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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 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 S. C. Termes

To help develop the basis for new fine-particle separation methods, the Bureau of Mines has investigated the use of cross-linked starches containing four chelating groups--carboxylate, iminodiacetate, dietha-nolamine, and xanthate--as flocculants for selected metal oxide and hydroxide mineral fines. It was found that those starches capable of interacting with the mineral surface by a chemisorpti,on mechanism (as indicated by zeta potential measurements) produced the highest recover-ies and'grades of the metal oxide or hydroxide when flocculated from a binary mixture with quartz. The effects of pH, dispersing agent, stirring rate, stirring time, and starch dosage on selective flocculation were studied for binary mixtures of hematite and chromite with quartz. Floc strength becomes important in achieving maximum recoveries by mechanical postflocculation separations.

Jan 1, 1985

By M. M. Jones

Natural brines are potential domestic resources of minerals. The brines of Searles Lake, CA, for example, contain an estimated one-fourth of our current reserve of tungsten. A key to Bureau of Mines research to recover this critical mineral is the ability to quantitatively measure concentrations of particular constituents in the large number of brine samples and process solutions produced under a multiplicity of test conditions. This paper describes procedures used to determine arsenic, boron, phosphorus, silicon, and tungsten in these solutions by simultaneous inductively coupled plasma spectrometry. A variable in-ternal standard method was used to compensate for tungsten interference on the other analytes in tungsten concentrates, and matching standards were used to determine tungsten in raw brine. Other solutions were analyzed using normal techniques. Analytes were determined down to 1 mg/L with an average precision of 2.5 pet relative standard deviation. Accuracy, estimated using synthetic solutions and by comparison with values obtained by other methods, averaged about 2.5 pet. The methods were rapid, required little sample preparation, and provided the needed sensitivity.

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 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 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 J. E. Gebhardt

External control of the electrochemical potential of a bed of mineral particles has been investigated by the Bureau of Mines as a method for controlling particle inter-action with organic collectors and thus, flotation response. A cylindrically shaped, 200-to 300-g bed of sulfide mineral particles was used as the working electrode to examine the potential distribution in the bed. The dissolved oxygen concentration of the electrolyte had a significant effect on the potential profile across the mineral bed. Low oxygen levels were necessary to achieve uniform electrochemical potential distributions. Flotation separation of a chalcocite-pyrite mineral mixture by controlled potential was achieved using ethylxanthate, but the flotation behavior of chalcocite and pyrite from the mixture does not follow the flotation behavior of the individual minerals. That is, the presence of another sulfide mineral alters the flotation behavior with ethylxan-thate. Galvanic interaction due to mineral-to-mineral contact between chalcocite and pyrite contributes to differences in the recovery. Chalcocite dissolution products had a deleterious effect on pyrite flotation by activating flotation below -0.1 V (saturated calomel electrode) and depressing flotation above -0.1 V. Pyrite dissolution products had no effect on chalcocite flotation.

Jan 1, 1985

By Jon K. Ahlness

The Bureau of Mines investigated technologies for testing the integrity of in situ leach mining wells, as required by environmental regulations. To test for leaks, inflatable packers were used to seal the well casing. Laboratory testing determined that the packers could contain a casing pressure up to 50 to 60 psi (345 to 414 kPa) less than the packer inflation pressure. Single-and double-packer configurations were successfully field-tested in 32 wells ranging from 500 to 530 ft (153 to 162 m) in depth. A rigid pipeline and a hoist truck were used to run the packers in and out of the wells for the double-packer tests, which averaged 2-1/4 h each. In an effort to decrease the time of the rigid-pipe double-packer test. a self-contained trailer-mounted test system was designed and built. It utilizes a winch and steel cable to run the packers in and out of the well and high-pressure nylon tubing for packer inflation. This system was successfully field-tested in eight wells averaging 650 ft (198 m) in depth and resulted in a time savings of 13 pct and an operator-hour reduction of 42 pct.

Jan 1, 1985

By J. P. Hansen

The Bureau of Mines has investigated the S02 leaching of MgO from high-MgO-bearing Florida phosphate concentrates. The S02 was effective in leaching some of the MgO from three phosphate concentrates; flow rate of the S02 and leach time were major factors in determining the amount of MgO leached. Calcining the samples, then grinding to minus 200 mesh, and elevating the leach temperature gave only small increases in the amount of MgO leached. The research also showed that some of the MgO was so intimately associated with the phosphate mineral that it could not be removed by S02 leaching. This amounted to about 0.6, 0.7, and 1.0 pct MgO in three leached residues. The calculated heads for the three concentrate samples averaged 1.4, 1.1, and 1.5 pct MgO, respectively, before leaching.

Jan 1, 1985

By Ronald H. Church

As part of the Bureau of Mines health and safety research program in strata control, a ground-penetrating radar (GPR) system capable of pene-trating approximately 10 ft into the mine roof has been devised to identify anomalistic conditions. The GPR system consists of a transmitter with carrier frequencies of 250, 500, and 1,000 MHz, utilizing a dipole antenna, and a receiver, consisting of a dipole antenna fed into a sampler with a time base housed in a storage oscilloscope. A computer was utilized for data acquisition and data processing. Data analysis by computer enhancement revealed recognizable return ra-dar signatures from the middle man rock and main roof of the test site. These stratigraphic anomalies can be cataloged for recognizable fea-tures, which from the past history of the mine may have been shown to create strata control problems. Early recognition of such features could lead to immediate corrective actions and result in the saving of lives.

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 B. W. Jong

The Bureau of Mines studied reinforcement of sulfur concretes using glass, polyester, and aramid fibers. The objective of this research was to determine the feasibility of fiber-reinforcing the sulfur concrete to enhance the flexural properties. Optimum fiber sulfur concrete compositions were formulated with a cement-to-fiber ratio of 9.0:1 for glass-fiber and polyester-fiber sulfur concretes and 12.1:1 for aramid-fiber sulfur concretes. Test samples were prepared using techniques developed by the Bureau of Mines. Flexural strength values of up to 50 pct of compressive strength values were achieved with fiber additions. With non-fiber-reinforced sulfur concrete, the values ranged up to 20 pct. The impact strength and fracture toughness of sulfur concretes were increased sig-nificantly by reinforcement with glass or with aramid fiber and were adversely affected by use of polyester fiber. Strain tolerance was doubled and failure mode was shifted from catastrophic to noncatastrophic type by adding glass fiber. The glass-fiber and aramid-fiber sulfur concretes are resistant to acid corrosion and have proved durable in freeze-thaw cycles. This laboratory and field evaluation has shown that fiber reinforcement of sulfur concrete is feasible and that it enhances the flexural properties.

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 C. W. Smith

The Bureau of Mines conducted physical and chemical beneficiation studies on three samples of waste investment casting molds to devise a method to liberate and recover zircon. Rod mill grinding, autogenous attrition grinding, and caustic leaching were liberation methods inves-tigated. Flotation, gravity separation, and caustic leaching and sizing were recovery methods investigated. Flotation techniques produced con-centrates containing up to 74.2 pct zircon with a zircon recovery of 53.4 pct. Gravity concentration produced concentrates containing up to 98.6 pct zircon; however, recovery of the zircon was only 57 pct. Caustic leaching and sizing produced concentrates containing up to 98 pct zircon with attendant recoveries of 81 pct.

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