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By F. E. Block, T. T. Campbell, D. Z. Hobbs

Several methods were investigated for the preparation of high- purity elemental boron in an attempt to develop a feasible process for producing boron on a large scale . In the work described in this report , the metal was prepared by metering boron trichloride gas into a crucible containing molten metal reductants . It was necessary to remove reaction byproducts by acid and aqueous leaching . Magnesium and sodium were tested as reductants , but best results were achieved using lithium or zinc as reductants . Contaminants originating from the materials of construction were the chief impurities in boron made by this method . Impurities ranged from 0.5 to 5.0 percent . Impure boron ( 85 to 90 percent ) was also prepared by the magnesium reduction of boron trioxide in a thermite - type reaction . This product contained magnesium as the chief contaminant . Impure boron made in this way could be upgraded by fusing with potassium fluoborate or potassium acid fluoride . After acid leaching the fusion cake , a product containing 95 to 97 percent boron was obtained . Analytical techniques for accurate determination of impurities in elemental boron are a major problem , requiring solution before a valid comparison can be made of the quality of boron prepared by these various methods .

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 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 James A. Wasson, Harry R. Johnson, Dean W. Boley

The Cow Run sand was cored and electrical and radioactivity surveys were made in C. E. Vandevender well 35 in the Burning Springs pool of the Burning Springs oilfield , Wirt County , W. Va . Laboratory tests , reservoir - fluid analysis , well - log interpretation , and available field data indicate that a substantial quantity of oil may be recovered from this pressure - depleted reservoir by waterflooding . Two formations erroneously believed to be the First and Second Cow Run sands were similarly evaluated in A. E. Mackintosh well 8 , Anns Run Pool , Wirt County , W. Va . , but were found unsuitable for secondary - recovery operations .

Jan 1, 1964

By F. E. Walker, S. J. Aresco, J. B. Janus

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal , expressed in British thermal units , and the composition as shown by proximate analyses . To these , when required , are added the ash- softening temperature , the free- swelling index , and the Hardgrove grindability index . Under most of these specification contracts the bidders guarantee the quality of the coal , and that guaranteed by the successful bidder becomes the standard of his contract . The deliveries are sampled in accordance with instructions 4/ issued by the Bureau of Mines ; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and , if it is not , a price adjustment is made . Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks ) provide valuable data for use in evaluating future bids . In addition , the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal . The Government purchased approximately 5 million tons of coal in fiscal year 1963 . In connection with these purchases , the Bureau analyzed 6,999 samples . These are published ( table 1 ) for the use of Government officials and the public . A series of publications has been completed on coal analyses by States or , where production is small in any one State , by groups of adjacent States . In addition to analytical data showing composition and quality of coals of the States , the publications contain brief descriptions

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 Albert W. Deurbrouck

This report describes the preparation characteristics of the Pittsburgh and Upper Freeport coalbeds in Hancock , Brooke , Ohio , and Marshall Counties , W. Va . Over 4.5 million tons of coal was produced in these four counties in 1962. Most of this production came from the Pittsburgh coalbed . Twelve coal samples were collected for this study , 11 from the Pittsburgh bed and 1 from the Lower Freeport bed . Two of these samples could be upgraded to produce metallurgical - grade coal . The sulfur content of the Pittsburgh- bed coals was generally excessive --as high as 4.9 percent in the raw coal and 3.19 percent in the float 1.30 specific gravity fraction . The rank of the coals in this area ranges from high-volatile A to high-volatile B bituminous .

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 H. R. Shell, Robert C. Johnson, Wilbur H. Warwick

Alpha silicon nitride fibers , Si3N4 , were successfully grown in graphite crucibles by a new method utilizing silicates and silicon ( S in equations below) as sources of silicon and using carbon , aluminum , and silicon as reducing agents (R in equations below ) . The basic reaction mechanism is believed to be generally as follows : 1,300 - 1,500 ° C S + R + N₂ SiO + RO + N₂ › 3Si0 + R + 2N₂ _1,300 - 1,500° C 3RO + Si¸N • ( 1 ) ( 2 ) A build - up of coatings on the solid raw- material particles hindered the evolution of silicon or silicon monoxide vapor and thereby slowed down further formation of silicon nitride fibers . Free oxygen in the crucible caused the formation of amorphous silicon dioxide ( SiO2 ) fibers . This problem was solved by passing , entering , and exiting gases through layers of lump graphite inside the reaction vessel . The silicon nitride fibers grew best around 1,400 ° C. Nitrogen flow rates from 4 to 6 liters per minute were adequate . The fiber widths were generally only a few microns whereas their lengths sometimes reached one - quarter inch or more . Chemical and X- ray analyses indicated that bulk fiber samples were usually 80 to 90 percent Si3N4 . The fibers had good oxidation resistance to about 1,260 ° C. Thermal shock resistance was excellent . Electrical resistance was determined .

