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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 C. A. Pearson, W. D. Dietzman, M. E. Hawkins

Results of chemical analyses and electrical resistivity measurements of 422 samples of oilfield brines from 120 east Texas fields in Railroad Commission of Texas Districts 5 and 6 are presented in tabular form . These samples represent water from all of the major petroleum- productive formations in the area . Water analyses and electrical resistivity data , when fully utilized by proper study techniques , are useful tools in the solution of many engineering problems such as detection of well leaks , identification of water sources , and interpretation of electrical well logs . In the area included in this study , these representative data should facilitate the solution of problems in which water analysis and water resistivity are factors .

Jan 1, 1964

By J. B. Zadra, J. M. Gomes, Don H. Baker

Electrolytic deposition at 1,000 ° C in an electrolyte essentially consisting of 7 parts sodium pyrophosphate , 2 parts sodium chloride , and 1 part sodium tetraborate yielded tungsten of 99.9 percent purity . Scheelite concentrates containing 25 to 73 percent WO, and varying quantities of iron , lime , and silica were used as feed materials for the electrolysis . The metal contained less than 0.01 weight - percent each of iron , calcium , silicon , aluminum , carbon , and oxygen . Modification of the electrolyte permitted deposition of equal - quality metal from scheelite concentrates containing higher quantities of iron , calcium , and silica . The electrolytic separation of molybdenum and tungsten was accomplished by minor variations in the operating procedures .

Jan 1, 1964

By Rolland L. Blake

Petrographic and mineralogical studies were made on unoxidized samples from the Cuyuna and Mesabi districts to study occurrence and properties of the iron phyllosilicate minerals . Examination of 96 thin sections from the thinbedded facies of the main iron - formation of the Cuyuna district indicates that the most abundant minerals are Mn - Mg - siderite , stilpnome lane , and minnesotaite . Reconstitution and recrystallization of minerals has occurred along certain beds , and textures indicate that some minnesotaite apparently formed at expense of stilpnomelane . Three samples of stilpnome lane and one of minnesotaite were concentrated from fracture - fillings within iron- formation . Results of chemical , optical , spectrographic , X- ray diffraction , and differential thermal analyses on these samples are reported . The detection of ammonia in stilpnome lane samples is the first such occurrence reported , and its significance is discussed . New mineral data are presented on greenalite and probable septechamosite from the Mesabi district .

Jan 1, 1964

By C. Q. Cupps, R. F. Zaffarano, J. Fry

Reservoir oil analyses from seven wells in the Greater Clareton area have been included in a study of the original characteristics of oil in the Newcastle sandstone reservoir . These data correlated with areal location of the wells show an increase of saturation pressure in a general north - south or downdip direction . The increase amounts to about 500 psi in more than 17 miles , which corresponds to a depth increase of about 1,600 feet . To facilitate application of the data to engineering analyses , average characteristics are given for arbitrary north and south divisions of the 22 - mile - long producing area . The downdip increase of saturation pressure is taken as evidence of updip diffusion of solution gas from a somewhat higher concentration at the bottom of the reservoir . This effect is opposite to that previously observed in two prominent high- relief reservoirs in the Rocky Mountain area . The increasingly greater saturation pressures southward or downdip in the Greater Clareton area suggest a continuing migration of fluids into the structure .

Jan 1, 1964

By R. L. Crosby, L. W. Higley

Magnesium- rich magnesium- aluminum- zirconium alloys in the cast and in the extruded and heat- treated condition were studied to identify the phases present and to determine phase distribution . In cast alloys , two intermetallic compounds were identified : ZrAla by X- ray diffraction ; and Mg₁ Al₁₂ by microscopical observation . Based on microscopical comparisons between the known phases in the cast structures and the phases in the structures of extruded and heat - treated rods , ZrAl₂ and Mg1 , Al12 were identified in the structure of the latter . The presence of these intermetallic compounds in rod specimens could not be confirmed by X- ray diffraction . ZrAl₂ was observed in the structure of extruded and heat - treated rod specimens containing as little as 0.01 weight - percent zirconium . The presence of aluminum restricts the solubility of zirconium in magnesium because of the strong tendency to form ZrAla . This intermetallic compound segregated in clusters of small particles in the matrix of cast alloys , and only slight improvement in distribution was noted when the alloying techniques were varied .

