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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

By J. S. Miller

The Bureau of Mines developed methods for fragmenting oil shale formations with chemical explosives to prepare oil shale for in situ retorting and to evaluate the extent of fragmentation by various methods. A combination of three methods of explosive fracturing was used: (1) The displacement and detonation of a liquid chemical explosive in a natural fracture system; (2) the use of 60-pct dynamite to relieve stress conditions of the rock around the wellbore; and (3) the use of pelletized TNT in a series of wellbore shots to fragment the oil shale. An attempt was made to seal or grout around the fragmented oil shale by drilling 67 holes and displacing approximately 200 bbl of neat cement in the fracture system to aid in evaluating the fragmented zone, Seven methods were used to evaluate the fragmented zone. The primary evaluation method was the recording of seismic waves to delineate the fragmented zone with results based on arrival time, amplitude, and record quality. The data from the seismic measurements indicated the extensively fragmented zone was approximately 95 ft in diameter and 70 ft thick. Results of the remaining methods of evaluating fractures--including air-flow tests, coring of the expected fragmented zone, elevation measurements to indicate overburden crowning, and surveys with high-speed camera, impression packer, and down-hole camera--agreed with and supported the data from seismic measurements. Further field application of explosive fracturing and evaluation methods is needed to determine when a zone of oil shale is effectively fragmented for efficient in situ retorting.

Jan 1, 1973

By W. W. Agey

The Calico silver-barite deposits near Barstow, Calif., are a potentially important resource. Exploration performed by two major mining companies out-lined large tonnages of ore that assayed at 2 to 3 ounces of silver per ton and 7 to 15 percent barite. Laboratory beneficiation work was done by the Bureau of Mines on four samples to develop methods for recovering the silver and/or barite. Cyanidation recovered from 47 to 60 percent of the silver from ore ground to approximately 100 percent minus 325 mesh. Salt roasting minus 10-mesh material, followed by regrinding and cyanidation, recovered 75 to 85 percent of the silver. From 75 to 90 percent of the barite was recovered in a plus 92-percent barite product from either the natural ore or from cyanidation residues. Salt roasting before cyanidation precluded recovery of the high-grade barite concentrate from the leach tails.

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 W. T. Abel

The difficulties associated with wet-processing fine size coal led the Bureau of Mines to investigate a dry process for removing pyrite from coal pulverized to powerplant fineness. The dry process that was investigated consists of two cleaning steps: First, centrifugal separation is used to remove a fine, pyrite-depleted portion as a product; second, the remaining coarser, pyrite-enriched portion is taken to electrostatic separation in which pyrite is concentrated and rejected. Ball milling and Hardgrove milling were used to pulverize the coal. Three coals from the Pittsburgh seam were treated by the dry-removal process. Over 55 pct of the pyrite, which amounted to 70 pct of the available pyrite, was removed in a reject of 10 to 20 pct from one of the coals. Similar treatment of the other two coals removed about 35 to 50 pct of the pyritic sulfur, which amounted to about 70 pct of the available pyritie, sulfur from these coals. Both centrifugal and electrostatic separations were more efficient when pyrite particles were as large as possible. Separation efficiency was improved by confining the particle size of the feed to a relatively narrow range and by avoiding excessive amounts (more than 10 pct) of dust in the electrostatic range. The removal efficiency was increased with the use of stage grinding.

Jan 1, 1973

By J. R. Ross

The extraction and recovery of nitrate from waste solutions generated in the production of titanium were investigated using solvent extraction techniques. Laboratory studies and continuous tests in a small solvent-extraction system showed that up to 98 percent of the nitrate can be selectively extracted by a solution of tributyl phosphate in kerosine. The extracted nitrate can be recovered as nitric acid, at concentrations suitable for reuse, by stripping the loaded organic with water.

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 F. W. Penn

An aircraft auxiliary power unit (APU) was used as an exhaust source for evaluation and refinement of sampling and analytical procedures for gas turbine engines. The unit was also used to determine the emission characteristics of APU's in service and to study the effect of fuel composition and combustor design on exhaust emissions. Carbon monoxide, carbon dioxide, oxides of nitrogen, hydrocarbons, aldehydes, particulate loading, and odor were measured at engine operating modes representing the duty cycle encountered in airline operation. Analyses showed good repeatability, and adequate sensitivity was attained in these experiments. Smoke opacity measurements were not taken owing to the lack of a high-sensitivity smokemeter. Results showed that the minimum emission levels occurred with the standard combustor and Jet A fuel. Emission rates were highly dependent on test mode, but emission patterns as a function of test mode were similar for all fuels and combustors tested. A comparison of three identical design production combustors showed a variation in average emission rates of less than 5 pct.

Jan 1, 1973

By B. J. Scheiner

Silver ores from the Candelaria District, Nevada, and Round Mountain District, Colorado, were investigated mineralogically and metallurgically. Silver minerals of four distinct groups were identified: (1) silver sulfide; (2) argentojarosite; (3) silver contained in the iron oxide; and (4) manganese carbonate-oxide minerals, Electrooxidation and acid-chloride leaching techniques were investigated as means of altering silver minerals, and their effects on subsequent silver extraction were determined. Application of the knowledge obtained from mineral leaching studies resulted in development of a sulfur dioxide-sodium chloride leaching sequence for extracting silver from these types of ores. Silver extractions of 80 to 85 percent were obtained by leaching the ores with a sulfurous acid-sodium chloride system. This was an increase of 9 to 61 percent silver extraction over that obtained by conventional cyanidation techniques.

Jan 1, 1973

By D. E. Anders

Saturated hydrocarbons from 60 selected samples of a 2,300-foot Green River Formation oil-shale core (Piceance Creek Basin, Colo.) were analyzed by gas-liquid chromatography techniques. Emphasis was placed upon the distribution of normal alkanes and 15 key-branched and cyclic alkanes. The latter compounds consisted of the C15, C16, C18, C19, and C20 chain isoprenoids, the 5-a and 5-ß C27, C28, and C29 steranes, three C30 pentacyclic triterpanes, and perhydro-ß-carotene. The results showed definite evidence of maturation of both the n-alkanes and the branched and cyclic alkanes; however, most if not all of the changes were limited to the indigenous soluble extract and were not the result of additional soluble extract generation from the insoluble kerogen. Source material and environmental variations were important factors in some of the observed differences in the branched plus cyclic alkane compositions.

Jan 1, 1973