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By R. G. Dressler

The Federal Bureau of Mines designed, constructed, and operated a demonstration plant at Louisiana, Mo., to produce gasoline, liquid fuels, and organic compounds from coal by a modified Fischer-Tropsch gas-synthesis process. Satisfactory equipment was developed to produce and purify synthesis gas and convert it into the desired products. Coal or coke was gasified with oxygen and steam to make a gas consisting essentially of carbon monoxide, hydrogen, and carbon dioxide. Dust in the raw gas was removed by cyclone separation, water scrubbing, and electrostatic precipitation. Carbon dioxide, hydrogen sulfide, and organic sulfur were removed with diethanolamine, iron oxide, and activated carbon. The gas was passed over iron catalyst and was converted into synthetic liquids, which were then separated and fractionated into gasoline, diesel oil, other liquid fuels, and oxygenated organic compounds. A 39-day continuous run demonstrated the feasibility of the process. Addition of 3 milliliters of tetraethylead per gallon of upgraded (or finished) gasoline gave a product with an octane rating up to 90 by the research method. After a caustic wash, the diesel oil was of a superior quality; its cetane number was 60 or above.

Jan 1, 1961

By F. P. Haver

The Federal Bureau of Mines developed a 10,000-ampere cell to determine the economic feasibility of producing high-purity electrolytic titanium from mill scrap or offgrade sponge. Operating variables were investigated, matetial handling procedures were established, and the cost of electrorefining titanium was determined. The prototype cell produced premium-grade metal (<100 Brinell hardness number (B.h.n.)) from very impure Kroll sponge at a processing cost of less than $0.60 per pound. Refined metal was deposited at the cathode in the form of coarse (85 percent plus 34-mesh), hexagonal crystals of a titanium when the cell was operated an 850° C. A cathode current density of 1,000 amperes per square foot and a molten sodium chloride electrolyte containing approximately 5 percent by weight of soluble titanium were used. In continuous operation, at the optimum number of ampere-hours, (40,000), the current efficiency averaged slightly less than 60 percent. It was possible to supply large enough amounts of electric current for electrolysis to maintain the temperature of the bath, thus reducing overall power consumption to less than 5 kilowatt-hours per pound of metal refined.

Jan 1, 1961

Comparative tests of four coals used industrially for coke production have been made by three laboratories of the Federal Bureau of Mines, each using its standard equipment and procedures for evaluating coal for coking. Two of the coals were blends used in the western and eastern sections of the United States, the third was a strongly coking coal widely used for producing coke in Alabama, and the fourth was a blend typical of those used for producing foundry coke in the Birmingham district. The coals used and the cokes produced from them covered a wide range of chemical and physical properties. The tests used at all three laboratories for determining the physical properties of the cokes were made according to ASTM (American Society for Testing Materials) methods. The excellent agreement found for the physical properties of the cokes indicated that, for the coals tested, the BM-AGA (Bureau of Mines-American Gas Association) 18-inch circular retort used at Pittsburgh, Pa" the 14-inch slot-type oven used at Denver, Colo., and the 17-inch slot-type oven used at Tuscaloosa, Ala., were substantially equivalent for evaluating coals for production of coke. Thus, added value is given to data obtained previously and independently at these three Bureau laboratories. INTRODUCTION Laboratory equipment to produce coke for evaluation has not been standardized by the industry. The results obtained with anyone design of equipment have been regarded as showing only the relative values of coal to produce coke of the requisite quality. Few systematic studies have been made to correlate results obtained in different types of equipment. Results of one, in which the Bureau of Mines participated, were published recently.2/ This

