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By F. R. Cattoir, R. E. Cumings

Columbium metal was electrorefined in a fused - salt electrolyte . Excellent results were obtained in lowering the impurity content in a 94 - percent columbium anode feed material to produce a 99.8- percent - pure metal . The reductions of the major impurities follow : Oxygen from 19,800 to 500 ppm , carbon from 9,700 to 25 ppm , iron from 9,200 to 630 ppm , nitrogen from 2,100 to 90 ppm , and silicon from 750 ppm to not detected . Columbium with a purity of 99.9 percent was produced from 99.5- and 99.8 - percent grades of columbium. The investigation was devoted to the evaluation of a fused - fluoride - salt electrolyte ( KF - NaF- K₂ CbF, ) for electrorefining columbium. The effects of the columbium concentration and the voltage upon the product's purity were investigated . The effect on the cathode current efficiency of ampere - hours of deposition and the formation of a dual valence state of the columbium was also investigated .

Jan 1, 1964

By D. J. Donaven, Manuel Gomez, W. S. Landers

Bulk density tests were made on a Western U.S. coke oven plant blend to obtain bulk density control data that would be directly transferable to plant practice . Maximum bulk density values were obtained at zero surface moisture . Increase in surface moisture to about 6 percent decreased the bulk density to a minimum value . Increase in the fine grinding of the blend , at constant surface moisture , decreased the bulk density . The effect of oil on bulk density was observed with five oils at concentrations ranging from 1/8 to 1-1 / 2 gallons per ton . Maximum bulk densities were obtained within the 1 / 2- to 1 - gallon - per - ton range . Essentially the same bulk densities were obtained with petrolatum- and nonpetrolatum- containing oils . Storage effects were observed on samples tested at selected intervals from 0 to 56 days . No significant change in bulk density took place if no surface moisture was lost during storage .

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 Oren C. Baptist, Carlon S. Land, Eliot J. White

The water sensitivity of the oil - gas - producing sandstones in three fields in the Patrick Draw area of southwestern Wyoming was estimated by laboratory testing . The tests used to estimate sensitivity , which is a measure of the loss of well productivity if the producing formation is invaded by fresh water , are : Porosity ; permeability to gas , water , and brines ; saturation characteristics with air displacing water from the samples and by mercury injection ; and identification of clay minerals by X - ray diffraction . Laboratory results indicate that the degree of water sensitivity of the sands in the Patrick Draw, Table Rock , and Desert Springs fields vary , in that order , from moderately sensitive to highly sensitive . The main cause of the sensitivity appears to be the movement of fine particles in the pores , but the swelling of a small amount of an expandible clay mineral may also contribute to the permeability reduction observed in the samples . Laboratory results further indicate that the permeability of the sands to fresh water is seriously reduced if they are first flushed with sodium chloride brine ; calcium chloride brine is less harmful to the sands than sodium chloride brine . The low original permeability of the oil sand in the Patrick Draw field , together with its moderate sensitivity , indicate that the rate of water injection for the secondary recovery of oil will be low . Limited field experience in two pilot - injection wells confirms this prediction .

Jan 1, 1964

By T. Estelle Gardner, A. R. Taylor

Heat capacity measurements were made on sodium bromide ( NaBr ) and sodium iodide ( NaI) in the temperature ranges of 7 ° to 300 ° K and 56 ° to 300 ° K using an adiabatic calorimeter . Smooth values of heat capacity, entropy , enthalpy function , and free- energy function were calculated from the heat capacity data at 10° K intervals and at 273.15° and 298.15° K. Entropy and free energy of formation values at 298.15° K also were calculated for the two compounds using entropy values determined in this study and other data reported in the literature . The entropy values calculated at 298.15 ° K were 20.75 ± 0.06 entropy units (eu ) for sodium bromide and 23.55 ± 0.07 eu for sodium iodide .

