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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 H. C. Fuller

Depletion of iron ore in the Nation's large deposits has directed attention to other sources. One of these is the titaniferous iron ore of the Iron Mountain, Wyo., area. Tests were made to determine the feasibility of smelting this ore, which contains about 20 percent titanium dioxide (Ti02), in an electric-arc furnace to produce pig iron. Initial tests, which were made in a 30-pound-capacity induction furnace, demonstrated that the iron could be easily reduced to metal and that limestone was a suitable and effective flux. Larger scale tests then were made in a 50-pound-capacity electric-arc furnace to obtain the more detailed information necessary for the planned continuous operation of a still larger arc furnace. The principal facts determined by preliminary batch-smelting studies were that (1) 9 pounds of limestone flux was required for each 100 pounds of ore smelted, (2) expensive coke was not required because coal proved to be a satisfactory reductant (near stoichiometric carbon was optimum), and (3) overreduction, which produced a viscous slag, must be avoided.

Jan 1, 1961

By Beverly W. Dunning

The effect of vacuum melting on the elimination of gases and nonmetallic inclusions for six low-alloy steels was investigated. The purpose of these studies was the analysis and comparison of differences in gas content and inclusions in air-melted and vacuum-melted steel. Data obtained from melts of 1-1/4 to 20 pounds indicate that vacuum melting decreases the number and size of nonmetallic inclusions and at the same time increases the degree of dispersion of the remaining inclusions. These improvements are undoubtedly related to the elimination of approximately 80 percent of the nitrogen and 90 percent of the oxygen as well as most of the undesirable metallic trace impurities.

Jan 1, 1961

By J. G. Walters

In 1928, the Coal Carbonization Section of the Federal Bureau of Mines, in cooperation with the American Gas Association, began a survey of the carbonizing properties of American coals. A standard test method for evaluating the carbonizing properties of coals that met the following conditions was developed: To yield products similar to those obtained in commercial operations. To produce yields sufficient to permit analyses and tests of quality. To be laboratory size. To be convenient to operate. To permit reproducible control of test conditions and results. This test method has become known as the Bureau of Mines-American Gas Association (BM-AGA) test (53),3/ and more coals of greater variety have been tested in this apparatus than in any other of similar scale.

Jan 1, 1961

By H. S. Caldwell

Molten zinc, condensed from zinc vapor, was used by the Federal Bureau of Mines to leach aluminum from an aluminum-silicon alloy made by carbothermic reduction of silicious aluminum ores. Zinc requirements were minimized by re-fluxing condensed zinc in a low-pressure, Soxhlet-type distillation unit. The minimum ratio of zinc used to aluminum in the crude alloy was approximately 2:1. When the system pressure was reduced from atmospheric pressure to 100 microns or less, the rate of aluminum extraction increased by a factor of 20. Leaching rates were much higher when the zinc vapor was condensed directly on the crude alloy than when molten zinc was passed over the alloy in the absence of appreciable zinc vapors. Observations indicated higher extraction efficiencies from crude alloys containing greater amounts of iron. Complete extraction was obtained with negligible loss of zinc. Assuming complete removal of zinc, the aluminum products will contain 1 to 6 percent silicon and about 0.5 percent iron plus titanium. The leached crude-alloy residue is a highly friable spongelike material containing about 80 percent silicon, several percent iron and titanium, with the remainder aluminum. This extraction method has been patented (Patent 2,810,637) and assigned to the Government. Research and development investigations are continuing at the College Park Metallurgy Research Center.

