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By R. H. Sprute

The Federal Bureau of Mines performed laboratory tests using direct current to dewater and densify fine-grained coal sludge in order to alleviate disposal problems and lead to recovery of high energy value often present in this waste. The laboratory tests described in the main body of the report were performed on thickened underflow (no flucculant added) from a northern Appalachian coal preparation plant. Solids in this slurry was very fine with 65 percent of the particles less than 0.1 mm in diameter. A variety of application procedures tested is exemplified by a test in which a soupy slurry (55 percent dry-weight moisture content) was converted into a firm dense material with a 20-percent dry-weight moisture content. These results were achieved in 3 hours with current density of 3.7 amp/ft2 and a power expenditure of 35 kwhr/yd3. The treated material has an average heating value of 10,400 Btu/lb. Varying current density, electrode configuration, and placement depth makes application of the treatment flexible. Two other types of sludge were tested briefly--thickener underflow from a southern Appalachian coal preparation plant with flocculant added, and sludge from an acid mine drainage treatment plant. The underflow responded well to the treatment, but response of the sludge from the acid mine drainage treatment plant was poor.

Jan 1, 1976

By W. L. Staker

The Bureau of Mines investigated the use of shredded automobile scrap for copper cementation. Air agitation was used to improve the cementation rate and prevent excessive buildup of copper on the iron. The pieces of scrap were too large to be properly evaluated in the laboratory; therefore, a pilot scale test unit was constructed and the process tested at field locations. Pregnant solution was obtained from industrial leaching operations, processed in the test unit and the barren solution and cement copper were returned to the plant process stream. The test results showed that the air-agitated launder containing auto-mobile scrap was an effective means for recovering copper from leach solutions. A continuous l4-day test run was made without a noticeable decrease in cementation efficiency. The most suitable scrap product was obtained from incinerated automobile hulks shredded in a hammer type of shredder. However, it was necessary to remove small pieces such as nuts and bolts because they interfered with the discharge of the copper product.

Jan 1, 1976

By J. M. Stuve

Low temperature and high-temperature calorimetric measurements were made by the Federal Bureau of Mines on high-purity samples of Re02(s) and Re03(s) to determine heat capacities and enthalpies. The temperature range of heat capacity measurements was 5 to 310 K for Re02 and 8 to 309 K for Re03. High-temperature enthalpy measurements alone were determined for pure Re207(s,1). The derived standard entropies are S°298 = 11.43±0.01 cal/deg mole for Re02(s) and S298 = 16.55±0.02 cal/deg mole for Re03(s). High-temperature enthalpy equations expressed in calories per mole are as follows: Re02 (s) , H-H298.15 = 16.002T + 1.600 X 10-3T2 + 3.522 X 105T-1 - 6,095 (298 to 1,400 K); Re03 (s) , H-H298.15 = 20.293T + 3.238 X 10-3T2 + 3.950 X 105 T-1 - 7,664 (298 to 1,000 K); Re207 (s) , H-H298.15 = 38.437T + 10.309 X 10-3T2 + 4.315 X 105 T-1 - 13,824 (298 to 413 K); Re207 (s) , H-H298.15 = 30.181 + 17.713 X 10-3T2 - 10,612 (413 to 600 K) ; Re207 (1) , H-H298.19 = 66.101T - 10,092 (600 to 700 K). Gibbs energy of formation (?Gf°) data and related functions over the temperature ranges investigated are tabulated for the three oxides.

Jan 1, 1976

By R. H. Jefferson

An electrochemical method to selectively determine sulfur dioxide in the presence of sulfur trioxide was investigated. A hydrophobic gas-permeable membrane separates the gas sample solution from an internal filling solution containing a fixed quantity of chloride ion and a sufficiently large excess of sodium bisulfite so that its concentration may be considered constant. Sulfur dioxide diffuses through the membrane to dissolve in the internal filling solution and liberates an equivalent quantity of hydrogen ions. The electromotive force between a precision-ground, flat-ended pH electrode, which acts as the sensing element, and a chloride sensing electrode, which acts as the reference element, gives a direct measure of S02 in the gas sample solution. Calibration curves in water, tetrachloromercurate (TCM) , and citrate buffer absorption solutions were closely parallel with slopes in their linear segments, ranging from 57 to 52 mv/decade of S02 concentration. The slopes compare reasonably well with the theoretically expected slope of 58 millivolts at 21° C. The water standard curve was linear with respect to the logarithm of S02 concentration from 1 to 1,000 ppm S02; the TCM standard curve was linear from 10 to 2,000 ppm S02; and the citrate standard curve was linear from 30 to 5,000 ppm S02' The high efficiency and nontoxicity of citrate favor it as a substitute for the conventionally used TCM in the absorption solution.