Jan 1, 1964

By R. V. Lundquist, H. Leitch

Sodium aluminate is the principal aluminum compound formed in the sinters prepared by the lime - soda sinter process for recovering aluminum from silicate source materials . The properties and characteristics of this compound were studied to improve the efficiency of the process . Crystalline sodium aluminate was prepared by sintering stoichiometric quantities of soda ash and calcined alumina for 1 hour at 1,250 ° C. The extent of aluminum extraction from sodium aluminate was determined in water and in solutions of NaOH and Na₂ CO3 . Nearly complete extraction of aluminum from sodium aluminate was achieved only in solutions containing free NaOH in excess of that supplied by the salt through hydrolysis . About 42.2 to 68.8 percent of the aluminum was extracted in water or in solutions of Na₂ CO . The precipitation of alumina trihydrate from sodium aluminate solutions was shown to be part of a continuous , reversible reaction according to the equation Al (OH ) A1 (OH )3 + OHThe reverse reaction dissolves alumina trihydrate in NaOH solutions to produce sodium aluminate . Approximate equilibrium concentrations were determined for the reaction at 30° , 50 ° , and 70 ° C. False apparent equilibrium conditions for the dissolution reaction appear when only a small excess of alumina trihydrate is present in the NaOH solutions . A large excess of alumina trihydrate must be present before the true equilibrium point is assured . The engineering significance of the data is summarized , showing controls that should be exercised for a successful and efficient process .

Jan 1, 1964

By Scott W. Hazen

This report presents the results of a statistical analysis of a limited amount of sample and assay data from a production panel in an open - pit phosphate mine in the Phosphoria formation in Idaho . A frequency distribution analysis is shown for the assays , sample interval lengths , and products of assay and sample interval length for the millshale , furnace - shale , and main phosphate beds . Correlation techniques were used to show the relationships between assays and sample interval lengths . Within- drill - hole and between - drill - hole correlation were also examined as a means of predicting grade trends in the ore . Simulation methods , utilizing a digital computer , were used to establish assay populations that could be used for estimating grade of ore , cutoff grades , and deposit or bed identification .

Jan 1, 1964

By K. A. Fowler, L. W. Higley

The effect of uranium on the transformation kinetics and the hardenability of a low- alloy steel was evaluated . Isothermal transformation curves were developed from metallographic studies , and hardenability was determined by standard Jominy end- quench tests . For the steels investigated , the addition of 0.15 weight- percent uranium was found to produce a significant shift in the isothermal transformation curve and caused a related increase in hardenability . These effects diminished rapidly when the uranium content was increased above 0.2 weight - percent .

Jan 1, 1964

By George H. Holmes

Beryllium deposits in the northern Virgin Mountains , Clark County , Nev . , and Mohave County , Ariz . , about 70 miles northeast of Las Vegas , were investigated by the Bureau of Mines . The investigation indicated a widespread occurrence of beryllium- bearing pegmatites within an extensive belt of mica - schist . Several deposits with significant beryllium mineral concentrations were encountered . Only a few of the samples analyzed contained more than 1 percent beryllium oxide ( BeO ) ; in many of the samples , no beryllium was reported . The average tenor of samples from the more important occurrences was 0.25 percent BeO . Chrysoberyl is the predominant beryllium mineral in the pegmatite sills ; beryl predominates in the more massive bodies . Minute quantities of cesium and lithium minerals also occur , but no columbium , tantalum , or other rare minerals were found . Ore dressing tests on a composite sample containing 0.28 percent BeO which was representative of the pegmatite sills , indicated an 85 percent recovery of the chrysoberyl ( 70 percent recovery of total BeO ) by gravity concentration in a concentrate containing 17.6 percent BeO .

