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By Jerry L. Huiatt

An accurate and reproducible procedure was developed using the gas-liquid chromatograph to quantitatively measure oleic acid on flotation products and in flotation water phases. The method comprised extraction of the oleic acid from the mineral surfaces with alcoholic NaOH, esterification of the extracted oleate, and chromatography of the methyl ester with an internal standard. Quantitative analysis of oleic acid on flotation products from test tube and bench-scale flotation tests with pure minerals and with natural ores proved the applicability of the method on a variety of minerals. The accountability of oleic acid added was 100 percent, ±5 percent.

Jan 1, 1968

By John J. Henn

Ten proposed processes for the recovery of manganese from domestic resources as a high-grade oxide product are described. Nine of the processes employ sulfur dioxide, sulfuric acid, or a combination of both for leaching. The tenth process utilizes sulfur dioxide to sulfatize the ore at 600° to 850°C before water leaching. In addiction to these ten complete processes, six processes from the patent literature are described. Methods for receovering MnSO4?H2O are also reviewed.

Jan 1, 1968

By Wilbur I. Duvall

The Bureau of Mines presents a theoretical solution for the stresses and displacements in an infinite elastic plate containing a circular hole whose boundary is subjected to applied shear loads over four separated arcs. The results for the applied shear loads can be superimposed on the results for applied radial loads, given in a previous publication, to obtain a complete two-dimensional approximation of the stresses and displacements induced in the rock by tunnel boring machines anchored in a circular tunnel by means of four props. Analysis of the various solutions shows that the tangential tensile stresses induced on the boundary of the circular tunnel by applied radial loads can be minimized in the roof and floor of the tunnel by the application of appropriate shear loads to each of the four props. Thus when planning tunnel boring operations, consideration should be given to the in situ stress field in the rock and the induced stresses in the rock resulting from the applied radial and shear loads produced by the props of the boring machine.

Jan 1, 1968

By W. F. Hughes

The thermodynamics of an electromagnetic field-fluid interaction system is discussed. A review of the thermodynamics of linear media (the permittivity and permeability taken as functions of density and temperature) is presented; then an extension is made to nonlinear media (the permittivity and permeability taken as functions of the fields). Expressions for thermodynamic properties and reversible work are derived and the first law of thermodynamics for magnetohydrodynamic flow is discussed.

Jan 1, 1968

By R. W. Freedman

The gas chromatographic method, devised by the Bureau of Mines for analyzing routine mine air samples, was compared with the infrared method used for confirmatory determination of methane in mine air. While maintaining the specificity of the infrared method for methane determination, the gas chromatographic method is more precise, much more rapidly performed, and more convenient.

Jan 1, 1968

By M. J. Ferrante

The preparation and subsequent reduction of vanadium trichloride was investigated as a process for the production of high-purity vanadium metal. Chlorine was reacted with vanadium oxide in the presence of carbon to vanadium tetrachloride. The contaminant vanadium oxytrichloride was also formed and later converted to tetrachloride by reaction with chlorine in the presence of activated charcoal. Vanadium tetrachloride was stirred continuously during thermal dissociation to vanadium trichloride powder from which volatile contaminants were removed by distillation. The vanadium trichloride powder was reduced to vanadium sponge by controlled feeding of the trichloride into molten magnesium. Excess reductant and byproduct salt were removed from the vanadium sponge by high-vacuum distillation. Batches as large as 6.5 kilograms of sponge metal were prepared at an average reaction efficiency of 98 percent. Vanadium sponge after consolidation by arc-melting contained 820 to 11330 ppm of interstitial impurities and had a hardness between Rockwell B 40 and 70, This metal exhibited excellent workability at room temperature. The purification of impure vanadium metal by electron-beam melting resulted in lowering interstitial impurities from 1,890 to 504 ppm and hardness from Rockwell B 87 to 28.

Jan 1, 1968

By R. K. Koch

The vapor pressures of liquid molybdenum and liquid zirconium were determined by the Langmuir free-evaporation method. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. The vapor-pressure data led to the following equations: [log p (atm) = 5.429 - 28,380 T for liquid molybdenum in the range 2,890° to 2,990° K, and log p (atm) = 6.521 - 30,940 T for liquid zirconium in the range 2,229° to 2,795° K.] Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 157.6 ± 1.8 kcal/mole and 148.4 ± 2.4 kcal/mole for molybdenum and zirconium, respectively, where the uncertainties are two standard devia¬tions. Second-law standard heats of sublimation determined from sigma plots and tabulated enthalpies were 143.5 ± 2.7 kcal/mole and 149.2 ± 3.8 kcal/mole for molybdenum and zirconium, respectively. The better agreement in heats of sublimation for zirconium is attributed to the 566° K temperature range studied which permitted a more accurate definition of the vapor pressure curve than could be obtained from the 100° K span for molybdenum. This supposition was verified by making a sigma-prime plot which utilized solid vapor pressure data for molybdenum to extend the evaluation range by 800° K. This gave a standard heat of sublimation of 155.2 ± 1.6 kcal/mole which is in good agree¬ment with the third-law value. The plot also gave a standard entropy of sublimation (298.15° K) of 35.73 ± 0.48 eu.

