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By W. K. Tolley

The Bureau of Mines is testing super critical fluids as solvents to selectively extract valuable components from complex matrices. Materials recovered during supercritical fluid extraction are often highly purified. Using laboratory apparatus designed specifically for supercritical fluid research, Bureau re-searchers have measured the solubility of titanium tetrachloride (TiCI4) in supercritical, liquid, and gaseous carbon dioxide (C02), CO2, a commonly used supercritical fluid, is inert, inexpensive, and nontoxic. Supercritical CO2 formed a single phase with TiCl4 at 45° C and 1,500 psig. When the solution was heated at constant pressure beyond 55° C, TiCl4 precipitated from the fluid. Results showed that TiCl4 solubility in supercritical CO2 is not controlled by the vapor pressure of the solute.

Jan 1, 1989

By P. C. Good

This Bureau of Mines report describes the preparation of phosphoric acid directly from phosphate ore, without prior beneficiation, in a small-scale, continuous process research unit, as part of an effort to improve minerals and metals recovery from domestic resources while minimizing environmental effects. Three phosphate-matrix samples, ranging in grade from 18.2 pct P20S5to 11.9 pct P205, were dry-fed at a rate of 1.82 kg/hr (4 lb/hr) to a continuous-circuit, 12-liter, single-tank digester to yield phosphoric acid and byproduct gypsum filter cake. Comparison with earlier data shows that a significantly improved filtration rate was attained in a single-tank reactor compared with that attained in a five-tank reactor train processing the same ore. Iron and aluminum impurities in the product phosphoric acid averaged about 60 pct higher than amounts reported in commercially prepared, concentrate-derived acid. All gypsum filter cakes prepared had a firm, sandy texture, rendering them physically suitable for stacking or landfill use. Introduction of dry attritioning and air classification approximately doubled the attainable filtration rate when the dry-beneficiated product was digested. In air classification, there was a 12-to 14-pct P205 loss. Depending on the technique used and the matrix grade, overall P205 recovery ranged from about 72 to 89 pct.

Jan 1, 1979

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961

By L. C. IlsLey

Cooperation between the United States Bureau of Mines and the Safety in Mines Research Board of Great Britain, continuous since 1924, has made possible this and other papers on safety subjects. Grateful acknowledgment is made to representatives of the Board for their assistance in arranging visits to several mine safety stations, and to F. R. Wynne, Deputy Chief Inspector of Mines, for arranging visits to mines in Great Britain and other countries in Europe. During the summer of 1927 the writer had the privilege of visiting the mine safety testing stations in great Britain, Belgium, Germany, and France, in the order named. All of these countries have large coal mines, many of which are rated as gassy. Therefore, when the installation of electrical equipment is contemplated, each of these countries is confronted with the same safety problem as is the United States - the development of electrical equipment that will not ignite gassy atmospheres which through neglect or accident might surround the equipment. The means employed by these countries in safeguarding gassy mines should therefore be of general interest to safety engineers in American coal mines, and it is proposed to give a brief survey for each of the four countries mentioned. The third of these surveys covers conditions in Germany.

Jan 1, 1929

By A. A. Cochran

Bureau of MinesThe Bureau of Mines studied the development of practical methods for recovering manganese from the extensive domestic resources of low-grade ores and open hearth slags. A one-step operation was developed on a laboratory scale in which manganese and iron compounds are treated with chlorine, volatilized, and separated by selective condensation. Manganese recoveries of 90 to nearly 100 percent were obtained from 9 of the most important domestic ores. Analyses of the manganese chloride product indicated that it was suit-able for aqueous electrolysis with little additional purification. A complete, integrated process that provides for the recovery and recycling of chlorine is proposed. This process appears to have distinct advantages over previously proposed manganese recovery processes, and, in sharp contrast to leaching procedures, it is applicable to practically any manganese-bearing material.