Jan 1, 1976

By John E. Kelley

Laboratory equipment, which simulates abrasive impacts between steel and minerals that might be present during pneumatic transport of coal, was used by the Bureau of Mines to characterize the potential explosion hazard of such collisions in an atmosphere of fine coal dust, air, and methane. A variety of coal mine rock materials, including sandstone, limestone, and pyrite-bearing limestone, were impacted with specimens of pipeline steel. Tests were con-ducted in atmospheres containing zero to 6.4 vol-pct methane mixed with zero to 300 mg/l coal dust. Coal dust in air alone was not ignited by abrasive impacts, but additions of as little as 1 vol-pct methane to the coal dust and air mixture resulted in ignitions. Steel impacting against sandstone caused ignitions in mixtures of coal dust, air, and methane, and the probability for ignitions increased with an increase in methane. No ignitions occurred with impacts of steel on lime-stone or pyrite-bearing limestone, even when large showers of sparks were produced. Studies of the effect of tangential collision velocity showed that no ignitions of coal dust, air, and methane occurred below 900 fpm (4.57 m/sec). Ignitions in coal-air-methane mixtures were found to be caused by a hot friction-induced smear on the impacted rock at the impact site rather than by sparks. High-speed photography was used to verify this observation.

Jan 1, 1976

By Roy L. Soderberg

Ground support for metal, nonmetal, and coal mines was examined through fill placement with a pneumatic stower to increase extraction, reduce ground pressures, and improve general mine safety. Several pneumatically stowed stope-fill products were tested to determine the effects of specific gravity, gradation, moisture, and impact velocity on the in-place density of the stowed fill. Hydraulic sand filling has now served the mining industry for several decades but because of the low density does not always provide ample support to the hanging wall; therefore, the sill and crown pillars sometimes build up excessive stresses that are detrimental to mining. Cementation of a dense fill adjacent to a pillar to allow 100-pct extraction of the pillar, or a fill that can be placed without the use of water and where water is a detriment to rubber-tired mining equipment, was found to be a possible use of pneumatic fill. Placing of coal mine washery products into abandoned underground workings is another possibility in order to completely eliminate surface impoundments.

Jan 1, 1976

By H. C. Ko

Calorimetric determinations of low-temperature heat capacities and the standard enthalpy of formation were made by the Bureau of Mines for aluminum sulfide, A12S3. The standard entropy (S°), enthalpy of formation (?Hf°), and calculated Gibbs energy of formation (?Gf°) at 298.15 K are 27.93±0.05 call deg-mole, -155.6±0.9 kcal/mole, and -153.0±1.0 kcal/mole, respectively.

Jan 1, 1976

By H. E. Hilliard

A method was investigated for detecting and counting filamentous iron bacteria in open recirculating cooling systems. It is simple and fast and does not require trained microbiologists. Samples from 26 systems were examined. Cells were cultivated on commercially prepared ready-to-use media. Cultures grew well on this medium and were identified as filamentous iron bacteria by microscopic examination and by their ability to deposit iron using the prussian blue reaction.

Jan 1, 1976

By B. D. Nash

The Bureau of Mines continued its research into the recovery of fluorine by the phosphoric acid acidulation defluorination of phosphate rock concentrates. A small process development unit with a capacity of about 10 kilo-grams of charge per hour was operated, and concentrates from both Idaho and Florida were processed. Over 80 percent of the fluorine was evolved and recovered as a dilute fluosilicic acid solution. Phosphate extraction from the concentrates always exceeded 98 percent. The fluorine was converted to a synthetic fluorspar product (3CaFa?SiOa) suitable for use as a slag conditioner in electric furnace steelmaking operations.