Jan 1, 1968

By E. L. Litchfield

The electrification of ammonium nitrate-fuel oil (AN-FO) blasting agents by pneumatic loaders is described and discussed. The consequences of the electrification are considered in light of the initiation requirements of electric blasting caps. It is recommended (1) that semiconductive loading tubing be utilized and (2) that the resistivity of the AN-FO be controlled; it is further recommended that the operator (3) test to assure continuity of the electric detonator legwire-bridgewire-legwire circuit prior to insertion of the cap into charge or borehole, (4) keep the legwires shunted but not otherwise connected to ground during loading of the blasting agent into the borehole, (5) assure that the borehole is discharged prior to hooking up the detonator leads, (6) assure that he is himself discharged prior to handling the detonator leads, and (7) assure that the blasting cap leads are never carried to the AN-FO loader. The basis and significance of these recommendations are explained.

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 Leland E. Paulson

This investigation examined the feasibility of altering the inorganic component of North Dakota lignite by ion exchange. Lignite of specific size consist was washed with various ionic solutions and examined for evidence of exchange. Ions of higher valance substituted preferentially at equivalent concentrations. Results indicate that a major portion of the inorganic material associated with lignite is combined in exchangeable form with the organic component. Particle size of the treated coal is a critical factor in determining the rate of exchange. The data indicate that monovalent ions are easily replaced by divalent and trivalent ions, and the presence of ionic material in slurries containing finely divided lignite significantly increases filtration rates.

Jan 1, 1968

By A. G. Starliper

The Bureau of Mines made laboratory investigations to determine the feasibility of utilizing fine tungsten wires to reinforce a number of nonferrous metals and alloys and a superalloy, S-8l6. The composites of tungsten filament and metals were chosen to attain elevated temperature strength and corrosion resistance. Oriented clean or precoated tungsten wires were incorporated with the other metals by extrusion, swaging, and infiltration casting. Although widely varying characteristics were found in the composites, none were considered satisfactory for high-temperature use, chiefly because of reactions between the matrix metal-tungsten surface. Diffusion, solution, and chemical reactions between matrix and tungsten wires were sufficiently slow for some combinations, such as 15 v/o 8-816, to exhibit increased high-temperature strength for a limited time. A few metals failed to wet or bond to the tungsten surfaces, while a few responded after precoating with a third metal.

Jan 1, 1968

By Herbert R. Babitzke

The purpose of this investigation was to optimize the high-temperature properties of columbium and tantalum. Columbium and tantalum were combined with selected alloying elements to achieve solid solution and dispersion strengthening. Fifty-six alloys were evaluated to determine their formability, hardness, strength at elevated temperatures, and oxidation resistance. The following six alloys showed high-temperature strength: [Cb-15Hf-5W-2Zr-4Al-4Ti-2N Cb-15Hf -5W-5Zr Cb-15.3Ti-4.1Zr-13.7Hf Ta-20Hf-4Al Ta-30Hf-4Al Ta-20Hf-5W-4Al] At 1,200° C, the columbium alloys had strength values of 40,000 psi or greater, and the tantalum alloys had strength values from 50,000 to 58,000 psi. For a 2-hour test period at 1,000° C, weight gains of only 9 and 8 mg/cm2, respectively, were observed on oxidation testing of two alloys, Cb-15Hf-5W-2Zr-4Al-4Ti-2N and Ta-20Hf-5W-4Al.

Jan 1, 1968

By Richard L. Jenkins

Systematic sampling, in reconnaissance fashion, of the continental shelves of the United States to define favorable areas of offshore mineral deposits, is one of the long-range marine mineral; programs of the U.S. Department of the Interior. In mid-1966 the Department of the Interior launched its Heavy Metals Program to stimulate domestic output of gold which is in serious short supply. The program is jointly conducted by the Geological Survey and the Bureau of Mines.

Jan 1, 1968

By B. J. Dalton

This report gives general expressions for evaluating various thermo-dynamic properties applicable to a two-component system, including liquid-vapor equilibria. In addition, expressions are developed for some of the quantities useful in making thermodynamic consistency checks on phase equilibria data. These formulas were developed from the general principles of thermodynamics and are expressed in terms of the compressibility factor, which is assumed to be an explicit function of the molal density, the absolute thermodynamic temperature, and the composition.

