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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

By Roger J. Morrell

Bureau of Mines laboratory experiments with reduced scale cutter and cutter forces were performed to (1) define the fundamental relationships governing disk cutter performance and (2) to develop a method of predicting disk cutter performance in soft, medium, and hard rocks. The rock cutting experiments were performed in four igneous and metamorphic rocks that ranged in compressive strength from 38,000 to 67,000 psi. A special testing machine called a linear cutter apparatus (LCA) was used to load and traverse a free rolling disk cutter across a smooth rock surface. Each pass of the disk produced a single crater, and runs were spaced to avoid breakage between craters. During each run the normal and tangential cutter forces were measured and recorded. The soft and medium rock data were obtained from previous Bureau experiments with disk cutters. Crater depth, tangential cutter force, crater volume, specific energy versus normal cutter force, and crater width versus depth are defined within this study. With the use of standard physical properties, performance prediction equations were developed using stepwise linear regression analysis techniques. A method of using these prediction equations to calculate the boring rate, the cutter spacing, and the torque and energy requirements of a full-scale boring machine was also developed.

Jan 1, 1974

By Eugene H. Skinner

This Bureau of Mines report describes the fieldwork and subsequent analysis to determine physical properties, stress distribution, and several aspects of rock behavior as a necessary evaluation for a typical mine opening. All work was done at a test site on the 3300 level, Crescent mine, Coeur d'Alene mining district, Idaho. Free field stress beyond the influence of the opening was also determined. Conventional overcore technique with the three-component borehole deformation gage developed by the Bureau of Mines was used in three drill holes. Three field verification tests were performed using a gage newly developed by the Spokane Mining Research Center in an approach herein termed "initial deformation method." Use of this method validated that aspect of overcore theory which predicts that similar deformation effect occurs in the wall rock around the perimeter of an opening in rock under stress. Also described are all drilling procedures and performances. Physical property determinations were made on rock samples obtained from the three overcore drill holes. Twelve physical properties with a total of [532] values were obtained at various drill hole orientations and depths. Exhaustive statistical tests were utilized in the analysis of these physical properties. Further elaborated are statistical inferences based on these analyses. Extensive analysis and interpretation of Crescent mine geology are also described.

Jan 1, 1974

By Roy L. Wilfong

Infrared reference spectra are presented of compounds of importance in lead sulfide flotation research. Included are the spectra of several short chain alkyl xanthates of lead and zinc, the corresponding dixanthogen compounds, and the common oxidation products of lead sulfide and their sodium analogs. The spectra of several frequently used industrial flotation reagent xanthates are also presented. A thorough, well-documented discussion is given of the various corrections made to correct the as recorded absorption band data to near absolute values.

Jan 1, 1974

By Richard A. Busch

Inadequate engineering design criteria for coal refuse embankments has allowed hazardous impoundment structures in coal mining areas to be created. A necessary first step to develop adequate design criteria is the determina¬tion of basic, respresentative physical property data on the materials that constitute typical refuse embankments. An extensive field and laboratory program was undertaken by the Federal Bureau of Mines. Much physical property data was generated. Additonal petrographic analysis and large scale triaxial compression testing was performed by others. The data presented here should aid in establishing design parameters for coal refuse embankments

Jan 1, 1974

By Ann G. Kim

Hydrocarbon gases, primarily methane but also the C2 through C5 paraffins, the C2 and C3 olefins and possibly the C4 and C5 olefins, are byproducts of coal formation. Although it is generally believed that coal formation occurred at temperatures below 200° C, most experimental work on gas formation from coal has been performed at temperatures between 200° and 1,000°C. The objective of this Bureau of Mines experiment was to determine if observable changes in the gases from coal could be produced at temperatures below 200° C in relatively short periods of time. The experiment involved heating coal samples from six coalbeds at constant temperatures and analyzing evolved gases. The composition of the gases at three temperatures was compared. At 35° C, over 99 pct of the gas is methane; at 125° and 150°, methane constitutes approximately half of the hydrocarbon gas. Isobutane and pentane are the predominant higher hydrocarbons at temperatures between 100° and 150° C.

Jan 1, 1974

By Ann G. Kim

Hydrocarbon gases, primarily methane but also the Ca through Cs paraffins, the Ca and C3 olefins and possibly the C4 and Cs olefins, are byproducts of coal formation. Although it is generally believed that coal formation occurred at temperatures below 200° C, most experimental work on gas formation from coal has been performed at temperatures between 200° and 1,000°C. The objective of this Bureau of Mines experiment was to determine if observable changes in the gases from coal could be produced at temperatures below 200° C in relatively short periods of time. The experiment involved heating coal samples from six coalbeds at constant temperatures and analyzing evolved gases. The composition of the gases at three temperatures was compared. At 35° C, over 99 pet of the gas is methane; at 125° and 150°, methane constitutes approximately half of the hydrocarbon gas. Isobutane and pentane are the predominant higher hydrocarbons at temperatures between 100° and 150° C.

