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By Sathit Tandanand

Massive roof overlying the working seam in longwall operations can cause hazards if it does not cave readily behind the face supports. The overhang thus formed can overload the supports and endanger personnel when it collapses suddenly as a large rock mass. This Bureau of Mines report proposes the use of a concentrated load, either strip or point loading, applied onto the roof with the help of the upward thrust of the face supports. An experiment was conducted in the laboratory to obtain information about break characteristics and the values of significant parameters of three sedimentary rocks. The results were used to determine the breaking load requirement for a strong roof possibly encountered in typical longwall operations. The results show that the roof slab of moderate thickness can be fractured within the load capacity of off-the-shelf powered supports.

Jan 1, 1979

By S. D. Sanders

Goals of the Bureau of Mines include utilizing readily available minerals as substitutes for scarce mineral commodities and minimizing occupational hazards associated with mineral processing occupations. Therefore, the Tuscaloosa Research Center investigated using rapid-set cement as a suitable molding sand binder for small ferrous castings; currently petroleum-based binders are used. Substitution of a rapid-set cement would eliminate organic vapors associated with the petroleum-based binders; these vapors constitute occupational hazards and environmental pollutants. A binder containing 60 percent white portland cement (WPC) and 40 percent calcium aluminate (CA) would be an acceptable and economic substitute for petroleum-based binders where the foundry requirements are compatible with its limitations. It produced a set time and a pattern strip time of less than 1 hour. Cement, sand, and water mixtures developed compressive strengths from about 40 to 75 psi after 2 hours and from 120 to 130 psi after 24 hours. Tensile strengths of 18 to 22 psi were obtained after 2 hours, increasing to 30 to 35 psi after 24 hours. The addition of about 1 percent polyphosphate to the sand-cement-water mixture doubled the compressive strength and increased the tensile strength about 50 percent after 4 hours, but also increased the set time from 30 minutes to 1 to 1-1/2 hours. Po1yvinylacetate (PVA) resin latex additions resulted in rapid strength development. When castings were poured into the cement-bonded molds, the surface finish was fair to good on gray iron castings, but some areas of burn-on were present on steel castings. Using a graphite wash on the cement-bonded molds produced good surfaces on gray iron castings.

Jan 1, 1979

By C. M. Flynn

The Bureau of Mines prepared and investigated xanthated sawdust adsorbents to determine their effectiveness in removing heavy metal ions from dilute aqueous solutions, mine-drainage waters, and brines. Stripping of the metal values from the metal-laden adsorbent was also investigated. The treated sawdusts had an adsorption capacity of 0.3 to 0.4 meg/g dry adsorbent for Mn, Co, Ni, Cu, Ag, Zn, Cd, Hg, or Pb from feed solutions with pH 5 to 6. The feed solutions tested included mine-drainage waters and geothermal brine. Effluent metal concentrations as low as 0.05 to 0.1 mg/l were obtained at effluent pH values of 6 to 9. The order of affinity of metals for the sawdust adsorbent is Na«Ca~Mg~Mn<Zn<Ni<Cd<Pb~Cu. The presence of Ca, Mg, or Na in concentrations as high as 2 g/l does not seriously impair the heavy-metal adsorption. Metals were desorbed from the metal-laden adsorbent by elution with dilute mineral acids, sodium cyanide, or salts of ethylenediaminetetra-acetic acid.

Jan 1, 1979

By M. J. Ferrante

New data on zirconium tetraiodide (ZrI4) have resulted from high-temperature enthalpy and X-ray powder diffraction studies conducted by the Bureau of Mines. These studies were undertaken as part of the Bureau&apos;s efforts to provide important thermodynamic data essential to the advancement of mineral resources technologies that can be employed with minimal energy requirements and minimal environmental degradation. Enthalpies were measured with a copper-block drop calorimeter. No transitions or other anomalies were found. Tabulated values are given from 298.15 to 772 K for relative enthalpy, heat capacity, entropy, and Gibbs energy function. Enthalpies are expressed in equation form and combined with data from the literature to calculate values of the standard enthalpy of formation and the Gibbs energy of formation. X-ray powder diffraction data indicate that ZrI4 is primitive cubic with a lattice parameter of 11.79 A and is isostructural with stannic iodide (SnI4).

