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By H. R. Babitzke

As part of a continuing project to develop refractory metal alloys for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation strengthening techniques to improve the properties of columbium alloys. The purpose was to investigate the effects of hafnium, tungsten, and boron on the formability, strength, and oxidation resistance of columbium. The experiment was of factorial design with two replications which called for 72 ingots of 36 basic compositions, weighing 150 grams each. Hafnium, tungsten, and boron were evaluated at 3, 3, and 4 levels, respectively. Values of alloy content are all in atomic percent. The highest strength observed was 29,000 psi at 1,200° C for alloys Cb-15Hf (No. 3), Cb-7.5Hf-5W-2B (No. 14), and Cb-15Hf-5W-2B (No. 15). At 1,200° C, the ternary alloy Cb-15Hf-5W (No. 6) which has shown good properties in previous Bureau of Mines investigations was the most resistant to oxidation For boron additions, the alloys oxidized more readily with increasing amounts of this element. The fabricability of the alloys high in boron became increasingly difficult, resulting in an inadequate number of alloys required for a complete statistical analysis for all the tests. As a result of the decrease in ductility, an insufficient quantity of tensile samples were available for a proper analysis for the high-temperature strength data.

Jan 1, 1970

By A. Aly Selim

This report describes the feasibility of predicting percussive drilling rates by equations derived from statistical regression analysis. The least squares statistical method was used and the analysis was performed both by direct and by stepwise linear regression analysis. The predicted penetration rate is a function of the drill power and the physical properties of the rocks penetrated. The results show promise that the technique may be of value in providing a mathematical model by which percussive drill manufacturers and users can predict the performance of a given drill. Experimental work involved two mining type percussive drills. Penetration data for these drills were determined from nine rocks drilled in the laboratory. Drill work rates (power) were determined in a separate series of experiments. Rock physical properties were measured from diamond-drill core samples taken from the same blocks used for percussive drilling.

Jan 1, 1970

By P. T. Brooks

Semipilot scale tests were made to demonstrate a newly developed electrorefining process which could be extrapolated to commercial scale in producing high-purity nickel and cobalt from crude nickel metal and high-grade ferronickel. The new process comprises application of solvent extraction techniques to remove and separate cobalt and iron from nickel and the electrodeposition in diaphragm cells of pure nickel and cobalt from chloride-based purified electrolyte. Using water insoluble organic amines, the solvent extraction operations enabled production of commercial-sized nickel and cobalt cathodes of higher purity than that of commercial electrolytic metals. The solvent extraction operation for separation of cobalt from nickel was made simpler than the conventional method. Furthermore, the solvent. extraction operation for iron removal made possible the electrorefining of ferronickel without the prohibitive loss of nickel resulting from the method ordinarily used for iron removal.

Jan 1, 1970

By Robert E. Wood

The temperature dependency of the low-density viscosity coefficients, ?°T, of helium and of nitrogen, 100° to 1,000° K, is correlated with empirical equations, and the temperature and composition dependencies of the low-density viscosity coefficients, ?°T, of helium-nitrogen mixtures are correlated with the Chapman-Enskog expressions by using the Lennard-Jones (6:12) potential function. The residual viscosity, ?T,P - ?°T (the difference between the viscosity of a compressed gas and the dilute gas at a given temperature), was found to be a function of the thermal pressure coefficient, (?P/?T)V, and two parameters, a and 1, which are characteristic of gas composition. The equation ?T, P = ?°T + a [(?P/?T)V]ß represented 1,340 higher pressure experimental viscosity values with a mean absolute deviation of 0.86 percent, and this equation was used to compute viscosities of the gaseous helium-nitrogen system for a range of temperatures and pressures including those encountered in Bureau of Mines helium purification processes and in a crude-helium conservation gas reservoir. Tabular viscosities for helium, nitrogen, and 13 helium-nitrogen mixtures are presented for 110 temperatures, 133° to 740' K, and 49 pressures in the range 1 to 240 atmospheres. The accuracy of the tabulated viscosities varies because correlation parameters were obtained from experimental data of unequal reliability. It is estimated that uncertainties in the computed viscosity values are ±5 percent for the region 325° to 740° K, ±2 percent for the region 183° to 325° K, and ±5 percent for temperatures below 183° K. The latter uncertainty may rise to y10 percent as critical conditions are approached.

