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By J. F. Neill, O&apos

The manganiferous schists occurring in the vicinity of Kings Mountain, North and South Carolina, suggest significant tonnages of potential submarginal ores. Although some reconnaissance work in connection with these deposits has been reported, no recent information has been published. Evaluation of the schists as a possible domestic manganese resource has not always adequately considered the fact that the manganese content occurs quantitatively both as oxide and as the silicate, spessartite. The Bureau of Mines investigation herein reported includes preliminary studies to indicate the extent of manganese oxide mineralization and to deter-mine the amenability of the material to sulfur dioxide leaching. The field reconnaissance studies suggest a resource containing in one area an average of 6.4 percent manganese as oxide. The procurement of depth information was beyond the scope of the investigation.

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 Thomas M. Garland

Reports that set forth the pertinent facts of existing secondary-recovery operations are an integral part of the work of the Bureau of Mines in promoting conservation and efficient utilization of the petroleum resources of the Nation. Knowledge of the success or failure of waterflood projects in an area is very useful to other operators. Although projects will not have identical results, information concerning the flood performance, method of operation, and difficulties encountered on one project will help operators to determine the feasibility of flooding a similar sand and to select the methods of operation most likely to prove successful. The increasing cost of discovering and developing new oil reserves, as well as the unending effort to reduce operating costs and increase ultimate oil recovery from known petroleum reservoirs, has required the petroleum industry to evaluate continuously the performances of various secondary-recovery methods. Waterflooding was recognized early by the petroleum industry as a possible means of increasing oil recovery. From the early accidental floods in Pennsylvania and through many haphazard attempts to inject eater into oil-bearing formations, waterflooding emerged as one of the more important methods of oil recovery. Waterflooding is important not only to the oil industry but also to the economy of the area concerned.

Jan 1, 1962

By E. Morrice

High-purity lanthanum metal was prepared by electrolysis of La003 in a LaF3-LiF-BaF2 bath at 950° C. The requisite bath temperature for the deposition of molten metal was maintained by supplying the heat as current directly to the electrodes. A current efficiency of about 60 percent was obtained. The lanthanum nodules contained carbon and oxygen as major impurities. The total impurity content was from about 0.1 to 0.2 percent.

Jan 1, 1962

By H. R. Shell

Fluorphlogopite mica was synthesized from inexpensive and abundant olivine, clay, feldspar, and sand (plus K2SiF6). The raw materials were melted in crucibles and in an internal resistance electric furnace. The melts yielded >95 percent mica. The major difficulty encountered was incomplete settling of the highly dispersed ferroalloy. This problem was not completely solved. Reducing agents tried in melts of 300 to 400 pounds were carbon, silicon, and silicon carbide. Carbon slowly reduced the iron of the raw materials, with much fuming. Silicon apparently was oxidized ahead of the melting and was ineffective under the conditions obtained. By far the best reducing agent was silicon carbide. With silicon carbide, fuming did not occur and ionic iron content of the mica flake approached 0 percent. However, even with SiC, the highly dispersed globular iron did not completely separate from the mica portion. The fluorphlogopite made during this investigation should be suitable for metallurgical use. A byproduct ferroalloy containing about 5 percent nickel, 3 to 5 percent chromium, and some cobalt was obtained. Because of the highly dispersed metallic ferroalloy, the mica was not deemed suitable for electrical or electronic uses.

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 J. G. Croeni

The titanium-iridium alloy system was investigated to determine whether alloys of this system would merit further development as control-rod material for nuclear reactors. A study was made to determine the titanium-iridium phase diagram by using melting-point, thermal analyses, X-ray diffraction, dilatometric, electrical resistivity, and metallographic techniques. The titanium-iridium alloy system was investigated between 500° and 2,400° C. Results indicate the formation of two intermetallic compounds, Ti3Ir rind TiIr3, and one intermediate solid solution centered about the 50 atomic percent iridium composition. A eutectic reaction occurs at 1,475° C, and 19 atomic percent iridium. The Ti3Ir decomposes peritectically at 1,520° C. The intermediate solid solution exhibits a maxima of 2,140° C. at 50 atomic percent iridium. This phase is also believed to undergo an order-disorder transformation at 1,750° C. Another eutectic reaction takes place at 2,000" C. and 60 atomic percent iridium. The compound TiIr3 formed at 75 atomic percent iridium decomposes peritectically at 2,115° C. Further increases in iridium content result in the formation of an iridium-rich terminal solid solution. Information obtained below 900° C. in titanium-rich alloys indicates that iridium acts as a beta stabilizer in titanium, and the authors believe that a eutectoid decomposition of beta-titanium occurs near 500° C. and 10 atomic percent iridium.

Jan 1, 1962

By P. A. Wasson

Drill cores from 15 holes in the West Central Mesabi Range were studied as part of the Lake Superior iron resource investigation begun in 1957 by the Bureau of Mines. Chemical, petrographic, and metallurgical analyses were made to determine grade, mineralogy, magnetic characteristics, and response to beneficiation. Data in this report were developed to provide a better under-standing of the nature and character of low-grade iron ore occurrences, to measure potential of usable ore, and to provide a basis for comparison with bank samples previously taken in the same general area. The average iron content of 4,445 feet of core was 31.8 percent. Iron oxides present were hematite, goethite, and magnetite; the gangue minerals were chiefly quartz, iron silicate, and iron-bearing carbonates.

