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By A. T. Iannacchione

Roof-rock instability in advancing sections of underground coal mines is a major contributing factor to accidents resulting in fatalities and injuries. Such roof-rock conditions can also result in loss of production due to additional cleanup time and increased amounts of reject material. The Bureau of Mines is investigating fundamental geologic factors affecting coal mine roof-rock instability in order to develop techniques to predict zones of potential unstable roof-rock. Two distinct directional trends of unstable shale roof-rock in a mine working the Upper Kittanning Coalbed are delineated: one trend is associated with the sandstone-shale transition zone, the other with a fault system. The unstable shale roof-rock associated with the transition zone, a consequence of differential compaction, is comprised of slickensided roof-rock. Whereas, the unstable shale roof-rock associated with the fault system, a consequence of structural deformation of the strata, is comprised of fault planes. These faults, small in comparison to the sandstone-shale transition zone, are difficult to delineate with a standard drilling program. Trends of the transition zone associated with the sedimentary facies change are projected into unmined portions of the coalbed with the aid of exploration core data.

Jan 1, 1981

By Benjamin W. Haynes

Materials from phosphate rock mining and processing were analyzed for fluorine and uranium content as part of the Bureau of Mines program to more effectively recover resources from mining and mineral processing reject materials. The analysis of both feed and waste materials generated in the beneficiation and acidulation of phosphate rock was performed to obtain information on the disposition and concentration of these elements in phosphate rock processing streams. Fluorine was determined by a distillation-titration method and by ion chromatography. Uranium was determined by the dibenzoylmethane (DBM) method, the reliability being confirmed by roundrobin analysis of samples within Bureau of Mines research centers. National Bureau of Standards (NBS) Standard Reference Material (SRM) 120b-Phosphate Rock was also analyzed for fluorine and uranium to verify procedures and results. Fluorine values ranged from 0.3 wt-pct in gypsum filter cake to 3.7 wt-pct in phosphate rock concentrate. Uranium ranged from less than 5 µg/g in gypsum filter cake to 200 µg/g in a dried clay slime.

Jan 1, 1981

By Earl L. Phillips

The Bureau of Mines conducted laboratory tests on samples of pozzolaniccement concrete to develop a low- strength backfill . Results show that support costs can be lowered by replacing a portion of the portland cement in mine backfill with pozzolan ( fly ash ) and lime . Unconfined compression tests on various ratios of fly ash to cement in 84 samples produced compressivestrength curves that can be used to estimate the best backfill mix for any mine .

Jan 1, 1964

By Seth C. Schaefer

The Bureau of Mines has determined the standard Gibbs energies (AGf°) of CoS1.035 (cobalt sulfide) and Ni2.515S2 (nickel sulfide) with high-temperature galvanic cells using stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, CoS1.035, CoO, S02(g, 1 atm)//Zr02//02(g, 0.0114 atm), Pt, with the overall cell reaction C0S1.035(c) + 1.535 02(g, 0.0114 atm) = CoO(c) + 1.035 S02(g)¬ These results, combined with the best available data for ?Gf° of CoO and S02 from the literature, give the standard Gibbs energy of formation of CoS1.035 for the reaction Co(c) + 0 5175 S2(g) = CoS1.035(c) ?Gf° = -38.890 + 18.87 x 10-3T ± 0.185 kcal/mole (866.0 - 1,104.9 K), where temperature (T) is expressed in kelvins. Similar measurements were obtained for the cell Pt, N12.515S2, NiO, S02(g, 1 atm)//Zr02//02(g, 0.0122 atm), Pt, with the overall cell reaction Ni2.515S2(c) + 3.2575 02(g, 0.0122 atm) = 2.515 NiO(c) + 2 S02(g). Combination of these results with data for ?Gfo of NiO and S02 from the literature yields the standard Gibbs energy of formation of Ni2.515S2 for the reaction 2.515 Ni(c) + S2(g) = Ni2.S1SS2(c) ?Gf° -65.377 + 24.67 x 10-3T ± 0.541 kcal/mole (968.6 -1,053.7 K).

