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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 J. B. Janus

This report, the 22d in a series, gives analytical data showing composition and quality of tipple and delivered samples of coal collected during fiscal year 1972. This coverage lists mines located in 20 States. Ultimate analyses are given for most of the coalbeds listed. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. The deliveries were sampled in accordance with instructions issued by the Bureau of Mines, and the samples were analyzed in the Bureau laboratory at Pittsburgh.

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 T. Kessler

As part of a respirable mine-dust research program at the U.S. Bureau of Mines, spark-source mass spectrometry has been used for the semiquantitative determination of trace elements (200 ppm weight or less) in raw coals. In addition, several minor and major elements have been determined using this technique. Sixty-four elements ranging in concentration from 0.01 to 41,000 ppm weight were determined in one anthracite, two mvb, four lvb, and six hvab raw coal samples. The samples represented 10 coal seams located in Pennsylvania, West Virginia, Virginia, Utah, and Colorado.

Jan 1, 1973

By M. A. Mahtab

This report presents the geometric parameters (attitude, spacing, extent, and aperture) of fracture patterns in a selected portion (study area) of San Manuel copper mine, Arizona. The geometric parameters are quantified for input to structural analyses for studies of the influence of fractures on cavability of ores. Using an orientation analysis procedure developed earlier by the Bureau, three prominent and nearly orthogonal sets of fracture orientations were delineated in the study area. Sets 1 and 2 dip nearly vertically, and generally strike east-west and north-south, respectively, whereas set 3 is nearly horizontal. Both a horizontal rotation (of 14° to 26° for sets 1 and 2, respectively) and a tilt (of 20° for set 3) is shown to occur between the 1415 and 2015 levels of the mine. Gomparison of the three major rock types present in the study area (quartz monzonite, monzonite porphyry, and rhyolite) show that the rhyolite is characterized by short extent, small spacing, and tightness of fractures as well as the general absence of fracture set 3, which may account for its generally observed strong resistance to caving.

Jan 1, 1973

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 P. D. Bergman

The high price of pollucite ore, its limited availability, and the need to provide stack removal of S02 present formidable obstacles to the use of pure cesium as a seeding material in MHD power generation. Cost estimates indicate that mixed potassium-cesium seeding is preferable to the use of either pure cesium or pure potassium. Cheaper electricity and higher open-cycle MHD operating efficiencies result from the use of mixed seed. Savings of $3,000,000 per year in power costs for a 1,000-MWE open-cycle MHD power-plant are envisioned if the mixed seeding technique is adopted.

Jan 1, 1972

By M. J. Kovalik

Illinois No.6, a high-volatile B coal of low fluidity, was blended with fluidized-bed char and coke breeze to improve the strength of the coke obtained from carbonizing this coal. Twenty-one tests, selected from those made in the small-scale Hanson carbonizer, were carbonized in the BM-AGA 13-inch-diameter, cylindrical retort, with a coal charge of about 90 pounds; the strength of the cokes was determined by the standard ASTM tumbler test. Using the same procedure, 10 tests were made with High Splint, a high-volatile A coal from Harlan County, Ky. Carbonization of the blends produced larger and stronger cokes than did the Illinois No.6 coal singly. The optimum blend contained 6 percent each of char and coke breeze. Further improvement in coke strength was realized by either preheating this blend prior to carbonization or by adding a small pro-portion of a premium blending coal. The former method could possibly eliminate the use of premium coking coals in blends with Illinois No. 6 coal to make an acceptable metallurgical coke. Except for no improvement in coke strength by preheating, results for High Splint coal showed behavior similar to that of the Illinois No.6 coal.

Jan 1, 1973

By A. Visnapuu

High-grade synthetic rutile has been produced in the laboratory from domestic ilmenite concentrates by a new carbonyl process. The ilmenite was first reduced to convert the iron oxides to metal and then treated at temper-atures over 1000 C in high-pressure carbon monoxide (CO) to convert the iron to the pentacarbonyl. Rapid carbonylation was achieved in the presence of small quantities of selected promoters. Maximum iron removal occurred at temperatures between 110° and 130° C at CO pressures from 1,000 to 1,400 psig. Iron pentacarbonyl appeared as liquid and vapor in the reactor and could be removed by gravity flow and vapor transport. More than 90 pct of the iron was extracted in 2-hr experiments at pressures of 1,000 psig and above. The Ti02 product is porous owing to the removal of the iron, has the rutile crystal structure, and is suitable for chlorination. Waste disposal problems associated with the process would be minimal because the iron pentacarbonyl can be decomposed to produce iron powder or pellets for sale and CO for recycling.

