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By R. B. Anderson

SULFUR poisoning of iron catalysts in the Fischer-Tropsch synthesis was investigated at the Bureau of Mines, because synthesis gas produced from coal contains sulfur compounds. Tests of two typical iron catalysts with synthesis gas containing known concentrations of H2S were made to determine catalyst life as a function of sulfur concentration to ascertain the type of gas purification required. Fixed beds of activated steel turnings and a fused iron oxide catalyst were investigated in sulfur poisoning tests at 21.4 atmospheres with IH2+100 gas containing 6.9, 23, or 69 mg S as H2S per cubic meter (0.3, 1.0, and 3.0 gr per 100 cu. ft.). In tests of reduced catalysts at constant temperatures, more than 80 percent of the activity was lost when 0.5 mg S/g Fe was introduced. Poisoning of nitrided or carbided fused iron oxide catalysts to a given extent required more than twice as much sulfur than for the corresponding reduced catalyst. When the synthesis temperature was increased to compensate for loss in activity, tests of the fused iron oxide catalysts at constant productivity could be continued for 19 to 98 days. The tests were terminated by clogging of the reactor, presumably caused by carbon deposition. One objective of the present work was to determine if synthesis gas, purified by the Bureau of Mines' hot-potassium carbonate process for removing H2S, OOS, and CO2, is suitable for synthesis on iron catalysts. The sulfur content of the gas purified by tills process is in the range of concentrations used in the present work. In constant-productivity tests of nitrided fused iron oxide catalysts with synthesis gas containing 6.9 mg S/m3, catalyst lives are nearly long enough for serious consideration of tills mode of operation. However, factors relating to selectivity and stability of the catalyst indicate that this type of operation is impractical for a commercial process. On this basis additional gas purification, such as iron oxide boxes following a hot potassium carbonate scrubber, is desirable.

Jan 1, 1965

By Heinz W. Sternberg

A method for the electrochemical reduction of the benzene ring was developed and applied to the electrochemical reduction of coal. Successive electrochemical reductions of a vitrain from low-volatile bituminous coal in ethylenediamine saturated with lithium chloride resulted in the addition of 53 hydrogens per 100 carbon atoms. Ultimate analyses and pyridine solubility of the vitrain recovered after each reduction showed that hydrogen added at the beginning has a much greater effect on solubility than hydrogen added at a later stage. Surprisingly, the removal of sulfur from the vitrain takes place only after the more reactive aromatic rings are reduced. Nuclear magnetic resonance analysis and average molecular weight determination of the extracts of the reduced vitrain samples, representing about 18 percent of the vitrain, showed that these fractions had 95 percent of their hydrogen content on saturated carbon atoms and an average molecular weight of 800 to 900. A study of the effect of operating variables on current efficiency showed that current efficiency is highest with aluminum as cathode material and with lithium chloride as electrolyte. A substantial increase in current efficiency of difficulty reducible olefinic double bonds was achieved by adding a proton donor. This result is significant in connection with the electrochemical reduction of coal which proceeds from readily reducible aromatic double bonds to difficultly reducible isolated double bonds. It is proposed that reduction is achieved by electrolytically generated and subsequently solvated electrons and hence does not require prior adsorption of the substrate at the electrode surface. This offers a distinct advantage for electrolytic reduction of sparingly or insoluble substrates such as coal.

Jan 1, 1967

By R. D. Brown

This Bureau of Mines report describes a new methodology for identifying and sorting scrap metals using two modern portable instruments: a thermoelectric sorter and a hand-held emission spectroscope. The method, tested on a 27-sample stainless steel and superalloy array, makes it possible to group and/or identify a typical mixture of high-value metal scrap in two or three steps, whereas as many as seven or eight steps are needed to perform the same separations using chemical spot tests. A portable fluorescent X-ray analyzer identified 19 of the 27 alloys in the sample array by name or type; these alloys are included in the microprocessor memory. The remaining alloys were identified by using the analyzer in its elemental analysis mode and comparing the results wit.h alloy specification chemistry.

