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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 K. K. Kelley

The heats of formation of two lead vanadates (Pb2V207 and Pb3V208) and manganese vanadate (MnV206) were determined by hydrochloric acid solution calorimetry, supplementing previous Bureau of Mines measurements of the vanadates of calcium, magnesium} and sodium. Heat and free energy data for 11 vanadates were assembled on a common basis. The stability of comparable vanadates (with respect to the oxides) increases in the following order: Magnesium, manganese, lead, calcium, sodium.

Jan 1, 1963

By L. B. Pankratz

High-temperature heat-content values of gallium and scandium sesquioxides were measured over the temperature range from 298° to 1,800° K. The results fill gaps in the thermodynamic information for these compounds; no previous similar data existed. The heat-content values were combined with heats and entropies of formation to obtain free energies of formation of gallium and scandium sesquioxides to 2,000° K. The thermodynamic stabilities of the sesquioxides of aluminum, gallium, scandim, and yttrium were compared.

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 W. L. Anderson

Standard tellurium analytical procedures were modified to obtain the greater sensitivity needed to support a survey of tellurium resources by the Bureau of Mines. Resulting volumetric and spectrophotometric methods for determining tellurium in all types of tellurium-containing materials are described. Sample decomposition and preliminary separations of interfering selenium, gold, and silver are the same in both procedures. The volumetric method is applicable to samples containing a minimum of 10 parts per million of tellurium, In this method the tellurium is reduced to elemental form, and the colloidal suspension is titrated with 0.01 normal iodine solution. The weight of sample for analysis, from 0.25 to 10 grams, should be selected so that the sample contains 0.1 to 5 milligrams of tellurium. To insure accuracy, duplicate samples should be run and the results averaged, particularly on samples of low tellurium content: The limit of determination is 0,001 percent tellurium, which is equivalent to 0.1 milligram of tellurium when using a 10-gram sample. The spectrophotometric method is particularly applicable to low-tenor materials containing from 0.5 to 50 parts per million of tellurium. Up to 10 gram samples are required for making accurate determinations in the low-concentration range. The sample used should contain between 5 and 100 micrograms of tellurium. The turbidity of a colloidal suspension of tellurium prepared from such a sample is determined in a spectrophotometer .t at a. wave-length of 440 millimicrons, and this value is compared with those of standard samples containing known amounts of tellurium.

Jan 1, 1963

By George H. Johnson

This report describes the procedures and summarizes the results of an investigation of surface subsidence above caving blocks at the San Manuel mine, San Manuel, Ariz., in order to obtain quantitative information on subsidence and ground movement caused by mining large volumes of ore. This investigation is one part of an overall study of rock mechanics being undertaken by the Bureau of Mines. Attention was given to the improvement of a rapid and precise method of surveying a large number of subsidence pins and cracks in the surface terrain. Photogrammetric methods were used as an adjunct to the triangulation subsidence surveying as well as in ordinary topographic work Maps of various kinds were prepared to show the results obtained. The computation of the survey notes was programed for an electronic digital computer at a saving of time and expense over the use of a desk calculator and trigonometric tables.

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 W. T. Benson

The nickel-bearing laterite deposits in the Pine Flat and Diamond Flat areas, Del Norte County, Calif., were investigated by the Bureau of Mines to determine the extent and nickel content of the two deposits and the amenability of the ores to metallurgical treatment. The work was based on drill-hole sampling and metallurgical tests in which attrition scrubbing and sizing, reduction roasting, and magnetic separation were used. Results of the sampling indicated that the deposits are comparatively small and are marginal or submarginal in grade. Metallurgical tests showed that no separation of cobalt from nickel and iron was made by sizing; however, a large portion of the chromium was separated. Reduction roasting and magnetic separation did result in upgrading the iron, nickel, and cobalt, and the simultaneous rejection of chromium.

Jan 1, 1963

By F. C. Gibson

An electrical method for the continuous determination of propagation velocities in opaque, confined explosives, and propellants is described. A resistance element imbedded in the reactive material generates electrical signals that are displayed oscillographically and indicate the position and progress of a reactive zone associated with progress of a reactive zone associated with burning or detonation. The method is applicable to both solids and liquids.

