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By David H. Yee

Because of environmental concerns, the Bureau of Mines investigated an anhydrous chlorination process for the recovery of copper from chalcopyrite, Pelletized concentrate was reacted continuously with chlorine in a vertical shaft reactor at 550° to 750° C to extract copper-iron chlorides and elemental sulfur. The resulting molten metal chlorides drained from the reactor and collected in a receiver while sulfur distilled from the top and condensed in a separate unit. The tests were conducted in a 10-cm-diam reactor constructed of glass and in l5-cm-diam reactors constructed from various refractory materials. A high-alumina ramming mix exhibited the best resistance to molten metal chlorides and elemental sulfur in chlorine atmospheres. A reactor made with this high-alumina refractory was operated for 55 hr under actual chlorinating conditions without suffering any deterioration. Tests results show that more than 96 pct of the chalcopyrite was converted to copper-iron chlorides and elemental sulfur. Good separation of the metal chloride and sulfur products was achieved. After filtration, elemental sulfur of greater than 99 pct purity was obtained.

Jan 1, 1977

By Noel N. Moebs

The Bureau of Mines investigated severe coal mine roof support problems along a section of main entries in the Pittsburgh coalbed in southwestern Pennsylvania to identify the causative factors. The mine roof was examined in detail, and various sedimentary structures are described that contributed directly to irregular and unstable roof. Small-scale paleochannels, scours, and related slickensides were identified as the leading cause of bad roof, and isopach maps were prepared to illustrate a method whereby the presence of these structures could be inferred in advance of mining. Probably second in importance was the occurrence of relatively incompetent flaggy, poorly cemented sandstone, weakened by coal and micaceous laminea. No effect of in situ stresses on roof stability was detected.

Jan 1, 1977

By Jack E. Fraley

In this Bureau of Mines study, sealants containing mineral wool, cement, etc, were sprayed through dry-process equipment that propels dry material pneumatically to the water-adding nozzle. Advantages over slurry applications include no mixing, no extensive cleanup, and freedom from hardened cement in equipment should power be lost. Sealants with large mineral wool nodules (>l-inch) were sprayable at rates to 900 square feet per hour for 1/2-inch thickness with little dust and smooth material flow through equipment, but they were weak for mine use, Materials containing small wool nodules (1/4-inch) were stronger but tended to plug lines because the nodules were inadequately separated in the shredder. Increasing the dedusting oil also increased line plugging by holding the nodules together in larger lumps. Best results were obtained using a 3/4-inch-nodule wool with cement binder, which provided both smooth flow through the machine and adequate strength.

Jan 1, 1977

By Charles D. Litton

A new prototype ionization-attachment fire detector was developed by the Bureau of Mines for detecting combustion-generated submicrometer particulates. It is much more sensitive than the conventional ionization smoke detector, and it has the following added features: 1. A primary charging current of unipolar air ions is generated by a gold-coated, radioactive center electrode of a cylindrical diode. 2. Submicrometer particulates are flowed axially through the unipolar cloud where they acquire charge. The charged particles impinge upon a third electrode, located downstream, resulting in a current which is directly proportional to the particulate concentration. 3. Additional electrodes analyze the particulates in terms of their mobility and thus determine their size distribution. 4. A filter and cyclone assembly protect the ionization chamber against ambient dust. An analysis of conventional ionization smoke detector performance is also presented in terms of source strength, chamber geometry, and applied potential.

Jan 1, 1977

By Ann G. Kim

The Bureau of Mines estimated the methane content of a coal, which depends primarily upon rank and pressure, from the adsorption equation V kpn, where k and n are constants related to rank. By incorporating corrections for moisture, ash, and temperature, and estimating pressure and temperature as a function of depth, the methane content of coal in place can be estimated from the following equation: [ ] Values calculated with this equation generally are in reasonable agreement with direct determinations. By assuming a standard moisture and ash content, and using the hydrostatic head to estimate pressure, a graph of rank and depth versus gas content was constructed. Although estimated values were consistently high for several high-volatile bituminous coals from an area where the pressure is known to be less than hydrostatic, the estimated methane content for most coals shows reasonable agreement with values determined by the direct method.

