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By George A. Savanick

The objective of this research is to develop a method for measuring the tensile strength at the interface between minerals in rock. These measurements reflect the strength of the attractive forces operating at crystalline interfaces in rock. Since these forces act in opposition to the forces set up in various rock fragmentation processes, measuring their strength may help in designing more efficient methods of rock fragmentation. The method developed for measuring the strength of intergranular adhesion in rock involves separating a bicrystal from the rock and determining the tensile strength at its solid-solid interface. This technique has been successfully applied to the study of quartz-feldspar interfaces separated from massive pegmatites, graphic granite, and the Rockville granite, yielding average tensile strengths of 5.86, 8.62, and 10.65 meganewtons per meter squared (MN/m2) (850, 1,250, and 1,524 psi, respectively). The data this technique provides indicate that the members of these bicrystals are strongly adherent. Examirtation of bicrystals broken at the crystalline interfaces indicates that the bonds responsible for this adhesion operate over only a portion of the interfacial area. This work conclusively demonstrates that tensile strength tests can be conducted on small selected areas; for example, grain boundaries in rock. The small-scale zones of strength or weakness determined in this way can be related to the overall strength of the rock.

Jan 1, 1972

By D. C. Fleck

Electrorefining yttrium from selected low-melting yttrium--base alloys is investigated, and various halide systems are studied as potential electrolytes for use in preparing low-oxygen yttrium by electrorefining unalloyed yttrium. Yttrium cathode products having significantly less metallic impurities than the anode materials were prepared from alloys containing nickel, iron, and manganese by electrorefining in LiCl-YC13 electrolytes at 900° to 1,000° C. Yttrium-copper and yttrium-magnesium alloys are not suitable as anode feed materials, An evaluation of chloride, fluoride, bromide, and mixed chloride-fluoride electrolytes showed that cathode products containing much less oxygen than the anode material can be obtained in the fluoride and mixed chloride-fluoride systems. Initial cathode current density has no apparent effect on the purity of the products obtained in both phases of the investigation.

Jan 1, 1973

By O. Q. Leone

A processing unit was developed for the complete cleaning of titanium alloy chips. The process uses solvent degreasing, magnetic separation, and anodic solution of nonmagnetic impurities in 10 weight-percent sulfuric acid. Vacuum arc-melted ingots weighing approximately 10 pounds each were prepared from cleaning chips according to ingot specifications.

Jan 1, 1973

By R. Blickensderfer

The sparking and gas-igniting tendency of steels and alloys were evaluated my measuring the radiance of spark showers produced by grinding a sample on an abrasive wheel in air, the time required for a spark shower generated on an abrasive wheel to produce an ignition in an explosive gas mixture, and the energy and speed required for impacts between various materials to ignite an explosive gas mixture. Mixtures of air-methane were found quite resistant to ignition by showers of sparks. A mixture of air-9.S pct hydrogen was used to increase the sensitivity of the tests and to thereby extend the range of materials that could be evaluated. The results of the spark-shower tests indicate that carbon steels and the alloy steels found in coal-cutter tools are among the most sparking and most incendive of any materials tested. Stainless steels, nickel alloys, and tungsten carbide are among the least sparking and least incendive. The brightness of the spark showers depended upon the degree of oxidation of the abraded particles. Impact tests against hard rocks such as solid quartz and sandstone, showed that high-carbon steel was more inc endive in the hydrogen mixture than were the softer steels or the alloy steels found in coal cutters. Ignitions were found much less likely to occur at speeds somewhat lower than the speeds currently in use in continuous mining machines.

Jan 1, 1972

By E. G. Valdez

Three cryogenic systems that utilized liquid nitrogen, dry ice, and methanol with dry ice were investigated in conjunction with crushing and classifying techniques. The systems were used to aid in separating and reclaiming the metallic components contained in insulated wires, shredded automobile nonferrous metal concentrates, small motors, generators, and rubber tires. Wire strands, 2 to 6 inches long and insulated with polyvinyl chloride and neoprene, were chilled at -60° and -195° C, then roll-crushed and processed by water elutriation; this procedure resulted in two products--a sink fraction that was 99 percent metallic and a float fraction that was 99 percent nonmetallic. Excellent separation of zinc die-casting alloys from copper and aluminum contained in shredded automobile nonferrous metal concentrates was attained by chilling at -72° C for 1 minute, crushing in a grateless hammer mill, and screening. From the screened products, 97.2 and 100 percent of the copper and aluminum, respectively, were recovered in the plus Pinch fraction, and 100 percent of the zinc was recovered in the minus 1-inch fraction of over 97 percent zinc die-cast purity. Laboratory experimental results comparing direct and indirect chilling indicated that a sufficiently low temperature could be attained by indirect chilling to permit use of a liquid C02-dry ice system on insulated wires and mixed nonferrous metallic concentrates.

