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By Sidney Katell

An economic analysis of underground gasification of coal, based on experimental results obtained by the Bureau of Mines, indicates that a gas suitable for use in a power plant might be produced for approximately $.62 to $.77 per million British thermal units. This estimate does not include cost of land purchase. The gasification experiments were conducted in a 3-ft. seam of high volatile A bituminous coal. The major factors which can influence a change in operating costs are height of overburden, power costs, thermal efficiency, and the gasification air inlet pressure. The following equations show the relationship of these factors to operating costs:

Jan 1, 1961

By D. Bienstock

A high-B.t.u, gas can be synthesized by the catalytic methanation of a mixture of 2.5 to 3 parts of hydrogen to 1 part of carbon monoxide, obtained in the gasification of coal, using a steel catalyst followed by Raney nickel in a hot-gas-recycle system. Conversion of 99 percent of the H2+CO yields a fuel gas with a heating value of 983 to 1130 B.t.u. per cubic foot containing 78 to 96 percent methane, no carbon monoxide, and very small amounts of unsaturated hydrocarbons. With the steel catalyst alone, conversions were 85 to 90 percent, giving a fuel gas of 810 to 868 B.t.u, per cubic foot, or 847 to 975 B.t.u. on a C02-free basis. INTRODUCTION In 1948 the U.S, marketed production of natural gas was 5.15 trillion cubic feet; by 1958 it had reached 11.0 trillion cubic feet, a rate of growth of 8 percent annually. 4 5 Although demand is expected to increase less rapidly, by 1966 it may reach 16 trillion cubic feet, based on an estimated 4.7 percent annual increase.6

Jan 1, 1961

By Perry G. Cotter

The objective of this investigation was to synthesize and investigate the properties of a high-temperature refractory material based on a combination of boron, silica, and magnesium. A magnesium-thermic reaction was used for the synthesis. X-ray examination of the product indicates that the crystalline portion of the composition is a combination of magnesium borides, magnesium silicate, and magnesium orthoborate. Chemical analysis of a representative sample shows, in weight-percent, boron 17.6, silicon 23.9, magnesium 17.8, and chromium 0.5. The balance is largely oxygen. The composition is resistant to high temperatures under oxidizing conditions and is stable in water, hydrochloric acid, and hydrogen. It has a low density (less than 3 grams per cubic centimeter) and a hardness value in the range of quartz. It has a melting point above 1,700° C. and can be hot-pressed to shape in the temperature range between 1,200° and 1,350° C. The properties described in this paper indicate that the material may have some uses as a high-temperature refractory, and because of its boron content it may have some value as a thermal-neutron-absorption material.

Jan 1, 1961

By S. L. May

Investigations by the Federal Bureau of Mines indicate that hafnium and zirconium compounds of acceptable purity can be extracted from Nigerian zircon concentrates. Chlorination and caustic soda fusion techniques were used to extract 85 to 95 percent of the valuable metals from the concentrate. The extracted hafnium and zirconium compounds were purified by recrystallization of the oxychlorides or by formation of complex salts during chlorination. The zirconium-hafnium product of the recrystallization method contained 15 parts per million of uranium, and the product of the salt-complex method contained less than 10 parts per million of uranium. The hafnium was separated from zirconium by solvent extraction methods. A zirconium product containing 0.3 percent hafnium and a hafnium product containing 4 percent zirconium were obtained. At the request of the Atomic Energy Commission (AEC), work was started to develop techniques for processing Nigerian zircon concentrates in commercial installations presently engaged in producing zirconium and hafnium metals from ores. The Nigerian zircon has a high hafnium content, but the presence of uranium and thorium is a problem not normally encountered in processing zircon concentrates.

