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By Raymond W. Hiteshue, Sam Friedman, Robert Madden

Experiments were made in a semicontinuous unit to provide engineering data for designing experimental continuous systems . These systems would be used to study the hydrogasification of hvab coal and char (from lowtemperature carbonization ) to high - Btu gas . In experiments at 800 ° C and with a coal residence time of several seconds , yields of hydrocarbon gases increased from about 2,000 scf / ton of maf coal at 250 psig to 7,000 scf at 1,000 psig . With 15 minutes residence time , yields increased from 8,000 scf/ton of maf coal at 250 psig to 17,500 cubic feet at 1,000 psig . In all cases , small quantities of heavy oils were produced along with the gaseous hydrocarbons . Production of oils could be minimized with a corresponding increase in gaseous hydrocarbons by increasing the retention time of the volatiles within the hot zone . Yields of gaseous hydrocarbons from char were slightly greater than from coal under similar conditions . Although the hydrogasification reaction is very pressure dependent , substantial quantities of coal (40 to 60 percent ) could be reacted to gaseous hydrocarbons at pressures as low as 50 psig provided reaction temperatures were increased to 1,200 ° C. It was also demonstrated that a hvab coal could be hydrogasified continuously without incurring agglomeration . This was achieved by dispersing coal in a relatively large reactor with concurrent flow of hydrogen . At 1,000 psig and 800 ° C , it was possible to react about 35 percent of the coal and to produce a gas containing up to 52 percent methane .

Jan 1, 1964

By Robert J. Brennan, Edward R. Navrocky, John W. Buch

In an effort to establish a highly productive mechanized mining system for anthracite beds pitching between 10 ° and 20 ° , for which conventional mobile equipment is not adaptable , the Bureau carried out an experiment in longwall mining using an Anderton- type drum cutter loader and friction - type yielding steel roof supports . The roof- support system proved to be inadequate for breaking the overhanging roof at the break line supports , with the result that the roof broke over the solid coal . The accompanying subsidence destroyed the continuity of the roof in the work area , and the project was discontinued .

Jan 1, 1964

By C. E. Wicks, J. E. Tress, F. E. Block

The Bureau of Mines investigated the effects of gamma radiation on materials and chemical reactions to obtain information that could be of value in modern metallurgical practices . Various combinations of metals and their ores and compounds were irradiated in attempts to effect reactions that might be applicable in the extraction and separation of metal values from minerals and The types of reactions studied included complexing of salts , decomposition of hydrated salts , metal chlorination reactions , leaching of ores and minerals , halogen exchange , and various reducing reactions . All irradiations were performed at the Materials Testing Reactor Gamma Facility of the U.S. Atomic Energy Commission at Idaho Falls , Idaho . Spent fuel elements were utilized as the source of the gamma radiation . Some irradiation - induced changes , ranging from mere color change to participation in chemical reactions , were noted . The greatest value of these investigations , however , was the experience acquired , which should be valuable in future explorations of similar nature .

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 I. L. Nichols, K. C. Dean, P. H. Johnson

Hydrochloric acid , sulfuric acid , and chloridizing roast- water leaching methods for dissolution of cesium and rubidium from Maine , Canada , and Southern Rhodesia pollucite ores and their flotation products were investigated by small- scale tests . Optimum conditions were determined to be ( 1 ) for hydrochloric acid leaching , use 12.7 equivalents of 8.8 normal acid per equivalent of cesium in the sample and leach for 6 hours at 100 ° C ; ( 2 ) for sulfuric acid leaching , use 12.7 equivalents of 14.4 normal acid and leach for 2 hours at 120° C ; and (3 ) for chloridizing roast - water leaching , roast minus 200 - mesh ore, limestone , and calcium chloride in a ratio of 2 : 4 : 1 , respectively , for 1 hour at 900 ° C , and leach the calcine for 1 hour at 80 ° C with enough water to give 35 pct solids . Extractions of cesium from ores and flotation products containing over 20 pct cesium were in excess of 97 , 93 , and 96 pct for the hydrochloric acid , sulfuric acid , and chloridizing roast - water leach processes , respectively .

