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By Leonard Obert

This report presents evidence indicating that when rock is stress-relieved during the course of mining or in drilling a core, it may be altered or damaged to the extent that the physical properties of the relieved specimen are not the same as those of the in situ rock. Furthermore, this type of damage may result from stress change other than that accompanying stress relief, such as the application of a relatively large compressive stress. In some instances the damage is microscopic, manifesting itself as incipient cracks or the failure of individual crystal bonds. However, if the sample is taken from a high-stress area, macroscopic damage may occur.

Jan 1, 1962

By Henry M. Harris

Low-carbon shales from 65 deposits and 11 sources of coal-mine waste in western Oregon and Washington were tested in a rotary kiln for their suitability as raw material for expanded aggregate. Shales from 41 sources bloated enough to produce crushed, expanded aggregates, weighing less than 65 pounds per cubic foot in the preliminary tests. The samples were judged on the basis of processing qualities, physical properties, and size and uniformity of the source. Nine low-carbon shale deposits and three coal-mine waste sources were selected for more extensive bloating tests and for examination of the expanded aggregates in concrete shapes. Composite samples from these 12 sources and from 2 commercial operations, when processed for testing in concrete shapes, had bulk densities ranging from 37.S to 72.9 pounds per cubic foot. Damp-cured concrete shapes made with these aggregates had bulk densities ranging from S6 to 119 pounds per cubic foot, and all but three of the lightweight concretes had crushing strengths ranging from 3,270 to 6,810 p.s.i. Properties of the lightweight concretes were compared with those of concrete shapes made with commercial aggregates, and with sand and gravel.

Jan 1, 1962

By Thomas L. McVay

The Bureau of Mines made laboratory batch and small-scale continuous flotation tests of a sample of pegmatite rock from a deposit of the Lithium Corporation of America, Inc., near Kings Mountain, N.C., to determine the feasibility of producing commercial-grade spodumene concentrates. Various reagents and flotation procedures were tested to determine the optimum conditions for floating the spodumene and retarding the gangue minerals. The best results were obtained when sodium fluoride and lignin sulfonate were used as the pulp conditioner and oleic acid was used as the spodumene collector. The continuous flotation tests indicated that commercial-grade. spodumene concentrates analyzing 6.4 pct. Li2O could be produced with recovery of 77 pct. of the lithia in the ore.

Jan 1, 1962

By R. L. Crosby

From studies of wrought magnesium alloys containing rare-earth elements, data are presented on the mechanical properties of the alloys at room temperature and at temperatures of 100°, 200°, and 300° C. Results of studies of the solid-solubility of cerium and zirconium in magnesium as determined by electrical resistance measurements are also discussed and are compared with those of other investigators. The strength of magnesium-cerium alloys did not increase with the addition of vanadium and titanium dioxide. The addition of zirconium increased the tensile strength of the alloys as much as 10,000 p.s.i. at room temperature, but this increase diminished above 100° C.

Jan 1, 1962

By T. T. Campbell

Research conducted by the Bureau of Mines demonstrated the feasibility of preparing columbium and tantalum metals by the application of Kroll-process techniques. Yields in excess of 95 percent were obtained in a modified Kroll-process reduction apparatus constructed from nickel and Inconel.4 Operating conditions during reduction and distillation were determined. Optimum temperatures during sodium reductions ranged from 650° to 750° C and for magnesium from 700° to 800° C with retort pressures ranging from 3 to 7 psig. Undesirable vapor phase reactions occurred when temperatures exceeded 750° C during sodium reductions or 850° C with magnesium. Vacuum distillation at 850° C effectively removed volatile salts and excess reductant from the reduced metals. Calculations based on the results obtained in small scale tests indicate that reaction rates of up to 34 lb/hr could be obtained during columbium reductions and up to 60 lb/hr during tantalum reductions in production scale reac¬tors. The small, laboratory-scale techniques used in this study could be adapted to commercial practice. The reduced powder or sponge metals can be consolidated by conventional arc-melting techniques, and the arc-melted metals can be fabricated into ductile sheet at room temperature. Analyses of arc-melted buttons prepared from Kroll-process tantalum or columbium showed that tantalum of greater than 99.8-percent purity was obtained and that columbium purity exceeded 99.7 percent. A significant purification of the reduced metals occurred when they were consolidated by electron-beam melting, and the purity and ductility of electron-beam-melted Kroll-process tantalum and columbium compared favorably with the commercial metals. After electron-beam melting, the purity of the tantalum exceeded 99.95 percent, and columbium purity was approximately 99.9 percent.

