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By T. A. Henrie

A technique was devised for measuring the rate of chemical reactions between reactive metals and molten-salt mixtures at high temperatures. The rate of the heterogeneous reaction between high-purity titanium metal and titanium trichloride in molten sodium chloride was determined. The reaction is surface-controlled, and the heat of activation is 8.29 kilocalories per mole TiC13. An active site or reaction nuclei is created by adsorbing a TiC13 molecule at the metal surface. Reaction of the second TiC13 species forms an activated complex that decomposes into three TiC12 molecules.

Jan 1, 1963

By James H. Gary

Data regarding the composition and physical properties of Florida land-pebble phosphate-waste slime are presented, and the feasibility of dewatering and beneficiating the slime by several different methods is discussed. Chemical analyses, electron micrographs, and X-ray diffraction data showed that principal constituents of the slime included quartz, attapulgite, and flaorapatite. Viscosity of the slime changed with pH; thixotropic, Newtonian, and rheopectic states were observed as the pH increased. Use of various flocculating agents was not effective in improving thickening properties of the slime. Dewatering tests using pressure filtration showed that temperature influenced the filtration rate more than pressure; the filtration rate at 165° C was tenfold that at room temperature. Selective flotation of the slime, using two different processes, gave promising results. About 25 pct of the phosphate was recovered in a concentrate assaying 31 pct P205, Other tests demonstrated that the slime could be successfully fractionated at 20-microns using a hydrocyclone. In hydrometallurgical tests about 80 pct of the phosphorus and alumina were chemically extracted from the slime using sulfuric acid. Limited bacteriological studies made of the slime showed that several types of microorganisms were present and grew in the material despite the presence of fluorine-bearing minerals.

Jan 1, 1963

By G. T. Krempasky

In an attempt to develop a suitable precast concrete support for underground use, two different models (1955 and 1958) of a five-piece concrete set were designed, fabricated, and tested under adverse loading conditions. Model 1955 was designed to withstand an ultimate, uniformly distributed, vertical load equivalent to what a three-piece, 12- by 12-inch wood set of intermediate-grade Douglas fir would withstand. A design figure of 138,000 pounds for the vertical load was used on both the 1955 and 1958 models. In addition, the 1958 model was designed to withstand a uniform horizontal load of 7,000 pounds per foot and additional concentrated-point loading. The step- by-step design of each model is presented in the appendixes. A series of five destruction tests was conducted underground on the 1955 model, and results of the tests showed that the type and method of blocking were of major significance.

Jan 1, 1963

By William C. Miller

This report describes investigations by the Bureau of Mines designed to establish the noise level and spectrum of various types of pneumatic rock drills and to furnish information that would be useful in conducting sound measurements in mining environments and in reducing the noise generated in pneumatic drilling. These investigations show that (1) the noise generated by the drills in the frequencies below 100 cps is caused by the impact of the piston and drill steel, in the frequency range between 100 and 2,000 cps by the exhausting of air from the ports, and in the frequencies above 2,000 cps by the resonant frequencies of steel drill parts and of drill steel; (2) satisfactory instruments and instrumentation systems are available for field and laboratory measurements; (3) reliable sound measurements can be made in mining environments; and (4) devices can be developed that will abate the noise.

Jan 1, 1963

By W. E. Robinson

Samples of raw oil shale and kerogen concentrates were oxidized by alkaline potassium permanganate, air, nitric acid, oxygen, and ozone to obtain information about the chemical structure of organic kerogen in oil shale. In one test, oil shale and oil-shale products were oxidized exhaustively with alkaline potassium permanganate, and the distribution of the organic carbon in the final oxidation products was determined. Comparing results of this oxidation with those obtained from other carbonaceous materials and known compounds gave information about the structure of kerogen. Alkaline potassium permanganate oxidation also was used partly to degrade kerogen into soluble products for characterization purposes. Structures present in these degradation products were indicative of type structures originally present in the kerogen. Nitric acid, oxygen, and ozone were used also for partly degrading kerogen to soluble oxidation products. Carbon-balance oxidation tests using alkaline potassium permanganate showed that Colorado oil-shale kerogen differs from many other carbonaceous materials such as coal and kerogens from other areas. Composition of the degradation products indicated that Colorado oil-shale kerogen is predominantly cycloparaffinic and saturated heterocyclic structures with some long-chain paraffinic and aromatic structures present. The ring systems may be connected through short carbon chains or bridges containing oxygen, nitrogen, and sulfur.

