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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

By T. A. Henrie, E. K. Kleespies

Carbon reduction of rutile and ilmenite in nitrogen and ammonia atmospheres was studied as a method of preparing titanium nitride . Ammonia was a better nitriding agent than nitrogen . The contact between the solid reactants , carbon and rutile , was a prime factor in nitrogen atmospheres and was of lesser import in dissociated ammonia . The reduction process for conversion of rutile to the nitride required carbon . The nitriding of ilmenite- carbon mixtures produced titanium nitride and elemental iron .

Jan 1, 1964

By D. W. Bridges, S. R. Borrowman

Thorium and yttrium oxides were recovered from siliceous ores of the Powderhorn , Colo . , area . Processing comprised ( 1 ) acid curing and subsequent ( 2 ) acid baking , ( 3 ) leaching , and ( 4) solvent extraction of thorium , using a primary alkylamine , and yttrium , using di - 2 - ethylhexyl phosphoric acid . About 95 pct of the contained thorium and yttrium was recovered from ore containing 1.2 pct Th02 and 0.5 pct Y₂ 03. The thoria product was 99 pct Tho ; the yttria product was 77 pct Y₂ 03. A 150 - to - 1 concentration ratio was effected on the latter , but some contaminating lanthanon - group oxides remained .

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 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 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 M. H. Kersten, G. A. Brady, Jerry W. Ramsey

Anthracite samples were oxidized with nitric acid to prepare products representing intermediate stages of oxidation . Similar oxidizing conditions affected different anthracites to varying degrees as characterized by peptization behavior with 0.1 N NaOH . Techniques used in attempts to separate and characterize the products included esterification , absorption spectrophotometry , sublimation , chromatography , electrophoresis , metal salt formation , and solvent extraction . Mellitic acid , either free or in the form of metallic salts , was identified in the acid- soluble products from 10 tests in which the anthracite was treated with nitric acid for periods varying from 24 to 1,000 hours . pentacarboxylic acid was also found in some products . Other benzene carboxylic acids were not present in amounts detectable by the methods used in this study . The acid- insoluble residue from nitric acid treatment varied significantly in solubility behavior toward different classes of solvents . The most effective ones tried included polar oxygenated solvents and pyridine . Infrared spectra of the extracted material indicated that similar compounds were extracted by the different solvents . Aliphatic amines and aniline peptized the residue and o- toluidine reacted with it . Organic material separated from the residue by peptization with dimethylformamide contained 1 percent ash , consisting of more than 50 percent zirconium .

Jan 1, 1964

By Foster Fraas

The response of minerals in magnetic separators is in accordance to dynamic rather than static magnetic susceptibility values . The dynamic value varies with respect to both passage speed through the separating field and time of exposure in a preliminary treatment field . Tests on 16 minerals and solids have demonstrated that both of these factors affect different minerals in different ways .

Jan 1, 1964

By D. Bienstock, J. H. Field, M. J. Lempel

A computer program is presented to perform the detailed and numerous calculations required for determining the interface temperatures and steady - state heat flow through a furnace wall composed of several refractories in layers . A method is developed that will allow the designer to determine the various thicknesses for each refractory layer to minimize either the total wall thickness or the cost of the wall per unit of area . A sample problem is presented and analyzed to illustrate the techniques involved .

Jan 1, 1964

By K. K. Kelley, L. B. Pankratz

The heat contents of four silicate minerals -- akermanite , cordierite , gehlenite , and merwinite --were measured from 298 ° to around 1,700 ° K by the dropping method . The results were compiled into tabular and equation forms suitable for thermodynamic calculations . The heat contents of these compounds are nearly additive with respect to their constituent oxides .

Jan 1, 1964

By J. B. Zadra, H. J. Heinen

Electrowinning molybdenum from oxide feed materials dissolved in a variety of molten baths was investigated . A NaCl - NaF - Na₂ B₁ O -Mo0, system operating at 1,000 ° C in a cell without a protective atmosphere gave the best current efficiency , metal - to - cathode adherence , and purity of electrowon Technical - grade molybdic oxide , containing associated impurities of aluminum , iron , copper , silicon , and tungsten in combined quantities of 10 percent , was used as feed material to produce dendritic crystals of molybdenum metal containing less than 0.5 percent total base metal , carbon , and oxygen impurities . Arc - melting molybdenum electrowon from either chemically pure or commercial - grade Mo0, produced ingots that contained less than 0.1 percent total impurities and had hardness readings of 168 to 200 Vhn .

Jan 1, 1964

By R. V. Lundquist, A. E. Morris, E. L. Singleton

This experimental research was performed to determine rate - of - reaction constants on the MnO - C and Mn , C₂ - 3MnO systems at 1,100 ° , 1,150 ° , and 1,185 ° C. Reactions were conducted at atmospheric pressure under controlled flow of purified helium through the furnace chamber . The weight - loss method defined reduction percentages , and reaction products were identified by X- ray methods . The system Mn0 - C followed a linear reaction rate , and experimental results produced an apparent activation energy of 55.8 kcal per mole of Mn0 . The system Mn, C - 3Mn0 followed a parabolic rate of reaction law and yielded an apparent activation energy of 114.4 kcal per mole for the reaction .

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

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 W. A. Stickney, J. W. Town

Studies on continuous - circuit leach - aluminum precipitation and leachelectrodeposition of mercury were made by the Bureau of Mines to determine optimum conditions and cost estimates for recovering mercury from mercury sulfide flotation concentrates . With 150 grams of sodium sulfide and 50 grams of sodium hydroxide per liter , from 98 to 99.8 percent of the mercury was extracted from flotation concentrates , with about 0.5 pound of sodium hydroxide used per pound of mercury produced . Precipitation of mercury from the caustic - sulfide solution with minus 8 - mesh aluminum shot required about 0.2 pound of aluminum per pound of mercury produced at a cost of $ 0.05 per pound of mercury . Electrodeposition cost with 7 mill power , based on 50 percent current efficiency , was below 2 mills per pound of metal deposited . Feed solutions ranged from 10 to 130 grams of mercury per liter , and current densities , from 2 to 70 amperes per square foot . The cost of open- pit mining 250 tons per day was estimated at $ 1.75 per ton , and flotation - leachingelectrodeposition of the ore , at $ 3.54 , resulting in a cutoff grade of about 0.1 percent mercury . The cost of underground mining 50 tons per day was estimated at $ 20.00 per ton , and the cost of milling the ore was estimated at $ 13.33 , which resulted in a cutoff grade of 0.6 percent mercury .

Jan 1, 1964