Jan 1, 1962

By G. H. Gronhovd

This report describes the design and initial operation of a slagging gasification pilot plant installed by the Bureau of Mines at the Lignite Research Laboratory, Grand Forks, N. Dak., in 1958-59. The tests covered in this report were conducted over a period of about 2 years, beginning in April 1959. The pilot plant was designed for eventual operation at pressures ranging from 400 to 600 p.s.i.g. (pounds per square inch gage); however, for the preliminary test reported here, the gasifier was fitted with a low-pressure slagging section and operated at atmospheric pressure and at 80 p.s.i.g. The reason for using a low-pressure slagging section for initial operation was to facilitate modifications in design during the development of a reliable slagging procedure.

Jan 1, 1962

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 instructions 5/ 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, 1962

By Eliot J. White

The physical properties and clay mineral content of the major oil-producing formations in the Powder River Basin of Wyoming were determined by analyses of cores from 100 wells. Interrelationships were established among permeability, restored water saturation, clay content, and bulk swelling capacity of the crushed sample and used to estimate the susceptibility of the formations to water damage. The ratio of water permeability to gas permeability (kw/ki) offers a convenient scale for semiquantitatively estimating the water sensitivity of sands. The irreducible water saturation was also found to have a similar relationship to the clay mineral content and the water sensitivity of the sands. The average relation of water permeability to gas permeability is different for each sand, as shown by the curves, and the relative positions of the curves indicate the degree of water sensitivity of each sand from which the susceptibility to water damage may be estimated. How accurately these estimates show formation behavior under field operations will not be known until studies of field performance can be made. The water permeabilities of the Muddy, Minnelusa, and Tensleep sands average about the same as the gas permeabilities, and these sands are classified as insensitive. The water permeabilities of the Sussex and Shannon sands, at the other extreme, are much less than the gas permabilities [when average ki is 30 millidarcys (md), kw is 6.1 md], and these sands are classified as highly water sensitive. The sensitivities of the five other sands are between these extremes.

Jan 1, 1962

By M. E. Tyrrell

The purpose of the work leading to this report was two-fold: (1) To determine the properties of cemented tungsten carbide modified by the addition of one, two, and five percent of titanium diboride, and (2) to compare the properties of these mixtures when sintered, hot-pressed, and flash-welded (resistance-sintered). Minor additions of titanium diboride to mixtures of 94 percent WC and 6 percent Co decrease mechanical strength but increase oxidation resistance in proportion to the amount of the addition. One percent of titanium diboride increased the hardness by 2 Rockwell A units. Hot-pressing produced compacts with the highest density and the best mechanical strength, but losses of cobalt were high and grain growth was pronounced.

Jan 1, 1962

By David Burgess

Natural gas is a general term applied to the gas obtained from oil or gas wells. It is the most widely used of all gaseous fuels. The principal disadvantage in the use of this and other gaseous fuels is the difficulty encountered in the storage and transportation of large quantities in the gas state. Handling in the liquid state is possible, but reduced temperatures are required since methane (table 1) is the principal component of most natural gases that are used as fuels. Actually, liquid storage has been utilized both here and abroad;3 however, the Cleveland disaster4 has pointed out the need for a critical evaluation of the hazards involved in the storage of this cryogenic fuel. Accordingly, a program was undertaken to obtain basic data that could be used to assess these hazards. In this report, the factors to be considered in an evaluation of the fire and explosion hazards associated with any fuel are each discussed briefly. These factors are then used to assist in the design of experiments for the evaluation of the hazards associated with liquefied natural gas (LNG) relative to those associated with other common fuels. Experiments have been conducted on the vaporization of LNG, the mixing of LNG vapors with air, the effect of temperature and nitrogen dilution on the limits of flammability of methane in air, the burning rates of LNG and other fuels, flame radiation, and extinguishment of fires above liquid pools. Based on the results of these experiments, LNG can be stored safely in suitably designed above-ground tanks surrounded by earthen dikes in much the same manner as gasoline.

