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By D. E. Emerson, C. G. Kirkland, E. M. Frost

An apparatus has been developed for determining the helium content of gases containing 40 percent or more helium . It utilizes activated coconut charcoal at liquid nitrogen temperatures to adsorb constituents other than helium in the mixture . Series of analyses have been run where the mean deviation was less than 0.05 percent helium . Twenty or more analyses can be made in an 8- hour day .

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

By Richard W. Lewis, Lloyd Carpenter

The objective of the investigation was to determine spectrochemically 19 elements in the general range of 0.5 to 1,000 ppm in high - purity hafnium and its compounds . Samples were converted thermally to hafnium dioxide , mixed with buffer - carrier - internal standards , and excited by a dc arc . Spectra were recorded on photographic plates . Transmittance values were recorded densitometrically and converted to relative - intensity ratios . Four groups of standards were used to establish analytical curves from which the concentrations of impurities were obtained . Average precision of the method was 14.2 percent relative standard deviation , and relative error was 4.2 percent .

Jan 1, 1964

By R. T. DeWoody, J. W. Chester, W. C. Miller

The work was done to develop a relatively efficient muffler for quieting the exhaust of a rock drill . The exhaust of a pneumatic rock drill is the source of the major part of the noise generated by the drill . The exhaust noise can be reduced in a number of different ways , but this study involved only reactive mufflers . The reactive muffler can be simulated by an electrical circuit . Information obtained from analogous electrical circuits was used to design an efficient exhaust muffler for pneumatic rock drills . Electrical analogies proved to be a valuable tool in the design of mufflers .

Jan 1, 1964

By L. C. George, J. W. Jensen

A new system for precisely counterbalancing and measuring vapor pressure operates by servomechanical principles . It was developed with the objective of determining the vapor - pressure equations of metal halides . The system is isolated from the vapor - pressure bulb by a diaphragm transducer that signals a pressure regulator to null any pressure difference that is detected . Pressure measurement and readout are continuously performed by a servomanometer , accurate to ±0.003 cm Hg for the range of 0.1 to 200 cm Hg . High response rate and sensitivity are obtained . Methods of use are described , and results for CdC1 and PbC1 , in agreement with data of other investigators , are given as examples .

Jan 1, 1964

By R. B. Stroud

This report, part 3 of a series, describes and gives results of field. investigations by the Bureau of Mines on manganese resources of the Batesville district, Arkansas, from July 1956 through June 1961. The purpose of the Bureau's work was to evaluate the manganese potential of the district in fur- therance of the Government's program with respect to domestic resources of critical and strategic minerals. The work comprised areal reconnaissance, mapping, churn and core drilling, and sampling. In more recent years, the investigations were confined to manganiferous limestone, which constitutes a significant potential resource of manganiferous material. The resources of manganiferous material in the district are inferred to be on the order of 198 million long dry tons averaging between 4 and 5 percent manganese.

Jan 1, 1964