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By M. J. Ferrante

Enthalpy and entropy increments above 298.15° K were determined for cop-per sulfate between 298° and 1,000° K and for copper oxysulfate between 2980 and 1,146° K by the method of copper-block drop calorimetry. Enthalpies, entropies, and heat capacities are tabulated for both compounds. In addition, free-energy functions are tabulated for the sulfate. Equations representing the enthalpies are given for each compound.

Jan 1, 1972

By W. E. Lamont

Flotation studies of phosphate-bearing waste pond materials, low-grade washer products, and raw ores, all from the Tennessee brown phosphate district, showed that these types of materials could be treated without des liming to recover high-grade phosphate concentrates. The investigation showed that fine grinding before flotation was a requisite for increased recovery of the phosphate values and that the optimum pH conditions were in the range of 10.0 to 10.5 when using anionic collectors. Multiple-cleaning of the rougher phosphate concentrate was required to produce high-grade concentrates. Phosphate recoveries ranged from 60 to 82 percent and were inversely related to the grade of concentrate produced.

Jan 1, 1972

By D. Montagna

The Kroll-Betterton process for debismuthizing lead is based on adding calcium and magnesium to impure molten bullion to form solid Ca-Mg-Bi inter-metallic compounds that float on the surface as drosses. Present practice in industry is to hand-skim off these drosses, often followed by hydraulic pressing to squeeze out some of the entrapped liquid lead. In an effort to develop an improved technique, the use of an argon-shrouded dipping centrifuge to perform the required phase separation was investigated. Centrifugation experiments demonstrated that the bismuth content of an impure bullion could be lowered from an initial 0.5 percent down to 0.03 percent with a lead recovery of 90 percent, which is comparable to lead recovery after hand skimming of drosses in commercial lead-debismuthizing operations. Centrifugation provides better control in removing drosses, faster operation with less oxidation and relatively little fuming, and recovery of a lead bullion that approaches commercial specifications.

Jan 1, 1972

By E. L. Singleton

The Bureau of Mines investigated extraction of aluminum from aluminum-silicon alloys as a means of utilizing domestic aluminum silicate ores for aluminum production. Aluminum was extracted from aluminum-silicon alloys by electrolysis in molten electrolytes of NaCl-KCI-AIC13 and NaCl-KCI-AIF3 in a laboratory-scale cell. Six alloys with aluminum contents ranging from 20 to 87 percent aluminum were tested, and aluminum products of primary grade or better were obtained. More than 80 percent of the aluminum was recovered with current efficiencies as high as 91 percent. Recovery of a metallurgical-grade silicon product from the anode residue by an acid leaching procedure was possible with the 50-50 and 65-35 Al-Si alloys.

Jan 1, 1972

By J. E. Dooley

A mass spectral scheme of analysis was devised which can be used to identify individually a single compound from a larger group of similar compounds. Mass spectra for 32 alkyl aryl sulfides are provided for future reference work, and analytical correlations used in producing the analytical scheme are discussed. Some of the correlations show that base peaks are either the same mass as the parent peaks or may be derived from cleavage alpha to the sulfur atom with migration of one hydrogen to the sulfur atom. Other spectral consistencies provide means of separating ortho-, meta-, and paratolyl arrangements in an overall analytical scheme. Determinations of chain lengths and separation of isomeric species are also discussed.

Jan 1, 1972

By M. E. Tyrrell

The Bureau of Mines produced building brick of good quality in an investigation designed to explore the possible utilization of high-glass fractions of municipal incinerator residues in the manufacture of building products. Common clays, lime, and sodium silicate were used as binders for the nonplastic residues Test bricks were formed by dry-pressing, soft-mud molding, and stiff-mud extrusion. A run of standard-size face brick dry-pressed and fired in the West Virginia University Coal Research Bureau pilot plant demonstrated that SW-grade glass-clay face brick can be produced on a commercial scale without difficulty. A cost evaluation made for production of the brick showed an estimated cost of $42.13 per thousand bricks for a shuttle kiln plant and $28.70 per thousand for a tunnel kiln plant.