Jan 1, 1962

By R. V. Lundquist

This report describes results of tests on the desilication of solutions resulting from the leaching of lime-soda sinters. Desilication was accomplished by heating the solutions in an autoclave. A liquor relatively free of silica was obtained after 30 minutes of heating at 200 p.s.i.g. in the presence of lime. The addition of lime improved desilication, but the rate and efficiency of desilication was effected by the quality of lime used. The optimum quantity of lime for effective desilication was about 6 grams per liter. A lesser quantity gave poorer desilication, and a greater quantity increased the alumina loss without improving desilication. The alumina loss was approximately proportional to the lime added. A complex structure, called artificial noselite in this report, was the only silica bearing compound detected in the desilication precipitate. Other compounds present were Ca(OH)2 (calcium hydroxide), CaCO3 (calcium carbonate), and Ca [A1(OH)6]2 (hydrated tricalcium aluminate). Sodium carbonate in the leach liquor retarded the formation of the calcium aluminate; hence it decreased the alumina lost to the precipitate. The extraction of alumina from aluminum silicate materials by the limestone soda-sinter process has been investigated by the Bureau of Mines for many years. The process consists of the following major operations: Blending the aluminum silicate with limestone and soda ash in such proportions that dicalcium silicate and sodium aluminate are formed on sintering; leaching the sinter in a carbonated caustic solution to extract the soluble alumina; purifying the leach liquor by the precipitation of soluble silica (this precipitate is designated desilication precipitate in this paper); precipitating alumina trihydrate from the purified liquors by carbonating with carbon dioxide gas; and calcining the trihydrate to alumina. Commercial grades of

Jan 1, 1962

By H. R. Babitzke

The purpose of this investigation was to evaluate the potential of columbium-hafnium alloys as structural materials for use at elevated temperatures. The work described in this report was conducted to determine the properties of columbium-hafnium alloys and to select the more promising ones for further improvement. Properties determined in this report were machinability, hardness, workability, tensile strength, and oxidation resistance. Ten ingots, ranging from 100 percent columbium to 70 atomic-percent hafnium, were prepared and subjected to tests. The test results showed that the alloys with 33 and 50 atomic-percent hafnium were superior in workability, strength, and oxidation resistance. For the alloy series tested, the strength and hardness values increased with the increasing hafnium content. Maximum values were reached with 50 atomic-percent hafnium. The oxidation resistance was poorest at the 1 atomic-percent hafnium level but improved with increasing hafnium content through 70 atomic-percent. Eight of the ten ingots were fabricable at room temperature. The two remaining ingots, those with 5 and 10 atomic-percent hafnium, required hot-working.

Jan 1, 1962

By E. C. Perkins

Preliminary experiments are reported utilizing bacteria to leach manganese from a variety of domestic low grade manganiferous materials. In two large leaches manganese extraction ranged from 71.7 to 92.5 percent, and the products analyzed over 48 percent manganese. Nutrient requirements and leaching time experiments were made. The mechanism of leaching is not understood, but is different than the mechanism encountered in the microorganism accelerated leaching of copper in the presence of sulfide minerals.

Jan 1, 1962

By W. W. Agey

This report summarizes results of bench-scale metallurgical studies by the Federal Bureau of Mines on three composite samples representative of the low-grade manganese ores purchased by the General Services Administration (GSA) and stockpiled at Deming, N. Mex., and Wenden, Ariz. Bench-scale flotation tests at the Salt Lake City Metallurgy Research Center showed that all three composites could be beneficiated by flotation to recover 88 to 90 percent of the manganese in concentrates that assayed from 38.5 to 39.0 percent Mn, 10 to 12 percent insoluble, 5 percent CaO, 3 to 5 percent Fe, and 1.3 to 1.7 percent combined Pb plus Zn plus Cu, Sintering studies indicated that specification-grade material could be made from these concentrates by sintering above 1,000° C, and adding either sodium or calcium chloride to the charge to insure removal of enough lead and zinc to meet the specifications.

Jan 1, 1962

By D. W. Frommer

Composite samples of nonmagnetic taconite from the western Mesabi range were evaluated by reductive roasting, fine grinding, and magnetic separation to determine potential sources of concentratable material. Although large tonnages of nonmagnetic taconite are known to occur in the western Mesabi district, these materials are not as yet a commercial source of iron ore. The technique employed permits the evaluation of individual composites and blocks of composites in terms of responsiveness to a process of potential commercial significance. The 159 composites, from open-pit mines located between Grand Rapids and Chisholm, Minn., were evaluated in the following sequence: 1. Minus 8-mesh material was roasted at 500° C. in hydrogen. 2. The roasted are was ground to one or more sizes in the minus 100-to minus 400-mesh range. 3. The roasted ground ore was magnetically separated in a Davis tube. 4. Composites were classified according to degree of grinding required to produce minimal concentrates. (Minimal concentrates are herein defined as those containing less than 10 percent silica, and responsive composites as those yielding minimal concentrates.)

