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By Je M. Oh

The Bureau of Mines is conducting research to determine the high temperature oxidation resistance of substitute stainless steels (SS) containing two less strategic elements, Al and Si, instead of Cr. Chromium is considered to be a critical and strategic metal. Although the Cr content was reduced to 8 wt pct, the alloys showed better oxidation resistance than did 304 SS containing 18 wt pct Cr. Specifically, the alloys that contained Fe-8Cr-16Ni with combinations of Al and Si showed excellent oxidation resistance even at temperatures up to 1,000° C. In this study, the effects of the alloying elements on oxidation kinetics and morphology of oxides were investigated using a Cahn Rg electrobalance, scanning electron microscopy, an energy-dispersive X-ray analyzer, X-ray diffraction, and an electron microprobe. Aluminum and silicon additions in combinatin were more effective in providing oxidation resistance than either element was alone.

Jan 1, 1986

By James C. Cawley

The Bureau of Mines conducted an investigation to statistically determine the mean current or voltage for resistive, inductive, and capaci-tive circuits that would cause spark ignitions in 8.3% methane-air, 5.3% propane-air, and 7.8% ethylene-air mixtures. Each mean ignition current or voltage was determined on the basis of 100 trials. Each trial consisted of 400 revolutions, 200 in each polarity, at 80 rpm of the standard breakf1ash apparatus. In general, spark ignition curves published in UL 913 for resistive and inductive circuits represent approximately the mean current values determined in this study, while published capacitive circuit values in methane are considerably less than the mean voltage values from this study, especially for a capacitance of less than 100 ~F. For resistive and inductive circuits, spark ignitions were obtained at currents con-siderably below those in the published curves, but this study was not optimized to find minimum ignition values. This report defines "safety factor" as applied to intrinsic safety testing as the energy ratio of the mean values of ignition current or voltage for two test gases. The safety factors presented in this report are not constant with voltage or current and, therefore, are not recommended for use.

Jan 1, 1986

By R. G. Burdick

The problems presented by old mine workings affect both present day mining and land development. An automated method of locating these old mines from the surface using electrical resistivity techniques was de-veloped earlier under a Bureau of Mines contract. Subsequent Bureau research has refined the techniques and expanded the area of study to a variety of geologic provinces. During this research, six mining areas in the United States were in-vestigated with the Bureau's automated resistivity method. This report describes the mining areas involved and the results of the resistivity investigations, which showed a high rate of success in detecting old mines. It also describes the field measurement techniques and data analysis procedures.

Jan 1, 1986

By L. Y. Sadler

The Bureau of Mines conducted a study Lo determine the loss in weight of silica (Si02) volatilization from low-alumina (A1203) refractories used as hot face liner materials in such process equipment as coal gasifiers, synthesis gas transfer lines, and ammonia plant secondary re-formers. Small specimens of 80-and 40-pct-A1203 brick and 95-pct-SiO2 brick were exposed to steam in high-pressure furnaces at pressures of up to 1,000 psig and temperatures up to 1,400° C for periods ranging up to 120 h. Weight losses from the 40-pct-A1203 brick after 40 h of exposure were highest, 2.75 pet at 1,400° C and 1,000 psig. The rate of weight loss had dropped to near zero after 80 h of exposure at all temperatures. No relationship between total silica content of the specimen and weight loss could be established nor did scanning electron microscopic examination of the specimens before and after exposure identify specific regions (e.g., surface) suffering a disproportionate share of the silica loss. It was concluded that minor silica volatilization is likely to occur, if at all, at temperatures of less than 1,000° C and pressures below 1,000 psig, and that low-alumina refractories should be used as dry-ash coal gasifier hot face linings.

Jan 1, 1986

By C. W. Huggins

The primary objective of this Bureau of Mines research was to measure the size distribution of respirable quartz collected at metal mines, nonmetal mines, and processing plants to select the best reference standard for use in quantifying quartz in mine and plant dust samples. The secondary objective was to size all the nonquartz particles collected at the same sites. Particle size measurements were made on 29 samples using a scanning electron microscope in the backscatter mode of operation, interfaced with an image analysis system. The Mine Safety and Health Administration, Denver, CO, provided the 29 samples, which were collected at mines and processing plants in 19 states. The accumulated particle size measurements indicate that NBS 1878, minus 5-f.lm Hin-U-Sil, and minus 5-f.lm Supersil would be preferred over Silver Bond B as reference standards for most quantitative determinations by X-ray diffraction and infrared spectrometry. The respirable dust samples collected at sand plants, however, would be better served by a new reference standard having a quartz particle size distribution of approximately 2.2 um, as none of the four existing reference standards matched closely with them. Commercially available NBS 1878 and minus 5-um Hin-U-Sil CQuid be used as reference standards for 28 of the 29 samples studied in this investigation.

