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By J. L. Potter

An inert-gas fusion technique was applied by the Bureau of Mines to the oxygen analysis of mixed-fluoride electrolytes used in electrowinning uranium and the rare-earth metals. Method development included: (1) Thermodynamic and experimental evaluation of the temperature required to quantitatively remove oxygen from a fluoride melt; (2) installation of a water and an acid trap to entrain the volatilized fluorides; (3) development of a suitable sample-preparation technique for the heterogeneous fluoride baths in which both pulverizing and pelletizing were necessary to achieve reproducible results; (4) comparison of platinum flux and dry crucible techniques, which showed that the use of platinum was not necessary. The accuracy of the method was evaluated by analyzing fluoride baths containing known amounts of oxygen added as the metal oxide. In the 0.05-to 0.5-percent range, the relative error was about ±5 percent.

Jan 1, 1962

By Michael G. Zabetakis

The spillage of liquid diethyl ether in rooms at floor level and 3 feet above the floor resulted in flammable vapor-air mixtures in the immediate vicinity of the exposed liquido The liquid temperature was found to decrease by as much as 35° C., with a resultant decrease in vaporization rate. A search of the literature yielded numerous references to unstable peroxide (residue) formed by the autoxidation of ether. Such residues appear to constitute an explosion hazard in the condensed state.

Jan 1, 1962

By J. G. Donaldson

Optimum conditions are given for chloridizing pyrite, marcasite, chalcopyrite, arsenopyrite, stibnite, and covellite with chlorine gas. The formation of metal chlorides is affected by the time and temperature of chloridizing, and by particle size of the sample. Chloridizing data also are given for chemically precipitated antimony (III) sulfide and copper (II) sulfide.

Jan 1, 1962

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 M. R. Geer

Information on the performance of coal-cleaning equipment is necessary to provide a basis for evaluating the performance of existing plants and projecting that of new plants. Performance data can contribute greatly to the wise selection and effective use of coal-washing equipment. The Bureau of Mines has published information on the performance of several commercial plants, as well as of some laboratory-scale equipment, 5 (2-9, 11, 12, 17-12, 21-25) from time to time for a number of years. A more intensive program to provide such information for all the principal types of cleaning equipment is underway. The present evaluation of table performance is part of this program.

Jan 1, 1962

By W. W. Agey

The Bureau of Mines examined and tested the rhodonite deposits of the Silverton lead-zinc district, San Juan County, Colo., as a possible source of domestic manganese. Exploration and development work by several mining companies and preliminary reconnaissance of the area by Bureau of Mines engineers indicated the presence of extensive manganese resources in the form of rhodonite. This report summarizes the results of laboratory beneficiation tests made on samples of different type and grade material obtained from surface and underground exposures of seven veins in the district. Surface and underground examinations revealed the presence of several prominent veins that could be traced up to 2 miles for a single vein along the surface. The principal veins average about 50 feet in width and apparently carry rhodonite to considerable depth. Underground samples were taken from the Sunnyside, Silver Queen, Washington, Independence, and Scotia veins. Samples also were taken from surface exposures of the Sunnyside Extension and Hidden Treasure veins.

Jan 1, 1962

By W. L. Dare

Tri-axial strains in pillars, created by pillar robbing, were measured in an experiment at the Dysart No. 1 uranium mine near Grants) New Mexico. At this mine, room-and-pillar stoping is used on the advance, and pillars are recovered on the retreat. The are deposit is, for all practical purposes, horizontal. Measuring devices were installed in pillars approximately 90 to 200 feet from the break line, and strains were recorded over a 4-to 6-week period. The measurements indicate that, in general, the algebraic magnitude of vertical strains increased, and the horizontal strains decreased, in turn, indicating that vertical (or near vertical) loads on the instrumented pillars lessened as pillars were recovered.

