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By W. L. Heidenreich

This report describes the methods and results of field investigations conducted by the Bureau of Mines between December 1956 and December 1957 on seven deposits of nickel-cobalt-iron-bearing laterite and weathered serpentine near the west coast of Puerto Rico east and south of Mayaguez. These deposits were named, for purposes of identification, Guanajibo, Punta Guanajibo, Las Mesas, north and south deposits of the Rosario Southeast group, and the west and east deposits of the Maricao Southwest group. In addition, the lower 17 miles of the Guanajibo River Valley was tested at widely spaced intervals for possible concentrations of magnetite and chromite in the alluvial sands. The objective of the investigations was to appraise, by drilling and sampling, the two largest deposits--the Guanajibo and Las Mesas. Testing of the smaller deposits was much more restricted. Field investigations consisted of mapping, drilling with power auger, sampling drill-hole sections, and pre-paring samples for chemical analyses, mineralogical studies, and metallurgical tests. The work was financed jointly under a cooperative agreement by the Bureau of Mines and the Economic Development Administration, an agency of the Puerto Rican Commonwealth.

Jan 1, 1959

By H. C. Carpenter

Data are presented comparing results obtained with 17 different catalysts in hydrogenating crude shale oil to gasoline in single-pass operation. A method is described for predicting the maximum yield of gasoline obtainable at constant pressure for each catalyst from results of a limited number of experiments at different temperatures. Operating variables have considerable influence on yields and properties of products. With most of the catalysts, at operating temperatures below 890° F. liquid yield exceeded 100 volume-percent. Above this temperature the volume of liquid product decreased rapidly. Maximum gasoline production in most instances was achieved at a temperature higher than that at which the maximum volume of liquid product was produced.

Jan 1, 1959

By John B. Goodman

This report summarizes the work done by the Koppers Company, Incorporated, in cooperation with the Bureau of Mines on the commercial evaluation of the primary low-temperature tars produced from Texas lignite in the Rockdale, Tex., plant of the Aluminum Company of America in conjunction with the Texas Power and Light Company. The interest of the Bureau of Mines in this project is twofold. First, through its cooperative agreement with the Texas Power and Light Company the Bureau has assisted in the technical design and practical operation of the prototype, externally heated, entrained-state carbonizer for producing char for electric-power production and for primary low-temperature tar. Second, the first successful operation of the prototype carbonizers employing the Bureau of Mines-Parry process on lignitic coal in 1953-54 led to the production of large quantities of primary lignitic tar, concerning which too little was known or had heretofore been published in this country.

Jan 1, 1959

By M. R. Geer

Traditionally, fine coal is more troublesome than the coarser sizes at every step of the coal-preparation process--screening, cleaning, dewatering, and drying. Therefore the present trend toward a higher proportion of fines in the run-of-mine product, brought about by changes in mining practice necessitated to increase productivity, has added greatly to the task of preparing coal for the market. One of the more difficult and costly problems involved is that of recovering fine solids from the washery water. These fine solids should be recovered in the interest of conservation, and they must be removed to provide recirculating water of proper quality. If there is a plant effluent, it must meet increasingly stringent requirements against stream pollution. Vacuum filtration has been used for years at a few plants to recover the extreme fines, but its additional cost discouraged general adoption until recently. Now, with growing emphasis on better solids recovery, filtration is becoming more widespread. Many coal slurries filter readily, giving high cake rates and clean filtrates. Others, however, particularly those containing either a high proportion of material finer than 200-mesh or an appreciable amount of clay, are much more difficult to filter. Many of these refractory slurries can be rendered more filterable by flocculation. A previous report of Bureau of Mines research dealing with flocculation alone was published in 1940.5/

Jan 1, 1959

By D. J. Bauer

This report covers a phase of an extraction project carried out as part of a research program on rare-earth technology. The current project--the production of pure cerium compounds--is an intermediate step between ore processing and metal reduction. In this connection, a study on a separatory-funne1 scale was made on nonreducing extractants for recovering cerium (IV) from tri-n-butyl phosphate (TBP) and of methods for recovering the cerium nitrate from the strip solution. Dilute sulfuric acid was found to be 100 percent effective in stripping cerium (IV). Several precipitants were effective in recovering the cerium from the strip solution, and ethanol was especially promising. A scaled-up investigation was made into the use of spray-tower type equipment to perform the function of extracting, washing, and stripping. This equipment, referred to as the pressure-bubbler, utilized the system developed on the separatory-funnel scale. Feed solutions were prepared from a bastnasite concentrate by two techniques. Of these, the sulfated bastnasite solution was most successful, resulting in 86-percent recovery of the cerium at 99.7+-percent purity.