Jan 1, 1977

By Natesa I. Jayaraman

A field study was conducted by the Bureau of Mines to determine the feasibility and effectiveness of a secondary ventilation system retrofitted onto an Eickhoff EDW 340L double-drum shearer as a technique for controlling respirable dust generated during a longwall mining operation. An airflow duct was formed by enclosing the bottom of the undercarriage with steel plate and cutting air channels through the ends of the undercarriage frame. Air intakes were provided behind each cutting drum and at several locations along the undercarriage. Grills were installed at the intakes to prevent the broken coal from entering the ducting. A dust collector consisting of 5,000-ft3/min fan, water sprays, and a minicyclone panel was installed on the shearer at the tailgate end. Field results indicated that the secondary ventilation system reduced respirable dust more than 60% along the face. Reduction was less near the intake airway and when secondary dust sources occurred.

Jan 1, 1977

By David Schlain

The Bureau of Mines investigated methods for electrodepositing platinum-group metals from molten cyanide baths. The preparation of thick, protective coatings on molybdenum, Inconel, graphite, stainless steel, copper, and other structural metals were studied, as well as the electroforming of platinum and iridium crucibles. Iridium, rhodium, and ruthenium can be electrodeposited under an inert atmosphere, while platinum and palladium require the presence of air. Electrolytes may be prepared by direct-current electrolysis in NaCN or mixtures of NaCN and KCN using anodes of the particular platinum-group metal. When the concentration of metal increases to about 0.3 or 0.4 percent, the deposits become bright, adherent, and coherent. Current densities may be 10 to 25 ma/cm2, and plating rates are often 0.5 mil/hr. Platinum and palladium baths deteriorate because of the oxidation of cyanide to cyanate and carbonate, and the precipitation of metal. Changes in the platinum cyanide bath are relatively slow. The protection against oxidation afforded by the platinum-group metal coatings is evaluated by testing encapsulated specimens in a thermogravimetric balance. Surface pretreatment and the use of undercoats are discussed.

Jan 1, 1977

By George J. Conroy

To provide data as a basis for proposed acceptance standards and procedures covering permanent splices in trailing cables, the Bureau of Mines conducted testing programs on the flexure life in flat types W and G dc trailing cable splices and ground conductors. Primary reliance was placed on laboratory testing, although some cross comparisons were made at manufacturers' plants and mine operations Besides providing data for acceptance standards and procedures, results of the program should promote the general improvement of commercially available splice kits.

Jan 1, 1977

By James R. Aggson

The theoretical relationships that are used to calculate in situ rock stress magnitudes and directions from borehole deformation data obtained during overcoring are based on the assumption that the rock is a linearly elastic material. Strictly speaking, this assumption is not valid in any rock. Thus, investigators using overcoring techniques must either accept various degrees of nonlinearity and the associated inaccuracies or use core testing techniques that address the problem and compensate for elastic nonlinearity. Previously developed test procedures for stress-relief overcores partially correct for nonlinearity. This Bureau of Mines paper describes a test procedure that completely corrects for elastic nonlinearity in stress-relief overcores.

Jan 1, 1977

By Curtis H. Elder

In studies conducted by the Bureau of Mines, two test areas were hydraulically stimulated and exposed by mining: One in the Pittsburgh coalbed at the Vesta No. 5 mine, Washington County, Pa.; and one in the Illinois No. 6 coalbed at the Inland mine, Jefferson County, Ill. Induced fractures were contained totally within the coalbed with no adverse effect on the stability of associated rock strata. Induced fractures were vertical and were propagated normal to the direction of least residual tectonic stress. Gas production was increased fivefold to twentyfold by hydraulic stimulation.

Jan 1, 1977

By J. L. Holman

The Federal Bureau of Mines has conducted research to delineate factors affecting relative fabricability of electrowon and electrorefined copper. The Bureau's Rolla Metallurgy Research Center coordinated and participated in a statistical round-robin chemical analysis and performed impact tests on lead-doped copper specimens. In a series of round-robin analyses, cathode, bar, or rod from a domestic lot of electrorefined copper and electrowon copper from a domestic and a Peruvian source were analyzed for Pb, Fe, Bi, Se, Ag, O, S, Sb, and seven other elements. The electrowon cathode from both sources surpassed requirements for electrolytic cathode, although lead in the Peruvian lot exceeded specification for oxygen-free electronic grade. The least interlaboratory agreement was for oxygen analysis, Copper specimens, doped with up to ~300 ppm Pb and consisting of as-cast material (fine-grained or coarse-grained) and hot-rolled material, were impact-tested at temperatures to 871° C (1,600° F). Impact energy of fine-grained material dropped 26 pct with increased Pb up to 20 ppm and more gradually thereafter. Coarse-grained specimens fractured at lower energy with little dependence on lead. Hot rolling raised impact energy substantially. Grain structure is evidently as significant as lead in influencing workability. Some discussion is given of possible effects of oxygen, sulfur, and porosity.