Jan 1, 1984

By W. R. Hardwick

This information circular describes mining methods and practices at New Cornelia Branch, Phelps Dodge Corp., Ajo, Ariz. It is one of a series being prepared by the Bureau of Mines on mining methods, practices, and costs in various mining districts of the United States. The New Cornelia mine (fig. 1) is at Ajo, a town in southwestern Arizona (fig. 2) on Arizona State Highway 85 in the western part of Pima County. The [oncentrator] and smelter are near the mine (fig. 3). Copper ore is mined, crushed, ground, and concentrated, and the concentrates are smelted. Copper is cast in anode form and sent to the Phelps Dodge Corp. refinery in El Paso, Tex.

Jan 1, 1960

By James P. Bennett

The Bureau of Mines is investigating the acid resistance of ceramic materials to identify construction materials for emerging technology in chemical and metallurgical processes. Eight commercial ceramic materials, were evaluated: two red shale, two fireclay, one silicon carbide, one silica, one carbon, and one high-alumina. Samples were exposed to 10 wt pct H2S04 at 50° C and 10, 30, 50, 70, and 90 wt pct H2S04 at 90° C for time periods of 110 days. Statistically significant changes in cold crushing strength were observed in the silicon carbide and car-bon materials. Weight changes and the leach rate of Al, Ca. Fe. K, Mg, Na. Si, and Ti were also monitored. The most severe corrosion conditions were at 90° C and 30 to 50 wt pct H2S04 for the acidproof and at 10 wt pct H2S04 for the acid-resistant materials. The silica and the high-alumina materials were the most acid-resistant, followed by the higher density red shale and fireclay.

Jan 1, 1986

By M. G. Zabetakis

At ordinary temperatures and pressures methyl ethyl ketone (MEK)-air mixtures containing between 2.0 and 11 vol.-pct. MEK and methyl isobutyl ketone (MIBK)-air mixtures containing between 1.5 and 7.5 vol.-pct. MIBK are flammable. However, MEK-bromochloromethane (BCM)-air mixtures containing at least 6.2 vol.-pct. BCM and MIBK-BCM-air mixtures containing at least 7.0 vol.-pct. BCM are nonflammable. Also, MEK-BCM-air and MIBK-BCM-air mixtures containing less than 18.7 vol.-pct. oxygen are nonflammable. To assure the formation of nonflammable mixtures when mixed with air, MEK-BCM vapor mixtures must contain at least 1.6 vol. BCM per volume MEK, and MIBK-BCM vapor mixtures must contain at least 2.8 vol. BCM per volume of MIBK; these quantities of BCM would be produced by liquid mixtures containing 55 vol.-pct. BCM in the first case and 60 vol.-pct. in the second. An MIBK-BCM-trimethylene chlorobromide mixture containing equal volumes of each liquid forms nonflammable mixtures with air at ordinary temperatures and pressures. The same is true of a liquid mixture containing 34.6 pct. (liquid volume) BCM, 34.b pct. perchloroethylene, 15.4 pct. MIBK, 7.7 pct. toluene, 3.85 pct. ethyl amyl ketone, and 3.85 pct. trimethylene bromide.

Jan 1, 1960

By H. W. Kilau

The Bureau of Mines evaluated synthetic fluorspars as substitutes for natural fluorspar in basic oxygen steelmaking using a high-temperature rotational viscometer and a quarter-ton basic oxygen furnace (BOF). Consider-able variation in stability and BOF slag fluidizing properties were found when using the initial synthetic products, but improved synthesis methods produced synthetic fluorspars that were generally comparable to natural fluorspar in laboratory testing. Trials in the furnace showed the synthetic products to be operationally the equivalent of natural fluorspar. Higher sulfur and phosphorus contents in some of the synthetic materials did not adversely affect the steel chemistry. Analyses of wet scrubber samples showed evidence that the pelletized synthetic fluorspars experienced greater physical and chemical disintegration than did natural fluorspar. It was also found that operation of a BOF without fluorspar is possible when making low-carbon steels because iron oxide is intrinsically generated as the slag fluidizer.