Jan 1, 1962

By R. C. Corey

Anticipating the need for convenient, economical, and safe means for disposing of combustible wastes contaminated with low-level activity, in connection with private and institutional uses of radioisotopes, the Atomic Energy Commission (AEC) has provided the Bureau of Mines with funds to develop an incinerator for this purpose. A prototype incinerator, designated hereafter as BOMAEC-30, was designed, constructed, and tested, based on fundamental and applied research investigations of the combustion characteristics of rubbish and sawdust, which will comprise the bulk of contaminated wastes. No radioisotopes were used in the tests; the objective was to remove as much particulate matter from the products of combustion as possible. The prototype unit was designed to burn 30 pounds per hour, using 100 percent over fire air admitted tangentially in an all-metal, cylindrical combustion chamber. The gas-cleaning system consisted of special fabric bags and absolute filters.

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 Foster Fraas

A method is presented for the linear evaluation of adsorption data using the equations dC = Ae-rv dv and v = [jT] - q, where dC is the phase composition increment, v a calculated parameter, T the absolute temperature, and A, r, h, g, and q the constants. The value of v is calculated from the composition C for both the adsorption surface and the immersion phase. A plot of v for each phase on Cartesian coordinates results in straight line graphs. With temperature variation, a plot of v versus,[ ] also results in straight line graphs. The equations are applicable to electronic and salt equilibria.

Jan 1, 1962

By R. V. Lundquist

The work described in this report, part of the Bureau of Mines long-range program to develop methods of utilizing submarginal domestic sources of aluminum, was undertaken to investigate the effects of iron in the lime soda sinter process, The approximate Fe2O3 content in a sinter for maximum alumina and soda recovery was 8 to 9 percent. Fe2O3 appears to inhibit gelation, and 15.5 percent Fe2O3 produces effects similar to those produced by 1 percent sucrose. In the lime soda sinter process, aluminum silicates are sintered with limestone and soda ash to yield dicalcium silicate and sodium aluminate. The sodium aluminate is extracted by leaching in caustic solution. The solution is purified by heating in an autoclave with lime to remove silica, and alumina trihydrate is precipitated with carbon dioxide. The reactions involved in sintering and leaching are complex. A number of studies by the Bureau of Mines4-9 and others1 indicate that the iron content of sinters influenced the recovery of alumina and soda and the gelation characteristics.

Jan 1, 1962

By A. B. Whitehead

A spectrographic method for the determination of 18 impurities in cerium is presented. The carrier distillation technique is utilized to separate the spectra of impurities from the complex spectrum of cerium. Metal samples are ignited to the oxide, mixed with silver chloride carrier containing an internal standard, and excited with a 20-ampere direct-current arc. An additional exposure, made after carrier depletion, provides for the determination of refractory elements. Experiments to determine the best carrier, sample-carrier ratio, electrodes, arc current, exposure conditions, internal standards, and any matrix effect are described. The relative standard deviation of the method at the 20- and 200-part-per-million levels is about 25 and 15 percent, respectively. The average relative error is about 20 percent in the 10- to 1,000-part-per-million concentration range.

Jan 1, 1962

By George E. Fish

This report describes investigations conducted by the Bureau of Mines from 1957 through 1959 in the Roseland anorthosite-titanium belt of Nelson and Amherst Counties, Va., for the purpose of studying the titanium resources of the area. Three titanium deposits containing much saprolite ore derived from the decomposition of anorthosite and diorite were selected for detailed study Following a reconnaissance of the reported titanium occurrences in the belt. These three deposits occur in or are associated with anorthosite. Most of the occurrences are situated on or near the contact between the anorthosite and the gneissic country rock. The saprolite deposits are as much as 1.5 miles long, 1,000 feet wide, and 100 teat deep and contain significant reserves of titanium-bearing material estimated in excess of 20 million tons. Where it was penetrated by drilling, the unweathered rock beneath the saprolite contains nearly the same titanium values as the saprolite.

Jan 1, 1962

By H. J. Seim

An ion-exchange-instrumental analysis technique is described for analyzing impurities at 1 to 1,000 parts per million level in rare-earth metals. A cation-exchange flame photometric method is used for the alkali and alkaline earth groups of metals, and an anion-exchange procedure is used in conjunction with polarographic and X-ray fluorescence techniques for selected transition elements. The standard deviation is about 6 percent, and the average error, about 5 percent.

Jan 1, 1962

By Jerry B. F. Champlin

The successful injection of liquids into subsurface permeable formations for production stimulation, storage, or waste disposal requires a rapid, precise, and accurate method of determining the permeability of porous solids. This report describes a method and apparatus, developed by the Bureau of Mines, that use the principle of specific-volume permeametry. Calibration of the apparatus over a wide range of permeabilities and standardization of several apparatus constants have eliminated many of the tedious calculations and problems of manipulation common to some other methods. Improvements in reproducibility and accuracy have resulted from reducing experimental measurements to one parameter--time. Specific permeabilities of reservoir rock samples are determined directly from a chart that relates elapsed time to a permeability equivalent to that determined by bubble-tube measurements.

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