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By J. S. Tosh

The Federal Bureau of Mines has investigated the equilibrium of the system potassium carbonate (K2C03) potassium bicarbonate (KHCO3) potassium bisulfide (KHS) carbon dioxide (C02) hydrogen sulfide (H2S) water (H20). Partial pressures of hydrogen sulfide, carbon dioxide, and water vapor were measured at 70° to 130° C. over solutions of 20-, 30-, and 40-percent-equivalent potassium carbonate containing from 20 to 3,000 grains of equivalent hydrogen sulfide per gallon of solution. This study was made to obtain equilibrium data for evaluating the feasibility of using solutions of hot potassium carbonate for removing, hydrogen sulfide from gas mixtures. The equilibrium partial pressure of hydrogen sulfide may be correlated with the ratio of the molal concentrations of the solutes (KHC03) (KHS)/ (K2CO3). The relationship is shown graphically for the 30- and 40-percent solutions. Once this ratio is determined, the partial pressure of hydrogen sulfide can be obtained from the curves. The equilibrium data show that effective removal of both carbon dioxide and hydrogen sulfide can be achieved simultaneously with hot solutions of potassium carbonate.

Jan 1, 1960

By Jerome J. Hoeppner, Walter W. Fowkes

The Federal Bureau of Mines has determined the distribution of forms of sulfur for several lignites and gasification chars and noted the changes induced by the gasification process . A method was adopted for quantitatively determining sulfide sulfur that was found to be present in the chars , although absent in the lignites . Changes in the behavior and distribution of sulfur forms were further investigated concerning the ashing of lignites and chars under standard conditions , as well as at various temperatures , and the determination of volatile matter applied to both chars and lignites . The authors concluded that the first and greatest change in the form of sulfur present in natural lignite , upon heat treatment , resulted from the reduction of pyritic and sulfate sulfur to sulfide . Organically - bound sulfur originally present is less reactive , but largely disappears on strong ignition . An appreciable part of the sulfur content of natural lignite is fixed in the char as sulfide and in the ash as water - soluble sulfate and will affect the summation of constituents , to a greater or lesser degree , in reporting the ultimate analysis of a lignite or char .

Jul 1, 1960

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

This report by the Federal Bureau of Mines describes the carbonizing properties of coals from the principal beds in Boone County , W. Va . Results are given for samples of coals from No. 5 Block , Stockton - Lewiston , Coalburg , Winifrede , Chilton , Hernshaw , Cedar Grove , Alma , and No. 2 Gas beds . Boone County coals rank as high -volatile A bituminous . Eighteen of the 21 samples tested contained from 3.3 to 7.9 percent ash and 16 of the samples contained from 0.6 to 0.9 percent sulfur . Two samples from the Alma and No. 2 Gas beds , the lowest stratigraphically of the seams tested in Boone County , contained from 1.4 to 2.7 percent sulfur . Most Boone County coals yield

Jul 1, 1960

By Carl Rampacek, W. A. McKinney

The feasibility of leaching calcareous and siliceous oxidized copper ores by downward percolation with dilute acid was investigated in the laboratory and in a small continuous plant operated by the Federal Bureau of Mines . The crushed ore was leached in deep columns with solutions containing 1 or 5 percent sulfuric acid to dissolve the oxidized copper . Bench - scale laboratory tests on two calcareous ores from the same deposit indicated that a maximum copper extraction , about 72 percent , could be expected from heap leaching a feed as coarse as 1 inch . Laboratory tests on a siliceous ore showed that almost 70 percent of the copper could be extracted by leaching a 1 / 4 - inch feed . The bench - scale tests were supplemented by larger continuous runs wherein the copper was recovered from the leach liquors by precipitation on detinned scrap iron . Leaching the calcareous ore for approximately 10 days recovered 62 percent of the total copper . The sulfuric acid consumption was 9.6 pounds per pound of copper recovered . Treatment of the siliceous ore recovered 62.5 percent of the total copper in a 2.5 - day leach and the acid consumption was 3.7 pounds per pound of copper recovered . Cement copper products that assayed over 71 percent copper were obtained from the leach solutions by precipitation on scrap iron . The bench - scale and continuous tests demonstrated that downward percolation leaching of the calcareous ores was technically feasible but not economically practicable because of high acid consumption by the gangue . Leaching of the siliceous ore was rapid and the acid and water requirements were nominal . The downward percolation leach procedure is simple and requires a minimum of plant equipment .

