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By Gene Asai

Properties obtained for columbium carbide-carbon castings ranging in car-bon content from 12 to 17 weight-percent were compared with those of hot-pressed composites of similar composition. The properties were oxidation resistance in static air between 500° and 700° C, linear thermal expansion between 20° and 2,400° C, electrical resistivity between 20° and 1,500° C; microhardness between 20° and 1,500° C, and modulus of rupture between 1,300° and 1,800° C. CbC-C castings differed markedly from hot-pressed material with respect to microstructure, electrical resistivity, and modulus of rupture, but behaved quite similarly with respect to oxidation resistance, thermal expansion, and hot hardness. In oxidation resistance, thermal expansion, and hot hardness both materials were independent of carbon content. Both castings and hot-pressed composites oxidize rapidly in air above 600° C, have thermal expansion coefficients very similar to columbium metal, and the logarithm of the hardness decreases linearly with increasing temperature. The microstructures of hot-pressed composites contained varying amounts of graphite in a CbC matrix but did not contain significant amounts of a eutectic structure present in all castings, nor did they contain graphite needles which were present in the hypereutectic castings. The higher electrical resistivity of hypereutectic castings over hypereutectic hot pressings was attributed to the presence of highly oriented graphite needles in the castings. The modulus of rupture of castings was 1-1/2 to 2 times that of hot-pressed composites. Both materials displayed bend ductility above 1,800° C.

Jan 1, 1971

By A. G. Starliper

Research was conducted by the Bureau of Mines to determine feasible roasting methods for the removal and the recovery of germanium, cadmium, and lead as enriched fractions from sphalerite concentrates. The two types of roasting processes studied were: (1) Batch, with a stationary bed, and (2) continuous, with a suspended bed, Results indicated that either method gave satisfactory metallurgical recoveries} but the continuous process is recommended because of inherent advantages. Final products were enriched fractions that could be treated by conventional methods for production of metallic germanium, cadmium, and lead. In the batch process, the concentrates were placed in a large tube furnace and heated at 1,080° C, an average of 3 hours. During the heating period, inert, reducing} or sulfur-laden gases were passed over the stationary charge to convey the sublimed metal sulfides from the hot portion of the tube to a lower temperature condensing zone at the end of the tube, where the metal sulfides were collected on baffles and recovered. In the batch and fluidizing roasting processes alike, the gases passed over or through the charge and served only as carriers for the sublimates and as suspension media in fluidization roasting. Since both processes depended on the volatilization, at relatively high vapor pressures, of the sulfides of germanium, cadmium, and lead, it was imperative that very little oxygen come in contact with the charge to alter the sulfide minerals. Germanium has a high affinity for oxygen, but in this instance it was buffered by being in solid solution in zinc sulfide.

Jan 1, 1961

By A. V. Hooker, E. J. Coggeshall

"The Bureau of Mines for some time advocated the firing of all blasts in coal mines as single shots, and this method of firing is the general practice in American bituminous-coal mines. All single shots can be fired with permissible single-shot units so designed that they will not ignite mixtures of methane and air.If several shots in a face are fired singly it is necessary to return the face after each shot. In some mines having steeply pitching coal seams, this may be dangerous or even impossible, under these conditions shots are usually fired simultaneously.Several shots cannot be fixed simultaneously with permissible single-shot blasting units, and safe types of multiple shots blasters are not readily available. This means that the firing of multiple shots in gassy mines is usually accompanied by the possibility of gas ignition as the blast occurs.Tests have been made at the Pittsburgh Experiment Station to determine the possibility of developing safe types of multiple-shot units suitable for such use, or of applying other type safely in gassy sections of mines where firing shots singly is impracticable.The tests may be divided into the following four groups:1. Tests to demonstrate hazard in the use of existing types of multiple-shot units of the portable generator type.2. Tests to show the electrical characteristics of multiple-shot generator units relative to the possibility of preventing igniting sparks and of modifying the design and application of such units in furthering safety."

