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By G. V. Sullivan, G. F. Workentine

Beneficiation studies were conducted by the Bureau of Mines on three samples of low- grade chromite - bearing material from the Stillwater complex of Montana . The objective of the study was to develop methods for recovering chromite from low- grade materials to improve the domestic reserve situation . Samples were obtained from the three largest deposits in the district , Mouat , Benbow , and Gish . The chromic oxide ( Cr₂ 0 ) content of the ore and of the chromite was about the same in each of the samples . The major gangue constituents ranged from clean olivine in the Mouat sample to such altered minerals as serpentine and talc in the Benbow and Gish samples . Tabling , flotation , high- tension electrostatic separation , and combinations of processes were applied to each ore . Treatment of the Mouat sample ( 9.95 percent Cr₂ 0 ) by high- tension electrostatic separation , a combination of tabling and high- tension electrostatic separation , and tabling with middling retreatment resulted in concentrates that graded 42.8 , 42.0 , and 40.7 percent Cr₂03 at chromium recoveries of 85 , 86 , and 84 percent , respectively . Other techniques were less selective . 2 The Benbow sample ( 7.75 percent Cr₂0 ) responded most selectively to tabling with middling retreatment and a combination of tabling and hightension electrostatic separation to produce concentrates of 40.1 and 39.5 percent Cr₂g with each process having a chromium 2 recovery of 69 percent . Response of the Gish sample ( 8.04 percent Cr₂03 ) to the various concentration techniques was about the same as that of the Benbow sample , but in general , somewhat less selective . A combination of tabling and high- tension electrostatic separation resulted in a concentrate that contained 71 percent The Mouat mine was reopened in 1953 when the American Chrome Co. contracted with the Federal Government to produce 900,000 tons of chromite concentrate . The ore , averaging 20.2 percent Cr₂03 , was treated by tabling to produce a 38.5 - percent Cr₂ O concentrate.

Jan 1, 1964

By J. J. Pfeiffer, J. W. Myers, A. A. Orning

A study was made of the feasibility of using washery refuse in the manufacture of lightweight aggregate for building materials . Preliminary caking and burning tests showed that the refuse could be converted into lightweight aggregate but that refuse passing a No. 14 U.S. Standard screen could not be used without additional processing . The aggregate was prepared by pelletizing the refuse and burning out the carbonaceous material on a chain- grate in a refractory - lined furnace . A small stationary - grate furnace was used to study the process variables involved and establish optimum ignition and combustion conditions . Maximum ignition rates were obtained at air rates of approximately 200 lb per sq ft hr , but air rates of 450 or higher were required in the burnout period to obtain temperatures high enough to sinter the ash . The data obtained from this unit were used as a guide in the operation of the chain- grate furnace . In the chain - grate furnace , satisfactory results were obtained by using primary air rates of 200 lb per sq ft hr in the ignition zone and 500 lb per sq ft hr in the burnout zone . The ignition- zone air was preheated to 500 ° F , but the air for burnout was not preheated . A total of 2-1/2 tons of aggregate was prepared in this unit and made into experimental block . A commercial development based upon the results of this study yielded a product which met the ASTM specifications C 130-42 for lightweight aggregate , and blocks made from the aggregate were of good color , durable , and light - inweight .

Jan 1, 1964

By E. G. Davis, H. P. LeVan, L. S. Smith

Leaching of a Georgia umber ore when using both ferrous sulfate and pickle liquor was studied in the laboratory . The ferrous sulfate content of the leach solution was the major factor affecting the extraction of manganese from the ore . Time , temperature , and the sulfuric acid content of the leach solutions had relatively little effect on leaching of manganese from the ore ; however , these factors did affect the amount of iron extracted from the umber and/or precipitated from solution . Simulated countercurrent leaching of the ore with pickle liquor containing 130 gpl (grams per liter ) ferrous sulfate ( 48 gpl ferrous iron ) produced a pregnant solution having 16 gpl manganese and 41 gpl iron . Filtration tests of the leach slurries indicated that separating the leach solution and solids by vacuum filtration was impractical , whereas pressure filtration was feasible when the cake thickness was limited to about three- fourths of an inch . Fired pellets of the filter cake yielded a firm , hard product analyzing 56 percent iron and less than 0.1 percent sulfur .

