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By Ralph Husack, J. W. Eckerd, G. A. Brady

The effect of gamma radiation on Pennsylvania anthracite and on reactions between anthracite and other materials was studied using a shielded , selfcontained 23,000 - curie cobalt 60 source . When anthracite was exposed to air at 65° C the reaction with oxygen was greater in the presence of radiation. than in its absence . Although drop- shatter tests indicated that exposure to radiation decreased the resistance to breakage of anthracite , this evidence of structural weakening was not supported by the results of grindability or particle- size studies . Irradiation caused definite changes in the gases evolved from evacuated samples of anthracite ; the percentages of hydrogen and carbon dioxide were increased, and the methane concentration remained unchanged . Carbon monoxide was evolved only from the unirradiated samples . Electron paramagnetic resonance (EPR ) measurements indicated large differences between evacuated samples and those exposed to air . There was little or no difference between irradiated and unirradiated samples , except that the free- radical content of unirradiated samples of anthracite increased progressively with higher temperatures of evacuation , but in the case of irradiated samples , no such behavior was found . Attempts to produce carbon disulfide and calcium carbide by reacting anthracite with sulfur up to 120 ° C , and with calcium oxide up to 400 ° C , were unsuccessful .

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 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 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 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 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 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

By R. R. Allen

Gieseler plastometer tests were performed on eight western coking coals at retort - immersion depths ranging from 2 to 3-3 /4 inches (measured to the center of the coal charge ) . Increased maximum fluidities were associated with greater retort - immersion depths , the most pronounced increases being observed on highly swelling coals when tested at 3-3 /4 inches . The maximum fluidity of one of these coals when tested at 3-3 /4 inches was 146 percent greater than that observed at 24 inches . Retort - immersion depth had no significant effect on the temperatures of initial softening , fusion , maximum fluidity , end of fusion , and solidification .

Jan 1, 1964

By Paul E. Bennett, James S. Browning, Thomas L. McVay

Continuous 1.0- to 1.5 - ton - per - hour pilot plant flotation tests were made to determine the technical and economic feasibility of recovering beryl from flotation tailing being produced at the spodumene concentrator of the Foote Mineral Company , Kings Mountain , N.C. Best results were obtained when using an acid circuit and amine - type cationic reagents to float a bulk beryl - feldspar concentrate and then selectively floating the beryl away from the feldspar , using a petroleum sulfonate collector . About 77 percent of the beryllium in the pilot plant feed was recovered in a concentrate containing 6.42 percent BeO . The capital cost of an integrated flotation plant capable of treating 500 dry tons of spodumene mill tailing per day for recovery of beryl and feldspar is estimated at $ 210,000 . Indicated direct operating costs for the plant were $ 1.52 per ton of dry spodumene flotation tailing treated . This approximated the value of beryl recovered , but potential profits of about the same magnitude lie in concurrent recovery of marketable spodumene and feldspar byproducts .

Jan 1, 1964

By R. W. Hiteshue, R. W. Fridy, W. Kawa

A study of the production of coronene , a high - melting ( 440 ° C ) , highboiling ( 525 ° C) , polynuclear hydrocarbon , was made by the Bureau of Mines to determine the maximum yield obtainable by the hydrogenation of coal and coalderived materials . Experiments were made with anthracite and bituminous coals and with asphaltenes and centrifuged residue obtained from heavy oil produced in a pilot plant by the hydrogenation of a bituminous coal at 2,000 psi and 480 ° C. With anthracite , yields of coronene of 0.5 to 0.7 wt pct of moistureand ash - free coal were obtained at 6,000 to 8,000 psi , 700 ° to 750 ° C , and a residence time of 30 minutes . With bituminous coal , yields averaging 0.4 wt pct of maf coal were obtained at 6,000 psi , 800 ° C , and 30 minutes ' residence time . With asphaltene and centrifuged residue , yields of less than 0.02 wt pct of maf coal were obtained at 6,000 psi , 700 ° C , and 60 minutes ' residence time .

Jan 1, 1964

By J. H. Holden, G. R. Strimbeck, L. F. Willmott, W. R. Huff

A pilot - scale fluidized feeder was developed for continuously feeding up to 1 ton of pulverized coal per hour to a pressure gasifier . Fluidization in the 3 - foot - diameter by 34-1 / 2 - foot - high feeder is effected by two streams of inert gas , a technique called zone fluidization . A stream of inert gas through a drilled plate in the base of a central column near the bottom of the feeder fluidizes the coal . Another stream through a drilled plate in the annulus between the central column and feeder wall provides a source of semifluidized coal for the central column . Fluidized coal from the central column discharges through an extraction funnel and discharge line . Zone fluidization provided good fluidization with moderate requirement for fluidizing gas . Instruments were developed for metering and recording the flow rate of fluidized coal . A system was developed for storing , and weighing pulverized coal , and then delivering it in fluidized form at about 1 to 8 tons per hour .