Jan 1, 1980

By D. N. Nilsen

The Bureau of Mines is developing a method to recover Ni, Co, and Cu from laterites containing less than 1.2 pct Ni and 0.25 pct Co. The method consists of the following basic unit operations: (1) reduction roasting, (2) leaching, (3) solvent extraction, and (4) electrowinning. The method reflects three Bureau of Mines objectives: (1) recovery of critical minerals that are domestically in short supply from low-grade domestic laterites, (2) lower processing energy requirements, and (3) solution recycling. This report deals with the extraction of cobalt and the preparation of a suitable cobalt electrolyte by solvent extraction from liquor produced by this method. Nickel and copper are coextracted with LIX64N from an ammoniacal ammonium sulfate leach liquor containing about 1.00 g/l Ni, 0.30 g/l Co, 0.03 g/l Cu, and 0.02 g/l Zn. Cobalt (III) in the nickel-copper barren raffinate is reduced to cobalt (II) with cobalt metal. Reduction of cobalt (III) to cobalt (II) greatly aids subsequent extraction. Commercially available XI-51 extracts about 94 pct of the cobalt from the treated raffinate in one stage in a laboratory mixer-settler continuous circuit. Ammonia loaded on the solvent is removed in two washing steps. About 94 pct of the cobalt then is stripped from the XI-51 in one stage with spent cobalt electrolyte containing about 77 g/l Co and 18 g/l sulfuric acid (H2S04), Electrolytes containing less H2S04 also may be used. Preliminary data indicate that coextracted zinc may be removed from pregnant cobalt eletrolyte containing 3 g/l or less H2S04 with di-(2 ethylhexyl) phosphoric acid (D2EHPA).

Jan 1, 1980

By J. M. Stuve

This Bureau of Mines investigation measured the low-temperature heat capacities of FeOC1(c) and FeC13(c) in the temperature ranges of 6 to 305 K and 4.6 to 300 K, respectively. The standard entropies (S°, 298.15 K) of FeOCl(c) and FeC13(c) were derived as 19.73±0.03 cal/deg-mole and 35.33±0.07 cal/deg-mole. A large lambda transition was observed in the heat capacity of FeC13(c) at 8.4 K. The standard enthalpy of formation (?H°f, 298.15 K) of FeOC1(c) was determined to be -98.23±0.22 kcal/mole by HC1 solution calorimetry. High-temperature enthalpy measurements (H-H298.15) of FeOC1(c) were determined to 700 K by precision drop calorimetry. Standard thermodynamic formation data and related functions were tabulated at various temperatures for FeOC1(c) and FeC13(c).

Jan 1, 1980

By K. J. Liles

To encourage the development and conservation of the Nation&apos;s ceramic raw materials, the Bureau of Mines, U.S. Department of the Interior, under an agreement with the Georgia Department of Natural Resources, evaluated samples from a clay resource located in Clay County, Ga., for use as a raw material for lightweight aggregate. The physical properties of clay samples, taken from 5-foot increments of drill cores from 11 holes, were determined. Raw materials were plasticized and extruded to produce 1/2-inch by 1-inch pieces and fired in a rotary kiln to produce lightweight aggregate samples. The resulting expanded material had excellent loose pour weights ranging from 30 to 37 lb/cu ft. The expanded test materials were crushed, sized, and used as aggregate to form concrete cylinders. The unit weight and compressive strength of the cylinders averaged 106 lb/cu ft and 3,350 lb/sq in, respectively; these values meet American Society for Testing and Materials specifications for structural concrete. The clay from the drill cores was also used to make test bars that were evaluated for building brick.