Jan 1, 1961

By Leland A. Yerkes

Refining aluminum from crude aluminum alloys by the subhalide reaction was investigated to develop a method of producing aluminum by means other than electrolysis of its oxide. The best materials and design for the apparatus and also optimum operating conditions, including temperature, pressure, vapor flow rate, and composition of alloy charge were studied. In the subhalide process, aluminum-trihalide vapor reacts with aluminum in the alloy under high temperature and low pressure, forming volatile aluminum monohalide which reverts to aluminum metal and aluminum trihalide on cooling. The only halide used in this investigation was aluminum trichloride. The crude aluminum-silicon alloys used as the principal raw material contained from 21.9 to 36 percent aluminum, and significant quantities of iron and titanium. These alloys were produced by direct electric smelting of clays. Graphite tubing that was heated by an induction coil proved to be satisfactory material for the laboratory reactor chamber, Enclosed in an insulated glass or quartz pipe, the reactor was used in both vertical and horizontal positions with various baffle and tray arrangements for directing the trihalide vapor both over and through the alloy. Aluminum trichloride vapor was generated in the sublimer at one end of the glass pipe, passed into the reactor where contact was made with the crude alloy, and aluminum monochloride gas was formed. When the gaseous mixture of aluminum monochloride and unreacted tri-chloride passed out of the reactor and entered the condenser, the gases were cooled to 900° C. or less, causing the monochloride to disproportionate into aluminum and aluminum trichloride vapor. The aluminum was deposited on the condenser walls while the aluminum trichloride vapor was carried out of the condenser and into the opposite end of the glass pipe where it solidified on the cooled copper coils.

Jan 1, 1961

By Miles B. Royer

The experimental blast furnace has attracted increasing interest during the past decade as a practical means for investigating a broad range of blast-furnace smelting problems. Under experimental-furnace conditions, information can be obtained with less expenditure of time and raw materials and, therefore, at lower cost than comparable information could be obtained under industrial operating conditions. Furthermore, the experimental furnace may be operated beyond the range of smooth operation, even to failure, to delineate the limits of operability. Such deviation from normal operating practice would be economically intolerable in industrial operations where production and operating stability might be disrupted. The Federal Bureau of Mines experimental blast furnace at Bruceton, Pa., near Pittsburgh, has been operated and under development since 1951. However, the usefulness of this experimental data to industrial practice was somewhat nebulous in early experiments, and the correlation of the experimental blast furnace with the industrial blast furnace was not known.

Jan 1, 1961

By Charles W. Huggins

Electron diffraction and electron microscopy were used to determine the unit cell parameters of garnierite [(Ni,Mg)3 Si2O5 (OH)4] and to examine its crystal habit. Bundles of ribbons, many less than 200 A. in cross section, make up the bulk specimen of the garnierite Electron diffraction revealed the unit cell to be monoclinic. Unit cell parameters were: a, 5.33 A,; b, 9.23 A.; c, 14.96 A.; and ß, 94°441.

Jan 1, 1961

By L. A. Stewart

This is one of a series of reports prepared by the Federal Bureau of Mines on mining methods, performance, and costs at individual mines in the United States. The primary purpose of these papers is to promote development and conservation of our mineral resources by disseminating technological information on methods, practices, and results that may be applied to the engineering analysis and solution of mining problems. This report discusses the highly selective mining methods of the Jaquays Mining Corp. at the Regal asbestos mine, 45 road miles northeast of Globe, Ariz. The milling method at the Globe plant is discussed briefly, and the extraction ratios of the various grades of fiber are tabulated. The proposed flowsheet of a new mill under construction is shown.

Jan 1, 1961

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1961

By N. H. Coates

As part of a joint program of the U.S. Atomic Energy Commission and the Federal Bureau of Mines for using nuclear energy to supply process heat, the Bureau designed and constructed a pilot-scale simulated nuclear reactor system. Although workable components were developed,5 the simulated nuclear reactor could not be operated continuously at its design conditions of 2,500°F. and 250 p.s.i.g. because the refractory materials used for insulation deteriorated. Replacement of these materials with porous carbon permitted sustained operation at design conditions, and a 1,000-hour demonstration run was completed successfully. No serious operating difficulties developed during the test. Leakage of helium after 1,000 hours was only 3 to 4 std. c.f.h. Inspection after the run revealed no damage to any of the components. Including earlier runs during previous research5 the system has been operated about 4,000 hours, of which 1,120 hours have been at 2,500° F. or higher. The helium-recycle compressor performed satisfactorily with no main¬tenance whatever for 2,445 hours, with about 2,000 hours at 900° to 1,000° F.

Jan 1, 1961

By J. S. Browning

The physical properties and specific gravity ranges of various liquids and salt solutions used for laboratory sink-float separations of rocks or minerals are presented. The test equipment and techniques employed by the Bureau of Mines in making sink-and-float separations of particles as coarse as 3 inches to as fine as 400 mesh are described. Also discussed are methods of recovering and reclaiming the liquids or salts from the minerals and wash solutions, as well as the hazards encountered and precautions to be followed while working with the materials. The laboratory use of various liquids for separating minerals of different specific gravities has been recognized for many years. During this time, laboratory sink-float procedures have proven their utility as a rapid and moderately accurate means for determining the mineral content of ores, test products, and plant products in certain nonmetallic concentrating operations, such as those producing mica, spodumene, kyanite, and so forth. These procedures also have been used as analytical tools for determining the mineral content and associations of other metallic and nonmetallic ores.

