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By C. M. McKinney

Sulfur content data from Bureau of Mines routine analyses of 1,060 United States crude oils were used with crude oil production data for the years 1956-66 to prepare tables and charts that illustrate the volume and percentage distribution according to sulfur content of crude oil produced in 10 geographical areas of the United States. Similar relationships for foreign crude oils based on analyses of 201 crude oils and production during 1966 are illustrated for Africa, Canada, Middle East, and South America. Tables are included giving field name, sulfur content, geologic name and age of producing formation, depth of producing formation, and production during 1966 for 882 United States crude oils and 201 .foreign crude oils. Between 1955 and 1966 the average sulfur content of crude oils produced in the United States decreased from 0.73 to 0.67 percent.

Jan 1, 1967

By J. L. Reuss

The Bureau of Mines derived information on the softening characteristics of both unfired and indurated iron ore pellets as measured by hot compression strength in a laboratory study. A surprisingly high hot strength (240 1b per ½ -inch spheroid) was developed by unfired magnetite pellets near 900° C; lesser maxima were developed by pellets made from hematite and specularite concentrates near 1,000° C. Those from goethite remained weak throughout the pre induration heating. Fully indurated commercial pellets retain a high resistance to softening when heated in air. On the contrary, in a hot reduing atmosphere their high cold crushing strength dissipates rapidly. At 1,000° C, for example, the average compression strength of seven different commercial pellets was 110 lb; at 1,100° C, the hot strength was only 60 lb. After a rather sharp initial drop, the loss of strength with increase of temperature was gradual. There was no sudden collapse, nor any significant difference, in behavior of commercial pellets whether made from magnetite or hematite concentrates.

Jan 1, 1968

By Elton L. Litchfield

The Bureau of Mines determined minimum energies for direct initiation of expanding gaseous detonation waves in acetylene-oxygen mixtures. Composition limit ranges for the initiation of detonation with fixed energies have been compared to data in the literature. Assuming that the stored electrical energy is completely converted to thermal energy, the agreement between the energy of primary explosive initiators and the energy of electrical discharge initiators was good. Minimum energies for initiation of detonation in the most sensitive composition (40 percent C20 plus 60 percent 0 2) were: 0.64 joule at an initial pressure of 1/4 atmosphere, 5.0X10-2 joule at 1/2 atmos¬phere, and 3.7X10-3 joule at I atmosphere. Fuel concentrations in mixtures initiated to detonation by 4.9X102 joules ranged from 10 to 65 percent C2H2 at 1/4 atmosphere, 10 to 67 percent C2H2 at 1/2 atmosphere, and 9 to 68 percent C2H2 at 1 atmosphere.

Jan 1, 1967

By R. K. Koch

The vapor pressures of liquid molybdenum and liquid zirconium were determined by the Langmuir free-evaporation method. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. The vapor-pressure data led to the following equations: [log p (atm) = 5.429 - 28,380 T for liquid molybdenum in the range 2,890° to 2,990° K, and log p (atm) = 6.521 - 30,940 T for liquid zirconium in the range 2,229° to 2,795° K.] Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 157.6 ± 1.8 kcal/mole and 148.4 ± 2.4 kcal/mole for molybdenum and zirconium, respectively, where the uncertainties are two standard devia¬tions. Second-law standard heats of sublimation determined from sigma plots and tabulated enthalpies were 143.5 ± 2.7 kcal/mole and 149.2 ± 3.8 kcal/mole for molybdenum and zirconium, respectively. The better agreement in heats of sublimation for zirconium is attributed to the 566° K temperature range studied which permitted a more accurate definition of the vapor pressure curve than could be obtained from the 100° K span for molybdenum. This supposition was verified by making a sigma-prime plot which utilized solid vapor pressure data for molybdenum to extend the evaluation range by 800° K. This gave a standard heat of sublimation of 155.2 ± 1.6 kcal/mole which is in good agree¬ment with the third-law value. The plot also gave a standard entropy of sublimation (298.15° K) of 35.73 ± 0.48 eu.