Jan 1, 1980

By Robert F. Holub

The Bureau of Mines has evaluated four working-level radiation-measurement methods and optimized them from the inherent and statistical error standpoint. Optimization with respect to various sampling and measurement times yielded no marked improvement over the existing methods. However, when appropriate approximations are made and evaluated, these two-measurement methods can be reduced to simple formulas, eliminating a need to use nomograms. These modified methods also have improved inherent error characteristics. A new method--a combination of two existing methods--with improved inherent and statistical errors has been suggested. All the pertinent equations are given, together with the computer program, so that any two-measurement method can be readily evaluated.

Jan 1, 1980

By George M. Lucich

This report describes a sensitive, proportional temperature controller developed by the Bureau of Mines that is useful in the temperature range from 40 to 400° C with an accuracy of ±0.10 C. A temperature controller of this kind is potentially useful for regulating temperatures in air chambers, liquid baths, furnaces, and reaction vessels, and for other applications. This instrument was developed to control the duration and temperature of the heating cycle of a charcoal-filled adsorber that is part of a special helium analyzer used by the Bureau. The controller was made from commercially available parts, and can be easily modified to provide continuous temperature control. The circuit is solid state and employs no electromechanical devices. Over a 2-year period of use as a component of the special helium analyzer, this temperature controller performed successfully and required no maintenance.

Jan 1, 1979

By P. W. Jeran, S. J. Pepperney, M. C. Irani, F. F. Kopsch

The Bureau of Mines has designed and put into operation a fail-safe control system for use in underground coal mines equipped with methane drainage pipelines. This control system can detect certain unsafe conditions and respond by automatically shutting off the flow of methane from the degasification borehole to the drainage pipeline. Methane flow is shut off when the methane content in the return airways reaches a predetermined level (typically 1.5 pct), when the methane drainage pipeline is ruptured by roof fall, or when there is an electric power failure. The fail-safe control system was designed using commercially available components and a methane analyzer system previously developed by the Bureau. The fail-safe system consists of a unit that combines a shutoff valve and pneumatic valve actuator, and electronic and mechanical equipment designed to detect hazards and effect shutdown. The fail-safe control system was designed to meet regulatory requirements issued by the Mine Safety and Health Administration (MSHA), U.S. Department of Labor, and State regulatory bodies for the safe operation of underground methane pipelines used for mine degasification. MSHA has inspected and tested this system and permitted its use in two mines. The Bureau installed the fail-safe system in two working coal mines, where successful performance has been demonstrated.

Jan 1, 1980

By M. C. Irani

The Bureau of Mines has designed and put into operation a fail-safe control system for use in underground coal mines equipped with methane drainage pipelines. This control system can detect certain unsafe conditions and respond by automatically shutting off the flow of methane from the degasification borehole to the drainage pipeline. Methane flow is shut off when the methane content in the return airways reaches a predetermined level (typically 1.5 pct), when the methane drainage pipeline is ruptured by roof fall, or when there is an electric power failure. The fail-safe control system was designed using commercially available components and a methane analyzer system previously developed by the Bureau. The fail-safe system consists of a unit that combines a shutoff valve and pneumatic valve actuator, and electronic and mechanical equipment designed to detect hazards and effect shutdown. The fail-safe control system was designed to meet regulatory requirements issued by the Mine Safety and Health Administration (MSHA), U.S. Department of Labor, and State regulatory bodies for the safe operation of underground methane pipelines used for mine degasification. MSHA has inspected and tested this system and permitted its use in two mines. The Bureau installed the fail-safe system in two working coal mines, where successful performance has been demonstrated.

