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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 A. G. Starliper

Laboratory studies were made to produce whiskers of tungsten over a wide range of operating temperatures. Hydrogen reduction of tungsten hexachloride in a vacuum furnace at temperatures from 2,7000 to 3,3000 C yielded a small quantity of tungsten whiskers, provided a low degree of supersaturation was maintained. Direct measurements of 3,000,000 to 4,000,000 psi were obtained for the ultimate tensile strengths of individual whiskers averaging 3 to 4 microns in diameter with average aspect ratios of 1,000. This compares with strengths of 300,000 to 400,000 psi for 13-micron-diameter commercial filaments.

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 Wilbert T. Malenka

A modified factorial experiment was used to determine the effect of operating factors in hydraulic mining of anthracite. Seven basic factors at various levels were considered. The significant factors were found to be pressure-volume, pattern, and jet traverse speed. Mining data were programed for computer, and a prediction equation was determined from printout information based on the hydraulic "jumbo" operating parameters and characteristics of anthracite, The source of error is discussed. The prediction equation is general in nature and might be useful in delineating performance characteristics in the design of equipment and/or more effective utilization in a medium with characteristics similar to those of anthracite.

Jan 1, 1968

By M. M. Tilman

A series of alloys was laboratory prepared by adding up to 4 weight-percent cobalt to the basic composition of type AM 350 (AISI 633) stainless steel. Aging curves were established for each alloy at 750° F, 850° F, and 950° F for lengths of time up to 100 hours. A series of annealed steels containing as much as 1 weight-percent cobalt was cold-rolled 50 percent and aged for 3 hours at 850° F. No improvement in hardness due to cobalt was observed in the steels transformed by heat treatment. Slight improvements in hardness were observed in the steels transformed by cold working.

Jan 1, 1968

By R. A. Friedel

Data on compositions of natural substances are important in the study of possible interrelationships. The similarity of the low molecular weight alkane isomers from crude oil and Fischer-Tropsch catalytic synthesis product has been reported (8).3 A similar composition for the alkane isomers from high-temperature coal carbonization has been found. The composition of the C4 to C 7 alkane isomers from these three sources can be calculated quantitatively with the equations previously developed to calculate alkane isomers in Fischer-Tropsch product. An KM sting reversal of the concentrations of the monomethyl isomers from C6(2 Me > 3 Me) to C7 (3 Me > 2 Me) occurs in all three products; fragmentary comparisons at higher carbon numbers indicate some dissimilarities. Naphthene isomers in the C6 to C7 range for crude oil and high-temperature coal carbonization also have similar compositions. Aliphatic hydrocarbons from low-temperature coal carbonization processes are considerably different, consisting mainly of normal alkanes.

Jan 1, 1968

By D. J. Bauer

Oxidation of mixed lanthanide solutions with ozone at pH 4.5 and at ambient temperature resulted in precipitation of 98 percent of the original cerium present. Corresponding cerium purity was increased from 50 to 98 percent. A second ozone oxidation-precipitation step produced cerium of 99.9 percent purity in high yield from the 98-percent-pure material. Alternately, ozonation at pH 6.5 and 85° C differentially precipitated cerium and rare-earth elements heavier than cerium and left 89 percent of the original lanthanum in solution at a purity of 95 percent. Subsequent recovery of cerium from the heavier rare-earth elements in the precipitate was accomplished by dissolving the precipitate in dilute mineral acid and reoxidizing the cerium with ozone at pH 4.5 and at ambient temperature. The filtrate contained an enriched praseodymium-neodymium-samarium-europium mixture that is amenable to separation by ion exchange or solvent extraction.