Jan 1, 1981

By Joan C. Biordi

A molecular beam-mass spectrometer-low pressure flat flame apparatus has been constructed for the purpose of examining the chemical microstructure of normal methane-oxygen-argon flames and those inhibited with Halon extinguishants. Details of construction and performance of this apparatus and of related flame temperature measurements are given. Particular attention is paid to the empirical characterization of the perturbation to the flame caused by the sampling probes. The composition profiles obtained for normal flames are compared to those of flames inhibited by CF3Br. In addition to the usual stable species (CH4, O2, CO, CO2, H2O, H2, and H2CO), the inhibitor, its products and intermediates associated with its reactions could be followed. In particular, hydrogen bromide, bromine atoms, hydrogen fluoride, and carbonyl fluoride were observed. The relatively rapid disappearance of inhibitor and early appearance of fluorinated reaction products suggest a short lifetime for the CF3 radical in this system. Observation of COF2 suggests that CF3Br is effective as an inhibitor, at least in part, by virtue of its interference with the oxygen containing species of the normal chain reaction. Profiles of the 17+ peak at low electron energy suggests that the hydroxyl radical may also be sampled, but the profiles obtained are not yet sufficiently accurate to determine the effect of inhibitor on this important flame radical.

Jan 1, 1973

By M. L. Glenn

The Bureau of Mines is conducting research on substitutes for chromium-containing alloys in order to conserve imported critical and strategic materials. Part of this research concentrates on finding low-chromium substitutes for heat-resisting stainless steels for the temperature range 600° to 800° C. Ferritic alloys are emphasized that have oxidation resistance provided by chromium contents as low as 10 pct and stress rupture strength provided by the precipitation of the chi(X)-phase intermetallic compound, (Fe36Cr12 (Mo, Ti)10). Initially, research was concentrated on selecting an alloy composition having a minimum chromium content with strengthening provided by the X-phase. An Fe-(10-12 pct)Cr-6 pct Mo-(1.5-2.0 pct)Ti alloy was selected. After the alloy selection, the tensile, stress rupture, and oxidation properties were determined. Stress rupture properties were found to be similar to those of 304 stainless steel. However, the alloys possessed brittleness during both stress rupture and tensile testing, possibly as a result of too high a content of molybdenum and titanium. Higher than expected oxidation rates were found that may be caused by the high molybdenum content.

Jan 1, 1984

By Irving Hartmann, John Nagy, Donald Mitchell

"SUMMARY AND CONCLUSIONThe test data indicate that water infusion of the Pittsburgh coal seam does not reduce the amount of fine dust produced during mining operations to the extent reported elsewhere. Wide variations in the amounts of dust collected in the air current were noted in duplicate samples and repetitive tests. Changes in depth and location of the infusion holes and amount of water injected and addition of a wetting agent to the water had little effect on the amount of dust liberated.Water was forced readily into the coal. Some water flowed out along the cleats, but an appreciable amount remained in the seam. Little or no water pene¬trated the coal seam above the upper infusion holes.The average dust concentration (with and without infusion) in the return air, 40 feet outby the working face, was 25 million particles per cubic foot during undercutting, 20 million during drilling, 75 million during shot firing, and 20 million during hand loading. At the working face the average concentration was 3 to 6 times higher. The concentrations were measured at an airflow of 1,600 cubic feet per minute (c.f.m.) at the face.On the basis of this short investigation, no final conclusions can be made on the effectiveness of water infusion in reducing the amount of fine dust liberated during mining in the Pittsburgh coal seam. However, the data indicate that dust reduction resulting from infusion would be small.INTRODUCTIONThe production of fine coal dust is an inherent part of nearly every phase of mining. The use of large, high-speed continuous-mining machines and other mechanical equipment has increased dust production. In addition, in coal seams that have been subjected to high pressures for a long period, and particularly in dry and friable seams, some very fine dust is in the seam before mining. Much effort has been devoted to allaying and collecting at its source the fine coal dust released during mining. One of the comparatively recent techniques that has been developed for this purpose is infusion of water or other liquids into the coal seam. This method consists of injecting water under pressure into a coal seam to neutralize the fine dust released during mining. The water generally is introduced through bore holes in the face before undercutting."

