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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

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 Robert M. Becker

A thick-wall cylinder solution applicable to the evaluation of anisotropic elastic parameters is derived for the interpretation of stress relief data. For a restricted class of problems, a special relationship among certain orthotropic moduli yields stress distributions for the plane orthotropic problem that are identical to the corresponding isotropic case. A ring or hollow cylinder with these specialized anisotropic properties subjected to uniform radial loads is one of the problems in this class. Consequently, known stress solutions are used to develop the strains and displacements for a specialized orthotropic thick-wall cylinder under uniform pressures. The results are consistent with anisotropic equations used in the evaluation of in situ rock stresses.

Jan 1, 1968

By C. I. Pierce

The Bureau of Mines conducted laboratory tests to determine if ultrasonic energy could reduce either the residual water or oil content of petroleum reservoir-rock samples from Appalachian area oilfields. Brine-saturated core samples were flooded with oil to residual brine saturation and subjected to 20 kilocycles per second ultrasonic energy. Then they were flooded with brine to residual oil saturation and again subjected to ultrasonic energy. Additional water displaced as a result of the application of ultrasonic energy to the flow system ranged from 0 to 4.3 percent of the original brine and averaged 1.9 percent. The increase in oil recovery as a result of the ultrasonic energy ranged from 0 to 9.0 percent of the original oil and averaged 3.1 percent. On the basis of the tests, it appears that 20-kcps acoustic waves would not have field application for oil recovery.

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