Jan 1, 1986

By Agnes Y. Lee

The Bureau of Mines has developed an effective hydrometallurgical method to recover high-purity Pb metal and elemental S from concentrates. This low-temperature process eliminates S gases and Pb emissions, in contrast to the current high-temperature smelting technology. The method consists of (1) oxidative leaching with H202, Pb02, and waste fluosilicic acid at 95° C to produce a solution of PbSiF6 and a residue containing elemental S, (2) electrowinning the PbSiF6 solution at 35° C to produce 99.99 pct Pb metal and H2SiF6, and (3) solvent extraction to recover S, leaving a residue containing Cu, Ag, and other metal values. Spent electrolyte was recycled repeatedly, with impurity buildup controlled by controlling the leach parameters.

Jan 1, 1986

By Bill M. Stewart

To decrease the potential for fine coal waste slurry impoundment failures, the Bureau of Mines investigated a new disposal technique. The fine coal waste slurry is rapidly thickened (i.e., dewatered) and deposited on a slightly sloping surface. To accomplish rapid dewatering, a chemical flocculation system using polymers was developed to treat the fine coal waste slurry stream. The fine solids formed flocs, settled from suspension, and rapidly released excess water. During the last 5 days of the field test, slurry flowing at rates from 498 to 675 gal/min with a specific gravity range of 1.15 to 1.33 was successfully treated and dewatered. During this period, untreated slurry had an average moisture content of 227.4 pct (30.7 wt pct solids). The effectiveness of the dewatering system was determined by monitoring the moisture content of the deposited waste with respect to time. Sixty-five hours after ending the field test the average moisture content was 54.9 pct (64.5 wt pct solids); 68 days after the field test the average moisture content was 28.8 pct (78.0 wt pct solids).

Jan 1, 1986

By Maria I. De Rosa

The Bureau of Mines performed experiments to determine concentrations of toxic gases and liquids, and smoke-particle diameters and diameter-concentrations evolved during degradation of PVC-derived brattice with and without nylon-woven fabrics, fiberglass, cotton, and jute brattices, and other mine materials. The samples were exposed in a 20-L chamber at temperatures of 1500 to 4500 C, with a chamber airflow of 10 L/min; 27.3 cm3/s of which was directed into a submicrometer-particle detector-analyzer. During the degradation of PVC-derived brattice, large concentrations of hydrogen chloride (TLV, 5 ppm; STEL, 100 ppm) evolved at a temperature as low as 2000 C. The minimum toxic load of 3.1 mg or 40 ppm in 50 L of dilution air, with O.l~g weight loss, may be reached at a mine face with 314,000 L of dilution air, at the 5th min, during which less than 1 kg of brattice undergoes combustion. Fiberglass, cotton, and jute brattices, pine wood dust, and coal dust showed small concentrations of carbon monoxide evolving during early stages of combustion. Hydrogen cyanide gas evolved from the PVC-derived, nylon-reinforced brattice; at a later stage of combustion, large concentrations pf carbon monoxide and dense smoke evolved from all PVC-derived brattices. Experiments to characterize smoke particles showed that marked differences exist in particle diameter-concentrations among the materials.

