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By M. J. Beus

The Bureau of Mines, under a cooperative agreement with Hecla Mining Co., is conducting a rock mechanics study of the 6,200-ft-deep circu-lar, concrete-lined Silver Shaft in northern Idaho. The objective of the project was to instrument and evaluate lining behavior and rock de-formation when a deep shaft is constructed in a high in situ stress field and anisotropic rock mass. Rock mass displacements were moni-tored with multiple-position borehole extensometers. Liner stress and strain were measured with concrete pressure cells and embedment strain gauges. Field data from the 5,955-ft test level show that rock displacement is controlled by rock mass anisotropy. Liner stress and strain levels reflect the high in situ stress field as well as nearby station and raise construction. Maximum stresses measured in the lining, as a result of shaft excavation, are about one-third of its compressive strength. Subsequent loading pocket excavation resulted in signifi-cantly increased stress and strain levels in the liner. Continued monitoring and preliminary analysis of the data indicate that concrete-lined, circular shafts are stable for the high, unequal horizontal stress fields and rock anisotropy encountered in deep-level mining. Adjacent development work can be expected to significantly alter the initial stress and displacement conditions.

Jan 1, 1984

By Arthur V. Petty

The Bureau of Mines has researched the utilization of mining and pro-cessing wastes as raw materials for the production of glass-ceramic pipe. Characterization of various wastes as to occurrence and chemical composition is reported. A computer program was developed and used to identify waste materials and mixes that would result in glass melts from which glass-ceramics could be produced after cooling and subsequent heat treatments. The production of abrasion-resistant pipe from inexpensive and readily available domestic resources could offer an economical substitute for high-alloy steels containing the critical and strategic materials cobalt and chromium.

Jan 1, 1984

By D. G. Foot

The Bureau of Mines investigated energy-efficient methods for recovering potash values from process and waste brines. Laboratory pan evaporation of four chloride brines produced crude salts containing predominantly sylvite, halite, and carnallite. Six sulfate-chloride brines produced crude salts containing primarily schoenite, kainite, leonite, sylvite, carnallite, and halite. Potash grades ranged from 7.2 to 22.2 pct K20, and recoveries from 84 to 99 pct. Sylvite flotation from chloride evaporites, with amine collector, recovered 90 to 97 pct of the potash in a concentrate containing 54.3 to 60.3 pct K20. Fatty acid flotation of the high-sulfate evaporite recovered 78 pct of the sulfate minerals in a 27.8-pct-K20 concentrate. Flotation of the chloride minerals with amine collector recovered 80 pct of the potash in a 59.7-pct-K20 concentrate. Solar evaporation of 10,000 gal of brine recovered 99 pct of the potash in a crude evaporite containing 24.5 pct schoenite and 20 pct sylvite. Continuous flotation in a 100-lb/h process research unit recovered over 95 pct of the potash in schoenite and sylvite concentrates containing 28.0 and 62.3 pct K20, respectively. An economic evaluation suggested a rate of return of 3 pct for a new facility and 9 pct if. the process is adapted to fit an existing plant.

Jan 1, 1984

By K. O. Bennington

The thermodynamic properties of aegirine, of composition [(Na0.869Fe30+7362 Fe20+16Mn0.03Ca0.1121)(A10.141Sil 9738)(06)], were experimentally determined at the Bureau of Mines as part of its efforts to advance minerals technology. The standard enthalpy of formation determined by hydrofluoric acid solution calorimetry is AHf298 = -641.12±0.73 kcal/mol. The standard enthalpy of formation from the oxides is AH298 = -37.136±0.509 kcal/mol. Low-temperature heat capacities were determined by adiabatic calorimetry from 19.1 to 304.6 K. The derived standard entropy is S298 = 38.03±0.14 cal/mol?K. The heat capacity was measured over the range 348 to 1,198 K by differential scanning calorimetry. These experimentally determined data were combined with data from the litera¬ture to calculate the Gibbs energies of formation and equilibrium constants of form¬ation over the temperature range of the measurements. Standard enthalpies of forma¬tion are given as functions of temperature. The standard Gibbs energy of formation at 298.15 K is AGf298 = -600.36 kcal/mol.

