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By T. D. Ralston

This Bureau of Mines report presents a mathematical model for heterogeneously catalyzed chemical reactors operating under turbulent conditions. The model includes reaction kinetics on the catalyst surface as well as diffusion of the reacting components within the reactor. Three applications of the model to tube-wall methanation reactors are discussed. The first application is a computation of catalyst activity from measured reactor data. This result is then used in a reactor sizing problem and a problem of reactor simulation with recycle. In addition to the reactor model, a novel approach to solving the recycled reactor problem is given.

Jan 1, 1974

By C. Melvin Lepper

The Bureau of Mines has developed an improved earth resistivity field system which employs a novel technique for obtaining null measurements. The instrument is designed to operate reliably in high-noise environments such as those found in the vicinity of operating mines. The system consists of a low-frequency transmitter, a sensitive receiver and an external battery pack, each in its own case to provide protection from the elements. The receiver and transmitter units have self-contained recharge-able batteries to supply power to the circuitry and separate built-in battery chargers that operate on standard 115 Vac power. The system is portable and simple to operate. Measurement accuracy, reliability, and dynamic range are superior to most commercially available equipment even though less time and effort is required to make null readings. Unlike some commercial systems, long integration times are not required to enhance signal-to-noise ratio in areas of high background noise.

Jan 1, 1974

By F. W. Wood

The Bureau of Mines has sought clarification of the Ti-TiN system by studying the phases formed by diffusion reactions between titanium and titanium nitride. Reaction couples were prepared by embedding pockets of TiN powder in arc-melted buttons of titanium. Specimens were vacuum annealed at nominal temperatures of 800°, 950°, 1,200°, and 1,500° C. Metallographically mounted cross sections from reacted specimens and from some that were not annealed were examined optically, with an electron microprobe, with an election microscope, and by X-ray diffraction. Each annealed specimen contained a segregated core primarily of d-phase material, an ?-phase diffusion layer, an a-phase diffusion layer, and host metal. On the basis of corresponding microprobe analyses, and considering results of certain other research, a new phase diagram is proposed. It contains no qualitative innovations, only quantitative adjustments. Results were also analyzed from the viewpoint of diffusion behavior. Diffusion coefficients calculated for the ? phase were sufficiently scattered that the parameters are very tentative. Nevertheless, the diffusion behavior reported is in reasonable agreement with one of two prior studies if it is assumed that the earlier investigators were mistaken in their identification of the nitride phase in which the diffusion occurred.

Jan 1, 1974

By H. G. Lucas

A feeder screw supplied at constant pressure by a hopper-orifice arrangement was developed for feeding solids in size ranges up to several hundred micrometers at constant flow rates. Performance of the feeder was evaluated by measuring the flow rates obtained with 3-to 7-micrometer coal ash, 70 percent through 200-mesh coal, and minus 325-plus 400-mesh coal ash. Constant feed rates within a few percent of set values were achieved for half-hour periods for the larger particles and for 5-minute periods for the finer particles. Suggestions are given for feedstock preparation and feeder operation for optimum performance.

Jan 1, 1974

By D. E. Hirsch

The Bureau of Mines has developed a systematic procedure for separation, characterization, and semiquantitative analysis of high-boiling (350° to 550° C) distillates of crude oils. Isothermal and molecular distillation were used to prepare the 370° to 530° C distillate of Recluse, Wyo., crude oil. The distillate was separated into fractions by chemical treatment, silica-alumina gel adsorption, and gel permeation chromatography (GPC). The fractions were analyzed by use of GPC correlations and mass and nuclear magnetic resonance (NMR) spectrometry. The increased knowledge of petroleum composition obtained from the data will contribute to improved petroleum processing and utilization and energy conservation.

Jan 1, 1974

By F. E. Armstrong

An instrument using a gamma-ray backscatter technique for determining the weight-percent incombustibles content of coal dust and rock dust mixtures in coal mines has been built and tested. The unit gives a direct readout in per-cent incombustibles for coal mine dust mixtures containing between 50 and 100 percent incombustibles; calibration of the device requires using a sample of the rock dust employed; this is usually limestone but occasionally dolomite or gypsum. A small americium-24l source is used with a scintillation detector whose output feeds a rate meter. The source-detector geometry used was chosen to reduce the effects of variation in bulk density. Accuracy of the system is within ±3 percent for most mixtures. The instrument is portable and completely self-contained; the rechargeable batteries supply power for 300 to 400 determinations.