Jan 1, 1968

By T. A. Sullivan

Refining in a molten salt electrolyte was investigated as a means of recovering nickel containing less than 1 percent and preferably less than 0.2 percent cobalt from nickel products containing up to 5 percent cobalt. Electrolytic separation of nick and cobalt was accomplished in a molten KCl-LiCl-NiCl2 electrolyte. Nickel containing less than 0.10 percent cobalt was routinely prepared. Factors that influenced the transfer of cobalt to the refined product were the nickel concentration of the electrolyte, the cobalt concentration of the electrolyte, the ratio of nickel to cobalt in the electrolyte, and cathode current densities. A method of recovering the cobalt from the electrolyte was developed. The possibility of preparing high-purity nickel by this process was shown, as well as the preparation of various cobalt-nickel-tungsten alloys.

Jan 1, 1968

By R. S. Fowkes

Jetstream pressure distributions and coal cutting rates were determined for a number of nozzles and under different operating conditions. The jetstrearn pressure distribution data were fitted to an assumed curvilinear equation by the utilization of a numerical least-squares technique with the aid of a digital computer. Subsequent manipulation of the approximation equation showed that the total force of the jetstream, rather than its maximum pressure or total kinetic energy per unit Lime, was the most significant quantity affecting the coal cutting rate. A shorter method for assessing the ability of a nozzle to cut coal was found.

Jan 1, 1968

By R. J. Leary

This investigation was conducted to determine the effects of various rare-earth metal addition practices upon the macrostructure and the pattern of sulfur distribution in steel ingots. Heats of plain carbon steel were melted in a 1-ton, basic electric-arc furnace. Melts were treated with mixtures of rare-earth silicides, aluminum, and cryolite either in the furnace before tap or in the ladle after tap to determine the effects of this form of rare-earth treatment upon ingot macrostructure. Steels thus treated with rare earths in the furnace were characteristically free of the gross subsurface nonmetallics which typically result from conventional rare-earth treatments. Steel treated in the ladle showed only a few such nonmetallics, and practical techniques were developed for eliminating most of these. Results showed that furnace deoxidation was controlled by the concentration ratio of rare earths: aluminum. During casting, deoxidation was controlled by the concentration of rare earths. Oxygen contents equivalent to vacuum ladle degassing resulted from air-melt furnace treatments with the rare-earth mixtures described. Rare earths in steel inhibited the onset of equiaxed grain formation during ingot freezing, and also virtually prevented interdendritic segregation of sulfides.

Jan 1, 1968

By R. V. Mrazek

The heat of formation of vanadium trichloride was determined at 298.15° K. Measurements were made in a solution calorimeter in which an aqueous hydrochloric acid-potassium dichromate solvent was employed. Data are presented for the heats of solution of vanadium trichloride and the vanadium trioxide "backup" compound, and for appropriate dilution reactions needed to preserve stoichiometry. The resulting heat of formation of vanadium trichioride (VCI3) at 298.15° K was found to be ?H°298.15° K = -138.89 ±0.37 kcal/g mole.

Jan 1, 1968

By Perry N. Halstead

This report describes two goniometers that, by simple manipulation, can be used to ascertain the attitude of a joint, vein, or fracture plane observed on the planar projection of a borehole photograph taken with an NX borehole camera of the type developed by the U.S. Army Corps of Engineers. One goniometer was designed to interpret photographs taken in vertical drill holes and the other for photographs taken in inclined drill holes. In practice, several measurements are made on each photograph with the goniometer. These data are then substituted into mathematical equations, which are derived in this report and the attitudes of fracture planes are determined.