Jan 1, 1973

By J. C. Nigro

Hematite-to-magnetite reduction kinetics were investigated mainly in CO-CO2 atmospheres at temperatures ranging from 500° to 1,000° C. Reduction rates were measured with a thermobalance, which recorded the weight loss as the specimen was reduced. Reduction data on both synthetic and natural hematite spheres showed good linearity of ro [1-(1-R)1/3] with time, t, up to over 85 pct conversion to magnetite; the rate coefficient (k[L], cm/min) obtained from the linear portion of the plot was used to characterize the penetration rate of the hematite-magnetite interface. Gas composition, porosity, and silica content were major factors affecting the rate. Temperature dependency of the reaction rate was small, yielding a mean activation energy of about 3 kcal/mole. Silica additions increased the reaction rate, probably through an increase in the effective surface area and diffusion; however, above 900° C, silica can react to form fayalite. Experimental data showed that the linear thickening rate of the magnetite layer, normally evidence of a chemically controlled reaction, can also be indicative of a reaction controlled by both mass transfer and diffusion. Evidence from this study indicates that the dominant rate-controlling factor in the reduction of hematite to magnetite at high temperatures is transport in the gas phase.

Jan 1, 1973

By G. L. Fitzpatrick

Future applications of seismic holography to "seismically transparent phase objects," such as rock inclusions, fracture zones, liquid-filled cavities, etc., will require techniques to improve the poor image contrast generally characteristic of these objects. Although conventional phase-contrast enhancement techniques could be used, these methods involve additional optical elements such as quarter-wave spatial filters. Owing to the anticipated practical difficulties of properly alining such optical devices and properly locating poorly defined image planes and filter planes, this approach is not considered to be well-suited to the case of seismic holograms and their laser reconstructions. Results similar to those achieved with spatial filters may be obtained without filters by specially processing the seismic hologram data. The new process, which is an extension of Gabor's subtraction holography, achieves an improvement in contrast by an interferometric technique. The process involves adding a ?before" hologram without an object present to a 90° phase-shifted "after" hologram with the object present. Then, the combination is reconstructed with a laser or by computer. Not only is the image contrast improved in such processed holograms, but the images are also phase-contoured. In general, the latter feature is not to be expected when conventional phase-contrast enhancement techniques are employed. The new technique is experimentally verified by examining computer-generated synthetic seismic holograms rather than by examining actual seismic field data. However, results of this study are directly applicable to real seismic data and should prove useful in future applications of seismic holography.

Jan 1, 1973

By E. Aamland

Preparation of high-purity magnesium-yttrium alloys by electroreduction of Y2O3 dissolved in a YF3-LiF bath and the subsequent deposition of yttrium in a molten magnesium cathode was investigated in laboratory-scale apparatus. Parameters such as temperature, current density, and electrolyte density were studied. Electrolysis was conducted in a specially designed MgO diaphragm cell at temperatures ranging from 780° to 970° C. Alloys containing up to 55 weight-percent yttrium were prepared at cathode current efficiencies of 21 to 60 percent. Cell design and operation are described, and some of the limiting conditions pertaining to the method are discussed.

Jan 1, 1973

By Joan C. Biordi

A molecular beam-mass spectrometer-low pressure flat flame apparatus has been constructed for the purpose of examining the chemical microstructure of normal methane-oxygen-argon flames and those inhibited with Halon extinguishants. Details of construction and performance of this apparatus and of related flame temperature measurements are given. Particular attention is paid to the empirical characterization of the perturbation to the flame caused by the sampling probes. The composition profiles obtained for normal flames are compared to those of flames inhibited by CF3Br. In addition to the usual stable species (CH4, O2, CO, CO2, H2O, H2, and H2CO), the inhibitor, its products and intermediates associated with its reactions could be followed. In particular, hydrogen bromide, bromine atoms, hydrogen fluoride, and carbonyl fluoride were observed. The relatively rapid disappearance of inhibitor and early appearance of fluorinated reaction products suggest a short lifetime for the CF3 radical in this system. Observation of COF2 suggests that CF3Br is effective as an inhibitor, at least in part, by virtue of its interference with the oxygen containing species of the normal chain reaction. Profiles of the 17+ peak at low electron energy suggests that the hydroxyl radical may also be sampled, but the profiles obtained are not yet sufficiently accurate to determine the effect of inhibitor on this important flame radical.