Jan 1, 1964

By J. A. Ruppert, P. M. Sullivan

A study was made of filtration techniques for recovering the major part of the tin contained in iron - tin alloys known as hardhead . Special smallscale filtering apparatus and a three - stage cyclic process were developed . Eighty- seven percent of the tin contained in an alloy of 82 percent tin and 17 percent iron was recovered as pure metal by pressing at 975° C followed by a second pressing at 800 ° C and a final filtering at 250 ° C. Small amounts of Sb , Cu , and Fe impurities were removed by adding Al to the molten product and performing another filtration at 250 ° C.

Jan 1, 1964

By Robert L. Rough, William E. Eckard

Laboratory data obtained from a Bureau of Mines rotary air core of a well near Sugar Grove , Warren County , Pa . , were instrumental in initiating hydraulic fracturing in the area to stimulate oil recovery from Glade sand oil reservoirs . This report outlines the general geology , lease development , reservoir- rock characteristics , and oil - production history of Glade and Clarendon sand reservoirs in Warren County . The methods of well completion for single- stage and multiple- stage hydraulic fracturing of old and new wells are discussed , and a range of hydraulic fracture treatment data from 29 Glade sand and 10 Clarendon sand wells is presented . A composite decline curve representing oil - production data from six wells shows probable results of hydraulic fracturing . Average cumulative oil production during the first 100 days after hydraulic fracturing with a sand - carrying liquid is compared with production after conventional shooting with liquid nitroglycerin .

Jan 1, 1964

By R. W. Hiteshue, C. O. Hawk, H. H. Ginsberg, M. D. Schlesinger

The Bureau of Mines studied single - step catalytic vapor - phase hydrogenation of oils derived from coal and oil shale . Treatment of middle oil , from hydrogenation of bituminous coal , gave good yields of gasoline with a German - made molybdenum- zinc - chromium catalyst . The Bureau also achieved good results with duplicates of this catalyst made from domestic raw materials . In one set of experiments with the German catalyst , 38 to 52 wt pct of feed was converted to gasoline . The total liquid product was 91 to 98 wt pct of the feed . Not all this gasoline can be claimed as production , however , because about 20 pct of the feed was in the gasoline range , and part of it undoubtedly survived the hydrocracking treatment . Hydrogenation of crude shale oil in the presence of cobalt molybdate catalyst produced a total liquid product of 89 wt pct of feed . The hydrogenation converted 27 wt pct of feed to gasoline and 44 wt pct of feed to diesel fuel . The remaining liquid product , 18 wt pct of feed , was residue boiling above diesel fuel . The gasoline was of poor quality , with an octane number of 39.1 . The overall product seemed a suitable feed stock for a conventional refining operation . Coker distillate hydrogenation , using a cobalt molybdate catalyst , gave a total liquid product of 97 vol pct of feed ; of this product 60 vol pct was jet fuel and 40 vol pct was diesel fuel . High nitrogen and sulfur in all three of these raw materials severely poison the usual refining catalysts . Thus , the common objective in these

Jan 1, 1964

By G. W. Birge, D. E. Wolfson, J. G. Walters

Seventeen samples were carbonized by the BM -AGA pilot - plant test method and in industrial ovens . Chemical and physical properties of the samples were determined , and the physical properties of the cokes prepared by the two methods were compared . Since the capacity of the plants from which these samples were obtained is about 30 percent of the 1959 total for the United States , the data given in this report are indicative of the chemical and physical properties of blends used to produce industrial cokes and the acceptable chemical and physical properties of the resultant coke .

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 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 Charles H. Atkinson, Robert T. Johansen

Tremendous volumes of petroleum ( crude oil and natural gas ) at present cannot be recovered economically . The feasibility of using nuclear explosions for production stimulation therefore has been investigated . Data from underground nuclear tests conducted by the Atomic Energy Commission were reviewed , and the physical effects were evaluated for stimulating petroleum production . Calculations of the effect on ultimate recovery of increasing reservoir temperature with nuclear explosives showed disappointingly small increases . Production increases caused by fracturing of massive low- permeability reservoirs appear technically and economically promising . Petroleum reservoirs that might be converted from submarginal to commercial production are being located and evaluated as to potential reserves and as a location for a field test .

Jan 1, 1964