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By W. A. Stickney, J. W. Town

Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .

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 K. E. Tame

An alkaline leaching procedure for recovering uranium from a submarginal 0.1 percent Ug Og calcareous carnotite ore from the Shiprock , N. Mex . , area was investigated . A recovery of 72 percent of the uranium was attained in a preliminary test embodying the commonly accepted practice of ( 1 ) alkaline leaching at 90° C , ( 2 ) multiple stage filtration and washing for recovery of a clear pregnant solution , and ( 3 ) caustic precipitation of uranium as sodium diuranate , with recycle of the barren solution to the leaching and washing circuits . Ion exchange resins were used in a second , less orthodox test that comprised ( 1 ) sodium carbonate leaching of minus 10- mesh ore at 90 ° C to dissolve the uranium , ( 2 ) filtration to recover the leaching reagent for reuse , (3 ) recovery of the uranium- bearing solution in the filter cake as a pregnant slime slurry by repulping of the filter cake followed by a sand- slime separation and countercurrent decantation (CCD ) washing for rejection of the sand fraction , (4 ) recovery of the dissolved uranium from the pregnant slime slurry by resin- in- pulp (RIP ) , ( 5 ) elution of the uranium from the resin with a solution of ammonium chloride acidified with hydrochloric acid , and (6 ) precipitation of the uranium with ammonia gas . About 83 percent of the uranium was extracted from the ore and 95.5 percent of the dissolved uranium recovered by ion exchange . Improved laboratory results were obtained using the RIP process , but larger scale tests would be necessary for economic evaluation of the two processes .

Jan 1, 1964

By C. E. Armantrout, H. Kato, M. I. Copeland, M. Krug

The investigation of the nickel - gadolinium phase diagram was undertaken to determine the alloying behavior of these two metals . The data from meltingpoint determinations , thermal analyses , metallographic examinations , and X- ray diffraction analyses revealed a phase diagram with three eutectic points and seven intermetallic compounds . Very limited solubility of the phases in each other was observed . The five phases , Ni Gd , Ni , Gd , Ni Gd , Ni, Gd , and NiGd¸ , melted incongruently at about 1,300 ° , 1,270 ° , 1,180 ° , 1,070 ° , and 775 ° C , respectively . Ni Gd and NiGd melted congruently at approximately 1,550 ° and 980 ° C , respectively . Four of the compounds were determined to crystallize in the hexagonal system : Ni Gd , Ni Gd , Ni , Gd , and Ni Gd . Ni Gd was determined to be cubic and NiGd , orthorhombic . The crystal system of NiGd was not determined . The eutectic points occurred at 13 , 67 , and 85 wt pct gadolinium , and the isotherms at 1,290 ° , 890 ° , and 700 ° C , respectively .

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 L. G. Trudell, J. W. Smith, K. E. Stanfield

Oil- yield data are presented for 40 sets of core samples and 83 sets of drill cuttings collected in 1952-62 from drilling operations in the Uinta basin of eastern Utah . This accumulated information on the location , extent , and richness of oil shales of the Green River formation is used to appraise the deposits as a source of oil and related products . Core samples used in the study were obtained specifically for evaluating oil shale , and they were satisfactory for this purpose , except they did not completely penetrate the formation . The drill- cutting samples were inferior to the core samples and yielded more erratic results . Consequently, oil yields based on cuttings should be regarded as indicative , rather than definite , until substantiated by other means . In general , the oil- yield data indicate Green River oil shale in Uinta basin is not as thick or as uniform as that in the Piceance Creek basin of western Colorado . However , it is an important potential source of oil . Estimates that beds 15 feet or more thick that average 25 gallons of oil per ton represent at least 120 billion barrels of oil in place are supported by the recent oil- yield data .