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 D. H. Chambers, Arnold M. Lansche

Electro recovery by amalgam methods was investigated to determine the feasibility of recovering pure cadmium from cadmium sponge produced during purification of zinc electrolyte at electrolytic zinc plants . Actual material used in this work was air- oxidized cadmium sponge . An acid rinse and zinc displacement technique was developed to amalgamate this oxidized cadmium . ( In - plant use of the recovery process would probably not require this step because of the fresh state of the sponge . ) Zinc was completely removed from amalgamated sponge by selective oxidation with air . Zinc - free cadmium amalgam was circulated by an electromagnetic pump through an electrolytic cell where cadmium of 99.9+ percent purity was electrodeposited onto a rotating aluminum cathode . Polarographic methods were developed for determining cadmium and zinc in mercury and in sulfuric acid solution .

Jan 1, 1964

By S. L. Payne, E. F. Foerster, C. W. Schultz, G. R. Zellars

The vapor pressure of copper in a series of liquid copper - nickel alloys was determined by the carrier gas method . The activity and activity coefficient of copper were calculated over the entire range of alloy composition . These data show a slight positive deviation from ideal behavior . The activity coefficient of copper was highest ( 2.10 ) at 0.05 mole fraction copper and approached unity at concentrations above 0.85 mole fraction copper . The results for nickel were calculated from the copper data by the graphical integration of the Gibbs - Duhem equation .

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 Joseph A. Sutton, John D. Corrick

The chemistry involved in the microbial dissolution of iron and copper from such sulfide minerals as pyrite, chalcopyrite, chalcocite, cove11ite, and bornite is described. The chemical criteria used to evaluate the activity of microorganisms on these minerals were changes in pH, ferric iron produced, and oxygen consumption. In a series of experiments in which a ferrous sulfate nutrient solution was percolated over small portions of the above-mentioned copper sulfide minerals for 56 days, the iron-oxidizing bacteria Ferrobaci11us ferrooxidans and Thiobaci11us ferrooxidans were capable of bringing about the dissolution of 23.7 percent of the copper from chalcocite, 56.3 percent of the copper from cove11ite, and 29.8 percent of the copper from bornite by the microbial production of ferric sulfate which reacted with these minerals. Laboratory tests have demonstrated that pure strains of the iron-oxidizing bacteria act as catalysts to the ferrous iron being oxidized by the Oxygen of a system containing pyrite and chalcopyrite. In a series of experiments during which nutrient solution was percolated over pyrite for 70 days, the ferric iron produced by the iron-oxidizing bacteria was 112 to 120 times greater than that produced atmospherically.

Jan 1, 1964

By G. W. Birge, D. E. Wolfson, J. H. Lynch

This report presents all available 900 ° C BM- AGA carbonization and related data for coals from the principal beds of the southwest Virginia field in a form which permits ready comparison of product yields and properties of coals and cokes . Thirty- one channel samples from Buchanan , Dickenson , Russell , Tazewell , and Wise Counties were carbonized at 900 ° C in an 18 - inch - diameter retort . Blending properties of 10 of the coals were studied , and expansion of most of the coals and blends was measured in the Bureau of Mines sole - heated oven . Ash Most of the samples were chemically suitable for metallurgical use in coking blends , and their coking properties generally were satisfactory . content exceeded 10 percent in only three samples , and none of the coals contained more than 1.5 percent sulfur . Dry , mineral - matter - free fixed - carbon content of the coals ranged from 62.1 to 77.5 percent . Expansion behavior varied widely , ranging from 16.8 percent expansion to 27.6 percent contraction .

Jan 1, 1964

By M. R. Geer

Three coals from the Wilkes on - Carbonado district of Pierce County , Washington , were subjected to washability analyses to estimate the amount and quality of washed coal obtainable . Because the coals were unusually difficult to clean , the washability examinations were supplemented by table tests , tests in dense - medium cleaning units , and flotation tests . None of the coals could be reduced to the desired 10 percent ash by tabling and the response to flotation by two of them was poor . Dense -medium treatment provided coal of the desired quality , but with the most difficult coal the recovery efficiency was lower than usual .