Jan 1, 1967

By P. L. Sibrell

The U.S. Bureau of Mines has tested cyanide leaching for recovery of palladium (Pd) from spent petroleum processing catalysts. Three different catalyst samples were supplied by a spent-catalyst processor. These catalysts consisted of a zeolite base and contained 0.4 to 0.7 pct Pd. During alkaline cyanide leaching, the catalysts exhibited ion-exchange properties due to their zeolite matrices. Hydrogen ions were released from the zeolite in exchange for sodium ions in solution, resulting in a significant decrease in solution pH. This could present a safety hazard because of the potential for release of toxic hydrogen cyanide gas. A pretreatment step where the catalysts were contacted with a 1.0M sodium hydroxide solution was found to prevent the pH shift from occurring. Following the sodium hydroxide pretreatment, two stages of leaching at 160 °C with solution containing 1 pct sodium cyanide and 0.1[M] sodium hydroxide gave at least 75 and up to 95 pct Pd recovery. The Pd was quantitatively recovered from the leach solution by thermal decomposition in an autoclave at 250°C for 1 h. The Pd content of the precipitate was over 50 pct. Thermal decomposition also decreased the total cyanide content of the barren solution to less than 0.2 mg/L. The catalyst leach residues passed the Federal Toxicity Characteristic Leaching Procedure and the California Waste Extraction Test, indicating that landfill disposal of the leach residues would be acceptable.

Jan 1, 2010

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

More than 400 academic, Government, and industry representatives attended the third symposium on ash utilization and technology held in Pittsburgh, Pa., March 13-14, 1973. Sponsored by the American Public Power Association, Edison Electric Institute, National Coal Association, National Ash Association, and Bureau of Mines, the symposium Featured 26 formal presentations by leading experts from Europe and the United States on all major phases of ash production, utilization, and research. Abstracts of all the papers are grouped right after this introduction, and the full symposium proceedings follow. Sponsoring organizations and their chief representatives were the National Coal Association, James R. Garvey, Bituminous Coal Research, Inc.; Edison Electric Institute, C. E. Brackett, Southern Electric Generating Co.; American Public Power Association, Herbert Blinder, Columbus (Ohio) Electricity Division; National Ash Association, Inc., James N. Covey, Rochester Gas and Electric Corp.; and the United States Department of the Interior, Bureau of Mines, William L. Crentz.

Jan 1, 1974

By Harry R. Nicholls

A simple economical method has been developed for determining the in situ longitudinal and shear velocities in rock from which its elastic constants can be calculated. By detonating small charges of high explosives in shallow drill holes near a free surface, both longitudinal and shear waves were generated simultaneously. Accelerometers and velocity gages mounted to the rock surface were used to record the arrival time for both waves over travel path lengths from 50 to 450 feet, Measurements were made in two rock types. From the arrival time measurements, the longitudinal and shear wave velocities were calculated. From these velocities and the density of the rock, the elastic constants were calculated. The dynamic elastic constants of drill core samples of the two rock types were determined in the laboratory by the resonant-frequency method, The lab- oratory and in situ elastic constants are compared and significant differences noted. In general, there is less spread in the in situ data than in the laboratory data, and Poisson's ratio does not fall outside the theoretical limits for the in situ data as is often the case for laboratory-determined elastic constants.

Jan 1, 1961

By George S. Rice

The major purpose of this bulletin, as indicated in the preface by Dr. John W. Finch, Director of the Bureau of Mines, is to give a critical review of the coal-mining methods used in the principal producing countries of Europe, to describe the reasons underlying the adoption of these methods, and to contrast them with coal-mining methods employed in the United States. The report includes discussions of various subjects intimately related to coal mining, such as geology of the principal coal fields; production and resources of the several countries; mine safety and health research; Government mining regulations; mine inspection and rescue procedure; safety lamps; fixed lighting methods under-ground; testing electric motors, mining machines, and mining explosives for permissibility; and special mining hazards, such as explosions of gas and coal dust, mine fires, instantaneous gas outbursts, ground movement and surface subsidence, and bumps. Commercial, economic, and labor problems of European coal mining, including miners' output, wages, and social-insurance schemes, as well as cost of mining, prices of coal, etc., are briefly described. It will be noted that data on most subjects are not given for Russia, which has become an important coal-producing country, owing to the lack of reliable published information concerning Russian coal mining.