Jan 1, 1961

By W. P. Haynes

The Bureau of Mines has been studying a modified steam-iron process using coal-derived producer gas for making either hydrogen plus carbon monoxide or methane. To provide a guide for this experimental study, compositions of equilibrium product gases for the reaction of steam plus carbon dioxide with iron were calculated and are discussed in this report. The calculations, which are described in this report, are based on thermodynamic data in the literature and cover temperatures from 800° to 1,300° K., pressures from 1 to 30 atmospheres, and hydrogen-to-carbon atomic ratios in the gas of 4 to 12. The equilibrium gas compositions are discussed in regard to making hydro-gen, carbon monoxide, and methane in the oxidation step of the modified steam-iron process. From the viewpoint of thermodynamics alone, assuming the reactions reach equilibrium, the discussion considers the effects of temperature, pressure, and composition of feed gas upon the composition of the product gas, the degree of oxidation of the iron, and the possible deposition of carbon. The results indicated the following: (1) Nearly all the carbon can be converted to methane at low temperatures (800° to 900° K.) and high pressures (over 20 atmospheres); (2) to obtain high yields of synthesis gas, high temperatures are required. For example, at 30 atmospheres, a temperature over 1,200° K. is required to convert 60 percent of the steam plus carbon dioxide to hydrogen plus carbon monoxide. Lower temperatures may be used at lower pressures) (3) oxidation of the iron increases with increasing pressure and decreases with increasing temperature; and (4) process conditions favoring carbon deposition were found within the range of variables studied, but it is thermodynamically possible to operate the oxidation process with steam and carbon dioxide outside this range of carbon deposition.

Jan 1, 1961

By Bernard Porter

The solubility of UO2 was determined at 1,250° C. in ternary melts of UF4 and BaF2 with CaF2, LiF, and SrF2. The solubility of Ce02 was measured at 800° and 850° C. in a solution of CeF3, BaF2, and LiF. The amount of La203 which dissolves at 950° C. in a binary mixture of LiF and LaF3 and a ternary of LiF, LaF3, and BaF2 was also measured. In each case, the amount of soluble oxide was mound to be less than 5 weight-percent. A procedure was developed for filtering fused, oxide-saturated fluoride melts in order to obtain a representative sample for chemical analysis. The oxide content of the samples was determined by an inert-gas fusion procedure.

Jan 1, 1961

By Alton B. Cook

The practice of using partly depleted oil reservoirs for gas-storage operations is proving successful. Moreover, this practice provides a method of secondary oil recovery when gas is cycled at full-storage reservoir pressure. Because of the relative newness of this operation, a study was undertaken to assist engineers in developing improved gas-injection and production procedures and in calculating the amount of gas needed for completely repressuring reservoirs. This paper is the third in a series reporting the progress of a study by the Federal Bureau of Mines of reservoir performance during complete gas repressuring and gas cycling. A procedure for estimating secondary oil recovery by this method is also under study. One report (7)3/ describes the laboratory equipment. The other report (8) gives (1) data on the New York City field, Clay County, Tex., which has been converted to gas-storage operations; (2) laboratory data from research with a model oil reservoir, in which primary production, complete gas repressuring, and gas cycling for the New York City field were simulated; and (3) theory to explain reservoir performance during gas repressuring.

Jan 1, 1961

By M. A. Hammer

In this study by the Federal Bureau of Mines Pennsylvania anthracite from the Eastern Middle field was oxidized by concentrated nitric acid at steam-bath temperature for 24 to 1,000 hours. The quantitative data obtained include yields of nitric-acid soluble and insoluble products and the distribution of carbon and ash in each. The acid-insoluble residues were examined for solubility in aqueous sodium hydroxide. With a sodium hydroxide concentration of at least 1 normal, a portion of the residue could be extracted in the form of a true solution. With lower alkali concentrations, peptization occurred. Alkali solubility of the residue increased with length of oxidation. However, when expressed in percentages of original coal weight, the alkali solubility remained essentially constant after 192 hours of oxidation. This suggests that the alkali-soluble products are converted to acid-soluble products at the same rate as the original coal substance is converted to alkali-soluble material. Microscopic observations of the peptization of the acid-insoluble residues revealed a gross micellar physical structure. The action of nitric acid is apparently not restricted to the surface of a coal particle. The acid penetrates the particle through the pore structure, dissolving some of the ash and altering the bonds between the coal micelles. The bond alteration, as indicated by ultimate analyses, involves the physical and chemical adsorption of the components of nitric acid. Some of the altered bonds are not thermally stable; this instability is shown by the complete loss of peptizing ability when the acid-insoluble products are heated above 200° C. This loss is accompanied by the evolution of water, oxides of nitrogen, and hydrocyanic acid.

