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By L. B. Pankratz

Heat contents were measured for Na2CaSi04 and Na2Ca2S02 between 298° and 1,300° K, for Na2Ca2Si309 between 298° and 1,500° K, and for Na4CaSi3O9 between 298° and 1,350° K. Copper-block drop calorimetry was employed. Reversible, first-order transitions were found for Na2CaSi04 and Na2Ca2Si309. The transition for Na2CaSi04 is at 830° K with a heat absorption of 160 cal/mole; that for Na2CagSi309 occurs at 750° K with a heat absorption of 1,550 cal/mole. Results for the other two silicates showed no irregularities. A table of heat content and entropy increments above 298.15° K and heat con-tent equations are included for use in thermodynamic calculations.

Jan 1, 1968

By R. H. Oitto

To determine whether reflectors could substitute for the trip lights referred to in the Federal Mine Safety Code, the Bureau of Mines studied trip safety devices under simulated haulageway conditions. The noticeability of reflectors compared with trip lights and fluorescent panels was evaluated from distances of up to 850 feet with light source intensities of up to 1-6 foot-candles (ft c). Reflectors tested consisted of a reflective lens in a holder secured to a frame that can be attached to a trip. Reflectors were found to be suitable for use as a trip safety device. In fact, for the conditions in many underground haulageways some reflectors would be more effective than a permissible trip light.

Jan 1, 1968

By Philip G. Freeman

The growth-promoting properties of coal-derived humus were tested by a variety of bioassay methods. Humate materials used included leonardite, a form of naturally oxidized lignite, and humic acids extracted from leonardite. It was found that the greatest effects were evident when water-soluble humic acid was applied to excised root tips. No significant short-term effect was noted when water-soluble humic acid was applied to stem or coleoptile sections. Root initiation was promoted in bean stems when high concentrations of coal-derived humate were applied. Gross weight of tomato plants was increased by up to 40 percent when coal-derived humates were added in concentrations of 101 to 104 ppm to the nutrient in a hydroponic growth test of 6 weeks' duration. It is concluded that coal-derived humate promotes the uptake of minerals, specifically iron, by serving as a metal chelate.

Jan 1, 1968

By C. B. Kenahan

The Bureau of Mines is developing methods for reclaiming the metal and mineral values contained in municipal incinerator residues. This report describes the first phase of the research, in which reliable methods for sampling and analyzing municipal residues were established and the composition and characteristics of the residues were determined. Samples were obtained from a variety of grate-type furnaces and also from a rotary kiln furnace. The samples were processed on a batch basis and separated into their natural categories by a variety of methods including screening, magnetic separation, air separation techniques, and handpicking. The main components of the residues were determined to be metal and metal oxides, glass, and ash.

Jan 1, 1968

By J. W. Town

The Bureau of Mines determined the physical properties of southeastern Idaho phosphate fines as related to mineral composition, particle size and liberation, beneficiation, and potential use in structural clay products. The phosphate mineral in the fines was identified by unit-cell dimensions to be essentially the same as the phosphate mineral fluorapatite identified in the coarser sizes. The mean particle frequency as determined by electron-microscopy and pipet-analyses was between 0.5 and 0.2 micron. Liberation of the phosphate could not be definitely determined because of the weathered condition of the minerals and their extreme fineness. No beneficiation scheme was developed that would concentrate the phosphate into a marketable fertilizer product; therefore, forming and firing tests were made to demonstrate that the fines can be used to manufacture structural clay products.

Jan 1, 1968

By James H. Aase

Selected glacial lake clay deposits in Minnesota were sampled, tested, and evaluated to determine their suitability for use as a bonding agent in iron ore pellet manufacturing. Preliminary tests conducted on clay samples obtained from five ancient glacial lake basins identified the clays in the Lake Agassiz glacial lake basin near Cook, Minn., as having the greatest bonding potential. An auger drilling program was conducted to obtain substantial quantities of representative material for detailed testing. The drilling indicated the presence of large clay reserves in excess of 500 million tons within the 12-square-mile area investigated. Bench scale tests indicated that the bonding properties of Cook area clays, when activated with relatively small quantities of sodium carbonate monohydrate (Na2C03?H2O), imparted excellent strength characteristics to iron ore pellets. Larger scale continuous pelletizing tests were made to confirm the bench scale results. These tests indicated that use of 1 percent activated clay alone as binder gave the iron ore pellets an overall strength slightly lower than with 0.75 percent bentonite, considered the industry standard. Use of 0.5 percent activated clay plus 0.5 percent bentonite produced better pellet strength qualities than use of 0.75 percent bentonite alone, without increasing the silica plus alumina content. The data from both bench scale and larger scale continuous tests suggest that the Cook, Minn., clays can be utilized after activation either alone or in combination with bentonite at an economic advantage over present pelletizing practice with bentonite.