Jan 1, 1964

By Paul W. Johnson, Ralph C. Kirby, Frank A. Peters

Alumina can be recovered from clay , using 30 percent nitric acid for digestion . Calcined clay is crushed and then digested at 325 ° F and 85 psig pressure with less than stoichiometric nitric acid required to form normal aluminum nitrate . In this way , a solution containing both normal aluminum nitrate , Al ( NO3 ) 3 , and basic aluminum nitrate , assumed to be Al ( OH ) ( NO3 ) 2 , is formed , and in which iron is virtually insoluble . The solution is filtered and then concentrated in vacuum evaporators to crystallize normal aluminum nonahydrate . The crystals are washed with 50 percent nitric acid and then decomposed to alumina and nitrogen oxides . The design that has been developed for this process is based on published work . For a plant producing 1,000 tons of alumina a day , the estimated operating cost is $60.69 per ton of alumina , and the estimated fixed capital cost is $ 76 million using a Marshall and Stevens chemical equipment index basis of 240.0 . This process is not competitive under current economic conditions with the production of alumina from bauxite via the Bayer process . For lowering costs , future research should include study of leaching at lower temperatures under atmospheric pressure and alternate aluminum nitrate decomposition methods .

Jan 1, 1964

By P. L. Woolf, N. Bernstein, M. M. Fine

Continuous experimentation utilizing a 3- by 36 - foot rotary kiln was conducted to demonstrate the feasibility of simultaneous induration and reduction of magnetic taconite concentrate . Lignite , or lignite - anthracite mixtures , and green magnetite pellets (64.2 percent Fe , dry basis ) were heated in a rotary kiln to about 2,100 ° F. After separation from excess reductant , the product pellets were found to be highly reduced and acceptably hard . A total of 140 tons of prereduced pellets with an average Fe content of 79.0 percent was produced at Minneapolis and smelted in the Bureau's experimental blast furnace at Bruceton , Pa . Two additional supplies of prereduced pellets were obtained from The Steel Company of Canada , Ltd. , Hamilton , Ontario , which contained 83.8 and 91.3 percent Fe , respectively . Smelting of prereduced pellets was compared with that of unreduced pellets obtained from The Hilton Mines , Shawville , Quebec , and from the Erie Mining Co. , Hoyt Lakes , Minn . Blast furnace tests established that a substantial decrease in coke rates and higher production result from the use of prereduced pellets .

Jan 1, 1964

By Bernard Porter, E. A. Brown

Electrical conductivities and densities of the LiF- UF , LiF- ThF4 , NaF - C1F4 , and NaF - ThF systems were measured as functions of composition and temperature . The specific conductance and density varied linearly with temperature . Molar and equivalent volumes , as well as heats of activation for conductance , were calculated from the experimental data . At 1,000 ° C , the molar volumes ranged from 16 to 40 cubic centimeters per mole and the specific conductance ranged from 9.8 to 2.5 per ohm- centimeter as the actinide metal fluoride concentration changed from 0 to 60 mole - percent . Heats of activation for conductance were 3 to 7 kcal per mole . The data are interpreted on the basis of a semilattice model for the melts .

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 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 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 Theodore L. Turner, Joseph H. Swift

A study on a small laboratory scale was made of the use of ammoniacalammonium carbonate for batch leaching Mn from low- grade manganiferous materials ( 6 to 16 pct Mn) obtained from deposits in the southern district of Aroostook County , Maine . These materials were partially reduced at 500 ° to 700 ° C with H₂ or CO and then leached with solutions of NH and CO₂ dissolved in water . Extraction of 80 to 90 pct of the Mn was obtained from some sample materials , but 10 to 34 pct of the iron was also extracted . Material from the Littleton Ridge deposit contained manganese intimately associated with Fe , a condition which contributed to difficulties in obtaining a commercially acceptable product . Extensive investigations of the leach and reduction processes with various mixtures of H₂ and water vapor , and CO and CO₂ , failed to disclose a set of conditions for selectively leaching the manganese . Finely divided metallic Fe was probably produced during the reduction steps so that Fe was leached with the Mn in the subsequent extractions .

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 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 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 A. F. Colombo, D. W. Frommer

Bench- scale tests were made to determine the applicability of flotation as a means of upgrading finished and semifinished magnetic concentrates prepared from reductively roasted iron ores . Both anionic and cationic flotation methods were used to remove siliceous gangue from the magnetic concentrates and produce upgraded products . Seven magnetic concentrates , containing from 6.7 to 13.7 percent SiO2 , were improved by the flotation treatment , yielding final concentrates containing less than 6.0 percent Si02 . Cationic flotation methods were studied on four of the seven samples ; of this group only one sample yielded better results by cationic flotation than by the anionic method .