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 D. W. Bridges, R. O. Dannenberg, Laird Crocker

Preliminary solvent extraction studies , reported by the Bureau of Mines (5) , have been continued and expanded to improve on the previous estimate of process requirements . The solvent extraction portion of the process was examined at a scale large enough to enable meaningful extrapolation of the results to geometrically similar equipment of plant size . About 82 pct of the beryllium was recovered from approximately 0.5 pct beryllium oxide (Be0) Spor Mountain , Utah , ore by a process involving ( 1 ) sulfuric acid leaching , ( 2 ) counter current decantation (CCD ) washing , (3 ) iron ( III) reduction by sodium hydrosulfide ( NaHS ) , ( 4 ) beryllium solvent extraction by di - 2- ethylhexyl phosphoric acid ( EHPA) , ( 5 ) caustic stripping of beryllium- bearing EHPA, (6 ) hydrolysis of sodium beryllate - caustic strip liquor , and (7 ) calcination of beryllium hydroxide (Be ( OH ) 2 ) formed in step (6 ) . The resulting beryllia assayed 98 to 99 pct Be0 and was suitable for most nonnuclear uses . Best overall results were obtained by using pH 2 , 1.6 grams of BeO per liter of leach liquor as feed and 0.25 N EHPA in kerosine containing 2 wt vol pct (grams per 100 ml of solution ) isodecanol ( IDA ) as solvent . Analysis of the data indicated that a commercial plant would achieve 95- pct overall extraction operating at 45 ° C with 20 hp per 1,000 gal of dispersion in each of seven mixer- settlers , having 290 gal per ton of ore hourly mixer capacity and 90 gal per ton of ore hourly settler capacity . At least 79 lb H2SO4 , 13 lb sodium hydroxide (NaOH ) , 3 lb NaHS , 0.25 lb kerosine , 0.07 lb polyacrylic flocculant , 0.03 lb EHPA , and 0.007 lb IDA would be required in H2SO4 leaching and subsequent processing to recover 1 lb BeO .

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 A. Gene Collins, Cynthia A. Pearson, Cathy J. Waters

The chemistry of selenium and tellurium is discussed , along with a method of preparing a synthetic oilfield brine , an oilfield brine sampling method , and methods for determining selenium and tellurium in complex oilfield brines . Selenium either can be reduced to the elemental form with sulfur dioxide and determined semiquantitatively by color comparison of the red amorphous form or can be converted to selenite and determined quantitatively by reacting it with 3,3 ' - diaminobenzidine and obtaining its spectral absorbance at 420 mu . Tellurium can be reduced to the elemental form with hypophosphorous acid , and the spectral absorbance of its red hydrosol can be measured at 400 mu . Less than 0.05 mg / 1 of selenium and 0.1 mg / 1 of tellurium can be determined by the described methods .

Jan 1, 1964

By R. H. Harrison, D. R. Douslin

The thermodynamic properties H - H° , (H - H° ) /T , S - Sideal , S - S° Fide al F - F° , (F F° ) /T , and activity coefficient Y for perfluorocyclobutane were calculated as functions of temperatures ( 115.22 ° to 350 ° C) and molal density (0.75 to 6.5 moles / liter ) . Improved analytical and graphical correlating techniques are described .

Jan 1, 1964

By William R. Wayment, David E. Nicholson

The Bureau of Mines studied some physical properties of hydraulic backfills and their paramount characteristics , and made preliminary attempts to compact this type of material . The in- place density of hydraulic backfills affects the properties of strength , consolidation , and water percolation . Dense fills give better support than loose fills . In - place density properties themselves are affected by grain size , grain size distribution , and the particular conditions of sedimentation in a stope ( the amount of work the slurry water does to compact the material ) . Field sampling of in - place densities of fills presently used in four different mines and laboratory and underground compaction tests using a standard concrete vibrator show that the initial in - place density of the cohesionless fill material tested can be significantly increased by vibratory compaction .