Jul 1, 1960

By F. R. Cattoir, D. H. Baker

Fused - salt electrorefining has been successfully applied to the purification of vanadium metal . The electrolyte used in this refining technique was sodium chloride to which had been added 3 to 6 percent vanadium as vanadium dichloride . The average deposition current efficiency was 91 percent . Oxygen and nitrogen , the impurities in commercially produced vanadium metal , were reduced by two - thirds of the amount contained in the feed material . Hardness of the vanadium- metal product was reduced from an initial 97 Rockwell B ( RB ) to a minimum of 35 Rg . The reduction of these impurities markedly improved the plasticity of the final product obtained by melting the crystalline cell metal into small ingots . These ingots could be given a 99 - percent cold reduction by rolling before edge cracking appeared . Growing interest in high - purity vanadium and the industrial need for purer metals and improved alloys for use under high temperatures and high speeds have demanded the elimination and/or control of impurities . Accordingly, research to eliminate or control the undesirable impurities has been expanded .

Jul 1, 1960

By R. W. Stahl

"This study by the Federal Bureau of Mines was confined to pillaring with continuous mining machines and to mines where total extraction is practiced. Many different conditions and practices in as many coalbeds as possible in Pennsylvania were observed.Pillar extraction or pillaring can be the most productive part of coal mining if done properly; but it also can be the most dangerous if done improperly.Because of the need for more careful planning before and caution during pillaring, many mining companies resort to the undesirable practice of stumping or hogging of pillars with subsequent unnecessary waste of valuable natural resources. Pillaring can be done at reasonable cost and safely, as proven at many mines where complete extraction is practiced and enviable cost and accident records are maintained.Although continuous mining machines are bulky and sometimes difficult to maneuver, they have been used with great success in pillaring. Occasionally, however, a machine is caught, or men are injured by a fall during pillar recovery. This Bureau survey was conducted to ascertain how safe and successful pillaring (especially the removal of final stumps in lifts or the final stump of a pillar), is accomplished in some mines, while others have considerable difficulty under similar conditions.The Bureau hopes the information to be presented in this publication will prove beneficial to those who wish to recover more pillar coal and to improve their accident record during such procedures."

Dec 1, 1959

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

"Investigations in the Federal Bureau of Mines Experimental coal mine near Pittsburgh, Pa., have shown that high-expansion foam containing at least 0.2 ounce of water per cubic foot of volume is effective in controlling exper-imental underground coal, oil, or wood fires. Some of the fires were extinguished, but more of the coal and wood fires were brought under enough control to permit direct attack with water or other extinguishing agent or loading the hot material into cars. The largest controlled experimental fire, which burned about 5 hours before attack, was in a coalbed 5 feet wide, 10 inches thick, and 100 feet long. The greatest distance foam was transported to control a fire was 1,010 feet.An incipient fire should be attacked promptly with water, rock dust, or other approved and readily available extinguishing agents. Where heat, roof falls, and smoke prevent direct approach, the more involved procedure of using foam may be advantageous. The effectiveness of the foam in controlling a deep coated fire of considerable extent H,vet to be proved by actual trials in aSome hydrogen, carbon monoxide, and methane gases are generated when a fire is attacked with foam. Calculations showed that in experimental fire tests an explosive mixture could form; however, this would occur only within a narrow range of combustible gas-air mixtures not likely to be found in practice. The principal explosion hazards are due to generation of gases by the foam, localized build-up of normally liberated methane, and volatiles liberated by the coal during heating. The quantity of combustible gases generated by the action of the foam on the fire is about the same as that when an equivalent amount of water is applied."