Jan 1, 1977

By Martin Hertzberg

The early and reliable detection of the self-heating of combustible substances in mines is of considerable importance to the mining community. This Bureau of Mines report describes the results of a variety of studies of incipient combustion and its detection. Heated samples of coal, wood, and various polymers were used to evaluate the relative sensitivities of several types of detectors. The laboratory results indicate that submicrometer particulate detection is the most universal and sensitive method. Carbon monoxide detection was as sensitive as submicrometer particulate detection for pyrolyzing coal but was relatively insensitive to pyrolyzing wood or plastics. The conventional type of ionization smoke detector was the least sensitive for coal and of intermediate sensitivity for wood and plastics. Self-heating experiments with Pittsburgh seam coal piles of varying particle sizes gave ignition temperatures of 170° C for 4-to 7-µm dust, which increased monotonically with particle size. The measured heating rates were compared with data from an adiabatic calorimeter to obtain preexponential rate constants. The preexponential rate constants varied linearly with the surface area per unit mass of sample as would be expected for heterogeneous surface oxidation. The propagation behavior of ignition waves and the overall self-heating appears to depend critically on the magnitude of the convective flows induced, which counteract the depletion of oxygen in the void spaces of the pile. Classical theories of thermal ignition require substantial modification to be applied reliably to such cases.

Jan 1, 1977

By Arne Landsberg

The Bureau of Mines measured the vapor pressure of FeC12 , FeBr2, FeI2, Sb, Bi, Cd, Mg, Pb, FeC13 , and VCl2 using the Knudsen-and torsion-effusion methods, and on FeC13 -NaC1 mixtures, Au2Cl6, and MgNi2 using only the Knudsen method. Apparent vapor pressures calculated from the experimental data vary with orifice size and method of determination. Reaction with residual oxygen in the instruments was noted to have an effect on the iron halide data. Vapor pressure curves plotted as log P versus 1/T (where P is pressure and T is absolute temperature) for one substance using several orifice sizes tended to converge at a single point when extrapolated beyond the experimental region. All of the data, except those of VC12, agree with previously published results. The importance of comparing effusion measurements with those obtained by other methods and the variations encountered with various orifice sizes are discussed.

Jan 1, 1977

By R. K. Koch

The Bureau of Mines developed a zircon sand molding process for static casting of small titanium or zirconium shapes. Castings with unfinished weights up to 3.5 kg (7.7 lb) were produced in an inductoslag furnace and castings up to 7 kg (15.4 lb) were poured in a consumable electrode skull-casting furnace. Molds and cores were made by ram-molding, foundry-grade zircon sand (AFS gfn 93 to 95) bonded by grade D waterglass and tempered with water. Molds and cores were cured either at 250° C (482° F) or 900° C (1,652° F). Castings from the higher temperature molds broke cleanly from the sand while the lower temperature molds produced castings that had to be cleaned by sand-blasting. However, low-temperature cured molds and cores have a number of advantages as follows: (1) A faster, less energy-consuming curing cycle is used; (2) expended cores are water soluble which greatly facilitates core removal; and (3) enough of the binder in crushed expended molds is reactivated by temper water so that the molding mix can be reused five times without any fresh binder additions and up to twenty times without exceeding a total cumulative binder addition of 52 ml/kg dry sand. Crushed used molds that had been cured at 900° C had no detectable binding strength when mixed only with temper water. A large number of oxide and silicate mold washes were studied for improved casting integrity. The most effective wash found for zirconium or titanium casting was monoclinic zirconia (325 mesh).

Jan 1, 1977

By L. W. Higley

Particulates generated in electric furnace (EF) steelmaking constitute approximately 1 to 2 pct of the charge. This flue dust is a rich source of zinc (values are substantially higher than in ore), but although there are several processes for recovering the metal, none are considered economic in the United States. This report reviews extraction technology and presents results of Bureau of Mines reduction-volatilization tests on pelletized EF dusts which achieved high recoveries of zinc. The data are sufficiently encouraging to warrant consideration of EF dusts as raw material for primary zinc smelters.