Jan 1, 1984

By L. Y. Sadler

This report summarizes the findings of a 9-yr research program, sponsored by the U.S. Department of Energy and conducted by the Bureau of Mines, to evaluate refractory liner materials for coal gasifier reactors. Commercially available refractories were exposed to coal gasifier reactor environments, reproduced in the laboratory with a high-temperature, high-pressure test facility, followed by extensive postexposure evaluation. Thirty-six castable or gunnable refractories and cements and 24 refractory brick were evaluated. The behavior of castable refractories reinforced with stainless steel fibers was also examined. Gas environments that were evaluated included steam, H2, CO2, CO, and typical high-and low-Btu gas mixtures. Exposure pressures ranged from 100 to 1,000 psig, temperatures from 5000 to 1,1000 C, for periods from 50 h to 2,000 h. In some exposures, sodium and/or potassium hydroxide were introduced in order to simulate a high-alkali environment. It was found that intermediate-and low-alumina refractories produced from domestically available raw materials, rather than high-alumina refractories produced from imported raw materials, gave the best service as liner materials and that alkali attack was probably not a serious problem with most refractories. Based on the results of this program, good choices of refractory liner materials for gasifier reactors can be made.

Jan 1, 1984

By Jon K. Ahlness

The Bureau of Mines conducted laboratory and field experiments to determine tne amount of permeability reduction in uranium sandstone after its exposure to different drilling fluids. Seven polymer and two bentonite fluids were laboratory-tested in their clean condition, and six polymer fluids were tested with simulated drill cuttings added. Sandstone cores cut from samples collected at an open pit uranium mine were the test medium. The clean fluid that resulted in the least permeability reduction was an hydroxyethyl cellulose polymer fluid. The greatest permeability reduction of the clean polymers came from a shale-inhibiting synthetic polymer. Six polymer fluids were tested with simu-lated drill cuttings added to represent field use. The least permeability reduction was obtained from a multipolymer blend fluid. A field experiment was performed to compare how two polymer fluids affect formation permeability when used for drilling in situ uranium leaching wells. For this test, the polymer fluid with the best laboratory results (multipolymer blend) was compared with a commonly used polymer fluid (guar gum) that gave poorer laboratory results. When fluid injection rates for the four wells drilled with the guar gum were compared with those for the four drilled with the multipolymer blend, no statistically significant difference was found.

Jan 1, 1984

By Lung Cheng

The Bureau of Mines has installed passive water explosion barriers in two operating mines to determine their usefulness in U.S. coal mines. The primary objective of this field trial was to determine the effect of the explosion barriers on mining operations. Data were also obtained on the ability of the barriers to withstand the mine environment and on the effect of the barriers on belt operation, ventilation, worker travel, and rock dusting. Fifty barriers were installed at three separate beltway locations, and periodic inspections were made. A year after installation, no defects of the barriers or support hardware were detected, nor was any complaint as to the presence of the barriers made by the mine personnel. To date, 2-1/2 years after installation, the barriers have had no detrimental ef-fect on rock dusting, belt operation, or ventilation. Costs of material, fabrication, and installation are reported herein.

Jan 1, 1984

By Virgil J. Stachura

The Bureau of Mines conducted a series of delayed blasting experiments at a West Virginia contour coal mine that resulted in smoother highwalls. The 17; were smoother due to reduced overbreak and inherently safer A, to reduced likelihood of rockfall. Reduced overbreak was accomplished by an increase in the highwall hole delays, which changed the effective delay pattern geometry and the direction of burden movement. The blast delays in the highwall holes were 50 to 100 ms longer than the mine's nominal design pattern (flat V, 17- by 42-ms surface delays, 200-ms in-the-hole delay). The burden movement was effectively changed from a 45* angle to 90* with respect to the highwall. The results of the blast delay changes were evaluated using terrestrial photogrammetry to generate vertical profiles at regular intervals. This evaluation showed that delay changes produced generally smoother vertical profiles.