Jan 1, 1968

By M. R. Geer

The Bureau of Mines examined the washability data for 25 Appalachian coals requiring low-density washing to reduce sulfur content to 1 percent, using the distribution-curve method. The purpose was to estimate how closely theoretical sulfur values could be approached, what yields of washed coal could be expected, and the recovery efficiencies that might be achieved. Assuming that the run-of-mine coal would be crushed to 3/8 inch and cleaned in dense-medium cyclones, the calculations indicate that theoretical sulfur contents could be approached closely when cleaning at a specific gravity of separation as low as 1.30. With coals that have favorable specific gravity compositions the recovery efficiency anticipated for cleaning at 1.30 specific gravity is surprisingly high. Similar calculations for cleaning with concentrating tables at intermediate specific gravities indicated that theoretical sulfur contents at 1.50 specific gravity could be approached closely with some coals but not with others. The calculations suggest that operating a table at a specific gravity of separation much lower than about 1.50 probably would be unsatisfactory with most coals.

Jan 1, 1968

By D. J. Bauer

A primary amine extraction system was investigated for fractionating a cerium-group, lanthanide sulfate mixture. Addition of diethylenetriaminepenta-acetic acid (DTPA) to the amine extraction system resulted in separation factors as high as 5.4 for lanthanum-cerium, 8.0 for cerium-praseodymium, 3.7 for praseodymium-neodymium, and 7.0 for neodymium-samarium. In multistage studies on a cerium-free lanthanide mixture, 96 percent of the lanthanum was recovered with a purity of 95 percent.

Jan 1, 1968

By Kenneth J. Miller

To determine the effectiveness of the many new flocculants available to the coal industry 20 of these reagents were evaluated treating slurry feeds to four refuse thickeners. Settling rates and supernatant liquid clarities were determined for each of the flocculants on the four slurries, and zeta potential measurements of the slurry solids were made. The test results showed that the flocculants provided comparable results when judged categorically as anionic, nonionic, or cattonic. It was also apparent that control of zeta potential insures maximum benefit from a flocculant.

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 instructions3 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, 1968

By M. R. Geer

The ever-increasing need to guard against stream pollution has intensified interest in the problems of handling and disposing of flotation tailing. Therefore, the Bureau of Mines investigated the possibility of using crushed washery refuse to adsorb the free water in thickened flotation tailings on a bench scale and then in a pilot plant because the conventional methods of disposing of coal flotation tailings--impounding them or filtering them so they are dry enough to be conveyed to the refuse dump--are sometimes either impractical because of space limitations or costly because of low filter capacity. Most of the refuse samples tested were of similar mineralogical composition and exhibited similar water retention capability. The amount of crushed refuse required to adsorb the water in a particular tailing was influenced greatly by the fineness of the solids in the tailing and hence the percentage of solids to which it could be thickened. The ratio of crushed refuse to tailing solids required to provide a mixture dry enough to be carried on an inclined conveyor belt varied from 2.4 to 6.4. Several chemical agents that were tested were very effective in turning the free water in tailings into a stable gel. Fly ash also was very effective in adsorbing water.

Jan 1, 1968

By B. D. Nash

The object of this research was to investigate the technical feasibility of preparing chromium metal by the thermal decomposition of bisbenzene chromium. Bisbenzene chromium, a pi-bonded sandwich type organometallic compound, was thermally decomposed under reduced pressure to form a metal plate on a heated substrate. Metal recovery was close to 100 percent of theoretical, with deposition rates up to 20.8 mg/hr/cm2. Metal purity was dependent not only upon the purity of the starting material, but also upon the sublimation rate of bisbenzene chromium. Total detectable metallic impurities ranged from a low of 18 ppm to several hundred ppm. In general, metallic impurities were less than 100 ppm. Carbon, the major nonmetallic impurity, ranged from less than 0.3 percent to more than 10 percent. The carbon contamination is most likely a result of the decomposition of the organic portion of bisbenzene chromium. An unusual property of some of the deposits was their outstanding corrosion resistance. Unlike pure electrolytic chromium, which dissolves readily, these deposits were insoluble in hot mineral acids.

Jan 1, 1968

By R. O. Dannenberg

A metallic displacement process, utilizing easily available steel wool or steel window screen, was devised and successfully used for the recovery of silver from waste photographic fixing solutions. Laboratory and prolonged commercial-scale testing established that the iron filament type unit will efficiently precipitate silver, as a high-grade sludge, from acidic waste photographic fixing solutions ranging in grade from less than 1 to over 10 grams of silver per liter. Data and design information are presented to facilitate the construction and operation of a practical unit of any desired size. A smelting process for recovering pure silver from precipitated sludge containing 27 to 80 percent silver was devised.