Jan 1, 1963

By Laird Crocker

This report describes a study of beryllium recovery from sulfate leach liquor by di-2-ethylhexyl phosphate (EHPA) solvent extraction in conjunction with caustic stripping. The work was one phase of Bureau of Mines research on process development for Spor Mountain, Utah, ores. Solution for the solvent extraction studies was prepared by sulfuric acid leaching of ore containing 0.6 pet BeO, Before solvent extraction of beryllium, the leach liquor was treated to prevent coextraetion of iron by either (1) removal of ferric iron by amine solvent extraction or (2) reduction of ferric iron to nonextractable ferrous iron by treatment with sulfur dioxide. Beryllim was extracted from the aqueous leach liquor by countercurrent multistage contacting with a kerosine solution of EHPA. The loaded organic solution was stripped with sodim hydroxide solution. Subsequently, beryllium hydroxide was precipitated by boiling the sodium beryllate strip solution and converted to beryllium oxide of 98 pct BeO-grade by calcining. Material of this grade can be directly processed into beryllium-copper alloy or be used as starting material for further refining to produce high-purity, nuclear-grade beryllium. Over 90 pct of the beryllium contained in the leach liquor was recovered as beryllia.

Jan 1, 1963

By Sara Jane Boles

The purpose of this Bureau of Mines investigation was primarily to isolate and examine the effect of liquid content upon the apparent porosity and bulk density of compacts pressed from high-purity, fused aluminum oxide, and, secondarily, to study the actual mechanism by which the liquid content affects the bulk density. No attempt was made to approach the theoretical maximum density of the oxide by introducing additives, particle packings, or similar variables; instead this study is an intercomparison of the bulk densities obtained as functions of the water contents of the compacting mixtures. Water content was varied from 7 percent to 25 percent, on a total-weight basis. The data gathered indicated a well-defined optimum water content for obtaining minimum apparent porosity and maximum bulk density, under the conditions of the experiment. During the course of this study, a number of additional variables in the forming process were discovered and are introduced in this report, although a thorough evaluation was found to be beyond the scope of this present investigation.

Jan 1, 1963

By Lloyd Carpenter

Eighteen elements were determined spectrochemically in vanadium metal and its compounds in the general range of 1 to 1,000 ppm by means of spark-ignited unidirectional arc excitation. The samples were converted to vanadium pentoxide and combined with a mixture of graphite, lithium carbonate, and gallium oxide. For the molybdenum determination, the oxidized samples were mixed with sodium chloride and packed in copper electrodes. Average precision of the method was 15.6 percent relative standard deviation and relative error was 4.4 percent.

Jan 1, 1963

By P. R. Tisot

Knowledge acquired from this research contributes to a better understanding of the physical structure of Green River oil shale and provides fundamental data and concepts that may serve to improve oil-shale technology. This study by the Bureau of Mines indicates that oil shale is a highly consolidated organic-inorganic system with no significant micropore structure, pore volume, or internal surface. This system is a form of physical structure that precludes rapid diffusion of either gases or liquids. The mineral matter consists essentially of nonspherical particles that tend to follow a log-normal size distribution. An excess of 99 weight-percent of these particles have equivalent spherical diameters of less than 44 microns--75 weight-percent are from 2 to 20 microns, and 15 weight-percent are less than 2 microns. The surface area (3 to 5 square meters per gram) of these mineral constituents is mainly external surface. The mineral constituents contain some micropore structure--pore radii ranging from 10 to 100 Angstrom--with the pore sizes randomly distributed. Distribution of the organic matter within the inorganic matrix is essentially interparticle and not intraparticle. The organic matter within the micropores of the mineral constituents is less than 4 percent of the total. Estimates made from surface area data suggest that perhaps only a small amount of the organic matter is bonded either physically or chemically to the mineral constituents.

Jan 1, 1963

By James S. Browning

The Bureau of Mines conducted laboratory batch and small-scale continuous selective flotation tests of barite-fluorspar ores from two deposits near Marion, Ky., to determine the technical feasibility of recovering commercial grade fluorspar and barite concentrates. The lignin sulfonate-sodium fluoride method of floating the fluorspar successfully produced acid-grade fluorspar concentrates. Flotation of the barite from the fluorspar tailing using petroleum sulfonate collector yielded concentrates suitable for use in compounding oil-well drilling mud. The fluorspar and barite recoveries were about 82 and 85 percent, respectively.