Jan 1, 1964

By H. O. Poppleton, F. E. Block

This investigation was made to develop a method of preparing high - purity thorium metal in quantities up to 20 kilograms per batch . Several methods for the preparation , purification , and reduction of thorium tetrachloride are discussed . Thorium tetrachloride was prepared by chlorination of decomposed thorium nitrate or oxalate with carbon tetrachloride or phosgene . tion of the crude tetrachloride was achieved by multiple distillations or by filtration of the molten chloride . It was found that high - purity thorium metal could be prepared by sodium reduction of thorium tetrachloride if chloride of sufficient purity were available . Byproduct salts and excess reductant were removed by vacuum distillation , and the resultant thorium metal sponge was consolidated by consumable - electrode or fixed - electrode arc melting . It was demonstrated that metal prepared by this method could be fabricated into bar , rod , or sheet , at room temperature .

Jan 1, 1964

By R. L. Hopkins, H. T. Rall, H. J. Coleman, C. J. Thompson

Two methods were tested for separating sulfur compounds in certain petroleum fractions into types . Such separation is preliminary to identifying the compounds . Each method involved extraction of sulfides from petroleum sulfur concentrates . In the first method , the sulfur concentrate was reacted with methyl - ptoluenesulfonate to form sulfonium compounds from which unreacted portions of the sample were removed by washing with solvent . The sulfides then were recovered by heating the sulfonium compounds with anhydrous triethanolamine . The second method consisted of passing anhydrous hydrogen iodide into a n-butane solution of the sample cooled in dry ice , whereupon the hydrogen iodide adducted with the sulfides to form sulfonium compounds . These adducts separated as crystalline solids or , more frequently , as glassy viscous liquids . The sulfide was regenerated by adding water to the filtered sulfonium compound and was recovered by steam distillation or by extraction with pentane . These methods have been evaluated , using individual pure sulfur compounds and blends of sulfur compounds . They also have been applied successfully to separating sulfides from sulfur concentrates derived from petroleum fractions .

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 R. Barany

The heat of formation at 298.15 ° K of muscovite was determined by solution calorimetry . The value obtained for the heat of formation from the elements was -1,421.2 ± 1.3 kcal / mole , and the value for the heat of formation from the oxides was -55.9 ± 1.3 kcal /mole .

Jan 1, 1964

By W. C. Wahl, M. M. Fine

Leonardite , a naturally occurring , partially oxidized form of lignite with a high content of humic acids , was investigated as a binder for iron ore pellets . Although insoluble in original condition , leonardite forms watersoluble salts with good binding properties when treated with certain alkalis such as sodium hydroxide . Soluble leonardite imparts excellent dry strength to pellets , but green strength is somewhat lower than that obtainable with bentonite . However , green strength can be improved by adding a small amount of calcium hydroxide to the leonardite - concentrate mixture . Leonardite binders were used successfully on three of the four different concentrates tested .

Jan 1, 1964

By R. W. Van Dolah, N. E. Hanna, F. C. Gibson

Measures that were taken to eliminate noise resulting from explosives work at the Bureau of Mines facility at Bruceton , Pa . , are described . A method for monitoring sound transmission characteristics of the atmosphere and control of the explosives testing is presented as a noise control measure that offered partial relief during the period in which the modifications were made . Design details of the replacement gallery , used for permissibility testing of explosives , and the modifications of four types of bombproofs are given . Operation of the closed facilities are completely satisfactory , and the noise problem has been entirely eliminated .

Jan 1, 1964

By Albert J. Rambosek

The objective was to obtain qualitative information on (1 ) the stress field in a core stub at the bottom, or face , of a cored borehole and (2 ) whether , and at what distance , in terms of core diameters from the face of the borehole , relief of stresses in the core is complete . The photoelastic and brittle lacquer techniques of stress analysis were used to determine the pattern of stresses in two- dimensional models , simulating the bottom of a borehole with a projecting stub of core . The core was stress- free at 1-1 /2 core diameters or more from the face of the simulated borehole . The analyses of the isoclinic and isochromatic patterns in the core near the face of the borehole reveal why core occasionally breaks into thin plates , when core or stress - relief drilling is attempted in highly stressed rock masses , such as heavily loaded mine pillars . stub broke away from the bottom in a hydrostatically loaded artificial rock specimen in a manner indicating that core " wafering" can result from tensile stresses developed in the core when a coring bit penetrates the highly stressed rock mass .

Jan 1, 1964