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By Charles Seitz

The Bureau of Mines has modified its parts-per-billion helium-4 analyzer to improve the analytical capabilities of the instrument. The modifications resulted in the following improvements: (1) The analytical precision of the instrument for 10 consecutive analyses was improved to ±1 ppb at the 5,000-ppb helium-4 level, (2) the helium-4 sensitivity was increased almost tenfold, and (3) the minimum detectable limit for helium-4 was improved to 0.5 ppb. The modifications made to improve the instrument included replacing the ion-source control circuit with a direct-current solid-state design, controlling the temperature of the ion source, stabilizing and reducing the pumping rate of the vacuum system, and optimizing peak integration.

Jan 1, 1986

By James P. Bennett

The Bureau of Mines is investigating the acid resistance of ceramic materials to identify construction materials for emerging technology in chemical and metallurgical processes. Eight commercial ceramic materials, were evaluated: two red shale, two fireclay, one silicon carbide, one silica, one carbon, and one high-alumina. Samples were exposed to 10 wt pct H2S04 at 50° C and 10, 30, 50, 70, and 90 wt pct H2S04 at 90° C for time periods of 110 days. Statistically significant changes in cold crushing strength were observed in the silicon carbide and car-bon materials. Weight changes and the leach rate of Al, Ca. Fe. K, Mg, Na. Si, and Ti were also monitored. The most severe corrosion conditions were at 90° C and 30 to 50 wt pct H2S04 for the acidproof and at 10 wt pct H2S04 for the acid-resistant materials. The silica and the high-alumina materials were the most acid-resistant, followed by the higher density red shale and fireclay.

Jan 1, 1986

By Rustu S. Kalyoncu

Nonoxide ceramics with improved high-temperature properties could substitute for high-temperature alloys and reduce toe Nation's dependence on imports of Cr, Co, Ni, and Mn. To meet this objective, the Bureau of Mines conducted research to synthesize u1trafine reactive boron nitride (BN) powders BN powders were prepared at temperatures ranging from -75? to 750? C. Low-temperature reactions (-75? to 200? C) between boron halides and N compounds led to formation of e1emento-organic compounds that were thermally decomposed to u1trafine (approximately 100-to 150-A particle size) reactive BN powders. BN powders were also prepared through the reaction of a 10w-me1tinginorganic B compound (boric acid, borax) with an organic N compound (carbimide and thiocarbimide) in N2 and/or ammonia (NH3) atmospheres at temperatures between 500? and 750? C.

Jan 1, 1986

By N. Greninger

The Bureau of Mines examined the possibility of a seasonal variation of respirable dust concentration in U.S. coal mines. The first step was to review company and MSHA-inspector dust samples that had been collected during the past several years in 14 selected mines for compliance purposes. Results indicated severe scatter in data; most standard deviations of the dust concentrations measured in winter and summer months were comparable in magnitude with the mean values of dust concentrations for the seasons. Therefore, a detailed statistical analysis was conducted. At the 90% confidence level, the company samples of three mines had winter means 0.15 to 0.54 mg/m3 higher than the summer means; six mines had negligible seasonal variations; and five mines had winter means that ranged from higher to lower than the summer means. Inspector data, however, were too sparse for analysis. In view of both the low frequency of occurrence of a seasonal effect and its wide scatter in several of the mines, the study was ended with the conclusion that seasonal varia-tion in respirable dust levels, in general, is an insignificant factor.

Jan 1, 1986

By D. R. Brooks

The Bureau of Mines has tested a dewatering technique for phosphatic clay waste. The technique utilizes a flocculant, polyethylene oxide (PEO), that forms strong, stable flocs that can be dewatered on a static screen followed by further dewatering on a rotary screen or trommel. In field tests conducted in central Florida, clay wastes containing approximately 4 pct solids have been consolidated to greater than 20 pct solids. The rate at which PEO-treated material continues to dewater in a mine cut also was monitored. Preliminary results indicate that PEO-treated material will dewater to 30 pct solids in 80 days. Pretreatment of phosphatic clay waste with lime lowers the PEO dosage required for dewatering.