Jul 1, 1957

This publication summarizes, for potential contractors and other interested parties, the research, development, and demonstration contract projects programed by the Bureau of Mines for fiscal year 1980 (October 1, 1979 - September 30, 1980) under its Minerals Health and Safety Research program. The objective of these projects is to provide an ordered and sequenced series of advances toward the Bureau's overall goal of providing the system technology required to create a healthier and safer working environment for the Nation's mining and minerals processing workers.

Jan 1, 1980

By Frank J. Perzak

This report describes a U.S. Bureau of Mines study on the hazards of large-scale conveyor belt fires in underground coal mines, as a function of both air velocity and distance from belt surface to gallery roof. The fire hazards considered were smoke obscuration, toxic effects of carbon monoxide (CO), and elevated air temperatures downstream of the fire. All of these hazards scale with the ratio of fire intensity to ventilation airflow. These hazards were all found to be greater at the lower belt-to-roof distance, owing to the greater fire intensities that resulted. The hazards of smoke obscuration and elevated CO levels were greater at lower air velocities. Smoke obscuration was found to be the earliest hazard, reaching critical levels before the stage of belt flame spread. Critical levels of CO and downstream air temperatures were not reached until the later stages of flame spread. Fire growth rates during rapid flame spread were much greater than rates measured during the early stages of belt burning. Data were analyzed to determine the early-warning capability of fire sensors. Smoke sensors provided the earliest warning, followed closely by CO sensors. Thermal sensors did not exhibit any early warning capability.

Jan 1, 2010

By Gary L. Hundley

The Bureau of Mines has devised a procedure to recover chromium chemicals from low-grade domestic chromites, which contain silicon and aluminum impurity levels that are too high to permit processing by present industrial processes. The Bureau procedure consists of reacting chromite with molten sodium hydroxide (NaOH) under oxidizing conditions to form sodium chromate (Na2Cr04). The reaction product is leached with methanol to remove the majority of the unreacted sodium hydroxide, then with water to remove the sodium chromate and the remainder of the sodium hydroxide. The sodium chromate product is recovered by evaporative crystallization from the aqueous solution. This report presents results of laboratory tests to determine the optimum fusion conditions and the chromium extractions obtained from several domestic chrotdte concentrates. These concentrates are from a variety of sources, including the Stillwater Complex in Montana, Kanuti River-Caribou Mountain, Red Bluff Bay, Kenai Peninsula, and Kodiak Island areas in Alaska, deposits in northern California, and a nickel-cobalt laterite from southern Oregon. All of these concentrates were successfully treated by the Bureau procedure. The best chromium extrac-tions obtained for each of these materials ranged from 69.5 to 98.9 pet.

Jan 1, 1985

7133. Clewell, D. H. The Gravimeter. Prec. and Trans. Texas Acad. Science 1941, Austin, Tex., vol. 25, 1942, pp. 86-88. Static gravimeters, unastatized and. astatized, are considered to be the most practical for oil exploration. One gravimeter is described using a beam whose moment about a pivotal axis is elastically balanced. Magnetic or electric fields are deemed unsatisfactory for balancing gravitational force because they cannot easily be kept constant. The gravimeter described is capable of detecting a change in altitude of 3 inches and a change in latitude of about 150 feet. V. S.

Jan 1, 1944

By L. S. Harner

This paper which describes the milling practice at the Golden Cycle mill is one of a series of similar papers being prepared by the United States Bureau of Mines. The mill of the Golden Cycle Corporation, formerly known as the Golden Cycle Mining and Reduction Co., is located at Colorado Springs, Colorado, and has been operated since 1907. It is now and has been from its inception almost exclusively a custom mill.

