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By R. J. Bielicki

A sorption apparatus for measuring the equilibrium sorption isotherm and the rate of diffusion of methane from fine-sized coal was designed and constructed. Preliminary work that used Pittsburgh and Pocahontas No. 3 coal shows that the diffusion coefficient varies with pressure and that the fracture spacing in these two coals is substantially different.

Jan 1, 1972

By Larry A. Haas

Carbonyl sulfide (COS) was decomposed to sulfur and CO in a silent electrical discharge. A threshold of about 4 kv at 60 Hz was required to dissociate the gas in a laboratory ozonizer at 790 torr with electrode gaps between 1 and 5.5 mm. Above the threshold value, the reaction rate increased with increasing voltage with helium or nitrogen diluent. With the latter diluent, higher voltages had to be applied to obtain the same yield in the 4-to 12-kv range. The COS decomposition rate increased with COS concentration, but a saturation value was reached at about 10 pct COS. The reaction rate decreased at low linear gas velocities as obtained at lower gas flows, larger electrode gaps, or larger reactor volumes. Increasing gas temperature also decreased the decomposition rate. The presence of solid adsorbents such as quartz wool, bauxite, or charcoal had no significant effect on the reaction rate. The addition of S02 did not affect the COS decomposition rate, but small amounts of water decreased the reaction rate. Over 50 pct of the COS was decomposed at room temperature and atmospheric pressure in a l7-kv ozonizer using a gas containing 0.9 pct COS in helium flowing at a rate of 0.3 liter/min. The average current was less than 5 ma. This method has possible application in eliminating the toxic air pollutant, COS, which is generated in petroleum refineries and in processes involving reactions between sulfurous and carbonaceous materials. Carbon monoxide that is formed can be further oxidized to CO2 after the collection of elemental sulfur.

Jan 1, 1972

By George J. Conroy

Electrical power generation was studied in a laboratory-scale, open-cycle vortex MHD generator, which offers several advantages over straight-channel generators that require separate combustors. Compactness, lower capital cost, and high-energy release are obtained by combining the combustor and generator into one unit in the vortex generator. In addition, the vortex generator uses a simple solenoid rather than the more complex and expensive saddle magnet required for straight channel generators. Although the vortex generator must utilize combustion gases with a low Hall coefficient in order to be efficient in direct comparison to the linear generator, the primary motivation for this experimental device in terms of ultimate objective was to investigate the vortex generator with applications to direct coal firing and with combustion taking place in specially designed expansion nozzles. The vortex device offers one decided advantage over the linear device in this regard because slag deposits do not degrade or short-circuit the coaxial electrodes as is the case for a linear machine. The experimental vortex generator consists of a modified cyclone burner 7 ½ in ID by 21 in long, with the inner wall used as one electrode together with a coaxial center electrode. Power was obtained by impressing an axial field of 3,000 G from an air core solenoid magnet. Tests were conducted by seeding natural gas seeded with potassium acetate and burning with preheated oxygen-enriched air. Power generation was lower than calculated because theoretical plasma velocities were not achieved.

Jan 1, 1972

By J. D. Kalasky, Stephen Krickovic

A degasification experiment was conducted in a Pocahontas No. 3 coalbed mine in Virginia. It involved (1) drilling holes in the coalbed in the out- side headings of a set of five being developed in virgin area, and (2) conducting a methane emission rate study as mining progressed and additional holes were drilled. Degasification from all drill holes except the longest in each of the outside headings and the first three drilled (excluding the in-situ pressure hole), was erratic and inconsequential in methane emission rates. The two longest holes liberated 66 and 79 cfm of methane, which is significant for the coalbed, but such quantity lasted a relatively short time; the first three were uniform but low in methane emission.