Mar 1, 1935

By B. W. Gandrud

[The Bureau of Mines is conducting an extensive investigation of coal preparation in the Alabama coal fields in cooperation with the University of Alabama coal-mine operators. In this investigation the drainage characteristics of typical coals from the Warrior and Cahaba fields were studied]

Jan 1, 1941

By Árpád B. Palotás, Adel F. Sarofim, John B. Vander Sande, Paolo Ciambelli, Lenore Rainey

"The evolution during oxidation of the internal structure of soot and carbon black particles was studied using high-resolution transmission electron microscopy (HRTEM) and an image analysis system. Increasing ordering to the carbon structure with increasing oxidation is observed. Measures of the increased order are increases in the fractional coverage of a cross section of the particles with a layered structure, a decrease in the mean interlayer spacing, and a decrease in the spread of the interlayer spacing. The changing structure of the carbon black impacts its properties, such as the rate of oxidation.There is considerable interest in the study of the structural changes of carbonaceous materials as a function of oxidation. Davis et al.1 measured the variation of carbon dioxide surface area of various coals as a function of residence time in a flow reactor. HRTEM measurements revealed that crystallite dimensions and interlayer spacings are altered by combustion. Ishiguro et al.2 showed that oxidation alters the structure of diesel soot. The aim of our current research is to develop a better understanding of the microstructural reordering of carbon blacks with implications to their properties. The carbon blacks used in this research have already been studied and their reactivities as a function of oxidation measured.3The methodology used in this work has already been described in detail elsewhere.4 This paper presents an application to quantify the structural changes of carbon black particles as a function of oxidation and graphitization. The technique used is based on the use of HRTEM (high-resolution transmission electron microscopy) and computational image analysis.It is well-known that carbonaceous materials like graphite, soots, coals, chars, etc., possess characteristic structural appearances which can vary from mostly random or amorphous to a perfectly ordered graphitic crystalline structure. The carbon structure has been variously described as turbostratic5 or as crumpled sheets6 to indicate that parallel layering, reminiscent of graphite, is observed over dimensions of nanometers but that these planes or crystallites show disorder over larger scales. The degree of order of such structures is strongly dependent on the thermal treatment of the material as well as the composition of the source of the carbonaceous material. The value of electron micros¬copy in studying the morphology of such materials has been well established,2,7,8 although only a few attempts toward quantification have been made.The sample observed was carbon black CB330 from De¬gussa. One set of carbon black samples were oxidized in a thermo-gravimetric analyzer (TGA) in air at 575 0C, so that the conversion varied from 0 to 96%. Another set of carbon black samples were graphitized (Graphpac-GB by ALLTECH) and then oxidized in the TGA at 680 °C until 92% burnout was reached. The latter samples are called GB 0% and GB 92%, respectively.For the HRTEM observation a small portion of each sample was ultrasonically dispersed in ethanol. The suspension was deposited dropwise on a copper TEM grid coated with a lacey carbon film. The examination of the samples was carried out on areas that extend over the holes in the supporting film in order to avoid interference from the amorphous carbon background film An oriented gold crystal was used as a calibration standard and subjected to the same techniques as the carbon black samples."

