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By G. H. Keith

The Bureau of Mines determined the mechanism(s) involved in observed anomalous changes in mechanical properties of vanadium-base alloys. Tensile properties of electrorefined and commercial-purity vanadium-base alloys containing up to 5 atomic percent molybdenum or titanium were measured between 77° and 673° K. Snoek oxygen and nitrogen peak heights were measured to determine the changes in dissolved interstitial content caused by increasing quantities of solute. In addition, changes in lattice parameter were followed wit: precision X-ray techniques. Softening, observed in alloys containing titanium, is explained by the formation of a second-phase titanium compound with oxygen or nitrogen. However, because of partitioning of titanium between compound formation and solid solution formation, about five times the stoichiometric amount was required for complete reaction. Addition of 1 percent titanium drastically lowered the strengthening due to strain aging, at 673° K, and 2 percent titanium essentially eliminated it. All alloys were ductile at 77° K. Variations in the tensile properties of the molybdenum-containing alloys are explained by variations in the amounts of interstitial impurities present. The molybdenum did not react with these impurities and had no effect on strengthening due to strain aging. Commercial-purity vanadium alloys containing more than 2 percent molybdenum were brittle at 77° K.

Jan 1, 1969

By Ralph B. Adair

The Bureau of Mines conducted laboratory and continuous pilot plant flotation tests to determine the feasibility of recovering commercial-grade mica from an Alabama graphitic-mica schist. Preconcentration of the ground ore on a Humphrey's spiral was employed to reject the heavy minerals and part of the quartz in a product virtually free of mica. The acid-cationic mica flotation process recovered over 89 percent of the mica in a product containing 98.7 percent mica. Grinding of the mica concentrate in a fluid energy mill produced a product with a bulk density of 12 lb per cubic foot.

Jan 1, 1969

By P. C. Good

The Bureau of Mines conducted a laboratory investigation of a sinter-leach method to recover aluminum and fluorine from waste carbon potlining residues from secondary cryolite recovery operations in aluminum reduction plants. After removal of carbon by burning, the residue was sintered at 900° to 1,100° C with silica and N2CO3, then crushed and leached with dilute NaOH solution, dilute Na2C03 solution, water, or water containing residual Na2O which remained in the sinter after reaction and decomposition of Na2CO3. Over 90 percent of the contained aluminum and up to 87 percent of the contained fluorine were extracted from this waste product in the form of a mixed alkaline solution. Treatment of the alkaline solution with CO2 yielded a white precipitate containing 89 percent of the original aluminum and 61 percent of the original fluorine as a mixture of synthetic cryolite and alumina, together with a variable excess of soda.

Jan 1, 1969

By J. E. Murphy

The high-purity thorium metal was prepared by the Bureau of Mines from electrolytically produced thorium alloys. The thorium-chromium and thorium-manganese alloys were separated into the component elements by vacuum distillation. Chromium and manganese impurities remaining in the thorium metal after distillation at 1,850° C were <0.005 weight-percent. Removal of volatile impurities such as aluminum, calcium, magnesium, and lead was also accomplished.

Jan 1, 1969

By R. L. Crosby

The Bureau of Mines investigated alloys of copper with 2, 3, and 4 vol pct alumina and with 2 vol pct yttria. Alloys were prepared by a coprecipitation process and were fabricated by pressing and sintering of powders, extrusion, and swaging. Tensile properties at room and elevated temperatures, stress-rupture strength, electrical conductivity, and density were measured. The superiority in elevated temperature strength of dispersion-strengthened copper to OFHC copper was confirmed. Increasing the oxide content from 2 to 4 vol pct produced only a small improvement in strength properties and decreased the electrical conductivity. The 3 vol pet alumina alloy had the best overall combination of properties.

Jan 1, 1969

By P. G. Clites

The Bureau of Mines developed techniques for induction melting of titanium in a split, water-cooled copper crucible. Calcium fluoride, which was used as an inert slag cover during melting, formed an insulating layer of solid slag between the ingot and the crucible wall. This thin layer of slag effectively insulated the ingot from the crucible and prevented the molten metal from shorting across the slits between adjacent segments of the crucible. The technique provides a means of melting loose titanium sponge and scrap and eliminates the need for fabricating a consumable electrode. This report describes the equipment developed and compares ingots produced from two varieties of titanium sponge, from titanium scrap, and from previously melted titanium with ingots prepared by vacuum-arc melting and electroslag melting. A melting scheme was also proposed and evaluated whereby loose titanium sponge was consolidated into a first-melt ingot for vacuum-arc remelting.

Jan 1, 1969

By Carl F. Wingquist

In support of Bureau of Mines studies of thermal fragmentation of rock, the elastic moduli of four types of rock were measured at temperatures ranging from room temperature up to 1,500° F (1,089° K). The sonic method was employed to determine the resonant frequencies of the rock specimens and from these frequencies, the elastic moduli were calculated. Data for Young&apos;s modulus, shear modulus, and Poisson&apos;s ratio are given as a function of temperature for Dresser basalt, Reserve taconite, Jasper quartzite, and Charcoal granite. Young&apos;s modulus and the shear modulus decreased with increasing temperature up to about 1,200° F and then became relatively insensitive to temperatures from 1,200° to 1,500° F.