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 R. C. Wang

Solid-liquid flow in different pipe geometries was investigated. This investigation was conducted by measuring delivered solids concentration and head loss. The delivered solids concentration was measured to study the effect of pipe geometry on the minimum carrying velocity above which solids do not lag behind the fluid. Head loss was measured to study the effect of pipe geometry on the friction loss. A mathematical formula was developed for determination of the minimum carrying velocity. Darcy-Weisbach's equation and Durand's equation were used for comparison of head losses of pipe shapes. Of the different pipe shapes studied, each having the same interior cross-sectional area, the rectangular pipe with the wide side oriented as the base yielded the lowest minimum carrying velocity at high solids concentrations. The minimum head loss at low velocity and high solids concentration also was attained with this pipe. Although the circular section is known to be the best for transporting liquid only, the present study suggested that pipe geometry is a factor in lowering the operating velocity and reducing head loss in solid-liquid flow.

Jan 1, 1973

By D. A. Doughty

The Bureau of Mines developed two methods for determining iron II and iron III in 2- to 5-mg samples of coal using electron paramagnetic resonance (EPR) spectrometry. One method used solid coal samples; the other method used aqueous solutions. The method using solid samples was more simple, technically, but required the use of X-ray fluorescent analysis, or another independent method, for determining total iron in the samples, and the results were subject to some uncertainty. The method using aqueous solutions appeared capable of greater certainty and did not require additional methods of total iron analysis but was more involved procedurally. The coals analyzed were found to contain much more iron II than iron III.

Jan 1, 1973

By John Ward Smith

Aragonite, co-occurring with calcite and dolomite as matrix minerals, has been discovered in Mahogany zone oil shales of Colorado's Eocene Green River Formation, posing puzzles on the geochemical patterns of their separate origins, reasons for their simultaneous existence, and their interrelation. The presence of aragonite is demonstrated by X-ray diffraction. Amounts of aragonite and dolomite are significantly and inversely related, but the calcite quantity is essentially independent of either aragonite or dolomite quantity. A geochemical pattern outlining the deposition conditions that created the Green River Formation oil shale is postulated from characteristics of the oil shale. The development of the three separate carbonates--aragonite, calcite, and dolomite--the inverse relationship between aragonite and dolomite, and the independence of amounts of calcite and the other two carbonates are shown to be natural consequences of this oil-shale genesis pattern.

Jan 1, 1973

By W. E. Lamont

The Federal Bureau of Mines conducted research to develop methods of removing phosphorus from the earthy, calcareous hematite ores of the Birmingham, Ala., iron district while simultaneously improving the grade and recovery of the iron values prior to furnacing. An attempt was also made to identify the phosphorus minerals present in the ores. The ores contained about 36 percent iron, 12 to 16 percent CaO, 15 to 20 percent hydrochloric acid insolubles, and 0.30 to 0.36 percent phosphorus. Fractions containing 5 to 15 percent phosphorus were isolated from the ores. Collophanite, Ca3P2O3?nH2O, a member of the apatite group, was the only phosphate mineral identified. Beneficiation methods using flotation and reduction roasting with magnetic separation yielded good grade iron concentrates, but were not as effective for reducing the phosphorus content of concentrates. Reduction roasting followed by fine grinding, magnetic separation, and acid leaching gave iron concentrates containing 62.5 percent iron and 0.04 percent phosphorus with an iron recovery of 82.9 percent and a phosphorus rejection of 93.7 percent. Reoxidation of reduced magnetic concentrates followed by acid treatment gave iron concentrates containing 58.1 percent iron and 0.02 percent phosphorus with 89.6 percent recovery of the iron and 96.5 percent rejection of the phosphorus.

Jan 1, 1973