Jan 1, 1998

By E. R. Maize, R. D. Currie

"Good ventilation is one of the first requisites in the safe and efficient operation of a coal mine. If a mine is gassy, the uninterrupted circulation of an adequate supply of fresh air is imperative if that mine is to operate with a relative degree of safety. That ventilation is not •only a safety consideration, but is an extremely important economic factor is shown by the fact that in many mines 50 per cent of the total power cost is for ventilation.The system used in the Graceton Coal & Coke Co. mine, Graceton, Pa., is believed to be unusual in many ways. Its application in this mine has re¬sulted in good ventilation of the working faces, no interruption to the venti¬lating current through the use of doors. a large- portion of the air circulated by the fan reaching the working places, low velocity air currents on traveling and haulage ways, low water gage and power consumption of the fan, and well-ventilated gob areas.This investigation was made possible through the courtesy of W. H. Robertson, mine superintendent. Fred Roberts, mining engineer, and Floyd Phillippi, mine foreman, assisted in the collection of information.The Graceton mine is a slope, opening the Upper Freeport or E bed, on the Pennsylvania Railroad about midway between Blairsville and Indiana at Graceton, Indiana County, Pa. The production is approximately 1,000 tons of coal per day and about 170 men are employed underground. The mine is considered gassy and was found to be liberating approximately 300,000 cubic feet of methane in 24 hours. The return airways terminate at a circular, concrete lined shaft 12 feet in diameter and about 115 feet deep at which is the exhaust fan.Mining is done by a block system with flat or level entries turned off the main slope at intervals of 1,350 feet, off which the butt headings are turned up the grade parallel to the slope. Rooms, which are about 225 feet long and 12 feet wide, are turned off the butt headings on 80-foot centers, leaving a block about 68 feet thick between rooms.Haulage on the main slope is by rope, with the hoist on the surface. This hoist is electrically driven through a 500-h.p., 2,300-volt motor. The rope used in this haulage is 1-1/8 inches in diameter. There are five electric trolley locomotives - one 10-ton and four 6-ton - which do all of the hauling in the flat and butt entries.Before it is blasted all of the solid coal and as much of the pillar coal as can be cut with safety is undercut by permissible mining machines. Shooting is done by shot firers who use permissible explosives, electric detonators, and dry-cell, nonpermissible batteries.In rooms where conditions are normal, timbering consists of two rows of posts on 4-foot centers. Posts are required to be within 6 feet of the face in machine-cut places and within 3 feet of the face in hand-mined places. Timbering on entries, where required, is of two types: a bar hitched into the ribs and supported by the coal, or 3-piece sets. The legs of the 3- piece sets used on the slope are set well back into the rib to prevent their being. knocked out by a wreck."

May 1, 1932

By R. Karl Zipf, Christopher Mark

Highwall mining continues to grow in importance as a coal production method from U.S. surface mines. It may account for as much as 4% of the total U.S. coal production, according to one recent estimate. Analysis of Mine Safety and Health Administration (MSHA) accident and injury statistics shows that, overall, highwall mining has maintained an admirable safety record. Its fatality and injury rates are comparable to those for other surface mining methods, and are significantly lower than those for underground mining. No mining method is risk free, however. Highwall mining injuries have been associated with handling materials, slips and falls, machinery, powered haulage, and other types of incidents. But perhaps the greatest risk, to both personnel and equipment, is from ground control. The two most significant ground control hazards are rock falls from the highwall and equipment entrapment underground. Highwall Stability Ensuring highwall stability through proper ground control engineering is of paramount importance to safe highwall mining operations. The only fatality to occur during the last five years at a highwall mining operation was due to highwall collapse. There have also been numerous near-misses, several of which have involved extensive damage to equipment. In the central Appalachians, where the majority of highwall mining occurs in the U.S., hillseams are the most prominent geologic structures that affect highwall stability. Hillseams (or mountain cracks) are near vertical fractures in the rock that are formed in response to natural weathering and erosion of hillsides. They extend hundreds of feet down from the surface. They typically run parallel to the hillside, but they can also extend across narrow points or ridge lines. The hazard arises when rock slabs that form along the hillseams detach and fall away from the highwall face (See Figure 1). [ ] Unfortunately, it is impossible to control the location of hillseams or reliably detect their presence within a highwall. There are, however, a number of measures that can be taken to minimize the risk of failure associated with hillseams: Planning-Most operators choose to skip those areas of the highwall where a prominent hillseam daylights (See Figure 2). Existence of such areas is known for several weeks in advance of highwall mining; therefore, planning engineers can adjust the layout of highwall mining panels to locate barrier pillars within areas of questionable highwall stability. [ ] Inspection and monitoring-Daily inspection of the benches above the active highwall mining area is a prudent precautionary measure. A crack in a bench immediately above a highwall miner is shown in Figure 3. Simple displacement monitors may be useful for detecting movement along cracks that may precede a significant life-threatening failure. New tools, such as slope monitoring radar, may also prove useful in detecting motion of the rock slopes above active highwall mining operations. Good blasting practice-Most surface coal miners in the central Appalachians use pre-splitting and the familiar halfbarrels are routinely seen throughout the pits. Shorter delays along the face and longer delays between rows can direct more of the blast force parallel to the face, potentially doing less damage to the wall rock. In addition to pre-splitting, decreasing the burden, spacing and charge weight in drill holes close to the highwall will also decrease damage to the wall rock. Decreasing the highwall slope angle-Decreasing the highwall slope angle from 90° (vertical) to 70°-80°, especially in areas of known hillseam concentration, could eliminate the hillseam hazard (See Figure 4). Angled highwalls are routinely employed in many Midwestern surface mines and in some