Jan 1, 1964

By C. Q. Cupps, R. F. Zaffarano, J. Fry

Reservoir oil analyses from seven wells in the Greater Clareton area have been included in a study of the original characteristics of oil in the Newcastle sandstone reservoir . These data correlated with areal location of the wells show an increase of saturation pressure in a general north - south or downdip direction . The increase amounts to about 500 psi in more than 17 miles , which corresponds to a depth increase of about 1,600 feet . To facilitate application of the data to engineering analyses , average characteristics are given for arbitrary north and south divisions of the 22 - mile - long producing area . The downdip increase of saturation pressure is taken as evidence of updip diffusion of solution gas from a somewhat higher concentration at the bottom of the reservoir . This effect is opposite to that previously observed in two prominent high- relief reservoirs in the Rocky Mountain area . The increasingly greater saturation pressures southward or downdip in the Greater Clareton area suggest a continuing migration of fluids into the structure .

Jan 1, 1964

By Ralph Husack, J. W. Eckerd, G. A. Brady

The effect of gamma radiation on Pennsylvania anthracite and on reactions between anthracite and other materials was studied using a shielded , selfcontained 23,000 - curie cobalt 60 source . When anthracite was exposed to air at 65° C the reaction with oxygen was greater in the presence of radiation. than in its absence . Although drop- shatter tests indicated that exposure to radiation decreased the resistance to breakage of anthracite , this evidence of structural weakening was not supported by the results of grindability or particle- size studies . Irradiation caused definite changes in the gases evolved from evacuated samples of anthracite ; the percentages of hydrogen and carbon dioxide were increased, and the methane concentration remained unchanged . Carbon monoxide was evolved only from the unirradiated samples . Electron paramagnetic resonance (EPR ) measurements indicated large differences between evacuated samples and those exposed to air . There was little or no difference between irradiated and unirradiated samples , except that the free- radical content of unirradiated samples of anthracite increased progressively with higher temperatures of evacuation , but in the case of irradiated samples , no such behavior was found . Attempts to produce carbon disulfide and calcium carbide by reacting anthracite with sulfur up to 120 ° C , and with calcium oxide up to 400 ° C , were unsuccessful .

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 Rolland L. Blake

Petrographic and mineralogical studies were made on unoxidized samples from the Cuyuna and Mesabi districts to study occurrence and properties of the iron phyllosilicate minerals . Examination of 96 thin sections from the thinbedded facies of the main iron - formation of the Cuyuna district indicates that the most abundant minerals are Mn - Mg - siderite , stilpnome lane , and minnesotaite . Reconstitution and recrystallization of minerals has occurred along certain beds , and textures indicate that some minnesotaite apparently formed at expense of stilpnomelane . Three samples of stilpnome lane and one of minnesotaite were concentrated from fracture - fillings within iron- formation . Results of chemical , optical , spectrographic , X- ray diffraction , and differential thermal analyses on these samples are reported . The detection of ammonia in stilpnome lane samples is the first such occurrence reported , and its significance is discussed . New mineral data are presented on greenalite and probable septechamosite from the Mesabi district .

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 D. W. Frommer, L. Bonicatto, M. M. Fine

A mineral - dressing investigation was conducted to demonstrate the ability of an anionic silica - flotation process to produce high- grade concentrates from submarginal iron ores of the western Mesabi and Menominee ranges . Commercially available equipment and reagents were used . Samples from the Menominee range were exclusively from the Groveland , Mich . , mine and contained hematite as the chief iron - bearing mineral . Bench- scale investigations established that the anionic silica flotation method can function effectively on a variety of undeslimed ores . Continuous tests completed on one Mesabi semitaconite ore and on Groveland mill feed , have verified the validity of the bench research . The Mesabi samples yielded a concentrate containing 60.3 percent Fe and 6.0 percent Sio with an accompanying iron unit recovery at 90.5 percent . Iron recoveries from the mill feed ranged from 79.0 to 87.4 percent .

Jan 1, 1964

By Oliver C. Fursman, Lloyd H. Banning

This research was undertaken to determine the feasibility of producing steel from hydrogen - reduced , pyrophoric iron powder . Before steelmaking tests were begun , investigations were made to develop procedures for handling the pyrophoric powder safely , and melting tests were made in a single - phase , electric - arc furnace to determine inert gas requirements for preventing powder oxidation . Steelmaking tests were conducted in a conventional electric - arc furnace , usually by a two - slag basic procedure . Results of the research indicated that ( 1 ) pyrophoric powder can be handled safely and can be prevented from oxidizing excessively during charging and melting in electric - arc steelmaking furnaces ; ( 2 ) little , if any , more electrical energy is required for melting Cerro Bolivar iron powder per unit of contained iron than is required for melting heavy melting scrap ; ( 3 ) high - quality steel can be produced readily from high- grade iron powder , having recoveries up to 95 percent of the total iron ; ( 4 ) steel can be produced from simulated titaniferous , chromiferous , and manganiferous iron powders ; and ( 5 ) the electrical energy required for melting increases with increase in the proportion of slag - forming constituents in the furnace charge .

