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By D. S. Burgess

The characteristics of gas-phase detonations were observed in 20 instrumented firings within earthen tunnels, in 100 such detonations in a 24-in-diam by l63-ft-long steel pipe, and in about 200 smaller scale firings. Most of the fuels studied were representative hydrocarbons--acetylene, propane, gasoline, and a roughly equimolar mixture of methylacetylene, propadiene, and propane. In a pipe with two closed ends, the detonable limits were demonstrated to be very nearly the same as reported limits of flammability. The side-on impulses (pressures integrated over 200-msec intervals) were shown to be the same function of concentration regardless of whether deflagration or detonation had occurred. In a pipe with only the initiation end closed, the impulses of all fuel-air systems tended toward the same level when averaged over comparable ranges of fuel concentration; the lower pressures with saturated hydrocarbons were nearly compensated by longer durations of pressure transient. In all fuel-air systems, unexpectedly high impulses were obtained with slightly lean mixtures. In earthen confining structures, the impulse, of the explosion was efficiently converted into momentum of the failing wall. In the configurations studied, an earth velocity of about 20 fps was critical to overcome the soil's resistance to shear. The destructive effect was determined by gas pressure rather than by total energy release. The assignment of a "TNT equivalent" to an explosive gas mixture is discussed in terms of the confinement of the mixture.

Jan 1, 1968

By Frank G. Schwartz

The Bureau of Mines developed a rapid test method for predicting the stability of motor gasoline during long-term storage. The amounts of gum and inorganic residue formed in 13 gasolines during a l6-hour oven test at 200° F were compared with the amounts formed in the same gasolines stored at 110° F, and analyzed following 8-, 16-, 32-, 44-, and 52-week storage periods. Satisfactory methods were developed for predicting gum and inorganic residue formation during fuel storage periods as long as 32 weeks at 110° F, the approximate equivalent of 5.7 years at 80° F. The only data required to apply the methods are the amount of gum and inorganic residue formed, and the amount of oxygen that reacted, during a l6-hour oven test. A direct relationship existed between inorganic residue formed during the oven test and during 110° F storage. Statistical treatment of the data showed predicted values were as reliable as determined values. By use of a modified Arrhenius equation, the 110° F storage time can be extrapolated to equivalent time at any temperature below 110° F. Thus by combining the stability prediction method with the mathematical extrapolation, the storage performance of motor gasoline for extended periods can be estimated at any temperature up to 110° F.

Jan 1, 1968

By David E. Nicholson

The Bureau of Mines has constructed a special compression chamber for developing stress-strain relationships of mine backfill and simulating the high compressive ground pressures encountered in underground mines. A one-dimensional, or Earth-Pressure-at-Rest model is proposed for backfills subjected to these pressures. Results of the compression tests performed in the chamber indicate that reliable stress-strain relationships can be developed from these tests. The primary objective of the test series was to evaluate the effectiveness of compaction of common backfills in retarding ground closure. Analysis of the stress-strain data shows an eightfold reduction in relative strain in optimum well-graded, compacted backfills over poorly graded, loose backfill material. Analysis of the one-dimensional compression test data also indicates a significant retardation of transmitted stress in dense compacted samples of backfill and natural sands. Although not fully understood, a deformation mechanism is thought to occur at the intergranular contacts in cyclic fashion causing frictional heat loss and a reduction in transmitted stresses in the densely packed materials. The experimental values of transmitted stress are compared with theoretical values of effective stress calculated from the one-dimensional compression relationships developed by Hendron (4).3 These experimental values of transmitted stress compare very closely with the theoretical values of effective stress.

Jan 1, 1968

By H. V. Makar

Laboratory tests were performed to obtain a quantitative description of the effectiveness of sodium sulfate (Na2SO4) for removing copper from molten iron and to determine the effectiveness of Na2SO4 on actual auto scrap. The tests were conducted on induction melted heats of iron averaging 0.58 and 1.50 percent initial copper and on cupola-melted auto scrap containing 0.45 percent initial copper. The Na2SO4 was added in powder form in amounts ranging from 2.9 to 43.8 percent of the weight of iron being treated. The data showed that copper removal for the various Na2SO4 treatments followed a similar trend, regardless of the iron composition that was tested. The equation Y = 1 - e-3.23x approximately reflects the relationship between copper removal and amount of Na2SO4 added, where Y is the fraction of copper removed and x is the ratio of the weight of Na2SO4 added to the weight of metal treated. Copper removals ranged from 3.3 to 74.5 percent and reductions down to less than 0.10 percent final copper were achieved in the auto scrap. Copper removals were generally accompanied by sulfur removal, and initial sulfur contents ranging from 0.10 to 0.20 percent were reduced to as low as 0.02 percent. High temperatures and long slag reaction times tended to induce copper and sulfur reversion from the slag, but, generally, the Na2SO4 treat¬ments were effective up to approximately 2,820° F with reaction times not exceeding 7 minutes.

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 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