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By C. M. McCulloch, Maurice Deul

A geologic study of Mines 32 and 33 in Cambria County, Pa., was conducted as part of a methane control research program. Areas of high methane emission and roof instability are encountered which are related to the structural and stratigraphic features that characterize the geologic setting of these mines. Locally the folds trend N 20° E ±2°, the direction of the butt cleat in the Lower Kittanning coal. The face cleat strikes at N 69° W ±2° and the systematic rock joint in the surface bedrock strikes N 67° W ±2°This suggests that a directional stress oriented N 70° W produced the folds and influenced the directions of coal cleat and systematic joint sets. Analysis of SLAR indicates three directions of prominent regional lineation: N 39° E, N 31° W, and N 70° W. Little gas was encountered during development mining; large volumes of gas are encountered when roof falls. Most of the gas comes from strata above the mined coal; therefore, to control methane, roof instability must be controlled. Roof falls and high rates of methane emission are most likely where less than 30 feet of many thin layers of limestone, shale, and sandstone occurs between the Lower Kittanning coal and the next coal and in zones along the margins of a sandstone channel.

Jan 1, 1973

By C. M. McCulloch

A geologic study of Mines 32 and 33 in Cambria County, Pa., was conducted as part of a methane control research program. Areas of high methane emission and roof instability are encountered which are related to the structural and stratigraphic features that characterize the geologic setting of these mines. Locally the folds trend N 20° E ±2°, the direction of the butt cleat in the Lower Kittanning coal. The face cleat strikes at N 69° W ±2° and the systematic rock joint in the surface bedrock strikes N 67° W ±2°. This suggests that a directional stress oriented N 70° W produced the folds and influenced the directions of coal cleat and systematic joint sets. Analysis of SLAR indicates three directions of prominent regional lineation: N 39° E, N 31° W, and N 70° W. Little gas was encountered during development mining; large volumes of gas are encountered when roof falls. Most of the gas comes from strata above the mined coal; therefore, to control methane, roof instability must be controlled. Roof falls and high rates of methane emission are most likely where less than 30 feet of many thin layers of limestone, shale, and sandstone occurs between the Lower Kittanning coal and the next coal and in zones along the margins of a sandstone channel.

Jan 1, 1973

By J. E. Doo1ey

To process and use the heavy ends of petroleum effectively, the development of suitable separation and characterization procedures not currently available was required. A systematic procedure was developed by the Bureau of Mines using such techniques as isothermal and molecular distillation, chemical treatment, silica-alumina gel chromatography, gel permeation chromatography, and spectrometry. Using these techniques, the Bureau achieved a detailed separation and characterization of a 370° to 535° C distillate from Gach Saran, Iran, crude oil. Such a systematic procedure and the semiquantitative data resulting therefrom should be of value in selecting feedstocks and in optimizing petroleum processing operations.

Jan 1, 1973

By E. G. Davis

Large-scale ultrafine grinding tests of a coarse kaolin were made using the Bureau of Mines developed attrition grinding process in continuous open-and closed-circuit systems. A 20-inch diameter attrition grinder, designed and constructed at the Tuscaloosa Laboratory, was used. Studies included single- and multiple-stage open-circuit grinding, and also continuous grinding tests in closed-circuit with a 6-inch-diameter solid bowl centrifuge. Clay feed, containing 9.0 percent minus-2-micrometer esd, was used at fates up to 840 pounds per hour. Multistage grinding tests gave better results than single-stage treatment when equivalent clay feed rates were used. Closed-circuit grinding tests yielded ground products containing slightly more minus-2-micrometer-esd clay than the open-circuit grinding when using the same clay feed. Energy consumption was lower in closed-circuit grinding than in batch or open-circuit grinding. A modified two-stage closed-circuit grinding system gave the best grade of product and amount of minus -2-micrometer-esd clay produced per pound of clay feed. The ground product from this test contained 88.5 percent minus-2-micrometer-esd material and electrical energy consumption was 327 kilowatt-hours per ton of minus-2-micrometer-esd material produced.

Jan 1, 1973

By T. F. Tomb

Past experience has shown that the penetration characteristics of the 10-mm nylon cyclone used on approved personal sampling equipment are significantly different from those determined in the laboratory using a nonpulsating flow source. The Bureau of Mines has developed and recommended a modification to presently approved equipment that will alleviate this difference. However, as a result of this modification, a new relationship for converting respirable dust concentrations measured with approved personal sampling equipment to equivalent concentrations as measured with an MRE instrument will have to be established. This Bureau of Mines report describes the underground sampling program conducted to establish a new factor for converting respirable dust concentrations measured with personal sampling equipment, modified with a recommended pulsation damping device, to an equivalent concentration as measured with an MRE gravimetric dust sampler.

