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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

By Joel N. Van Sant

THIS REPORT describes the occurrence, mining, and use of refractory clay in Colorado within Region III of the Federal Bureau of Mines, which includes the States of North arid South Dakota, Nebraska, Wyoming, Colorado, Utah, New Mexico, and Arizona. Field work by the Bureau of Mines, United States Department of the Interior, included examination of active and abandoned refractory-clay mines as well as a reconnaissance survey and sampling of numerous clay-bearing formations exposed in Colorado. Information from the survey and the sampling will help guide private industry in its search for virgin sources of refractory clay. Library research of published and unpublished reports from various Federal, State, and private sources was conducted during the early phase of the investigation. Most of the refractory clay mined in the Denver-Golden district of Colorado is not used for refractory purposes but is blended with other clays in the manufacture of structural clay products. The predominantly flint-clay de-posits in the Pueblo and Fremont County districts are mined and utilized chiefly in fabricating refractory products.

Jan 1, 1959

By J. B. Zadra

Tungsten metal, chemically equivalent to commercial grade, is produced by electrolysis of impure tungsten compounds or scheelite in an alkali, phosphate or borate electrolyte. A preliminary investigation of fused-bath electrolysis shows the effect of electrolyte composition, temperature, and current density on current efficiency, yield, crystal structure, and purity of product. Experiments show that tungsten can be electrowon from scheelite in a fused alkali, phosphate, or borate bath with similar results. Studies on electrolyte composition show that the addition of sodium chloride is essential to both electrolytes in treating scheelite. Although its main function is to react with or flux the CaO, it also increases the bath fluidity. Temperature studies revealed optimum ranges between 900° and 1,100° C.; 900° C. proved satisfactory for tungsten trioxide, and 950° to 1,050° C. for scheelite. Current efficiencies were satisfactory for all current densities ranging from 10 to 57 a./dm.2. Yields were 400 to 650 g./kw.-hr. over the same current-density range. Crystal size and purity of the product are functions of temperature, current density, and amount of impurities in the electrolyte. Deposited crystals vary in shape from spherical grains to clusters of dendritic hexagonal needles, and in size from smaller than 35 to 570 microns. The purity of the tungsten metal produced ranges from 99.7 to 99.94 percent.

Jan 1, 1959

By E. D. Calvert

Molybdenum has been successfully cast into static and rotating molds in conventional equipment used for casting titanium and zirconium. Melting was accomplished by using an arc potential of 36 to 40 volts with a current of 10,000 amperes. Pouring efficiency, after a skull had been formed in the crucible, averaged 70 percent. Techniques are described by which four successful castings were made. Tensile properties on specimens cut from one centrifugally cast tube averaged: Tensile strength, 39,800 p.s.i.; yield strength (0.1 pct. offset), 35,300 p.s.i.; elongation, nil; reduction in area, nil; impact strength, 2 ft.-lb.; hardness DPH (diamond pyramid hardness) 180. Mold reaction was not evident in shapes cast in machined graphite. This was not true, however, for rammed graphitic-base molds.

Jan 1, 1960

By R. F. Tenney

This report has been prepared because little detailed information has been published on the production and use of anthracite producer gas for industrial-process and brick-kiln heating. To obtain this information, an investigation was conducted by the Federal Bureau of Mines in cooperation with a building-brick manufacturer (firing both periodic and tunnel kilns with anthracite producer gas) and with a manufacturer of anthracite-gas producers. In addition to a study of available plant records, 2 weeks was spent in systematic observation and measurement during regular operation of the Hazleton Brick Co. plant, Hazleton, Pa., in July 1953. This report presents the results of this investigation and a description of producer and periodic-kiln equipment, operating procedures, and labor requirements. A summary of the conditions of producer and kiln operation is given for the 2-week observation and for the 11 preceding months. The two 10-foot standard anthracite-gas producers consumed 301 tons of Rice and Buckwheat No. 1 anthracite, as delivered, averaging over 13,000 B.t.u. per dry pound during the 2-week period, with a producer hot-gas efficiency of 95 percent, at an average gas offtake temperature of 5400 F. The yield of gas5/ of 153 gross B.t.u. per cubic foot amounted to 140,000 cubic feet per ton of fuel as fired, or 73,500 cubic feet per kiln heating hour, which was sufficient for kiln requirements.