Jan 1, 1984

By M. J. Ferrante

Relative enthalpies of CuBr from 298.15 to 1,301 K were measured at the Bureau of Mines to provide thermodynamic data needed for the advancement of mineral technology. The temperatures of transition were measured by differential scanning calorimetry (DSC) and the standard enthalpies of transition[ (IlH~r) by drop calorimetry. The combined results gave reversible transitions at 657 K with llH~r= 1.10 kcal/mol, at 741 K with lm~r == 0.51 kcal/mol, and at 759 K with an enthalpy of fusion (AH~) of 1.22 kcal/moL ] An anomalous increase in heat capacity preceded the first crystal transition at 657 K. Tabulated values are listed for the standard relative enthalpy, heat capacity, entropy, and Gibbs energy function from 298.15 to 1,500 K. Standard relative enthalpies are also given in equation form and combined with thermodynamic data from the literature to derive values of standard enthalpies of formation and Gibbs energies of formation.

Jan 1, 1984

By M. L. Glenn

The Bureau of Mines is conducting research on Fe-based alloys using Si and Al additions to reduce the Cr required for heat-resisting appli-cations. Part of this research is being done to evaluate alloys containing (8-10)Cr-(10-14)Ni-(0-8.5)Si-(0-4) Al to determine which of these alloys have austenitic structures, as well as fabrication properties and oxidation resistance sufficient to substitute for type 304 stainless steel. Based on initial results, an Fe-lOCr-11Ni-5Si alloy and an Fe-8Cr-13Ni-5Si alloy were selected for evaluation of oxidati.on, stress rupture, and tensile properties. Both alloys have oxidation resistance at 7000 and 8000 C that is better than that of type 304 stainless steel. The stress rupture strengths are less than that of type 304 stainless steel but significantly better than that of commercial heat-resisting steels with similar Cr contents. Yield strengths of the alloys were equivalent to that of type 304. Both alloys had high tensile strengths comparable to those of stainless steels that transform to martensite during straining (e.g., type 301). These alloys have weld-hot-cracking resistance comparable to that of type 304 stainless steel. This initial study shows that Si has potential as a substitute for Cr in stainless steels for heat-resisting applications.

Jan 1, 1984

By D. J. Singleton

Erosion corrosion of 12 alloys in phosphoric acid waste water was studied by the Bureau of Mines. Tests were conducted on oblate spheroids or cylindrical specimens in 12-and 60-cm-diam ball mills by grinding phosphate rock in gypsum pond water with a starting pH of 1.6. For comparison, tests were conducted while grinding phosphate rock in plain water. Static corrosion tests in gypsum pond water also were conducted. For all alloys, the wear by erosion-corrosion (milling with gypsum pond water) was greater than the sum of erosion (milling with water) plus static corrosion. Erosion-corrosion wear was about 1,500 to 3,000 mpy for the alloyed white cast irons, 1,000 to 1,400 mpy for commercial steel ball material and type 316 stainless steel, and 600 to 900 mpy for nickel-base alloys and a high-manganese, nitrided stainless steel. Alloy costs per unit of phosphate rock 'processed favor a low-alloy, high-carbon steel or a high-manganese, nitrided stainless steel.

Jan 1, 1985

By A. Visnapuu

The Bureau of Mines has upgraded high-iron domestic chromite concentrates by a carbonyl process. The upgraded chromite concentrates show as much as 10 wt pct higher Cr203 content and up to a threefold in-crease in the Cr:Fe ratio, compared with the starting concentrates. The high-iron chromites were first reduced to convert the iron oxides to the metal, and then treated with CO at elevated pressures and low temperatures to convert part of the metallic iron fraction to iron pentacarbonyl. Carbonylation was accelerated by the addition of H2S in small quantities. The iron pentacarbonyl was extricated from the con-centrate in the pressure reactor during carbonylation by a CO sweep through a pressure-reducing valve and passed through a decomposer at atmospheric pressure to convert it back to iron metal and CO. CO pres-sure, temperature, promoter trends, and other factors enhancing iron pentacarbonyl formation are presented.