Jan 1, 1933

By R. B. Tippin

To study continuous operation of the heavy liquid separation (HLS) of minerals, the Bureau of Mines concentrated spodumene from a typical ore. The studies included heavy liquid concentration, removal of the heavy liquid from the mineral products, and recovery of the heavy liquid for reuse. The research program examined the influence of feed moisture, steam consumption, stripping time, and condition of steam. Operation of multiple cyclones in series resulted in spodumene concentrates assaying 92 to 95 percent spodumene and indicated mineral recoveries of 86 to 89 percent. Continuous filtration and steam stripping produced mineral products containing less than I pound of heavy liquid tetrabromoethane (TBE) per ton of material. Problems unique to this process are discussed, including heavy liquid properties and viscosity, toxicity, material handling hazards, and safety precautions.

Jan 1, 1970

By W. F. Faragher, W. A. HORNE

Previous interrogation of German scientific personnel by numerous in- vestigators and the examination of evacuated documents indicated that fur- ther information was desirable on a miscellany of products and processes of interest to the Petroleum Industry. Accordingly, Dr. Pier and a large number of other men of the I.G. Farbenindustrie, A.G. plant at Ludwigshafen/ Oppau were further interrogated in July-1945. The information contained in this report supplements that previously reported in the CIOS report of 16 August, 1945: "Report on Investigations by Fuels and Lubricants Teams at the I. G. Farbenindustrie A.G. works at Ludwigshafen and Oppau", edited by Lt. Col. R. Holroyd, (FP).

Aug 1, 1943

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 H. F. Yancey

Although a general relationship exists between the two criteria used to measure sharpness of separation -error area and probable error -they sometimes give quite different appraisals of a particular washing operation. Error area takes into account how the entire raw coal was treated, whereas probable error reflects only how the material of intermediate density was separated, ignoring completely the recovery of clean coal and the rejection of heavy impurity. Error area is thus more reliable for general use. In heavy-medium cleaning, sharpness of separation decreases with increase in separating density, but ordinarily the change is not great enough to affect the yield and ash content of washed coal measurably. Therefore, distribution curves for heavy-medium units can be transposed from one separating density to another, at least in the range of separating densities ordinarily used in the United States.

Jan 1, 1955

By Kenneth G. Broadhead

The objective of this rare-earth oxalate study by the Bureau of Mines was to determine systematically by radiochemical techniques what effects, if any, could be attributed to the several variables--temperature, digestion time, acid concentration, rare-earth concentration, oxalic acid concentration, stirring, and the presence of other rare-earth ions. A Latin Square experimental design was used to evaluate statistically some of the variables. Precipitation losses ranged from near zero to about 7 percent, and mineral acid and rare-earth concentration were the predominant factors affecting completeness of precipitation. Quantitative oxalate precipitation of the rare-earth elements was achieved by controlling the experimental conditions as follows: (1) Maintaining rare-earth concentrations above 0.01M; (2) stirring the mixture several minutes after precipitation; (3) using an adequate (two to five-fold) excess of oxalic acid; (4) precipitating at room or iced temperature and digesting for at least 1 hour; (5) avoiding an excess of mineral acid and, if possible, maintaining the pH above 2.0; and (6) avoiding excess complexing agents such as EDTA (ethylenediaminetetraacetic acid). In the past 20 years research aimed at developing more efficient separation and purification techniques applicable to the rare-earth elements and yttrium has been extensive. Common to most of these procedures has been the use of oxalic acid to precipitate this group of elements selectively. However, this particular use of oxalic acid has a much earlier origin; its application in precipitating yttrium was first reported by Mosander (8)4 in 1843. Despite long and popular employment of this technique, only limited and somewhat conflicting data are available regarding the many factors affecting the degree of rare-earth oxalate precipitations.

Jan 1, 1961