Jan 1, 1963

By E. C. Pattee

A mobile spectroscopic laboratory was completed by the Bureau of Mines in 195 to provide a rapid, inexpensive means of field testing samples for beryl¬lium and other associated metals of possible commercial importance. Spectro-copes have been used in laboratories for many years in various types of research and routine analyses, but this spectroscope is probably the first mobile unit. The laboratory provides for spectroscopic, radioactivity, fluorescent, and limited chemical tests of samples. The unit has been a valuable reconnaissance tool. It has been used to search for beryllium, cesium, columbium, tantalum, rubidium, and lithium in Idaho, Washington, and Montana. Several very low grade deposits of these elements were found, and occurrences of other important elements were identified; however, none are of economic importance. The spectroscope permits the detection of elements by analysis of visible light produced when elements in a small powdered sample are volatilized in an electric arc., A total of 70 elements can be detected; 29 can be detected at or below 0.01 percent, Electric power for the arc is supplied by a gasoline motor-driven generator, Equipment is housed in an aluminum van, mounted on a 4-wheel-drive vehicle for easy maneuverability on mountain roads, A trailer with crushing, pulverizing, and splitting equipment permits the reduction of samples to a small representative pulp.

Jan 1, 1963

By B. K. Shibler

A highly flexible laboratory-scale fluidized-bed reactor was designed, constructed, and successfully operated continuously at temperatures up to 1,300° C during an investigation of thermal methods for decomposing gypsum. This report discusses briefly the many problems encountered in developing the 10-inch-diameter reactor and describes its design and construction in sufficient detail to enable other research organizations to build a comparable unit. The reactor consists of a 10-inch-inside-diameter vertical tube which can be varied from 6 to 10 feet high; it is formed from 2-and 3-foot sections of silicon carbide pipe. The tube is surrounded by a 3-inch heating space formed by an outer 4.5-inch-thick circular wall of insulating firebrick. A cone-shaped fluidizing chamber is bolted to the bottom of the reactor. Fluidizing gas enters through the bottom of the cone, and ore is introduced by means of a screw feeder connected to an inlet located just above the gas port. A silicon carbide overflow tube of 1.25-inch inside diameter extends upward into the reactor. The depth of the bed is controlled by substituting different lengths of overflow tube. Twin dust-recovery systems, each composed of a cyclone and Fiberglas filter, are attached to two gas outlets at the top of the reactor tube. The reactor is designed for research on both exothermic and highly endothermic reactions. It can be fired externally by means of four natural gas burners that jet tangentially into the annular space at the base of the reactor. Alternatively, it can be fired internally, using a mixture of air or oxygen and natural gas as the fluidizing medium. A separate instrument panel contains flowmeters, manometers, an automatic program controller, and a multiple-point recorder for printing a record of the temperatures measured by thermocouples located at critical points in the reactor.

Jan 1, 1963

By Frank Parrish

History and performance data of 17 water-injection projects in Cooke and Grayson Counties in north Texas are presented for the purpose of studying and comparing operating practices and oil-recovery techniques. Water is injected into Strawn and Canyon sands of Pennsylvanian age. The principal formation flooded is the Strawn, which ranges in depth from 725 to 6,900 ft in the projects covered. Estimated ultimate recoveries range as follows: Primary, 22 to 494 bbl per acre ft; and secondary; 63 to 296 bbl per acre ft. These figures represent the following percentages of original oil in place: Primary, 10 to 46 pct; and secondary, 8 to 23 pct. Shallower projects; 725 to 1,500 ft in depth, had higher average primary and secondary recoveries than did deeper projects. Crude-oil gravity, which ranges from 20° to 45° API, was not relatable to yield of secondary recovery oil. Analysis of the data indicates that five-spot injection patterns will yield the highest percentage of oil remaining at start of flooding; that is, 28.8 pct for five-spot injection patterns, compared with 20.8 pct for line-drive patterns and 11.6 pct for random patterns. Waterflooding in this area appears to be very successful. Secondary recoveries of most projects are expected to nearly equal primary recoveries.

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 F. D. Stevenson

A metal diaphragm pressure relay system was constructed to measure vapor pressures of the metal halides, oxyhalides, and other substances at temperatures up to 700° or 800° C. The vapor pressure of arsenic (III) oxide (As2O3) was determined to verify the reliability of the apparatus for such measurements. The data for the liquid AS2 Os (2820 to 4830 C) are represented by the equation, log Pmm = 6.875 - 2,929/T, from which the normal boiling point was calculated to be 461° C. The heat of vaporization calculated from this equation was 13.40 ±0.09 kcal/g mole As4OS and is essentially constant over the interval studied. The melting point of the octahedral arsenic (III) oxide was determined to be 278° C from the inter-section of the solid and liquid vapor pressure curves, A thermal analysis apparatus is also described by which melting and transition temperatures could be checked by a method independent of vapor pressure data. The melting points of the monoclinic and octahedral forms were determined to be 314.4 ±1.4° C and 278 ±5° C, respectively.

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