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By V. E. Edlund

Pyrometallurgical studies by the Bureau of Mines demonstrated the feasibllity of sintering and smelting a low-grade flotation concentrate made by pilot-plant processing 10-percent manganese ore from the Maggie Canyon deposit, Mohave County, Ariz. Under optimum conditions 85 percent of the manganese in a flotation concentrate that assayed 36 percent manganese was recovered as standard ferromanganese. A blend of this flotation concentrate with high-grade dithionate pilot plant precipitate was similarly processed with a recovery of 90 percent of the manganese. Thorough mixing and pelletizing of the charge before treatment on the sinter hearth was necessary to produce a well agglomerated product by single pass sintering. Although satisfactory sinter was produced from a variety of material combinations, best results were obtained on a charge that contained 80 percent flotation concentrate and 20 percent return sinter fines. This combination was mixed with 6 percent coke, based on weight of concentrate; and 12 percent moisture. Sintering such a charge yielded a well agglomerated product containing over 80 percent coarse material, The results of standard crushing tests showed that the product was physically comparable to iron ore sinters and manganese nodules.

Jan 1, 1962

By K. C. Dean

A flotation method was developed by the Bureau of Mines for concentrating pollucite, a cesium-aluminum-silicate mineral that may contain from 20 to 40 percent cesium oxide. Separation of the pollucite from three typical ores was achieved by froth flotation of the associated micas, feldspars, and other gangue minerals, using sulfuric and hydrofluoric acids and a cationic-type collector. A low-tenor, 8 percent cesium ore from Maine was upgraded to 20 percent cesium with recovery of 87 percent of the cesium. Relatively high- grade ores from Canada and Southern Rhodesia were beneficiated at lower ratios of concentration to 28 and 29 percent cesium content respectively with recovery of over 92 percent of the cesium. In addition to concentrating the cesium content of ores, the method also effectively separates cesium from sodium, potassium, and lithium, and in certain ores from rubidium. This is accomplished by selective froth flotation of the alkali metal-bearing gangue minerals such as lepidolite, other micas, and feldspars. Since the alkali metals, especially potassium and rubidium, are difficult to separate chemically or thermally from cesium to prepare high- purity cesium products, separation by physical mans is important.

Jan 1, 1962

By R. O. Dannenberg

This report describes aperiments by the Bureau of Mines and reviews theoretical aspects of the use of organophosphate solvent extraction for recovering beryllium from sulfate leach liquors. The leach liquors were prepared by sulfuric acid leaching of lime-sintered low-tenor beryl flotation concentrates. The experimental work on sulfate leach liquors showed that the acidic esters of organophosphates extracted beryllium slowly but in preference to aluminum. Three common alkylphosphoric acids, di- (2-ethylhexyl) (EHPA), heptadecyl (HDPA), and dodecyl (DDPA), in order of decrmsing selectivity, yielded a partial separation of beryllium from aluminum.

Jan 1, 1962

By D. J. Bauer

A pure scandium solution was concentrated from 10-4 mole per liter to 0.5 mole per liter by continuous foam fractionation in a spaced, packed column. Recovery in the foam was 77 percent using a spaced, packed draining column with sodium n-methyl-n-"coconut oil acid" taurate as the surfactant. The technique was first studied batchwise in a small unpacked column to determine the more important variables. Optimum surfactant concentration was found to depend on scandium concentration. Extraction and, in general, enrichment ratios were highest in the 2.5 to 3.5 pH range at temperatures ranging from 50° to 70° C. An airflow rate of 136 ml./min. was satisfactory in the equipment used.