Jan 1, 1959

By J. E. Wilson

The Pittsburgh carbonization laboratory of the Bureau of Mines has determined the expansion or contraction of more than 300 coking coals in a modified Bethlehem-type sole-heated expansion tester. Information on the actions of coals or blends of coals when coked is extremely valuable to operators of commercial-scale coke ovens. Coals that expand abnormally or beyond expectations can cause extensive damage to coke ovens and result in costly shutdowns and repairs. Although test results for many of the coals have been given in various Bureau of Mines publications, considerable information was not published. Thus, it is the purpose of this report to furnish coal operators and the coking industry with a current appraisal of the expanding properties of all coals tested by the Bureau before September 1, 1958. These data should be useful in the normal long range planning of coal and coke production and will be essential if the demand for coking coals increases abnormally or when reserves of higher grade coals are depleted.

Jan 1, 1959

By William J. Campbell

These investigations were undertaken as part of a program to determine the optimum X-ray spectral lines to use for analyzing the wide variety of samples received by the X-ray Laboratory. Theoretical calculations and experimental data derived from these investigations show that longer wavelength spectral lines, > 2A, are very useful for many analytical problems. Because of the low fluorescence yield of the elements of atomic numbers 13-22 and the small depth of penetration of their X-ray spectral lines, these elements were originally considered to be insensitive; however, these studies show that the wide dispersion of their spectral lines, coupled with their weak beta lines, permits the use of wide collimation, thus increasing the line intensity. More importantly, the background due to scattered primary radiation is very low in the long-wavelength region.

Jan 1, 1959

By V. A. Nieberlein

Problems of design involving the high-temperature characteristics of materials of construction have focused attention on tungsten, the metal with the highest melting point. To study the properties of this metal a method was needed to produce tungsten of high purity easily and consistently. The Bureau of Mines has made tungsten metal in massive form on a laboratory scale by hydrogen reduction of tungsten hexafluoride (WF6). Metal made in this manner had a purity of 99.99 percent or better, with reference to all detectable impurities, including gases. The process tolerated a wide variation in operating conditions, and the results with respect to total impurities as low as 0.01 percent were reproducible.

Jan 1, 1959

By A. C. Rice

This report describes a chemical process for preparing solutions of trivalent rare-earth chlorides from sulfate solutions obtained by treating bastnasite concentrate. The chief impurity in the final solution is cerium, and this element is less than 1 percent of the rare-earth oxides. The solution is used directly in the separation of rare-earth elements by ion-exchange methods. The attractive features of the process are that the chemicals are inexpensive and the steps few. The process starts with precipitating the rare-earth hydroxides from sulfate solutions with caustic soda. After the hydroxides are dried to oxidize the cerium, they are treated with dilute hydrochloric acid to dissolve away the trivalent rare-earth elements, leaving the tetravalent cerium. Details for controlling the leaching step are described. The process shortens older procedures by omitting the usual oxalate or double-sulfate-precipitation step.

Jan 1, 1959

By R. M. Jimeson

Pressure-drop measurements through beds of granular iron, lathe turnings, steel wool, and parallel-plate assemblies were made at linear velocity and gas-density ranges expected in the Fischer-Tropsch hot gas recycle process.4/ Equations relating pressure drop, linear velocity, gas density, and bed porosity were derived. The results indicate that the exothermic heat of reaction can be removed at a lower cost by using catalyst beds with high porosity. INTRODUCTION The Fischer-Tropsch hot-gas-recycle process requires a catalyst offering low resistance to gas flow as one condition to economic feasibility. Conventional granular or spherical catalysts used during early development of the process in Germany did not meet this requirement. Large pressure drops across these beds made the cost of recirculating the gas excessive. The Federal Bureau of Mines is investigating the process by using novel and unusual catalysts that offer little resistance to gas flow. Pressure-drop measurements across these types of catalyst beds are discussed in this report.