Four actual coal mine waters were used in various phases of the research program. All were from the Sewickley Creek area In Westmoreland County, Pennsylvania. The BCR designations, site locations, and nature of the mine water samples are described briefly in the following paragraphs.

Jan 1, 1971

By D. B. Taliaferro

Information regarding the pores or voids in reservoir rocks is vitally important in the scientific extraction of petroleum from natural underground reservoirs, and petroleum technologists concerned, with subsurface, conditions have devised various methods that give reasonably accurate information as to the porosities of oil and gas-bearing sands.5/ In this, work, several investigators have made use of the experience of the ceramic and other industries. The method of determining the effective porosity of oil sands described in this report falls within the general classification of gas-expansion methods. It was devised and developed at the United States Bureau of Mines Petroleum Experiment Station, Bartlesville, Okla., as a part of the research dealing with fluid and energy relations in reservoirs and improved oil-recovery methods. The apparatus and procedure are well adapted to the requirements of the Bureau, and the following detailed description has been prepared so that others may make use of the information. A tabulation at the end of the report gives the results of several hundred porosity determinations for oil sands in fields of 11 States.

Jan 1, 1937

By D. B. Taliaferro

Information regarding the pores or voids in reservoir rocks is vitally important in the scientific extraction of petroleum from natural underground reservoirs, and petroleum technologists concerned. with subsurface conditions have devised various methods that give reasonably accurate information as to the porosities of oil and gas-bearing sands.5/ In this work, several investigators have made use of the experience of the ceramic and other industries. The method of determining the effective porosity of oil sands described in this report falls within the general classification of gas-expansion methods. It was devised and developed at the United States Bureau of Mines Petroleum Experiment Station, Bartlesville, Okla., as a part of the research dealing with fluid and energy relations in reservoirs and improved oil-recovery methods. The apparatus and procedure are well adapted to the requirements of the Bureau, and the following detailed description has been prepared so that others may make use of the information. A tabulation at the end of the report gives the results of several hundred porosity determinations for oil sands in fields of 11 States.

Jan 1, 1937

By Richard A. Allwes

The Bureau of Mines conducted an in-mine case study on two consecutive three-entry gate road systems designed in accordance with the stiff-yield pillar design concept. This Bureau study was conducted in order to further develop technology that will improve the health and safety aspects of longwall mining. Support loading and strata activity were monitored to determine the effects of retreat longwall mining on the gate road ground control system. Analyses of pillar stress and roof bolt loading histories revealed that headgate roof support elements ex-perienced cumulative loading throughout the life of the longwall panel. Tailgate pillar loadings had significantly different histories from the loading histories of the headgate pillars. Stress relief occurred in the tailgate pillars following the passage of the longwall face. More-over, the stiff-yield pillar design, with the abutment pillar placed adjacent to the working panel when part of the headgate system, provided effective ground control in that no major roof falls or roof problems were experienced in the headgate or tailgate systems during longwall mining.

Jan 1, 1985

By Albert L. Toenges, Henry E. Dekay, James N. Scudder

Support of the immediate roof in coal mines is essential for their safe operation, and timbers are the most common means of support. Their effectiveness depends upon their resistance to decay. The theory has been advanced by some mine operators that rock dust, which is applied to ccal-mine workings to prevent propagation of explosions, accelerates the decay of mine timbers. As the results of part 1 of this study were inconclusive, the study was continued. Its principal objectives are: 1. To determine the effect of rock dusting upon decay of mine timber. 2. To compare the extent of decay of timbers in two mines in which underground conditions are similar. 3. To determine the loss in strength of the timbers after exposure to mine atmosphere. The studies were carried on in the Crucible mine of the Crucible Fuel Co. where the first part of this study was made, and in the Isabella mine of the Weirton Coal Co. The mines are on the Monongehela River and are adjacent.