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 Kenneth G. Broadhead

The objective of this rare-earth oxalate study by the Bureau of Mines was to determine systematically by radiochemical techniques what effects, if any, could be attributed to the several variables--temperature, digestion time, acid concentration, rare-earth concentration, oxalic acid concentration, stirring, and the presence of other rare-earth ions. A Latin Square experimental design was used to evaluate statistically some of the variables. Precipitation losses ranged from near zero to about 7 percent, and mineral acid and rare-earth concentration were the predominant factors affecting completeness of precipitation. Quantitative oxalate precipitation of the rare-earth elements was achieved by controlling the experimental conditions as follows: (1) Maintaining rare-earth concentrations above 0.01M; (2) stirring the mixture several minutes after precipitation; (3) using an adequate (two to five-fold) excess of oxalic acid; (4) precipitating at room or iced temperature and digesting for at least 1 hour; (5) avoiding an excess of mineral acid and, if possible, maintaining the pH above 2.0; and (6) avoiding excess complexing agents such as EDTA (ethylenediaminetetraacetic acid). In the past 20 years research aimed at developing more efficient separation and purification techniques applicable to the rare-earth elements and yttrium has been extensive. Common to most of these procedures has been the use of oxalic acid to precipitate this group of elements selectively. However, this particular use of oxalic acid has a much earlier origin; its application in precipitating yttrium was first reported by Mosander (8)4 in 1843. Despite long and popular employment of this technique, only limited and somewhat conflicting data are available regarding the many factors affecting the degree of rare-earth oxalate precipitations.

Jan 1, 1961

By J. T. Dunham

Zirconium has possible use in industry where severe corrosion conditions are encountered because it resists attack from a variety of corrosive environments. However, very little experimental testing has been done to evaluate the corrosion behavior of zirconium when simultaneously subjected to high tensile stresses and exposed to corrosive environments. This investigation was initiated for an evaluation test, but was limited to environments consisting of ferric chloride solutions which were known to attack zirconium and were shown to promote stress-corrosion cracking in preliminary tests. Tests for cracking susceptibility were conducted by the Bureau of Mines to show the effect of stress, solution concentration, air aeration of solution, and the method of mechanical processing. Tensile stress was applied to the specimens by a constant-load method which proved more reliable than a constant-strain method.

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 H. Kenworthy

The purpose of the study described in this publication is to develop methods for recovering simple master alloys or single metal components from discarded and scrapped S-816 alloy, The Bureau of Mines started this investigation late in 1955 after the need became apparent for a method of reclaiming high-temperature alloys from an ever-increasing accumulation of rejected and wornout jet engine turbine buckets. Laboratory studies showed the following: (1) Pyrometallurgical separations are not selective enough, (2) several methods can be used for effective chemical dissolution of the major constituents of the alloy, (3) a master alloy or complex salts of cobalt and nickel can be separated, (4) chromium, contaminated by several other metals, may be segregated, and (5) more time and effort need to be expended in separating the minor constituents and improving the purity of the major metals removed. Difficult and incomplete chemical separations were attributed to the complexity of alloy composition, as were the long tedious chemical analyses o' products. For determination of several of the metallic components, standard methods of separation and routine analytical procedures had to be considerably modified to achieve satisfactory results. The overall technical problems involved in separating S-816 components do not appear to be insurmountable; however, refinement of several of the methods used in this investigation is desirable.

Jan 1, 1961

By Edwin B. Cook

Studies of flame and combustion phenomena at the Bureau of Mines have been facilitated by computer evaluation of the thermodynamic properties of gases formed by constant-pressure burning.4 5 This report is the sixth of a series6-10 presenting results of such calculations; it deals also with constant-volume deuterium-air flames.

Jan 1, 1961

By C. I. Pierce

This report describes and presents results of a phase of a laboratory study conducted at the Morgantown Petroleum Research Laboratory, Federal Bureau of Mines, Morgantown, W. Va., to determine the response of shielded electrodes of different dimensions in thin, noninvaded beds and to stimulate interest in the use of focused-type logging devices in the Appalachian oilfields. A blotter model was used to obtain plots of the potential field in the vicinity of a model shielded electrode. Three plots are presented. The difference in curvature of equipotential lines and the variation in measured resistance values for different blotter-model conditions suggest that the shielded electrode will give resistivities higher than normal when measurements are taken in a thin conductive bed located between resistive beds, and resistivities lower than normal when measurements are taken in a thin resistive bed located between conductive beds.

Jan 1, 1961

By A. L. Engel

This report describes results of laboratory-scale experimental treatment of nine ores containing gold and silver, including samples of products of previous plant treatment, from ore deposits in California and Nevada. The samples treated were taken by engineers of the Bureau of Mines during investigations of these ore deposits. The information reported is of interest for development of the mining districts represented or in future Investigations of similar ores from other sources. The treatment methods were as simple as possible. More complicated treatments were tried when required, The applicability of the methods and their limitations in treating the ores are shown by the data in this report. The following treatment methods were employed in the experiments described: Screen analyses were made to determine distribution of values in various screened-sized portions of crushed ore, or to determine optimum size to which a particular ore should be crushed or ground to liberate values, and some-times to determine residual values in various-sized portions of treated material.

