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By L. O. Bacon

This Bureau of Mines report summarizes the results of laboratory work in the design of instrumentation for obtaining the dynamic tensile strength of rock at minimum loading. Minimum loading is defined as the lowest tensile loading by pulse reflection to cause fracturing. The instrumentation for obtaining dynamic tensile strengths of rock cores evolved into the use of a compressed-air pellet gun to impact one end of a rock core, suspended by wires, at increasing increments of air pressure. Maximum strain was measured on most or all of the impacts, and the strain at fracture of the core was obtained by extrapolating the pellet velocity-strain curve to the pellet velocity at fracture. Stress at tensile fracture was obtained from the maximum s train, and the dynamic Young's modulus was calculated from the rod velocity by using simple rod theory.

Jan 1, 1962

By Eugene L. Grumer

High-expansion foam was applied to the flames of six fuels burning in a 1-foot-diameter tray. The flames of three hydrocarbon fuels were more readily extinguished than the flames of methanol, acetone, or unsymmetrical dimethyl hydrazine. The result is rationalized on the basis that heat transfer from flame to fuel surface is primarily radiative with the hydrocarbons and more largely convective with the nonhydrocarbons. INTRODUCTION Equipment for producing high-expansion foams has been developed by the Bureau of Mines to control coal mine fires.5 Recently such equipment has been redesigned for portability and has now been produced commercially for other fire-fighting applications. In May 1961, a 50-by 50-foot gasoline fire was extinguished within 2 minutes by a trailer-mounted foam unit that produced 12,000 cu.ft./min. of high-expansion (1,000:1) foam.6

Jan 1, 1962

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 Charles W. Huggins

The Bureau of Mines investigated palygorskite, a natural asbestiform material, to accumulate knowledge that might serve as a foundation for future synthesis of a similar material. Unit cell, chemical analysis, DTA, TGA, optical constants, and electron microscopy data were obtained. Selected palygorskite samples of bettor than 97-percent purity were used to obtain this information. Chemical analysis revealed the following formula: (OH2)4 (OH)2 Ca0.01Fe0.02K0 .c3Mg2.10A12.00Si7.93020.3.91 H2O. The optical constants for sodium light are a = 1.522; S = 1.530; ?=1.533; biaxially (-). The following orthorhomibic unit cell constants were determined: ao = 12.690 A, Z = 2, bo = 17.857 A, Dx = 2.327. co = 5.207 A, Identical diffraction patterns resulted from the three palygorskite samples that were studied. X-ray, chemical, DTA, TGA, and optical data were compared with literature values for similar fibrous materials. X-ray diffraction lines were indexed. Several electron micrographs were made to compare the structures of palygorskite and attapulgite with that of chrysotile. The micrographs revealed extremely short laths for attapulgite, very long flexible laths for palygorskite, and tubular structure for chrysotile.

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 Charles B. Kenahan

Application of ultrasonics in the electrolytic deposition of metallic manganese and manganese dioxide from sulfate electrolytes had several effects. Ultrasonics produced finer-grained deposits of electrolytic manganese at all current densities than obtained in normal cell operation, but at high current densities it resulted in less adherent deposits. Ultrasonic radiation did not affect cell voltage or cathode current efficiency. In the electrodeposition of manganese dioxide at 70° C., ultrasonic-; increased the current efficiency and decreased the cell voltage at a current density of 9 amperes per square foot, but it had little effect at current densities above this. The decrease in cell voltage was caused by the depolarizing action of ultrasonics at both anode and cathode. Ultrasonic radiation produced a smooth, glossy, adherent, and pit-free deposit at all current densities and at each temperature. Radiation had no effect on current efficiency or cell voltage at 90° C. Ultrasonics was more effective than conventional agitation in producing all of these effects.

Jan 1, 1962

By R. C. Ellman

Significant effects of in-the-mill drying on the pulverization of lignite have been demonstrated in an experimental impact-type pulverizer by tests in which the primary variable was temperature of the sweeping gas. Reduced power requirements and increased product fineness were observed as the extent of drying was increased. Pulverization with in-the-mill drying was studied in comparative tests made on lignites from five mine sources. All of the lignites responded in a similar manner; however, differences in the pulverizing characteristics of the individual lignites were significant. For one lignite, the electrical input to the pulverizer driving motor with minimum sweeping-gas temperature was 33.9 kw.-hr. per ton, decreasing to 14.0 kw.-hr. per ton with a sweeping-gas temperature of 658° F.; for another lignite, at comparable operating conditions, the electrical input decreased from 59.1 to 19.0 kw.-hr. per ton. In the first case, the product fineness increased with increasing temperature of sweeping gas from 65.2 to 79.2 percent through a 200-mesh sieve, and in the second case, from b2.7 to 86.9 percent through a 200-mesh sieve.

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

The systems MgO-MgFa-SiO2, at 2 and 4 weight-percent Li2O and at 3.8 and 7.7 weight-percent Na2O were investigated by solid state reaction at 1,200° C. The results are summarized in four ternary diagrams. Besides the expected humites and simpler silicates or fluorides, proto-amphibole and water-swelling fluormicas or fluormontmorillonoids were found in the systems containing lithium and monoclinic fluoramphiboles, water-swelling fluormicas or fluormont-morillonoids, and nonwater-swelling fluormicas were found in the systems containing sodium. These latter compounds were not in the base system MgO-MgF2-SiO2.

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 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 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 W. A. Calhoun

A method for concentration of the nickel-cobalt-bearing mineral, siegenite, from a table middling has been developed by the Bureau of Mines at Rolla, Mo. The table middling is composed of a complex series of sulfide minerals, occurring in mill operations in the southeast Missouri "lead belt." In these operations the siegenite is lost as a separate concentrate, being diverted to other products. The procedure also includes recovering commercial-grade concentrates of copper and lead. A low-grade zinc concentrate, a potential coproduct, was also made.

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 J. W. Montoya

The chemical, mineralogical, and physical properties of berylliferous tuff from Spor Mountain, Utah, were determined in laboratory research conducted by the Bureau of Mines. Two beryllium-bearing minerals--a hydrated form of bertrandite and a berylliferous saponite--were found to be present in the tuff. Each of the beryllium mineral forms predominated in samples from certain areas of the district. The possibility of practicably separating the beryllium minerals from the tuff by physical methods appears remote because of the complexity and nature of the mineral associations. Beryllium mineralization in the region occurs in a rhyolitic tuff usually overlaid by unaltered rhyolite. The beryllium is distributed erratically throughout the tuff in individual mineralized bodies. Many samples of mineralized tuff were examined and found to contain from 0.2 to 1.8 percent BeO. All samples contained a hydrated form of bertrandite that was nearly cryptocrystalline, whereas samples from one area also contained a berylliferous saponite of variable beryllium content. Neither mineral has been previously reported, although related bertrandite-like minerals have been found in the U.S.S.R. and berylliferous minerals of the montmorillonite group have been synthesized. Most of the minerals of the tuff are finely crystalline, intergrown, and have similar densities. The complexity and intimacy of the mineral associations, the difficulty of achieving effective mineral liberation, and the highly friable nature are characteristics that lead to the conviction that tuff of the type examined cannot be effectively concentrated by gravity, magnetic, electrostatic, attrition, washing, sizing, or flotation methods.

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