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By Jack I. Paige

The Bureau of Mines conducted studies to provide data on the room temperature mechanical properties of Ti-6Al-4V alloy cast in waterglass-bonded zircon sand and to determine the effect of hot iso-static pressing (HIP) on these properties. Data on the cast and annealed Ti-6Al-4V alloy were compared with published data for forged and investment-cast Ti-6Al-4V alloy. The average Charpy V-notch impact strength compared favorably with the typical values of 17 ft?lbf for wrought material and 19.2 ft?lbf for investment-cast material. The room temperature mechanical proper-ties of cast and annealed material compared favorably with published values for investment-cast Ti-6Al-4V alloy and exceeded the specifications for (1) titanium and titanium alloy castings, grade C-5 according to ASTM B367-69, and (2) titanium alloy bars and forgings as specified in AMS4928H, except for the AMS4928H minimum requirement for reduction in area (25 pct). The minimum requirements are: tensile strength, 130 ksi; yield strength, 120 ksi (0.2 pct); and elongation, 6 pct. None of the specimens tested met the AMS4928H minimum requirement for reduction in area. The HIP process healed the internal casting porosity in the test specimens, but the fatigue strength was not significantly improved. The fatigue properties of both the cast and cast plus hot isostatically pressed castings were significantly lower than those of wrought products.

Jan 1, 1984

By R. P. Vinson

The Bureau of Mines examined the effects of high humidity and water droplets on the GCA Corp. real-time aerosol monitor (RAM--l). which uses a lO4mm cyclone preseparator. Tests were conducted both in a laboratory and in a full-scale model mine entry. The laboratory tests were conducted in a test chamber saturated with moisture and water droplets. Under these extreme conditions. the RAM-I responded by indicating dust concentrations of 1-1/2 to 2 mg/m3? although the air was dust free. Within the first 2 h of each test. water accumulated in the cyclone and affected the cyclone particle separation characteristics. resulting in readings of 3 to 4 mg/m3. In addition. condensation formed inside the RAM-I case and affected the liquid crystal display (LCD). However. the full-scale mine entry tests revealed that the RAM-I can function ac-ceptably in an atmosphere of water vapor and water droplets similar to the most severe conditions found in an underground mine.

Jan 1, 1984

By M. M. Tilman

The Bureau of Mines evaluated corrosion resistance of Split Set friction rock stabilizer mine roof bolts to aid in better prediction of useful service life. Electrochemical corrosion testing was conducted utilizing an automated corrosion measurement system. Natural and/or synthetic mine waters from four uranium and two copper mines were the test media for the two types of high-strength, low-alloy (HSLA) steels from which Split Set stabilizers are manufactured, and for galvanized steel. Tests were conducted with waters of minimum and maximum dissolved oxygen content at in-mine water temperatures. Retrieved Split Set stabilizers were also evaluated for property changes. Galvanized steel was found to be far superior to the unprotected steel in general corrosion resistance; limited tests indicate little ten.dency to pitting, contrary to behavior for the uncoated steel. Copper-bearing HSLA steel was slightly more corrosion resistant than non-copper-bearing HSLA steel. Statistical analyses resulted in development of equations relating dissolved oxygen, chloride, sulfate, and magnesium contents of mine waters to corrosion rates of the two HSLA steels (nongalvanized). An equation was developed that relates corrosion rates of galvanized steel to mine water temperature and dissolved oxygen content. Variable conditions in mine environments make corrosion damage difficult to predict and emphasize the need for corrosion prevention and control.

Jan 1, 1984

By W. C. McBee

Technology for the preparation of densifiable sulfur concrete (sulfapave) materials has been devised by the Bureau of Mines. The materials are intended as new construction materials for use in corrosive areas where conventional materials fail. A series of modified sulfur cements were developed, which can be used in combination with dense-graded aggregates to prepare sulfapave materials with excellent corrosion-resistant properties. The materials can be mixed, laid, and compacted into place with conventional hot-mix asphalt pavi.ng equipment. Mixture designs utilizing 5-to 30-pct-modified sulfur cements and dense-graded aggregates gave material properties ranging from rigid to flexible. Laboratory corrosion tests in sulfuric acid showed no material loss or deterioration of physical properties over a 1-year test period in concentrations ranging from 0 to 60 pct at ambient temperatures. Preliminary results on field testing the materials for durability to weathering, corrosion, and traffic have been excellent, with no evidence of failure in the materials.