Jan 1, 1939

By J. Koster

[In lQ jG thc E'lcct,ro:~(: L7.l :~u..-ic:ll S;%cti ?n of t?c :I. tcIl~tr,-;lcal 3:vi cioa, ?U~CE~U of lv!irtos, bc,~m an 9.ct iv.t In-:?*t ik7;5i GI of r.:ct.l-;c?;is for rccovcrin,; niclrel, cop?ir, an2 ?? cciou:; ~ot-1 c 1;-on or; :; of tile 3unl~crvi~.l~~ tiistrict in C1ni.k Coult:r, !Icl.r. ]

Jan 1, 1939

By J. Koster

[In 1178 thn S-00n of thr !~Viluralcal Divicion, pur--'11 cf Mines, bcran an o. 't iv in': n-t!Y_Vnn of vothod; for recoverin'-1, Achol, copp~r, nK precioun notnin Zycn o;. -z of tic Bunkcrvillo KOH& in Clark County, Tcv. Tho Bunkcrvillo ran arc of t,-j)(,e of -iincrilization similar to that of 02 SWbury, Ontario, CannO, nichvl dc-?o?-:.t,. At prcoont, only n anall tonnes? p of ore has loan cxDr)scd in t*ic' :hui:er7ilIp rc: inn, ann. there is decided nce! for orjn: izod OrospectiAg ina drvclo-nnnt "crk there. It wann believod, howevar, t4it the dc,cuits varo 3ilficUntly siSnIficant to warrant an investigation iito their]

Jan 1, 1939

By A. C. Fieldner

The past full year of war has increased greatly the demand for virtually all kinds of fuel, and the Bureau of Mines research and service facilities have been extended to meet these unprecedented requirements. Liquid fuels, such as aviation and motor gasolines, are fundamental to modern warfare. Bituminous coal and anthracite are needed, not only to servo the expanded industrial program for which coal normally is used but also to replace natural gas, wherever possible, and fuel oil in the Eastern States, New England, and the Pacific Northwest. Railroad transportation with energy derived from coal is replacing much of the motor-vehicle transportation that has been stopped or curtailed to conserve rubber. Pulverized coal hoe been sound to be a satisfactory and cheaper substitute for fuel oil in metallurgical heating furnaces. Celloidal fuel - a mixture of coal dust and oil - may offer a partial substitution for curtain coal-burning equipment. Several industrial experiments have been made with this type of fuel. The expansion of the steel industry in connection with the war program has required a corresponding increase in the production of metallurgical coke and its associated byproducts - light oil, tar, ammonium sulfate, and surplus gas. If the war is of long duration and new reserves of petroleum are not discovered, wartime trends from fuel oil to coal probably will not be reversed.

Jan 1, 1945

By Frederick C. Kohout

An advanced water-in-oil emulsion hydraulic fluid has been developed which meets defined laboratory performance criteria and which has given fully satisfactory results in a one-year underground mine test in two continuous miners. A novel method of monitoring fluid water content was demonstrated and incorporated into a test kit for use at or near the mine site. Test fluid fire resistance integrity as measured by the MSHA Schedule 30 procedure was maintained during the test and important fire resistance test variables identified.

Jan 1, 1979

By E. E. Maust

The literature on the activation of sphalerite for flotation by short¬chain xanthates leaves unanswered the question of whether a compact surface film of activator sulfide is necessary or merely sufficient for high flotation recoveries. Studies by Guarnaschelli and Plaksin indicate that xanthate adsorption and flotation of sphalerite are increased with increasing hole/ electron ratio. These results, and the known acceptorlike behavior of many heavy-metal impurities in zinc sulfide, suggest that activation may result from a traditional semiconductor doping effect at the surface. Using the theory of chemisorption states on ionic crystals as developed by Levine and Mark, the Bureau of Mines has carried out A calculation to estimate the surface-state energies of various metals when they are substituted at zinc sites on (110) sphalerite surfaces. Based on a simple Madelung-Born treatment of ionic solids, the calculation indicates that many of the metals known to activate sphalerite for subsequent flotation have lower surface-state energies than nonactivators. The results of these calculations are discussed from the standpoint of consistency with the proposed activation mechanism and observed flotation results. The satisfactory agreement obtained is taken to be support for the proposed mechanism, and further elaboration of a surface-doping model is attempted.