Mar 1, 1960

By Gerald W. Elger

The Federal Bureau of Mines developed a modification in the conventional Kroll process for preparing high - purity hafnium metal . This modification involved the partial replacement of magnesium by sodium in the batch reduction of purified hafnium tetrachloride to sponge metal . The raw tetrachloride was purified either by thermal degassing of the volatile contaminants to the atmosphere or by fused- salt treatment . In the fused- salt treatment , the tetrachloride was contacted with molten alkali chlorides to remove the impurities . The reaction byproducts were removed from the metal by heat treatment in an evacuated furnace . The metal sponge was consolidated by melting into buttons or ingots , which were analyzed for impurities . The purity of the metal prepared by the modified process is superior to that of the metal produced by the conventional method . The hafnium metal was comparable to crystal - bar hafnium except for the oxygen content , despite the abnormally high impurity concentrations in the raw tetrachloride . Several ingots were successfully cold - rolled to sheet .

Jul 1, 1960

By P. L. Woolf, J. P. Morris, E. Foerster, G. R. Zellars

Measurements of vapor pressure can be used to determine the thermodynamic activities of the components of metallic solutions . The determination of activity by this method requires accurate values for the vapor pressure of the pure component and for its partial pressure above the alloy solution . This investigation was conducted to measure the vapor pressure of liquid manganese for use in future studies of the activity of manganese in various liquid alloys . In related investigations in the Bureau's Pyrometallurgy Laboratory , vapor pressures of copper , iron and nickel have been measured and activit 4 5 6 have been determined in the iron- copper and iron- nickel systems . Difficulties were experienced with manganese which were not encountered in the previous investigations . Manganese oxidizes readily and greater care was needed to maintain an oxygen- and moisture - free atmosphere in the furnace . In addition , liquid manganese wet the refractories and there was a tendency to foam and splash on introduction of the carrier gas . Because of these difficulties several variations in the experimental procedure were studied . These were first tested with silver which has a vapor pressure of the same order of magnitude as manganese but is relatively inert at high temperatures . Although no significant changes in the original procedure resulted from this work, considerable data were obtained for silver and have been included in this report . Bauer and BBrruunnnneerr7/ have reported the only extensive investigation of the vapor pressure of liquid manganese . However , their results are not consistent with the data obtained by McCabe and Hudson for solid manganese . Measurements of the vapor pressure of silver have been reported by McCabe and Birchenal1,2/ Schadel and Birchenall , 10/ Harteck , 11 / Fischer , 12/ and von Wartenberg.13 / Generally , these investigators conducted their measurements at lower temperatures than were used in this study .

Jul 1, 1960

By Oren C. Baptist

Umiat field contains the largest accumulation of oil discovered so far in Naval Petroleum Reserve No. 4 in Arctic Alaska. The Umiat anticline was tested with 11 wells; 6 produced oil in varying quantities. Behavior of the wells during testing was unpredictable. For example, one well was abandoned as a dry hole after all tests failed to recover any oil, yet an offset well, only 200 feet from the dry hole, produced 400 barrels of oil a day. The main oil reservoirs are less than 1,000 feet deep and are in the permanently frozen zone (permafrost). Reservoir pressures are low, and most primary production will be by expansion of gas-in-solution in the oil. Because of the unusual reservoir conditions and the difficulties encountered in drilling and completing the wells, the Department of the Navy asked the Federal Bureau of Mines to make laboratory studies of the reservoir sand to determine the cause of well plugging and to provide laboratory information, to be used as an aid in estimating oil recovery from frozen reservoir rocks under solution-gas expansion from low-saturation pressure conditions.

Jan 1, 1960

By M. M. Gilkey

Pegmatites in Colorado occur for 150 miles along the Front Range (eastern-most range of the Rocky Mountains) from Larimer County on the north to Canon City on the south, and west into the Gunnison area. Many of the deposits have been classified. Minerals found in the various dikes include beryl, scrap and possibly punch mica, lithium-bearing minerals, columbite-tantalite, feldspar, and several rare minerals. Pegmatites are abundant in the Crystal Mountain district in Larimer County. About 5 miles south of the Crystal Mountain district and often identified with that district is the Hyatt pegmatite area. The Hyatt Ranch deposit has attracted particular attention because of the comparatively high beryl con-tent of the upper part exposed in opencut workings.