Jan 1, 1968

By Martin Berman

The Bureau of Mines has investigated the mineral matter content of 38 American coals using X-ray fluorescence. Measurements of the Ka intensity for magnesium, aluminum, silicon, sulfur, calcium, and iron permit the determination of those elements as well as an indirect determination of the ash con-tent of the coals. The percentage of each of the six elements was corrected for absorption by all six elements as well as by hydrogen, carbon, nitrogen, and oxygen. It made little difference whether the values used for hydrogen, carbon, and nitrogen were obtained from chemical analysis or whether average values for all coals were used. In all cases, oxygen was obtained by difference. The correction for absorption by all these elements involved the inversion of a 6 X 6 matrix and was performed by computer. Assuming that the elements magnesium, aluminum, silicon, calcium, and iron were present in the ash as oxides, the quantity of ash was determined. The results for the mineral elements as well as for ash and oxygen were in good agreement with chemical results. Particle size was found to have a significant effect on fluorescence intensities. A study of size effects was made for pyrite particles, since the sulfur content of coals is of particular interest. Theoretical equations were derived and verified relating the intensity to particle size. It was found that the coal samples must be ground to less than 2 microns. Sulfur appears in several forms in coal, and the effect of sulfur form on intensity was investigated. It was found that the Ka intensity was independent of sulfur form but the Kß intensity varied with the type of sulfur. Thus, the Ka intensity was used for determination of the quantity of sulfur present. Utilization of the sulfur KB intensity did not permit a determination of the proportions of sulfur forms present in coal. However, for synthetic mixtures of cystine and pyrite in carbon black, measurement of sulfur Ka and Kß permit determination of each constituents from measurements of sulfur intensities alone.

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 John D. Corrick

A dilute sulfuric-acid leach was developed for extracting lead and copper from lead blast furnace mattes and the chemistry was defined. The possible application of Ferrobacillus ferrooxidans to the problem of salvaging lead and copper from blast furnace mattes was also investigated. Operating conditions were varied to determine their effect on the oxidation and hence extraction of lead and copper from the matte. Conditions varied were temperature, pH, reaction time, aeration in the slurry, and particle size of the matte. A set of optimum conditions were developed that resulted in maximum lead and copper sulfide oxidation. Tests employing these optimum conditions resulted in 82.3 percent of the lead and 98.7 percent of the copper being extracted by a dilute acid leach, while maximum lead and copper extracted using F. ferrooxidans was 69.8 percent of the lead and 78.4 percent of the copper. Tests conducted with a different sample of blast furnace matte indicated that the dilute acid leach might have wide application in extracting lead and copper from other such blast furnace mattes.

Jan 1, 1968

By C. M. Mason

Mechanical mining produces large quantities of very fine coal dust called float dust. The associated increase in hazard requires a reexamination of the Bureau of Mines method of evaluating the incendivity of explosives in coal dust-gas-air mixtures. A technique recently developed by Bureau of Mines laboratories for evaluating the incendivity of explosives in coal dust-air mixtures was applied, with modifications, to coal dust-air-natural gas mixtures. A series of permissible explosives were evaluated by this modified technique. Results indicate that the modified technique could be the basis of a more discriminatory procedure than that presently in use.

Jan 1, 1968

By Hillary W. St. Clair

Reaction rate coefficients were determined from analyses of the effluent gas for the reduction of granular ferrous oxide to metallic iron by passing carbon monoxide through a packed bed of oxide at a controlled rate in the temperature range 1,000° to 1,300° C. Coefficients were determined by the comparison of observed analyses and calculated analyses using a mathematical model that takes into account the nonuniform composition of both the solid oxide and the gas. A method is also given for finding the value of the rate coefficient that best fits the observed data.

Jan 1, 1968

By Ronald P. Hollenbeck

Shales in the Appalachian Region of Kentucky and Tennessee were sampled and tested to determine their use as raw materials for the manufacture of lightweight aggregate by the rotary-kiln method. Nine samples were obtained from eastern Kentucky and 143 samples were obtained from eastern Tennessee. As a result of preliminary testing of these samples, two sources in eastern Kentucky and 11 sources in eastern Tennessee were resampled for rotary-kiln tests. The rotary-kiln tests showed the two sources in Kentucky and seven sources in Tennessee contained shale that would produce satisfactory aggregate. Lightweight aggregate processed from these nine sources was tested in concrete shapes and was found to be suitable for use in structural concrete.

Jan 1, 1968

By A. G. Starliper

The Bureau of Mines made laboratory investigations to determine the feasibility of utilizing fine tungsten wires to reinforce a number of nonferrous metals and alloys and a superalloy, S-8l6. The composites of tungsten filament and metals were chosen to attain elevated temperature strength and corrosion resistance. Oriented clean or precoated tungsten wires were incorporated with the other metals by extrusion, swaging, and infiltration casting. Although widely varying characteristics were found in the composites, none were considered satisfactory for high-temperature use, chiefly because of reactions between the matrix metal-tungsten surface. Diffusion, solution, and chemical reactions between matrix and tungsten wires were sufficiently slow for some combinations, such as 15 v/o 8-816, to exhibit increased high-temperature strength for a limited time. A few metals failed to wet or bond to the tungsten surfaces, while a few responded after precoating with a third metal.