May 1, 1943

By Dorothy M. Richardson

The Bureau of Mines has participated in the American Petroleum Institute Research Project 48A (API-RP48A) program on the Separation and Identification of Sulfur Compounds in Crude Petroleum. The lack of reference compounds or infrared spectral data has made difficult the identification of individual sulfur compounds boiling above 140° C. The recent acquisition of 24 alkylthiophnnes has made possible a limited study of this important class of sulfur compounds. The infrared spectra of 2-monoalkylthiophenes and 2,5-dialkylthiophenes for the 2 to 15p range are reported. Correlations for determining the 2-alkyl and 2,5-dialkyl substituted thiophenes are derived from this information. The 2-alkylthiophenes show a unique pattern in the 5.50 to 6.54 region, while the 2,5-dialkylthiophenes show a distinctive pattern in the 5.6µ to 6.7µ region. A skeletal vibration occurs in the 9.5 to 10.0µ region for all of the thiophenes investigated. These data will aid the infrared spectroscopist in the identification of compounds of the type reported.

Jan 1, 1961

By Thomas M. Kohler, Gerald L. Finfinger, Gregory M. Molinda

The Bureau of Mines has completed an investigation of the effectiveness of methane drainage in the Lower Sunnyside Coalbed at Kaiser Steel Corp.'s Sunnyside No. 1 Mine in Utah. Most of the previous at- tempts to drain methane gas using long horizontal holes were conducted in the Eastern Coal Province. From the high degree of success realized in these efforts and the large body of knowledge gained from associated research, it seemed natural to extend the technology to western coalfields. Previous work had indicated that properties affecting gas drainage were variable in the Sunnyside Coalbed. In an attempt to characterize these properties, four degasification holes were drilled from the out- side entries of an advancing section. The holes were drilled to lengths of 780, 1,680, 1,315, and 1,047 ft and produced initial flow rates of 50,000, 180,000, 340,000, and 240,000 f t3/d, respectively. A total of over 300 million f t3 of commercial-quality gas has been removed from the Sunnyside Coalbed. The four holes have reduced face emissions by 78 pct.

Jan 1, 1986

By Sathit Tandanand

This report presents a Bureau of Mines study on the time-dependent behavior of coal measure rocks for future implementation in stability analysis and safety evaluation of in-mine rock structures. This initial study focused on moisture adsorption rate and strength degradation of shales in Pennsylvanian coal-bearing strata in the Illinois Basin. A reaction of clay minerals in Illinois shales with atmospheric water vapor was hypothesized as the adsorption and strength degradation mechanism. Part of energy exchange between shales and the environment was attributed to a free energy controlled by pore pressure of the rock and partial pressure in the environment. The relationships between adsorption versus time and strength degradation versus moisture content were derived and correlated with the experimental data. Partial saturation at various levels of relative humidity occurs within approximately 2 weeks at room temperature. The strength of shales tested decreases linearly with increasing moisture content. When the moisture exceeds 7 pct of the dry weight, these Illinois shales become unstable. To this end, the moisture content is a good predictor of rock strength for shales.

Jan 1, 1987

By F. W. Hoertel

The effects of certain process variables on the grain size, grain type, and microhardness of vapor-deposited tungsten were established, and the near-optimum parameters and the efficacy for the vapor deposition process were determined. No significant change in the grain size or microstructure resulted from ultrasonic vibration of the substrate during deposition, from variations in the hydrogen (H2) to tungsten hexafluoride (WF6) ratio, or from small increases in reaction-chamber pressure. Near-optimum conditions were continuous deposition at atmospheric pressure, a deposition rate of 2-mils thickness/square inch of substrate area/hour, a temperature of 5500 C, and a hydrogen to WF6 ratio of 4:1. The addition, individually, of about 2 volume-percent of butane, 24 volume-percent of carbon dioxide, or 4 volume-percent of propane to the hydrogen and WF6 mixture produced deposits with the finest grain size for each gas. A corresponding increase in microhardness accompanied the decrease in grain size. The addition of gases did not alter the columnar microstructure found in vapor-deposited tungsten.