Jan 1, 1959

By Foster Fraas

Almost all minerals show irreversible changes in electrical conductivity after heating in the temperature range 100° to 800° C. This effect can be detected with only a limited number of minerals with the standard ionizing-electrode-type separator, which differentiates between nonconductors and conductors in the single-particle resistivity range of 1011 to 1013 ohms. Tests outside this range with other type separators, such as the static field type, increase the number of minerals with which the effect can be detected to almost all that were tested. Irreversibility may be the result of an alteration of adsorption layers, volatilization of surface cations or anions, or an oxidation or reduction. One example is limonite, which decomposes to hematite and passes through two minima and two maxima in conductivity in the temperature range 100° to 900° C.

Jan 1, 1959

By M. J. Ferrante

A process was investigated for preparing Specification-grade nickel (containing less than 1 percent cobalt) by stripping it electrolytically from a nickel sulfate-boric acid solution and using the stripped electrolyte for the preferential dissolution of nickel from basic carbonates of nickel and cobalt. The basic carbonates were produced at the plant at Nicaro, Cuba, owned by the U.S. Government. Determination of the optimum conditions for deposition of Specification-grade nickel indicated that the upper limit of cobalt concentration was 0.1 gram per liter. The pH, temperature, and concentrations of nickel and boric acid in the electrolyte were not critical. An aluminum cathode and two lead anodes were used at a cathode current density of 1.2 amperes per square decimeter.

Jan 1, 1959

By Raymond O. Dannenberg

The gas-combustion retort developed by the Federal Bureau of Mines at the Rifle Oil Shale Project near Rifle, Colo., is a continuous, gravity-feed retort. The heat required to convert the kerogen in the oil shale to liquid oil is generated by the combustion of product gas and carbonaceous residue remaining on the retorted shale after the kerogen has been converted to oil, gas, and residue. A study of the effects of the process variables on retort operation, product yields, and product properties is important to the successful solution of the problems encountered in the development of a satisfactory process. Statistical methods were used to design the experiments and analyze the effects of the rate of shale throughput, the composition of dilution gas, the height of the shale bed above the air entry, air-gas distributor design, shale size range, and the ratios of the flow rates of the various gas streams entering the retort to the rate of shale throughput.

Jan 1, 1960

By F. P. Haver

The purpose of this investigation was to determine the effect of common impurities, that is, oxygen, nitrogen, carbon, and iron, on the Brinell hardness of electrolytic titanium. On a weight basis, nitrogen had the greatest hardening effect, followed by oxygen, carbon, and iron in order. The hardening effects of oxygen and carbon were almost identical up to a concentration of approximately 0.1 percent by weight. Above this concentration, the relative hardening effect of carbon decreased rapidly, possibly because of its limited solid solubility in a-titanium. Hardness vs. composition curves for both oxygen and nitrogen were essentially straight lines over the range of Brinell hardness numbers (B.h.n.) covered in the investigation. The hardness of titanium was also determined as a function of the percentage of impurity atoms. On this basis, iron in concentrations up to 0.17 atomic percent had a greater hardening effect than either oxygen or carbon. INTRODUCTION Determination of the as-cast hardness of arc-melted titanium is a method of quality control widely used in industry. Numerous studies4/ have been made of the effect of impurities on the hardness obtained by this method. However, most of them have been based on the use of either iodide titanium or commercially pure Kroll sponge (B.h.n. >90), as a starting material.