Jan 1, 1972

By Stephen Krickovic

A degasification experiment was conducted in a Pocahontas No. 3 coalbed mine in Virginia. It involved (1) drilling holes in the coalbed in the out-side headings of a set of five being developed in virgin area, and (2) con-ducting a methane emission rate study as mining progressed and additional holes were drilled. Degasification from all drill holes except the longest in each of the outside headings and the first three drilled (excluding the in-situ pressure hole), was erratic and inconsequential in methane emission rates. The two longest holes liberated 66 and 79 cfm of methane, which is significant for the coalbed, but such quantity lasted a relatively short time; the first three were uniform but low in methane emission.

Jan 1, 1972

By Richard A. Dick

Eight blasts were fired in a 2-1/2-ft bench in the Stewartville member of the Galena Limestone formation in an aggregate quarry near Stewartville, Minn. The shots were dimensionally proportional to production-size bench blasts and were about 5 to 10 percent of full scale. The effects of site, timing of initiation, and burden-to-spacing ratio were studied in a 2 x 2 x 2 factorial experiment, using three boreholes, caw;, containing a 1/2-in charge diameter of high-density ammonia dynamite, in each blast. Detonation velocity measurements indicated that the dynamite detonated satisfactorily in the 1/2-in charge diameter. The effects of the three experimental variables were analyzed by weight for the percentage of oversized material produced and for size distributions determined by screening the entire muckpiles. The bench faces were painted before each shot in an effort to determine the origin of the oversized material. The square pattern (burden and spacing = 15 in) produced finer overall fragmentation and less oversized material than the rectangular pattern (burden = 15 in; spacing = 22-1/2 in). Sites 1 and 2 were about ft apart. Although site 2 produced slightly better overall fragmentation than site 1, the amounts of oversized material produced showed no significant difference. The timing of initiation (instantaneous or delayed) did not significantly influence the overall fragmentation or the amount of oversized material produced.

Jan 1, 1973

By Robert B. Worthington

This investigation was undertaken to develop a more efficient copper smelting practice that would help meet the increasingly stringent antipollution standards. Continuous smelting to copper and a 0.8-to 5-percent copper slag using pure oxygen has been demonstrated for several hours at a time in a unique double furnace, which was devised to overcome the heat losses inherent in a laboratory furnace. The use of pure oxygen to effect the smelting and conversion of copper sulfide concentrate in a single unit to produce blister copper and a very high S02 concentration provides a much reduced gas volume for more economical and thorough sulfur recovery. Although the process was successfully demonstrated for several hours at a time, extended test work using longer runs will be required to balance the system and to obtain test data for adequately demonstrating its technical feasibility.

Jan 1, 1973

By Robert C. Steckley

A study of joints in Marathon County, Wis., was made to determine the orientation of regional paleotectonic stresses and to develop a method of using optical diffraction analysis (ODA) in studying joint orientations and spacings. Standard geologic and petrofabric techniques employing the use of a geologic compass and a Schmidt net were used in gathering, describing, and reducing joint orientation data. Analysis of selected outcrops with ODA indicates that ODA can be applied to study both joint orientations and spacings. ODA is shown to be a rapid method that can be used to complement standard petrofabric techniques, especially in the study of joint spacings.

Jan 1, 1972

By Alan H. Goode

Glass wool meeting requirements for commercial use was made from glassy fractions of urban solid wastes by the Bureau of Mines. This research was a part of the Bureau's program to develop building products and other usable materials from reclaimed urban waste materials. Mixes of molten glass were fiberized into glass wool during laboratory studies by impingement of a jet of compressed air on a stream of the molten glass. The principal test variable studied was composition of the melt; this was varied by adding dolomite and alumina to obtain molten glass with the handling characteristics required for producing final wool products of the desired composition and physical characteristics. When no charge is made for the waste glass and approximately $75 per ton can be obtained for the wool product, an interest rate of return on investment after taxes of about 12 percent can be obtained. If a charge of $5 per ton is required for the waste glass, a selling price of about $78 per ton would be necessary to obtain a l2-percent-interest rate of return on investment after taxes.