Jan 1, 1964

By H. R. Shell, John L. Miller, M. V. Denny

In the mica research program conducted by the Bureau of Mines at Norris , Tenn . , many micas other than silicon fluorphlogopite have been synthesized . It has been well established since the initiation of the program that synthetic micas are important materials useful for their superior or unique properties as well as substitutes for natural micas . The possibility of controlling the physical properties of synthetic mica by isomorphic substitution of other ions in the fluorphlogopite lattice further emphasizes the importance of these materials . Accurate measurement and reporting of their properties constitute an essential part of the research program . The study of germanium fluorphlogopite is in keeping with the requirements of a comprehensive study on isomorphic substitution , specifically to identify precisely the material -- chemically , structurally , and optically . The X- ray measurements , including indexed powder and single crystal data , with a description of the methods used to obtain these data , are provided . 5 Earlier work on germanium mica by R. A. Hatch et al . (5) gave an estimate of the cell parameters from X - ray powder data , but no attempt was made to index the diffraction pattern or to determine the space group symmetry . Later work by E. A. Schatz and J. C. Withers (9) listed X- ray and optical measurements , but no attempt was made to index the mica or determine its symmetry . Roth (7) found that germanium dioxide having the a - quartz structure , when heated with equimolar percentages of MgO , CaO , Sr0 , or Ba0 at 1,235 ° C , formed ABO3 -type compounds , e.g. MgGe03 isostructural with enstatite (MgSiO3 ) . Geo₂ also has a rutile - type polymorph with Ge ++ ions in octahedral coordination . Germanium was substituted for silicon in the serpentine structure by Roy and Roy (8 ) using hydrothermal techniques . These authors wrote as follows : "The substitution of Ge + for Si + yielded a magnesia - germania serpentine , formed easily in euhedral hexagonal plates which in some instances were visible in the light microscope . Electron micrographs and the sharp X - ray diffraction patterns confirm a plate - like rather than tubular habit . " It has been shown in this investigation that substitution of germanium for silicon in the mica structure is readily accomplished without radically changing the characteristics of the mica . Substitutions in the mica structure take place in three locations : Tetrahedral , octahedral , and interlayer positions . The tetrahedral positions are normally occupied by Sit or by a combination of Sit with Al +3 the most common combination being 2A1 +3 and 6Si +4 · , The octahedral position , which has six - fold coordination in phlogopite , contains a larger cation such as magnesium . In muscovite it contains only 2A1 ions ; therefore , this mica is considered a dioctahedral mica , whereas phlogopite is considered trioctahedral . +3 The interlayer position has twelve - fold coordination with six oxygen ions from each of two adjacent tetrahedral silica layers . This is the cleavage plane of the mica and commonly contains the largest cation in the mica structure (e.g. potassium) .

Jan 1, 1964

By Sarkis G. Ampian

Published optical microscopic and X- ray diffraction characteristics of the following compounds are critically evaluated and compared with Bureau of Mines data : Tricalcium aluminate , calcium monoa luminate , dodecacalcium heptaluminate , dicalcium silicate , tricalcium silicate , and sodium aluminate . A recommended set of definitive optical and X- ray diffraction characteristics is presented . These values are used to identify products of the lime soda sinter process for production of alumina . Polymorphism of gamma- , beta- , and alpha prime - dicalcium silicate is reexamined , and new data are presented on polymorphism of tricalcium silicate and sodium aluminate by high- temperature X- ray diffractometry . Polymorphism is not observed for tricalcium aluminate , calcium monoaluminate , and dodecacalcium heptaluminate . Bureau of Mines data indicating a stoichiometry of 12Ca0.7A10 for the phase 5Ca0.3A1 0₂ are discussed . A critical review of the literature concerning calcium dia luminate and sodium undecaluminate ( 8 -A10 ) is also included .

Jan 1, 1964

By Raymond W. Hiteshue, Sam Friedman, Martin D. Schlesinger

The Bureau of Mines in cooperation with the El Paso Natural Gas Co. investigated the effect of high temperature and pressure at short residence times on the hydrogenation of a New Mexico coal to gaseous and liquid hydrocarbons . The study was made in a bench - scale semicontinuous unit at pressures of 500 to 6,000 psig , 480 ° to 1,000 ° C , and residence times of less than 1 minute to 15 minutes . Ammonium heptamolybdate was impregnated on the coal to furnish 1 percent molybdenum based on maf coal . Coal could be rapidly hydrogenated at elevated temperatures and pressures to yield large quantities of gaseous hydrocarbons and small quantities of lowboiling oils , high in single - ring aromatics . At 800 ° C and 6,000 psig and a residence time of 1 minute , the yield of hydrocarbon gas was 43 percent and of liquid hydrocarbons 9 percent , based on maf coal . With a 15 - minute residence time , the yield of gaseous hydrocarbons increased to 68 percent with a decrease in yield of oil to 6 percent . At higher hydrogen velocities , the yields of oil were much greater but contained large quantities of asphaltene . Low concentrations of molybdenum (0.01 and 0.1 percent ) or a high concentration of iron ( 1 percent ) were ineffective at 800 ° C , 6,000 psig , and short residence time .