Jan 1, 1973

By K. J. Liles

The Bureau of Mines conducted laboratory semicontinuous and continuous heavy liquid tests to determine the feasibility of producing commercial-grade products from the high-clay sylvinite ores of the Permian Basin in New Mexico. Continuous test operations demonstrated that concentrates containing 59.9 percent K2O and recoveries of over 75 percent of the contained potash can be obtained. The organic heavy liquid was effectively recovered by vaporization, condensation, and absorption methods. Less than 5 parts per million of heavy liquid vapors were released to the atmosphere. This loss represents only 0.02 pound of heavy liquid per ton of ore treated.

Jan 1, 1973

By G. A. Wancheck

Shear tests were performed on several prepared samples of granular and powdery bulk materials to investigate the following parameters: Particle size and distribution, particle movement, moisture content, consolidation of material, bulk density, void ratio, porosity, volume change, and strain rate. A series of shear tests was performed with weight-percent-ratios of minus 0.185-inch tertiary sand and 1-1/2-by l/2-inch tertiary gravel mixtures, and weight-percent-ratios of minus 200-mesh limestone (rock dust) and minus 200-mesh bituminous float coal dust. A comparison was made for shear test results obtained with rectangular and circular shear cells utilizing the large and small direct shear testers. Specifically, the shear results obtained include the angle of internal friction or shear strength of the tested material under known consolidating pressures, and the kinematic angle of friction or coefficient of friction between the interface of a bulk material and a sample wall material. The experimental procedure, tests, and results are given for each parameter investigated.

Jan 1, 1973

By J. R. McVey

A 10-channel automatic data acquisition system has been designed and environmentally packaged for use with underground strain-gage applications and associated instruments. The system uses commercially available components and is assembled in two plastic enclosures. Environmental control is provided through a specially designed (compressed-air) air-conditioning system and water-resistant cabling. Accuracies of 0.01 pct and resolution of 1 µV have been obtained in underground tests.

Jan 1, 1973

By L. K. Barker

The purpose of this research was to determine how much, if any, improvement would be made by subjecting hydrogenated shale-oil naphtha to a catalytic reforming process. Preselected ranges of temperature and pressure within the commercial reforming ranges were chosen for investigation and other possible variables were held constant. All tests were made with a liquid hourly space velocity (LHSV) of 3 volumes of liquid feed per volume of catalyst per hour (Vf/Vc/hr) and a hydrogen feed rate of 3,000 scf/bbl. Operating temperatures of 850°,875°, and 900° F were used at pressures of 200,400, and 600 psig. The greatest octane improvement in the naphtha was obtained at a temperature of 900° F and pressure of 200 psig. The reformed naphtha had a clear research octane number of 89, a liquid yield of 80 vol pct, and a yield-octane number of 71.1. The data indicate that a higher temperature could have produced a higher yield-octane number.

Jan 1, 1973

By F. E. Joyce

This paper describes the development of a process for producing manganese and iron pellet concentrates from low-grade manganiferous iron ores of the Cuyuna range by a two-stage sulfatization-reduction roast. First, the manganese minerals (7.5 percent manganese) were converted to water-soluble manganese sulfate by roasting in sulfur oxide gases at 700° C, then, the hematitic iron minerals (31 percent iron) in the hot sulfatized are were reduced to magnetite with simulated reformed natural gas in the temperature range of 350° to 425° C. Batch tests were made in a 3-inch-ID by 6-inch-long, gas-heated, stainless steel retort, and continuous countercurrent experiments were performed in a 2-inch-ID by 10-foot-long, electrically heated shaft furnace. Manganese sulfate was removed from the roasted product by leaching with water, and over 90 percent of the manganese was recovered in an oxide product (65 percent manganese) obtained by precipitation, drying, and thelmal decomposition of the sulfate. An iron oxide concentrate (60 percent iron) with an iron recovery of 75 percent was obtained from the water-insoluble residue by magnetic separation.

