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By J. J. Wallace

This report describes the initial phase of Bureau of Mines research in the hydraulic mining of bituminous coal. The mining site and equipment are described, and the test procedures and results obtained with a bar-mounted monitor are given. Tests showed that hard Pittsburgh-bed coal can be mined hydraulically from a solid face at water pressures of 4,000 pounds per square inch.4 Coal was penetrated to a depth of 4 feet in 20 seconds with 225 gallons of water per minute coming from a 3/8-inch nozzle at 4,000 pounds per square inch pressure. Some difficulty was encountered in cutting the binders occurring in the coal; it was not possible Lu penetrate directly the overlying draw slate.

Jan 1, 1961

By S. R. Borrowman

This investigation by the Bureau of Mines was undertaken to develop information on the extractive metallurgy of thorite ores because potential ore bodies of this mineral have been found recently in Colorado, Idaho, and Montana. Basic information on thorite ore treatment that would be useful in appraising the potential of these and other domestic thorium resources was developed. The work was done mainly on thorite ore containing 3.87 percent ThO2 from the Powderhorn district, Colo., and on a composite sample containing 0.52 percent ThO2 from the Wet Mountains district, Colo. Limited tests of d corroborative nature subsequently were made on a sample containing 2.30 percent ThO2 from the Lemhi Pass area on the Idaho-Montana border.

Jan 1, 1962

By M. I. Copeland

The investigation of the iron-gadolinium phase diagram is part of a project undertaken by the Bureau of Mines and sponsored by the Atomic Energy Commission to investigate rare-earth alloys. Data from the investigation of the iron-gadolinium phase diagram revealed a single eutectic system with very limited terminal solubility and three intermediate phases. The eutectic point occurs at about 85 percent gadolinium, and the eutectic isotherm, which occurs at 850° C., extends from the compound Fe2Gd to 99-plus percent gadolinium. Very little solubility of the solid phases in each other was observed. The three intermediate phases, FegGd, Fe3Gd, and FeaGd, melt incongruently at peritectic isotherms at 1,320°, 1,150°, and 1,080° C., respectively. The crystalline systems of the three phases were determined as follows: FegGd, hexagonal; Fe3Gd, hexagonal or rhombohedral; and FeaGd, face-centered cubic. No lowering or raising of the alpha-gamma iron transformation at 910° C., the gamma-delta iron transformation at 1,388° C., or the gadolinium transformation at 1,262° C. was observed. The principal methods used in determining the iron-gadolinium phase diagram were melting-point determinations, thermal analyses, metallographic examination, and X-ray diffraction analyses. Melting, heat treating, and thermal analyses were conducted in a vacuum or under a helium atmosphere because of the avidity with which oxygen combines with gadolinium at elevated temperatures. A few hardness values were determined, but they had no part in the derivation of the phase diagram. No other mechanical properties were determined.

Jan 1, 1962

By C. S. Tout

While investigating methods for determining the best temperatures for hot-working experimental stainless steels, the Bureau of Mines Albany Metallurgy Research Center developed a machine in which hot-twist tests could be made in a few minutes. This machine is similar to some used previously except that specimens are heated by induction instead of by radiation, and their temperature is measured by a calibrated radiation-detection unit instead of by a thermocouple. In. developing the technique for using the new machine, tests were made on specimens of medium-carbon steel, mild steel, and AISI (American Iron and Steel Institute) type 304 stainless steel. Tests also were made on as-cast specimens and preworked specimens of experimental AISI type 202, low austenitic stainless steel, and as-cast specimens of AISI type 301 experimental stainless steel. The optimum hot-working temperatures were determined for all types of steel tested. Also, data were gathered on the effects of test speed and temperature on torsional strength and the effect of twisting on tensile stress in the specimen.

Jan 1, 1962

By A. A. Berk

The Bureau of Mines devised a test nipple for the field study of corrosion in the condensate-return lines of Federal heating plants. Corrosion surveys, made with this device, showed that the deterioration of the piping was caused principally by carbonic acid in the steam condensate. Corrosion problems were brought under control when the carbonic acid concentration in the condensate was decreased. In many instances, this was effected by decreasing the total carbon dioxide content of the feedwater; in others, the condensate acidity was neutralized with volatile, alkaline chemicals. Filming treatment with octadecylamine, reported successful in controlling return-line corrosion in industry, was much less effective in Federal area-heating plants. Laboratory study by the Bureau disclosed that octadecylamine is unstable in heating systems. Analytical methods were developed for this chemical and its degradation products in heating-plant condensate. Field surveys, in using these methods, confirmed the instability of the filming material. Laboratory tests showed that the degradation products are not useful film formers. Since filming treatment has little effect on condensate corrosivity, the piping was corroded where it was not coated by the treatment chemical.