Jan 1, 1962

By J. Robert Wells

The Bureau of Mines has developed a spectrochemical procedure for determining 19 impurity elements in high-purity titanium metal, titanium oxides, and titanium halides in which all samples are converted to titanium dioxide. Determination of these impurities was studied in the general concentration range of 0 to 1,000 p.p.m., but different determination limits were found for the various elements. The procedure is quantitative for 18 elements but semi-quantitative3 for beryllium and has an overall relative standard deviation of 15.8 percent. Two mixtures were used, one composed of graphite and lithium carbonate plus gallium oxide and the other of graphite and lithium carbonate plus germanium dioxide. Each mixture was blended mechanically with an equal weight of titanium dioxide. Lithium carbonate served as buffer-diluent. Gallium was the internal standard for 1 impurity element, germanium for 7, and titanium for the remaining 11.

Jan 1, 1962

By R. C. Bates

Uranium mine workers? daily exposure to radon daughters was estimated by two methods of sampling, detailed and spot-check. Both methods involve time- weighting measured exposure levels to arrive at an average exposure figure. Random sampling, or sampling without regard for the duration of exposure, has proved inadequate for estimating average exposure levels. During the first phase of the study, the breathing zones of eight workmen in three underground uranium mines were sampled for an entire shift; 20 to 36 radon-daughter samples were collected per man-shift, Analysis of these data indicated that a suitably accurate estimate of the full-shift exposure could be made by time weighting a considerable lesser number of representative radon-daughter samples. This analysis led to the spot-check method of estimating full-shift exposures to radon daughters. Additional detailed studies were made in seven mines to Learn more about the full-shift radon-daughter exposures and to test the spot-check method, In all, 617 radon-daughter samples were taken in 10 underground uranium mines during 26 man-shifts, and the spot-check method was tested 35 times.

Jan 1, 1962

By A. G. Starliper

The report covers studies by the Bureau of Mines on the removal of metallic values in two waste products from the Longhorn tin smelter at Texas City, Tex. One product was a slag that contained tin, tungsten, iron, tantalum, and columbium. The other product was a spent acid solution that contained tin, tungsten, iron, lead, copper, zinc, and silver and that came from presmelting treatment of impure tin concentrates. Molten slag was treated with sulfur or sulfur compounds and with coke, calcium carbide, or gaseous reductants to form tin sulfide that volatilized from the charge and to reduce tungsten along with iron and silicon to form a carbon-bearing metallic layer. The metallic layer was treated by an oxidizing alkali roast and then was water-leached to extract the tungsten. The waste acid was used in other experiments to dissolve an iron-tin- tungsten alloy (hardhead) obtained by direct reduction of the slag. An insoluble fraction containing tungsten, silver, silicon, columbium, and tantalum was removed, and copper was cemented on metallic iron, Tin was recovered by cementation on zinc plates, and lead was precipitated by adding sulfate ion. Iron was precipitated by increasing the pH which left a solution containing principally zinc. Slabs of hardhead were electrolyzed in an electrolyte consisting of waste acid to plate out groups of metals at different pH?s. The time did not permit thorough exploration of this method of treatment.

Jan 1, 1962

By R. W. Lewis

Spectrochemical procedures were developed using dc arc excitation for the determination, in parts per million, of 18 impurity elements in electrorefined beryllium and high-purity beryllium oxide. The metal samples were dissolved in dilute hydrochloric acid, evaporated to dryness, and converted to the oxide in a muffle furnace at 900° C. Germanium oxide was added as an internal standard for the determination of 15 of the elements, copper oxide for boron and molybdenum, and neodymium oxide for calcium. The average coefficient of variation was 11 percent with the exception of copper, which averaged about 43 percent.

Jan 1, 1962

By P. S. Jacobsen

In 1960 over 93 percent of the coal cleaned mechanically in the United States was cleaned in processes that utilized water or dense-medium suspensions of fine solids in water. Thus, in the process of removing deleterious ash-forming and sulfur-bearing minerals, another deleterious substance--water-- is added to the coal. The subsequent removal of the water from the coal, and the concomitant recovery of the coal from the water, is not troublesome in the sizes coarser than 1/4-inch. In the finer sizes, however, it is a difficult procedure that often costs more than the original washing operation. Because of the importance of liquid-solids separation in coal preparation, the Bureau of Mines has a continuing program of research in this field. The objective is to make available information on the performance characteristics of various types of equipment available for liquid-solids separations, thus promoting the wise selection of equipment for specific applications, and, thereby, more effective processing of coal. Results of work on flocculation as an aid to filtration5 and the sieve bend screen6 have been published. The present investigation of the screw-type classifier operating in combination with the cyclone was undertaken primarily because such classifiers are comparatively new to coal preparation and information on their performance is not available. The cyclone has become well-known since its introduction in this country by the Bureau of Mines in 1948.7 Use of the cyclone in conjunction with the screw-type classifier represents an attempt to provide the maximum recovery of solids at minimum moisture content.

Jan 1, 1962