Jan 1, 1978

By M. Hertzberg

This Bureau of Mines report describes experimental and theoretical studies of diffusion flames in free convection. The cross-coupling between buoyancy-induced flows and the combustion process is explored as it relates to the size, structure, and radiative balance of flames. New data are presented for the size-dependent radiance oscillations of diffusion flames and for the angular distribution of the total radiant intensity from a small methanol pool flame. Both amplitude and frequency of the measured oscillations are compared with theoretical predictions that are based on a new view of the structure of diffusion flames. This new view, which is at variance with the traditional one, assumes uniform reaction in the diffusive mixing zone, and recognizes the significance of the role played by convective buoyancy and its duality in both aiding and impeding flame propagation. Buoyancy quenches propagation at low burning velocities, introducing a real discontinuity in the combustion rate. A "flammable volume" is thus defined as that bound between lean- and rich-limit contours. However, in the flow disturbances generated by combustion waves that consume that volume, buoyancy aids propagation by promoting the convective mixing of a new flammable volume. The measured radiance oscillations are manifestations of these propagation and remixing cycles.

Jan 1, 1978

By S. Ralph Austin

Emanation coefficients of 950 samples of domestic uranium ore were successfully and rapidly determined with fair precision by modifications of the closed-can, gamma-only assay method, using commercially available or similar equipment. Coefficients range from <1 to 91 percent. Emanation varies considerably within each mine and area, but distinct differences among major mining areas were found, ranging from 7.5 percent for Moss Back Member, Chinle Formation, Southwest Lisbon Valley, Utah, to 56.6 percent for Ft. Union Formation (?), Powder River Basin, Wyoming. Coefficients also vary with (1) uranium mineralogy; (2) radium mineralogy; (3) lithology of host rocks; (4) grain size of uranium and radium minerals; (5) comminution of ore; (6) estimated porosity and permeability; (7) moisture content; (8) ore grade; (9) supposed mobility of deposits; age of deposits is unknown but limited by (10) age of host rocks which shows only doubtful correlation with emanation. Data obtained may be used to evaluate effects of investigated parameters on radon concentration in mines and thus to select efficient control measures. Drill-core emanation data allow estimates of probable radon problems in undeveloped deposits.

Jan 1, 1978

By K. O. Bennington

[Thermodynamic properties of two amphibole asbestos minerals were determined by the Bureau of Mines. The enthalpies of formation were determined by the hydrofluoric acid solution calorimetry method. Heat capacity measurements were made with an adiabatic calorimeter over the range of 5 to 315 K. High-temperature enthalpies above 298 K were determined with a copper-block drop calorimeter to 852 K for amosite and to 902 K for crocidolite. Thermodynamic data determined for amosite of the composition Fe5+2.2766Mg1.5209 Fe+03.12Mn0.0825) Si7.9163Al0.0837022.0363)(OH)1.9637 are: S°298 = 168.8 ± 5 cal/deg-mole; ?Hf°298-15 (elements) = -2419.24 ± 2.95 kcal/mole; ?Hf298.15 (oxides) = -30.92 ± 2.47 kcal/mole; and ?Gf° -2260.1 kcal. Corresponding data found for s3 ,1s = crocidolite of the composition (Na1.9Ca0.1)(Fe2+.024Fe2.5 01Mg0.475) (Si7.9713024Fe+2 2.501Mg0.475) (Si7.971 Al0.029022.095) (OH)1.905 are: S2.98-15 - 161.1 ± 4 cal/deg-mole; ?Rf° 2 298.15 (elements) = -2433.56 ± 2.99 kcal/mole, 10298.1s (oxides) = -87.69 1.70 kcal/mole, and ?Gf°298.15 = -2269.8 kcal.] Calorimetric values from this investigation were combined with other data from the literature to calculate the Gibbs energies of formation and equilibrium constants of formation over the temperature range of the measurements. Tables of enthalpies of formation and Gibbs energies of formation are given as a function of temperature both from the elements and the constituent oxides.