Jan 1, 1970

By Jack I. Paige

In this Bureau of Mines study, two fluidized-bed reactors were designed, built, and operated, one as a sorber for S02 and the other as a contactor for the regeneration of the sulfur-laden alkalized alumina. The target of 90 percent removal of S02 from a flue gas stream containing 0.3 percent S02 was attained by using a sorbent feed of 10-15 grams per minute into a 5-inch bed depth of alkalized alumina. The sorption unit was operated at about 330° C. Complete regeneration of the laden alkalized alumina containing 5 to 10 percent sulfur was accomplished in approximately 1/2 hour. An excess of reformed propane at about 730° C was the regenerating gas. Attrition losses, a major problem with this sorbent, ranged from 0.9 to 7.9 percent of the inventory. Data from these tests demonstrate, within experimental error, the validity of equations developed from short-term, thin-bed tests related to sorption and regeneration rates.

Jan 1, 1970

By B. D. Sartwell

Multiple-charged beams originating from a 300-kv ion accelerator are important tools in the study of metal surfaces and thin films. A knowledge of the particle range is necessary for an understanding of the interaction processes of the ions with the targets. Utilizing a theory developed by Lindhard for determining the range of low-energy ions in solids, the ranges of H, He, C, N, 0, and Ar ions in A1203, Al, Fe203, Fe304, CuO, Cu20, Fe, Cu, Sn, and W were calculated for the energy range 60 to 400 kev using a computer program written in BASIC. The range, presented in graphical form, is given in both µg/cm2 and angstroms. In addition, heavy ion ranges were calculated for comparison with published experimental values. For ions with Z > 5, the discrepancy between the calculated values and published experimental values generally ranged from 2 to 40 percent; the largest deviations were probably due to experimental error.

Jan 1, 1970

By K. J. Miller

A laboratory electrophoresis column was designed to separate pyrite from fine coal by utilizing an observed difference in the electrophoretic mobilities of the two materials in water. The apparatus worked well when tested with synthetic mixtures of coal and pyrite, but some modifications in design and procedure were necessary to provide a sharper separation. After these changes were made, the column was tested with a high-pyritic-sulfur raw coal sample. The column successfully fractionated the sample, removing not only the pyritic refuse, but a siliceous refuse as well. The invest ion demonstrated on a laboratory scale that pyrite and other impurities can be separated from fine coal by electrophoresis.

Jan 1, 1970

By D. S. Burgess

An investigation of the hazard of spillage of liquefied natural gas (LNG) onto water is described. About 2,000 gallons of LNG were consumed in various tests. The initial vaporization rate of LNG following spillage was found to be 0.037 lb/ft2 sec; when the spill was confined, this vaporization rate was moderated after about 20 seconds by the growth of an ice layer on the water surface; when the spill was unconfined, a coherent ice floe was not observed and the vaporization rate was essentially time independent. The maximum diameter (in feet) of the spreading LNG pool was found to be given by 6.25 Wo 1/3, where Wo is the weight of LNG in pounds, Downwind of a natural gas source, time-averaged methane concentrations were given in good approximation by standard air pollution equations. However, peak concentrations were as much as twentyfold higher than average, adding an additional factor to the assessment of hazard. The effect of layering by the cold vaporized natural gas was similar to the effect of a temperature inversion on normal gases in the atmosphere. Small-scale explosions were observed on pouring LNG onto a water surface; no single explanation seems pertinent to all of the incidents observed.

Jan 1, 1970

By E. F. Ferrell

Electrowon molybdenum powders and a commercial hydrogen-reduced powder, all with different minor impurities, were investigated by the Bureau of Mines with respect to inherent properties, to fabrication techniques, and to proper-ties of the fabricated sheet. Compared with the commercial hydrogen-reduced powder, the electrowon powders had a larger particle size, a greater flow rate, a higher apparent density, and a lower oxygen content. Sheet materials prepared from the two types of powders showed similar mechanical properties, under the same conditions of heat treatments, except for low-temperature ductility. Yield strengths varied with carbon content, heat treatment, and test temperature.