Jan 1, 1964

By M. E. Tyrrell, C. W. Houck

Mixtures of zirconium diboride and refractory metals of group VI were resistance sintered to high - density compacts using modified electric welding equipment . To evaluate the use of chromium , molybdenum , or tungsten as binders for zirconium diboride the sintered compacts were examined in polished sections and tested for crushing strength , hardness , microhardness , oxidation rate , and resistance to mechanical shock . Chromium yielded the highest compressive strength , the greatest resistance to mechanical shock and oxidation , and a satisfactory Rockwell hardness . Molybdenum did not yield a satisfactory cermet . Tungsten yielded compacts having high microhardness but very low mechanical strength .

Jan 1, 1964

By Alla D. Mah

The heat of combustion of aluminum carbide (Al, C3 ) , obtained directly by combustion calorimetry , was AH298.15 -1,029.6 ± 1.9 kcal / mole . == The heat of formation of aluminum carbide corresponding to this value was AH298.15 = -53.4 ± 2.0 kcal /mole .

Jan 1, 1964

By L. H. Adami, E. G. King

The heats of formation of four sulfides --MnS ( alabandite ) , FeS ( hexagonal pyrrhotite ) , ZnS ( wurtzite ) , and CdS ( greenockite ) -- were determined by hydrochloric acid solution calorimetry . The heats of formation from the metals and rhombic sulfur at 298.15 ° K are , respectively , -51.01 ± 0.19 , -23.81 ± 0.24 , -45.86 ± 0.20 , and -35.70 ± 0.30 kcal /mole . The corresponding free energies of formation were calculated from the heats of formation and the pertinent entropy values .

Jan 1, 1964

By M. E. Tyrrell, J. Koster

This work was undertaken to determine the feasibility of making mixed diborides of two metals directly from the metal oxides , boron carbide and carbon . The diborides (Ti , V ) , B₂ , (Ti , Cb) B₂ , and ( Ti , Ta ) B₂ were prepared in a crucible resistance furnace at 2,100 ° C , and X- ray- diffraction analyses showed each was a homogeneous solid solution containing approximately equal molar contents of the given diborides . The diboride powders were cold - pressed ; sintered to 2,300 ° C , and evaluated for mechanical strength , rate of oxidation , and resistance to molten metals . The diboride ( Ti , Ta ) B₂ exhibited the best mechanical properties ; the diboride ( Ti , Cb ) B₂ , the lowest cumulative rate of oxidation . The mixtures were stable in the presence of molten aluminum and copper but were attacked by molten Ti , Zr , and Cr .

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 Scott W. Hazen, Richard F. Link, George S. Koch

The Mi Vida mine , Big Indian district , San Juan County , Utah , is in an ore deposit of uranium and vanadium minerals disseminated in certain sedimentary beds of the Triassic Chinle formation . Statistical analysis of assays of samples taken from the ore body affords an estimate of the grade of the ore body and provides a prediction about the direction of best mineralization beyond the sampled area . The basic data analyzed are assay results for uranium ( Uз Og ) , vanadium (V₂O ) , and lime (CaO ) from 225 channel samples cut at 79 sample points . Through the use of appropriate statistical methods , particularly regression analysis , the grade of ore may be estimated more precisely than by conventional means , and the most favorable direction to extend the mine may be predicted . Frequency distributions of assay residuals for uranium , vanadium , and lime are compared to frequency distributions of assays without regard to trend . Correlations among these variables are obtained and interpreted . The statistical methods employed illustrate certain techniques that may be used to analyze assay data from ore deposits in general .

Jan 1, 1964

By H. D. Hess, C. P. Mabie

This report describes in detail the results of petrographic research conducted on 21 phosphate ores representing important deposits in southwestern Montana , southeastern Idaho , and northeastern Utah . The ores are described and categorized by mineralogical and chemical composition , thermal behavior of organic carbon , and textural constitution . Descriptive and genetic classification schemes applicable to western phosphate ores are discussed ; results from related studies made of the collophane mineralogy are also presented . The latter studies were centered on determining unit - cell dimensions and CO₂ , P2O5 , and fluorine content of collophane concentrates of 11 high - grade phosphate- rock hand specimens selected solely for this purpose . On the basis of this investigation , operational methods have been developed for quantitatively describing textural and compositional features that are likely to be significant in determining the response of phosphate ores to conventional beneficiation treatments ; systems for classifying the ores in relation to these features have been proposed . Studies to date point out distinct textural and compositional variations in the western phosphates and illustrate their importance in determining optimum beneficiation procedure .

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