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By Henry M. Harris, John E. Kelley, Thomas D. Roberts

A penetrometer apparatus for measuring viscosity of glass at temperatures up to 1,450 ° C was developed for use in establishing the viscosity coefficients required for high- temperature forming of ceramic materials . The major advantage of the method is that it can be used with samples of almost any shape or size without the necessity of forming or measuring shapes to close dimensional tolerances . Also , it has proved accurate in the range of 106 to 109 poises , a gap between the normal limits of other methods . The device , which operates on a single penetrometer principle , was used to determine the absolute viscosity coefficient of substances in centimeter - gram- second units of poises instead of relative penetration - rate units as with other penetrometers . Penetration of the viscous sample was sensed with a linear , variable differential transformer . The output of this transformer was recorded versus time , and the penetration rate was used in calculating the viscosity coefficient . The general equation relating penetration rate and viscosity coefficient was found to be 11 = F ( ln L/a 0.72 ) 2 π UL · where is the viscosity coefficient in poises , F is the penetrator load in dynes , L is the penetration depth in centimeters, a is the penetrator radius in centimeters and U is the penetration rate in centimeters per second . The penetrometer was tested using a standard viscosity sample of sodalime - silica glass obtained from the National Bureau of Standards ( NBS ) . Values obtained at several temperatures all agreed within 10 percent with comparable data calculated from the Fulcher equation derived by NBS for this glass . Equivalent accuracy was obtained with other glasses used to evaluate the apparatus .

Jan 1, 1964

By Charles C. Myers, Robert M. Doerr

The apparatus described was developed for determining the kinetics of gas - solid reactions at high temperatures by measuring the volume of gas consumed with respect to time . This apparatus consists essentially of a horizontal precision- bore glass tube connecting a small reaction chamber in a furnace to a large constant - temperature reservoir . A drop of mercury in the tube separates the two sides of the system and serves as an indicator that moves at a speed proportional to the rate of gas consumption . The sensitivity of the apparatus depends inversely on both the density of the gas in the system and the cross - sectional area of the tube ; with a tube having an area of 0.079 cm² , the sensitivity for oxygen at 308 ° K and 0.5 atm is 20 cm/mg . The reproducibility of data with the volumetric apparatus is good .

Jan 1, 1964

By V. E. Homme, M. M. Wong

Tests were made in reactors ranging from 12 to 30 inches in diameter to develop methods for the preparation of sodium chloride - titanium lower chlorides ( dichloride and trichloride ) melts that contain titanium predominantly in the divalent state . Such melts are desirable as a starting material for the production of titanium metal or as an electrolyte for electrorefining of titanium . Sodium reduction of TiCl with an 18 - hour period of holding the reaction products in the molten state produced melts that contained titanium lower chlorides in TiCl₂ - to - TiCl , molar ratio of approximately 8 to 1. Sodium reduction of TiCl in a reactor with a shielded pipe weir , that required no melt -holding period , produced melts with a TiCl₂ - toTiCl , molar ratio as low as 4 to 1 . Reduction of TiCl4 with scrap titanium metal in molten sodium chloride produced relatively pure melts containing about 27 percent titanium in a Ticl₂ - to - Ticl , molar ratio of approximately 4 to 1 .

Jan 1, 1964

By W. L. Falke

Research was conducted to develop methods on a laboratory scale for recovering manganese from manganiferous slimes and limestones . The procedure is a low- temperature modification of the carbamate process , in which manganese is dissolved and the valence reduced by treating slimes and limestones with controlled amounts of sulfurous acid . Manganese ( II) hydroxide is precipitated and leached with ammonium carbamate solution , and manganese carbonate is separated by warming the leach solution . A major portion of the reagents is regenerated and recirculated . About 75 percent of the total manganese in manganiferous slimes , and from 50 to 75 percent of the total manganese in manganiferous limestones , are recovered as manganese carbonate containing 45 percent manganese .

Jan 1, 1964

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 Raymond W. Hiteshue, Henry H. Ginsberg, Paul S. Lewis

Coal was gasified in the presence of up to 3.57 million roentgens of gamma rays by the Bureau of Mines to determine whether the irradiation increased the gasification rate or yields of methane and hydrogen . High volatile A bituminous coal was gasified with steam at 500 and 1,500 psig and temperatures of 1,400 ° and 1,800 ° F ; five other coals ranging in rank from lignite to anthracite were gasified at 500 psig and 1,800 ° F. The average results of replicate experiments with and without radiation were compared for possible effects of radiation from 40,000 curies of radioactive cobalt . The irradiation had no gross effect on the gasification rate or on the yield and distribution of methane and hydrogen . It was concluded that gammaray irradiation produced no improvement in the technology or economics of coal gasification .

Jan 1, 1964

By K. D. Plants, J. H. Holden, L. F. Willmott

Pulverized high- volatile A bituminous coal was gasified with oxygen and superheated steam in a pressure - gasification pilot plant equipped for steampickup feeding . The pilot plant operated satisfactorily at relatively high steam- to - coal ratios , but steam- to - coal ratios could not be reduced much below 0.5 lb / lb without condensation of steam or softening of the coal . Carbon gasified , gas composition , and coal and oxygen requirements were essentially the same as for a pilot plant equipped with a fluidized coal feeder . Average results from the pilot plant equipped for steam- pickup feeding were coal requirement , 37.3 lb/M ( 1,000 ) scf of CO + H₂ produced ; oxygen requirement , 358 scf /M scf CO + H₂ produced ; and carbon gasified , 87.7 percent .

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 Foster Fraas

Review of the literature on solid solutions discloses that the relation between composition and magnetic susceptibility is not linear . Recalculation using a transformation of composition values to parameter v values provides for a linear relation with the magnetic susceptibility to the 1/2 power . Application to minerals is illustrated by the olivine and enstentite series .

Jan 1, 1964