Jan 1, 1973

By James J. Olson

The Bureau of Mines used micro fracture density analysis of quartz grains in thin sections and diametric pulse velocity measurements along preblast and postblast cores to determine the nature and extent of rock damage produced by small (0.25-,0.50-,1.0-, and 2.0-kg) charges of high intensity explosive (C-4) in granite. Pulse velocities from the postblast cores were significantly lower than velocities from the preblast cores and, with the core logs, provided clear identification of the upper and sometimes the lower limits of most severe damage. These zones ranged from about 1.68 ft for the 0.25-kg blast to 4.16 ft for the 2.0-kg blast. Microfracture densities from postblast cores were significantly higher and more variable than densities measured from preblast cores. The microfracture density measurements showed that microscopic damage was present far past the zones of most severe damage as delineated by the pulse velocity logs and core logs. An exponential relation-ship was observed between the micro fracture density levels and the charge weight.

Jan 1, 1973

By D. S. Burgess

This report summarizes the incidents that preceded the December 9, 1970, propane-air explosion in Port Hudson, Mo., and then attempts to establish the nature of the explosion from the ensuing events. Special emphasis is given to possible ignition sources, the distribution of flammable vapors, and the analysis of blast damage. Both near-and far-field damage indicated that this explosion may be attributed to the detonation of propane in air with an energy release equivalent to that from about 50 tons of detonating TNT.

Jan 1, 1973

By F. N. Kissell, C. H. Elder, C. M. McCulloch

The applicability of the "direct method" for determining the methane content of virgin coalbeds was tested. Preliminary results indicate that the direct method, when applied to exploration cores, can be successfully used to estimate coalbed gas content and also approximately predict the total gas emission from a prospective mine located in the coalbed at the exploration site.

Jan 1, 1973

By A. G. Kim

Methane and other hydrocarbon gases, byproducts of coalification, are emitted from coal at widely varying rates and often present ventilation problems during mining. The air in some coal mines apparently contains no methane. To determine if coals from mines which bid no history of detectable gas emission contained adsorbed methane, samples of coal at the shaft bottom and at an active face were obtained and placed in sealed metal cylinders. The atmosphere around the coal was sampled and analysed by gas chromatography. Methane, ethane, ethylene, propane, propylene, and butane were found to have been desorbed from these coals. Hydrogen and helium were also detected. An estimate of the amount of residual gas per ton A coal indicated that coal samples from the active face generally contained more adsorbed gas than coal samples obtained from the shaft bottom, although in both instances the total amount of gas was relatively small.

Jan 1, 1973

By William J. Campbell

This analytical method development and evaluation was undertaken by the Bureau of Mines to provide accurate determinations of eight minor elements in low-alloy steels prepared from ferrous scrap. Fluorescent X-ray spectrography was the principal method investigated. Confirming analyses were made by conventional instrumental and chemical methods. All X-ray data were processed by a timesharing computer. No corrections were found necessary for inter-element effects or overlapping spectral lines. Concentrations were calculated from the least-square fit of a linear calibration equation derived from measurements on three sets of standard steels. These studies show that X-ray spectrographic analysis of lathe-finished surfaces provides accurate determinations of aluminum, copper, chromium, manganese, nickel, phosphorus, silicon, and tin.

Jan 1, 1973

By J. B. Rosenbaum

Prolonged laboratory and limited pilot plant tests have shown that the Bureau of Mines buffered S02 -H2S process is capable of removing 95 to 99 percent of the S02 from industrial waste gases. Most of the S02 is converted to elemental sulfur; only about I percent converted to sulfate The process comprises (1) washing the flue gas to remove particulates and S03, (2) absorption of the S02 in citric acid or other carboxylate solution, (3) reaction of the loaded solution with H2S in a closed vessel to precipitate the absorbed S02 as elemental sulfur, and (4) separation of the sulfur from the regenerated solution by oil flotation and melting. Two-thirds of the molten sulfur is converted to H2S for use in the sulfur precipitation step by reacting sulfur vapor with natural gas and steam in the presence of an alumina catalyst. The chemistry and mechanism of the process are described, initial laboratory and pilot plant data are summarized, and second-generation laboratory operation and pilot plant design are reviewed. Preliminary cost estimates are presented for recovering sulfur from copper smelter gas, powerplant flue gas, and Claus plant tail gas.

