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By T. A. Henrie, J. D. Marchant, E. S. Shedd

Cerium metal was electrowon in a fluoride bath from cerous oxide and tapped from the cell during prolonged operation . Electrolyte constituents were CeF , BaF₂ , and LiF. Twenty- seven pounds of metal of 99.8 percent purity were produced at a rate of 3 pounds per hour and tapped from the cell . Principal impurities were molybdenum , aluminum , oxygen , and carbon . The operating parameters , such as electrode geometry , bath compositions , and oxide feed rate , were investigated . Anode reactions were found to be important factors in cell operation . Stable cerous oxide reacted more uniformly at the anode surface than ceric oxide . Electrowinning was conducted in crucible hearths consisting of both frozen electrolyte and molybdenum metal . Both materials proved satisfactory and did not react with the molten cerium . Stable cerous oxide was prepared by carbothermic reduction and used as a feed material . Cell design proved to be an important factor in continuous cell operation . Complementary to the investigations of electrowinning of cerium , the metal was purified by electrorefining in a chloride electrolyte .

Jan 1, 1964

By Dean C. Holt

This work was done to appraise the potential of titanium minerals in known titanium- bearing placer deposits and potential titanium- bearing placer areas in western Montana . Reconnaissance studies were made of more than 225 stream areas . Churn drilling and other placer exploration techniques were used in sampling eight deposits . The sampling results indicate that areas containing more than 10 pounds of ilmenite and other titanium- bearing black - sand minerals per cubic yard occur in the Bitterroot , Upper Clark Fork , and Jefferson River drainages . The chief source for the constituents of the black sands appears to be the Idaho batholith , and the highest black - sand concentrations are generally found near the source . Sample testing methods include gravity and magnetic separation and visual microscopic as well as chemical and radiometric analyses on deposits sampled in detail .

Jan 1, 1964

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

To increase safety and productivity in mining , the potential uses and hazards of rigid foam were investigated by the Bureau of Mines Experimental Coal Mine . This research resulted in the development of chemical formulations , spraying equipment , and application procedures that permit safe and effective use of urethane foams for improving mine ventilation , for reducing weathering of mine rock and steel , for constructing seals in fire areas , and for thermal insulation .

Jan 1, 1964

By C. E. Wicks, F. E. Block, F. D. Stevenson

The vapor pressures of tungsten (VI ) chloride ( WC1 ) and hafnium ( IV ) iodide ( HFI ) were measured by a metal diaphragm technique . Vapor pressure values were obtained to permit calculation of the thermodynamic properties of the vaporization processes of the compounds . The vapor pressure data of WC16 are represented by the following equations for the liquid , B - solid , and a- solid over the temperature intervals indicated : - log P = 8.194 3,253 /T Liquid , 281.5 ° to 325 ° C : B - solid 230.0 ° to 281.5 ° C : log P a - solid 185.0 ° to 230.0 ° C : log Pam *** = 8.794 - 3,588 / T = 9.615 - 3,996 /T where T is the absolute temperature in degrees Kelvin . The heats of vaporization and sublimation are 14.9 , 16.4 , and 18.3 kcal / g mole , respectively . The entropy of vaporization at the normal boiling point , 330 ° C , was 24.3 eu . The fusion temperature , 281.5 ° C , and transition temperatures , 230.0 ° and 185 ° C , were found by thermal analysis .

Jan 1, 1964

By Theodore L. Turner, Joseph H. Swift

A study on a small laboratory scale was made of the use of ammoniacalammonium carbonate for batch leaching Mn from low- grade manganiferous materials ( 6 to 16 pct Mn) obtained from deposits in the southern district of Aroostook County , Maine . These materials were partially reduced at 500 ° to 700 ° C with H₂ or CO and then leached with solutions of NH and CO₂ dissolved in water . Extraction of 80 to 90 pct of the Mn was obtained from some sample materials , but 10 to 34 pct of the iron was also extracted . Material from the Littleton Ridge deposit contained manganese intimately associated with Fe , a condition which contributed to difficulties in obtaining a commercially acceptable product . Extensive investigations of the leach and reduction processes with various mixtures of H₂ and water vapor , and CO and CO₂ , failed to disclose a set of conditions for selectively leaching the manganese . Finely divided metallic Fe was probably produced during the reduction steps so that Fe was leached with the Mn in the subsequent extractions .