Jan 1, 1962

By John J. S. Sebastian

A laboratory-scale investigation was made of the basic problems involved in developing a ceramic heat exchanger to operate at high temperatures for using nuclear heat from gas-cooled process-heat reactors. Technical data were obtained on transferring heat by forced-convection from helium to air in a single-tube vitreous-alumina heat exchanger. Coolant air was passed through the annulus parallel with, and either concurrently or counter to, the flow of helium inside the tube. The data obtained pertain to removing heat from the helium. Average inside film coefficients were determined at mean surface temperatures of 200° to 1,570° F., inlet-gas temperatures of 1,450° to 2,665° F., and Reynolds numbers up to 560. The gas-to-surface temperature ratios were varied from 1.05 to 7.6. The tabulated results are shown in the appendix at the end of this report. The film coefficients of heat transfer were correlated by taking into account the physical properties of the helium at the average fluid temperature. With experimental conditions pointing to a laminar flow, the Nusselt number was found to decrease as the ratio of gas-to-wall temperature was increased to a value of 3. However, within the range tested, gas-to-wall temperature ratios above 3 did not affect the Nusselt number, regardless of the value of the Graetz number. Thus, beyond this point any increase in this ratio ceased to influence the heat-transfer relationship.

Jan 1, 1962

By Michael G. Zabetakis

Limits of flammability of normal propyl nitrate (NPN) vapor were investigated at ambient and elevated temperatures. Minimum spontaneous ignition and decomposition temperatures were determined with laboratory apparatus over the pressure range from 0 to 4,000 p.s.i.g. Flame speeds and the detonation susceptibility of NPN vapor were measured at elevated temperatures. Stable detonation was obtained with liquid NPN at elevated temperatures, and the detonation velocity was determined to be between 4,700 and 5,100 m./sec.

Jan 1, 1962

By E. R. Palowitch

Two samples of the Lower Hartshorne (Spadra) bed were collected: A sample of the raw coal with the machine cuttings excluded, and a sample of the machine cuttings exclusively. Analysis of the 5-inch by 200-mesh size fraction of the raw coal, excluding machine cuttings, showed that a product meeting minimum quality specifications could be produced by washing at 1.60 specific gravity, yielding a theoretical 93.7 percent of clean coal. A negligible amount of near-gravity material at the separation gravity indicated an easy washing problem. The sample of machine cuttings had a maximum size of 2 inches and contained about 50 percent ash. Washability tests of the 2-inch by 200-mesh size fraction indicated that a theoretical yield of 30.0 percent of specification-grade coal could be achieved by washing at 1.49 specific gravity. As the machine cuttings represent an estimated 10 percent of the total coal mined, their inclusion in the mine output would increase the theoretical net yield of salable coal by only 3.7 percent. Because the machine cuttings contained a high percentage of sink 1.80 specific-gravity material, they had neither an effect on the separating gravity required to clean the raw coal nor on the difficulty of separation. Gabbing underground versus transporting the cut-tings to the surface for disposal or washing either separately or combined with the raw coal involves a number of practical, economic; and intangible factors; hence, no specific recommendations could be made. A discussion of some of the factors involved in dealing with a similar problem is given by Gandrud and Riley.4

Jan 1, 1962

By Roy L. Wilfong

The thermal decomposition of the ammonium sulfate, carbonate, nitrate, oxalate, and sulfate salts of praseodymium, neodymium, and samarium was investigated thermogravimetrically in the temperature range 25° to 1,500° C. Each salt was decomposed at a heating rate of 2.5° C, per minute. The pyrolytic sequences have been identified and the temperatures of formation of inter-mediates, the minimum oxide formation temperatures, and values for loss on ignition have been determined. The nonstoichiometric ranges between Pr6011 and Pr203 and the extent of these ranges have been determined for oxides derived from the carbonate, nitrate, and oxalate salts of praseodymium. The alum and sulfate salts of praseodymium produced the sesquioxide without forming the intermediate non-stoichiometric oxides. The temperature limits of formation and regions of stability for the alums and sulfates were better defined than were those for the carbonates, nitrates, and oxalates. The minimum oxide formation temperature increased in the order of samarium, neodymium, and praseodymium irrespective of the anion.

Jan 1, 1962

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 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 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 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