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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 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 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 G. H. Cobb, J. L. Johnson, H. H. Heady

An infrared absorbance technique is described for analyzing anodic gases produced during the electrowinning of uranium , thorium , and rare - earth metals in molten fluorides . Typical components determined qualitatively in a gas sample are CO , CO₂ , CF4 , C₂ Fe , C3F8 , COS , CS₂ , and SiF4 . About 20 minutes are required to record and interpret the spectrogram , and report quantitative results for CO, CO₂ , CF4 , and SiF . The procedure is used for control during electrolysis .

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

An investigation was conducted to determine the relationship between ASTM and Micum tumbler data and to develop equations that would enable the conversion of data from one test method for comparison with those determined by the other , and thereby facilitate the international exchange of data . Relative strengths of 18 commercially produced cokes were determined by ASTM and Micum tumblers and ASTM shatter test . Two of the samples were coke produced for foundry use , and two were produced in beehive ovens . The remaining 14 samples were produced for blast furnace consumption and had ASTM tumbler stabilities of 36 to 58. Statistical procedures were used to relate the three test methods and also to evaluate the effect of charge weights , top sizes of coke , and types of screens specified by the two standard tumbler procedures , square - hole wire mesh for the ASTM tumbler and punched round - hole for the Micum . A significant result was that the data obtained with like screens have a higher degree of correlation with a smaller standard deviation than data from the screens specified for each tumbler .

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

By R. D. Groves

Laboratory research has demonstrated that high - grade copper powders can be produced under controlled conditions from cement copper products . The technique should enable small producers to prepare a directly marketable product by means other than smelting and electrolytic purification . A continuous drum- type precipitator was the preferred unit for producing fine - sized particles of cement copper that were further processed by chemical digestion in a copper sulfate solution , by reduction and sintering in a hydrogen atmosphere , and by grinding to a powder . The effects of variables related to all stages of the process were investigated . Treatment of leach solutions from three different sources resulted in copper powders containing 99.2 to 99.8 pct Cu , apparent densities of 1.97 to 2.25 grams per cu cm , good powder flow rates , and a size distribution of 54.9 to 60.1 pct minus 325 - mesh material .

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 M. M. Wong, J. E. Klosterman

Scrap beryllium chips ( nominally 96 to 97 percent Be ) were electrore fined in a prototype cell with 408 lb of electrolyte composed of 52.4 mole - percent LiCl , 36.3 mole - percent KC1 , and 11.3 mole - percent BeCl2 . The cell temperature was 500 ° C. In a typical 10-3 /4 - hour deposition cycle , 0.415 pound of metal was produced ; the metal contained impurities in parts per million as follows : C , 700 ; 0 , 610 ; Al , 34 ; Ca , 32 ; Cu , 20 ; Fe , 25 ; Mg , 9 ; and Mn , 23 . Operation of the prototype cell for 2 years demonstrated that adapting the electrorefining process to an enlarged scale of operation presented few difficulties in mechanical functions , maintenance of optimum operating conditions , and control of product purity . After the spent anode feed was leached in a 5 - percent nitric acid solution and the fine - sized particles were removed , it was recycled in some tests . The metal produced was somewhat higher in impurities than metal from the fresh scrap chips .

Jan 1, 1964

By Leonard Obert

A triaxial procedure is described for measuring the modulus of elasticity and Possion's ratio of stress relief cores , that is , the concentric hole cores obtained by the overcoring technique . The elastic constant determinations can be made at stress levels comparable with those encountered in underground mining . The results from tests on an aluminum alloy calibration specimen and four rock specimens are included .

Jan 1, 1964