Jan 1, 1974

By W. T. Abel

The Bureau of Mines tested 48 materials for their ability to absorb H2S from hot simulated producer gas (1,000°-1,500° F). The material found best from the standpoint of absorption capacity, durability, and amenability to regeneration was sintered pellets of 75 percent fly ash-25 percent Fe203. The performance of this absorbent under simulated and actual conditions is described. The effect of absorbent composition, absorbent temperature, steam content of the gas, and tar vapors and dust in producer gas is discussed.

Jan 1, 1974

By T. O. Llewellyn

The Bureau of Mines investigated the use of a heavy liquid in combination with fluid cyclones to separate brucite from a Nevada ore on a continuous basis, using a mixture of dibromomethane and trichloroethylene having a density of 2.44 grams per cubic centimeter. Single-stage cyclone separation produced a concentrate that contained 84 percent of the total magnesia at a grade, on a calcined basis, of 95.6 percent MgO.

Jan 1, 1974

By E. D. Calvert

The room temperature tensile properties of commercially pure titanium and seven titanium alloys prepared by skull casting were determined in the as-cast and heat-treated conditions. Data were compared with property data from tensile tests on wrought alloys of the same compositions in the as-worked and heat-treated conditions. The alloys evaluated were Ti-5Al-2.5Sn, Ti-6Al-4V, Ti-6Al-4V-lSi, Ti-6A1-2Sn-4Zr-2Mo, Ti-6A1-6V-4Zr-4Mo, Ti-6A1-6V-2Sn, and Ti-11.5Mo-6Zr-4.5Sn. Test specimens were prepared from both static and centrifugal castings and from plate fabricated by forging and rolling vacuum-melted ingots. The data indicate that the alpha and alpha-beta alloys have strength properties in the as-cast condition that are reasonably close to the strength properties of their wrought counterparts in the as-worked condition. An exception to this was the Ti-6A1-6V-4Zr-4Mo alloy for which insufficient data were available to form any firm conclusions. Fine-grained cast structures of Beta III (Ti-11.5Mo-6Zr-4.5Sn) were shown to be generally stronger in the as-cast condition than the wrought alloy in the as-worked condition except for the yield strength of one structure that was unusually low. Heat treatment of this alloy produced properties that were unpredictable. Indications are, however, that optimization of heat treatment parameters for each cast structure could produce strength properties equal to that of wrought materials.

Jan 1, 1974

By H. O. Poppleton

This Bureau of Mines study was made to investigate a possible method for selectively removing the Si02 component of silicate minerals and ores. Of specific interest were aluminum ores and zircon. Methods are described for removing Si02 from these ores as volatile silicon sulfides by treating the ore with sulfur and carbon; with sulfur, carbon, and a reducing gas; or with sulfur compounds and carbon. Comparative results are also given for the desilication of some of the ores with carbon alone to form volatile silicon monoxide. The silica component can be removed partially from bauxites at temperatures above the sublimation temperature of SiS (940° C) by treatment with carbon, sulfur, and methane; however, it is more difficult to remove the silicon from kyanite, manganese silicate, red muds from aluminum processing, kaolinite, lateritic nickel ores, and zircon. Complete desilication requires temperatures ranging from 1,100° C for bauxite to 1,450° C for zircon. Although the high temperatures required and the undesirable metal sulfides produced eliminate practical application of this method using present technology, the Bureau is reporting this data so that they will be available to future investigators.

Jan 1, 1974

By M. C. Irani

The Bureau of Mines, in cooperation with the Mine Safety Appliances Co., has developed a continuous-recording methanometer utilizing a catalytic combustion detector. The methanometer, which is presently operating at 22 exhaust fans at 14 mines in the Eastern coalfields, is reliable and simple to install, operate, and maintain. The instrument and the details of its installation and calibration are described. Analytical data obtained by infrared spectrophotometer and gas chromatograph are presented to substantiate its re liability.

