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By H. G. Iverson

The effects of adding boron and boron plus carbon to electrorefined vanadium were evaluated with respect to mechanical properties at low temperatures and response to heat treatment. Grain size was significantly decreased with the addition of 0.05 percent boron, the decreases ranging from 30 percent at 800° C to 75 percent at 1,100° C. Increasing the boron content resulted in only a small increase in strength at room temperature, but at 77° K, boron contents of 0.005 to 0.076 percent increased the yield strength of vanadium over 50 percent, from 70,000 psi to 110,000 psi. When boron and carbon were present together, the individual grain-refining effects obtained with either element were retained. Approximately a twofold increase in strength was obtained by age-hardening the alloys containing both boron and carbon. Alloys with only boron additions did not age-harden.

Jan 1, 1968

By K. R. Dorman

To develop the potential of precast concrete sets as a support medium in underground mines, a three-piece precast concrete drift set was designed for a small opening and tested to destruction in an underground straining frame. Thirty-six tests were made with three sizes of members using three different loading conditions. In addition, 14 members were tested individually in the laboratory. Test results are compared with theoretical calculations. A cost comparison shows the use of concrete sets would be advantageous where conventional wooden timber requires excessive replacement.

Jan 1, 1968

By John S. Berber

Olefin and paraffin mixtures (C10-C16 and C10-C22) were separated from low-temperature lignite tar by urea adduction and sulfated to yield secondary alkyl sulfate detergents. The C10 ?C16 secondary alkyl sulfate showed a 99.3 percent biodegradability, and the C10-C22 fraction showed a 96.8 percent biodegradability, exceeding the required standard of 80 percent for the biodegradability of anionic detergents in washing and cleaning compounds. Chlorination of paraffins yielded a detergent of 93.2 to 93.4 percent biodegradability.

Jan 1, 1968

By Herbert R. Babitzke

The purpose of this investigation was to optimize the high-temperature properties of columbium and tantalum. Columbium and tantalum were combined with selected alloying elements to achieve solid solution and dispersion strengthening. Fifty-six alloys were evaluated to determine their formability, hardness, strength at elevated temperatures, and oxidation resistance. The following six alloys showed high-temperature strength: [Cb-15Hf-5W-2Zr-4Al-4Ti-2N Cb-15Hf -5W-5Zr Cb-15.3Ti-4.1Zr-13.7Hf Ta-20Hf-4Al Ta-30Hf-4Al Ta-20Hf-5W-4Al] At 1,200° C, the columbium alloys had strength values of 40,000 psi or greater, and the tantalum alloys had strength values from 50,000 to 58,000 psi. For a 2-hour test period at 1,000° C, weight gains of only 9 and 8 mg/cm2, respectively, were observed on oxidation testing of two alloys, Cb-15Hf-5W-2Zr-4Al-4Ti-2N and Ta-20Hf-5W-4Al.

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 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 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 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 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 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 A. F. Colombo

Bench-scale research was undertaken to determine if adding ammonia to cyanide leaching solutions would enhance the extraction of copper from an argillaceous Michigan copper ore. Two leaching techniques, (1) rolling using a tumbling bottle and (2) aerating using a modified Buchner funnel, and variations in pulp temperature; were employed in evaluating the effect of ammonia concentration on copper extraction. Under these experimental conditions, the extraction of copper was shown to be independent of ammonia concentration and entirely dependent on cyanide concentration.

Jan 1, 1968

By E. L. Litchfield

The electrification of ammonium nitrate-fuel oil (AN-FO) blasting agents by pneumatic loaders is described and discussed. The consequences of the electrification are considered in light of the initiation requirements of electric blasting caps. It is recommended (1) that semiconductive loading tubing be utilized and (2) that the resistivity of the AN-FO be controlled; it is further recommended that the operator (3) test to assure continuity of the electric detonator legwire-bridgewire-legwire circuit prior to insertion of the cap into charge or borehole, (4) keep the legwires shunted but not otherwise connected to ground during loading of the blasting agent into the borehole, (5) assure that the borehole is discharged prior to hooking up the detonator leads, (6) assure that he is himself discharged prior to handling the detonator leads, and (7) assure that the blasting cap leads are never carried to the AN-FO loader. The basis and significance of these recommendations are explained.

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

By Manuel Gomez

Bituminous coals having maximum fluidity values in the 40- to 25,400-dial-divisions-per-minute (ddpm) range were carbonized in a continuous, entrained-bed reactor. Carbonization was conducted in an 8-inch diameter, vertical reactor at temperatures from 955° to 1,345° F and at air-to-coal ratios ranging from 4.63 to 16.12 scf/lb of moisture-and ash-free coal charged. Carbonization rates from about 118 to 360 lb/hr, as-carbonized basis, were examined. It was demonstrated that carbonization temperature and air-to-coal ratio must exceed minimum values for continuous operation. Within the operating conditions discussed, highly fluid bituminous coal was carbonized to produce tar and nonagglomerated char. The yield of tar ranged from 21.3 to 38.9 gallons per ton and the char yield ranged from 1,109 to 1,563 pounds per ton, all units expressed on a moisture-and ash-free basis. It was demonstrated that the maximum fluidity and the average size of the coal along with the air-to-coal ratio and the carbonization temperature act together to influence the carbonization product yields and certain properties of the products. Prediction equations were developed from the data for product yields and selected properties of the char, tar, and gas.

Jan 1, 1968

By P. M. Johnson

A design for a laser-powered optical interferometer, using a specimen whose thermal expansion is to be measured as part of the optical system, was conceived and applied in a prototype dilatometer. The object of thin work was the development of an absolute dilatometer capable of use at elevated temperature, particularly above 1,000° C. The prototype has been operated at temperatures exceeding 1,510° C. Results obtained with this device agree within 2.5 percent with the published data for the coefficient of expansion of columbium.

Jan 1, 1968

By M. J. Ferrante

The preparation and subsequent reduction of vanadium trichloride was investigated as a process for the production of high-purity vanadium metal. Chlorine was reacted with vanadium oxide in the presence of carbon to vanadium tetrachloride. The contaminant vanadium oxytrichloride was also formed and later converted to tetrachloride by reaction with chlorine in the presence of activated charcoal. Vanadium tetrachloride was stirred continuously during thermal dissociation to vanadium trichloride powder from which volatile contaminants were removed by distillation. The vanadium trichloride powder was reduced to vanadium sponge by controlled feeding of the trichloride into molten magnesium. Excess reductant and byproduct salt were removed from the vanadium sponge by high-vacuum distillation. Batches as large as 6.5 kilograms of sponge metal were prepared at an average reaction efficiency of 98 percent. Vanadium sponge after consolidation by arc-melting contained 820 to 11330 ppm of interstitial impurities and had a hardness between Rockwell B 40 and 70, This metal exhibited excellent workability at room temperature. The purification of impure vanadium metal by electron-beam melting resulted in lowering interstitial impurities from 1,890 to 504 ppm and hardness from Rockwell B 87 to 28.

Jan 1, 1968

By N. E. Hanna

An investigation was made of pressure pulses produced by unconfined explosive blasts in underground openings. Four tests were made with TNT or modified amatol charges ranging in weight from 60 to 2,000 pounds; each test involved either single or multiple charges. Pressure-time profiles were obtained using mechanical self-recording pressure gages. The cube-root scaling law for peak pressure was found to be valid within about 1 tunnel diameter; at greater distances, the pressures obtained along direct paths were generally higher than this scaling law would indicate.

Jan 1, 1968