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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 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 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. 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 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 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 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

By T. H. Jeffers

The Bureau of Mines conducted a laboratory investigation of copper electrowinning from electrolytes produced by solvent extraction. The purpose of the research was to gain a better understanding of the fundamental relationship between copper electrowinning conditions, anode corrosion, and cathode purity. Processing variables were evaluated in a cyclic semicontinuous system in which the depleted electrolyte was used to strip copper from loaded organic extractant. For the production of high quality copper cathodes, the electrolyte was dosed with cobalt and stripped of organic solvent extraction reagent. An optimum cobalt addition of 60 ppm, and removal of the entrained extractant with activated carbon provided the best conditions for electrowinning copper containing the least amount of lead and controlling anode corrosion. As little as 13 ppm of the entrained organic extractant, LIX 64-N, significantly accelerated anode corro-sion. However, the addition of 1,000 ppm of organic diluent kerosine did not affect anode corrosion. After cobalt dosing and removing the entrained extractant, cathodes containing less than 2 ppm lead were consistently electrowon at widely varied current densities, electrolyte copper and acid concentrations, and temperatures. Dosing of the electrolyte with selected impurities including magnesium, aluminum, manganese, and iron did not affect the cathode purity. However, 0.05 giL of chloride ions markedly increased anode corrosion and the sub-sequent transfer of lead to the cathode copper.

Jan 1, 1985

By H. E. Hilliard

The Bureau of Mines investigated hydrometallurgical procedures for concentrating precious metals from a mechanically processed metal fraction of obsolete military electronic scrap. Feed material for the leaching procedures described in this report was the high-tension-separated metal concentrate obtained as a fraction from mechanically processing partially stripped electronic units. Initial pretreatment with a 20-wt-pct-NaOH solution solubilized most of the aluminum. After washing, the resulting residue was incinerated to destroy any organics attached to metal particles. The incinerated residue was leached with 20-vol-pct H2S04 solution using two methods, countercurrent pressure and ultrasonic-aided leaching to solubilize the base metals, predominantly copper. Silver was recovered from the base metal leach residue using 50-vol-pct HN03, and gold contaminated with several percent palladium was recovered from the silver leach residue using aqua regia. The impure silver and gold plus palladium products represent about 1.5 wt pct of the high-tension-separated metal concentrate. Included is a three-step process evaluation study of mechanical processing of general electronic scrap and two hydrometallurgical procedures for leaching high-tension-separated metallic concentrates obtained from the mechanical processing step. Process evaluation concluded that only mechanical processing is economically viable.

Jan 1, 1985

By J. S. Hansen

To advance technology that can conserve critical materials, the Bureau of Mines investigated a cast-on hard-surfacing that wear resistance and confines alloy additions to wear-prone surfaces. Wear-resistant material in form is on a polystyrene , the is embedded in a mold of unbonded s and the wear-resistant material is transferred to a cas surface at the time of For low-stress abrasion, derived from high-carbon ferro-chrome had higher wear resistance than did commercially available weld-hard. The microstructure of the was typi-white iron carbides. Free carbon added to the ferrochrome powder produced more M7C3 carbides than did material contained in surfacings made from ferrochrome alone, and improved the wear resistance. Several white iron powders with greatly reduced chromium contents also white iron contain-M7C3 carbides. One derived from white iron powder had wear resistance to that of weld-deposited hard facings. Among the parameters investigated, surfacing thickness was found to have a or influence on diffusion of elements out of the , microstructure, and wear resistance. The results of field tests on bucket-wheel excavator teeth and plowshares with cast-on hard surfacing are given.

Jan 1, 1985

By M. M. Tilman

The Bureau of Mines conducted research to determine the feasibility of strengthening experimental magnesium-base sheet alloys by strain softening induced by controlled cold rolling followed by selective heat treatment. Relatively small alloying additions having potential for producing strain softening were selected from metals that are readily avail-able. Tensile properties comparable to minimum properties of the most commonly used magnesium-base sheet alloy AZ31B, in the H24 condition (strain-hardened and partially annealed), were obtained in an Mg-IMM (mischmetal)-O.5Mn alloy after strain-softening rolling followed by heat treatment. Tensile properties of the experimental alloys in certain conditions are also compared with minimum tensile properties of other standard magnesium sheet alloys. Incidental to the principal objectives, apparent superplastic behavior was observed in three experimental magnesium-base alloys containing MM, MM plus manganese, and MM plus zirconium.

Jan 1, 1985

By M. Hayashi

The Bureau of Mines conducted laboratory studies on Idaho mudstones to examine techniques for extracting vanadium. Recovery of vanadium from low-grade sources could contribute to future vanadium production and reduce reliance on imports. An Idaho mudstone surface sample containing 0.30 pct V205 and an underground sample containing 0.21 pct V205 were used in the extraction tests. Leaching of the surface sample for 18 h at 800 C with the addition of up to 1,000 lb/ton H2S04 recovered 70 pct of the vanadium. How-ever, leaching of the underground sample under the same conditions re-covered only 47 pct. By adding 15 wt pct NaCl and roasting the samples at 7500 C for 2 h, followed by leaching with 800 lb/ton H2S04, vanadium extractions were increased to 78 pct from the surface sample and 83 pct from the underground sample. Water leaching of samples roasted at 7500 C for 4 h with a 25-wt-pct NaCI addition yielded about 60 pct of the vanadium from both surface and underground samples. Autoclave leaching at 2000 C for 3 h with 1,000 Ib/ton H2S04 extracted 97 pct of the vanadium from the surface sample and 86 pct from the underground sample. An exploratory solvent extraction investigation to purify and concentrate vanadium in the leach solution using several organic reagents was also conducted.

