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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 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 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 Harold M. Smith

The data in this report were prepared to show how Bureau of Mines routine crude oil analyses could be used to evaluate crude oils in terms of common commercial products . The use of Bureau of Mines routine analyses to determine hydrocarbon - type relationships for the gasoline and gas - oil fractions is demonstrated . For this purpose the correlation index , the aromatic profile and the naphthene profile are used to establish reasonably acceptable values for hydrocarbontype relationships . The derivation and meaning of these indications are discussed . These analytical interpretations are applied to a group of high - sulfur crude oils from the Near East , the Permian basin of West Texas , Venezuela , Colombia , California , and other locations , and the resultant data for gasoline , gas oils , lubricating oils , and asphalt are compared by appropriate tables and graphs . Because the Near East crude oils contain higher quantities of paraffins in the gasoline and gas oil ranges , they will yield good , lowsolvency solvents and good kerosine , jet fuel , and diesel fuels , but straightrun gasoline of inferior quality compared to similar products from either West Texas or Venezuelan high - sulfur oils . The Near East oils also should be good sources of lubricating stock . However , when used as stock for catalytic cracking or reforming , the Near East oils suffer by comparison because they are deficient in naphthenes .

Jan 1, 1964

By William R. Wayment, David E. Nicholson

A modified percolation - rate test is proposed for use in determining flow rates through hydraulic backfill ; in contrast to the conventional test , a percolation- rate versus void - ratio relationship is established . requirements and a detailed test procedure are described . Equipment Results of a conventional test are compared with those of the proposed modified test . The proposed modified test method yields more accurate , realistic , and usable percolation- rate ( permeability ) data . The significance of obtaining accurate percolation rates for use in analyzing waterflow through hydraulic backfill is discussed .

Jan 1, 1964

By A. E. Schwaneke

Plans and specifications are given for constructing a quartz composite oscillator designed to measure internal friction in metals and alloys . The characteristics of the system are listed , and detailed procedures for its operation are explained . Typical measurements on manganese - copper alloy , on single - crystal magnesium , and on polycrystalline magnesium are shown to illustrate applications of the system .

Jan 1, 1964

By John Nagy, Henry G. Dorsett, Murray Jacobson

Laboratory studies show that ignition of a dispersed combustible dust in an open vessel may be prevented by adequate inerting . Factors affecting the inerting requirements are -- dust concentration , spark energy , ignition temperature , composition of the substances used for inerting , fineness of dust and type of combustible . The oxygen concentration of the atmosphere and in some instances the proportion of admixed inert powder and moisture required to prevent ignition are given for 367 dust samples . Variations in inerting requirements with strength of igniting source are discussed .

Jan 1, 1964

By T. A. Henrie, J. D. Marchant, E. S. Shedd

Cerium metal was electrowon in a fluoride bath from cerous oxide and tapped from the cell during prolonged operation . Electrolyte constituents were CeF , BaF₂ , and LiF. Twenty- seven pounds of metal of 99.8 percent purity were produced at a rate of 3 pounds per hour and tapped from the cell . Principal impurities were molybdenum , aluminum , oxygen , and carbon . The operating parameters , such as electrode geometry , bath compositions , and oxide feed rate , were investigated . Anode reactions were found to be important factors in cell operation . Stable cerous oxide reacted more uniformly at the anode surface than ceric oxide . Electrowinning was conducted in crucible hearths consisting of both frozen electrolyte and molybdenum metal . Both materials proved satisfactory and did not react with the molten cerium . Stable cerous oxide was prepared by carbothermic reduction and used as a feed material . Cell design proved to be an important factor in continuous cell operation . Complementary to the investigations of electrowinning of cerium , the metal was purified by electrorefining in a chloride electrolyte .

Jan 1, 1964

By J. A. Ruppert, P. M. Sullivan

A study was made of filtration techniques for recovering the major part of the tin contained in iron - tin alloys known as hardhead . Special smallscale filtering apparatus and a three - stage cyclic process were developed . Eighty- seven percent of the tin contained in an alloy of 82 percent tin and 17 percent iron was recovered as pure metal by pressing at 975° C followed by a second pressing at 800 ° C and a final filtering at 250 ° C. Small amounts of Sb , Cu , and Fe impurities were removed by adding Al to the molten product and performing another filtration at 250 ° C.

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 J. H. Holden, C. C. Shale, G. R. Strimbeck, W. S. Bowie

Electrical characteristics of positive corona are presented for air in a 2 - in - diam electrostatic precipitator operating under dynamic conditions at temperatures of 600 ° to 1,500 ° F and pressures of 0 to 80 psig . Results show that current - voltage relationships depend solely on air density . Comparison of data on positive corona with previously published data on negative corona demonstrates a higher sparkover voltage and a wider range of operability for positive corona at temperatures above 375 ° F. The possibility of achieving higher voltages with positive polarity as indicated by these experiments implies several advantages for the use of positive corona in precipitators to allow better removal of suspended material from hot gases . Based on the physics of an ion in an electrical field , a theoretical equation is derived to define current - voltage characteristics of positive corona in terms of air density . Constants for the equation are evaluated from Calculated current - voltage values at different air densities agree reasonably well with experimental data .