Jan 1, 1976

By R. L. Grant

An investigation was undertaken by the Bureau of Mines to determine the relationship between freespace and ignition probability for borehole shots. A series of experiments was concluded which covered six freespace conditions for a pemissible explosive in a 3/4-inch borehole and encompassed some 700 shots. The results were analyzed statistically. From the analysis of variance, it was concluded that the freespace means were different and that this conclusion is not impaired by possible differences in the explosives used. Within the limitation of this experiment, a definite relationship was found between the freespace and the ignition probability. Specifically, the incendivity increases with increased freespace up to a maximum; beyond this maximum there is some indication of decreasing incendivity. Further investigations are in progress to establish whether the effects of freespace on ignition probability reported here are applicable to the large test gallery, INTRODUCTION A borehole loaded with an explosive charge is a common feature of the routine gallery tests for determining the permissibility of coal-mine explosives, of Experimental Coal-Mine shots, and of the small steel cannon shots used in connection with certain research programs on the ignition of firedamp (6, 10).6/ The question of the interrelationship of freespace, weight of charge, and ignition probability of the methane-air atmosphere has been raised

Jan 1, 1959

By James J. Snodgrass

The Bureau of Mines designed and constructed a series of calibration models for geophysical borehole logging. A nominal hole diameter of 3 inches was selected as representative of typical core holes drilled for mining and engineering purposes, although additional hole diameters of 2, 5, and 8 inches are provided in one of the models for determination of empirical correction factors for variations in hole diameter. The physical properties of the models were determined by laboratory analyses of drill core samples and evaluated statistically for reliability. This report outlines the location of the models, elements of design and construction, and results of the laboratory tests. The models are available at the Denver Federal Center, Denver, Colo., for use by Government agencies and private industry to calibrate logging equipment for measurements of density, sonic velocity, magnetic susceptibility, and electrical resistivity.

Jan 1, 1976

By Martin H. Stanczyk

The direct dissolution of a typical zinc sulfide flotation concentrate by elevated temperature and pressure leaching was investigated. The concentrate assayed about 55 percent Zn, 32 percent S, 6 percent Fe, and 1 percent Pb and contained minor quantities of copper and precious metals. The influence of various factors on the dissolution of the zinc in acidic and ammoniacal pulps when using oxygen as the oxidant was determined. The tests revealed that the sphalerite was difficult to oxidize. Complete dissolution of the mineral required vigorous and intimate nixing of the gaseous, liquid, and sold phases. The addition of pyrite or sulfuric acid to water slurries of the concentrate was required to obtain a high zinc extraction when leaching under acidic conditions. The quantity of pyrite and acid used was about 0.125 and 0.25 pound, respectively, per pound of zinc sulfide contained in the leach charge. In tests with acid, about 96 percent of the zinc was extracted from the concentrate in 1 hour at 200° C. when the oxygen partial pressure was 75 pounds per square inch gage or higher. Leaching with a continuous flow of air as the oxidant gave results that were almost as good as those obtained when oxygen was used, In tests with air fed through the autoclave at 320 liters per hour, 95 percent of the zinc was dissolved in 1 hour, Acid leach solutions assaying approximately 58 grams Zn per liter and containing Fe, Ni, Cr, and Cu impurities were produced in the better tests. The leached residue consisted essentially of red iron oxide together with substantially all of the lead and precious metals.

Jan 1, 1961

By G. W. Elger

The Bureau of Mines conducted laboratory and larger scale studies on samples of domestic perovskite and ilmenite ore concentrates to devise a procedure for recovering TiC from these ores. From the concentrates, mixtures of titanium and calcium carbides were produced. The carbides were then ground and reacted with water. This reaction decomposed the CaC2 to acetylene and hydrated lime and simultaneously liberated the TiC. Using a combination of elutriation and gravity-separation techniques to separate the hydrated lime, approximately 93 pct of the titanium was subsequently recovered as purified carbide containing 54 to 70 pct titanium with CaO content as low as 0,6 pct. This combination of techniques can be used to separate more than 90 pct of the CaO from the TiC. Therefore, this carbiding procedure is a viable method for treating titaniferous materials, including perovskite, that contain more than 20 pct CaO. Tests made in a static-bed reactor showed that for the reaction of TiC with elemental chlorine to produce titanium tetrachloride (TiCI4), a temperature of at least 940° F is desirable to achieve a suitable extraction of titanium in a laboratory chlorination reactor. In fluidized-bed tests at 840° F, 98 pct of the titanium contained in TiC was extracted.

Jan 1, 1980

By Nan C. Jensen, Oliver Bowles

Stone , the foundation of the continents and the floor of the oceans , is one of the most substantial and enduring of all substances that constitute the material universe . Stone furnished rude shelter for aboriginal man , and through all succeeding ages it has provided a lasting and serviceable structural material . Limestone is one of the most widely used building stones .

Oct 1, 1947