Jan 1, 1972

By N. N. Moebs

The atmosphere in part of an air-sealed coal mine was monitored continuously through a drill hole for oxygen content to determine the effectiveness of sealing a mine against the entrance of air and the major force that caused the phenomenon of mine breathing through the overburden. The differential pressure across the seal and the barometric pressure on the outside also were recorded. A general correlation, obtained between the oxygen level, differential pressure, and barometric pressure, indicates that changes in air pressure are the cause for periodic replenishment of the oxygen in the mine. Mine effluent quality was determined by conditions in many sections of the mine and could not be related to the oxygen level at the drill hole.

Jan 1, 1972

By G. L. Fitzpatrick

Preliminary results of an experiment in seismic holography indicate that the techniques of acoustical holography may be successfully used with seismic waves to determine the size and general shape of underground objects. This experiment was carried out under field conditions on a moderately large scale compared with the typical laboratory experiments in acoustical holography. The object to be mapped was a 100-foot-diameter, spherical, low-velocity zone of explosively fractured rock in oil shale at an average depth of 80 feet. The seismic wavelength of the Fourier component wave used in making the seismic holograms was 50 feet at a frequency of 140 cps. The hologram sampling aperture was 226 feet square and was sampled by 441 geophones in a 21 by 21 rectangular array. One novel aspect of the experiment was the use of a wide-band polychromatic explosive source of seismic waves rather than a narrow-band quasi-monochromatic vibrator source. A successful laser reconstruction of the object image from a lensless Fourier-transform hologram in the form of a 5/l6-inch-square photographic transparency is illustrated. The size of the underground object measured from the laser reconstruction of the object and the size inferred from a knowledge of the amount of explosives used to fracture the site and the tensile strength of the oil shale are found to agree.

Jan 1, 1972

By A. W. Deurbrouck

This report describes the washability characteristics of 18 coal samples taken from 11 drill hole cores from the San Juan Basin area of New Mexico and Colorado. The ash content of these coals could generally be substantially reduced by removing the heavy impurities. The coals were characteristically low in sulfur content; only one sample contained more than 1 percent sulfur after removing the sink-I.50 specific gravity material. The coals ranged in rank from subbituminous C to high volatile C; 11 of the samples were subbituminous A. Many of these core samples came from areas where very little fieldwork has been done; consequently, an outgrowth of this work has been an increase in known coal reserves of the San Juan Basin area.

Jan 1, 1972

By M. D. Schlesinger

Mercury exists in coal in minute quantities, but the large tonnages of coal consumed could represent relatively large amounts of mercury entering the environment. Limits have now been placed on the emission of mercury, and it is important that reliable analytical methods be available to the chemist. The Bureau of Mines has evaluated analytical techniques used by a number of laboratories; most used vapor phase atomic absorption as the final detection method. Neutron activation was used by some of the laboratories. All of the methods described could be applied, but they require careful manipulation to prevent loss or mercury contamination. In the samples analyzed the mercury content ranged between 0.05±0.01 and 0.4l±0.06 part per million.

Jan 1, 1972

By Foster Fraas

In this Bureau of Mines report, use of the photoemission of electrons to produce electric charges for the electrostatic separation of sonic dispersed minerals, which had previously been ground to pass a 43µ-opening sieve, is demonstrated. It appears that many of the oxides, carbonates, sulfides, and arsenides will respond to photoemission. Minerals least responsive are the oxides of silicon, the oxides of aluminum, and minerals that have a high concentration of these oxides. Although several synthetic ore mixtures did not yield to complete separation in a one-stage operation, it is probable that preliminary neutralization of the initial electric charges produced by powder dispersion will provide complete separation. That the separation can be carried out in air and without the use of reagents or heating, which are required in the present practice of electrostatically separating coarse granular feeds, is of special significance.