Jan 1, 1986

By R. L. King, J. Cervik, A. A. Campoli

The Bureau of Mines performed laboratory experiments to evaluate the triboelectric effect of particulate-laden gas streams on polyethylene pipe at various velocity, humidity, dust-size, and dust-load conditions. Charges in excess of 10 kV were produced on the outside and inside surfaces of laboratory pipe samples, when exposed to 40 pct relative humidity (RH) gas stream containing coal dust. However, no charges were produced in laboratory tests that duplicated the over 75 pct RH and dust-free gas streams found in working underground pipelines. Bare cop- per wire, which is wound around the polyethylene pipe in a 1-ft (31-cm) spacing and grounded, eliminated the charge on the outside surface of the pipe, but not on the inside of the pipe surface,

Jan 1, 1986

By M. J. Ferrante

Relative enthalpies of high-purity disodium hexatitanate (Na2Ti6013) were measured at the Bureau of Mines to provide new thermodynamic data needed to advance the technology of materials. Measurements from 298.15 to 1,478 K were made by drop calorimetry with a copper block. Tabulated values are listed for the standard relative enthalpy, heat capacity, en-tropy, and Gibbs energy function between 298.15 and 1,500 K. Enthalpy data are also given in equation form and are combined with thermodynamic data from the literature to derive values of standard enthalpies of formation, Gibbs energies of formation, and logarithms of the equilibrium constants of formation. Similar calculations were made for the reaction of Na20 with Ti02.

Jan 1, 1986

By S. C. Termes

The Bureau of Mines has used Fourier transform infrared spectroscopy (FT-1R) to study in situ reactions of aqueous solutions of potassium ethylxanthate with CU(II)-and Pb(II)-activated sphalerite plates, in which the plates were both the infrared-transparent windows and the reacting surfaces. A copper (I) ethylxanthate formed predominantly with Cu(II)-activated sphalerite, regardless of the activation time. The products formed on Pb(II)-activated sphalerite depended on the activation times; a short activation time (30 min) yielded a lead ethylxanthate-like product, but a long activation time (90 min) yielded a considerable amount of dixanthogen.

Jan 1, 1986

By G. A. Smyres

A GaC12--B2 l-eachtng procedure and meEal-recovery method for treating an arsenical Cu-Co sulfide concentrate was developed by the Bureau of Mines as an alternative to smelting, which is no longer considered an environmentally acceptable method for treating arsenic-containing ores. The procedure involved leaching in a CaC12 solution with CaC03 for 96 h at 26 pct solids (concentrate and CaC03), 1150 C, and a pressure of 50 psig (345 kPa) with oxygen. More than 98 pct of the cobalt and 97 pct of the copper were extracted, and 99.98 pct of the arsenic and 99.9 pct of the iron remained in the leached residue. A filtration rate of 2.9 gal/(ft2.h) [118 L/(m2.h)] and a cake formation rate of 36 Ib/(ft2.h) [172 kg/(m2.h)] were obtained by filtering reacted pulp at 1000 C. More than 99 pct of the copper in the pregnant solution was extracted as CuCl2 by golvent extraction with a new copper extractant. Copper was stripped from the loaded organic with a sulfate-chloride solution, which was used as the anolyte for electrowinning of copper in a membrane cell. Copper plate produced was more than 99.99 pct pure and requi.red 0.81 (kW'h)/lb Cu [1.78 (kW·h)/kg Cu]. Cobalt sulfide was precipitated at pH 3 with Ca(HS)2.

Jan 1, 1986

By D. A. Stanley

The Bureau of Mines is investigating a method of dewatering flocculated fine-particle waste that involves treating the waste with a high molecular-weight polymer such as polyethylene oxide (PED) followed by dewatering on a static screen and/or in a trommel. Dilution of the polymer solution used for dewatering and use of the ion-exchanged form of the montmorillonite clay were found to be major factors determining the amount of polymer required to dewater clay-containing slurries. The amount of polymer, A, required to dewater ion-exchanged montmorillonite can be described by the equation, An = kC + b where n, k, and b are empirical constants and C is the concentration of the polymer solution used for dewatering. Clays that require large amounts of polymer for dewatering also dewater to a lower solids content. The concentration of the polymer solution is important because it affects the radius of the polymer coil in solution and hence its ease of transfer to a bridging configuration by shear. The constant, n, a function of the charge to hydrated radius of the exchange ion, relates to the strength of the bond between the polymer and the surface of the clay through a water bridge. The constant k is related to the hydrated radi-us for sodium or to the unhydrated radius for the other exchange ions.

Jan 1, 1986

By R. G. Sandberg

The Bureau of Mines investigated a hydrometallurgical procedure to recover gold, silver, and byproduct lead from a complex lead-zinc sulfide ore. A ferric chloride (FeCI3) preleach, at 40° C in 6 h, extracted about 50 pct of the zinc and formed insoluble silver and lead chlorides. Subsequent acid thiourea leaching, for 1 to 3 h at 40° C, extracted about 85 pct of the gold and silver. Lead chloride was solubilized from the remaining residue with NaCI brine solution at 55° C in 1 h. Lead metal was recovered from the brine solution in an electrolytic cell with an anion perms elective membrane at a current efficiency of 95 pct and current density of 100 A/m2. Spent FeCl3 leach solution was reoxidized in the anode compartment at a current efficiency between 75 and 95 pct.