Jan 1, 1986

By J. E. Pahlman

Spontaneous oxidation and combustion of sulfides and resultant fires are serious problems in underground mines. The Bureau of Mines has con-ducted fundamental thermal gravimetric analysis (TGA) research to deter-mine the mechanisms and factors governing the rate of low-temperature pyrite oxidation, and to identify possible inhibitors to spontaneous oxidation and combustion. The mechanism of low-temperature pyrite oxidation was found to be topochemical, meaning that the oxidation process is controlled by the chemical reaction at the interface between pyrite (FeS2) and iron sulfate (FeS04)' An activation energy of 8.9 kcal/mol FeS2 was obtained for oxidation of minus 500-mesh pyrite in an atmosphere of 60 vol pct water vapor and 40 vol pct . Water-vapor content of the atmosphere was found to be the critical factor in the rate of spontaneous oxidation of pyrite, with a water-vapor content greater than 20 vol pct needed for accelerated oxidation. An atmosphere of pure oxygen resulted in negligible oxidation. The rate of pyrite oxidation is also greatly affected by the particle size of pyrite. Pyrite-oxidation rate increased drastically for particles less than 40 ~m. Room-temperature pyrophoric behavior was observed for freshly ground unoxidized pyrite (55 pct minus 5 ~m) upon exposure to air. Addition of water-adsorbing materials such as activated alumina (Alz03) decreased the rate of pyrite oxidation.

Jan 1, 1986

By F. Garacia, J. Cervik

Gob holes are routinely used by the mining industry to vent methane from gobs and to prevent it from entering the mine ventilation system. In some cases, flows from gob holes are measured by centering an anemometer on the end of a discharge pipe. These measurements are erroneous and tend to be high by as much as 30 pct. The Bureau of Mines deter- mined method factors (correction factors) for anemometer measurements taken in this manner. Method factors for 4-, 6-, and 8-in (10.2-, 15.2-, and 20.3-cm) ID pipe are 0.68, 0.71, and 0.78, respectively. Comparisons between horizontal and vertical flows indicated no significant change in method factors. Consequently, the method factors for horizontal pipe flows can be applied to vertical upward flows.

Jan 1, 1987

By Maureen M. Foss

Underground coal mining is hazardous due to changing geological conditions. One geophysical method showing promise for in-seam hazard detection is ground-penetrating radar (GPR). The Bureau of Mines recently completed preliminary studies to demonstrate the feasibility of using GPR for in-seam hazard detection. Investigations included air and coal tests for the purpose of checking equipment accuracy, coal penetration, and other factors such as the effects of receiver orientation. Further investigations involved using both a short pulse and a new prototype synthetic-pulse system to locate a clay vein in a coal seam using trans-illumination. Data were gathered on multiple travel paths, and a back projection processing technique was then used to create a tomographic image using the calculated velocities. A computer model of the same coal seam was subsequently processed using the same tomographic tech-nique, and the results were compared with those of the actual data. Analysis of the tomographic images shows the presence of the clay vein, although its boundaries are unclear due to the tomography method used. Results of these preliminary studies show that GPR is feasible for use in in-seam hazard detection and point the direction that future research should take. A need has been shown for research involving more sophisticated tomography techniques, transmission studies on thicker coal seams, and reflection studies using the synthetic-pulse system.

Jan 1, 1987

By K. O. Bennington

The thermodynamic properties of two manganese silicates, pyroxmangite and fowlerite (zincian rhodonite), were experimentally determined by the Bureau of Mines. The standard enthalpies of formation were determined by hydrofluoric acid (HF) solution calorimetry, the low-temperature heat capacities by adiabatic calorimetry, and the high-temperature heat capacities by differential scanning calorimetry over the range 322 to 1,372 K. Data for the standard enthalpy of formation (AH298), the derived standard entropy (S298), and the standard Gibbs energy of formation (AGf 298) are as follows: Pyroxmangite [(Mn0.9554Cao,0446)(Si03)J- AHf298 319.668±0.46 kcal/mol AH298 (from oxides)... -7.215±0.11 kcal/mol 5295 23.785±0.048 cal/(mol'K) AGf298 -301.190±7.96 kcal/mol Fowlerite [(Mno.7o3Zno.0884Ca0.2086)(Sio3)]--AHf298 ?... -329.914±0.419 kcal/mol AH298 (from oxides)... -8.400±0.104 kcal/mol 5598 21.949±0.059 cal/(mol-K) AGf298 -310.716±7.99 kcal/mol These experimentally determined values were combined with data from the literature to calculate the Gibbs energies and equilibrium constants of formation over the temperature range of the measurements. Standard enthalpies, Gibbs energies, and equilibrium constants of formation are given as a function of temperature from both the elements and the constituent oxides.