Jan 1, 1985

By C. M. K. Boldt

The Bureau of Mines studied the compaction characteristics of metal and nonmetal tailings. Densities of the tailings and zone of compaction influence, compactive effort, and cost of equipment are related to changes in the factor of safety for specific grain-sized tailings and embankment configurations. Field testing was accomplished in two distinct phases. The first phase investigated the effectiveness of using a nuclear gauge on metal and nonmetal tailings to produce rapid, instantaneous measurements of moisture content, wet density, and dry density. The results of the nuclear gauge testing are presented in chapter 1. Chapter 2 presents a comparison of the compactive effectiveness of three different pieces of construction equipment on a coarse-grained metal tailings pond. The three pieces of equipment chosen for study were a DBH track-mounted dozer, a DSOO rubber-tired dozer, and a SP848 vibratory smooth-drum compactor.

Jan 1, 1985

By L. E. Schultze

The Bureau of Mines devised a technique to recover a Zn-Pb concen-trate from a geothermal brine. More than 99 pct of the Zn and Ph was precipitated by treating the brine with H2S and controlling the pH with lime. Recycle of the sulfide precipitates increased crystal size and resulted in easily filterable products. A typical sulfide precipitate contained 53 pct ZnS, 8 pet PbS, 24 pct MnS, and 15 pct FeS. Addition of sulfide as FeS or CaS was not effective in precipitating Zn and Pb, but Zn in the brine was selectively removed with a strongly basic ion-exchange resin. A proposed flowsheet for metals recovery is discussed.

Jan 1, 1985

By Robert L. Virta

The Bureau of Mines examined a fibrous talc sample from the Gouverneur talc district in New York by transmission electron microscopy (TEM) and polarized light microscopy to determine the mineralogical relationship of the fibrous talc to the amphiboles present in the sample. Two am-phiboles, anthophyllite and tremolite, were present in the sample. Tremolite occurred as a separate mineral phase, which was blocky in habit. Only a few composite tremolite-talc grains were observed. An-thophyllite, however, was present only in the fibrous talc grains. Mi-crodiffraction study of the fibrous talc grains containing anthophyllite showed that the anthophyllite was intermixed with the talc on a fine scale and that there was a crystallographic relationship between the talc and anthophyllite lattices in the fibrous talc grains. A mechanism similar to the process that forms biopyriboles could explain the structural defects, the fibrous habit of the talc, and the structural relationship between the talc and anthophyllite in the fibrous talc grains. Because of these characteristics, phase contrast microscopy and a provisional TEM technique for monitoring asbestos exposure would not distinguish between fibrous talc and fibrous amphiboles. TEM techniques employing electron diffraction and energy-dispersive X-ray analysis are recommended to positively identify the fibrous phases for regulatory purposes.

Jan 1, 1985

By John R. Bartels

In laboratory testing, the Bureau of Mines established criteria by which common resin-grouted roof bolting systems can be evaluated and compared. Ultimate strength and stiffness were determined for nonten-sioned full-column, point-anchor, tensioned full-column, and debondable resin-grouted bolts, and for variations on full-column boltsn Bolt per-formances were compared using the performance of the 3/4-in full-column resin-grouted bolt as the standard. New and innovative systems can also be qualitatively compared against this standard. Since the medium into which a resin-grouted bolt is installed is one of the most important parameters affecting bolt performance, various host mediums were used in the testing: sandstone, concrete, simulated coal, simulated shale, and plaster. Bolt performances expected in other mediums can be inferred from the response patterns obtained in these mediums. Results indicate several functional differences among bolt types. Where resistance to shear is important, point-anchor bolts may outperform nontensioned full-column bolts at a lower cost. In medium-to soft-strength rock, tensioned full-column bolts perform best. Also, varying the resin-steel ratio seems to have little effect on the properties of a full-column bolt, when proper resin mixing is ensured.