Jan 1, 1986

By D. N. Tallman

The electrokinetic properties of MgO have been utilized to simultaneously filter suspended solids and remove trace amounts of dissolved heavy metals from synthetic mine water. Greater than 95 pct removal of metals from influent at neutral pH containing 1 to 6 mg/L of dissolved Cd, Cu, Mn, Ni, and Zn can be routinely achieved by filtering through a granular bed of MgO at flow rates typical of rapid sand filtration (0.3 cm/s). Filtrate concentrations of most metals can be maintained below 0.1 mg/L for 160 bed volumes or more loading. The more mobile metals (those with larger solubility products) are more difficult to remove, and are strongly bonded to the MgO granules so that chemical stripping with chelating agent is required to clean the bed. Less mobile ions are easily removed by the filter and are effectively stripped by conventional filter backwashing. The fraction of metals recovered by chemically stripping the loaded MgO filters correlates to the zero points of charge of the metals. This process may be applicable to removal and recovery of trace amounts of heavy metals in mine drainage that is partly neutralized by liming. Also, since many of these metals are critical and strategic, the technique can be adapted not only to recycle process water from mineral and milling waste streams, but also to reclaim their metal values.

Jan 1, 1986

By Dennis A. Hansen

The solubility of anhydrous aluminum chloride in solutions of titanium tetrachloride and vanadium tetrachloride was determined as part of a re-search project-by the Bureau of Mines to make a homogeneous alloy sponge of titanium, vanadium, and aluminum. Solubility curves were established using an autoclave at 75°, 100°, 125°, and 150° C. The solubility of AJC13 in TiC14 is 0.2 wt pct at 75° C; it increases to 18.3 wt pct at 150° C. The data concur with data from earlier researchers of this bi-nary system for 75° to 125° C. For the VC14-AlC13 binary system the solubility of AlC13 is 0.1 wt pct at 75° C, increasing to 1.6 wt pct at 150° C. For the TiC14-AlClrVC14 ternary system the solubility of AlC13 decreases from the values found with a pure TiC14-AlC13 system to the lower values found with a pure VC14-AlC13 system at the respective temperatures.

Jan 1, 1986

By J. C. Judd

The Bureau of Mines investigated the recovery of vanadium, uranium, and phosphorus from low-grade phosphorite ores and concentrate by leach-ing with H2S04. Samples containing 0.12 to 0.23 pct V20S, 0.009 to 0.012 pct U30S and 18 to 30 pct P20S were treated by batch-agitation leaching, roasting followed by acid leaching, salt-roasting followed by acid leaching, and leaching under pressure. Maximum recoveries using leaching alone ranged from 78 to 98 pct of the V20S and 74 to 88 pct of the U30S-Leaching under pressure resulted in extractions of 88 to 95 pct of the V20S and 84 to 89 pct of the U30S. Leaching following roasting--with or without NaCI--produced extractions of 97 to 99 pct of the V20S and 86 to 91 pct of the U30a. Depending on the technique(s) employed, phosphate extractions ranged from 89 to 99 pct. Solvent extraction laboratory tests were conducted to selectively re-cover vanadium and uranium values from acid leach solutions. An average of 95 pct -of the U30a was recovered using di(2-ethylhexyl) phosphoric acid, plus trioctylphosphinic oxide. Essentially all of the V20S was recovered with octylphenyl acid phosphate plus isodecanol. The phosphate remained in the raffinate.

Jan 1, 1986

By John W. Kopp

A major concern with blasting at surface mines is generation of ground vibrations and airblast and their effects on nearby residences. This Bureau of Mines report looks at the use of millisecond delays in blast design and their effect on the resulting ground vibrations and airblast. A total of 52 production blasts were instrumented and monitored at a surface coal mine in southern Indiana. Arrays of seismographs were used to gather time histories of vibrations and airblast. The data were analyzed for peak values of vibration and airblast and for frequency con-tent. Various delay intervals were used within and between rows of blastholes. Delay intervals within rows were 17 and 42 ms, and those between rows ranged from 30 to 100 msj these intervals are equivalent to 0.5 and 1.3 ms/ft within rows and 1.2 to 4.3 ms/ft between rows. Sub-sonic delay intervals within rows reduced airblast by 6 dB. Large delay intervals between rows reduced the amplitude of ground vibrations; their frequency depended primarily upon the geology of the mine site.