Jan 1, 1985

By Seth C. Schaefer

The Bureau of Mines investigated the thermodynamic properties of Bi203 (bismuth sesquioxide) and Sn02 (stannic oxide). Standard Gibbs energies of formation (AGfO) of these compounds were determined with high-temperature electromotive force (emf) cells using stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained from the cell

Jan 1, 1984

By D. J. Bauer

The Bureau of Mines has conducted extensive studies on the recovery of alumina from kaolinitic clay by a HCI leaching-HCI sparging process. The current study reports a modification of the process, which involves a double-leaching system. The first leach of the calcined clay is made at as high a HCI acid strength as possible so that the dissolution of aluminum chloride hexahydrate (AlCI3*6H20) is suppressed, Most of the impurities, but very little aluminum, are soluble in the strong acid. After liquid-solid separation and washing, the solids are leached with recycled weak HCI, which dissolves the AICI3'6H2O. The pregnant liquor is separated from the gangue, and AICI3'6H2O is crystallized from solu-tion by injecting HCI gas. A proposed flowsheet is presented, and the effect of bleedstream size on AlC13'6H20 purity is discussed.

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 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 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 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 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 Charles A. Seitz

This Bureau of Mines report describes a chromatographic method for analyzing impurities in helium that utilizes a helium carrier gas contain-ing 25 to 30 ppm Ne. An example of the effect of trace amounts of nitrogen, methane, and moisture on the detector's response is shown. The added neon in the carrier does away with irregularities of the analysis which were experienced when the carrier contained up to 3 ppm Ne. The addition of 25 to 30 ppm Ne causes a loss of sensitivity, but the re-maining sensitivity is adequate for routine analyses. The high-neon carrier allows positive and more linear responses for eight impurities: neon, hydrogen, argon, oxygen, nitrogen, methane, carbon dioxide, and ethane. Neon concentration levels of 0.02 to 125 ppm in helium carrier gases were studied. The high-neon carrier has been in successful rou-tine use in Bureau of Mines helium facilities since October 1981.

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 F. J. Perzak

The Bureau of Mines conducted a study to develop a standard fire test for 5-gal containers used for storing combustible fluids in underground coal mines. A standard test method was developed which evaluates the performance of the container in a 4-min tray fire. Bureau investigators used the standard test method to evaluate several types of closed 5-gal plastic and metal cans in outdoor tests. Each can tested contained 1 gal of nonfire-resistant (NFR) hydraulic oil. A container failed the test if it lost its contents in any of seven trials. Contents spilled either as a result of thermal rupture or melting. Fewer than 10 pct of the metal containers failed this criterion, but all the plastic containers failed. The metal container failures were usual-ly due to tipping over during pressure relief, which spilled the NFR oil. Replacing the NFR oil in the container with kerosene resulted in failure of more than 30 pct of the metal containers. The standard tests and preliminary tests showed that plastic containers are not equivalent to metal containers in their ability to contain combustibles such as lubricants and greases in a fire. For solvents and lubricants more volatile than NFR hydraulic oil, approved metal safety containers are recommended.

Jan 1, 1985

By G. A. Smyres

The Bureau of Mines conducted laboratory studies to determine the feasibility of chlorine-oxygen leaching for treating low-grade zinc sul-fide flotation concentrates. Recovery of zinc sulfides by flotation from complex fine-grained sulfide ores is substantially higher in low-grade bulk sulfide concentrates than in the high-grade cleaned concen-trates required for smelter feed. However, there is no commercial process in the United States for the treatment of low-grade bulk zinc sul-fide concentrates. Leaching experiments using reactors of 500-mL and I-gal capacity were conducted on a bulk concentrate containing 19.3 pct Zn, 35.6 pct Fe, and 39.4 pct S. The effects of pressure, temperature, and percent solids on extraction were investigated. The chlorine-oxygen leaching procedure showed promise for treating the concentrates. Zinc extractions of 95 pct or more were obtained by leaching at 50 pct solids in the temperature range of 1000 to 1200 C. Zinc extractions by leaching with chlorine followed by oxygen at reactor pressures of 50 to 100 psig were independent of pressure.

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