Jan 1, 1968

By J. L. Reuss

The Bureau of Mines investigated the technical feasibility of smelting copper concentrates containing chalcocite (Cu2S) and native copper using nonpyritic sulfur-bearing materials to aid matte formation. The procedure consisted of combining various proportions of commercial chalcocite concentrate, smelter slag, fluxes, and matte-forming constituents to produce charges of comparable compositions. The mixtures were charged in fire-clay crucibles and smelted in an induction furnace at 1,300° C. The research proved that either sulfur or gypsum can replace pyrite as a matte-forming material, and that gypsum produces an exceptionally high-grade copper matte. The addition of small quantities of metallic iron to the nonpyritic smelting charge furthers the removal of sulfur, improves the recovery of copper, and makes it possible to utilize gypsum as the exclusive flux and matte-forming ingredient, thereby eliminating the necessity of adding limestone.

Jan 1, 1968

By R. K. Koch

The vapor pressures of liquid columbium and liquid hafnium were deter-mined by the Langmuir free evaporation method as a part of the Bureau of Mines program on the study of transition metals. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. Least-squares analyses of the vapor pres-sure data gave the following equations: [Logp (atm) = 5 .429 -31,310 T] for liquid columbium in the range 2,740° - 3,140° K, and [Log p (atm) = 5,690 28 T] for liquid zirconium in the range 2,500° -2,810° K. Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 175.1±3.2 kcal/mole and 148.3±1.2 kcal/mole for columbium and hafnium, respectively. Second-law standard heats of sublimation determined from sigma plots and from sigma-prime plots agreed fairly well with the third-law values. The sigma-prime plots gave standard entropies of sublimation of 30.96±0.84 eu and 33.S6±0.44 eu for columbium and hafnium, respectively.

Jan 1, 1968

By R. P. Adams

Because of the extreme interest in materials with high melting temperatures and the advantages offered over the powder route for making high-density material, arc-melting and centrifugal-casting methods were investigated for preparing shapes of hafnium carbide with and without excess carbon. Highly satisfactory equipment was constructed and efficient operating procedures were established. Also, methods for preparing consumable electrodes and shrink-tolerant graphite molds were developed. Although crack-free hafnium carbide (6.3 weight-percent carbon) shapes were not made, coherent castings containing 9 to 13.5 weight-percent carbon were produced; the same compositions were shown to be resistant to thermal shock. Selected physical and chemical tests were performed on castings chosen for investigation by chemical and nondestructive inspection techniques. Electrical conductivity and thermal expansion measurements were made. Measurable oxidation of all the compositions studied was observed to start between 500° and 600° C. Attack by nitrogen, however, did not occur until temperatures exceeded 2,000° C. A linear relationship of the logarithm of the diamond pyramid hardness to the temperature was noted. Considerable scatter of the bend-rupture strengths at room temperature and of the tensile strengths up to 2,000° C was found. However, at the latter temperature and above, a definite relationship of strength to temperature was observed and some ductility was noted.

Jan 1, 1968

By Philip C. Good

Red mud residue from Bayer process treatment of Jamaican bauxite was dewatered in batch and in continuous centrifuges. Solids content of the residue was increased from its original value of 20 to 25 percent to about 40 percent by centrifuging. Clear effluent amounting to approximately 40 percent of the slurry liquid was recovered containing dissolved alumina and soda values for potential recycle to the alumina plant" Addition of a chemical flocculant to the centrifuge increased capacity by about 35 percent. Manufacturer's estimate of large-scale equipment requirements, based on data collected in this investigation, was that a proposed installation for dewatering 16,000 tons per day of Jamaican red mud would require twenty-two 24-by 60-inch solid-bowl-type centrifuges. Cost analysis of a proposed installation, based on a Jamaican red mud tonnage of 16,000 per day, is included also.

Jan 1, 1968