Jan 1, 1972

By Harold E. Marr

The Bureau of Mines evaluated two drill-hole probes for the delineation of Missouri lead ores. The battery-powered, portable instruments, weighing less than 30 pounds, were designed for logging holes of 1.8 inches in diameter or larger. These probes have dual scintillation detectors, balanced filters with a pass band for lead Ka radiation, and a cobalt-57 source of radiation. The results of field tests in Missouri confirm laboratory tests indicating that probe response can be correlated to lead ore grade using counting times of 10 seconds or less at any selected depth in the hole.

Jan 1, 1972

By R. B. Schluter

Drying and preheating (partial induration) the green, unfired iron ore pellets is a means of reducing the energy required to produce metallized pellets. The Bureau of Mines processed three magnetite and two hematite concentrates through the unit operations of pelletizing, preheating in air, and reduction to metal to determine the effects of preheating upon the properties of the metallized pellets. The pellets were prepared in a 16-inch-diameter laboratory balling drum. Preheating and metallization were carried out in an externally heated 4-inch-ID by 4-inch-long stainless steel drum using air for the preheating atmosphere and lignite char as a reductant. The results 'varied considerably: two of the magnetites spalled when preheated in air at temperatures of 900° C and above, and the third magnetite and the hematite flotation concentrate required complete induration at 1,300° C to produce satisfactory pellets. The earthy hematite ore yielded excellent pellets at all preheat temperatures.

Jan 1, 1972

By Joseph L. Condon

High-speed movies were taken of crater experiments in two-dimensional plates of Tennessee marble to study craters being formed primarily by stress-wave action. The contribution of gas action to the cratering process was minimized because the two-dimensional models did not contain the expanding gases from the explosive. Four burdens were studied for solid plates and one burden for a segmented plate. After cratering, the plates were reassembled for dye penetrant studies of fracturing. Flyrock velocities were calculated and related to the degree of fracturing, and compared with those from quarry shots. In general, the smallest burdens produced the highest flyrock velocities and the least amount of fracturing. Flyrock velocities compared favorably with initial flyrock velocities in quarry blasts, but did not show step accelerations due to gas effects as did the quarry blasts. The test with a segmented plate was used to simulate cratering in a jointed material and showed that stress-wave effects can be important for crater formation in jointed rocks.

Jan 1, 1972

By R. E. Peterson

Scrap iron is partially oxidized at elevated temperatures in the selective oxidation process to produce iron oxide and a dense residual metal of high purity. Investigation of the process was confined to converting automobile hulks into useful products. In one test series, compressed, sheared automobile scrap was processed at 1,000° C in a 36-foot-long rotary kiln at feed rates ranging from 300 to 1,200 lb/hr. Less fuel was required to maintain the temperature at the higher feed rates because of the heat generated from the burning of the combustibles and the oxidation of the iron. The bulk density of the residual metal exceeded 75 pounds per cubic foot. In an attempt to lower the quantity of contaminants in the residual metal, another test was designed using automobile hulks which had been prepared by ripping, a low-cost method of scrap fragmentation. Before oxidizing the ripped scrap approximately 62 percent of the total copper was removed in a tumbling, screening, magnetic separation and hand-sorting system. Cast iron made from the residual metal obtained by selective oxidation contained 0.15 percent copper; iron oxide scale obtained from the kiln averaged 0.13 percent copper. Pellets made from the scale demonstrated compressive strengths necessary for blast furnace reduction; lead and zinc were removed by volatilization when the induration was performed in a reducing atmosphere.

