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By D. R. Mathews

Electrorefined vanadium was evaluated with respect to tensile properties and the effects of interstitial contaminants in the temperature range of 77° to 273° K. The yield strength of 18,500 psi and hardness of 63 diamond pyra-mid hardness (DPH) of electrorefined vanadium are approximately equal to that of iodide crystal bar vanadium. The ductile-brittle transition temperature was found to be below 77° K, but with 0.175 weight-percent oxygen or 0.10 weight-percent nitrogen, it increased to between 123° and 190° K. With carbon content up to 0.11 weight-percent, the transition temperature remained below 77° K. The yield strength of the interstitial-containing alloys can be expressed by: au = 7.5 + 480 (pct N) + 290 (pct 0) + 280 (pct C), where au is the upper yield stress in 1,000 psi at 273° K. Profuse deformation twinning occurred in the alloys tested at 77° K. However, twinning could be suppressed by dissolved oxygen or nitrogen in excess of 0.15 and 0.086 weight-percent, respectively. Carbon, even though present in excess of the solubility limit, did not affect twinning.

Jan 1, 1965

By Jr. Norman

Thermoelectric properties of depleted uranium selenides and tellurides were investigated from room temperature to 700 C. Several depleted uranium monoselenides and monotellurides were doped with selected cationic and anionic materials to determine the effect of impurity additions on the thermoelectric properties. The undoped uranium selenides and tellurides were semimetallic conductors exhibiting low Seebeck coefficients and electrical resistivities. Partial or complete degeneracy was in evidence, indicating a charge carrier energy distribution similar to that in a metal. Doping increased the Seebeck coefficients of the uranium monoselenides and monotellurides; however, the corresponding change in the power factor in the figure of merit was small because of the increase in electrical resistivity.

Jan 1, 1965

By Foster Fraas

The Bureau of Mines investigated a method for calculating values of adsorption energy; the goal was to devise an equation consistent with experimental data accumulated in the investigation of adsorption as related to ore separation processes. Numerical identification of the constants of a previously formulated equation provided an equation by which values of adsorption energy could be calculated. Values thus calculated checked with those obtained by calorimetric measurement.

Jan 1, 1965

By J. M. Stuve

Provisional values for the heat of formation of europium trichloride and europium sesquioxide were determined by solution calorimetry utilizing europium metal of more than 99-percent purity. The resulting values for the heats of formation of Eu203 (cubic) and EuCls (hexagonal) were -386,970 ±l,200 cal/mole and -218,740 ±650 cal/mole, respectively, measured at 298.15° K.

Jan 1, 1965

By A. Gene Collins

This report discusses some of the chemistry and geochemistry of cesium and rubidium. Knowledge of the cesium and rubidium content of oilfield waters aids in resolving the origin of waters and petroleum, exploring for petroleum and other valuable minerals, discovering water pollution sources, and augmenting the knowledge of geologic formations. The methods described in this report permit the detection of less than 0.01 mg/l of cesium and/or rubidium in a complex oilfield brine or water. Solvents possessing high-dielectric constants were evaluated for their ability to extract cesium and rubidium tetraphenylboron from oilfield waters and for their flame emission characteristics. Nitroethane was selected and used for the extraction and flame spectrophotometric determinations because it gave the highest sensitivity. Cesium 137 and rubidium 86 were used to determine the extraction efficiencies, which were about 87 percent and 58 percent respectively using a single 10 ml nitroethane extraction from a distilled water matrix. The standard deviation of the determination was 0.0008 mg for cesium and 0.0007 mg for rubidium in the 0.01 mg range.

Jan 1, 1965

By R. R. Nothdurft

The internal friction of eight single crystals of magnesium with orienta-tion ranging from 10° to 84° was measured at 33.5 kc and 272° C, and the results were interpreted in terms of the pinned-dislocation model proposed by Granato and Lucke. Results show that the strain-amplitude-dependent decrement varies with orientation in a manner predictable by the G-L model. Different values of strain-amplitude-independent decrement were observed at different orientation angles, but correlation with the theory was not conclusive. Problems and steps for further study are discussed.

Jan 1, 1965

By H. E. Powell

Basic data were recorded on the decompositions that take place during thermal decomposition of siderite (FeC03). Both the naturally occurring and a synthetically prepared mineral were studied by differential thermal, thermo-gravimetric, X-ray-diffraction, and chemical (including gas) analyses. Thermal decomposition was studied in the media of dry air, moist air, dry carbon dioxide, dry helium, and dry carbon monoxide and at atmospheric and at reduced pressures. Results showed the thermal decomposition of FeC03 to be an extremely complex process, dependent on environmental factors and side reactions that cannot now be completely controlled. Therefore, full understanding of the reaction involved must depend on additional research with advanced evaluation techniques.