Jan 1, 1961

By E. Morrice

This report of the Federal Bureau of Mines presents a laboratory procedure, with the requisite equipment, for electrowinning ingot (liquid) cerium metal from a fused-fluoride bath, the metal purity being about 99.9 percent. Physicochemical studies, including bath properties and electrochemistry, are included, with a speculative model of the mechanisms involved. An historical review of the methods used for electrowinning misch metals and yttrim-group metals, as well as individual rare-earth metals, is presented. The electrolytic preparation of metal from fused salt and nonaqueous media is summarized, along with the unsuccessful attempts at depositing the metals from aqueous solutions.

Jan 1, 1961

By Harvard Eng

An industrial survey was made for the Missouri Basin Field Committee of the Department of the Interior to determine the type and quantity of water-borne mineral wastes and the water requirements of metal-processing industries in the basin in Kansas and western Missouri. Data are presented on metal-processing plants visited through June 30, 1959. Most of the plants were in the greater Kansas City area. This report is to be supplemented with a similar publication on other industries, including those producing sand and gravel, coal, petroleum, and chemicals. In 1958, 19 million pounds of waste materials was discharged from metal processing industries. Approximately 14 million pounds of this waste was in the form of ferrous sulfate, and 2 million pounds was ferric phosphate. Galvanizing, other hot dipping, and automotive industries contributed the greater part of iron compounds wasted; some of this waste occurred as sludge that was not discharged to water courses but was hauled to refuse dumps, podium was present in nearly all industrial wastes, and the total of more than 900,000 pounds constituted one of the larger material losses. Although small in quantity, electroplating and allied coating wastes contained metals that were expensive when originally purchased.

Jan 1, 1961

By A. E. J. Gallagher

This report summarizes the results of flotation studies conducted by the Federal Bureau of Mines on samples of extremely fine-grained lead-zinc sulfide ores. Samples from five ore deposits in the Pine Creek area, Coeur d'Alene district, Idaho, and one deposit in the Metaline district, Washington, were studied at the Albany Metallurgy Research Center to determine the recovery of sulfide lead and zinc by flotation. During the investigation it was found that flotation could be effectively applied to the selective recovery of exceedingly fine-grained lead and zinc sulfide minerals. Separation of galena and sphalerite was obtained on pulps ground through 1,600-mesh, in which most of the particles were smaller than 5 microns. Selectivity and recovery of minerals in this fine size range were enhanced by use of a chemical dye, diphenylthiocarbazone, as a galena promoter. Although unsuccessful on one ore, application of the dye in treatment of two other very fine-grained ores yielded lead concentrates containing over 62 percent Pb at recoveries in excess of 85 percent. More than 55 percent of the lead in these concentrates occurred as particles smaller than 2 microns.

Jan 1, 1961

By M. D. Carver

The purpose of this investigation was to determine the effects of variations in content (near the residual level) of the impurities aluminum, nitrogen, manganese, and copper on the corrosion rate in pressurized hot water and in pressurized steam of zircaloy-3, a zirconium-base alloy of 0.25 percent tin and 0.25 percent iron. Thirty-five 10-pound ingots were cast with the appropriate additions of impurity elements, and these were converted to wrought sheets. These specimens were then tested both in water and in steam. The analysis of the resulting data showed that in environments of either pressurized hot water or superheated steam, corrosion rates increased with increasing content of aluminum, nitrogen, or manganese, but were not affected by variations of copper. The effects of aluminum and nitrogen were found to be greater than the effect of manganese. INTRODUCTION At the request of the Atomic Energy Commission (AEC) in August 1956, the Federal Bureau of Mines, in cooperation with Bettis Plant of Westinghouse Electric Corp., began investigating the effects of certain impurity elements on the corrosion rates of zircaloy-3 in pressurized hot water and in pressurized steam. It was necessary to know these effects in order to set control limits on residual impurity levels in zirnaloy-3, intended for heat transfer service in the nuclear reactor of the pressurized water type. A factorial expert it was designed by Westinghouse statisticians. The Atomic Energy Commission provided raw zirconium sponge purchased from Wah Chang Corp. The Bureau's laboratory at Albany, Oreg., made material of different combinations of impurity levels and subjected the material to corrosion tests. This report will describe the work done at the Bureau laboratory and will show, quantitatively the effects of different residual levels of aluminum or nitrogen, or manganese or copper on corrosion rates.

