streamline was found to equal the burning velocity of a stoichiometric homogeneous fuel-air mixture. In addition, it was observed that the composition of the lean fuel-air mixture at the boundary of the combustion zone appears to be less than that defined as the fuel's lower flammable limit.

Jan 1, 1968

By T. N. Rushton

Rate minima are encountered in the reduction of magnetite with hydrogen. In a certain temperature zone, the reaction rate decreases with rise in temperature. This is inexplicable by classical kinetic theories; neither is a transition in reduction mechanism suitable for interpreting the observed behavior, This anomaly can be fully explained by hypothesizing two species of chemisorbed hydrogen with different adsorption coefficients and activation energies for adsorption. Competition between two energetic states of adsorption occurs with temperature rise, with the low energy state predominating below the anomalous temperature zone and the high energy state above it. The presence of two possible adsorption sites appears to be characteristic for oxidic adsorbents.

Jan 1, 1968

By L. A. Neumeier

Sound experimental ingots of zinc alloys for use as rolling slabs were cast with a specially constructed, semicontinuous casting machine. Nominal alloy compositions of Zn-1.0 percent Cu, Zn-0.12 and 0.36 percent Ti, and Zn-1.0 percent Cu-0.03 to 0.36 percent Ti were cast. This Bureau of Mines study was conducted to evaluate the suitability of the casting procedure for providing stock for rolling into sheet. Microscopic examination of ingot sections revealed structures in which grain size varied from the outer to center ingot zones. Columnar grains present in the center zone of the Zn-1.0 percent Cu ingot were absent in the titanium-containing ingots. The ingots with titanium displayed a finer grain size and eutectic structure in the center ingot zone than in the outer zone; the transition in grain size between the two zones was quite abrupt in some ingots. The overall grain size of the titanium-containing ingots was finer than that of alloys cast by more conventional methods. Chemical analysis revealed that compositional segregation is not a significant factor in the formation of the ingot structure. Microstructural studies of small ingots of similar alloys solidified at slow, fast, and intermediate rates confirmed that the ingot structure in the semicontinuous-cast ingots is related to cooling rate, which is, in turn, related to the particular casting machine design and the influx of cooling water on the withdrawing ingots. Microstructures of thin sheet hot-rolled from slabs of the semicontinuous-cast ingots demonstrated that the ingot structure does not preclude the rolling of sheet having a uniform microstructure. Results of hardness surveys of the semicontinuous-cast ingots demonstrated that copper and titanium exert essentially additive hardening effects in these cast alloys.

Jan 1, 1968

By Perry N. Halstead

This report describes two goniometers that, by simple manipulation, can be used to ascertain the attitude of a joint, vein, or fracture plane observed on the planar projection of a borehole photograph taken with an NX borehole camera of the type developed by the U.S. Army Corps of Engineers. One goniometer was designed to interpret photographs taken in vertical drill holes and the other for photographs taken in inclined drill holes. In practice, several measurements are made on each photograph with the goniometer. These data are then substituted into mathematical equations, which are derived in this report and the attitudes of fracture planes are determined.

Jan 1, 1968

By M. R. Geer

The Bureau of Mines examined the washability data for 25 Appalachian coals requiring low-density washing to reduce sulfur content to 1 percent, using the distribution-curve method. The purpose was to estimate how closely theoretical sulfur values could be approached, what yields of washed coal could be expected, and the recovery efficiencies that might be achieved. Assuming that the run-of-mine coal would be crushed to 3/8 inch and cleaned in dense-medium cyclones, the calculations indicate that theoretical sulfur contents could be approached closely when cleaning at a specific gravity of separation as low as 1.30. With coals that have favorable specific gravity compositions the recovery efficiency anticipated for cleaning at 1.30 specific gravity is surprisingly high. Similar calculations for cleaning with concentrating tables at intermediate specific gravities indicated that theoretical sulfur contents at 1.50 specific gravity could be approached closely with some coals but not with others. The calculations suggest that operating a table at a specific gravity of separation much lower than about 1.50 probably would be unsatisfactory with most coals.

Jan 1, 1968

By Kenneth J. Miller

To determine the effectiveness of the many new flocculants available to the coal industry 20 of these reagents were evaluated treating slurry feeds to four refuse thickeners. Settling rates and supernatant liquid clarities were determined for each of the flocculants on the four slurries, and zeta potential measurements of the slurry solids were made. The test results showed that the flocculants provided comparable results when judged categorically as anionic, nonionic, or cattonic. It was also apparent that control of zeta potential insures maximum benefit from a flocculant.

Jan 1, 1968

By Raymond L. Lowrie

For many years it has been considered that an average of 50 percent of the coal in the deposits exploited has been recovered. Owing to many changes in mining methods during the past two decades, this study was initiated to obtain an up-to-date measurement of recovery percentage and thus establish part of the basis from which presently recoverable reserves may be estimated. Recovery percentages were determined within mined areas of 200 underground coal mines. These comprised a statistical sample selected to be representative of operating mines in relation to their significance to depletion of reserves. The results ranged from 29 to 91 percent and averaged 57.0 ± 1.7 percent (95-percent confidence limit). Six factors were identified mathematically as significantly affecting recovery percentages: (1) Pillaring system, (2) top rock and conditions, (3) bottom rock and conditions, (4) marketability, (5) coalbed thickness, and (6) productivity. Skill and attitude of mine operators toward recovery, although not measured, were probable factors. Five other variables that were tested did not show any significant relationship with recovery percentages. Also, five mining equipment features were identified, through discussions with mine officials, as affecting adversely recovery percentage at some mines.

Jan 1, 1968

By R. V. Higgins

This paper describes a method and a computer program for calculating shape factors and areas of channels that turn more than 90° and conduct fluids into the backs of wells. The program represents an improvement over a previous Bureau of Mines investigation by using a 4-point Lagrange interpolation equation instead of a 3-point and by summing areas of trapezoids with either x altitudes or y altitudes. Some of the techniques reported in this paper can also be used to compute the areas between contours and the lengths of lines that turn more than 90°.

Jan 1, 1968

By K. R. Dorman

To develop the potential of precast concrete sets as a support medium in underground mines, a three-piece precast concrete drift set was designed for a small opening and tested to destruction in an underground straining frame. Thirty-six tests were made with three sizes of members using three different loading conditions. In addition, 14 members were tested individually in the laboratory. Test results are compared with theoretical calculations. A cost comparison shows the use of concrete sets would be advantageous where conventional wooden timber requires excessive replacement.

Jan 1, 1968