Jan 1, 1960

By G. V. Sullivan

This report describes an investigation by the Bureau of Mines of flotation techniques for the recovery of chromite from fine-grained disseminated ores. Reported work on the concentration of chromiferous materials shows that flotation has been applied almost exclusively to slime-free pulps. Therefore, chromium recoveries that could be obtained by flotation were related to the amount of slime rejected. However, results of recent studies by the Bureau of Mines showed that des liming is not a requisite to selective concentration of chromite. Laboratory-scale tests on seven ore types from the more important chromium-bearing areas of the Pacific Northwest showed flotation to be technically feasible for treatment of all but one of the samples. Concentrate grades were affected more by the composition of the chromite mineral than by the grade or character of the ore. Test results from three of the samples showed that, without prior desliming of the pulp, 78 to 91 percent of the chromium could be recovered in concentrates of 90 percent or more chromite; two samples responded to similar treatment, resulting in concentrates of more than 80 percent chromite with recoveries of 85 and 89 percent chromium. One sample of mill products, subjected to severe weathering, required removal of the primary slime to obtain a concentrate of 65 percent chromite with only 75 percent chromium recovery.

Jan 1, 1960

By H. E. Powell

A laboratory mineral-dressing investigation was conducted by the Federal Bureau of Mines on four limonitic and four sideritic iron ores from the North Basin of the east Texas iron-ore district. The samples, composited from drill cores, were considered representative of the iron-ore reserves of the area. The objectives of this research were twofold: (1) To devise a mineral-dressing method whereby the yield from currently mined east Texas iron ores might be increased and the grade improved, and (2) to extend such treatment to include the lower grade ferruginous materials that are not amenable to beneficiation by simple washing and, therefore, are not being exploited. Of the mineral-dressing methods used in this investigation, magnetic separation of roasted are was shown to be the most effective. Results show that, by this method, a laboratory recovery of 82 percent of the iron is attainable at a grade surpassing that obtained by current plant practice and that both limonite and siderite are amenable to concentration by the process. The existence of large deposits of iron are in eastern Texas has been recognized for over 100 years. These ores were first exploited during the Civil War and were mined intermittently until about 1911. From that time until 1944 when the Defense Plant Corporation financed the erection of three blast furnaces to use these east Texas ores, production was almost at a standstill.4/

Jan 1, 1960

By T. E. Gray

This report describes preparation characteristics of the significant coalbeds in Marion County, W. Va., as determined by the Bureau of Mines. It is one in a series telling what coals are suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.4 million tons of coal was produced in Marion County, W. Va., in 1958, of which almost 6 million tons was cleaned mechanically in nine cleaning plants. All of the coal mechanically cleaned came from the Pittsburgh bed. The Bureau of Mines estimated that 1,578 million tons of recoverable coal remained in the county in beds 28 inches or more thick as of January 1, 1955.

Jan 1, 1960

By D. Bienstock

The Fischer-Tropsch synthesis is practicable in a reactor where the exothermic heat of reaction is removed by circulating large quantities of recycle gas through a catalyst bed of high-voids content. At an hourly space velocity of 1100, the feed gas, a mixture of 1.5 parts hydrogen to 1 of carbon monoxide, was converted 90 percent, producing hydrocarbons predominantly in the gasoline range. At these conditions a recycle-to-fresh gas ratio of 40:1 was enough to give excellent temperature control with a pressure drop of 1.5 p.s.i. per foot of bed using a steel catalyst in the form of lathe turnings. Steel parallel plates, although offering lower resistance to gasflow, were less reactive and less durable. INTRODUCTION The Federal Bureau of Mines has been engaged in a research and development program since 1944 on the synthesis of gasoline from coal. Gasification of coal with steam and oxygen to yield a synthesis gas--a mixture of carbon monoxide and hydrogen--is being investigated at Morgantown, W. Va.; and the synthesis of gasoline by catalytically reacting the carbon monoxide and hydrogen over iron by the Fischer-Tropsch reaction is being investigated at Bruceton, Pa.

Jan 1, 1960

By James S. Browning

Heavy liquids have been used to separate minerals of different specific gravities for many years.4 5 6 7 8 9/ The method permits substantially quantitative evaluation of a variety of minerals and requires much less time than the usual methods of chemical analysis. This Bureau of Mines investigation was conducted to determine the applicability of heavy liquid mineral separation to the evaluation of certain spodumene and kyanite ores, prepared mixtures, and plant products. After careful standardization of the particular mineral and associated gangue, estimates of chemical analyses could be obtained from results of heavy liquid separations.

