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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 Heinz W. Sternberg

The literature on electrochemical treatment of coal is reviewed, and possible avenues of further research in this field are discussed in this report. Electrolytic reduction of finely distributed coal resulted in the addition of as many as 9 atoms of hydrogen to 100 atoms of carbon. Reduction of coal extracts at controlled potentials indicated the presence of condensed aromatic hydrocarbons and reducible quinones in coal. As much as 65 percent of low-rank coal can be made alkali soluble by electrochemical treatment. Higher rank coals gave smaller yields of alkali-soluble products. However, the nature of this reaction is not clear. The difficulty of reducing coal electrolytically is probably due to the insolubility of coal and not to any structural peculiarity. Reduction of coal by electrolytically generated radical anions appears to be a promising approach for further research.

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 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 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 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. 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 W. T. Benson

The Bureau of Mines has examined selected deposits of titanium minerals throughout the United States. The titaniferous magnetite deposits in the western San Gabriel Mountains, Los Angeles County, Calif., were among those selected for study, and in 1956-58 field work was conducted to determine the extent and character of the titaniferous magnetite deposits occurring in the area. This report describes this work and summarizes earlier work in the area by the Bureau and others. The titaniferous magnetite occurs disseminated as seams and lenticular pods in an anorthosite belt 4 to 6 miles wide that trends about. N. 80° W., extending from sec. 13, T. 3 N., R. 12 W., to the west boundary of R. 14 W., at which point the titaniferous magnetite-bearing rocks disappear beneath the sediments in the Santa Clara River Valley.

Jan 1, 1962

By William J. Campbell

The purpose of this investigation was to extend the analytical services which are required for Bureau of Mines programs in developing and evaluating high-purity materials. Determination of trace elements in minerals and ores as an aid in geochemical evaluation and prospecting was considered. Serious consideration should be given to the merits of using the avail- able fluorescent X-ray spectrographic instrumentation and techniques for determining trace elements. Limits of detectability for trace elements in metal, oxide, solution or mineral samples range from 0.1 to 100 p.p.m, depending on the element being determined, overall sample composition, and the complexity of the X-ray spectra; limits of detectability range from 0.01 to 1 microgram for elements that have been preconcentrated by a chemical or physical process, for example, by ion-exchange membrane.

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

By Alla D. Mah

Thermodynamic calculations for antimony and its compounds have been hampered by the lack of adequate basic thermal data; much work rains even to fill the more important gaps. This paper supplies heat and free energy of formation values at 298.15° K, for the sesquioxide and tetroxide, based upon new measurements conducted by the Bureau of Mines. The heats of formation were obtained by combustion (bomb) calorimetry, and the free energies of formation were obtained by combination of heat and entropy data. The new values are believed to substantially improve the accuracy of thermodynsunic considerations involving these oxides.

Jan 1, 1962

By A. R. Taylor

This report describes the design, construction, and operation of a low temperature adiabatic calorimeter for measuring heat capacities of solids or liquids from 60° to 300° K. A brief discussion of the basic theory involved in chemical thermodynamics and the problems involved in obtaining accurate experimental data is presented. The operation of the calorimeter was tested by measuring the heat capacity of a sample of benzoic acid obtained from the National Bureau of Standards over a temperature range of 60° to 300° K. The measured heat capacity values of the benzoic acid compared favorably with similar values obtained by the Bureau of Standards, the maximum deviation being 0.5 percent. THEORY A brief discussion of the basic theory involved in chemical thermodynamics will illustrate the applications of heat capacity data and the problems involved in obtaining accurate experimental data.

Jan 1, 1962

By Charles Zahn

Direct mass spectrometric determination of alcohols in the presence of hydrocarbons has not been possible because of the similarity of hydrocarbon and alcohol mass spectra. Experiments have demonstrated that by converting the alcohols to their trimethylsilyl derivatives, characteristic mass spectra are obtained free of interference from hydrocarbon ion fragmentation. Hexa- methyldisilazane is the reagent selected for the conversion, An improved method of preparing the reagent is given, Mass spectrometric determination of alcohols as trimethylsilyl ethers now is not only possible without prior separation from other materials, but the range of the room-temperature mass spectrometer is also extended to include the C10 alcohol region. Water does not interfere because it is converted to hexamethyldisiloxane, which has its own distinctive mass spectral peak, Experience indicates that other compounds such as glycols, amines, and phenols probably could also be determined by mass spectrometry of their trimethylsilyl ethers. Studies on the similar detemination of phenols in coal oils have been started, When mass spectrometry is not available, gas-liquid chromatography of alcohols before and after their conversion to the trimethylsilyl derivatives probably could be performed. The preparation and properties of the trimethylsilyl derivatives of 23 alcohols, 2 glycols, 3 amines, and 1 mercaptan are detailed. INRODUCTION During investigations by the Bureau of Mines at the Pittsburgh Coal Research Center relative to the development of Fischer-Tropsch processes, complications were encountered in the mass spectrometric analysis of alcohols in hydrocarbon oils. The fragmentation peaks of the alcohols and the hydrocarbons were so similar that an accurate analysis was not possible, Since involved separation techniques are necessary to isolate alcohols from hydro-carbons for separate determinations, efforts were turned to the search for a

Jan 1, 1962