Jan 1, 1965

By Jr. Joyce

This report describes sulfatization of nickeliferous laterites from Puerto Rico and the Philippines for recovery of water-soluble nickel and cobalt sulfates. Temperatures ranging from 665 C to 710 C and a 10-percent sulfur dioxide-air reaction gas were employed during batch-roasting tests and during continuous countercurrent treatment in a 2-inch-diameter shaft furnace. A maximum of 69 percent of the nickel and 76 percent of the cobalt were recovered from one sample of Puerto Rican laterite, and a maximum of 96 percent of the nickel and 91 percent of the cobalt were recovered from the Philippine laterite.

Jan 1, 1965

By George R. Schottler

The objective of this research is to find the extent of the range of applicability of previously developed statistical methods for determining grade and tonnage of ore to bedded uranium deposits. Uranium assays obtained from gamma-ray logs of exploratory drill holes are used to compute grade and tonnage of ore in the deposit by a standard polygonal method and by statistical analysis. The results obtained by the two methods are compared. The uranium-assay frequency distributions are shown to be lognormal and a simple transformation permits the use of standard normal curve statistics. The effects on the assay frequency distributions of stratified sampling, a required minimum mining thickness, and increased assay-interval length are investigated. The addition of low-grade mineralization to make up the required minimum mining thickness results in a distinct change in the skewness of the assay frequency distribution. Any statistical inference regarding grade-tonnage relationships that will be produced, using the minimum mining thickness, should be made on the basis of this "revised" assay frequency distribution.

Jan 1, 1965

By Juel H. Stears

Research was done to determine if a hydraulically operated penetrometer developed by the Bureau of Mines could be used to estimate the roof-bolt anchorage capacity of mine roof rock. Tests were conducted both in the laboratory using cement cylinders and underground in shale rock. Hardness readings were measured by the penetrometer around the periphery of the bolt holes at the anchorage horizon. Roof bolts Nere then installed and subjected to an anchorage test. The results showed that the penetrometer readings could be used to determine the optimum stratum for roof-bolt anchorage but could not be used to make an accurate estimate of the anchorage capacity.

Jan 1, 1965

By R. J. Leary

Oxidation testing of copper-clad steel strip was performed in a muffle furnace to determine whether copper in contact with steel scrap could be removed by oxidation in an airstream at high temperatures. Substantially all of the copper was oxidized before any significant iron oxidation occurred. The rate of copper oxidation was not affected by contact with iron. Copper oxide scale separated spontaneously from the underlying metal during cooling. Results indicate the possibility of removing light-gage copper coatings and components from ferrous scrap by oxidation in an incineration process.

Jan 1, 1965

By James D. Brown

The Bureau of Mines has written a computer program in FORTRAN to facilitate the calculation of concentrations from X-ray intensities in electron probe microanalysis. Philibert's absorption and Castaing's secondary fluorescence corrections are used; no atomic number correction is included. Background and dead time corrections are applied to the data before calculating the relative intensities. Data from any type of electron probe microanalyzer can be used with the program.

Jan 1, 1965

By Arne Landsberg

A study of the chlorination kinetics of germanium, silicon, iron, tungsten, molybdenum, columbium, and tantalum has been made to determine the effects of temperature, chlorine concentration, geometric surface area and gamma radiation. The reaction products were volatile at the temperatures used this making it possible to follow the reaction rates by weight loss of the solid. Chlorination rates of germanium, silicon, and iron were found to be directly proportional to chlorine concentration while the rates for tungsten, molybdenum, columbium, and tantalum were proportional to the 0.5 to 0.6 power of chlorine concentration. A good correlation of reaction rate and geometric surface areas was not obtained because the true surface area of the samples could not be measured. Intense gamma radiation had no effect on reaction rates. The Arrhenius activation energies determined over the temperatures used are as follows: Germanium, 27 kcal/mole (233°-241° C); silicon 33 kcaL/mole (375°-517° C); iron, cold rolled, 20 kcal/mGle (259°-325° C) annealed, 21 kcal/mole (293°-337° C); tungsten, 43 kcal/mole (617-776° C); molybdenum, 37 kcal/mole (445°-4910 C); columbium) 34 kcal/mole (229°?255° C); and tantalum, 29 kcal/mole (370°-449° C).

Jan 1, 1965

By L. F. Heising

The Bureau of Mines evaluated 191 composites from the central Mesabi Range, Minn., chiefly by reductive roasting and magnetic separation. After reductive roasting and magnetic separation at minus 325 mesh, 28 composites produced concentrates that contained an average of 66.0 percent iron with less than 10 percent silica. Recovery of contained iron was over 90 percent. Natural magnetic material in excess of 5 percent was present in 142 composites. Trial flotation tests were used to evaluate three samples unresponsive to reductive roasting and magnetic separation procedures, and satisfactory concentrates having low silica contents (averaging 6.6 percent) were achieved.

Jan 1, 1965

By Jack I. Paige

The devitrification of lithium silicate glasses was studied to determine the effect of annealing temperature, composition, and additives on nucleation and crystallization. High-purity glasses, prepared from reagent-grade chemicals, had close to optical quality when prepared by a vacuum induction melting method developed during this research, The progress of devitrification was traced by differential thermal analysis and thermal expansion for those lithium metasilicate-silica compositions containing 80 to 90 percent silica. Microscopic studies of glasses partially devitrified at various temperatures and annealing times indicated that the primary initial mode of formation of individual crystals ,vas from densely crystalline zones that filled in as crystallization advanced Of the additives tested, calcium, potassium, and sodium helped promote devitrification with the least cracking or surface deformation. Tin oxide was most effective in reducing volume contrast ion during devitrification, but was not ClS effective in preventing cracking as calcium or potassium additions.