Jan 1, 1960

By C. A. Frenzel

Extensive spectroscopic data are needed in making reliable vibrational assignments for use in calculating thermodynamic functions of polyatomic molecules. The fundamental vibrations of organic molecules may be observed at any wavelength from 2.5 to 200 microns (micron = µ = 10-4 centimeters), but most often in the region from 3µ to 50µ. Raman spectra generally cover the range in which fundamental vibrations occur, but equally important infrared spectra usually are not measured at wavelengths longer than 25µ. This limitation results because most infrared spectra are determined for analytical purposes, which seldom require information outside the region 2µ to 25µ. Measurements of infrared spectra in the range 15µ to 35µ recently were begun by the Bureau of Mines to obtain data needed in making vibrational assignments. This report presents the spectra of the following thirteen compounds: Tetrahydrofuran, 1-methylpyrrole, piperidine, 2-methylpyridine, 3-miuthylpyridine, 2-propanethiol, cyclopentanethiol, 2-methyl-2-butanethiol, 3,3-dimethyl-2-thiabutane, cyclohexanethiol, cyclopentyl-l-thiaethane, 2,4-dimethyl-3-thiapentane, and hexamethyldisiloxane.

Jan 1, 1960

By R. L. Montgomery

Heats of solution of yttrium chloride and oxide in hydrochloric acid were measured by Bureau of Mines researchers. Using the heat of combustion of yttrium mentioned in the literature, the Bureau calculated the heat of formation of yttrium chloride to be -239.16 + 0.50 kcal./mole. The Bureau experiments gave evidence that the heats of solution of yttrium chloride from the literature are mostly too low because of water and/or oxychloride impurities. Heat of combustion of yttrium (8)3/ and its heat of solution in hydrochloric acid (2, 14) have been measured. The earlier heat of solution measurement (2) is unreliable because of possible potassium contamination (4). Heat of solution of yttrium chloride has been measured by three researchers (3, 9, 15), who obtained widely different results. Spedding and Flynn (14) report the heat of formation of yttrium chloride as -232.69 kcal./mole from their solution studies. The present work was designed to check the reported heats of solution of yttrium chloride and to determine the heat of solution of yttrium oxide. The latter measurement would allow the results of solution and combustion data for yttrium to be intercompared.

Jan 1, 1960

By J. H. Field

Results of studies by the Federal Bureau of Mines on a pilot-plant scale for removing hydrogen sulfide and carbonyl sulfide from gas mixtures by the hot carbonate system are given in this publication. Gases containing up to 10 pet. hydrogen sulfide and 48 grains carbonyl sulfide per 100 cu.ft. were treated. In most tests carbon dioxide also was present and was removed simultaneously with the sulfur compounds. Because the rate of absorption of hydrogen sulfide is much more rapid than that of carbon dioxide over a wide temperature range, selective removal of hydrogen sulfide occurred in the bottom section of the absorber near the point of gas entry. Hydrogen sulfide was removed to pipeline specifications with carbonate solutions by using split-stream flows in the absorber and regenerator.

Jan 1, 1960

By T. A. Henrie

The Federal Bureau of Mines has investigated methods of sodium reduction of titanium chlorides to produce high purity titanium metal (14).4/ This investigation was made to obtain a better understanding of the reactions involved in sodium reduction of titanium chlorides and was part of the Bureau's activities toward improving the technology of titanium. Theoretical and experimental evidence show that sodium reduction of titanium tetrachloride occurs by stepwise reactions. The first stage reduction between sodium vapor and vapors of titanium chlorides produces titanium di-and trichlorides which subsequently condense with sodium chloride to form a salt mixture. The second stage reduction takes place in the condensed salt mixture between sodium and titanium subchlorides. Final reduction is a heterogeneous reaction between two separate phases, the a phase which consisted of sodium dissolved in sodium chloride and the ß phase titanium subchlorides dissolved in sodium chloride. The mechanism of the heterogeneous reaction between these phases is electrochemical in nature. The model proposed is a galvanic reaction at the interfacial region.

Jan 1, 1960