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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 J. Burlin Johnson

This report describes an investigation of the relationship between crater dimensions formed in laboratory blasting experiments and the mechanical properties of the material cratered. Scaled field data have been included when available. The results show that tensile strength and possibly other mechanical properties may be useful in predicting maximum crater dimensions.

Jan 1, 1963

By W. W. Agey

Past investigations on waterborne impurities in the flotation process have been concerned primarily with the treatment of specific ores with particular local waters. Although some anions and cations present in water are known to react with flotation reagents, a definitive study has not been made on the effect of such common ions upon the flotation process. This report describes the fundamental research undertaken to define and measure the adverse and/or beneficial effects of different concentrations and combinations of several common anions and cations when oleic acid is used to froth-float limestone from a pulp of quartz and limestone. Research on the effect of waterborne impurities upon the flotation process was composed of two equally important phases. The first phase comprised development of a procedure for floating limestone from quartz that would give the same results in test after test. Some difficulty was encountered, but once such a procedure was developed, the second phase, comprising study and measurement of the effect of various ions c on to natural water upon the flotation of limestone, was quickly completed.

Jan 1, 1963

By G. S. Scott

The flammability of trichloroethylene vapors in air has been determined in a 7-inch cyclindrical vessel. Saturated flammable mixtures were formed with air at atmospheric pressure between 30° C (86° F) and 82° C (180° F); the trichloroethylene concentrations at these temperatures are 12.5 (lower) and 90 (upper) volume-percent, respectively. Further study is necessary to assess the effects of different variables on the flammability of this material. INTRODUCTION Trichloroethylene (TCE) (ClHC = CCl2), sold under various trade names (Blacosolv, Perm-A-Clor, Tri, Triad, Triclene, Trivec, Tromex, Vapoclean, Vapoclor, Westrosol, etc.), is an important industrial chemical. A summary of its physical and chemical properties is given in table 1. It is used to degrease metals, leather, and textiles, to extract residual oils from vegetable oil cakes, for dry cleaning, and in soap. It is a powerful solvent for fats, resins, bitumens, rubber, sulfur, and phosphorus. Several explosions in which trichloroethylene was involved prompted an investigation by the Bureau of Mines to determine the conditions under which such accidents can occur.

Jan 1, 1963

By W. W. Weller

Heat-capacity measurements of sodium dimolybdate (Na2Mo207) and sodium ditungstate (Na2W207) were conducted over the temperature range from 51° to 298° K. The entropies of the two compounds at 298.15° K were calculated from the heat-capacity values and were used, in conjunction with other entropy data, to evaluate the entropies of formation of the compounds from their constituent elements and oxides.

Jan 1, 1963

By John E. Miller

Supercompressibility factors, Fpv, were derived from experimental compressibility data for five helium-nitrogen mixtures containing from 50 to 100 pct helium. These Fpv values are required as volumetric correction factors for or if ice meter measurement of "crude helium" (helium-nitrogen) purchased by the Government in a program of helium conservation. Although compressibility measurements were made by the Burnett method (2)3 - for pressures from 100 to 3,400 psia and temperatures from 40° to 100° F, Fpv values were needed only for pressures from 400 to 2,000 psia. Consequently, values at increments of 2° F, 2 pct helium, and 10 psia were tabulated only for the required pressure range. Values for pressures outside this range can be calculated from information shown in the tables. Values for the second, third, and fourth coefficients in the equation Z = 1 + BP + CP2 + DP3 are also included.

Jan 1, 1963

By Martin H. Stanczyk

Acid leaching of selected copper sulfide minerals, impure copper sulfide flotation concentrates, and a cement copper precipitate at elevated temperatures and pressures was investigated. Copper extractions of 97 to 99 pct were obtained by leaching chalcopyrite and the flotation concentrates with water under oxidizing conditions at 200° C for 30 to 60 min. In tests with bornite, chalcocite,and cement copper, addition of sulfuric acid or pyrite to the autoclave was required to obtain similar copper extractions. The chemistry of leaching copper minerals was studied. It was determined that different copper sulfides altered to covellite as one step in their dissolution.

Jan 1, 1963

By D. Bienstock

To develop a rugged catalyst capable of withstanding hydraulic attrition resulting from the oil-circulation process for synthesizing liquid fuels, use of an iron catalyst containing an active coating surrounding an inert solid core of metal was investigated. This massive-iron catalyst in the form of steel shot and lathe turnings was activated by partial oxidation with steam at 600° C, impregnated with alkali, and reduced with hydrogen at 450° 6. The massive-iron catalysts were resistant to oxidation and spalling, and a 6-month catalyst life was attained. Higher operating temperatures could be employed than with fused iron oxide catalysts, resulting in greater gasoline yields. Because the lathe turnings pack with void volumes of 70 to 90 percent, it has become possible to employ a fixed bed without the danger of cementation that occurs with fused iron oxides.

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 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 A. S. Peck

This report presents the results of a cooperative study between the Bureau of Mines and the University of Utah to define the mechanism involved in the adsorption of oleic acid and sodium oleate on fluorite, calcite, and barite, using an infrared spectrophotometer for identifying and measuring the adsorbed reagents and reaction products. Fluorite, calcite, and barite react with oleic acid and sodium oleate in a water system, forming chemisorbed and solution products. The chemisorbed species is a surface mineral cation-collector anion salt, Chemical analysis of solution resulting from the adsorption reaction indicates that the adsorption process causes displacement of mineral anions, namely, fluoride, carbon ate, and sulfate from the surface of these minerals.

Jan 1, 1963

By C. M. Mason

Bureau of Mines studies were made on the sensitivity of several ammonium nitrate-fuel oil (AN-FO) mixtures to bullet impact. The experimental work was done with one military rifle and two high-velocity sporting rifles with a variety of ammunition. For the three rifles used, the order of efficiency in initiating detonation in AN-FO mixtures was 220 Swift >300 Weatherby Magnum >30-&apos;06. The velocity of the bullet was found to be a decisive factor in the initiation. The sensitivity of various materials studied increased as follows: Clay-coated prills with 4 percent oil <fresh surfactant-coated prills with 4 or 6 percent oil <surfactant-coated prills with 4 or 6 percent oil and aged 270 days <crushed prills with 6 percent oil <very low-density, surfactant-coated prills (micronized), with 4 percent oil.

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