Jan 1, 1972

By George A. Savanick

The objective of this research is to develop a method for measuring the tensile strength at the interface between minerals in rock. These measurements reflect the strength of the attractive forces operating at crystalline interfaces in rock. Since these forces act in opposition to the forces set up in various rock fragmentation processes, measuring their strength may help in designing more efficient methods of rock fragmentation. The method developed for measuring the strength of intergranular adhesion in rock involves separating a bicrystal from the rock and determining the tensile strength at its solid-solid interface. This technique has been successfully applied to the study of quartz-feldspar interfaces separated from massive pegmatites, graphic granite, and the Rockville granite, yielding average tensile strengths of 5.86, 8.62, and 10.65 meganewtons per meter squared (MN/m2) (850, 1,250, and 1,524 psi, respectively). The data this technique provides indicate that the members of these bicrystals are strongly adherent. Examirtation of bicrystals broken at the crystalline interfaces indicates that the bonds responsible for this adhesion operate over only a portion of the interfacial area. This work conclusively demonstrates that tensile strength tests can be conducted on small selected areas; for example, grain boundaries in rock. The small-scale zones of strength or weakness determined in this way can be related to the overall strength of the rock.

Jan 1, 1972

By D. C. Fleck

Electrorefining yttrium from selected low-melting yttrium--base alloys is investigated, and various halide systems are studied as potential electrolytes for use in preparing low-oxygen yttrium by electrorefining unalloyed yttrium. Yttrium cathode products having significantly less metallic impurities than the anode materials were prepared from alloys containing nickel, iron, and manganese by electrorefining in LiCl-YC13 electrolytes at 900° to 1,000° C. Yttrium-copper and yttrium-magnesium alloys are not suitable as anode feed materials, An evaluation of chloride, fluoride, bromide, and mixed chloride-fluoride electrolytes showed that cathode products containing much less oxygen than the anode material can be obtained in the fluoride and mixed chloride-fluoride systems. Initial cathode current density has no apparent effect on the purity of the products obtained in both phases of the investigation.

Jan 1, 1973

By O. Q. Leone

A processing unit was developed for the complete cleaning of titanium alloy chips. The process uses solvent degreasing, magnetic separation, and anodic solution of nonmagnetic impurities in 10 weight-percent sulfuric acid. Vacuum arc-melted ingots weighing approximately 10 pounds each were prepared from cleaning chips according to ingot specifications.

Jan 1, 1973

By J. B. Janus

This report, the 22d in a series, gives analytical data showing composition and quality of tipple and delivered samples of coal collected during fiscal year 1972. This coverage lists mines located in 20 States. Ultimate analyses are given for most of the coalbeds listed. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. The deliveries were sampled in accordance with instructions issued by the Bureau of Mines, and the samples were analyzed in the Bureau laboratory at Pittsburgh.

Jan 1, 1973

By R. Blickensderfer

The sparking and gas-igniting tendency of steels and alloys were evaluated my measuring the radiance of spark showers produced by grinding a sample on an abrasive wheel in air, the time required for a spark shower generated on an abrasive wheel to produce an ignition in an explosive gas mixture, and the energy and speed required for impacts between various materials to ignite an explosive gas mixture. Mixtures of air-methane were found quite resistant to ignition by showers of sparks. A mixture of air-9.S pct hydrogen was used to increase the sensitivity of the tests and to thereby extend the range of materials that could be evaluated. The results of the spark-shower tests indicate that carbon steels and the alloy steels found in coal-cutter tools are among the most sparking and most incendive of any materials tested. Stainless steels, nickel alloys, and tungsten carbide are among the least sparking and least incendive. The brightness of the spark showers depended upon the degree of oxidation of the abraded particles. Impact tests against hard rocks such as solid quartz and sandstone, showed that high-carbon steel was more inc endive in the hydrogen mixture than were the softer steels or the alloy steels found in coal cutters. Ignitions were found much less likely to occur at speeds somewhat lower than the speeds currently in use in continuous mining machines.