Jan 1, 1987

By Keith S. Olson

During 1982 and 1983, the Bureau of Mines concentrated its fugitive dust control research on haulage road dust suppression by newer chemi-cals relatively unknown in the mineral industry, innovative dust control designs for haulage trucks, chemical tailing basin stabilization, and combined chemical and vegetation tailing basin stabilization. Relatively unknown dust suppression chemicals and innovative aerodynamic modifications to haulage truck fender designs were tested on a Minnesota sand and gravel operation haulage road. Magnesium chloride salt at 95-pct control efficiency and a petroleum derivative at 70-pct control efficiency were effective in suppressing dust generated by haulage vehicles; however, none of the fender modifications were successful. Commonly used dust suppressant chemicals were tested on a Minnesota taconite tailing basin to reduce the dust lift-off during the spring and fall dry seasons. The most successful chemical was lignin sulfonate with a seasonal cost of less than $200 per acre to achieve 90-pct dust control. When chemical treatments for immediate dust control were com-bined with revegetation for permanent control, the most promising chemical treatment based on vegetation response was lime-neutralized lignin sulfonate.

Jan 1, 1987

By E. G. Davis

As a result of interest by the U.S. Department of Energy, the Bureau of Mines conducted studies on comminution of bituminous coal to the 2-um particle size range using the Bureau-developed turbomill. Both "plant grind" size (80 pct minus 75 um) and microsize (minus 10 um) coal can be produced in a single step with the Bureau's turbomill. In 15 min, minus 2.4-mm coal milled in water with steel shot was reduced tc 65 pct minus 75 m and 26 pct minus 2 m, with an energy requirement of 139 kW^h/mt coal. Plant-grind size coal milled in water, with Ottawa sand as the milling medium, was reduced to more than 45 pct minus 2 m in 15 min, at 175 kW?h/mt. Plant-grind coal milled with steel shot was reduced to 57 pct minus 2 um in 15 min, at 138 kW?h/mt. When diesel fuel was substituted for water, the milling of the coal was less effective and less energy efficient. Keeping the pulp dispersed was critical. Without an effective dispersant, the slurry became very viscous with increased milling time, resulting in higher energy requirements, low heat dissipation, and poor grinding efficiency.

Jan 1, 1987

By M. J. Ferrante

Relative enthalpies of cuprous iodide (CuI) were measured at the Bureau of Mines to provide thermodynamic data for the advancement of min-eral technology. Enthalpy measurements between 298.15 and 1,396.3 K were made with a copper-block drop calorimeter. The temperatures of transition were measured by differential scanning calorimetry (DSC). Reversible transitions were determined at 643 K with a standard enthalpy of transition [(6Htr)] = 0.74 kca1/mol, at 679 K with a [6Htr = 0.65 kca1/mo1, and at 868 K] with a standard enthalpy of fusion [(6H~) = 1.895 kca1/mol.] Tabulated values are listed at selected temperature increments from 298.15 to 1,600 K for the standard relative enthalpy (HO -H298), heat capacity (CpO), entropy (SO), and Gibbs energy function [-(Go -H298)!T]. The enthalpy data are also given in the form of equations and combined with thermodynamic data from other investigations to derive values of standard entha1pies of formation [(~HfO)], Gibbs energies of formation [(6GfO)], and logarithms of the equilibrium constants of formation (log Kf).

Jan 1, 1987

By Sterling J. Anderson

Through the use of nondestructive testing techniques, the Bureau of Mines is pursuing a goal of improving the efficiency of the rock excava-tion process. Toward this end, 44 laboratory tests were conducted to identify a practical method of monitoring fracture development in rock, as caused by an excavation tool. An acoustic emission CAE) transducer was used to monitor the test samples as they were loaded. The signal from this instrument was recorded in real time along with the radial and axial loads generated by the fracturing device. Through the review of these signals on a common-time base, it was possible to see the relationship between the developing fracture and the loading conditions. As a part of the posttesting investigations, samples that were pletely fractured were sawn and ground to expose the fractures. examination of these samples allowed approximations to be made incom-Visual of the total surface created. Surface area approximations were also made for the completely fractured samples. Quantitative analyses· of the AE signals were conducted for comparisons with the calculated surface areas.