Jan 1, 1979

By T. G. Carnahan

The Federal Bureau of Mines investigated, on a laboratory scale, a technique for recovery of silver from pregnant solutions generated in the hydro-metallurgical treatment of complex base-metal sulfide concentrates with oxidizing chloride media. This technique provides a means for recovery and simplified reduction of accessory silver to metal from chloride solutions. The method consists of adding NaI or KI to the solution to precipitate AgI, which is then contacted with Na2S to produce Ag2S and to regenerate the iodide salt solution. Silver recoveries range from 99 pct with 20 pct excess iodide precipitant, to 92 pct when the theoretical stoichiometric amount of precipitant is employed. The Ag2S product can be reduced to silver metal by contact with aluminum chips in NaOH solution followed by purification with conventional fire refining techniques.

Jan 1, 1980

By R. S. DeCesare

Operation of the Bureau of Mines raw refuse continuous separation pilot plant is described, including modifications made to plant equipment for improved performance. Products recovered from refuse, many of which have been evaluated by other laboratories and private firms, are discussed. Sampling procedures used in the pilot plant and detailed data obtained from processing refuse from 13 municipalities are presented in appendixes. Fuel evaluations made on combustible fractions of refuse from the various municipalities are also presented. Information and data obtained at the pilot plant have been used to assist many municipalities in solving their urban refuse problems.

Jan 1, 1980

By J. E. Pahlman

As part of its goal to minimize the requirements for mineral commodities through conservation and substitution, the Bureau of Mines is conducting research to determine the resistance of alumina refractories to corrosion by alkali-containing slags that could result from burning of the abundant Western lignites in metallurgical operations. Static corrosion tests were performed at 1,000° to 1,350° C and dynamic tests were performed at 1,400° to 1,600° C to investigate the stability of refractory specimens in slag environments. In general, the degree of refractory attack increased with decreasing alumina content in the refractory and with increasing alkali content of the lignite ash. The parabolic kinetics observed in static tests suggested that a reaction product layer is formed through which ionic diffusion must occur to sustain the reaction with the refractory material. The linear kinetics observed in dynamic tests in high-viscosity slags indicated a shearing of the reaction product layer by viscous slags. The observed lesser attack of refractories by low-viscosity slags can be explained on this basis. Two 99-percent-alumina refractories and two 90-percent-alumina refractories formed an expanded protective layer with the more viscous slags but not with the less viscous slags. Corrosion of 90-percent-alumina refractories increased exponentially with temperature. In refractories with the same nominal alumina content, those that contain a combination of a-Al203 and mullite (3A1203?2Si02) have better corrosion resistance than those containing a combination of a-Al203, cristobalite (Si02 mineral), and mullite. In alkali environments (1,300 to 1,400° C), 90-to 99-percent-alumina refractories are recommended for use as furnace linings.

Jan 1, 1980

By B. S. Covino

The Bureau of Mines, U.S. Department of the Interior, is conducting research to devise substitute corrosion-resistant materials by using ion implantation to form alloyed regions near the surfaces of metals. These alloys were prepared by implanting 25-kev Cr+ and/or Ni+ ions into iron. Their resistance to corrosive attack was evaluated by determining their anodic polarization behavior under potentiodynamic conditions in a solution containing sodium chloride, boric acid, and sodium borate. These electrochemical studies have shown that the general corrosion resistance of ion-implanted alloys was comparable to nominally equivalent bulk alloys. The pitting-corrosion resistance of the ion-implanted alloys was superior to that of iron, although not as good as that of most of the bulk alloys tested.

Jan 1, 1980

By J. T. May

The Federal Bureau of Mines investigated the extraction of lithium from hectorite-type clay deposits found on the Nevada-Oregon border. Two clay samples were used in the investigation; one contained 0.36 pct Li and the second contained 0.64 pct Li. The purpose of this laboratory-scale research was to determine how these clays responded to different extraction techniques. Extraction techniques investigated were sulfuric acid leach, sulfuric acid bake-water leach, and roast-water leach procedures with cholorides, sulfates, carbonates, and combinations of these reagents. The processing characteristics of the clay samples showed significant variations, and no one technique was effective for both materials. Lithium extractions near 90 pct were achieved during these exploratory studies.