Jan 1, 1964

By Joseph M. Singer

Ignition of hybrid coal dust - methane - air mixtures by hot- turbulent - pulsedgas jets was investigated . The turbulent jets were generated by explosions in a primary chamber of stoichiometric mixtures of methane , oxygen , and nitrogen . The hot - gas ignition apparatus provided an adjunct means of testing , on a small scale , the type of ignition that exists in large - scale galleries or in coal mines . = coal particle The temperature Ignition variables were channel diameter , channel length , size , fuel concentration , and temperature of the hot - gas jet . of the hot jet was varied by changing the oxygen indices ( OI ) of the primary explosion mixtures . Coal dust having approximately 37 percent volatile matter was used . 02 O2ટ + N₂ The hybrid coal dust - methane - air mixtures required higher jet temperatures ( higher oxygen indices ) for ignition than the single fuel component methane - air mixtures . Methane in air concentrations less than the lower flammable limit of methane could be ignited in the presence of coal dust if the jet temperatures were increased . A specific explosion transmission ( ignitability ) curve existed for each coal dust concentration . The total fuel concentrations at the lower limit of each ignition curve was always close to or greater than stoichiometric , indicating that not all the coal dust was involved in the ignition .

Jan 1, 1964

By Charles J. Stehlik

This report deals with the changing behavior of mine roof bolt and roof rock as a result of repetitious production blasting . Observations were made in the upper shale production headings at the White Pine Copper Co. room and pillar mine , White Pine , Mich . Roof bolt compression pads and a stratascope were used in the investigations , which were carried out in three separate test sites in which nearly identical procedure produced comparative , repetitive , and anomalous observations . Results indicate roof bolt tension change and roof quality deterioration anomalies were coincident with blasting . The hypothesized cause of the anomalies is a seismic shock generated by the blasts .

Jan 1, 1964

By Charles S. Allbright, Frank G. Schwartz, Marvin L. Whisman

Radioactive tracer techniques were used to gain a better knowledge of the types of compounds that cause gum formation in gasoline during storage . A selected organic compound was labeled with tritium and purified . An unstable gasoline was tagged by adding a small amount of the labeled compound . After storage of the gasoline at 110 ° F for 16 weeks , the gum that had formed was recovered . The amount of the test compound converted to gum was determined by liquid scintillation counting . About 70 compounds , including several classes and types , were studied . The compounds , listed in order of descending reactivity in the test fuel , were sulfur compounds , nitrogen compounds , polycyclic hydrocarbons , olefins , alkylbenzenes , and saturates . In the order of decreasing percentage of each in the gum , the compounds were monoolefins , alkylbenzenes , sulfur compounds , polycyclic hydrocarbons , nitrogen compounds , and diolefins . This type of information should be helpful in developing a method for predicting the storage stability of gasoline .

Jan 1, 1964

By E. R. Andersen, F. E. Block, T. T. Campbell

This work was done to develop methods for increasing the yields and purity of vanadium prepared by bomb reduction of vanadium compounds . Compounds reduced were V₂ 05 , V203 , VC , and VC13 . Sodium , calcium , and magnesium were used as reductants . Variables considered included reductant form , bomb size , pressure during reaction , method of ignition , and the use of slag fluidizing additives . It was concluded that yields of 85 to 90 percent can be effected by the calcium reduction of V205 in reactors measuring as much as 14 inches in diameter and 60 inches in height . Optimum charge composition included V₂05 , 65 percent excess calcium , and 0.4 moles sulfur per mole vanadium . Purity of the vanadium produced in large reactors varied from 99.5 to 99.8 percent . The higher purity metal , depending upon the amounts of interstitial impurities present , was usually cold ductile . Although high yields of up to 99.5 percent can be effected by bomb reduction of VC1 , the high pressures developed in the bombs and attack of the reactor walls by the byproduct chloride slags discourages this method of preparing vanadium . It was found that significant purification of impure regulus metal occurred when it was hydrided , crushed , acid leached , and vacuum dehydrided . Metal so treated can readily be converted to ductile sheet . A cost estimate based on the production of 100 tons of vanadium per year was prepared . It was concluded that pure ductile vanadium could be produced for approximately $ 20.00 per pound .

Jan 1, 1964

By Roy L. Wilfong, LeRoy R. Furlong, Louis P. Domingues

The bulk and apparent densities , particle size , and surface area of ceria powders derived from the ammonium sulfate , carbonate , nitrate , oxalate , and sulfate salts and heated at 950 ° to 1,500 ° C for 1 to 24 hours were studied . The bulk and apparent densities and particle size generally increased , and surface area decreased with increase in temperature and time of heating ; surface area was more sensitive to changes in temperature and time than the other properties studied . These properties of the ceria powders had a marked dependence on temperature and a lesser dependence on duration of heating at a given temperature ; and the source of oxide and thermal treatment cannot be considered optional in the preparation of refractory powders by thermal decomposition . The ammonium sulfate and sulfate salts heated at 950 ° and 1,200 ° C produced oxide powders with the lowest bulk density , the smallest particle size , and the highest surface area . The highest apparent densities were achieved for oxides resulting from the carbonate and the sulfate but the carbonate - derived material was considerably coarser . The surface areas of ceria powders derived from cerium salts decrease in the order of sulfate , ammonium sulfate , nitrate , oxalate , and carbonate . The observation of these physical properties are useful in predicting the sintering behavior of various oxide powders .