Jan 1, 1972

By Hillary W. St. Clair

This report gives the results of an experimental study of the progressive changes that occur in particle size and size distribution when a homogeneous and isotropic mineral is subjected to crushing by impact. The mineral used in the study was uniformly sized quartz, which was crushed in a simple drop¬-weight machine that applied impact energy up to about 100 kg-cm per g. Screen analyses of the crushed products were analyzed by the method of moments to determine the mean size, variance, skewness, and kurtosis. Analysis of the data from these experiments shows that the mean size of the crushed product is a function of the energy input and the initial size. The size distribution is functionally related to the degree of size reduction. As the mean particle size is decreased, at first there is a corresponding increase in the variance and decrease in the skewness, But, as size reduction is carried further, each tends eventually to approach a steady value, and the form of the size distribution becomes stable.

Jan 1, 1972

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of the Ohio coalfield. Washability analyses were made on 39 coalbed samples collected from a 14-county area. None of the samples were of metallurgical quality as received. Nine of the samples could be sufficiently upgraded to produce metallurgical-grade products, and the remaining 30 samples could not be upgraded to this quality because their sulfur contents could not be lowered to meet the standard. For steam or power generation, 10 of the samples were of medium sulfur content as received and one could be upgraded to a low sulfur content. Of the 29 samples having a high sulfur content as received, 18 could be upgraded to a medium sulfur content. The original sulfur content of the other 11 samples having a high sulfur content as received can be appreciably reduced by removal of the sink 1.58 specific gravity material; however, these coals would be classified as high sulfur coals both before and after removal of the sink 1.58 specific gravity material.

Jan 1, 1972

By T. A. Sullivan

The processing of sweated aluminum electronic scrap was investigated to develop methods for recovering the aluminum and concentrating the other metals, including copper, lead, gold, and silver, into a product that can be separated by known methods. Two molten-salt electrorefining processes were developed and tested. The first process utilized a three-layer refining cell with a BaCI2-NaF-AIF3 electrolyte, which operated at 750° to 850° C. The second process used an all-chloride electrolyte of NaCI-KCI-AICI3 at 750° to 800° C, with separate anode and cathode compartments. High-quality aluminum was recovered that averaged 99.8-percent pure in the three-layer cell and 99.6-percent pure in the compartment cell. Over 94 percent of the aluminum was recovered with cathode current efficiencies of approximately 90 percent in both methods. The copper, lead, tin, silver, gold, and other metals were concentrated threefold in an anode product. Separation of lead and part of the tin by liquation from this product seemed feasible. The anode product was smelted to prepare a 96-percent copper bullion that contained 690 ounces of silver and 65 ounces of gold per ton, with 98 percent recovery of these values.

Jan 1, 1972

By A. F. Colombo

The differences in starch demands that occur between ore types subjected to the anionic flotation of calcium-activated gangue and the range of residual starch contents expected to give the best metallurgical response were evaluated on a batch and pilot plant basis. A phenol-sulfuric acid procedure was used to determine the residual starch contents in the iron ore slurries. Three pilot plant campaigns on samples from a group of orebodies located on the Marquette Range, Michigan, showed that in the rougher flotation pulp, a residual carbohydrate range of 25 to 100 ppm, which is equivalent to a 0.5 lb/short ton spread, yielded optimum results. Concentrates assaying at least 65 percent Fe and less than 6.0 percent Si02 and containing more than 80 per-cent of the recoverable iron were obtained. Both batch and continuous research indicated that starch adsorption is calcium modulated and relatively unaffected by the fatty acid additions employed. Residual starch level is not a critical control factor, but the addition must be adjusted to about 25 to 50 ppm residual starch and kept in this range for most effective utilization of the added tapioca flour.

Jan 1, 1972

By John P. Capp

Addition of sintered fly-ash/bottom-ash mixtures to rubber formulations failed to increase the skid resistance of the resulting products. Wear, tensile and hot-tear strengths, and resilience of the ash-rubber material, as determined in laboratory tests, were significantly less than that of comparable rubber. The material appeared unsatisfactory for automobile and truck tire manufacture, but might prove suitable as a filler in other rubber goods. Raw fly ash could not be satisfactorily compounded with rubber.

Jan 1, 1972