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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 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 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 A. L. Engel

This report describes laboratory-scale experimental treatment of six base-metal ore samples taken by engineers of the Bureau of Mines, Region II, while investigating ore deposits in California and Nevada. The information is of interest in developing the mining districts represented or when similar ores from other sources are being studied. Simple treatment methods were employed as far as possible. More complex treatments also were tried when necessary. The possibilities and limitations of the methods applied to the several ores are shown by the data herein reported.

Jan 1, 1960

By R. V. Higgins

As part of a study of application of the Buckley-Leverett method to an analysis of oil-reservoir performance covering a wide range of relative permeabilities and oil saturations, a method has been devised for quickly deter-mining average water saturation at breakthrough from relative permeability data. The base for the relative permeability used in the report is either the permeability to air or the effective permeability to oil at the irreducible water saturation. The permeability to air also was used because of the large backlog of air permeabilities available to reservoir engineers. The basic data were calculated by an electronic computer and are presented in a single graph from which the point of breakthrough may be obtained. In this study the water saturation at the beginning of the depletion is the connate or interstitial or irreducible water saturation. These water saturations are considered to be synonymous and to have a practical value.

Jan 1, 1960

By T. E. Gray

This report describes the preparation characteristics of the more significant coalbeds in Monongalia County, W. Va. It is one of a Bureau of Mines series planned to determine coals suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.5 million tons of coal was produced in Monongalia County in 1957, of which more than 7 million tons was cleaned mechanically in 8 cleaning plants. On January I, 1954 the Bureau of Mines estimated that 1,576 million tons of recoverable coal remained in the county in beds 28 inches or more thick.

Jan 1, 1960

By J. H. Holden

The Federal Bureau of Mines is doing research and development work on a pressure-gasification pilot plant for producing synthesis gas directly from pulverized coal, oxygen, and steam. A pressure-gasification pilot plant has been constructed, and an investigation was made with the following basic objectives: 1. Determining the effect of varying pressure (75, 100, 150, and 300 p.s.i.g.), coal rate (400, 700, and 1,000 pounds per hour), and oxygen-to-coal ratio (8 to 11 std, c,f. per pound), on percentage of carbon gasified, oxygen and coal requirements per unit of CO + H2 produced, exit-gas temperature, and heat loss. The steam-to-coal ratio was maintained at approximately 0.3 pound per pound. 2. Development of a stabilized gasification zone or reaction space. 3. Improvement in operability of the pilot plant.

Jan 1, 1960

By C. M. Frost

Two Federal Bureau of Mines recycle hydrogenation experiments to prepare catalytic cracking feed stock were made at 3,000 pounds pressure with crude shale oil retorted from Green River (Colo.) shale in the gas-combustion retort. The hydrogenated product from the first experiment, made at 784° F., was used for investigating the effects of nitrogen content on catalytic cracking yields and for determining the quality of the catalytically cracked gasoline. Hydrogenated product containing 0.14 percent or more of nitrogen produced less gasoline when cracked in a CAT "A" unit than was obtained from East Texas light gas oil cracked at the same conditions; product containing 0.10 percent or less nitrogen produced a quantity of cracked gasoline equal to that obtained from the East Texas light gas oil. The catalytically cracked gasoline had research octane numbers calculated to be approximately 95 clear and 103 with 3 ml. of tetraethyl lead. The principal product from the second experiment, made at 828° F., was a low nitrogen content gas oil which was used for investigating the yields of cracked products obtained when it was catalytically cracked to different degrees of conversion. Yields of cracked products, when plotted as functions of conversion, were essentially the same, within the experimental range of the data, as published yields from catalytic cracking of East Texas heavy gas oil; however, yields from cracking the shale-oil product did not display the sensitivity to change of cracking temperature that has been found for East Texas gas oil.

Jan 1, 1960

By Oliver C. Fursman

This work was conducted to determine the feasibility of producing aluminum-silicon alloys in a pit-type, three-phase electric-arc furnace. Two carbon-lined furnaces were used in the tests. The power input ranged from 120 to 240 kw. in the small furnace and from 420 to 460 kw. in the large furnace. Energy consumption ranged from 5.3 to 11.5 kw.-hr. per pound of alloy produced and electrode consumption, from 240 to 510 pounds per ton of alloy produced. A wide range of crude aluminum-silicon alloys was produced by direct smelting of clays or similar aluminum silicate raw materials, using hogged fuel or wood chips as the major source of carbon in the furnace charge, and silicon of high grade was produced by smelting quartz. The aluminum content of the aluminum-silicon alloys ranged from 15 to 55 percent. Alloys produced from a white opaline-silicate clay were relatively free of iron, titanium, and other impurities. Those produced from western fire clays and kyanite, although richer in aluminum, contained considerable amounts of impurities. The purity of the alloys depended largely on the composition of the raw materials.

Jan 1, 1960

By W. L. Hunter

This report describes results of beneficiation and smelting studies conducted by the Federal Bureau of Mines on chromite samples from the Emma Belle and Seiad Creek prospects in the Seiad Creek area, northern California. Samples were chosen from this area because the ore is typical of disseminated types that represent a sizable domestic reserve. The two samples were similar in composition, and both responded in like manner to gravity beneficiation. As the ore was banded, considerable coarse gangue was rejected in laboratory sink-float from a minus-3/4-inch, plus-6-mesh fraction without excessive chromium loss at a medium density of 3.32. An average of 85.6 percent of the chromium was recovered in the sink product, which analyzed 35 percent chromic oxide (Cr203). Tabling yielded concentrates containing 49 percent or more Cr203; however, recoveries, ranged from only 33 to 45 percent. A combination of tabling and electrostatic separation of the table middlings showed that the chromium recovery could be increased to about 73 percent; the composite concentrate averaged 53 percent Cr203.

Jan 1, 1960