Jan 1, 1965

By Joseph A. Cavallaro

This report describes the timed release analysis technique that was developed to serve as a tool for assessing the froth flotation cleaning potentials of fine-size coals. Using this developed technique, 16 coals from 10 different coalbeds were tested. All of the coals included in this study were quite amenable to froth flotation with float coal yields ranging from 80.7 to 99.5 percentage points. Float-and-sink analyses of the coals tested are shown to be of limited value in predicting froth flotation cleaning potential. Generally the float-and-sink analyses indicated a better product could be obtained than froth flotation could provide; although, in four of the coals tested froth flotation results were superior to those expected from the gravimetric analysis. The fixed carbon content of the samples collected was found to correlate with the floatability of the coals. The higher rank coals were the most readily floatable coals while the lower rank coals did not respond quite as well to flotation.

Jan 1, 1965

By Stephen Utter

Stresses induced by block-caving mining were estimated from in-place measurements of strain or deformation in rock and concrete around mine openings. The four types of gages used for measurements in the Climax Molybdenum mine during 1959-61 were Whittemore gage, Carlson strain meter,2 Valore strain cell, and Climax extensometer. Gage performance in the laboratory was evaluated by stressing instrumented rock and concrete specimens in a universal testing machine and by comparing measurements taken by the gages and a standard gage. Gage performance in the mine was evaluated by comparing measurements taken during an 18-month test. The Whittemore gage, Carlson strain meter, and the Climax extensometer proved suitable for the investigation; the Valore strain cell, effective in the laboratory tests, gave erratic measurements in the mine.

Jan 1, 1965

By J. M. Kuchta

Experimental data are presented on the autoignition temperature (AIT) characteristics of the hydrocarbon jet fuel, JP-6, in various oxygen-nitrogen atmospheres under conditions of constant volume and constant pressure. AIT's of this fuel in air varied little with fuel injection pressure but increased greatly with decreasing fuel content at low fuel-air-ratios. They also increased with decreasing oxygen content of the fuel vapor-oxidant atmosphere. Consistent with thermal ignition theory, the ignition temperatures increased with decreasing initial pressure, ignition delay, and vessel radius; expressions are given which define the observed variation of AIT with these variables for JP-6 fuel vapor-air mixtures. The significance of autoignition temperature data obtained using various ignition criteria is discussed to show the usefulness of such data in evaluating fire and explosion hazards. In addition, data are presented on the extent of oxidation that occurs prior to autoignition of this fuel in air at various temperatures.

Jan 1, 1965

By C. O. Hawk

Distillable oils derived from coal were desulfurized and hydrogenated at 2,500 psig in a two-step vapor-phase catalytic operation to give a product rich in saturated cyclic hydrocarbons. The first step was mainly a desulfurization at 400 C, the second a saturation at 300 C. One of the oils used as feed stock was from low-temperature carbonization of a bituminous coal, the other was from the liquid-phase hydrogenation of coal in the Bureau's pilot plant. The product from the saturation step was distilled to remove the light ends and high-boiling residue and to recover a fraction having acceptable properties with respect to heating value, density, freezing point, viscosity, and boiling range according to specifications suggested by the Air Force for ultra-high-speed aircraft fuel. Quantities of the fuel fraction available were too small for the thermal stability test approved by the Air Force. The experiments, performed on laboratory scale, comprised mostly a study of the effect of varying the oil feed rate (at constant oil-to-hydrogen ratio) on the yield of the desired fuel fraction. The yield of the fuel fraction made from low-temperature carbonization oil was a little more than 1 percent of the weight of coal carbonized; that from coal-hydrogenation oil was about 12 percent of the weight of coal hydrogenated. A few attempts to do both desulfurization and saturation in one operation with sulfur resistant catalysts, developed for vapor-phase hydrogenation or hydroforming, were unsuccessful. By leaving the low-boiling ends in both feed stocks to desulfurization, another product was obtained: a low-sulfur aromatic cut boiling below 200 C. This material would be suitable as a solvent or a chemical raw material.

Jan 1, 1965

By K. C. Dean

This report is the first of a series concerned with processes for producing magnesium. These reports will evaluate metallothermic, carbothermic , and electrolytic production methods, and will furnish a cost basis for comparing the processes. Areas deemed most promising for future research will be delineated for each procedure. This report presents briefly the history of the metallothermic process, and describes the operations of the Defense Plant Corp. (DPC) plants that employed the process. A hypothetical plant designed to produce 12,000 tons of magnesium per year, using ferrosilicon as a reductant, is described, and raw materials, energy, and major equipment requirements are estimated. Several process modifications are suggested for future research.

Jan 1, 1965