Jan 1, 1963

By Kenneth G. Broadhead

Four applications of radiotracer techniques in metallurgical research are described: (1) In electrowinning tungsten from scheelite, molybdenum 99 was used to detemine the molybdenum concentration of the fused alkali-phosphate bath and the electrowon tungsten; (2) an attempt to detemine the solubility of tagged ceric oxide in molten CeF3-BaF2-LiF was unsuccessful, but a high rate of cerium ion exchange was observed; (3) iron 59 was added to cerium during casting and used to follow the migration of iron during solid state electrolysis; (4) radiotracers were used in developing special analytical techniques applicable to high-purity rare-earth metals produced by molten salt electrolysis.

Jan 1, 1963

By R. F. Zaffarano

Reservoir oil in the Greater Aneth area, Utah, part of the Paradox basin, was studied to detect variation in oil characteristics within the reservoir and to determine its relation to age of accumulation and fluid equilibrium. At least three subsurface oil samples were obtained from each of the four largest of five field divisions comprising a producing area of 45,000 acres. Height of the oil column in the Pennsylvanian Desert Creek zone is about 230 ft. In general, the oil characteristics were found to be uniform across the area, and averages were developed for use in engineering applications. Average saturation pressure was 1,780 psia; the oil was undersaturated at the initial reservoir pressure, 2,200 psia. Variation in saturation pressure shows a lack of complete fluid equilibrium and continuing diffusion of solution gas from the main body of the reservoir to two extensions linked by narrow arms. By assuming early accumulation, the time involved in this diffusion process was calculated to be about the same as the age of the reservoir formation. Cause of the concentration of gas in the main body is attributed to differential entrapment during accumulation of oil and gas from an exterior source.

Jan 1, 1963

By P. A. Wasson

The investigation described in this publication was conducted by the Bureau of Mines to determine the effectiveness of the anionic silica flotation method on goethitic iron-bearing materials from the Cuyuna Range, Minn. Samples used in this investigation were a composite of drill core from 13 holes, and 3 samples from lean ore stockpiles. These samples are believed to be typical of the mineralization occurring in an area with a potential reserve of several million tans of submarginal iron ore. Results from batch tests showed that the iron-bearing minerals could be effectively concentrated by flotation removal of the siliceous gangue. The drill hole composite yielded laboratory flotation concentrates from locked tests containing 56.8 percent Fe and 6.1 percent silica, with an accompanying iron unit recovery of 94.2 percent. Concentrates containing 52.4 to 53.7 percent Fe also were produced from the lean ore stockpile materials; corresponging iron recoveries ranged from 71 to 79 percent in the batch tests, with the possibility remaining for additional recovery of iron from the middlings.

Jan 1, 1963

By Raymond L. Carpenter

The thermal conductivity, electrical resistivity, and Seebeck coefficient for nine compounds, based on the formula for enargite Cu3AsS3, were measured in a search for efficient materials to be used in thermoelectric generators or refrigerators. Results indicate that one of these compounds, Cu3SbSe4, has thermoelectric properties approaching those of bismuth telluride. An investigation of the effect of adding small quantities of tellurium to Cu3SbSe4 and Cu3SbS4 in order to improve their properties also was made. A figure of merit of 2.1 x 10-4 °C-1 was obtained for Cu3SbSe4 + 0.1 percent tellurium.

Jan 1, 1963

By A. C. Rice

Aminopolyacetic acid chelating agents were added to separatory-funnel-scale solvent-extraction systems to determine the effect on separating rare-earth elements. Average values for separation factors between adjacent elements obtained with Primene JM-T2 increase 36 percent when EDTA is added to the aqueous phase. Adding HEDTA or DCTA also improves separation factors for certain rare-earth elements. Percentage of extraction and the separation factors exhibit marked sensitivity to concentrations of amine, chelating agent, and hydrogen ion. The chelating agents improved separation in Primene JM-T, BHDA, and Primene 81-R extraction systems.

Jan 1, 1963

By Hal J. Kelly

A number of problems that developed in processing the halloysitic clays of eastern Washington and northern Idaho were investigated by the Bureau of Mines. The deflocculating effect of tetra sodium pyrophosphate is compared with several other compounds, and on the basis of current theory, the advantage of sodium pyrophosphate as a deflocculating agent is explained. The adsorption of the sodium ion by clay in a clay"-water system was established by a radioactive tracer technique, and the deflocculating action of sodium pyro- phosphate was postulated. The effective dispersion of the halloysitic clays was limited by the occurrence of tightly bound aggregates of small, individual crystals. Disaggregation of the agglomerates was investigated by liquid extrusion and ball milling of dilute slurries and by extrusion of the clay in a plastic state. The greatest increase in the production of small particles was by high? pressure liquid extrusion.