Jan 1, 1964

By Raymond W. Hiteshue, Sam Friedman, Robert Madden

Experiments were made in a semicontinuous unit to provide engineering data for designing experimental continuous systems . These systems would be used to study the hydrogasification of hvab coal and char (from lowtemperature carbonization ) to high - Btu gas . In experiments at 800 ° C and with a coal residence time of several seconds , yields of hydrocarbon gases increased from about 2,000 scf / ton of maf coal at 250 psig to 7,000 scf at 1,000 psig . With 15 minutes residence time , yields increased from 8,000 scf/ton of maf coal at 250 psig to 17,500 cubic feet at 1,000 psig . In all cases , small quantities of heavy oils were produced along with the gaseous hydrocarbons . Production of oils could be minimized with a corresponding increase in gaseous hydrocarbons by increasing the retention time of the volatiles within the hot zone . Yields of gaseous hydrocarbons from char were slightly greater than from coal under similar conditions . Although the hydrogasification reaction is very pressure dependent , substantial quantities of coal (40 to 60 percent ) could be reacted to gaseous hydrocarbons at pressures as low as 50 psig provided reaction temperatures were increased to 1,200 ° C. It was also demonstrated that a hvab coal could be hydrogasified continuously without incurring agglomeration . This was achieved by dispersing coal in a relatively large reactor with concurrent flow of hydrogen . At 1,000 psig and 800 ° C , it was possible to react about 35 percent of the coal and to produce a gas containing up to 52 percent methane .

Jan 1, 1964

By Hillary W. Clair

An equation is derived for the rate of reaction of a sphere of metal oxide in a restricted enclosure through which a reducing gas is flowing . The equation takes into consideration the reaction rate coefficient , transport through the gas and through the porous shell of reduced oxide , the rate of gas flow , and the volume of the enclosure . The equation serves as a model for predicting the course of reduction of a particle of metal oxide in a shaft furnace .

Jan 1, 1964

By Robert J. Brennan, Edward R. Navrocky, John W. Buch

In an effort to establish a highly productive mechanized mining system for anthracite beds pitching between 10 ° and 20 ° , for which conventional mobile equipment is not adaptable , the Bureau carried out an experiment in longwall mining using an Anderton- type drum cutter loader and friction - type yielding steel roof supports . The roof- support system proved to be inadequate for breaking the overhanging roof at the break line supports , with the result that the roof broke over the solid coal . The accompanying subsidence destroyed the continuity of the roof in the work area , and the project was discontinued .

Jan 1, 1964

By Richard F. Link, George S. Koch

Through the use of statistical methods, estimates of metal content and tonnage of an ore body made by using data from 18 diamond-drill holes are compared with actual values established with data from 1,829 drift samples. The reliability of the estimates made from the drill holes is assessed in several ways. The relationship of metal content (assay-width product) to grade is explained. It is concluded that useful estimates can be made from 18 drill holes provided that reasonable assumptions are made and certain risks accepted. The ore body investigated is the Don Tomas vein of the Frisco mine, San Francisco del Oro, Chihuahua, Mexico.

Jan 1, 1964

By C. E. Wicks, J. E. Tress, F. E. Block

The Bureau of Mines investigated the effects of gamma radiation on materials and chemical reactions to obtain information that could be of value in modern metallurgical practices . Various combinations of metals and their ores and compounds were irradiated in attempts to effect reactions that might be applicable in the extraction and separation of metal values from minerals and The types of reactions studied included complexing of salts , decomposition of hydrated salts , metal chlorination reactions , leaching of ores and minerals , halogen exchange , and various reducing reactions . All irradiations were performed at the Materials Testing Reactor Gamma Facility of the U.S. Atomic Energy Commission at Idaho Falls , Idaho . Spent fuel elements were utilized as the source of the gamma radiation . Some irradiation - induced changes , ranging from mere color change to participation in chemical reactions , were noted . The greatest value of these investigations , however , was the experience acquired , which should be valuable in future explorations of similar nature .