Jan 1, 1964

By D. A. Elkins

Design plans and detailed cost estimates of mining and treating ore from Maggie Canyon deposit by two alternative methods which can be used in the event of a sudden need to exploit this resource are given . Lower costs are estimated for the operation employing oil - emulsion flotation . The total capital investment required for this operation is estimated at $ 11,750,000 . Assuming an 85 percent recovery in mining , 55.6 pct of the manganese in the ore reserve would report in 153,333 tons of ferromanganese containing 75 pct manganese . The production cost for the 5 - year operation would be about $ 245 per ton of ferromanganese . The total annual operating cost would be approximately $ 7.5 million , distributed , in pct , as follows : Mining 11.9 , milling 24.4 , sintering 9.9 , smelting 47.2 , hauling ore and sinter 2.8 , and general offices 3.8 . Recovery and costs are both higher for the operation employing dithionate leaching . In this operation the required investment is about $ 17,220,000 . Manganese recovery would be 67.6 pct in 186,160 tons of ferromanganese . Production cost would be about $ 284 per ton of ferromanganese . The total annual operating cost would be about $ 10,575,000 , distributed , in pct , as follows : Mining 8.4 , milling 44.4 , sintering 7.4 , smelting 34.7 , hauling ore and sinter 1.3 , and general offices 3.8 . Potential process modifications might reduce the operating cost of the first operation by as much as 7 pct and that of the second operation by as much as 9.5 pct , but exploitation of the deposit by the techniques studied is not economical today .

Jan 1, 1964

By H. E. Powell, T. E. Hill, W. A. Calhoun

The object of this investigation was to determine the effectiveness of certain cationic flotation collectors , Ethomeens , in recovering fine particles of lead minerals from mill tailings at a grade equal , at least , to that of the mill feed ( 1.7 percent lead ) . The Ethomeens , derived from tertiary amines having one fatty alkyl group and two polyoxyethylene groups attached to the nitrogen , were evaluated by bench- scale flotation tests . The 14 Ethomeens tested consisted of four groups : Coco amine , soybean amine , tallow amine , and stearyl amine . The best results were obtained with coco amine C / 12 , soybean amine S/ 15 , tallow amine T / 12 , and stearyl amine 18/20 . From a feed containing 0.23 percent lead , rougher concentrate grades of 2.12 to 3.89 percent lead were obtained , with recoveries of 17.3 to 27.5 percent of the total lead . Some of the lead mineral particles recovered had diameters of less than 1 micron . In comparative tests , the Ethomeens , or polyethoxylated amine types of cationic surface active agents , were more selective than conventional xanthate collectors for flotation of slimed lead minerals .

Jan 1, 1964

By C. H. Schack, K. C. Dean

An investigation was made to devise and evaluate a flexible flotation method for beneficiating typical tactite types of calcareous scheelite - bearing ores ; these scheelite - bearing ores are available in large tonnages in deposits containing 0.2 to 0.3 pct tungsten trioxide . The objective was to achieve a high recovery of the tungsten in concentrates , containing a minimum of 10 pct WO3 , that would be suitable for chemical processing into high- quality synthetic scheelite . The principal problems encountered and resolved by bench- scale flotation tests on ore samples from five different deposits were to define the conditions and reagent combinations essential for ( 1 ) achieving selective flotation of a small amount of scheelite from a large amount of calcite and ( 2 ) controlling the effect of small amounts of calcium , magnesium , and iron salts in the ores and water used . The flotation process was evolved from batch tests and continuous runs in a pilot - scale mill with a capacity of 100 lb per hour . The flotation process comprised ( 1 ) removal of sulfide minerals , ( 2 ) conditioning the residual ore pulp with sodium carbonate , quebracho , and trisodium phosphate , and ( 3 ) rougher flotation and single - stage cleaning of a scheelite concentrate . In a pilot plant run , over 91 pct of the tungsten was recovered from ore containing 0.27 pct WO3 , in a concentrate containing 11.2 pct WO3 .

Jan 1, 1964