Jan 1, 1962

By T. T. Campbell

This investigation was undertaken by the Bureau of Mines to determine if high-purity ductile molybdenum of uniform quality can be prepared by bomb reduction techniques. Molybdenum trioxide (Mo03) and mixtures of molybdenum dioxide (Mo02) and trioxide were reduced by magnesium in closed steel bomb reactors. Very high pressures in excess of 5,000 p.s.i. developed during magnesium reductions of Mo03. The addition of calcium oxide to the bomb charges caused a significant reduction in pressure. Reaction efficiencies higher than 95 percent were obtained during magnesium reductions of either Mo03 or mixtures of Mo02 and Mo03, but high pressures were encountered when the charges contained from 30 to 60 percent Mo02. Reaction efficiencies were usually low (less than 80 percent) when the bomb charges contained more than 40 percent Mo02. The charges with the best composition considering operating pressure, yield, and purity contained from 10 to 30 percent Mo02. The addition of small amounts of carbon to the reaction charges was helpful because some deoxidation occurred during the reduction and also during subsequent arc-melting of the regulus metal. The purity of the bomb-reduced, arc-cast molybdenum metal ranged from 99.2 to 99.8 percent and in some instances the metal contained as little as 5 parts per million oxygen.

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 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 Richard F. Hewlett

Engineers at the Bureau of Mines Denver Mining Research Center have been a research program investigating the theory and application of mine sampling. Part of this program is an investigation of the efficiency of sampling methods that involves development of sampling-method theory through simulating ore-deposit samples and assays, using - electronic digital computer. Theoretical developments are checked against actual ore-deposit sampling, assay, and production data by the commonly used polygonal and triangular methods of computing grade and tonnage of ore reserves. To speed the computing procedures, a program has been developed utilizing a medium-size digital computer for computing ore reserves by the polygonal method. This program calculates nine prismoids per minute at a total cost of $0.21 per prismoid. The complete program, written for an augmented IBM 650 computer, is described in detail; it can be used without change for computing ore reserves for a low-grade deposit. Modifications necessary to convert the program to compute ore reserves for virtually any other type of deposit or grouping of ore horizons also are given; however, the program is limited to using only vertical drill-hole data.

Jan 1, 1962

By V. F. Swanson

As part of the Bureau of Mines titanium resources examination program, samples of altered rock (saprolite) and unaltered rock from the Roseland anorthosite near Roseland, Nelson County, Va., were tested for amenability to beneficiation by flotation. A flotation technique was developed to produce bulk concentrates of ilmenite, rutile, sphene, and leucoxene. It was necessary to first float apatite using oleic acid as the collector, in an alkaline pulp with dextrine as a titanium mineral depressant. The titanium minerals could then be floated from the apatite tailing, using fluosilicic acid to depress the remaining apatite, morin to depress ferromagnesian minerals (when present), and oleic acid as the collector. A bulk titanium mineral concentrate, analyzing 66.0 percent Ti02 and 0.08 percent P205, was obtained from a sample of the unaltered rock which contained 5.45 percent TiO2 and 2.81 percent P205. Overall recovery in the concentrate was 47.1 percent of the total TiO2 in the ore. About 55 to 65 percent of the saprolite sample was clay and was removed by attrition scrubbing and decantation. The apatite prefloat procedure was applied to the saprolite sands; subsequent titanium mine: 1 flotation recovered 72.2 percent of the Ti02 in a bulk concentrate containing 65.1 percent TiO2 and 0.20 percent P205.

Jan 1, 1962

By L. M. Irwin

This Bureau of Mines investigation relates the physical properties of copper reverberatory furnace slags to changes in composition, The smelting of upper Michigan copper ore presents some problems that probably differ from those of other copper smelting areas. The study of these problems has, however, provided important data regarding slags in general and therefore will be of value to other operations as well. Conclusions reached from this study were: (1) Slag fluidity and refractive indices varied directly with the iron content and inversely with silica, lime, and alumina, and (2) there was no apparent correlation between slag fluidity and its copper content.

Jan 1, 1962

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 M. E. Tyrrell

To promote greater use of abundant domestic raw materials in the manufacture of synthetic mullite, the Bureau of Mines has undertaken a comprehensive investigation to determine the effects of the impurity oxides TiO2, Fe203, and alkali on physical properties of sintered mullite-forming mixtures. The first part of the report presents the results of work covering a major area within the mullite study; namely, the effect of impurity oxides on volume stability, one of the outstanding characteristics of mullite refractories. The volume stability of 20 compositions in each of 3 alumina- to-silica ratios, which blanket the range commonly found in purchase specifications, has been determined following procedures of Navy Specifications B-15606 A for Grade A high-alumina refractories. Results indicated that so long as 5 percent of impurities are combined approximtely in the proportions of 3 percent Ti02, 1 percent Fe203, and 1 percent alkali, sintered mullite-forming compositions in the almina to silica range tested will be volume stable. A permissible tolerance of one-half per- cent in each impurity oxide provides a range that includes values common in the natural minerals from which sintered mullite may be made. Within the total range of 5-percent impurity mixtures, a greater number of volume-stable compositions were obtained by increasing the alumina-silica ratio.