Jan 1, 1974

By Harold H. Fukubayashi

The effect of various zinc electrowinning solution impurities on the surface morphology of deposited zinc was investigated. Impurities studied included Al, Ag, Cd, Co, Cr, Cu, Ge, Mn, Ni, Sb, Sn, Ti, Pb02, PbSO4, and HC1. Also, the effect of animal glue, gum arabic, and Na2SiO3 additives on the deposited zinc surface structure was studied. Results were compared with deposits from a pure electrolyte consisting of H2SO4 and Zn+2, 200 and 65 gpl, respectively. Zinc was deposited on a Al cathode, 99.9 pct pure, using Pt anodes. Time, temperature, current density, and impurity concentrations were con¬troller The bulk of the tests were conducted at 40° C and 75 A/ft2 (82 mA/cm2). A scanning electron microscope (SEM) was used to examine the surface morphology. X ray diffraction techniques were used to determine crystal orientation and nondispersive X-ray spectrometer analyses were employed in an attempt to locate impurity concentrations on the zinc deposit when pitting or re-solution occurred. The impurities were categorized by their effect on current efficiency, morphology, and apparent mechanism of H2 evolution from the cathode.

Jan 1, 1974

By C. H. Elder, Maurice Deul

A 5-hole pattern was drilled from the surface at a site near Oak Grove, Jefferson County, Ala., to degasify the gassy Mary Lee coalbed in advance of mining. Gas and water production was monitored for 1 year, 4 months to allow gas flow to stabilize fully. A thickened water stimulation treatment was designed and applied in one hole of the pattern to evaluate this degasification technique for the Mary Lee coalbed. A gas production rate of 70,000 ft3 /day after stimulation treatment indicates that the use of vertical boreholes coupled with hydraulic fracturing in advance of mining the Mary Lee coalbed would provide for more rapid degasification and could provide a possible source of natural gas.

Jan 1, 1974

By C. H. Elder

A 5-hole pattern was drilled from the surface at a site near Oak Grove, Jefferson County, Ala., to degasify the gassy Mary Lee coal bed in advance of mining. Gas and water production was monitored for 1 year, 4 months to allow gas flow to stabilize fully. A thickened water stimulation treatment was designed and applied in one hole of the pattern to evaluate this degasification technique for the Mary Lee coalbed. A gas production rate of 70,000 fts/day after stimulation treatment indicates that the use of vertical boreholes coupled with hydraulic fracturing in advance of mining the Mary Lee coalbed would provide for more rapid degasification and could provide a possible source of natural gas.

Jan 1, 1974

By Ann G. Kim

Methane in coal constitutes a serious hazard during mining. Draining the methane from large blocks of coal in advance of mining is an effective method of improving the safety and efficiency of coal mining. Because of the similarity of the two gases, drained methane can be recovered and added to pipeline supplies of natural gas. To effectively apply advance drainage techniques and recover drained gas, a gross estimate of the methane content of coal is necessary. Using data from previous investigations, the virgin reserves of the Pittsburgh coal in the central and southwestern parts of Washington County, Pa., are estimated at over 1.5 billion tons, with a methane content of 50 to 100 fts/ton. The Pittsburgh bed in this area of approximately 265 mi2 contains over 130 billion ft3 of methane.

Jan 1, 1974

By G. L. Hundley

An anhydrous chlorination process has been developed by the Bureau of Mines for the production of copper, ferric oxide, and sulfur from chalcopyrite. The first part of the process is a chlorination step in which elemental sulfur and a mixture of iron-copper chlorides are produced. This paper describes the second step of the process in which the copper and iron chlorides are reacted with oxygen to selectively convert the iron chloride to ferric oxide and chlorine leaving the copper in the chloride form. The chlorides are pulverized and dropped countercurrent to a flow of oxygen in a vertical 20-cm-diam. reactor at 800° C. By leaching with brine, the copper chloride may be separated from the insoluble iron oxide and reduced to copper powder by electrowinning. It has been demonstrated that 70 to 80 pct of the iron can be converted to oxide in a single-stage operation with a chlorine content in the offgas of 80 pct. After removal of the oxygen, this chlorine could be recycled to the chlorination step. A two-stage operation will convert 98 to 99 pct of the iron in the mixture to insoluble oxides. The offgas from the second stage contains 70 pct chlorine.

Jan 1, 1974

By Michael J. Beus

This Bureau of Mines report describes the development of load cells for measuring compressive loads in timber and lock-bolt support systems commonly used in. coal; metal, and nonmetal mines Design and evaluation is covered in detail to insure a reliable, accurate, and practical instrumentation scheme. The load cells are relatively inexpensive and adaptable to various size support systems. User-oriented procedures are emphasized, and design equations were reduced to a series of nomographs. Laboratory evaluation, destructive testing, environmental testing, and tests to determine the effect of extraneous loads were conducted. Field performance was evaluated in conjunction with ongoing Bureau projects at a metal mine in North Idaho and a coal mine in Utah. Load cells utilizing a titanium alloy as the cell body and weldable strain gages as the strain-sensing components satisfied the basic design and performance criteria, and with minor design modifications, the load cells can be adapted to many mining applications.

Jan 1, 1974