Jan 1, 1972

By T. Kessler

As part of a respirable mine-dust research program at the U.S. Bureau of Mines, spark-source mass spectrometry has been used for the semiquantitative determination of trace elements (200 ppm weight or less) in raw coals. In addition, several minor and major elements have been determined using this technique. Sixty-four elements ranging in concentration from 0.01 to 41,000 ppm weight were determined in one anthracite, two mvb, four lvb, and six hvab raw coal samples. The samples represented 10 coal seams located in Pennsylvania, West Virginia, Virginia, Utah, and Colorado.

Jan 1, 1973

By M. A. Mahtab

This report presents the geometric parameters (attitude, spacing, extent, and aperture) of fracture patterns in a selected portion (study area) of San Manuel copper mine, Arizona. The geometric parameters are quantified for input to structural analyses for studies of the influence of fractures on cavability of ores. Using an orientation analysis procedure developed earlier by the Bureau, three prominent and nearly orthogonal sets of fracture orientations were delineated in the study area. Sets 1 and 2 dip nearly vertically, and generally strike east-west and north-south, respectively, whereas set 3 is nearly horizontal. Both a horizontal rotation (of 14° to 26° for sets 1 and 2, respectively) and a tilt (of 20° for set 3) is shown to occur between the 1415 and 2015 levels of the mine. Gomparison of the three major rock types present in the study area (quartz monzonite, monzonite porphyry, and rhyolite) show that the rhyolite is characterized by short extent, small spacing, and tightness of fractures as well as the general absence of fracture set 3, which may account for its generally observed strong resistance to caving.

Jan 1, 1973

By E. G. Valdez

Three cryogenic systems that utilized liquid nitrogen, dry ice, and methanol with dry ice were investigated in conjunction with crushing and classifying techniques. The systems were used to aid in separating and reclaiming the metallic components contained in insulated wires, shredded automobile nonferrous metal concentrates, small motors, generators, and rubber tires. Wire strands, 2 to 6 inches long and insulated with polyvinyl chloride and neoprene, were chilled at -60° and -195° C, then roll-crushed and processed by water elutriation; this procedure resulted in two products--a sink fraction that was 99 percent metallic and a float fraction that was 99 percent nonmetallic. Excellent separation of zinc die-casting alloys from copper and aluminum contained in shredded automobile nonferrous metal concentrates was attained by chilling at -72° C for 1 minute, crushing in a grateless hammer mill, and screening. From the screened products, 97.2 and 100 percent of the copper and aluminum, respectively, were recovered in the plus Pinch fraction, and 100 percent of the zinc was recovered in the minus 1-inch fraction of over 97 percent zinc die-cast purity. Laboratory experimental results comparing direct and indirect chilling indicated that a sufficiently low temperature could be attained by indirect chilling to permit use of a liquid C02-dry ice system on insulated wires and mixed nonferrous metallic concentrates.

Jan 1, 1973

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 K. J. Liles

The Bureau of Mines conducted laboratory semicontinuous and continuous heavy liquid tests to determine the feasibility of producing commercial-grade products from the high-clay sylvinite ores of the Permian Basin in New Mexico. Continuous test operations demonstrated that concentrates containing 59.9 percent K2O and recoveries of over 75 percent of the contained potash can be obtained. The organic heavy liquid was effectively recovered by vaporization, condensation, and absorption methods. Less than 5 parts per million of heavy liquid vapors were released to the atmosphere. This loss represents only 0.02 pound of heavy liquid per ton of ore treated.

Jan 1, 1973

By D. A. Doughty

The Bureau of Mines developed two methods for determining iron II and iron III in 2- to 5-mg samples of coal using electron paramagnetic resonance (EPR) spectrometry. One method used solid coal samples; the other method used aqueous solutions. The method using solid samples was more simple, technically, but required the use of X-ray fluorescent analysis, or another independent method, for determining total iron in the samples, and the results were subject to some uncertainty. The method using aqueous solutions appeared capable of greater certainty and did not require additional methods of total iron analysis but was more involved procedurally. The coals analyzed were found to contain much more iron II than iron III.

Jan 1, 1973