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 John E. Shelton

Flotation tests were conducted on two samples of copper-nickel-bearing ore from the Harriman area near Rockport, Maine. The samples were taken by Roland F. Beers, Inc., for tests in cooperation with the Federal Bureau of Mines. One sample, analyzing 0.38 percent copper and 0.71 percent nickel, was essentially a disseminated pyrrhotite in hypersthene. Pentlandite, chalcopyrite, pyrite, and millerite were intimately associated with the pyrrhotite. Locked series flotation tests on this sample showed that 87.4 and 73.4 percent of the copper and nickel, respectively, could be recovered in a bulk concentrate that analyzed 3.47 percent copper and 5.34 percent nickel. The copper-and nickel-bearing minerals were collected with sulfhydric collectors in an alkaline circuit. Cleaning the concentrate three times with the addition of pH regulators was sufficient to attain the previously stated grades. The second sample had analyses of 0.31 percent copper and 0.85 percent nickel; talc and hypersthene were the main gangue minerals. Bulk sulfide flotation, made while depressing the talc, resulted in a concentrate that analyzed 2.33 percent copper and 4.70 percent nickel at recoveries of 70.0 and 54.4 percent, respectively. Flotation of the talc followed by bulk sulfide flotation resulted in a nickel content greater than 5 percent. A locked-series test showed that 60.7 percent of the copper and 73.7 percent of the nickel could be recovered at grades of 1.29 and 4.85 percent, respectively.

Jan 1, 1961

By H. F. Yancey

Traditionally the Pacific Northwest has relied on hydroelectric power, which has been both abundant and cheap. However, comparatively few hydroelectric sites capable of providing low-cost power remain, therefore the need for supplemental thermal generation, perhaps within the next decade, is generally recognized. Based on the present cost and availability of competing fuels, coal seems to be the logical choice for projected thermal power plants. Power companies and public utilities have become interested in establishing reserves of coal for future use. One deposit explored in 1958-59 lies in southern Thurston and northern Lewis Counties, Wash., near Centralia. Drilling, totaling 22,700 feet, proved the existence of 70 million tons of strippable coal--an ample reserve for the projected power plant. The coal, like most others and particularly those of Washington and Oregon, when mined in full seam section by mechanical methods, would require cleaning to make it suitable for use. The amount and nature of the impurities in this coal dictated a thorough investigation of its cleaning characteristics to establish economic factors and to insure proper preparation-plant design. Therefore, arrangements were made through a cooperative agreement to conduct such work at the Seattle Coal Research Laboratory of the Bureau of Mines. This report describes that investigation. The results are of interest primarily in connection with the utilization of this particular deposit, but some of the information developed is applicable to other deposits of low-rank coals in the West, because the impurities in these coals differ greatly in behavior from those generally associated with the higher rank coals of the Appalachian field.

Jan 1, 1961

By H. J. Heinen

This report summarizes preliminary research studies by the Bureau of Mines in electrowinning molybdenum directly from pure or impure molybdenum trioxide (MoO3) by fused-bath electrolysis in an open graphite cell without need of a protective inert atmosphere. A formulated electrolyte of the tertiary system containing 41.6 percent sodium pyrophosphate, 16.7 percent sodium tetraborat, 33.3 percent sodium chloride, and 8,4 percent molybdenum trioxide, by weight, electrolyzed at 1,000° C,, gave excellent results. Current density studies were made over a range from 20 to 260 amperes per square decimeter. Current efficiencies of 80 to 90 percent were obtained over the entire range. Yields up to 500 grams of molybdenum per kilowatt-hour were obtained. Higher current densities, however, reduced yields and produced a finer grained metal. The two most important facets in electrowinning molybdenum from MoO3, in an open cell, are temperature and electrode spacing to minimize or eliminate the formation of the suboxide MoO2, the major source of oxygen contamination. At temperatures of 1,000° C. and higher, together with the proper spacing of the electrodes, formation of oxides are practically eliminated. Molybdenum metal electrowon from pure MoO3 was 99.9 percent pure and contained 0,056 percent oxygen and 0,007 percent carbon. This metal, when arc-melted, had a Vickers hardness number of 175 and contained 50 parts per million oxygen and less than 10 parts per million carbon. Molybdenum metal electrowon directly from an impure MoO3 containing 90 percent MoO3 resulted in a metal of 99.8 percent purity.