Jan 1, 1974

By W. K. Overbey

The Bureau of Mines conducted surface joint and stress measurements, airborne remote sensing imagery studies, compass-oriented borehole televiewer surveys, numerical simulation of fractured wells, and well productivity studies in a four-quadrangle study area of Ohio, to determine the effects of earth fracture systems on the deliverability of gas storage fields. The results of these studies indicate that much useful information about a gas storage reservoir can be obtained and put to practical use by studying--(1) oriented cores for fractures and directional permeability, (2) orientation of induced hydraulic fractures for alignment of well patterns, and (3) aerial photos and multispectral scanner imagery for general surface geology comparison and to determine if some, development patterns can be generated by such results. The absence of known tectonic elements associated with flat-lying sediments, such as faults or fracture zones that can be seen on the surface, indicates that the use of remote sensors such as radar or aerial photography is not likely to be useful in picking well locations for drilling. Studies similar to those discussed here should be conducted in gently folded and strongly folded sedimentary formation areas to determine if the increased knowledge of earth fracture systems under these conditions might be beneficial in gasfield and gas storage reservoir development.

Jan 1, 1974

By M. B. Shirts

Bench-scale studies were made on a reductive hydrometallurgical procedure to convert chalcopyrite flotation concentrate to copper metal or a readily leachable sulfide. Reductive conversion of chalcopyrite and dissolution of iron and sulfur were accomplished in hydrochloric or sulfuric acid solution by the addition of metallic copper, iron, or lead. Use of metallic copper as the reductant enabled extraction of 95 and 46 percent of the iron and sulfur, respectively. The products were ferrous iron, hydrogen sulfide, and a copper sulfide. Use of metallic iron or lead as the reductant enabled extraction of 95 percent of both the iron and sulfur. The products obtained with metallic iron or lead were ferrous iron, hydrogen sulfide, and metallic copper.

Jan 1, 1974

By D. P. Lindroth

The thermal diffusivity above 298 K, up to 400 K and at pressures from ambient down to 10-10 torr was measured for the following six igneous rock types: tholeiitic basalt, obsidian, rhyolite, granodiorite, gabbro, and dunite. The thermal diffusivity data were obtained by the laser flash method. Extreme values range from a low of 5.3X10-3 cmF/sec for rhyolite at 383 K and 2X10-7 torr to a high of 13.4x10-3 crrf/sec for dunite at 298 K and 760 torr. Data are also included on a commercial fused silica, which was used as a standard.

Jan 1, 1974

By J. L. Holman

The Bureau of Mines, at its Rolla Metallurgy Research Center, has devised methods for separating and reusing the major portion of waste plastics discarded in urban and industrial refuse. Waste plastic concentrates from a local collection drive, recycling center collections, urban refuse pilot plants, and the secondary metals industry were separated into three major thermoplastic families--polyolefins, styrenes, and vinyls--based on differences in density using a Bureau-designed sink-float-elutriation hydraulic separator. Other separation methods and systems such as air classification, jigging, liquid media, screening, and electrostatics were studied. Vinyl plastics contain up to 50 percent HC1. It was found that over 90 percent of the HC1 in vinyls can be recovered as usable hydrochloric acid by pyrolysis at 350° C. The remaining pyrolysis products which had heats of combustion in excess of 12,000 Btu/lb, could become valuable as a future source of energy. A characterization study conducted on eight chopped wire insulation wastes from secondary copper and aluminum processors showed that most wastes contained 2 to 7 percent residual metal and large percentages of vinyl. The residual metal content of some of these wastes was lowered to 0.1 percent and the vinyl portion segregated using various separation techniques. The research also suggests ways in which reclaimed thermoplastics may be fabricated into useful products.

Jan 1, 1974

By Z. J. Fink

Ultraviolet-visible and infrared emission spectra from propagating methane-coal-dust-inhibitor mixtures have been obtained in a 0.2-by 0.2¬by 5.3-m vertical duct over a range of flame speeds from 2 to 100 m/sec. Results serve as a basis for the design and evaluation of thermal radiation detectors for triggered barriers that suppress ongoing mine explosions. Of particular significance is the large continua superimposed on the methane-air spectra when small amounts of coal dust are present and the variation of emissivity with infrared (IR) wavelength in dust flames. In conjunction with the spectral measurements, studies of flame speed, particle size, gas sampling plus thermodynamics, and dust sampling are presented and discussed in order to gain insight into the more fundamental aspects of propagating explosions. Sampling results have shown that only a near-stoichiometric amount of dust is consumed in the flames studied even though initial concentrations are five times stoichiometric. Difficulty in propagating coal-dust inhibitor flames of realistic mine characteristics in a cold-walled laboratory duct has been encountered. A simplified analysis of the flame zone utilizing spectral and sampling results indicates that the stability of slowly propagating flames is more dependent upon thermal radiation than upon convection losses to the walls. It is predicted that thermal radiation losses will make any measurements of coal dust burning velocities, "quenching diameters," or flammability limits more apparatus dependent than those corresponding to gaseous fuels.