Jan 1, 1968

By D. E. Wolfson

The Bureau of Mines carbonized 21 coal samples from Fayette, Greene, and Washington Counties, Pa., at 900° C, using the Bureau of Mines-American Gas Association (BM-AGA) method, and determined yields of products and physical properties of the coke. These samples represented high-volatile A Pittsburgh, Sewickley, Waynesburg, and Upper Freeport and medium-volatile Upper Freeport and Lower Kittanning coals. About 20 percent of all coals presently carbonized in commercial coke ovens in the United States are mined in Greene and Washington Counties, principally from the Pittsburgh seam. Sulfur content of the Pittsburgh coals in these counties is moderately high (1.0 to 3.2 percent) but, because of extremely large reserves, accessibility to eastern United States markets and excellent blending characteristics to yield strong coke, these counties will continue to be an important source of metallurgical coals in the future. Most coals from the other seams contained more than 2 percent sulfur, which would limit their use as metallurgical coals.

Jan 1, 1968

By Henry G. Dorsett

Dust explosion data obtained in laboratory tests by the Bureau of Mines are presented for 73 chemical compounds and mixtures, 29 drugs, 27 dyes, and 46 pesticides. Information is given on ignition temperatures of cloud and layer, minimum igniting energy, minimum explosive concentration, percent of inert dust required to prevent flame propagation, limiting oxygen concentration in the atmosphere to prevent ignition, and pressures and rates of pressure rise at dust concentrations of 0.1, 0.2, 0.5, 1.0, and 2.0 ounces per cubic foot. Explosibility indexes are computed where data are available to permit comparison of the relative explosion hazard. Variations of explosibility parameters with chemical composition are discussed. General means for minimizing the dust explosion hazard are reviewed.

Jan 1, 1968

By Basil Dimitriades

Five recently developed methods for determining nitrogen oxides in automotive exhausts have been evaluated from the standpoint of accuracy and applicability in current exhaust studies. Results showed that methods requiring conversion of nitric oxide to nitrogen dioxide as a part of the analytical procedure are subject to errors introduced by the instability of NO2. The extent of some of these errors has been determined and procedures have been developed to minimize undesirable influences. On the basis of the results obtained from this study, recommendations are made regarding procedures for batch type or continuous measurement of nitrogen oxides in exhaust streams.

Jan 1, 1968

By R. B. Tippin

Research investigations conducted on five ore samples show the applicability of heavy liquid separation (HLS) techniques to mineral processing. Under proper operating conditions, semicontinuous tests in small fluid cyclones yielded 90 percent sink-float concentrates with recoveries exceeding 90 percent on minus 35-mesh ore samples of kyanite, potash, spodumene, fluorspar, and beryl. Although none of the ores were examined in detail, their response to this novel concentration method provides basic examples that are typical of the process. Various aspects of cyclone design and operational characteristics of heavy liquid cyclone circuits were studied which demonstrated the flexibility of HLS by using multiple units connected in series. A comparison of two heavy liquid solutions, tetrabromoethane and methylene bromide, exhibited their individual advantages and limitations. Unique problems relative to this process are discussed including liquid viscosity, mineral composition of the ore, toxicity, and material handling hazards.

Jan 1, 1968

By Jerry L. Huiatt

An accurate and reproducible procedure was developed using the gas-liquid chromatograph to quantitatively measure oleic acid on flotation products and in flotation water phases. The method comprised extraction of the oleic acid from the mineral surfaces with alcoholic NaOH, esterification of the extracted oleate, and chromatography of the methyl ester with an internal standard. Quantitative analysis of oleic acid on flotation products from test tube and bench-scale flotation tests with pure minerals and with natural ores proved the applicability of the method on a variety of minerals. The accountability of oleic acid added was 100 percent, ±5 percent.

Jan 1, 1968

By Ted C. Briggs

Equations for the elastic pressure distortion of the volumes of a Burnett compressibility apparatus are developed and presented in this report for volumes under internal and external applied pressures. An experimental method for the determination of the external pressure distortion coefficients is presented. Young?s modulus and the internal-pressure distortion coefficients are computed from the experimentally determined external-pressure distortion coefficients. The temperature dependence of the pressure distortion coefficients and of Young's modulus is evaluated for the temperature range 0° to 80° C.

Jan 1, 1968