Jan 1, 1969

By R. K. Koch

The vapor pressures of liquid titanium and liquid platinum were studied under the Bureau of Mines program for the determination of thermochemical data on the transition elements. Beating was done in a 2-kw electron-beam furnace with a water-cooled copper crucible to contain the melt. Temperature was measured with a disappearing-filament brightness pyrometer. The vapor pressure data for liquid titanium in the range 2,008° to 2,379° K are represented by the least-squares derived equation [log p (atm) = 6.268 - 22, T] Two series of determinations were made on liquid platinum. Results of the first series are expressed by the least-squares derived equation [log p (atm) = 8.240 - 30,460T] for the range 2,0860 to 2,4200 K. Results of the second series are expressed by the least-squares derived equation [log p (atm) = 7.795 - 29,580 T] in the range 2,045° to 2,442° K. Third-law evaluations of each series gave mean standard heats of sublimation of 112.4 kcal/mole, 133.3 kcal/mole, and 133.8 kcal/mole for titanium first series on platinum, and second series on platinum, respectively. Second-law heats of sublimation and equations for heats, free energies, and entropies of vaporization were obtained from sigma plots of each data set.

Jan 1, 1969

By L. B. Pankratz

The Bureau of Mines determined low-and high-temperature thermodynamic properties for anhydrous ferric sulfate and anhydrous indium sulfate. Low-temperature heat capacities were measured between 50° and 298° K, and enthalpy increments above 298° K were determined. The high-temperature measurements of Fe2(S04)3 extended to 900° K and those of In2(S04)3 to about 1,000° K. A minor transition was found for Fe2(S04)3 at 800° K, with a heat of transition of 540 cal/mole. Tabulations were made of the low-temperature heat capacities and the high-temperature enthalpy and entropy increments. The 298° K entropies derived from the low-temperature measurements were 67.6±0.S ca1/deg mole for ferric sulfate and 72.2±O.5 cal/deg mole for indium sulfate. High-temperature enthalpy increments were also given in equation form.

Jan 1, 1969

By R. S. Fowkes

The Bureau of Mines constructed a fully automated pilot plant facility to study the hydraulic transportation of solids through a lock hopper feeder system. An equation for the energy requirements to transport coarse solids hydraulically proved applicable to this system. Optimum velocities were obtained for limestone, mine refuse, and bituminous coal. The experimental data, calculations, and graphs show the effect of velocity, specific gravity, and solids concentration on head loss and power requirements. Other data were obtained and evaluated to determine the effect of particle size on head loss. Results also are given for (a) tests using friction reducing polymers; (b) tests using seven test sections of steel alloy pipe to determine their wear characteristics; (c) tests to determine spatial segregation of moving particles; and (d) tests to determine the effect of shape, size, and specific gravity on particle velocity in a horizontal pipeline. The lock hopper feeder system was found practical for continuous hydraulic transportation of the material types and size ranges tested.

Jan 1, 1969

By Ted C. Briggs

The Bureau of Mines is evaluating the thermodynamic properties of helium and helium-containing mixtures. Twenty-two compressibility runs were made with helium at 0° C and pressures to 800 atmospheres using a Burnett-type apparatus. Data from the 22 runs were treated simultaneously and as separate runs while different functional forms and weighting factors were used. A fourth-degree-polynomial equation in the pressure gives a statistically satisfactory representation of the compressibility factor when the data are treated simultaneously and a weighting factor of Pr-3/4 is used. The second virial coefficient of helium at 0° C from this investigation is 11.997±0.015 cm3 mole-1. The stated uncertainty is the random error standard deviation. Compressibility factors determined by this investigation are precise to better than 0.01 percent and are believed to be accurate to better than 0.02 percent.

Jan 1, 1969

By Danton L. Paulson

Elevated temperature electrical resistivity measurements were made by the Bureau of Mines on arc-melted, spin-cast, and hot-pressed columbium carbide¬carbon (CbC-C) and zirconium carbide-carbon (ZrC-C) materials up to 2,000° C. The CbC-C materials displayed electrical resistivity values ranging from 35.20 microhm cm at 23° C for hot-pressed material containing 12 wt pct carbon to 242.64 microhm cm at 1,622° C for arc-cast material containing 17.0 wt pct carbon. Electrical resistivity values ranged from 29 microhm cm at 20° C for arc-cast ZrC-C containing 16 wt pct carbon to 279 microhm cm at 1,951° C for hot-pressed ZrC-C containing 21 wt pct carbon. Data from a previous report were included to establish comparison between the electrical resistivities of the CbC-C, ZrC-C, and HfC-C systems.

Jan 1, 1969

By L. C. George

The Bureau of Mines measured the vapor pressures of selected mixtures in the binary systems CdCl2 ?SnCl2, CdCl2 -ZnC12, PbCl2 ?SnCl2, and PbCl2 -ZnCl2 by the static pressure method. These data were evaluated by the second-law (sigma-plot) method. Equations expressing the vapor pressures and the heats and free energies of vaporization as functions of temperature are given.