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 S. L. Payne, E. F. Foerster, C. W. Schultz, G. R. Zellars

The vapor pressure of copper in a series of liquid copper - nickel alloys was determined by the carrier gas method . The activity and activity coefficient of copper were calculated over the entire range of alloy composition . These data show a slight positive deviation from ideal behavior . The activity coefficient of copper was highest ( 2.10 ) at 0.05 mole fraction copper and approached unity at concentrations above 0.85 mole fraction copper . The results for nickel were calculated from the copper data by the graphical integration of the Gibbs - Duhem equation .

Jan 1, 1964

By Foster Fraas

The response of minerals in magnetic separators is in accordance to dynamic rather than static magnetic susceptibility values . The dynamic value varies with respect to both passage speed through the separating field and time of exposure in a preliminary treatment field . Tests on 16 minerals and solids have demonstrated that both of these factors affect different minerals in different ways .

Jan 1, 1964

By James M. Nishi, Lloyd Carpenter

Sixteen elements were determined spectrochemically in the general range of 3 to 1,000 ppm in high - purity columbium . Samples were converted thermally to Cb2 O , mixed with graphite and Ge02 , and excited for 15 seconds using a 15 - ampere dc arc . For the molybdenum determination , the oxidized samples were mixed with NaCl and Geo₂ and excited for 30 seconds . Spectra were recorded on photographic plates , and spectral line transmittance values were measured photometrically . Relative - intensity ratios of selected analytical and internal standard spectral lines were plotted against concentrations of standards to form curves from which concentrations of impurities were read . Average precision of the method was 11.2 percent relative standard deviation .

Jan 1, 1964

By G. W. Birge, D. E. Wolfson, J. H. Lynch

Fourteen coal samples representing the Flag , Fire Clay , Whitesburg , Amburgy , Upper Elkhorn No. 3 , Upper Elkhorn No. 2 , Upper Elkhorn No. 1 , and Lower Elkhorn beds in Letcher County , Ky . , were carbonized by the Bureau of Mines - American Gas Association ( BM- AGA ) method , and yields of products and physical properties of cokes were determined . The samples tested were high- volatile A bituminous in rank , with dry , mineral - matter- free fixed - carbon contents ranging from 55.3 to 62.2 percent . Five of the samples , as received , were chemically unsuitable for metallurgical use because of excessive ash and/ or sulfur content . Generally , strength indexes of the cokes were low and all of the coals would require blending with higher rank coal to obtain satisfactory blast furnace fuel .

Jan 1, 1964

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

A process was developed on a laboratory scale in which iron contained in galvanizers ' zinc dross and aluminum contained in scrap zinc die - cast alloy were removed simultaneously . Melting both types of scrap together in the proper proportions resulted in formation of solid intermetallic Fe₂ Alg , which was readily removed from the melt by filtration and centrifugation . Recovery was 87 to 92 percent of the available zinc . Refined filtrate contained 0.02 percent iron and 0.20 percent aluminum. Aluminum content was further reduced to less than 0.01 percent by fluxing with zinc chloride . Low temperatures employed and inexpensive equipment requirements make the process commercially attractive .

Jan 1, 1964

By Gilbert M. Farrior

Tests of resistance to molten metals , to oxidation at elevated temperatures , and to various chemical reagents were made for a series of compositions in the TiB₂ - CrB₂ subsystem . In reaction with molten metals , there was no noticeable difference in reaction of the various compositions in the ( Ti , Cr ) B₂ series . The oxidation tests were ( 1 ) a rising - temperature test in which the specimen temperature was increased 4° per minute to 1,200 ° C and ( 2 ) a constanttemperature test in which the specimen temperature was held constant at 1,000 ° C. Compositions near Tio.6 Cro.4 B2 had the best oxidation resistance . Ti。.6 The chromium- rich alloys showed marked superiority to the titanium- rich alloys in resistance to corrosion by the chemical agents investigated . The chemical reagents used were sulfuric , nitric , and hydrochloric acids and sodium hydroxide of different concentrations .

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