Jan 1, 1964

By J. C. Meeks, C. L. Klingman

An instrument that is sensitive , portable , safe , and low in cost was developed by the Bureau of Mines for detecting helium leaks by comparing the thermal conductivity and flow rate of the atmosphere around the suspected leak against a reference of helium- free air . A vacuum pump pulls the sample gas through a restriction and over thermistor elements , the combined electrical output of which is affected by thermal conductivity and flow rate of the sample gas . Tests showed that the battery - operated Helium Leak Detector was effective and rugged instrument that could be operated safely in explosive atmospheres . The instrument could also detect , but not identify , other gases such as methane , hydrogen , argon , carbon dioxide , and Freon 12 .

Jan 1, 1964

By R. W. Hiteshue, C. O. Hawk, H. H. Ginsberg, M. D. Schlesinger

The Bureau of Mines studied single - step catalytic vapor - phase hydrogenation of oils derived from coal and oil shale . Treatment of middle oil , from hydrogenation of bituminous coal , gave good yields of gasoline with a German - made molybdenum- zinc - chromium catalyst . The Bureau also achieved good results with duplicates of this catalyst made from domestic raw materials . In one set of experiments with the German catalyst , 38 to 52 wt pct of feed was converted to gasoline . The total liquid product was 91 to 98 wt pct of the feed . Not all this gasoline can be claimed as production , however , because about 20 pct of the feed was in the gasoline range , and part of it undoubtedly survived the hydrocracking treatment . Hydrogenation of crude shale oil in the presence of cobalt molybdate catalyst produced a total liquid product of 89 wt pct of feed . The hydrogenation converted 27 wt pct of feed to gasoline and 44 wt pct of feed to diesel fuel . The remaining liquid product , 18 wt pct of feed , was residue boiling above diesel fuel . The gasoline was of poor quality , with an octane number of 39.1 . The overall product seemed a suitable feed stock for a conventional refining operation . Coker distillate hydrogenation , using a cobalt molybdate catalyst , gave a total liquid product of 97 vol pct of feed ; of this product 60 vol pct was jet fuel and 40 vol pct was diesel fuel . High nitrogen and sulfur in all three of these raw materials severely poison the usual refining catalysts . Thus , the common objective in these

Jan 1, 1964

By Louis A. Panek, John A. Stock

A flat slot is created in rock to cause stress relief effects in a pair of hydraulic borehole pressure cells (previously installed in drill holes above and below the slot ) , which act as sensing devices . This relief is annulled by repressuring the slot by means of a flat hydraulic cell . The slot pressure at annulment is taken to be the existing ground stress at right angles to the plane of the slot . A number of trial installations in the rib of a mine drift showed that for a valid determination of ground stress the sensing devices that respond to relief and repressuring must be within a specified zone close to the pressure transmitter ; otherwise the indicated ground stress may be excessive . By using an additional pair of borehole pressure cells , installed a few feet away , the existing rock stress can be redetermined at intervals , irrespective of a change of stress intensity subsequent to the initial installation . Based on these findings , equipment and procedures have been developed that make possible the installation and operation of a permanent rock stress monitoring station for observing mining - induced stress changes . The station consists of a 12 - in - wide hydraulic pressure cell cemented in a flat slot and four 2- by 8 - in flat hydraulic pressure cells in nearby drill holes . All drilling for the installation can be done with an air leg drill and conventional bits . Once the installation is completed , all required information is obtained by Bourdon pressure gage readings . The apparatus is simple , relatively inexpensive , and reliable under operating conditions in a wet mine . Unlike most methods of rock stress determination , this scheme permits periodic remeasurement of absolute rock pressure over several years , without additional drilling or instrumentation . Similar to other flat slot procedures , stress measurements are obtained without making auxiliary tests to determine elastic

Jan 1, 1964

By H. Kato, G. Asai, R. Blickensderfer, R. Siemens

Some relationships were established among crystallographic orientation , rollability , deformation texture , annealing behavior , slip planes , and ductile- brittle bend transition temperature of molybdenum single crystals . Six large molybdenum single crystals obtained from an ingot melted by electron beam were oriented by X - ray diffraction and rolled on crystallographic planes of low indices in a known direction . During room temperature rolling , cleavage occurred on 100 type planes . At 300 ° C the crystals were rolled to 95- percent reduction in thickness . The crystals ( 001 ) [ 110 ] and ( 011 ) [ 100 ] were most easily rolled . Pole figures were used to correlate the deformation textures of the rolled crystals with the initial crystallographic orientation . Several of the textures which developed could be explained as a rotation about a < 110 > axis of symmetry . The cube crystal ( 001 ) [ 100 ] retained much of its " cubic " orientation . The (001 ) [ 110 ] crystal developed the simplest texture , whereas the ( 211 ) [ 113 ] and ( 211 ) [ 120 ] crystals developed the most complex textures . The 1 - hour recrystallization temperature of the crystal ( 211 ) [ 113 ] was 700 ° C , which is about 300 ° C lower than that of commercial polycrystalline molybdenum . The poles of the slip planes ( as determined from gross slip lines at relatively low magnification ) tended to lie within 20 to 60 degrees of the pole of the rolling plane . The Knoop hardness was slightly dependent upon crystallographic orientation but more dependent upon rolling direction . The ductile- brittle bend transition temperature was dependent upon the rolling orientation and the dislocation density .

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