Jan 1, 1959

By Sidney Katell

An estimated capital investment of $76,499,800 will be required for a plant designed and built to produce 90 million standard cubic feet per day (std.c.f.d.) of synthetic pipeline gas through Lurgi gasification of bituminous char. This investment figure does not include the pretreatment plant, the cost of which is assumed to be reflected in the cost of the char fed to the gasification system. Shift conversion, C02 removal, and methanation are required after gasification in the Lurgi unit to make a gas suitable for pipeline transmission. Capital investment data are based upon equipment costs, January 1959. Based on a 90-percent or 330-day operating year, the operating cost before profit and Federal taxes with the char price as a variable will amount to the following: [ ]

Jan 1, 1959

By John Nagy

Limited experiments in the laboratory with specimens of mine rock from a Virginia bituminous coal mine indicate that natural gas-air mixtures can be ignited by sparks generated by rubbing friction of sandstone against sand-stone, shale against sandstone, sandstone against (roof-bolt) steel, and shale against steel. Such sparks, generated during a roof fall, may have initiated a recent gas explosion in this Virginia mine, although this cannot be stated with certainty. No ignitions of gas were produced by sparks or heat generated by impact friction between mine rocks or steel, during tension breaks of roof bolts, or by pull tests of roof bolts through their washers and roof plate. However, this negative result of limited experiments does not preclude the possibility of gas being ignited by these conditions.

Jan 1, 1960

By E. Morrice

The metallurgical laboratory data developed in this study indicate an improved electrowinning process for producing higher purity cerium ingot. A typical sample of the Reno electrocerium contains 99.9 weight-percent cerium and the following impurities: Total other rare-earth elements, less than 0.04 percent; iron not detected; silicon and aluminum, less than 0.02 percent each; calcium plus magnesium, less than 0.01 percent; carbon, 0.01 percent; oxygen, 0.002 percent; hydrogen, 0.0003 percent; and nitrogen, 0.0015 percent.

Jan 1, 1960

By D. W. Frommer

Mineral dressing research was conducted by the Federal Bureau of Mines under a cooperative agreement with the St. Joseph Lead Co., on three samples of iron ore from the Pea Ridge deposit in central Missouri. The objective was to provide information on how to upgrade these submarginal ores and produce marketable concentrates. Samples were prepared from drill-hole cores of similar composition and character to produce (1) a medium-grade mixed hematite and magnetite, (2) a high-grade mixed hematite and magnetite, and (3) a high-grade magnetite. In all three ores phosphorus and sulfur constituted objectionable impurities; excessive amounts of silica were also present in the medium-grade ore.

Jan 1, 1960

By Charles W. Huggins

DEVELOPMENT of the electron microscope has permitted man to examine many small objects that could not be resolved by the light micro-scope. Diffraction, spherical aberration, and chromatic aberration are the main factors that limit resolution to about two-tenths micron with the light microscope. No matter how perfectly a light microscope is constructed and operated, it cannot possibly resolve points separated by less than two-tenths micron. Rapid development following World War II has produced many electron microscopes capable of 20 A resolution. Fibrous inorganic minerals are well suited for electron microscopic study. Many micrographs of chrysotile have been published, but electron microscopic study of the amphiboles has been somewhat neglected. New techniques in sample preparation have simplified the study of fibrous material. Ultrasonic energy has been very helpful in sample dispersion. This publication contains a representative group of electron micrographs of natural inorganic fibers that have industrial value. These fibers commonly are referred to as the asbestiform minerals. The Bureau hopes that the knowledge gained through electron microscopy and other scientific study of the natural inorganic crystalline fibers eventually will lead to the production of synthetic fibers that will satisfy the requirements of industry.

Jan 1, 1959

By Eldon C. Pattee

THE BUREAU OF MINES began an investigation of tungsten resources of Montana in September 1953. This report presents information obtained from July 1955 to September 1957 on tungsten deposits in and near the Mount Torrey batholith. The batholith comprises part of the Pioneer Mountains of Beaverhead County in the southwest corner of Montana. Included in the report are assays and preliminary-examination data on 22 properties. Tungsten minerals are known to occur in 19 of the properties. The major producer is the Brown's Lake mine which has produced more than 625,000 tons of ore. Nearly all of the deposits are in the Lost Creek, Utopia, and Bald Mountain mining districts along the east and south margins of the Pioneer Mountains. The districts are less than 27 miles from Dillon, Mont.

Jan 1, 1960