Jan 1, 1964

By J. W. Eckerd, W. S. Sanner, P. L. Woolf, R. E. McKeever

The Bureau of Mines experimental blast furnace was operated successfully with anthracite metallurgical briquets . Tuyère pressures were higher and more erratic than for operations using coke , and furnace " hangs " occurred more frequently . Higher hot - blast temperatures were required to maintain the quality of the metal . By using higher hot blast temperatures , the fuel and production rates and slag volumes were comparable to those obtained for all - coke operation . The anthracite metallurgical briquets exhibited excellent mechanical strength and descended through the shaft of the furnace with little breakage or reduction in size .

Jan 1, 1964

By Richard W. Lewis, Lloyd Carpenter

The objective of the investigation was to determine spectrochemically 19 elements in the general range of 0.5 to 1,000 ppm in high - purity hafnium and its compounds . Samples were converted thermally to hafnium dioxide , mixed with buffer - carrier - internal standards , and excited by a dc arc . Spectra were recorded on photographic plates . Transmittance values were recorded densitometrically and converted to relative - intensity ratios . Four groups of standards were used to establish analytical curves from which the concentrations of impurities were obtained . Average precision of the method was 14.2 percent relative standard deviation , and relative error was 4.2 percent .

Jan 1, 1964

By C. H. Schack, K. C. Dean

An investigation was made to devise and evaluate a flexible flotation method for beneficiating typical tactite types of calcareous scheelite - bearing ores ; these scheelite - bearing ores are available in large tonnages in deposits containing 0.2 to 0.3 pct tungsten trioxide . The objective was to achieve a high recovery of the tungsten in concentrates , containing a minimum of 10 pct WO3 , that would be suitable for chemical processing into high- quality synthetic scheelite . The principal problems encountered and resolved by bench- scale flotation tests on ore samples from five different deposits were to define the conditions and reagent combinations essential for ( 1 ) achieving selective flotation of a small amount of scheelite from a large amount of calcite and ( 2 ) controlling the effect of small amounts of calcium , magnesium , and iron salts in the ores and water used . The flotation process was evolved from batch tests and continuous runs in a pilot - scale mill with a capacity of 100 lb per hour . The flotation process comprised ( 1 ) removal of sulfide minerals , ( 2 ) conditioning the residual ore pulp with sodium carbonate , quebracho , and trisodium phosphate , and ( 3 ) rougher flotation and single - stage cleaning of a scheelite concentrate . In a pilot plant run , over 91 pct of the tungsten was recovered from ore containing 0.27 pct WO3 , in a concentrate containing 11.2 pct WO3 .

Jan 1, 1964

By William I. Nissen, Richard Havens

Continuous flotation studies were made at a 50 - lb - per - hr feed rate to confirm the effectiveness of a batch - scale procedure for concentrating phenacite and bertrandite minerals from Mount Wheeler ores that contained , in percent , 0.47 , 0.78 , and 4.7 BeO . The procedure for selective froth flotation of the beryllium minerals from a gangue composed chiefly of calcite , fluorite , and mica comprised closely controlled preconditioning with sodium fluoride and sodium hexametaphosphate in a series of small mechanically agitated tanks and use of a mixture of oleic acid with kerosine , fuel oil , or turpentine as a collector . It was difficult to adapt the laboratory flotation procedure to continuous operation . The principal problem of achieving adequate conditioning to depress calcite and fluorite ultimately was resolved by conditioning in series . Thereafter , three ore samples of different grades treated on a continuous basis yielded concentrates containing from 12 to 25 percent Beo from these relatively complex and difficult ores . Recoveries , on a BeO basis , ranged from 75 to 88 percent . Losses , which primarily were due to incomplete liberation , probably could be lowered in a commercial operation .

Jan 1, 1964

By I. L. Nichols, K. C. Dean, P. H. Johnson

Hydrochloric acid , sulfuric acid , and chloridizing roast- water leaching methods for dissolution of cesium and rubidium from Maine , Canada , and Southern Rhodesia pollucite ores and their flotation products were investigated by small- scale tests . Optimum conditions were determined to be ( 1 ) for hydrochloric acid leaching , use 12.7 equivalents of 8.8 normal acid per equivalent of cesium in the sample and leach for 6 hours at 100 ° C ; ( 2 ) for sulfuric acid leaching , use 12.7 equivalents of 14.4 normal acid and leach for 2 hours at 120° C ; and (3 ) for chloridizing roast - water leaching , roast minus 200 - mesh ore, limestone , and calcium chloride in a ratio of 2 : 4 : 1 , respectively , for 1 hour at 900 ° C , and leach the calcine for 1 hour at 80 ° C with enough water to give 35 pct solids . Extractions of cesium from ores and flotation products containing over 20 pct cesium were in excess of 97 , 93 , and 96 pct for the hydrochloric acid , sulfuric acid , and chloridizing roast - water leach processes , respectively .

Jan 1, 1964