Jan 1, 1977

By Stephen A. Hare, O&apos

The melting, casting, and welding of the Raney nickel alloy (42 pct Ni-58 pct A1), a methanation catalyst useful in coal gasification, were investigated. Melting was done in graphite crucibles by heating aluminum and adding nickel using a cryolite slag cover. Casting conditions were found to be optimum when the melt temperature ranged from 1,125° to 1,200° C and the mold temperature ranged from ambient to 250° C. Suitable mold materials were found to be quartz, heat-resistant glassware, olivine, and zircon. Welding of the alloy can be accomplished using tungsten inert gas process. Tensile strength of the alloy, in the as-cast condition, was found to be 2,000 1b/sq in with an impact strength of less than 1 ft-1b. The coefficient of thermal expansion was determined to be 18.4 x 10-6/° C after heat treatment.

Jan 1, 1977

By D. L. Paulson

The Bureau of Mines is investigating pyrometallurgica1 and" chemical methods to recover valuable constituents from metallurgical dusts and slags. Under this program a technique was developed to recover iron from molten copper smelting furnace slags by carbon injection. Slags from gas-fired reverberatory and electric copper smelting furnaces were treated in an 800-kva electric-arc furnace by injecting coke breeze into the bottom of the molten bath. Over 95 pct of the iron and over 90 pct of the copper contained in the smelting furnace slags were recovered, while up to 85 pct of the carbon injected into the system was utilized. It is anticipated that the metal product containing approximately 95 wt-pct iron and 2 wt-pct copper will be a satisfactory medium for recovering copper by cementation.

Jan 1, 1977

By P. W. Jeran, M. C. Irani, D. H. Lawhead

The Beckley mine is one of five new mines in a heretofore unmined portion of the Beckley coalbed. The remoteness of these new mines from prior mining and their greater overburden preclude applying methane emission experience obtained in the old mines. Four sections of the Beckley mine were monitored. The data gathered show that variations in methane emission cannot be explained by variations in coal production. Although overburdens varied by as much as 30 pct, no correlation with methane emissions could be determined. The rib emissions increase with increased length of rib from a section advancing into virgin coal and do not decline over a prolonged idle period (32 days) whereas some decline has been measured for a section not mining into virgin coal. The indication is that degasification prior to mining will reduce the hazard of methane emissions in this area of the Beckley coalbed.

Jan 1, 1977

By P. W. Jeran

The Beckley mine is one of five new mines in a heretofore unmined portion of the Beckley coalbed. The remoteness of these new mines from prior mining and their greater overburden preclude applying methane emission experience obtained in the old mines. Four sections of the Beckley mine were monitored. The data gathered show that variations in methane emission cannot be explained by variations in coal production. Although overburdens varied by as much as 30 pct, no correlation with methane emissions could be determined. The rib emissions increase with increased length of rib from a section advancing into virgin coal and do not decline over a prolonged idle period (32 days) whereas some decline has been measured for a section not mining into virgin coal. The indication is that degasification prior to mining will reduce the hazard of methane emissions in this area of the Beckley coalbed.

Jan 1, 1977

By J. B. Janus

This Bureau of Mines publication updates a series of reports on the quality of coal purchased under specifications for Government use. Listed are analytical data on the composition and quality of tipple and delivered samples of coal collected during the period July 1975 through September 1976.

Jan 1, 1977

By M. J. Sapko

The Bureau of Mines conducted laboratory-scale flammability experiments to investigate the possible use of water spray systems for inerting or quenching mine-gas ignitions, such as those encountered at the working face of a coal mine. The inerting results for premixed methane-air-water mixtures indicated that water droplets of less than 10 µm tend to be as effective as the vapor. Water requirements for inerting such mixtures were much smaller than those for quenching the sustained flame propagation by the application of water sprays. The minimum water mass concentration for quenching methane-air flames increased linearly with increasing droplet diameter (surface weighted mean) and decreased with increasing spray temperature, whereas the droplet surface area required per unit volume was essentially constant for a given gas mixture composition. Data extrapolations indicated that a quenching system may be feasible for the longwall mining application.

Jan 1, 1977

By Jack E. Fraley

Because of their noncombustibility, silicate and magnesium oxycements are desirable for sealing shale in underground coal mines. In this Bureau of Mines investigation, cement samples were cured and tested (nonstandard tests) for submersion to note resistance to dissolution (breaking into parts), which is an important property for a coating. Nonappreciable dissolution during 1 week of submersion was set for passing the test. Over half of the coatings passed the test.

Jan 1, 1977