Jan 1, 1985

By James C. Barker

The analytical variability encountered when sampling for platinum-group metals (PGM) was statistically evaluated during a 1983 study by the Bureau of Mines and the University of Alaska. Sampling procedures were designed to systematically incorporate commonly used reconnaissance exploration techniques under actual field conditions. Analytical variability was evaluated at each procedural step. Analytical data from each sample from a single deposit grouped relatively well around the calculated mean for that deposit. Standard deviations did not exceed 43 pct of the mean for any of the deposits; more commonly, the deviation was about 25 pct. Statistical treatment of the data by analysis of variance indicated the most important source of error is selection of the sample site. Two or more replicate samples appear necessary to adequately quantify the PGM content. Secondly, significant variation occurs during preparation of a pulverized split for fire assay. The optimum sample size was in the 11-lb range; larger samples did not appreciably reduce variability. Smaller samples generally indicated a higher degree of variability. Evaluation of the sample method suggested the common grab sample, if carefully taken, is a useful indicator of the general range of PGM concentration but potentially includes a considerable margin of error.

Jan 1, 1985

By D. R. Hanson

This Bureau of Mines study examines the acoustic vibrational spectra of rock slabs in the range of 0 to 5,000 Hz. The power spectra of so-called drummy rocks were found to be diagnostically enhanced in the range of 200 to 1,000 Hz. Comparison of the power in this band with that in a band from 3,000 to 3,500 Hz provides a quantitative measure of rock stability. A prototype field instrument was designed, constructed, and field-tested. This battery-powered instrument computes the power contained in the two frequency bands mentioned, compares the magnitude of these two quantities, and displays a number that is related to the detachment of the block tested. Field tests show that this instrument is capable of giving reliable measurements of block stability under conditions of noise and dust that would seriously degrade the accuracy of normal sounding techniques.

Jan 1, 1985

By Gary P. Sames

Shale roof deterioration in coal mines. caused by ventilation air humidity fluctuations, is a common ground control problem. Shale roof deterioration often results in increased accidents, decreased production, inadequate ventilation, and increasing operating costs in maintaining haulage roads and airways. The results of Bureau of Mines research indicate that air tempering entries are an effective method of controlling deterioration prone shales. Some of the conclusions and recommendations drawn from Bureau research include (1) moisture sensitive shales will react adversely to moisture gains and losses, (2) the majority effect of specific humidity fluctuations can be concentrated in and absorbed by tempering entries, (3) tempering entry panels should be located as near to the main intake as possible, (4) tempering panels should be designed for a conservative recovery and provide a minimum of 20-to 30-min air residence time, (5) ventilation and escapeway requirements must be considered early in panel design, and (6) an efficient support and sealant plan can increase the life expectancy of a tempering panel.

Jan 1, 1985

By R. B. Prater

The Bureau of Mines conducted research to separate the F from byproduct Zn concentrates obtained from fluorspar (CaF2) production, as part of the Bureau's effort to devise efficient, environmentally acceptable technology for recovering Zn from resources considered undesirable by Zn producers. Sulfuric acid (H2SO4) was found to be effective in F removal, while ammonium carbonate [(NH4)2C031 was not. The most important variables for reducing the necessary residence time were found to be temperature and agitation. Optimum leaching conditions were 75° C and 500 r/min for 2 h at 40 pct solids with 0.2 g acid per gram of concentrate, which resulted in a 98.3-pct F extraction. Zinc losses during F removal were in the range of 2 to 3.3 pct. Other elements such as Fe, Cd, Ca, and Cu were also partially dissolved. About 93 pct of the F was removed from the leach solution by neutralization and precipitation with calcium hydroxide [Ca(OH)2]. Additional treatment might be necessary to limit the buildup of soluble elements in the recycled leach solution.

Jan 1, 1985

By R. L. Soderberg

Large open stopes mined by vertical crater retreat or sublevel s are sometimes backfilled with uncemented sand to support the stope walls and alleviate rock bursts. The failure of bulkheads in two different mines prompted a research project at the Bureau of Mines to prevent a recurrence of these failures. A series of laboratory tests with drains and sand filters was conducted to measure the bulk-head pressures when adequate drainage was maintained. Results showed that bulkhead pressure was reduced to near zero while drains were in operation, as compared to full hydrostatic pressure when drains were blocked or drainage was restricted. A relatively simple, free-draining bulkhead was shown to be adequate.

Jan 1, 1985

By R. D. Brown

There are techniques for separating aluminum alloys from mixed scrap, but there are no efficient ways to separate wrought aluminum from cast aluminum. This Bureau of Mines report describes a novel technique for separating mixed aluminum alloy scrap into cast and wrought aluminum alloy fractions. The technique, which uses conventional heating, fragmentizing, and screening equipment, exploits differences in the mechanical properties of cast and wrought aluminum alloys at elevated temperatures. The cast alloys become brittle at high temperatures owing to intergranular melting of regions of eutectic composition. This melting begins to occur as the solidus temperature for each alloy is reached. Solidus temperatures for casting alloys generally range from 520° to 580° C, but are above 600° C for most wrought alloys. Thus, the casting alloys are easily fragmented while the wrought alloys remain ductile in the proper temperature range. Starting with a mixture containing approximately 80 pct cast and 20 pct wrought alloys, fractions of 100 pct cast and 98 pct wrought have been produced.

Jan 1, 1985