Jan 1, 1962

By M. E. Tyrrell

Magnesia spinel (MgO.Al203) recovered from dusting slags in the system MgO.Al203-2Ca0.SiO2 is in the form of single crystals most of which will pass 35-mash. This investigation was undertaken by the Bureau of Mines to evaluate the concentrates as a refractory raw material. Three specific types of refractory bricks were studied: (1) dense, (2) lightweight bubble, and (3) insulating. Test specimens ware fabricated 1 by dry pressing, fired to 1,675° C., and tested by procedures common to the industry. The concentrates produced a refractor, having satisfactory density and mechanical strength; however, spinal is sensitive to thermal shock and the possibility of producing a spall-resistant brick using aggregate of such small grain-size must be considered remote. Lightweight refractorias fabricated of spinel bubbles were the most promising of the types tested. They were 30 percent lighter in sight than the dense refractory, their mechanical strength was good, and definite superiority in thermal shock resistance was indicated.

Jan 1, 1962

By D. J. Stoops

The object of the research described in this paper was to investigate the effect of metallurgical and surface treatments on the corrosion behavior of arc-melted reactor-grade zirconium in cupric or ferric chloride solutions. An apparatus was constructed and specimens of various metallurgical conditions and surface treatments were tested for 6 days at 35° C., with aeration. Some correlations were observed between corrosion rate and the metal's condition and treatment, Specifically, the unattacked or least attacked specimens were those that had been etched as a final treatment before testing. The most severely attacked specimens were those that had been vacuum-annealed as a final treatment before testing. The moderately attacked specimens were those neither vacuum-annealed nor etched, but having a final surface treatment which left a cold-worked surface. Attack by cupric and ferric chloride was by pit- ting with no preference for grain boundaries, The corrosion scale was cow posed predominately of very fine zirconim particles, Particles from the FeC1,-corroded specimens were more pyrophoric than those from CuCl2-corroded specimens, and appeared to have a higher surface area to volume ratio. Comparison of results to those of previous investigators showed that at certain salt concentrations the more pure, reactor-grade zirconium was quite resistant to attack while the less pure, graphite-melted zirconium was severely attacked.

Jan 1, 1962

By Edwin E. Maust

In response to the ever- increasing demand for high temperature materials, the Bureau of Mines instituted a program for the study and development of superrefractories, One of the major tools obtained for use in this research was an image furnace of the double-paraboloidal mirror type. Although extensive theoretical analyses of solar furnace performance may be found in the literature, comparable detailed information on the double-paraboloidal-mirror image furnace has been nonexistent. This report presents an analysis based on an investigation undertaken to ascertain the limitations and characteristics of the furnace so that it can be used most effectively. The quantitative determination of the energy available at the image, the control of this energy by mans of a 60-inch iris diaphragm, and its variation with position and time relative to the heat source used have all been dealt with in detail. The quantitative results were obtained using a specially designed waterflow calorimeter and these measurements, in conjunction with the theoretical analysis, are used to present a fairly complete description of the furnace and its capabilities.

Jan 1, 1962

By G. L. Hopps

Various chemicals, including compounds of copper and lead, were added to a mixture of No. 2 and No. 6 fuel oils that was fired in an experimental furnace. Tests were made to determine (1) the effectiveness of these chemicals in removing soot deposits on probes devised to simulate heat-transfer surfaces in boilers and (2) the effectiveness of the chemicals in preventing the deposition of soot on the probe surface. Test conditions were regulated so that the temperature of the products of combustion adjacent to the probes was in the range of 625° to 700° F. The clean-metal temperatures of the air-cooled probes were comparable with the water-tube temperatures in boilers operated at 40 to 100 p.s,i.g. The dosages of the fuel oil additives used in these tests were generally larger than those usually recommended for most proprietary compounds.