Jan 1, 1961

By F. E. Armstrong

This report describes development and application by the Bureau of Mines of techniques and instruments for using radioactive inert-gas tracers to determine flow paths through petroleum reservoirs that have natural fracture systems and for which water injection has been selected as the stimulative production method. A field test was made to prove the techniques and evaluate instrumentation. The feasibility of applying the techniques and instruments to the solution of reservoir problems in other stimulative methods of production also is discussed. Oil commonly is displaced from sandstone host rocks by the action of a driving force that causes the oil to move through interstices of the rock and into production wells. In addition to the requirements of oil being trapped within the sand pores and the presence of an effective displacement mechanism, the rock itself must have adequate permeability to permit flow of oil and other fluids.

Jan 1, 1961

By Wilbur I. Duvall

Surface vibrations of ground, rock, and structures resulting from blasting or other sources are often measured with portable seismographs. These instruments are usually supported by a three-point mount or tripod which is simply placed on a horizontal surface on which vibration levels are to be measured. The rigid-body motion of a tripod-supported seismograph is considered from the point of view that there should be no slippage of the feet with respect to the surface and none of the feet should leave the surface as a result of imparted motion. From these studies the following design criteria are deduced which assure that the seismograph will respond accurately to vibration levels as large as 1/2 g.:3/ First, the coefficient of friction between the feet and the surface on which the instrument rests should be as large as possible, preferably approaching unity; second, the center of gravity of the instrument should be vertically above the centroid of the three-point mount; and third, the vertical distance between the center of gravity of the instrument and the centroid of the three points of contact with the surface should be less than the perpendicular distance between the centroid point and anyone of the three sides of the triangle formed by the three points of contact. Portable seismographs that do not satisfy these conditions should be clamped to the surface if vibration levels above 0.1 g. are to be recorded.

Jan 1, 1961

By M. D. Schlesinger

As part of the development of processes for producing synthetic fuels from coal, the Bureau of Mines prepared a special jet fuel in a pilot plant for evaluation by the Air Force. This jet fuel had all the required physical properties, including the important specifications of high heating value and high density. However, the finished fuel did not pass the stability test specified by the Air Force and conducted by the Southwest Research Institute in a high-temperature research coker. The cause for this instability is being investigated because pure compounds of the type identified in this fuel are known to be stable. The tar acid oil used was a 230° to 300° C. fraction of low-temperature tar obtained by carbonization of a West Virginia bituminous coal in the pilot plant of the Consolidation Coal Co. Both the desulfurization at 400° C. and saturation at 300" C. were done in the vapor phase at 2,500 p.s.i.g. After catalytic treatment and distillation the final jet fuel had a boiling range of 194° to 247° C., a net heating value of 18,420 B.t.u./lb. and a specific gravity of 0.8463 60° F./60° F. It also had u pour point below -62° C., and at 0° C. its viscosity was 4.5 cs. The oil was virtually all bicyclic, 41 pct. noncondensed and 56 pct. condensed.