Jan 1, 1981

By J. H. Maysilles

The Bureau of Mines is conducting research on various technologies to recover alumina from domestic resources for feedstock to existing aluminum smelting capacity as a means to reduce dependence on imported bauxite, which represents 93 pct of U.S. aluminum requirements. One of the more promising technologies being investigated is the hydrochloric acid leaching of kaolinitic clay. In the hydrochloric acid leaching technology, alumina is recovered from iron-free aluminum chloride leach liquor and separated from impurity elements by sparging the liquor with HC1 gas to crystallize aluminum chloride hexahydrate (ACH). A large-scale crystallizer with a 336-gallon usable volume was constructed and operated to obtain engineering and design data for potential scale up and to demonstrate the ability of the technology to produce specification grade alumina. Test campaigns involving about 1,400 hours of operation were completed. ACH meeting all chemical purity requirements could not be produced by a single crystallization, but was produced by recrystallizing the product from the calcined kaolin clay leach liquor. Product crystals with a size distribution of more than 80 pct plus 100 mesh and 65 pct plus 65 mesh were made at a rate of 10 pounds of ACH/(hr)(ft3). The zirconium tube heat exchanger used to maintain constant process temperature operated with an over-all heat transfer coefficient of 420 to 500 BTU/(hr)(ft2)(°F).

Jan 1, 1981

By J. A. Eisele, D. J. Bauer, D. E. Shanks

As part of its effort to produce cell - grade alumina from clay , the Bureau of Mines investigated the hydrogen chloride gas - sparging crystallization of aluminum chloride hexahydrate ( ACH ) from aluminum chloride liquor , to provide information for optimizing the crystallization operation . Four parameters important in controlling the crystallization of the aluminum chloride hexahydrate and the concentration of impurities , particularly phosphorus and magnesium , in ACH crystals are ( 1 ) aluminum chloride concentration in the feed solution to crystallization , ( 2 ) hydrogen chloride gas flow rate , ( 3 ) temperature , and ( 4 ) concentration of phosphorus and magnesium also in the feed solution . Parameters 1 , 2 , and 3 affect crystal formation . The combined effects are very important because the phosphorus and magnesium concentrate in the crystals during the early stages of crystal growth . Aluminum chloride hexahydrate of cell -grade purity was crystallized from saturated aluminum chloride solutions containing less than 0.003 wt - pct P205 and 0.010 wt - pct Mg0 . Crystallization temperatures less than 60° C decreased crystal purity .

Jan 1, 1965

By Syd S. Peng

The design of retort interchamber pillars is important in determining surface stability over in situ retort mines and to the health and safety of miners, particularly with respect to possible escape of heat and toxic gases from retort chambers. Stress distribution in retort interchamber pillars, roof, and floor was examined with the aid of linear, finite-element analysis using data from experimentally determined mechanical properties. Properties determined included elastic moduli, strength, and creep constants in laboratory tests on core covering a 100-foot depth interval in the oil shale from the Piceance Basin in Colorado. The most critical stress concentration was found in the rib side of the interchamber pillar at a height above the floor line of 1.25 times the width. Guidelines for pillar design that consider pillar strength, creep, and retorting temperature effects are proposed.

Jan 1, 1981

By William D. Riley

In order to evaluate the corrosion resistance of zirconium in mineral extraction processes, such as a clay-hydrochloric acid leaching process for extracting alumina, the Bureau of Mines conducted corrosion studies in HCl-AlC13-FeC13 environments. A series of weight loss and electrochemical tests were conducted at 25° and 65° C in aluminum chloride (AlC13) plus hydrochloric acid (HCl) solutions containing 0 to 1,000 ppm ferric ion. It was determined that zirconium, which normally exists in a passive state in chloride-containing solutions, undergoes pitting attack in solutions containing more than 100 ppm of ferric ion. It is also shown that an oxide film prepared in air at high temperature offers protection in acid solutions containing levels of ferric ion from 300 to 1,000 ppm.

Jan 1, 1981

By K. O. Bennington

The thermodynamic properties of synthetic acmite, NaFe3+Si206, were determined by the Bureau of Mines. The enthalpy of formation was determined by hydrofluoric acid solution calorimetry. The values of the standard enthalpy of formation at 298.15 K, ?Hf°298.15, from the elements and from the oxides, ?H°298.15, are ?Hf°298.15 = -615.87 ±0.71 kcal/mole, ?H°298.15 (from oxides) = -32.08 ±0.53 kcal/mole. Various experimental data were combined with other data from the literature to calculate all the related thermodynamic properties in the range of 298 to 1,263 K. The standard Gibbs energy of formation is ?Gf°298.15 = -575.8 kcal/mole.