Jan 1, 1962

By Kevin Malone

Chrysotile asbestos occurs in many counties in California, and a small production had been reported at times, but development of deposits had been disappointing. A reconnaissance survey by the Bureau of Mines indicated that several deposits in the serpentine belt in Shasta, Trinity, and Siskiyou Counties might contain enough asbestos of filler grade to supply the growing demand on the west coast. Accordingly from 1956 to 1958 parts of the Mount Eddy and Shasta View deposits were investigated by trenching and diamond drilling to determine their potential. The work comprised construction of roads, bulldozer trenching, excavation of areas for diamond drilling, sampling, and upping. The trenches were excavated to expose the surface extent of some of the asbestos-bearing areas, To determine the downward continuation of asbestos-bearing sections and to secure samples for test purposes, six diamond drill holes, totaling 1,738 linear feet, were drilled in two selected areas. The trenching and core-drilling indicated that the asbestos-bearing material occurs as ribs and lenses of varying thicknesses in a broad belt of serpentine, about 600 feet wide and several miles long,

Jan 1, 1962

By R. L. Lincoln

The effects of adding from 1 to 50 atomic percent (a/o) to vanadium were investigated by the Bureau of Mines. Properties studied included as-cast and annealed hardness, microstructure, fabricability at room temperature and elevated temperature, tensile strength, electrical resistivity, and oxidation resistance at 625° and 800° 2. Additions of small amounts of hafnium resulted in lessened as-cast hardness, decreased electrical resistivity, impaired roll- ability, increased oxidation resistance, and greater tensile strength. Larger amount of hafnium caused greater as-cast hardness, increased electrical resistivity, further impaired rollability, continued increase in oxidation resistance, and lessened tensile strength. INTRODUCTION The purpose of this study was to determine the effect of hafnium additions on the properties of vanadium and to learn if this binary alloy had any special or unusual properties. This investigation is a part of a larger research project in which new and expanded uses of vanadium are being sought. Domes tic vanadium is found frequently in combination with uranium, and because of the demand for uranium as a nuclear fuel, there now exists a surplus of vanadium-bearing minerals and vanadium pentoxide as a byproduct of uranium production. Primary principles of conservation demand that greater use be made of this readily available surplus; finding suitable metals to alloy with vanadium to enhance its properties is one way to increase its utilization. This report is the result of an investigation of the effects on the properties of vanadium when hafnium is added in amounts from 1 to 50 a/o.

Jan 1, 1962

By Robert S. Warfield

The Federal Bureau of mines and U.S. Geological Survey conducted exploratory investigations and geologic mapping in the Wishbone Hill district of the Matanuska coalfield almost continuously from 1942 through 1958. These investigations delineated reserves of high-volatile bituminous coal necessary to supply the rapidly expanding military and civilian requirements in the Anchorage area. This report describes the program conducted by the Bureau of Mines from 1949 through 1958, and briefly summarizes previous investigations, the results of which have already been published. The coal-bearing structure on both the north and south limbs of the prominent Wishbone Hill syncline was explored by 8,719 feet of churn drilling and 25,460 feet of diamond-core drilling. A total of 33 holes were drilled ranging in depth from 60 to 2,114 feet. To supplement the drilling operations, bulldozer and dragline trenching were undertaken at key locations; about 25,000 cubic yards of dragline trench were excavated in the vicinity of the old Premier mine.

Jan 1, 1962

By E. D. Calvert

This Bureau of Mines report discusses the electric-arc reduction of zirconium and hafnium oxides with carbon yielding a metal-metallic carbide mixture. The carbon to oxide ratio in the feed determines the metal to carbide ratio in the product. A sample of this product was produced -or testing as a feed for the deBoer iodide-dissociation process. A new technique for producing pure carbides is described, which uses the intense heat of the arc to volatilize the carbide. The condensed vapor form , crystals of nearly stoichiometric carbide, INTRODUCTION This research examines the preparation of refractory metal carbides in the controlled atmosphere electric-arc furnace.