Jan 1, 1973

By William J. Campbell

This analytical method development and evaluation was undertaken by the Bureau of Mines to provide accurate determinations of eight minor elements in low-alloy steels prepared from ferrous scrap. Fluorescent X-ray spectrography was the principal method investigated. Confirming analyses were made by conventional instrumental and chemical methods. All X-ray data were processed by a timesharing computer. No corrections were found necessary for inter-element effects or overlapping spectral lines. Concentrations were calculated from the least-square fit of a linear calibration equation derived from measurements on three sets of standard steels. These studies show that X-ray spectrographic analysis of lathe-finished surfaces provides accurate determinations of aluminum, copper, chromium, manganese, nickel, phosphorus, silicon, and tin.

Jan 1, 1973

By J. B. Rosenbaum

Prolonged laboratory and limited pilot plant tests have shown that the Bureau of Mines buffered S02 -H2S process is capable of removing 95 to 99 percent of the S02 from industrial waste gases. Most of the S02 is converted to elemental sulfur; only about I percent converted to sulfate The process comprises (1) washing the flue gas to remove particulates and S03, (2) absorption of the S02 in citric acid or other carboxylate solution, (3) reaction of the loaded solution with H2S in a closed vessel to precipitate the absorbed S02 as elemental sulfur, and (4) separation of the sulfur from the regenerated solution by oil flotation and melting. Two-thirds of the molten sulfur is converted to H2S for use in the sulfur precipitation step by reacting sulfur vapor with natural gas and steam in the presence of an alumina catalyst. The chemistry and mechanism of the process are described, initial laboratory and pilot plant data are summarized, and second-generation laboratory operation and pilot plant design are reviewed. Preliminary cost estimates are presented for recovering sulfur from copper smelter gas, powerplant flue gas, and Claus plant tail gas.

Jan 1, 1973

By Laurence G. Trudell

Geology and oil-yield data are presented for a 58-square-mile area encompassing the U.S. Department of the Interior oil-shale leasing program tracts in the western Washakie Basin, Sweetwater County, Wyo. Lithology and oil yields of samples from three Bureau of Mines coreholes are evaluated and correlated with Kinney Rim surface sections measured and sampled by the U.S. Geological Survey. Minable sections of oil shale averaging up to 25 gallons of oil per ton crop out on Kinney Rim in the Laney Member of the Green River Formation. Thick oil-shale sections in the Laney Member that average 15 gallons per ton represent 155 million barrels of oil in place per square mile. In the lower part of the Green River Formation the Tipton Shale Member contains a 20-to 40-foot section averaging 15 gallons per ton. Beds of high-volatile C bituminous coal up to 6 feet thick are present in intertongued parts of the lower Green River Formation and upper Wasatch Formation.

Jan 1, 1973

By L. L. Oden

The purpose of this research was to develop a method to remove copper and tin from the magnetic fraction of incinerated municipal refuse, as recovered by the Bureau of Mines pilot plant in College Park, Md. Copper, present in the scrap in a metallic form bonded to ferrous objects, was amenable to leaching in cupric ammonium carbonate solution. Copper levels in small 5-to 10-lb lots of treated scrap were reduced from the initial level, 0.5 to 0.6 pct, to 0.1 to 0.2 pct. Larger lots of scrap (100 lb) were treated less effectively because of poor contact of solution and scrap. Oxidation in the air or in aerated aqueous solution was applied to liberate tin from the dilute solid solution present on the surface of incinerated tinplate. Shredding of air-oxidized scrap or caustic leaching of scrap oxidized in solution reduced tin levels from the initial 0.25-pct level to about 0.1 pct.