Jan 1, 1981

By Bill M. Stewart

The Bureau of Mines conducted laboratory tests to determine the effects on the physical properties of coarse coal waste of adding large amounts of fine coal waste. Maximum laboratory dry density, optimum moisture content, shear strength, and permeability tests were conducted on samples that contained 18 to 60 pct minus No.4 (U.S. Standard sieve size) coal waste. For the nonslaky materials, maximum laboratory densities were highest and permeabilities lowest when the samples contained between 30 and 40 pct minus No.4. Shear strength increased rapidly when the proportion of minus No. 4 was increased from 20 to 40 pct, but then increased only slightly or leveled off when the minus No. 4 was increased to 60 pct. Optimum moisture content and permeability were the physical properties most affected by the addition of fines. Optimum moisture content increased as much as 3 pct, and permeabilities decreased up to three orders of magnitude. Slaky coal waste material had physical property reactions to the addition of fines substantially different from those of nonslaky material.

Jan 1, 1981

By E. D. Calvert

As part of its goal to minimize the requirements for critical and strategic minerals, the Bureau of Mines is conducting research to foster the use of domestically abundant materials such as molybdenum. This report describes the development of an investment shell molding technique that can be used to make castings of molybdenum and its alloys. The mold material is cubic Zr02 with a monoclinic Zr02 binder. The shell, formed by standard investment molding techniques described in the text, is prepared for molybdenum casting by firing for 6 hours at 1,550° C (2,822° F) or for 4 hours at 1,650° C (3,002° F). The resulting castings have predictable and reproducible dimensions with good detail. As-cast strength is poorer than the strength of wrought materials below 1,600° F. At and above this temperature, tensile strengths of cast and wrought materials are nearly equal. Aqueous corrosion of the castings in most media is insignificant.

Jan 1, 1982

By J. M. Kuchta

The Bureau of Mines investigated four simulated coal gob fires to obtain a more reliable data base for defining the state of a sealed mine fire and to evaluate the performance of various fire detectors. The fires were conducted in a multiple-entry section of the Bruceton Experimental Mine by heating 4,000 to 21,000 pounds of rubblized bituminous coal to ignition and monitoring the temperature, gas emissions, and smoke under ventilated and sealed combustion conditions. Product gas concentrations depended upon the coal bed size, coal temperature, heating rate, and oxygen concentration or ventilating condition but varied little after the fires were sealed. Expressions are given that define the temporal variation of CO and O2 after sealing when the coal temperature decreased rapidly. The CO/C02 ratio is a more sensitive fire indicator than the CO/?02 ratio, although the latter is universally used for detecting the incipient state of a coal fire. In comparison, the Jones-Trlckett ratio [ CO2 + ¾ CO ? ¼ H2 ?O2] is less reliable for this purpose. The best detector for determining the state of a mine fire after it has been sealed was a prototype submicrometer smoke particulate sensor. Limitations of the various detector systems are also discussed.

Jan 1, 1982

By R. H. Lien

The Bureau of Mines developed a flue gas desulfurization process as part of its goal of minimizing the undesirable environmental impacts associated with energy and mineral-processing plants. The modified citrate process involves absorption of sulfur dioxide (S02) in a buffered citric acid solution. The S02-loaded solution is regenerated by countercurrent contact with steam in a packed tower. The wet S02 product is then dried and can be liquefied or further processed to make sulfuric acid. Test data from process investigation unit studies are presented. Material balances, flowsheets, and cost estimates are given for recovering S02 from copper smelter reverberatory gas, lead smelter sintering machine tail gas, and power-plant stack gas. Operating cost estimates show the process will add $0.04 per pound of copper, $0.01 per pound of lead, and $0.015 per kwhr to the cost of the respective operations. These costs could be substantially reduced if a source of waste heat was avail-able to provide the process steam requirements.

Jan 1, 1982

By C. Melvin Lepper

Microseismic energy is generated when stresses accumulated in rock formations are released in the form of fracturing. The acoustic emissions resulting from these rock fractures and movements are detectable as velocity signals in the earth near the energy source. A Bureau of Mines microseismic system that is capable of detecting the acoustic emissions from pit slope movements is described. The digital circuitry incorporated in the system allows a microprocessor program to immediately calculate and present the location coordinates for the seismic energy source in the mine pit wall. This monitoring system is compact, portable, reliable, and relatively inexpensive and rapidly provides accurate information to the mine operators about the stability of a pit slope.

Jan 1, 1982

By Ernest W. Loya

A method for preparing gravimetric primary standards of helium in the parts per trillion range has been developed by the Bureau of Mines. The standards are used to calibrate a specially modified mass spectrometer used in determining the abundance of helium-3 and helium-4 in geochemical samples and of helium-3 in isotopically purified helium-4. The desired gas standards are prepared in 5-kg metal cylinders filled to 1,800 psia. Relative errors of less than 1 pct have been attained in the parts per trillion range using a successive dilution technique.