Jan 1, 1970

By Alfred E. Schwaneke

A versatile torsion creep tester was instrumented with electromechanical and servomechanical components to operate automatically and unattended, producing digital printed outputs. The apparatus uses an electrical system for applying torsional stresses, and a unique angular transducer as a null detector operating a servocontrolled strain measuring system with the digital readout. The tester is designed to measure the creep in single-crystal or polycrystalline zinc, zinc alloys, magnesium, magnesium alloys, or other metals and alloys. Applied stresses may be varied from zero up to 2,000 psi in the outermost fibers of a 1/8-inch-diameter, 4-inch-long specimen. Strain readings to 0.001 degree, equivalent to a strain of 2.73 X 10-7, may be made automatically from one every 5 seconds to one per month. The apparatus has provisions for programed temperature control and special atmospheres or vacuum operation. A discussion of applications of the system to other mechanical testing apparatus is included.

Jan 1, 1970

By C. Daniel Kealy

Finite-element,, mathematical models that solve LaPlace's and Richard's equations numerically were used to locate the phreatic surface within tailings pond embankments and to define the subsurface flow of water from the pond. Both must be known to design structurally and environmentally safe tailings dams. The permeability distribution within and beneath the embankment, the fluid potential values upgradient and downgradient from the embankment, and the geometry and elevation of an approximately impermeable layer at some depth beneath the embankment were used as computer inputs in analyzing over a dozen finite-element models of tailings dams varying structurally from simple to complex. Results predicted with the finite-element model were confirmed with measurements in a laboratory model of a tailings pond and in the field. Of particular importance to the design of safe slopes, all data indicated that the phreatic surface within a tailings dam is concave upward, a configuration opposite that in most earth dams. The close correlation between predicted and experimental values confirmed the practicability of using the finite-element technique to design safe tailings dams.

Jan 1, 1971

By C. Kenneth Eilerts

A method is described for controlling instability in finite-difference computations of liquid saturation near the borehole of a recovery well. Differences of pressure-and saturation-dependent variables are indexed offcenter, upstream and downstream alternately, to provide a stabilizing average. It was found that size of the time step could be increased by a factor of 4 without loss of numerical stability. Finite differences of the variables occur in a variety of relative numerical sizes and combinations. Those relationships of the differences that contribute to instability may be identified by the computing program in which they occur and modified to assist convergence of the computations and execution of the partial differential equations of liquid and gas flow.

Jan 1, 1971

By Robert M. Doerr

The research objective was to determine the effect of aluminum alloy additions on the oxidation behavior of cobalt-nickel alloys. Thirty high-purity alloys were reacted with 02 at 0.5 atm at 1,351°, 1,389°, and 1,429° K in a volumetric apparatus for about 300 min. The alloy compositions consisted of Co-Ni master alloys (0, 22, 50, 70, 91, and 100 wt pct Ni) with aluminum additions of about 0, 1, 2, 4, and 8 wt pet. Large early deviations from, or changes in, the parabolic rate constant were encountered, but in most cases, the reaction rate declined approximately in accordance with the parabolic rate law. A sharp peak in the parabolic oxidation rate constant was observed for specimens containing a to 22 percent nickel and 1 to 2 percent aluminum at 1,351° K, and the rate constants for these compositions were lower at the higher temperatures. Specimens containing 8 percent aluminum reacted far more slowly than did any of the others.

Jan 1, 1971

By Foster Fraas

Calculations based on data related to the electrostatic precipitator illustrate the variation in the electric forces on a particle with change in position in the ionized field. The feeble forces in some separators are explained by the low field intensity at midpoint locations between the electrodes. When the particles are in contact with the exterior surface of a rotating cylindrical electrode, a high field intensity at the electrode surface combined with the image charge results in large electric forces. The permissible feed velocity increases as the square root of the electrode diameter, providing high values in efficiency and feed rate capacity, particularly in surface-to-mass ratio separations such as are encountered in secondary materials recycling operations.