Jan 1, 1974

By Masami Hayashi

Cost evaluations were made for five processes for producing 100,000 tons of electrorefined copper per year from a chalcopyrite concentrate. The processes were (1) conventional smelting with all furnace gases vented to the atmosphere; (2) conventional smelting with converter gases routed to an acid plant and reverberatory gases vented to the atmosphere; (3) conventional smelting with converter gases routed to an acid plant and reverberatory gases to a citrate system plant; (4) conventional smelting with all furnace gases routed to a citrate system plant; and (5) a modified smelting process in which the concentrate is roasted before being charged to the reverberatory furnace, with roaster and converter gases routed to an acid plant. The total fixed capital costs of the plants were estimated as (1) $56.7 million, (2) $77.4 million, (3) $87.2 million, (4) $73.9 million, and (5) $77.0 million, respectively. Total S02 removal from stack gases as sulfuric acid or sulfur for each process was (1) none, (2) 66 percent, (3) 99 percent, (4) 98 percent, and (5) 78 percent. Assuming no credit for byproduct sulfur or sulfuric acid, total operating costs per pound of electro-refined copper produced were estimated as (1) $0.081, (2) $0.103, (3) $0.119, (4) $0.111, and (5) $0.103, respectively.

Jan 1, 1974

By W. L. Brien, O&apos

Molybdenum alloys with good strength properties at elevated temperatures were produced by the powder metallurgical internal oxidation method previously applied to tungsten and known as oxyreaction strengthening. Commercial molybdenum powders were blended with 0 to 10 pet of a reactive powder, ZrMo2. The effects of composition, blending procedure, and sintering conditions on strength properties at elevated temperatures were studied. Strengthening was attributed to zirconium in solid solution with molybdenum and to the presence of submicrometer particles of Zr02. Several alloys had tensile strength and stress-rupture properties com-parable with those of the best commercial alloys. The maximum tensile strengths obtained were 92 kpsi at 1,200° C and 53 kpsi at 1,316° C. The maximum stress-rupture life at 30 kpsi and 1,200° C was 145 hours.

Jan 1, 1974

By Paul Biggs

This Bureau of Mines report contains information on 63 water flood projects in Colorado. Water was injected in 10 formations located in 58 oilfields. Specific field data presented include location, discovery, development, water supply, fluid injection, oil and water production, oil reserves, and oil recoveries by primary and secondary methods. An estimated 3.5 billion barrels of water has been injected to recover approximately 533 million barrels of oil, a ratio of 6.57 to 1. Most of the injection water is from alluvial deposits, although produced water is used in many fields. Injection water treatment is not a major problem. Appraisal of project success or failure in this report is based on technical, rather than economic, information.

Jan 1, 1974

By K. J. Miller

Electrophoretic mobility measurements of coal and pyrite particles in distilled water revealed a difference between the migration speeds of the two materials toward the anode in a dc electric field. This information led to the development of a laboratory electrophoresis column for separating fine pyrite from coal by utilizing the electrokinetic and the specific gravity differences between coal and pyrite. The study demonstrated on a laboratory scale that pyrite and other impurities can be separated from fine coal by electrophoresis using a stage separation technique. In a cost analysis, electrical power for electrophoresis was extrapolated to about $1 per ton of clean coal product. But, since the only successful tests ever made were in the laboratory with prewashed samples of minus 100-plus 325-mesh coal in distilled water, the cost figure derived is not representative of conditions prevalent in commercial coal cleaning operations. True conditions would reflect costs many times as great. In the course of the work, several scale-up techniques were considered but their feasibility became academic in view of the physical and economic problems associated with electrophoretic separation of pyrite from coal. Although the process and apparatus were finally deemed impractical for commercial coal preparation, the electrophoresis column may have some application as a laboratory device.

Jan 1, 1974