Jan 1, 1961

By M. J. Ackerman

This study was undertaken to make a comparison between the cost of mining coal under roof bolt and under conventional timber methods of roof support. Studies were made at 14 mines in Pennsylvania, eastern Ohio, and northern and southern West Virginia. At each mine data were obtained for sections of the mine where the physical conditions, mining equipment, and mining systems were similar. Coal, recognized as one of the basic industrial fuels, is very competitive with other fuels, and management, in order to protect and enlarge its market, must be continually alert to find more efficient methods of production. Continuous production of coal is desired by all operators but never obtained. In mechanized mining the performance and production vary with operating time, which can be interrupted by many variable factors, such as condition of the roof, method of roof support, condition of equipment, water, ventilation, power, transportation, efficiency of operating crew, and supervision.

Jan 1, 1961

By Donald F. Smith

This report describes the construction and calibration of two ice calorimeters and includes results of high-temperature heat-content measurements, made by the Federal Bureau of Mines, on rubidium fluoride, hafnium tetrafluoride, cesium chloride, and cesium iodide. The heats and entropies of fusion of rubidium fluoride, cesium chloride, and cesium iodide have been calculated at their respective melting points using equations derived from the experimental heat-content data. Hafnium tetrafluoride did not melt within the range of temperatures investigated. Heat and entropy of transition of cesium chloride from the alpha to the beta form were also determined. INTRODUCTION Free-energy data usually afford the cheapest and quickest means of determining the feasibility of experimentally untested reactions. For known reactions, free-energy data show the variation of the equilibrium constant with temperature and make it possible to calculate, without experiment, the maximum ratio of product to raw material for a given chemical process.

Jan 1, 1961

By J. B. Gayle

During the past several decades, there has been a steady increase in the number and size of experimental ovens used for carbonization research. Although many were originally intended principally for studies of coal expansion, current practice usually includes determinations of the properties of the experimental cokes. With respect to size and shatter characteristics, the cokes from the larger experimental ovens closely approximate those from duplicate charges carbonized in commercial ovens; however, they are consistently lighter and frequently less resistant to degradation by abrasive forces. To minimize these differences, some operators dry the experimental charges before carbonization. The resulting higher dry coal charge densities do, in fact, yield cokes with gravities closely approximating those produced commercially from the same coal or blend but without drying. The drying of the experimental charges may be criticized on the grounds that it represents a departure from commercial practice and may result in oxidation of the samples; for these reasons, the practice has not been universally adopted.

Jan 1, 1961

By A. N. Fried

With the growing importance of fluid injection in recent years, the petroleum industry has been investigating and field- testing a variety of new methods designed to modify the physical properties of reservoir oil to improve the efficiency of gas and water injection. These procedures include condensing-gas drive, LPG (liquefied petroleum gas) injection, alcohol-slug process, high-pressure-gas displacement, detergent-solution flooding, and in situ combustion (30, 37).3 A new and different method to increase the effectiveness of gas and water injection has been tested by the Bureau of Mines, Consideration of both fundamental and practical factors that operate to limit the oil recovery attain- able by conventional oil-displacement mechanisms led to the concept of a displacement mechanism called the foam-drive method. This report describes the experimental study that tested this concept in the laboratory.

Jan 1, 1961

By E. G. King

An earlier Bureau of Mines report4 provided low-temperature heat-capacity and entropy data for three sodium vanadates. This report continues the study of vanadates by presenting analogous data for three crystalline calcium vanadates - calcium metavanadate (CaV206), calcium pyrovanadate (Ca2V2O7), and calcium orthovanadate (Ca3V208). No similar data for these compounds have been published previously. MATERIALS All three vanadate samples were prepared by the Bureau of Mines by heating stoichiometric mixtures of reagent-grade calcium carbonate and vanadium pentoxide.5 Calcium metavanadate was prepared at 610° to 660° C. A stoichiometric mixture was heated for 17 days with intervening grindings, mixings, and adjustments of composition, as shown necessary by chemical analysis. The final analysis gave calcium oxide, 23.48 pct. (theoretical, 23.57 pct.) and vanadium pentoxide, 76.32 pct. (theoretical, 76.43 pct.). The sample also contained 0.11 pct. acid-insoluble matter. The X-ray diffracton pattern showed no lines of free calcium or vanadium oxides. No X-ray diffraction patterns were found in the literature for any of these substances.

Jan 1, 1961