Jan 1, 1969

By Hillary W. St. Clair

This report describes a mathematical procedure for analyzing size distribution data by the method of moments. The method was applied to Andreasen&apos;s data on a variety of grinding mill products. It was found that the observed size distributions could be represented by gamma and beta distribution functions over a wide range of sizes. A computer program, written in BASIC, is described for calculating moments, distribution parameters, and the weight fraction in any size range.

Jan 1, 1969

By B. J. Dalton

The Bureau of Mines Helium Research Center has as a long-range objective the development of an equation of state for helium that will allow all of the thermodynamic properties to be calculated within the accuracy with which they are known. If this objective is to be realized, a method of calculation must be known. This report gives the principles of the method we use in such problems. A computer program was developed for predicting these properties, including those at the critical point, that is perfectly general and applicable to any equation of state. To demonstrate the efficacy of our method, this computer program was used to evaluate thermodynamic properties of a Redlich-Kwong fluid in the two-phase region. Expressions for calculating various thermodynamic functions specific for this particular equation of state are derived. Numerical values are tabulated and graphs are presented for all functions calculated. It is shown that for a Redlich-Kwong fluid there are finite discontinuities in (1) the second temperature derivative of the Gibbs free energy or chemical potential at the critical point, (2) the second derivative of the vapor pressure curve with regard to the temperature on passing through the critical point, and (3) the measured heat capacity at constant volume on passing through the critical temperature when the calorimeter is filled to the critical density. It is also shown that the heat of vaporization is infinite for a Redlich-Kwong fluid at absolute zero.

Jan 1, 1969

By D. H. Chambers

The Bureau of Mines developed a process for producing high-purity zinc and tin by electrorefining from liquid amalgams. Commercial grade metals were dissolved in mercury to produce saturated amalgams at room temperature. Amalgams were also prepared by electrolytic transfer from soluble anodes of the metals to a mercury cathode. Amalgams formed by both methods were used as anodes in electrorefining cells to produce high-purity cathodes. Metal impurities, excluding mercury, were at levels of less than 5 ppm in zinc and 9 ppm in tin. Mercury content was about 2 to 10 ppm in zinc products, and this was effectively removed by heating the cathodes in a vacuum. Mercury was excluded from tin cathodes by pumping the tin electrolyte through tin turnings and controlling the cell temperature.

Jan 1, 1969

By P. T. Brooks

This Bureau of Mines study describes a process for recovering nickel, cobalt, molybdenum, and chromium contained in complex waste superalloy grindings that, for lack of an economical domestic recovery process, are being largely marketed abroad. The process, devised by laboratory scale operations, includes scrap preparation, dissolution of metallics in hot chlorinated acidic liquor, carbon adsorption, three successive solvent extraction separations, and selective chemical precipitations. Nearly 90 percent of the nickel, cobalt, molybdenum, and chromium were separated and recovered as oxides, carbonates, and basic sulfate products.

Jan 1, 1969

By Jack L. Henry

The ternary system A14C3-AIN-Al203 has been examined to determine compositions which may display desirable high-temperature refractory properties. Powder methods were employed in the synthesis of all test compositions. Forming and sintering behavior was examined and hot-pressing parameters were measured. Several properties were studied for each composition of interest in the system. The properties included hydrolysis rate in moist air, elevated temperature oxidation rate, density, softening point, tensile strength, and rupture strength. In most cases equilibrium was not achieved, and the data are representative of a nonequilibrium system. Approximately 16 separate phases have been observed in the system. Forming behavior and selected properties of five compositions of interest were compared with those of aluminum oxide and aluminum nitride. None of the compositions compared favorably. Oxidation and vaporization appear to be serious drawbacks to the use of these compositions at elevated temperatures.

Jan 1, 1969

By E. G. King

Heats of formation of three crystalline oxides of rhenium (Re02, ReO3 and Re207) have been determined by the method of solution calorimetry, using an aqueous perchloric acid--ceric perchlorate solvent. Copper metal and cupric oxide were utilized as auxiliary substances. Heats were determined at 298&apos; K for the reactions Re + 2CuO = Re02 + 2Cu, Re + 3CuO = ReO3 + 3Cu, and 2Re + 7CuO = Re207 + 7Cu. Standard heats of formation were derived using the value of -37.23 ±0,15 kcal/mole as the heat of formation of CuO. The standard molal heats of formation of the rhenium oxides were determined: Re02, -107.3 ±0.8 kcal; ReO3, -140.8 ±0.9 kcal; and Re207, -301.9 ±1.8 kcal.

Jan 1, 1969

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of Beaver and Lawrence Counties, Pa. Washability analyses were made on seven coalbed samples, none of which were of metallurgical quality as received. Five of the samples could be sufficiently upgraded to produce acceptable products, and the remaining two 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, one sample was of low sulfur content as received, one sample could be upgraded to low sulfur content, and three samples could be upgraded to medium sulfur content. The original sulfur content of the remaining two samples can be appreciably reduced by removal of the sink 1.58 speci fic gravity material; however, these coals would be classified as medium sulfur coals both before and after removal of the sink material.

Jan 1, 1969