Jan 1, 1966

By W. E. Anable

The Bureau of Mines studied the purification of commercially available yttrium by melting it in a 100-kw electron-beam furnace. Button-scale melts were made to determine the ultimate purification that could be attained by melting yttrium at 1,733° to 1,770° C at low pressure (0.05 to 0.1 micron) for 1 to 120 minutes. In addition, numerous melts were made to study the effect of doping yttrium with carbon, 17 selected metallic additions, and 3 compounds. Except for nickel and zirconium, the metallic impurities in yttrium were lowered significantly on extended treatment; silicon was lowered only slightly. The nonmetallic impurities} oxygen, nitrogen, and carbon, were not lowered except on short exposures. In isolated instances, the oxygen content was lowered from 5,860 ppm to about 5,000 ppm. In most instances the carbon con-tent was lowered from 545 to about 220 ppm in 20 minutes and then increased again. It was concluded that yttrium cannot be purified by direct heating or by the doping technique employed.

Jan 1, 1965

By R. W. Lewis

The Federal Bureau of Mines Boulder City Metallurgy Research Laboratory conducted experiments in order to develop a spectrochemical method for determining the concentrations of impurities In high-purity tungsten. This report presents a procedure, developed by these experiments, for determining 19 impurities in high-purity tungsten. Metal samples were thermally converted to the oxide, mixed with graphite, which was prepared and mixed with an internal-standard element, and excited in a d.c. arc. Sixteen of the impurity elements were determined with one set of conditions, using germanium as an internal standard. Lanthanum was used as an internal standard in the tests for boron and chromium. Molybdenum required the substitution of sodium chloride for the graphite and the use of copper electrodes. Data on the precision of the method are included in this report. The coefficients of variation vary considerably but average about 15 percent. Higher concentrations of impurities than those investigated may be determined with some modifications of the testing procedure, provided attention is given to the possibility of interelement interferences.

Jan 1, 1961

By W. H. Oppelt

Two exploratory gasification tests of limited duration were made at Dorsten, Germany, with strongly coking Pittsburgh-bed coal in a fixed-bed pressure gasifier. To reduce the coking potential of the Arkwright coal, ash refuse from the gasification of Dorsten (Leopold) coal was added to pre-pare coal-ash mixtures which contained nominal 20 and 30 percent ash. Major adjustments in principal process variables at the beginning of the tests resulted in wide fluctuations in the rate of gas production, gas offtake temperature, and carbon dioxide concentration in the gas. Because a higher steam-to-oxygen ratio was used in the tests than was customarily employed for routine operation, gas production was lower, and steam and oxygen consumption was higher. After operating conditions had been improved, the results of a 12~-hour-long test with addition of sufficient ash refuse to obtain a nominal 30 percent ash concentration indicated that operation is feasible with this coal mixture using a fixed-bed pressure gasifier equipped with a rotating coal distributor and stirrer.

Jan 1, 1966

By D. W. Frommer

Composite samples of nonmagnetic taconite from the western Mesabi range were evaluated by reductive roasting, fine grinding, and magnetic separation to determine potential sources of concentratable material. Although large tonnages of nonmagnetic taconite are known to occur in the western Mesabi district, these materials are not as yet a commercial source of iron ore. The technique employed permits the evaluation of individual composites and blocks of composites in terms of responsiveness to a process of potential commercial significance. The 159 composites, from open-pit mines located between Grand Rapids and Chisholm, Minn., were evaluated in the following sequence: 1. Minus 8-mesh material was roasted at 500° C. in hydrogen. 2. The roasted are was ground to one or more sizes in the minus 100-to minus 400-mesh range. 3. The roasted ground ore was magnetically separated in a Davis tube. 4. Composites were classified according to degree of grinding required to produce minimal concentrates. (Minimal concentrates are herein defined as those containing less than 10 percent silica, and responsive composites as those yielding minimal concentrates.)

Jan 1, 1962