Jan 1, 1980

By M. M. Jones

A procedure for the spectrophotometric determination of uranium has been developed in support of minerals research being conducted by the Bureau of Mines. Uranium is separated from the sample by tributylphosphate extraction from acid solution containing added aluminum nitrate and (ethylene dinitrilo)-tetraacetic acid solutions. The colored uranium-dibenzoy1methane complex is developed in the organic phase by adding an ethanol solution of dibenzoylmethane buffered with triethanolamine. Absorbance is measured at 410 nanometers, and the response is linear up to at least 100 micrograms U30S in the aqueous aliquot taken for analysis. Aliquots containing as little as 8 micrograms U30S may be analyzed with relative errors no greater than ±5 percent. For aliquots containing at least 35 micrograms U308, relative standard deviation at the 95-percent confidence level is about ±2.2 percent. Appropriate procedures are given for analyzing a wide variety of samples.

Jan 1, 1980

By B. D. Sartwell

The formation of alloyed regions near the surface of metals using ion implantation is being investigated by the Bureau of Mines as a means of providing corrosion resistance using much smaller amounts of the strategic alloying metals. Two ion implantation systems that can implant low-energy chromium, nickel, or aluminum ions into low-cost substrate materials such as iron or carbon steel have been designed and constructed. The development of the ion source, ion beam acceleration stage, mass analysis system, and target chamber are described in detail. The ion-implanted alloys have been characterized using proton-induced x-ray emission to give the total number of atoms implanted and to determine the extent of any surface contamination introduced by the ion implantation process. Research conducted at other laboratories on metallurgical applications of ion implantation is given.

Jan 1, 1980

By Michael J. Beus

This Bureau of Mines report describes field investigations conducted in the Coeur d&apos;Alene mining district of Idaho to obtain data on rock stress and physical properties. The resulting information has been utilized as input to detailed finite-element analyses to establish structural design criteria for deep-vein mine shafts. Measurement techniques include the Council for Scientific and Industrial Research biaxial and triaxial strain cells, the U.S. Geological Survey solid-inclusion probe, and the Colorado School of Mines dilatometer. Physical property testing was conducted in the laboratory on core obtained from each test site. Limited in situ physical property tests were also conducted. Reason-able success was obtained with the CSIR equipment, which was considered the most suitable for stress measurement in the study area. Test sites ranged in depth from 1,200 to 7,700 feet and are described in detail. The stress data were reduced by least-squares linear regression techniques to enable prediction of vertical and horizontal stresses to 7,500 feet. Ratios between the horizontal stresses as utilized for shaft design varied considerably, and a hydrostatic condition is the exception, based on Bureau measurements. Physical properties also varied widely, due to the complex geologic structure. Analyses of the data in terms of the tectonic history of the area show reasonable correlation. Data from previous rock mechanics investigations from the Coeur d&apos;Alene district were also compiled and presented as part of this report to justify any generalizations regarding stress conditions and physical properties of the district as a whole.

Jan 1, 1980

By A. G. Smelley

As part of research conducted in its mission to effect pollution abatement, the Bureau of Mines, U. S. Department of the Interior, is developing a dewatering technique that allows for disposal of phosphatic clay wastes, for reuse of water now lost with clays, and for reclamation of mined land. The technique utilizes a high-molecular-weightnonionic polyethylene oxide polymer (PEO) that has the ability to flocculate and dewater phosphatic clay wastes. A synergistic flocculation study was made to determine whether a portion of PEO could be replaced by other reagents. Several groups of reagents were tested: (1) those that increased the zeta potential of the phosphatic clay wastes; (2) those capable of hydrogen bonding; and (3) those which flocculated the phosphatic clay waste. Reduction in PEO consumption occurred only with addition of those reagents able to flocculate the slime. The use of natural guar gums resulted in a lower PEO requirement and also yielded a dewatered product of higher solids content, 43 to 45 percent, versus 33 to 35 percent obtained with PEO alone.

Jan 1, 1980