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By H. C. Fuller

Rhodonite, a manganese silicate, occurs as an important component of extensive veins in the San Juan district of Colorado. Recent work by the Bureau of Mines has demonstrated that typical ores of the area can be upgraded to about 30-percent manganese content. Because of their siliceous nature, such concentrates require further processing to convert the manganese into more usable forms. The investigation described in this report demonstrates the technical feasibility of producing silicomanganese from a rhodonitic concentrate by electric smelting methods. The rhodonitic concentrate used in the smelting research was prepared by dry high-intensity magnetic separation of ore from the Silver Queen vein. The concentrate contained 29 percent manganese, 2 percent iron, and 41 percent silica. The principal minerals in the concentrate were 35 percent rhodonite, 30 percent rhodochrosite, and 25 percent quartz and chalcedony. Limestone was used as the flux and coal was used as the reductant. These minerals were crushed and screened to minus 1/2-inch plus la-mesh size.

Jan 1, 1962

By L. H. Banning

This investigation was undertaken to obtain basic information necessary for the design and operation of a plant for recovering metallic values from nickeliferous laterite and serpentine of the Philippine Islands. It was divided into three parts: (1) Mineralogical studies and preliminary mineral dressing tests; (2) electric smelting of the ores, upgrading of ferronickel by blowing with oxygen, smelting laterite slag to produce crude iron, and the production of mild steel; and (3) nickel and cobalt recovery from upgraded ferronickel. Results of the investigation indicate that it should be feasible to recover nickel, iron, and possibly cobalt products from the laterite and ferro-nickel from the serpentine. Mineralogical studies were made on representative fractions of the laterite and serpentine tonnage samples and on five selected samples; mineral dressing tests were made only on laterite. The nickel occurs principally associated with hydrous iron oxides and chemically combined with serpentine; garnierite was the only discrete nickel mineral identified, and it was found in a highly decomposed serpentine. The bulk of the cobalt was found in wadlike manganese oxide material. Approximately twice as much chromite was found in the laterite as in the serpentine, By mineral dressing techniques, laterite was separated into two fractions: one fraction contained over 90 percent of the nickel and cobalt, and 83 percent of the iron; the other fraction contained 74 percent of the chromium. A cobalt concentrate (1.1 percent Co) was produced by a scrubbing and sizing procedure.

Jan 1, 1962

By J. R. Ross

A reconnaissance for sources of scandium and a metallurgical investigation of recovery methods for byproduct scandium from uranium mill solutions were conducted by the Bureau of Mines. The work on scandium was undertaken to obtain information on domestic resources and to explore and develop recovery procedures in consonance with the Bureau's long-range program for conservation and wise utilization of mineral resources. The element scandium is widely distributed in the earth's crust in trace amounts, but it seldom occurs as an important constituent in any mineral. An exception is thortveitite, (Sc,Y)2 Si207) a rare mineral that contains various amounts of scandium and yttrium and may contain up to 42 percent scandium oxide (SC203). Knowledge of the chemistry of scandium has expanded rapidly in recent years (1, 4, 9)4 but only fragmentary information is available about the metal because it is still largely a laboratory curiosity without established uses (2, 3). A recent study shows some of the physical proper-ties of the metal are (1) density of 3.05 grams per cubic centimeter) (2) melting point of 1,540° C, (3) hexagonal close-packed structure) (4) hardness of about 50 Brinell (500-kilogram load), and (5) an alloy behavior similar to yttrium and rare-earth metals (2). The price of $2,850 a pound for scandium oxide of 99.9 percent purity and $2,700 a pound for oxide of 99 percent purity reflects the scarcity and complex chemistry of the element.

Jan 1, 1962

By William R. Wayment

The objective of this investigation was to obtain data on friction-head losses of sand slurries during their transport in pipelines. The data ultimately will be used in designing hydraulic transport systems. Information that was incidental to the primary objective was gathered on degradation, changed percolation characteristics, and critical velocities of the slurries~ Tests were made in a closed-circuit pilot plant, with one type of tailing, through horizontal 2-, 3-, and 4-inch-pipe test sections at various pulp densities and flow velocities. Tests were made in a closed-circuit pilot plant, with one type of tailing, through horizontal 2-, 3-, and 4-inch-pipe test sections at various pulp densities and flow velocities. Approximately 2,000 tests were run in the pilot plant. The ranges of flow velocities used in the experiment were 2.8 to 19 f.p.s. in the 2-inch line, 4 to 14.5 f.p.s. in the 3-inch line, and 4 to 11 f.p.s. in the 4-inch line. Velocities were varied in increments of 0.5 f.p.s. through the entire velocity range in each pipe size. Densities were varied in 3-percent increments from 40 to 70 percent solids by weight except for one series of tests in the 2-inch line; in this series, densities were varied in 5-percent increments from 5 to 65 percent solids by weight.

Jan 1, 1962

By John D. Bardill

Data from extensive tests was obtained on friction-head losses of various sand slurries, composed of materials of different specific gravities and under varying transport conditions, to provide useful information for designing hydraulic transport systems. The tests were run in a pilot plant through 2-, 3-, and 4-inch lines with slurries composed of relatively pure barite and limestone solids. Available grinding and classification equipment did not permit attaining a comparable size distribution in the two materials tested, thus preventing direct correlation of friction-head loss values to physical properties or mineral composition. A total of 495 measurements were made of limestone slurries in the 2-, 3-, and 4-inch pipe test sections at flow velocities from 6 to 14 feet per second and pulp densities from 40 to 70 percent solids. A total of 640 measurements of barite slurries were made in the 3-and 4-inch pipe test sections at flow velocities between 7 and 14 f.p.s. and pulp densities ranging from 40 to 80 percent solids.

Jan 1, 1962

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