Jan 1, 1973

By Mark I. Copeland

The Bureau of Mines investigated the effect of up to 1 wt-pct of copper and silicon on the heat treatment response and hardness, tensile, and impact properties of hot-rolled medium-carbon steels. The steels were prepared by induction melting and fabricated into plates by forging and rolling. The tensile strength of 0.2-wt-pct carbon steels containing 0.3 wt-pct silicon was affected significantly by copper in both the hot-rolled and heat-treated (600° C) conditions, whereas the tensile strength of the 0.3-wt-pct carbon steels was less affected. A 600° C treatment was considered optimum as a post-rolling treatment to strengthen the steels by copper precipitation. Strengthening of 0.2-wt-pct carbon steels by silicon was reduced by increasing copper contents.. Optimum impact strengths occurred at about 0.3 wt-pct silicon in 0.2-wt-pct carbon steels containing 0.6 and 0.8 wt-pct copper. The impact strengths were lowest for 0.2-wt-pct carbon steels containing over 0.8 wt-pct copper and greater than 0.3 wt-pct silicon, especially in the heat-treated condition. Copper and silicon solutes and copper precipitates strengthened the steels. This effect was augmented slightly by strengthening through grain refinement by these solutes.

Jan 1, 1973

By K. O. Bennington

Enthalpies of formation of three sodium titanates were determined by hydrofluoric acid solution calorimetry, The values obtained for formation from the elements at 298.15° K are -370.9±0.5 kcal/mole for Na2TiO3, -832.1±0.9 kcal/mole for Na2Ti307, and -1,510.9±1.7 kcal/mole for Na2Ti6013. Tables of enthalpies of formation and Gibbs energies of formation are given as a function of temperature both from the elements and from the component oxides for Na2Ti03 and Na2Ti307.

Jan 1, 1973

By M. Hertzberg

Results of a comprehensive study of the absolute spectral radiance of the infrared emissions from methane-air explosions are reported. The spectral growth of these expanding flames were recorded with a time resolution of 1 msec in the spectral range of 1.7 to 5.0 µm. Time-resolved spectra were obtained for methane-air mixtures as a function of stoichiometry, nitrogen dilution, and Halon dilution, in a 9-liter vessel under different venting conditions. Data are also presented for coal dust-air explosions. Temperatures, obtained from the absolute radiances and from a band ratio technique for methane-air, are internally consistent and are generally 50° to 200°K below adiabatic flame temperatures. All near limit mixtures gave essentially the same flame temperatures (1,500° to 1,600° K) regardless of whether the limit was obtained by dilution with excess air, excess methane, excess nitrogen, or Halon. The coal dust explosion spectrum is essentially a blackbody continuum at 1,500° K with some selective emission at 4.4 µm from hotter CO2. The data are analyzed in terms of the radiative dynamics of a sperically expanding flame zone. The importance of radiative transport is assessed. An equation is derived which relates the instantaneous fraction of combustion power radiated to adiabatic variables.

Jan 1, 1973

By L. A. Haas

Hydrogen sulfide was decomposed to elemental sulfur in an electrical discharge. With He, N., or Ar diluents, a threshold voltage between 1 and 3 kV was required for the decomposition reaction to occur in a laboratory ozonizer. Above the threshold voltage, the HAS decomposition rate increased with increasing voltage, but the increase was more pronounced with argon diluent than with either nitrogen or helium. In common with other reactions in an electrical discharge, the B2S decomposition decreased with increasing temperature in the range of -410 to +61° C. The reaction did not appear to be rate-controlled by a solid-gas sorption step because the introduction of activated charcoal into the electrical discharge zone did not significantly affect the decomposition yield. In the presence of polymeric chlorofluoro-carbon oil, 90 pct conversion of the 3 pct H2S in helium was obtained at 14 kV, 60 Hz, a 2-mm electrode gap, and a gas-residence time greater than 1 min. Under the same experimental conditions in the absence of oil, the conversion was only about 50 pct.

Jan 1, 1973

By Charles W. Huggins

To determine the nahcolite and dawsonite content in oil shales, the Bureau of Mines compared X-ray diffraction, infrared spectroscopy, thermal methods, and a previously published method by Smith and Young based on the selective solubility of sodium compounds. The Smith and Young method and a new method based on the weight of carbon dioxide produced by thermal decomposition are recommended for determining nahcolite. X-ray diffraction and the Smith and Young method are recommended for determining dawsonite. X-ray diffraction, infrared spectroscopy, and differential thermal analysis were useful for identifying other minerals in the samples.