Jan 1, 1978

By Laurance L. Oden

The Bureau of Mines is developing nickel catalysts for converting synthesis gas derived from coal to synthetic natural gas. The present report describes the relationship between the composition of aluminum-nickel alloys in the composition range NiAl3 to Ni2Al3 equilibrated at 840° C and the properties of catalysts obtained from them. Methanation activity was determined in the temperature range of 300° to 360° C in a flowing gas stream containing 1 pct CO, 8 pct H2, and the remainder He. One part per million of H2S was added to the gas stream at 400° C to evaluate the susceptibility of catalysts to sulfur poisoning. The total surface area was measured by the adsorption of nitrogen at liquid nitrogen temperature, and the active surface area was measured by the adsorption of hydrogen at room temperature. Total surface area and active surface area were found to increase with increasing proportion of aluminum-saturated Ni2Al3 in the precursor alloy, but methanation activity and resistance to poisoning by H2S were nearly constant. However, the methanation activity of the catalyst prepared from stoichiometric Ni2Al3 was less than half that of the other catalysts.

Jan 1, 1978

By G. K. Derby

Five different types of drilling systems were developed under the flexible drill program that was initiated by the Federal Bureau of Mines to protect roof bolter operators. The systems were designed for underground coal mines with seams as low as 30 inches, and with roof bolts longer than the height of the seam opening. Four of the developed systems were true flexible drills; the fifth was a remote-controlled, automatic rod changer concept. Only two of the five firms successfully completed testing requirements under the original contracts: BendixCorp.,4 with a true-flex drill; and Ingersoll-Rand Research, Inc., with the rod changer concept. The Bendix drill was rated best, and the Ingersoll-Rand drill was rated second. Because of the closeness of the ratings and the vast differences in the two development concepts, both systems had sufficient potential to justify further development funding for design updating and testing. Also, both systems warranted consideration for inclusion into other ongoing development projects under both safety and energy directed programs.

Jan 1, 1978

By James R. Aggson

This Bureau of Mines report describes floor heave ground control problems that have been encountered in a new underground coal mine in West Virginia. Previous experience in the coal seam, the results of physical property investigations, and in situ rock stress determinations are discussed. The apparent cause of the ground control problems is the existence of a high, biaxial, horizontal stress field coupled with a floor member that has time-dependent deformation characteristics, A theoretical analysis of the failure process is developed. The analysis is assisted by finite element techniques. Mine design recommendations based on this analysis are presented.

Jan 1, 1978

By Michael J. Beus

This Bureau of Mines report describes a tunnel stress relaxation gage (TSR) developed to measure initial radial displacement around full-sized underground openings. The TSR technique was shown to be a valid concept in previous field verification tests. Sensitivity has been improved by employing a titanium alloy cantilever in the transducer head, which also permits a deeper sensor location. Use of improved fabrication methods such as stainless steel bellows and sputtering techniques and use of an environmental chamber for testing greatly increased overall reliability. A miniature data acquisition system (DAS) was interfaced directly to the transducer for increased versatility and containment entirely within a borehole. The present TSR system is suitable for use around full-size underground excavations, particularly machine-bored openings. Field evaluation of the improved instrumentation verified the design goals.

Jan 1, 1978

By Joan T. May

Federal Bureau of Mines studies showed that some organic amine hydrochlorides can be used as dehydrating agents for producing anhydrous magnesium chloride from hydrates and brines. Laboratory-scale tests showed that double salts are formed by reacting 35 percent magnesium chloride brine or spray-dried magnesium chloride with pyridine hydrochloride. Heating decomposed these double salts to anhydrous magnesium chloride and recycle pyridine hydrochloride. Pyridine hydrochloride also chlorinated any magnesium oxide in the spray-dried magnesium chloride. The anhydrous magnesium chloride obtained by the method described contained less than 0.8 percent oxygen. More than 98 percent of the organic amine hydrochloride was recovered.

Jan 1, 1978

By D. E. Traut

A fluidized countercurrent ion-exchange system was developed, operated, and evaluated by the U.S. Department of the Interior, Bureau of Mines. The system consisted of integrated multiple-compartment absorption and elution columns in which the solution flows were continuous except for short periods when resin increments were withdrawn. The exchange of uranyl carbonate between a simulated in situ uranium leach liquor and a strong-base ion-exchange resin together with the subsequent elution with an ammonium chloride solution was studied. The effects of the number of sections, section height, amount of resin withdrawal, solution flow rate, and column diameter were investigated. The kinetic and equilibrium relationships for the absorption and elution steps were also examined. The experimental data indicate a strong interdependence between variables. Solution retention time appears to be a major limiting variable in the absorption process, while resin residence time is the determining factor in the elution process. The column was efficient over a range of conditions, but close control was needed for optimum operation.

Jan 1, 1978