Jan 1, 1968

By L. A. Haas

The degree of reduction of various silica-graphite mixtures was studied in a batch reactor to determine optimum physical conditions for maximizing the carbothermic reduction of silica. The extent of interaction was determined for reactant mixtures in loose powder and briquet forms at pressures less than 0.01 torr and temperatures up to 1,445° C. Molar ratios were varied from 0.05 to 6.5 with maximum reaction at a ratio of about 1.5. The solid-solid reaction did not appear to involve gaseous intermediates. The extent of reaction better correlated with the number of interparticle contacts than with the true surface area of the reactants. Carbonized dextrose was a better reductant than graphite.

Jan 1, 1968

By John Nagy

Dust explosion data obtained in laboratory tests by the Bureau of Mines are presented for 181 miscellaneous materials that present an explosion hazard. Data are given also for 50 dusts that present primarily a fire hazard and for 88 dusts that did not present an explosion hazard.

Jan 1, 1968

By Sam Friedman

The Bureau of Mines conducted experiments using bench-scale apparatus to explore the effect of large changes in process variables on the yield and composition of the gases produced by passing 800° C steam through a fixed bed of Pittsburgh seam (hvab) coal. The total yield of combustible gases increased throughout the given range for the following variables: Superficial steam velocity increasing from 0.02 to 0.12 fps, pressure increasing from 1,000 to 6,000 psig, residence time increasing from 0 to 60 minutes, and temperature increasing from 800° to 900° C; however, a greater increase in the yield of hydrogen in comparison with the increase in yield of methane reduced the gross heating value of the gas to around 470 Btu per scf at conditions giving the maximum yield. Pressures of 1,000, 3,000, and 6,000 psig at 0.09 fps steam velocity, 800° C, and 60 minutes residence time, respectively, produced methane yields of 20, 24, and 22 percent, based on maf coal, with the gross heating value of the CO2-free gas decreasing from 552 to 520 and to 470 Btu per scf. Methane concentrations in the CO2-free gas were 26, 22, and 14 percent, respectively. Based on the gross heating value of the coal, the percentage of the heating value recovered in the gas was 60, 71, and 87 percent, respectively. The use of tungsten sulfide as a catalyst for converting carbon oxides and hydrogen into methane was explored briefly using both a sulfur-free gas rich in methane and a sulfur-bearing synthesis gas (3H2:1CO).

Jan 1, 1968

By Gerald W. Elger

To determine the feasibility of removing nonferrous metal impurities from automobile scrap by thermal treatment in a rotary kiln, the Bureau of Mines conducted four series of tests with synthetic scrap mixtures heated at various temperatures under oxidizing and reducing conditions. The treated scrap mixtures were melted in an electric-arc furnace and cast into small ingots for impurity evaluation. Analyses showed that the ingots were essentially free of residual metal impurities except for copper. Test data indicated that in an oxidizing atmosphere the percentage of copper removed increased with treatment temperature. Percent of copper removed in a reducing atmosphere was found not to be temperature dependent. A significant finding was that copper was embrittled under some of the operating conditions and was mechanically removed by fragmentation.

Jan 1, 1968

By Herbert R. Babitzke

As part of a project to develop refractory metal alloys suitable for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation-hardening techniques to columbium and tantalum alloys. Thirty-three alloys were evaluated to determine their formability, strength, and oxidation resistance. Three alloys had tensile strengths near 40,000 psi at 1,200° C: Cb-1N-5W-5V-10Hf (No.4), Cb-15Hf-5W-0.5B (No. 31), and Cb-15Hf-SW-IB (No. 32). Oxidation resistance of the high-strength alloys was good. Alloy4 gained only 34 mg/cm2 at 1,200° C, and 21 mg/cm2 at 1,000° C in 2 hours. Hot forming was done without any protection from oxidation.

Jan 1, 1968

By E. L. Singleton

The electrochemical reduction of aluminum chloride to aluminum was investigated in a closed, two-compartment cell utilizing a molten chloride electrolyte. The externally heated cell was divided into a reduction compartment and a combination AICl3 feed and metal removal compartment. Aluminum was deposited at 700° C on a molten aluminum catbode from a KCI-NaCI-AICI3 electrolyte. The AICl3 content of the electrolyte was replenished by either vapor or solid additions. The chlorine evolved was collected and measured to give a quantitative evaluation of AICl3 reduction. The effects of anode and cathode current densities and AIC13 concentration on anode current efficiencies were studiedo A range of 64 to 84 percent anode current efficiency was obtained with the 25-pound electrolyte capacity cell and related auxiliary equipment.

Jan 1, 1968

By Philip C. Good

Preliminary studies showed that direct hydrolysis of H2SiF6 to SiO2 and HF at elevated temperatures was subject to many mechanical difficulties, and that corrosion of construction materials was a serious problem. Elimination of SiO2 from the HF product was generally poor. An alternative procedure, hydrolysis of lime-neutralized H2SiF6 by steam at 950° to 1,100° C, yielded a product very low in SiO2. Condensates containing up to 300 g/1 HF were prepared.