Jan 1, 1961

By J. H. Field

Synthesis of hydrocarbons by the Fischer-Tropsch reaction in a hot-gas- recycle system was demonstrated to be technically feasible. This project was undertaken, by the Bureau of Mines, to determine if the system was operable and to ascertain the optimum conditions for the production of gasoline. Carbon steel turnings packed with a void volume from 88 to 90 pct. were satisfactory catalysts, but steel catalysts with greater void volume, either turnings or steel wool, were not as active. Good temperature control with a pressure drop of less than 0.5 pounds per square inch (p.s,i,) per foot of catalyst bed of turnings was obtained by operating with a recycle to fresh feed ratio of 20 and by splitting the total gas flaw and injecting portions into the reactor at different entry ports.

Jan 1, 1961

By Perry G. Cotter

The borides of the transition metals in Groups IV and VI exhibit, in addition to a certain degree of hardness, considerable resistance to heat and oxidation. They have high melting points (1,850°-3,060° C.) and low coefftcients of thermal expansion and can be bonded with other materials and hot-pressed to desired shape (cermets). Suggested uses for the borides include use in rockets and jet engines, as thermocouple protection tubes, as containers for molten metals in die casting, as flame-plated coatings on less refractory compositions to prevent erosion by hot gases, and as control rods and neutron shielding material in nuclear engineering, The Federal Bureau of Mines investigation of zirconium diboride started in 1950 at the Boulder City Nev,, Metallurgy Research Laboratory, Its purpose was to reduce the cost of raw materials for the production of zirconium diboride.

Jan 1, 1961

By R. W. Van Dolah

An important function of stemming used to confine explosives in shot holes in underground coal mines is to minimize the chance of ignition of firedamp or coal dust by the detonation products. Until 1952, the Bureau of Mines approved only the use of fireclay or similar incombustible material for stemming permissible explosives. At least 2 feet of stemming were required except in holes less than 4 feet deep; in such short holes the stemming was required to be half the depth of the hole. Over the years, several special stemming devices have been proposed in the United States as substitutes for fireclay. Many economic and safety advantages were claimed for these devices, but only one approved device has been marketed in this country. Bureau requirements for stemming explosives in coal mines were modified at that time to permit the approved stemming device to be used as a substitute for the required fireclay.

Jan 1, 1961

By C. L. Klingman

In extracting helium from natural gas at Bureau of Mines helium plants, a continuous analysis of the helium content of inlet and outlet gas streams is required to determine extraction efficiency. An analyzer, using established principles of gas chromatography to effect the analysis, has been developed by the Bureau of Mines to meet this need. It will record the helium content of inlet or discharge gases from helium-extraction plants every five minutes, continuously, without the attendance of an operator. A 25-inch column of activated charcoal is used as a partitioning agent; nitrogen is the carrier gas; and a hot-wire, thermal-conductivity cell is the detector. A 1.0 mv, strip chart indicates the unbalance of the detector cell, Sample size is 0.37 cc, and carrier gas flow rate is 75 cc, per minute. Significant improvements in helium extraction have been demonstrated by using the chromatograph in three helium-extraction plants.

Jan 1, 1961

By Ruth F. Brinkley

This report is the 18th of a series of reports originally issued annually, and more recently bienially, to acquaint the public with the work of the Federal Bureau of Mines in explosives technology. Part I reviews briefly the overall activities during fiscal years 1957 and 1958.4/ Part II presents in abstract form the publications prepared by the Bureau that appeared during the period.5/

Jan 1, 1961

By Max J. Spendlove

The secondary copper industry is comprised of numerous enterprises which collectively employ many of the recovery and refining processes now used in primary plants as well as many other processes that are unique to the industry. Effective methods are used for identifying and segregating all types of scrap according to widely accepted standard classifications. Segregated scrap and waste materials usually require some preliminary processing to remove both valuable and deleterious associated constituents. Smelting, melting, alloying, and pyrorefining are common methods used for producing secondary metal, but operating techniques usually differ from primary metal operations because of the difference in physical and chemical properties of the respective raw materials. Some copper scrap is converted to copper chemicals rather than to refined metals or alloys. Recovery efficiencies of all processes are reasonably high, and the quality of products meets rigid specifications.