Jan 1, 1985

By J. C. Edwards

The Bureau of Mines developed a mathematical model that decribes the interaction of an automated breathing and metabolic simulator, or lung, with a self-contained· self-rescuer that is supplied compressed oxygen. The model can be used to predict the gas partial volumes of 0z, Nz, and COz in the lung and in the self-rescuer breathing bag for a prescribed metabolic state that characterizes the lung. Nonlinear rate equations are used to describe the temporal evolution of the gas partial volumes. A numerical procedure was established with a FORTRAN computer program to solve these equations, which correspond to a given metabolic state. Examples are presented of applications of the model to predict bag volume and bag oxygen concentration changes with time when the bag is controlled by an automated breathing simulator. Under certain restrictive conditions, the model equations can also be used to analytically pre-dict the time required for the bag to reach a maximum or minimum volume. The model equation in this latter case was extended to transi-tions between metabolic states, with transitions described as exponential growth or decay processes.

Jan 1, 1985

By T. H. Jeffers

Significant amounts of cobalt, a strategic and critical metal, are present in readily accessible spent copper leach solutions. For example, recovery of cobalt at two major u.S. copper operations could produce about 1,300,000 lb Co annually, about 13 pct of domestic consumption. However, techniques such as solvent extraction and precipitation have not proven cost effective in separating and recovering the cobalt from these low-grade domestic sources. The Bureau of Mines has devised a procedure using a chelating ion-exchange resin to extract cobalt from a pH 3.0 copper leach solution containing 30 mg/L Co. Cyclic tests in 4-ft-high by 1-in-diam columns gave an average cobalt extraction of 95 pct when 65 bed volumes of solu-tion were processed at a flow rate of 4 gpm/ft2 of resin area. After an impurity scrub, eluates contained, in grams per liter, 0.4 Co, 0.2 Ni, <0.001 Cu, 1.3 Fe, 2.8 Zn, and 0.008 AI. Solvent extraction procedures to remove impurities, reject nickel, and concentrate cobalt produced a cobalt sulfate solution containing 80 g/L Co, 0.05 g/L Ni, and not more than 1 mg/L Cu, Fe, Zn, or AI. Based on data from commercial electro-winning operations, this solution appears suitable for production of metallic cobalt.

Jan 1, 1985

By D. E. Shanks

The Bureau of Mines investigated the effects of HCI concentration and solution temperature on the solubility and crystal form of the chlorides of Co, Mn, and Ni when sparged with HCI gas at temperatures of 20°, 40°, and 60° C. Increasing HCI concentration in solution caused the chlo-rides of Co, Mn, and Ni to crystallize (salt out) because of the common ion effect. The salting-out crystallization was most effective for NiCI2, which had a solubility of 0.7 pct at 20° C and maximum HCI concentration. COCl2 salted out to a minimum solubility of 9.4 pct at 20° C and 22 pct HCI concentration and increased in solubility at greater HCI concentrations because of the formation of chloride complexes. MnCl2 was intermediate in behavior. The effect of temperature on solubility was greatest for CoCl2 and least for NiCI2, 15 and 7 pct change, respectively, over the temperature range of 20° to 60° C. The salted-out chlorides of cobalt and nickel formed the hexahydrates and those of manganese formed the tetrahydrate in saturated metal chlo-ride solutions at 20° C and low concentrations of HCI. Increasing the temperature or the HCI concentration caused a 108s in waters of hydra-tion. At 60° C, the salted-out crystals of NiCl2 formed the tetrahydrate in HCI concentrations up to 18 pct and the dihydrate at higher concentrations, while cobalt and manganese chlorides formed the dihydrates, even in water.

Jan 1, 1985

By W. D. Riley

The Bureau of Mines is conducting research on methods for the rapid identification and sorting of mixed scrap metals and alloys so that domestic scrap resources can be fully utilized. One method, spark testing, is the examination of the pattern of sparks that results when a metal or alloy is ground on an abrasive wheel. This technique requires experienced sorters. Bureau researchers have shown that spectrophotometric methods can be used in lieu of the highly skilled sorter. The spectra of a mild steel, an HSLA steel, several stainless steels, and four nickel-base alloys have been measured. Differences in the spectra that are sufficient for identification are apparent.

Jan 1, 1985