Jan 1, 1982

By W. L. Falke

The Bureau of Mines has developed a system that permits the "soft" soldering of aluminum and aluminum alloys with standard tin-lead solders. The method employs application of a thin nickel-copper-alloy coating to the substrate, which enables the tin-lead solders to wet readily and spread over the areas to be joined. With conventional technology, aluminum and aluminum alloys are extremely difficult to solder because tenacious surface oxide films prevent wetting. With the Bureau-developed method, the aluminum substrate is mechanically or chemically cleaned to facilitate bonding to a minute layer of zinc that is subsequently applied with an electroless zincate solution. The nickel-copper-alloy (30 to 70 pct Ni) coating is then applied electrolytically over the zinc, using immersion cell or brush-coating techniques. Development of acetate electrolytes has permitted deposition of the proper alloy coatings. The coated areas can then be readily joined with conventional tin-lead solders and fluxes. The joints so formed are ductile, strong, and relatively corrosion resistant, and exhibit strengths equivalent to those formed on copper and brass when the same solders and fluxes are used. The method has also been employed to soft-solder magnesium alloys.

Jan 1, 1983

By H. C. Ko

Heats of solution of calcium carbon-ate (calcite) and calcium oxide in hydrochloric acid were determined by solution calorimetry. Combination of these two heats yields a value of 42.643±0.024 kcal/mole for the enthalpy of calcination of calcite at 298.15 K. Literature data on ?H°298.15 of calcination of calcite were reviewed and compared. Thermodynamic properties for the calcination process were calculated from 298.15 to 1,500 K using Gibbs energy functions. This research was undertaken by the Bureau of Mines as an effort to provide thermodynamic data for the advancement of minerals technology, energy conservation, and environmental preservation.

Jan 1, 1982

By J. S. Dunning

The Bureau of Mines investigated a series of Fe-Al-Mo alloys strengthened by ZrC (zirconium carbide) precipitates as chromium-free substitutes for stainless steels. Melting and fabrication methods were devised, and the effects of minor additions of columbium (niobium) and cerium on the mechanical properties and oxidation resistance were determined. Zirconium carbides could not be con-trolled reliably to produce fine precipitate dispersions. A more reliable carbide strengthening mechanism is required if the high-temperature strengths of types 304 and 316 stainless steels are to be duplicated. Workability and oxidation resistance of the alloy series were excellent.

Jan 1, 1982

By E. A. Johnson

The Bureau of Mines determined the effect of slag additives on copper solubility and the distribution of typical impurity elements between copper-iron matte and silica-saturated fayalite (iron silicate) slag at 1,250° C, in CO-C02 atmospheres with 10 pct S02. Small additions (<10 pct) of CaO, A1203, and MgO were shown to decrease copper solubility in the slag. Additions of CaO increased the solubility of bismuth and tellurium in the slag at lower matte grades. Al 20 3 additions decreased the solubility of tellurium in the slag, but increased that of bismuth at lower matte grades. A1203 additions increased the solubility of both at lower matte grades. With no additives, matte grade did not affect the solubility of bismuth in slags, whereas increasing matte grade resulted in a slight decrease in the tellurium solubility in slag. Additions of CaO or As203 alone to the slag increased selenium and arsenic distribution to the matte, but had little or no effect on antimony distribution; whereas small MgO additions decreased antimony distribution to the matte but had no effect on arsenic and selenium distribution. In slags with no additives, selenium distribution to the matte increased with increasing matte grade, while that of antimony decreased and that of arsenic was unchanged.

Jan 1, 1982

By Jerry W. Stengel

The Bureau of Mines subjected two manufacturers&apos; chemical oxygen (K02) self-rescue breathing apparatus to a series of laboratory environmental treatments designed to simulate various conditions in underground coal mines. The environmental treatments consisted of extremes of temperature, shock, and vibration. The tests were designed to be used as predictors of the ability of the self-rescuers to survive those environmental insults with no degradation in their protection to the wearer. Based on the severity of the treatments, simulating conditions more severe than offered by the mining environment, the two apparatus tested should be able to withstand the abuse offered by the mining environment and still function as intended in an emergency. Correlation of these tests with results of long-term field evaluations is needed to provide confidence in the laboratory tests as predictors.

Jan 1, 1982