Jan 1, 1963

By P. A. Bloom

Bureau of Mines research was conducted to develop effective separation methods that might be used in exploiting substantial tonnages of complex barite-fluorspar ores in Arizona. The exploitable reserves now may be increased as recent batch and continuous flotation tests demonstrated that a complex barite?-fluorspar ore from the Red Chief deposit, Yuma County, Ariz., could be selectively treated to concurrently produce (1) fluorspar and (2) a barite byproduct of marketable grade. The sample contained 24.8 percent CaF2 and 24.3 percent BaS04. Processing comprised production of a fluorspar product containing 97 percent CaF2 with an 82 percent recovery, using a sodium fluoride-lignin sulfonate-fatty acid reagent combination. Concurrent retreatment of the fluorspar tailing, using sodium cetyl sulfate as a collector, yielded a barite product of 94 percent BaS04 grade with a 71-percent recovery. The products met specifications for acid-grade fluorspar and drilling mud-type barite.

Jan 1, 1963

By Robert V. Berryhill

Reconnaissance studies of beach deposits along approximately 220 miles of the shoreline of Bristol Bay, Alaska, were made to determine if more detailed investigations were warranted. In addition to preliminary mapping of the deposits, samples were obtained from auger borings spaced at 1-mile intervals in key areas; shovel samples were collected to supplement the borings. Most samples were roughly concentrated in the field; magnetic separation tests, petrographic analyses, and determinations for radiometric equivalent uranium, gold, platinum, iron, and titanium were made in the Bureau of Mines laboratory at Juneau, Alaska. Spot samples from some beaches along the shores of the Alaska Peninsula indicate small deposits containing up to 10 percent recoverable titaniferous magnetite; some larger deposits were indicated to contain from 1 to 2 percent total heavy metal, principally as titaniferous magnetite. Significant amounts of other commercial minerals were not detected.

Jan 1, 1963

By W. A. McKinney

Bureau of Mines Research has demonstrated that it is technically feasible to segregate oxidized copper ores by use of a direct-fired, refractory-lined rotary kiln. Previously, the segregation process had been effected only in much more complicated indirect-fired, stainless steel kilns, The method comprises heating crushed ore premixed with small quantities of salt and carbonaceous material, such as coke, to about 830° C to produce copper as fine flake and metallic films on the surface of the coke particles. After grinding of the cooled furnace calcines, the copper is recovered by conventional flotation. During direct-fired segregation it was necessary to closely control the air-gas mixture in the burner. Good copper recoveries were obtained only when adding air in the limited range of 1.15 to 1.2 times the theoretical amount required for combustion of the natural gas. Batch trials of the new technique on quartzite-, limestone-, sandstone-, and limonite-type oxidized copper ores containing from 1.4 to 6.2 percent copper yielded flotation concentrates containing from 3.7 to 45 percent copper, representing 84 to 95 percent recoveries. Analyses of the furnace gases showed that loss of copper by volatilization was negligible. The preliminary direct-firing segregation studies were complemented by continuous runs on the quartzite ore, containing 1.4 percent copper, in an integrated segregation-flotation pilot plant having a 60 pound-per-hour capacity. In a typical test, 84 percent of the copper was recovered in a cleaner flotation product containing 25 percent copper. The study will be continued to further delineate the conditions for good segregation as effective use of standard ceramic-lined kilns will render the process more attractive from a commercial standpoint.

Jan 1, 1963

By Scott W. Hazen

This Bureau of Mines report presents the results of a study and statistical analysis of part of the initial exploration churn-drill sampling and some of the subsequent underground diamond-drill-core sampling in the North are body at the San Manuel copper mine, Arizona. These data were derived from regular exploration and mine sampling, not from special samples obtained solely for statistical analysis. The study was conducted as part of the Bureau's continuing program on sampling-methods research. The major objective of the study was to investigate the feasibility of using the techniques of statistical analysis in evaluating sample and assay data and computing grade and tonnage of Ore from porphyry-type copper deposits. It was recognized that using existing data acquired over a period of several years by different methods would introduce problems and limitations for precise comparisons. However, it was expected that the study would provide some general conclusions and certainly a number of preliminary conclusions on the nature of the mineral characteristics and their effect on sampling procedures, the requirements for sampling deposits of this type, and the comparative results of churn-and diamond-drill sampling in the same area of the deposit. All of this information would be essential for future sampling-methods research for computing grade and tonnage of ore.

Jan 1, 1963