Jan 1, 1987

By Alex C. Smith

This report describes laboratory studies conducted by the Bureau of Mines on the spontaneous combustion of U.S. coals. Approximately 11 pet of U.S. underground coal mine fires are attributed to spontaneous combustion. The relative self-heating tendencies of 24 coal samples were evaluated in an adiabatic heating oven. Minimum self-heating temperatures (SHT's) in the oven ranged from 350 C for a lignite and high-volatile C bituminous (hvCb) coal, to 1350 C for two low-volatile bituminous (lvb) coals. An empirical expression was determined predicting a bituminous coal's minimum SHT in the adiabatic oven based on the coal's dry ash-free oxygen content. Several factors that can affect the self-heating process were also evaluated. The self-~eating tendency of a coal increased when the coal was dried and exposed to humidified air, and was dependent on the particle size and oxygen concentration of the air. A new moderate-scale apparatus is described, in which the self-heating tendencies of larger coal samples, 3 kg, can be evaluated. The minimum SHT's of two coals were determined and the results were in good agreement with those found in the adiabatic oven. Finally, results of a test in the moderate-scale apparatus indicated a strong dependence of the self-heating rate of a low rank coal on the moisture content of the air.

Jan 1, 1987

By John W. Kopp

Stemming is used in blasting operations to help contain explosive gases as long as possible. Stemming can reduce airblast, improve fragmentation, and reduce the chances of hot explosive gases igniting methane and dust explosions in underground mines. Stemming is required in underground coal mines but is generally not used in underground metal and nonmetal mines. Some underground metal and nonmetal mines are classified as gassy and can require special blasting procedures such as the use of stemming to minsure the safety of miners. The types and amounts of stemming material that are desirable in underground metal and nonmetal mine blasting to ensure good or improved fragmentation while containing the hot gases are largely unknown. This Bureau of Mines research examined the effectiveness of differing lengths of stemming by measuring stemming ejection times as related to burden movement. With properly stemmed blasts, stemming is contained until some burden movement has occurred. Test blasts at two surface limestone quarries were evaluated using high-speed photography. For the conditions of these tests, a stemming length of at least 26 charge diameters was found to prevent premature stemming ejection. In tests with stemming lengths of 16 charge diameters, the stemming was effective but there was early venting of hot gases through fractures in the rock. Further testing with other rock types, hole diameters, explosive types, and stemming materials as they affect incendivity is recommended.

Jan 1, 1987

By F. J. Perzak

The Bureau of Mines conducted a flammability study of plastic ventilation ducts. Six rigid 16-in-diam fiberglass-reinforced plastic ducts from five manufacturers were examined using laboratory-scale, large-scale, and full-scale fire tests. The laboratory-scale tests included the American Society for Testing and Materials E162 radiant panel test, the E2863 oxygen index test, and the standardized small-scale flammability test (S3FT) developed by the Mine Safety and Health Administration (MSHA), U.S. Department of Labor, and replicated by the Bureau of Mines. Ten-foot lengths of the same ducts were also subjected to a large-scale vertical fire test, and 20-to 30-ft lengths were tested in a full-scale in-mine fire test at the Bureau's Lake Lynn Laboratory mine. The data from the laboratory-scale radiant panel test and oxygen index test indicated that the ducts were fire-resistant, However, five of the six ducts failed the S3FT and vertical fire tests, and four of the ducts failed the full-scale in-mine tests with flame propagation rates that ranged from 3 to 10 ft/min. The results indicate the need for improved fire-resistant plastic ducts. The good agreement between the S3FT re-sults and the vertical and full-scale tests show that the S3FT provides a good indication of the flammability of fiberglass-reinforced plastic ducting under realistic fire conditions.

Jan 1, 1987

By J. C. Kerkering

The Bureau of Mines used mathematical reliability theory to define, for use in the mining industry, the concepts of risk, safety, reliability, hazard, and mean time between accidents. In this report, the definitions are explained theoretically and illustrated by application to actual underground mine accident data extending over a 9-1/2-year period. The theoretical development proceeds along two parallel analytical paths. For each line of reasoning, the data are presumed to be independent. If they are not, the analysis stops, although there are interesting implications when dependency is demonstrated. The first method uses the elapsed times between accidents as the basic data. These elapsed times are fitted to a negative exponential distribution function using least squares and yielding the function parameter, P1 The P1 is used to form the Poisson distribution function for the data, which is then used to define the safety-related concepts. The second method uses the maximum likelihood estimator to formulate a Poisson distribution function for the data. The function is tested for adequacy by a goodness-of-fit test; if the fit is acceptable, the Poison function is used to define the concepts. Both methods were applied to the data base, yielding nearly identical results.

Jan 1, 1987