Jan 1, 1960

By H. R. Shell

Variations between laboratories on the silica and alumina content of calcined kyanite led to this Bureau of Mines study of the extent and nature of the differences. In particular, Bureau scientists hoped the study would lead to correction of the causes of the dissimilarities. A sample of calcined Kenya kyanite was analyzed by seven different laboratories familiar with silicate analysis. The compiled data indicated differences originating from lack of recovery of silica after two acidic dehydrations, from high alumina caused by several factors, from loss or gain of iron during sample fusion, and from indifference regarding the accurate determination of minor constituents.

Jan 1, 1959

By Robert L. Rough

This report presents the results of an investigation by Federal Bureau of Mines engineers of water-injection projects in the northwestern Pennsylvania and southwestern New York area, where oil-producing wells have been converted from pumping to flowing. Data from 24 leases converted to flowing were collected and examined. Only 10 leases had information of significant scope for inclusion in the final analysis. The projects were classified in one of two categories. Group I consisted of leases operated to permit an evaluation of operational changes in terms of existing pressure differentials between injection and producing wells. Group II included remaining properties, for which enough information was available to justify an economic analysis but which did not have sufficient production data to support an engineering study because of radical changes in operational techniques. Variations in production and costs resulting from conversion to flowing were examined for production methods, well-spacing and completion techniques, and reservoir characteristics. Where water-injection rates were constant, oil production usually decreased rapidly at the time of conversion; production then increased slightly for 6 to 8 months before resuming a normal decline rate considerably below the estimated pumping rate. The abrupt decrease in production after conversion is indicative of lower pressure differentials between injection and producing wells, caused by the increased hydrostatic head in the producing wells.

Jan 1, 1960

By G. R. Strimbeck

The Federal Bureau of Mines has been developing processes for producing synthesis gas directly from coal, oxygen, and superheated steam. An atmospheric-pressure pilot plant was constructed and operated to: 1. Determine the operability of the plant for gasifying coals of different ranks under various operating conditions. Listed in decreasing order of rank, these coals included a Pennsylvania anthracite, a bituminous A coal from the Sewickley bed, West Virginia, and a subbituminous C coal mined in the Lake de Smet region of Wyoming. 2. Determine the effect of varying operating conditions on: (a) Standard cubic feet (std.c.f.) of oxygen and pounds of coal of different rank required to make M std.c.f. of product gas (carbon monoxide plus hydrogen); (b) carbon gasified, percent; (c) exit-gas temperature, degrees F.; and (d) heat loss, B.t.u. per pound coal. 3. Compare the gasification characteristics, indicated in item 2, of coals of different rank: Bituminous A, anthracite, and subbiturninous C. 4. Determine the concentration of dust in the gases produced and the efficiency of dust removal, and investigate the relation between the sulfur content in the coals gasified and the gases produced.

Jan 1, 1960

By R. W. Stahl

Increasing use of continuous miners, especially the boring type, has focused attention on the inadequacy of face ventilation in coal mines. The bulk of the machine, the rapid advance of working faces, and the increased liberation of methane from the larger expanse of freshly exposed coal surfaces have created ventilation problems that were unknown with conventional mining equipment. Ignition of gas, especially that caused by machine bits striking hard rock or pyritic inclusions, have increased at an alarming rate. As the mines penetrate beds under thicker cover at an ever-increasing rate of face advance, this problem will probably increase unless face ventilation is improved. A previous survey, described in Bureau of Mines Report of Investigations 5414, Auxiliary Ventilation of Continuous Miner Places, disclosed that auxiliary fans with tubing generally improved circulation of air and removal of gas at the face. The study here reported attempts to examine, face ventilation at various mines and to note any plan or innovation of. air coursing that industry might adopt to reduce the danger of gas ignition. ACKNOWLEDGMENT The mines visited were very cooperative in the study-and-generously supplied any data requested.

Jan 1, 1960