Jan 1, 1962

By E. G. King

An earlier Bureau of Mines report4 provided low-temperature heat-capacity and entropy data for three sodium vanadates. This report continues the study of vanadates by presenting analogous data for three crystalline calcium vanadates - calcium metavanadate (CaV206), calcium pyrovanadate (Ca2V2O7), and calcium orthovanadate (Ca3V208). No similar data for these compounds have been published previously. MATERIALS All three vanadate samples were prepared by the Bureau of Mines by heating stoichiometric mixtures of reagent-grade calcium carbonate and vanadium pentoxide.5 Calcium metavanadate was prepared at 610° to 660° C. A stoichiometric mixture was heated for 17 days with intervening grindings, mixings, and adjustments of composition, as shown necessary by chemical analysis. The final analysis gave calcium oxide, 23.48 pct. (theoretical, 23.57 pct.) and vanadium pentoxide, 76.32 pct. (theoretical, 76.43 pct.). The sample also contained 0.11 pct. acid-insoluble matter. The X-ray diffracton pattern showed no lines of free calcium or vanadium oxides. No X-ray diffraction patterns were found in the literature for any of these substances.

Jan 1, 1961

By J. H. Holden

Operations involving the processing of coal, oxygen, and steam into synthesis gas by means of two pressure-type gasifiers have demonstrated the effect of heat loss and operating variables on carbon gasified and oxygen and coal requirements. Carbon gasified is the fraction of carbon in the coal that is converted to gas. Oxygen and coal requirement is the quantity of each that is needed to produce a unit volume (M std. c.f.) of carbon monoxide and hydrogen. Operating pressure of the gasifiers ranged from 150 to 300 p.s.i.g. and coal was fed at 200 to 500 lb./hr./cu.ft. of reaction-zone space. Oxygen-to-coal ratios were 8.5 to 10.5 std. c.f./lb. Heat loss and residence time have opposite effects on carbon gasified; increasing the heat loss decreases the carbon gasified, but increasing the residence time (by raising the operating pressure or reducing the coal-feed rate) increases the carbon gasified. The effects of these two factors are difficult to separate because they usually change simultaneously. A comparison of the results obtained from the operation of two gasifiers with different levels of heat loss, however, permitted the effect of heat loss to be separated from that of pressure and coal-feed rate. When the results were deter- mined on the basis of constant heat loss, increase of the residence time increased the carbon gasified until the reaction virtually had come to completion. For example, at 150 p.s.i.g., decreasing the coal-feed ratio from 500 lb./hr./cu.ft. to 200 lb./hr./cu.ft. substantially increased the carbon gasified. At 300 p.s.i.g., however, changing the coal-feed rate had little effect on the carbon gasified because the reaction had almost reached completion and further increase in residence time resulted only in a negligible change.

Jan 1, 1962

By J. M. Riley

This report summarizes Bureau of Mines experiments in purifying sulfate leach liquors, which were prepared from low-tenor beryl concentrates by modifying the Degussa process. The leach liquor was prepared from a beryl concentrate containing 2.7 percent BeO by (1) sintering the beryl concentrate with limestone in a rotary kiln at about 1,150° C. and by (2) treating the sinter first with sulfuric acid and then with water to form and extract beryllium sulfate. About 80 percent of the beryllium was dissolved. The resulting leach liquor contained 2.4 grams of BeO, 20 grams of Al203, and 6 grams of Fe203 per liter. The laboratory solution contained much more aluminum and iron than a solution derived from treating 10 percent BeO concentrate, which is the standard raw material used by industry. Tests were made to determine the behavior of the solution toward alum purification and limestone neutralization both of which were employed industrially in conventional Degussa procedure.

Jan 1, 1962

By D. F. Smith

The thermodynamic data presented in the literature for zirconium compounds are incomplete. Among the compounds for which adequate data are Zacking are zirconium fluoride and sulfate. This paper reports experimental heat-content values determined by the Bureau of Mines for these two zirconium salts throughout the temperature range of 273° to 1,200° K. No crystalline transformations were found in the two compounds investigated, and neither of the compounds melted over the temperature range studied. MATERIALS TESTED The Oak Ridge National Laboratories, Oak Ridge, Tenn., supplied the two zirconium salts used in this investigation. The zirconium fluoride was high- purity reactor grade material. The zirconium sulfate contained between 0.01 and 0.10 percent hafnium and calcium, and other elements in concentrations below 0.01 percent, A spectrographic analysis of the two compounds is given in table 1. Before use the compounds were dried at 400° C. for several hours to removed adsorbed moisture.