Jan 1, 1961

By Kenneth H. Johnston

Records show that waterflooding was tried in Osage County as early as 1934, but it was not economically important until a large unitized flood in the North Burbank field was begun in 1950. Development was rapid and by the end of 1960, there were 70 active water flood projects and 16 active pressure-maintenance projects in the County. The locations and status of the water-flood and pressure-maintenance projects in Osage County on December 31, 1960 are shown in figure 1, and information pertaining to these projects as of July 1, 1960 is given in table 1. For the past several years, Bureau of Mines petroleum engineers have arranged tours of selected waterflooding projects for the spring meeting of the Kansas-Oklahoma Water flood Association. These tours are conducted to demonstrate unique operating methods and new field equipment and to provide additional opportunities for exchanging information. Each of these tours has been supplemented by a published report describing in detail the projects visited. This report has been prepared for distribution during the 1961 spring tour of three waterflooding projects and a pressure-maintenance project in Osage County, Okla. (fig. 2).

Jan 1, 1961

By K. K. Kershner

This report describes an investigation by the Bureau of Mines designed to provide background data for extending and improving the applications of chlorine metallurgy in extracting metals from ores. Optimum conditions are given tor chloridizing galena, sphalerite, and chalcocite by contact with chlorine gas. Petrographic and chemical analyses of the sulfides used in the experiments are listed. Graphs are furnished showing the extent of chloridization of each metal sulfide over the temperature range of the observations. In each case, the first tests were made with the reaction chamber at room temperature. This temperature was increased by regular increments in succeeding tests until the temperature was reached at which quantitative conversion of the sulfide to chloride was observed. The data are also plotted for screen-size fractions of the sulfide minerals investigated. Data show that the extent of metal chloride formation was affected by chloridization time, particle size of the sample, and usually, the temperature of the reaction chamber. At 300° to 400° C. an anomaly was noted for both galena and sphalerite. The temperature at which this anomaly was observed varied according to the particle size of the mineral. Comparisons are made between the chloridizing characteristics of the mineral sulfides and their chemically prepared counterparts.

Jan 1, 1961

By G. V. Sullivan

This report summarizes the results of metallurgical investigations by the Federal Bureau of Mines of manganese oxide ore, averaging 23 to 25 percent manganese, stockpiled at the Butte-Philipsburg depot of General Services Administration (GSA). The oxide ores were stockpiled in two general classifications, straight oxide ore and mixed oxide-carbonate ore. Continuous-circuit flotation tests at the Albany (Oreg.) Metallurgy Research Center of the Bureau of Mines showed that each of these ore types could be concentrated by an oil-emulsion scheme to produce a concentrate that could be sintered to meet program specifications. About 88 percent of the manganese was recovered in the concentrate from the straight oxide sample, with the sintered concentrate containing 48 percent Mn. The sintered concentrate from the mixed oxide-carbonate sample contained 41 percent Mn with a recovery in the concentrate of 95 percent.

Jan 1, 1961

By M. E. Tyrrell

Despits its high melting point (2,135° C.), resistance to attack by molten metals, and its hardness (8), spinel (MgO?Al203) synthesized by the fusion of alumina (Al 2 0.) and magnesia (MgO) is not used on a large scale as a commercial furnace lining, mainly because of the prohibitive cost. This investigation by the Federal Bureau of Mines was prompted by the possibility of producing synthetic spinel from inexpensive raw materials by methods outlined in U.S. Patent 2,029,773, "Process for Obtaining Products Containing Spinets," dated February 4, 1936. In this patent Ture B. Haglund described a process for recovering crystalline spinels from melts in the system Mg0?Al203-2CaO-SiO2, a system well suited to the use of starting materials such as dolomite CaMg(C03)2, olivine [2(Mg?Fe)0.Si02], and bauxite (Al203?2H20) which are abundant in the southeastern United States. Compositions, ranging from a low content in the eutectic mixture of 35 percent spinal and 65 percent dicalcium silicate (2 CaO?SiO2) to a high of 75 percent spinel and 25 percent dicalcium silicate, were fused in electric furnaces of the arc-resistance and internal-resistance types. So long as members of the system were in proper chemical balance, "dusting" slags could be produced over the entire range of spinel concentration.

Jan 1, 1961