Jan 1, 1973

By Joseph Grumer

In addition to nine powder and gaseous extinguishants of propagating Pittsburgh seam coal dust-air explosions earlier evaluated,6 10 other powders have similarly been evaluated under like conditions such that wall quenching of the coal dust-air flames was virtually absent and the dust concentration was temporally and spatially uniform to within about ±5 percent. None of the newly examined extinguishants was better than Purple-K (potassium bicarbonate); the 10 of this report are anhydrite (calcium sulfate), monobasic (4 types) and dibasic ammonium phosphate, natural and synthetic cryolite (sodium fluoalumi-nate), sodium sulfate, and tricalcium phosphate. Except for anhydrite, sodium sulfate, tricalcium phosphate, and the cryolites, these materials were about equally effective, when present in relatively low concentrations (weight-percent of the coal dust-extinguishant mixture). The maximum oxygen concentration for the extinguishment of otherwise uninhibited coal dust explosions and the influence of coal dust particle size and the volatile content of the coal were also explored. For the present, the choice of the inhibitor among the good ones evaluated is not as critical as the system to be used to deploy the extinguishant against a coal dust explosion.

Jan 1, 1973

By E. L. Burwell

Application of the in situ recovery process to oil shale was tested during two field experiments near Rock Springs, Wyo. The results of these tests demonstrate that a self-sustaining combustion zone can be created in an oil shale body, that this zone can be moved through the oil shale, and that the process will produce shale oil. Evaluation of the combustion process by monitoring produced fluids for physical and chemical properties and volumes is described. The material and energy balance obtained is compared with a second evaluation based on extensive coring of the test area after the test was terminated. Several side results of the research are noted such as ground surface heating by underground burning and production of low-to medium-Btu gas during retorting.

Jan 1, 1973

By J. W. Walkiewicz

Studies were conducted by the Bureau of Mines to develop a method for fabricating Sm-Co permanent magnets. This method consisted of arc-melting, crushing and grinding the alloy, alining and pressing the powder, and sintering the green compacts. Results indicated that the optimum composition was 36.7±0.3 weight-percent Sm and 63.3±0.3 weight-percent Co. This composition was obtained by blending together Sm2C07 and SmCo5. The maximum values exper¬imentally obtained were MHC = 27.4 kOe, BHc = 7,510 Oe, Br = 7,810 G, and (BH)max = 15.1 MGOe. The optimum sintering temperatures and grinding times for maximum MHc and (BH)max were determined. Lowering the grinding temperature from 0° C to -60° C resulted in a significant increase of magnetic properties.

Jan 1, 1973

By Stanley C. Rhoads

The Bureau of Mines investigated the complete ternary system K2 HfF6¬K2ZrF6-l.25 weight-percent HF at 40° C. In addition, solubility curves have been established at 25°, 30°, 500, 60°, and 70° C. These solubility data implemented a study of hafnium enrichment in feed solutions for liquid-liquid extraction processes.. Selected K2HfF6-K2 ZrF6-1.25 weight-percent HF mixtures were equilibrated in a constant temperature bath. Compositions of the equilibrated solutions and wet residues were established from combined hafnium and zirconium oxide and total fluorine analyses. All solubility curves were essentially parallel on triangular coordinates. At 40° C, the solid phase of the K2HfF6-K2ZrF6-1.25 percent HF system is a series of solid solution hydrates with K2HfF6-H20 and K2ZrF6.3H2O segments existing at the respective extremes. Since this system contains K2HfF6-H20 and K2ZrF6.3H20 segments, it is not ideal for simple separation of high-purity K2HfF6 from K2HfF6-K2ZrF6 mixtures by recrystallization. However, it would be useful for producing hafnium-enriched feed solutions from zircon concentrates for liquid-liquid extraction of hafnium from zirconium.

Jan 1, 1973

By F. E. Spencer

This Bureau of Mines report provides a complete mathematical description of the algorithm employed by a general multiphase chemical equilibrium program developed particularly for the purpose of studying problems in coal combustion, although the generality of the program will allow its application to any equilibrium system in which an appreciable gas phase is present. When applied to coal combustion problems, the program predicts composition and quantity of slag and unconsumed carbon phases as well as calculates accurately the composition of the gas phase including trace species such as free electrons and ions which are important for predicting electrical properties.

Jan 1, 1973

By Parviz F. Rad

The increased use of tunnel boring machines (TBM) has stimulated laboratory research to optimize the cutting parameters of these machines with the objective of increasing machine efficiency and penetration rate. Laboratory-scale rock cutting experiments have succeeded in identifying many of the important parameters involved in rock-cutter interaction. Although scaling factors may be required to apply the results directly, the concepts developed can be used qualitatively as design guidelines for boring machines. The Bureau of Mines Twin Cities Mining Research Center has recently developed a large-scale rock cutting device (RCD) that will simulate many of the operating parameters of the tunnel boring machines in the laboratory under a controlled environment. The results of the experiments with this device will be directly applicable to the design of TBM's.

Jan 1, 1973