Jan 1, 1973

By Mark I. Copeland

The Bureau of Mines investigated the effect of up to 1 wt-pct of copper and silicon on the heat treatment response and hardness, tensile, and impact properties of hot-rolled medium-carbon steels. The steels were prepared by induction melting and fabricated into plates by forging and rolling. The tensile strength of 0.2-wt-pct carbon steels containing 0.3 wt-pct silicon was affected significantly by copper in both the hot-rolled and heat-treated (600° C) conditions, whereas the tensile strength of the 0.3-wt-pct carbon steels was less affected. A 600° C treatment was considered optimum as a post-rolling treatment to strengthen the steels by copper precipitation. Strengthening of 0.2-wt-pct carbon steels by silicon was reduced by increasing copper contents.. Optimum impact strengths occurred at about 0.3 wt-pct silicon in 0.2-wt-pct carbon steels containing 0.6 and 0.8 wt-pct copper. The impact strengths were lowest for 0.2-wt-pct carbon steels containing over 0.8 wt-pct copper and greater than 0.3 wt-pct silicon, especially in the heat-treated condition. Copper and silicon solutes and copper precipitates strengthened the steels. This effect was augmented slightly by strengthening through grain refinement by these solutes.

Jan 1, 1973

By M. Hertzberg

Results of a comprehensive study of the absolute spectral radiance of the infrared emissions from methane-air explosions are reported. The spectral growth of these expanding flames were recorded with a time resolution of 1 msec in the spectral range of 1.7 to 5.0 µm. Time-resolved spectra were obtained for methane-air mixtures as a function of stoichiometry, nitrogen dilution, and Halon dilution, in a 9-liter vessel under different venting conditions. Data are also presented for coal dust-air explosions. Temperatures, obtained from the absolute radiances and from a band ratio technique for methane-air, are internally consistent and are generally 50° to 200°K below adiabatic flame temperatures. All near limit mixtures gave essentially the same flame temperatures (1,500° to 1,600° K) regardless of whether the limit was obtained by dilution with excess air, excess methane, excess nitrogen, or Halon. The coal dust explosion spectrum is essentially a blackbody continuum at 1,500° K with some selective emission at 4.4 µm from hotter CO2. The data are analyzed in terms of the radiative dynamics of a sperically expanding flame zone. The importance of radiative transport is assessed. An equation is derived which relates the instantaneous fraction of combustion power radiated to adiabatic variables.

Jan 1, 1973

By Joseph Grumer

In addition to nine powder and gaseous extinguishants of propagating Pittsburgh seam coal dust-air explosions earlier evaluated,6 10 other powders have similarly been evaluated under like conditions such that wall quenching of the coal dust-air flames was virtually absent and the dust concentration was temporally and spatially uniform to within about ±5 percent. None of the newly examined extinguishants was better than Purple-K (potassium bicarbonate); the 10 of this report are anhydrite (calcium sulfate), monobasic (4 types) and dibasic ammonium phosphate, natural and synthetic cryolite (sodium fluoalumi-nate), sodium sulfate, and tricalcium phosphate. Except for anhydrite, sodium sulfate, tricalcium phosphate, and the cryolites, these materials were about equally effective, when present in relatively low concentrations (weight-percent of the coal dust-extinguishant mixture). The maximum oxygen concentration for the extinguishment of otherwise uninhibited coal dust explosions and the influence of coal dust particle size and the volatile content of the coal were also explored. For the present, the choice of the inhibitor among the good ones evaluated is not as critical as the system to be used to deploy the extinguishant against a coal dust explosion.

Jan 1, 1973

By Stanley C. Rhoads

The Bureau of Mines investigated the complete ternary system K2 HfF6¬K2ZrF6-l.25 weight-percent HF at 40° C. In addition, solubility curves have been established at 25°, 30°, 500, 60°, and 70° C. These solubility data implemented a study of hafnium enrichment in feed solutions for liquid-liquid extraction processes.. Selected K2HfF6-K2 ZrF6-1.25 weight-percent HF mixtures were equilibrated in a constant temperature bath. Compositions of the equilibrated solutions and wet residues were established from combined hafnium and zirconium oxide and total fluorine analyses. All solubility curves were essentially parallel on triangular coordinates. At 40° C, the solid phase of the K2HfF6-K2ZrF6-1.25 percent HF system is a series of solid solution hydrates with K2HfF6-H20 and K2ZrF6.3H2O segments existing at the respective extremes. Since this system contains K2HfF6-H20 and K2ZrF6.3H20 segments, it is not ideal for simple separation of high-purity K2HfF6 from K2HfF6-K2ZrF6 mixtures by recrystallization. However, it would be useful for producing hafnium-enriched feed solutions from zircon concentrates for liquid-liquid extraction of hafnium from zirconium.

Jan 1, 1973