Jan 1, 1968

By W. J. Wenger

Results of the analyses of 151 crude oils from 123 oilfields in the Williston basin are presented. Production statistics are compiled by geographical areas within the basin, by geological age of the producing zones, by States, and by field for the nine fields with the greatest production. Characteristics of the oils are tabulated, and correlations are included to show relationships between properties of the oils and some factors in the environment. Properties of the oils in some instances imply that there has been migration and mixing of the oils between productive formations of different geological time periods.

Jan 1, 1968

By E. Morrice

Techniques developed by the Bureau of Mines for the preparation of high-purity rare-earth metals and their alloys by electrolysis of the oxides in fluoride media are summarized. Cerium, lanthanum, neodymium, praseodymium, dysprosium, gadolinium, and yttrium metals, the mixture didymium, and specific alloys of these metals and samarium with iron, nickel, chromium, and cobalt were prepared. Individual metals were electrodeposited in the liquid state on tungsten or molybdenum cathodes. Alloys were prepared by electrodepositing the rare-earth metal on a consumable cathode, at a temperature above the melting point of the eutectic formed between the rare-earth element and the cathode material. Cells were designed for electrowinning metal products in gram and pound quantities, and methods for continuous electrowinning of cerium and lanthanum were developed.

Jan 1, 1968

By H. V. Makar

Laboratory tests were performed to obtain a quantitative description of the effectiveness of sodium sulfate (Na2SO4) for removing copper from molten iron and to determine the effectiveness of Na2SO4 on actual auto scrap. The tests were conducted on induction melted heats of iron averaging 0.58 and 1.50 percent initial copper and on cupola-melted auto scrap containing 0.45 percent initial copper. The Na2SO4 was added in powder form in amounts ranging from 2.9 to 43.8 percent of the weight of iron being treated. The data showed that copper removal for the various Na2SO4 treatments followed a similar trend, regardless of the iron composition that was tested. The equation Y = 1 - e-3.23x approximately reflects the relationship between copper removal and amount of Na2SO4 added, where Y is the fraction of copper removed and x is the ratio of the weight of Na2SO4 added to the weight of metal treated. Copper removals ranged from 3.3 to 74.5 percent and reductions down to less than 0.10 percent final copper were achieved in the auto scrap. Copper removals were generally accompanied by sulfur removal, and initial sulfur contents ranging from 0.10 to 0.20 percent were reduced to as low as 0.02 percent. High temperatures and long slag reaction times tended to induce copper and sulfur reversion from the slag, but, generally, the Na2SO4 treat¬ments were effective up to approximately 2,820° F with reaction times not exceeding 7 minutes.

Jan 1, 1968

By W. L. Eaton

This report is the second in a series concerning the Bureau of Mines program for microfilming maps of abandoned mines in the Pennsylvania anthracite region; a catalog of the microfilmed maps of mines in the Wyoming Basin of the Northern anthracite field is presented. The first report I.C. 8274, published in 1965, was a catalog of microfilmed maps of mines in the Eastern Middle anthracite field. Additional catalogs will be published as the microfilming of significant mining areas is completed.

Jan 1, 1968

By D. S. Burgess

The characteristics of gas-phase detonations were observed in 20 instrumented firings within earthen tunnels, in 100 such detonations in a 24-in-diam by l63-ft-long steel pipe, and in about 200 smaller scale firings. Most of the fuels studied were representative hydrocarbons--acetylene, propane, gasoline, and a roughly equimolar mixture of methylacetylene, propadiene, and propane. In a pipe with two closed ends, the detonable limits were demonstrated to be very nearly the same as reported limits of flammability. The side-on impulses (pressures integrated over 200-msec intervals) were shown to be the same function of concentration regardless of whether deflagration or detonation had occurred. In a pipe with only the initiation end closed, the impulses of all fuel-air systems tended toward the same level when averaged over comparable ranges of fuel concentration; the lower pressures with saturated hydrocarbons were nearly compensated by longer durations of pressure transient. In all fuel-air systems, unexpectedly high impulses were obtained with slightly lean mixtures. In earthen confining structures, the impulse, of the explosion was efficiently converted into momentum of the failing wall. In the configurations studied, an earth velocity of about 20 fps was critical to overcome the soil's resistance to shear. The destructive effect was determined by gas pressure rather than by total energy release. The assignment of a "TNT equivalent" to an explosive gas mixture is discussed in terms of the confinement of the mixture.

Jan 1, 1968

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of Clarion County, Pa. Of the 15 samples collected, 1 was of metallurgical quality as received, 4 could be sufficiently upgraded to provide acceptable products, and the remaining 10 samples could not be upgraded to metallurgical quality because their sulfur contents could not be lowered to meet the standard. For steam or power generation, 1 sample was of low sulfur content as received, 1 sample could be upgraded to low sulfur content, and 10 samples could be upgraded to medium sulfur content. The original sulfur content of the remaining three samples can be appreciably reduced by removal of the sink 1.58 specific gravity material; however, these coals would be classified as medium sulfur coals both before and after removal of the sink material.

Jan 1, 1968