Jan 1, 1964

By Henry M. Harris, Hal J. Kelly

Electrical dewatering tests are described in which the laboratory cells were designed for continuous operation using an endless metal belt as the anode . The test slurries were dilute , containing from 2.5 to 14.4 percent solids (specific gravity of 1.02 to 1.10 ) that were all minus 8 microns in size . Recovery of the solids of low water content was the practical objective of the investigation . Process variables evaluated and reported are : The effect of feed rate , amount of electrolyte , samples from different sources , and the use of two cells in series . These variables are evaluated on the basis of yield of clay per kilowatt - hour , recovery , and the amount of solids in the deposited clay . Recovery , yield , and solid content of the belt anode product are interdependent , and changes that will improve one of these characteristics often are accomplished at the expense of the others . Tests in which recoveries range from 50 to 60 percent usually result in yields of 8 to 9 kilograms (kg ) of dry clay per kilowatt- hour (kwhr ) . Under these conditions , the solid content of the deposited clay approximates 50 percent . One test sample , composed of kaolinite , showed very high yield , 13 to 16 kg per kwhr ; high recovery , 53 to 58 percent ; and 52 to 54 percent solids in the cake .

Jan 1, 1964

By E. Morrice, R. D. Smith

Thermal expansion and electrical resistance measurements were made on cerium metal from 4° to 300° K. The apparatus developed , including a specimen holder and a cryostat system , are described along with the experimental techniques used in obtaining the measurements . The total linear thermal expansion Data at of 99.83 weight - percent cerium metal between 4 ° K and room temperature was 4.24 percent . The resistivity at 4° K was 7.0 x 10-6 ohm- centimeter . 4° K indicate a fundamental relationship between residual resistivity and purity of cerium metal . The effects of annealing and repeated thermal cycling on resistivity were determined .

Jan 1, 1964

By V. E. Edlund

This report presents the results obtained in a study of the technical feasibility of recovering a usable pig iron by pyrometallurgical treatment of typical copper reverberatory slags . The iron in the slag was readily reduced with carbon , but the copper and sulfur content of the metal was best controlled by a three - stage procedure comprising ( 1 ) melting the slag with pyrite to remove copper as a low- grade matte , ( 2 ) smelting the partly decopperized slag with fluxes and carbon to reduce the iron , and ( 3 ) refining the impure iron alloy from step 2 with a flush slag to remove sulfur and residual copper . Laboratory - scale tests demonstrated that washing with 8 wt pct of pyrite lowered the copper content of a typical reverberatory slag from 0.58 to 0.12 Subsequent smelting of a mixture composed of 70 pct decopperized slag , 25 pct lime , and 5 pct coke reduced 84 pct of the iron to metal containing 2.27 pct sulfur . This metal then was successfully desulfurized by treatment with a basic flush slag to produce a finished metal that contained , in percent , 93.5 Fe , 0.02 S , 0.26 Cu , and 4.9 C. Overall recovery of iron under the conditions of trial was about 80 pct . This could be increased if higher tolerances for copper could be accepted . Commercial processing would be accomplished in three furnaces with molten materials passing from one to another . Currently produced smelter slag could be treated fairly inexpensively , because the molten product would require only a little additional heat to produce an iron byproduct that undoubtedly would be attractive to local foundries .

Jan 1, 1964

By J. R. Hauger, P. A. Romans, W. J. Niebuhr

With suitable instrumentation and techniques it is possible to determine the presence of tantalum in columbium to 20 ppm . This paper discusses the selection of X- ray spectrographic instrumentation and describes a technique for accomplishing the low level determination of tantalum . An ion- exchange method of separating tantalum from columbium is also described .

Jan 1, 1964

By A. L. Service, C. C. Popoff

Phosphate deposits in Montana , Idaho , Wyoming , and Utah are important factors in the mineral , agricultural , and industrial economy in the western part of the Nation . This report presents background information , including geology , mining , beneficiation , processing , resources , and economics , assembled to provide a comprehensive introduction to a series of four area reports . About 20 percent of the Nation's phosphate is produced from the Western field where there were 6 surface and 9 underground mines in operation in 1963 . This region also has an estimated 58 percent of the Nation's phosphate reserves , and continuing development is assured by these abundant resources and an increasing demand for phosphate products . Long range forecasts indicate that the United States will continue to use increasing amounts of both agricultural and industrial phosphate products . Beneficiation has become an important part of the phosphate processing industry , and two flotation plants and several washing plants were in operation in 1963. Recent studies by the Bureau of Mines Metallurgy Research Center , Albany , Oreg . , have been directed toward developing flotation processes applicable to treatment of marginal phosphate rock . Other Bureau of Mines research is being directed toward improved methods of ore recovery , ground control , and mining .

Jan 1, 1964