Jan 1, 1986

By T. M. Barczak

The term "resultant load vector" is defined as the representation of the forces applied to a longwall roof support element by strata activity through a single, quantifiable measure of support resistance. The relatively complex kinematics of the shield structure prohibits determination of support resistance simply from the summation of leg forces. In the research reported in this Bureau of Mines study, the mechanics of the shield structure were evaluated, and a technique was developed whereby the resultant shield loading could be determined by instrumenting supports with pressure transducers and strain gauges to measure leg, canopy capsule, and lemniscate link forces. This technique has been laboratory tested in the Bureau's Mine Roof Simulator. Functional relationships among variables were assessed, and confidence intervals were established for prediction of the resultant load vector parameters. Resultant load measurements were taken on five instrumented shields on an active longwall face in Colorado. Results were analyzed and found to be consistent with shield mechanics and anticipated roof behavior. Benefits to be derived from this research, future efforts, and long-range goals are discussed.

Jan 1, 1986

By Thomas L. Ochs

The Bureau of Mines is investigating the fundamental behavior of electric arcs in electric furnace operations. The electric arc is a poorly understood phenomenon. If the arc in a steelmaking furnace can be more carefully controlled, it should be possible to increase heat transfer to the melt, reducing both electrical and acoustical noise. As a first step toward a better understanding of the are, voltage and current signals from operating furnaces were analyzed. The results of the initial analysis show that instrumentation used in monitoring and controlling furnaces, such as meters and strip-chart recorders, gives incomplete or erroneous information to the operator and therefore leads to less than optimal control. Advanced instrumentation and analysis techniques, such as the waveform analysis used in these investigations, can improve the understanding of operation and the control of electric furnaces. This report describes the instrumentation and the numerical analysis methods used and compares these methods with standard metering and recording techniques.

Jan 1, 1986

By R. D. Wilson

Ten to twelve million tons of dust is produced by cement kilns annu-ally in the United States, resulting in a serious waste disposal problem. The Bureau of Mines investigated two alkali volatilization methods for converting this dust into materials for making portland cement and a useful potassium product. Portland cement kiln dust was found to be composed of finely ground cement raw materials (CaC03 and 8i02) having a layer of alkali sulfate (K2S04 and Na2S04). In this form, it cannot be directly recycled to cement kilns because concrete is weakened by a reaction between the alkali and the aggregate. Portland cements with 28-day strengths above 5,000 psi were produced from low-alkali residues using sintering and melting methods. For nearly complete removal of alkalies, primarily potassium sulfate, from cement kiln dust, a temperature above 1,300° C and a reducing atmosphere were required.

Jan 1, 1986

By Laxman S. Sundae

The Bureau of Mines designed, fabricated, and is using an in-seam tester (1ST) for in situ determination of coal cutting forces. This re-port describes the results of field tests conducted in the Pocahontas No. 3 and Upper Freeport seams to obtain peak and mean cutting forces during coal cutting with several bit geometries, including radial and point attack bits currently used on drum-type machines. Comparisons were also made between new and worn bits, and using data obtained from a Bureau-modified chisel bit. The test results show that longwall plough cutting (horizontal cuts) in bony coal bands (shale) requires >3 times the cutting force for the same cuts in a vertical direction. When no bony coal is present, the cutting forces required to make horizontal and vertical cuts are equal. Worn bits require 4 to 5 times more cutting and normal force than new or undamaged bits. Normal force increased drastically for the worn chisel bit. Peak force encountered in making independent cuts was found to be ~3 times higher than that required to make interactive cuts using a spacing-to-depth-of-cut ratio of 2. Both rake and clearance angles were found to have a significant effect on normal and cutting force.

Jan 1, 1986

By J. L. Holman

The Bureau of Mines is conducting research to recover strategic and critical metals such as Ni, Co, and Cr from mixed contaminated super-alloy scrap. One approach being studied involves melt refining of superalloy scrap to produce anodes for electrolytic deposition of Ni-Co alloy. This melt refining of superalloy turnings is described based on melt-oxidation and oxidation-carburization experiments, using roasted superalloy grinding sludge to supply the 0 needed to oxidize Cr and other readily oxidized elements to the slag. Controlled melt-carburization subsequent to oxidation improved the metal phase recovery of Ni and Co to well over 90 pct and decreased electrolytic solubility of Cr, Mo, and W by carbide formation. Electrolytic refining experiments were conducted using a controlled-potential mode (preset cathode potential). Data show effects of Fe and Cr impurities, cation concentration, electrolyte pH, S04-Cl electrolyte ratio, temperature, cathode potential, and cation-selective membrane use on current efficiency, current density, and deposit composition. Disposition of Ni, Co, Cr, MO, W, and Fe is compared for melt-oxidized versus oxidized-plus-carburized anodes. Deposits containing >97 pct Ni + Co (major impurity Fe) have been routinely obtained from scrap anodes. Research is continuing to improve deposit quality in sustained deposition and to recover Cr and other metals from refining slags and anode sludges.

Jan 1, 1986