Jan 1, 1962

By J. P. McGee

The Bureau of Mines is doing research and development work on a coal-fired gas turbine plant initially developed by the Locomotive Development Committee, (LDC) of Bituminous Coal Research, Inc. The Bureau is redesigning the turbine blading and some of the auxiliary equipment, and is reerecting, the plant at the Morgantown (W. Va.) Coal Research Center. The present goal is a 1,500-hour run at virtually the same operating conditions used by the LDC in their final 1,100-hour test with the turbine. This will allow the Bureau to properly evaluate the new blade design. Erosion of the turbine blades (particularly the roots) by ash in the hot gases from the combustion of coal was the most serious problem in extended operation in earlier experimental work. New blades made of Stellite6 are being fabricated for the stator and rotor, and armored wear strips of titanium carbide will be inserted in the blades at the areas of probable maximum ash velocity and concentration. The trailing edges of the rotor and stator blades are being thickened and thinned, respectively, to induce the ash to travel to the casing and prevent it from returning to the base of the rotor blades. The first stage rotor and second stage stator blades are being removed to provide an annular space for maximum quantities of coal ash to centrifuge to the casing. Additional blades will be added to most of the rows in the stator to stop secondary flow of dust-laden gas toward the rotor. A contract has been awarded for fabrication of the new blades. The 1,500-hour run will be started as soon as the new blades are installed.

Jan 1, 1962

By M. M. Wong

Beryllium possesses attractive properties for use in the nuclear and space fields. Since fused-salt electrorefining can be employed to produce this metal in high-purity form from low-grade or scrap metals, the Bureau of Mines investigated electrorefining of beryllium in electrolytes composed of a LiC1-KC1 eutectic mixture plus varying amounts of BeC12. Results showed a 99- percent or better reduction of oxygen and magnesium and a substantial reduction of other minor metallic impurities. Extremely pure beryllium metal was produced. Operating variables, including BeCl2 concentration in the bath (3.5 to 16.5 mole-percent), temperature of operation (450° to 550° C.), and cathode current density (45 to 770 a,/sq, ft.), were studied; their effects on the deposition of metal, working condition of the bath, and purity of the refined metal are discussed. The safety precautions used in handling beryllium in the laboratory are also described.

Jan 1, 1962

By J. W. Town

This report summarizes the results of laboratory investigations made by the Bureau c! Mines on the recovery of mercury from caustic sulfide solutions by aluminum precipitation and by electrodeposition. Statistical methods were used to design the experiments and evaluate the resulting data. Precipitation studies demonstrated tint metallic mercury could be recovered from mercury sulfide-sodium sulfide solutions with aluminum. Other metals and their salts and aluminum, salts precipitated only black mercury sulfide. Over 95 percent of the mercury was precipitated from solutions prepared with reagent-grade chemicals and from cinnabar leach solutions. Two equivalents of aluminum were required to obtain 95 percent precipitation of the mercury. Under optimum conditions 1 gram of aluminum precipitated from 4 to 7 grams of mercury; the excess Aluminum was recovered for reuse. The effects of time and temperature on the precipitation of mercury were minor when compared with the effects of mercury concentration and aluminum equivalents. The particle size of aluminum had no significant effect over the ranges studied. When aluminum was used as a precipitant, the mercury concentration in solution was reduced to below 1.0 grams per liter. Adding arsenic and antimony sulfides to the mercury solution resulted in their coprecipitation with the mercury when the aluminum was added From 95 to 99 percent of both the arsenic and antimony were precipitated as metal, which amalgamated with the mercury.

Jan 1, 1962

By H. F. Yancey

About 65 percent of the more than 400 million tons of coal produced annually in the United States is mechanically cleaned to remove the inorganic impurities before being sent to market. The impurities, principally shale and clay with some pyrite, average about 20 percent of the raw coal treated. Nearly 95 percent of the tonnage is treated by wet processes, in which water, suspensions of solids in water, or occasionally calcium chloride solutions are employed. Difference in density of coal and impurity is the basis of these processes. Of major importance in the separation is the competency of the impurities, that is, the resistance of the impurities to size disintegration in water. In general, the impurities are more resistant in geologically older coals or those in effect made older by metamorphism. If the impurities suffer reduction in particle size when immersed in water, the separation of organic from inorganic material becomes more difficult, Recently the Scientific Department of the National Goal Board (Great Britain) undertook fundamental research into the interaction of shale and water and also developed an empirical method of assessing shale breakdown or disintegration. 6

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