Jan 1, 1968

By Edwin M. Murphy

Methods are described for filling underground cavities remotely with dry material pneumatically injected through a borehole to seal openings, prevent air movement, and reduce subsidence; this often brings underground fires under control by limiting the access of air. Large-scale tests were made in the Bureau of Mines Experimental Coal Mine, Bruceton, Pa., in an operating mine, and in an abandoned Pennsylvania mine. Supplemental trials were made aboveground in galleries and in the laboratory. The parameters studied include horizontal and inclined passageways, obstructions in the entry, water leakage into the borehole, dry material, and grout and slurry mixes. The materials studied were fly ash, crushed and pulverized limestone, and sand. Best results were obtained with dry fly ash, though satisfactory seals were obtained with the other materials. When a borehole is dry and ends at an open void, casing is not necessary. If more than 5 gpm of water flows in the borehole, if the void contains loose debris, or if coarse material is injected, a material feedpipe should be inserted through the borehole. Fly ash was most suitable for remote filling because of its low angle of repose (8°) and its good flow characteristics. The depth of borehole through which the fly ash is injected has no appreciable effect on the filling operation.

Jan 1, 1968

By M. E. Tyrrell

Research objectives were to determine the reasons for erratic behavior of semisilica horizontal zinc retorts in service; to investigate potential corrective measures including the possible utilization of more refractory materials in the retort body; and to delineate laboratory tests suitable for process control in the manufacture of retorts. Correlation of laboratory test results and data supplied by the cooperating smelters indicated that structural failures due to thermal shock and laminations in the retort body are largely responsible for the erratic behavior of horizontal zinc retorts in service. The most promising modifications made in the retort body and evaluated on a laboratory scale included finer grinding of the plastic clay fraction, substitution of mullite grog for calcined fire clay and grain alumina for silica, plus the use of an organic binder. Lamination-free extrusions having excellent thermal shock resistance were prepared from a mixture composed of 50 percent low-silica Missouri plastic clay through 100 mesh, 25 percent mullite grog through 6 mesh, and 25 percent alumina through 100 mesh. The mix was pugged under 28-inch vacuum with 1 percent ligno sulfonate binder in 12 percent tempering water. Laboratory tests suitable for process control in the manufacture of retorts are described.

Jan 1, 1969

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of Clay, Gilmer, and Lewis Counties, W. Va. In 1966, almost 1.3 million tons of coal was mined in these counties, of which more than one-half was from the Pittsburgh coalbed. Washability analyses were made of 16 coalbed samples. Of these, only 11 samples could be upgraded to metallurgical quality. For steam or power generation five of the coals were of low sulfur content as received. The remaining samples were generally of medium sulfur content even after upgrading.

Jan 1, 1969

By Alla D. Mah

The heats of combustion of three chromium carbides, Cr23C6, Cr7C3, and Cr3C2, were determined by combustion calorimetry. Heats of formation calculated from the results follow: ?Hf°298 (Cr23C6) = -94.7 ± 5.0 kcal/mole, ?Hf°298 (Cr7C3) = -43.3 ± 1.7 kcal/mole, and ?Hf°298 (Cr3C2) = -22.5 ± 0.8 kcal/mole.

Jan 1, 1969

By R. R. Brown

The Bureau of Mines undertook a limited feasibility study to determine the practicality of removing copper from automobile scrap by thermal treatment. Test specimens, prepared by wrapping bare and insulated copper wire around small steel coupons, were heated at 600° to 1,150° C in various atmospheres for different lengths of time under both static and dynamic conditions. The tests indicated that adequate removal of copper cannot be effected by thermal treatment of scrap above the melting point of copper. Tests showed that copper present in scrap as insulated wire is embrittled by thermal treatment at 800° to 900° C if the insulation contains lead, and that the embrittled copper is almost completely removed by a mechanical action such as tumbling. Also chemical pretreatment of specimens to effect embrittlement of copper and the magnetic separation of oxide scale were studied. Tests showed that bare copper can be embrittled by depositing waterglass (Na, Si409) on copper prior to thermal treatment.

Jan 1, 1968

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instruction3 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1969

By Edward W. Parsons

To determine in what part and to what extent creep or movement exists in an installed rock-bolt anchor and the effect of the creep or bleedoff on the tension load on a rock bolt, as well as the effect of normal mining activity on the rock-bolt load and anchor, the Bureau of Mines conducted tests in the laboratory and in two mines using four types of expansion-shell anchors, the wedge bolt, and in one mine, explosive-anchored rock bolts. Specially mounted heavy-duty springs, calibrated to obtain load readings from spring movement, were installed on the test bolts to prevent a drastic reduction in tension load caused by slipping or seating of the anchor. A dial gage, reading to 0.0001 inch, measured movement of the anchor shell against the rock and seating of the anchor wedge plug in the shell. While all bolts had electrical resistance strain gages for load reading, only readings from the laboratory tests were used because those from the field tests were erratic. The tests revealed that most load loss resulting from static loading is due to the slippage and seating of the serrations on the anchor shell into the drill-hole wall. Dynamic loading, primarily from sudden shocks from nearby blasting, and possibly from ground movement or mining activity, will cause the anchor wedge plug to seat in the anchor shell.

Jan 1, 1969