Jan 1, 1971

In 1962 and 1963, two in situ combustion pilot tests were conducted in the shallow Second Venango sand near Reno, Pa. Because of poor oxygen utilization and lack of production response, both tests were considered failures and were terminated. The area was then relatively inactive until late 1966, when a development well drilled near the 1963 test site had surprisingly good production in what was considered to be a pressure-depleted reservoir. Other wells drilled in and around the old thermal pilot areas also came in as good oil producers. This report presents a study of the increased oil production from the Second Venango sand in the Reno area, and the apparent connection of the present production response and the old thermal pilot tests. Apparently combustion occurred in the Second Venango sand after the 1962 and 1963 experiments were terminated and, supported by large volumes of air left in the reservoir after the 1963 test, generated carbon dioxide which helped repressure the formation. This field evidence of combustion warrants another pilot experiment to further explore the use of properly designed in situ combustion techniques in increasing production from the Second Venango sand.

Jan 1, 1971

By R. V. Higgins

The results of two separate but related studies are given. In the first study, four equations were tested; the object was to determine which would produce a curve that would best fit data points that represent a trend of declining oil production in 90 California fields. Two conventional equations (the Arps and semilog) and two novel equations (extreme-c and double semilog) were tested. The curves were first fitted to the initial 9 years of the 15-year production data and then extrapolated for 6 years to determine how well the extrapolated curve would fit the data points. The generated curves were also extrapolated beyond the last data point to predict rates of future production. The results of the first study showed that no equation was clearly superior to the others in all respects. The semilog equation resulted in the best fit to production data for the first 9 years, but the Arps and extreme-c equations produced a better fit for the extrapolated data for the period of 9 to 15 years. The Arps and extreme-c also gave more realistic production rates when extended to the point where cumulative production equaled reserves. A second study was made to determine if the least-squares technique applied to the Arps equation would result in more accurate extrapolations. The merits of the logarithmic and the nonlogarithmic forms of the Arps hyperbolic equation were also tested. For the logarithmic expression, it was found that one of the constants of the Arps equation reached a value so small or so large that the equation was not applicable to the data of 40 of the 90 California fields. The nonlogarithmic form of the Arps equation was applicable to neither the same 40 fields nor to a few additional ones. When the data and the Arps equation were compatible, the use of the least-squares technique as compared with other methods improved the extrapolation accuracy somewhat.

Jan 1, 1971

By T. T. Campbell

Studies were conducted by the Bureau of Mines to develop a process for preparing thorium-magnesium master alloys or pure thorium metal by magnesium reduction of thorium tetrachloride in a semicontinuous reactor. Thorium tetrachloride was prepared in a fluidized-bed reactor by chlorination of thorium oxide or thorium oxalate. Conditions were established for producing a suitable thorium oxide feed for a fluidized-bed reactor. Thorium tetra-chloride was purified by vacuum sublimation and subsequently reduced by magnesium in a semicontinuous reactor to form thorium-magnesium alloys. Relatively pure thorium was produced by removing magnesium from the alloys by vacuum sublimation. Close to 100 percent of the thorium fed into the reactor was recovered either as metal (~93 percent) or as thorium oxide (~7 percent). The oxide can be recycled directly into the process.

Jan 1, 1971

By William G. Pariseau

A small displacement-small strain finite element technique utilizing the constant strain triangle and incremental constitutive equations for elastic-plastic media that are nonhardening and obey a Coulomb yield condition has been applied to the analysis of gravity flow initiation in a V-shaped hopper containing a powder under lunar environmental conditions. Three methods of loading were examined. Of the three, the method of computing the initial state of stress in a filled hopper prior to drawdown by adding material to the hopper layer-by-layer is superior (as expected). Results of the analysis of a typical hopper problem show that the initial state of stress, the elastic moduli, and the strength parameters have an important influence on material response subsequent to the opening of the hopper outlet.

Jan 1, 1971

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 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