Jan 1, 1962

By Alla D. Mah

The heat of formation of scandium sesquioxide (Sc203) has not been measured previously, and existing values for gallium sesquioxide (Ga203) are subject to large uncertainties. As a consequence, thermodynamic calculations involving these oxides hare lacked scientific exactness. This paper reports newly determined values of the heats of formation of gallium and scandium sesquioxides at 298.15° K., by combustion calorimetry. The corresponding free energies of formation are derived from heat and entropy data.

Jan 1, 1962

By A. R. Taylor

In recent years, thermodynamic data have been used to a greater degree than ever by the chemical and metallurgical engineer as a means of predicting and controlling chemical reactions. To satisfy the spiraling demand for basic physical data needed for the calculations, the Bureau of Mines is studying the heat capacities of a variety of chemical compounds at high and low temperatures. This paper is one of a series presenting such data. The heat capacities of two alkaline earth compounds, strontium bromide and strontium nitrate, were measured in a temperature range of 60° to 300° K. in an adiabatic calorimeter and at temperatures of 300° to about 1,200° K. in a Bunsen ice calorimeter. The construction and operation of the calorimeters are discussed in other reports.3 4 The heat-capacity data presented in this report were extrapolated to 0° K., and smooth values of heat capacity, entropy, enthalpy function, and free-energy function were calculated and tabulated at even 10-degree intervals. The enthalpy data were fitted with algebraic equations by applying the method of least squares; calculations a£ heat-capacity values, entropy, enthalpy function, and free-energy function were made at even 50-degree intervals. The heat and entropy of fusion of strontium bromide were calculated from the enthalpy measurements.

Jan 1, 1962

By Wilbur I. Duvall

In a review of so 40 papers on damage to residential structures resulting from blasting, only 3 were found that present data on the observed amplitude and frequency of the vibration levels produced by blasting together with an observed degree of damage to a residential structure. The data from these three reports have been analyzed statistically to determine if one of the quantities, displacement, velocity, or acceleration, is more reliable than the others for estimating the degree of damage to a residential structure. From this analysis the conclusion is drawn that a given degree of damage to a structure is most closely related to the magnitude of the particle velocity of the wave motion passing thru the earth at the structure location. On the average, only minor damage it observed for peak particle velocities of 5.4 inches per second, and major damage is observed for peak particle velocities of 7.6 inches per second. When the spread of the data is taken into consideration, the following statement can be made: Wave motions that have a peak particle velocity in excess of 2 inches per second have a fair probability of producing some damage to structures, whereas wave motions that have a peak velocity less than 2 inches per second have a very low probability of causing any damage. Therefore, the recommendation is made that vibration levels in the vicinity of residential structures should be maintained below a peat particle velocity of 2 inches per second. The above criterion for safe blasting is considered to hold over a wide variety of soil and rock conditions because the original data were obtained for a wide range of soil and rock conditions and on various types of residential structures. INTRODUCTION Ever since explosives were discovered and developed for mining purposes, there has existed the problem of what effects the air and ground vibrations resulting from blasting have on structures of various types. This problem is

Jan 1, 1962

By F. L. Wideman

This report describes a computer program that is used for the calculation of the coordinates and elevations of subsidence survey pins located by intersection. This program was developed for the Federal Bureau of Mines by the Numerical Analysis Laboratory, University of Arizona. These calculations, although relatively simple, are both tedious and time-consuming when computed with a desk calculator and trigonometric tables. In this survey, a large number of pins were surveyed repeatedly, and it was evident that both time and money could be saved by using a digital computer.

Jan 1, 1962