Jan 1, 1961

By J. G. Croeni

The high thermal-neutron cross section of gadolinium and the good mechanical and corrosion properties of titanium suggest that alloys of these two metals might be useful as control rod material. To aid in establishing the feasibility of this combination, the Federal Bureau of Mines investigated the titanium-gadolinium system. The results indicate that the system is composed of a single eutectic reaction and a peritectoid reaction involving the alpha-beta transformation of titanium. The eutectic isotherm extends from 1 to 99 pct, gadolinium at 1,240° C. The established eutectic composition is about 95 pct, gadolinium. The peritectoid reaction occurs at 885° C. and extends almost over the entire composition range. Hardness increases slightly with additions of gadolinium, and little change is obtained by heat treatment. Alloys containing less than 10 pct. gadolinium are amenable to extensive cold-working, but alloys having higher percentage of gadolinium content are only moderately cold-workable. All alloys can be hot-worked in iron sheathing at 750° C. Observation indicates that all compositions possess good machinability. Corrosion resistance to water at room temperature is apparently poor, especially in the gadolinium-rich alloys. INTRODUCTION A combination of the good mechanical and corrosion properties of titanium and the variety of thermal-neutron cross sections characteristic of the rare-earth metals suggests that alloys of these metals may be used for control rod materials. For this reason the Bureau of Mines proposed a study of the titanium-gadolinium alloy system, and the Atomic Energy Commission sponsored the investigation.

Jan 1, 1961

By Thomas C. Atchison

The experimental work described in this report is part of a continuing study by the Federal Bureau of Mines of the fundamental physical processes involved in breaking rock with explosives. Six explosives were tested for their strain-producing abilities in a dolomitic marble. The explosives selected for testing had a tenfold variation in detonation pressure and a fivefold variation in characteristic impedance (product of loading density and rate of detonation). Strain pulses produced by the detonation of small charges of the explosives were recorded at distances of 5 to 130 feet. Peak strain, ?, was found to decrease with distance, R, in accordance with an exponential propagation law previously determined for other rock types, namely ? = (K/R)e ?aR The absorption constant, a, did not vary significantly with the explosive and was of the same order of magnitude as that for other rock types. The different explosives produced a fivefold variation in the value of the intercept constant, K.

Jan 1, 1961

By J. W. Davis

The storage stability characteristics of a diesel type fuel were determined to evaluate the effect of the polar compounds in the fuel. These compounds, comprising most of the nitrogen and oxygen containing compounds and many sulfur containing compounds, were separated from the fuel with a chromatographic column. This fraction was further separated into three polar extracts by graded elution through the column. Each extract was characterized. A storage program using the depolarized fuel, the fuel as received, and blends of the extracts with both fuels, was conducted. Results showed that the removal of the more polar components stabilized the fuel. Blending the polar extracts with the original fuel and with the depolarized fuel in the same ratio as they existed originally and at two and three times the original ratio increased the amount of gum present before storage, but had little effect on the formation of additional gum during storage. Distillate fuels produced by commercial refining of petroleum contain traces of organic nitrogen, sulfur, and oxygen compounds that are more polar4 than the remainder of the fuel. Recent laboratory studies by the Federal Bureau of Mines (1),6 in which these compounds were removed from a fuel, have shown that they influence its storage stability. The objective of this work was to determine the amount of these compounds present in a fuel and their effect upon its stability in storage. To evaluate the role of these polar compounds, it is necessary to remove them from the distillate fuel. Many can be removed by chemical treatment (2), but such treatment precludes reblending the polar components to approximate the original fuel composition. Solvent extraction is free of some of the criticism of chemical treatment, but it is more difficult because of the complex mixture from which compounds must be removed.

Jan 1, 1961