Jan 1, 1964

By David Schlain, C. B. Kenahan, F. X. McCawley

The electrodeposition of protective coatings of tungsten from a sodium and lithium borate - tungstate - tungstic oxide fused salt electrolyte was investigated . Soluble tungsten anodes were employed . Deposits were made on molybdenum , Carpenter 20 stainless steel , Inconel , and nickel . An atmosphere of argon was maintained around the electrolytic cell , and the electrolyte was stirred by rotating the cathode . Thick deposits of tungsten (up to 26 mils ) were made at a temperature of 900 ° C and cathode current densities of 0.3 to 0.4 ampere per square inch with high current efficiencies . The effects of variations in temperature , current density , electrolyte agitation , and tungstic oxide content of the electrolyte and of the presence of impurities such as moisture , air , iron , and nickel were investigated .

Jan 1, 1964

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 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 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 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 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 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 James S. Browning, W. H. Eddy

Laboratory batch and small - scale continuous flotation tests were conducted on a ferruginous barite - fluorspar ore from near Sweetwater , Tenn . , to determine the feasibility of producing commercial - grade fluorspar and barite concentrates . The lignin sulfonate - sodium fluoride - fatty acid method of floating fluorspar produced acid - grade concentrates . Flotation of the barite from the fluorspar tailing using petroleum sulfonate yielded concentrates suitable for use as a weighting agent in oil -well drilling muds . The continuous flotation tests , treating about 150 pounds of ore per hour , yielded fluorspar concentrates that assayed 98.3 percent CaF2 and barite concentrates that assayed 91.2 percent BaSO4 . The recovery of the two minerals was 91.2 and 85.2 percent , respectively .

Jan 1, 1964

By Richard F. Hewlett

This Bureau of Mines report presents the computer programing methods and mathematics required to generate either random numbers or normal random numbers to be used for the construction of statistical probability models for simulating mineral deposits by Monte Carlo techniques . Theoretical frequency functions are evaluated as an illustration of simulation applications . Numerical and analytical methods of simulating and dissecting some complex frequency distributions are described .

Jan 1, 1964

By F. R. Cattoir, R. E. Cumings

Columbium metal was electrorefined in a fused - salt electrolyte . Excellent results were obtained in lowering the impurity content in a 94 - percent columbium anode feed material to produce a 99.8- percent - pure metal . The reductions of the major impurities follow : Oxygen from 19,800 to 500 ppm , carbon from 9,700 to 25 ppm , iron from 9,200 to 630 ppm , nitrogen from 2,100 to 90 ppm , and silicon from 750 ppm to not detected . Columbium with a purity of 99.9 percent was produced from 99.5- and 99.8 - percent grades of columbium. The investigation was devoted to the evaluation of a fused - fluoride - salt electrolyte ( KF - NaF- K₂ CbF, ) for electrorefining columbium. The effects of the columbium concentration and the voltage upon the product's purity were investigated . The effect on the cathode current efficiency of ampere - hours of deposition and the formation of a dual valence state of the columbium was also investigated .

Jan 1, 1964

By F. R. Cattoir, T. A. Sullivan

Commercial uranium metal was electrore fined to a high- purity product using molten- salt electrolytes in an inert atmosphere cell . Electrorefined uranium that contained , after consolidation , less than 30 ppm of metallic impurities was prepared . A method of leaching the electrolyte crystals to remove the salts was developed . Cathode current efficiencies from 90 to 100 percent were obtained . Two molten- salt electrolytes were prepared and evaluated : (1 ) lithium chloride - potassium chloride - uranium trichloride and ( 2 ) sodium chloridepotassium chloride - uranium trichloride . Very little difference was found in the purity of the uranium metal produced in either system . The lithium chloride - potassium chloride - uranium tri - chloride electrolyte was preferable from an operational standpoint .

Jan 1, 1964