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By R. O. Dannenberg

Applicability of the fluosilicate sintering process to recovering beryllium from beryl-spodumene concentrate analyzing 1.4 to 3.7 percent BeO (10 to 30 percent beryl) was investigated. The work was one phase of a Bureau of Mines research program undertaken to assess applicability of conventional processes and to devise new procedures for treating various potential beryllium feed materials. Beryllium recovery of about 70 percent in a product of 99-percent BeO grade was achieved in treating 3D-percent beryl concentrate. The process consisted of (1) sintering a briquetted charge of concentrate, soda ash, and sodium fluosilicate for 3 hours at 750° C.; (2) extracting the soluble beryllium by multiple stages of water leaching; (3) adding caustic to the leach solution and boiling to hydrolyze and precipitate crude beryllium hydroxide; (4) dissolving the crude beryllium hydroxide in sulfuric acid and separating the solution from undissolved silica; (5) sulfidizing the acid beryllium solution to precipitate heavy metal impurities; (6) adding ammonia to the clarified sulfate solution to precipitate beryllium hydroxide; and (7) converting the hydroxide to beryllium oxide (beryllia) by calcining at 900° C. About 60 percent more sodium fluoSilicate was required per unit of beryl than is used industrially in treating 10-to 12-percent BeO concentrate (80 to 90 percent beryl). Recovery decreased, and flux requirements increased, when treating concentrates containing less beryl.

Jan 1, 1963

By F. R. Cattoir

This report presents the results of preliminary studies for the evaluation of some fused-salt electrolytes for refining tungsten metal, and describes the equipment used. Some impurities could be eliminated with electrolytes composed of sodium chloride, sodium iodide, or sodium tetraborate in combination with tungstic oxide or sodium tungstate. Electrolytes composed entirely of chlorides were unusable because of the volatility of tungsten chloride. Refining 96-to 98-percent tungsten to produce a commercial grade was more successful than further refining of 99.9-percent tungsten. No electrolyte tested yielded a product pure in all respects. Electrolyte temperatures of about 900° C were necessary to maintain a good dissolution rate at the anode and acceptable cell operation. Cathode current densities at the beginning of a deposition cycle were limited to approximately 1 ampere per square inch. Higher current densities resulted in a finely divided product that frequently failed to adhere to the cathode. The most conspicuous impurities in the tungsten produced were carbon, iron, and molybdenum; the former two came from the iron cell and the graphite cell liner. Electrolytes com-posed of tungstic oxide or sodium tungstate in sodium iodide, or 2Na, 0.B203, were capable of producing tungsten carbide.

Jan 1, 1963

By James R. Welty

Heat content values were experimentally determined for yttrium metal between temperatures of 400° and 1,300° K and for iron pentacarbonyl between 301° and 380° K. The drop technique was used; that is, a sample of material sealed in a protective capsule was heated to 3 desired temperature in a furnace and then dropped into an ice calorimeter. A revised technique for determining heat content values from calorimetric data is described. Heat content and corresponding entropy-increment data above a reference temperature of 298.15° K are presented in tabular form. Equations for heat content and heat capacity as functions of temperature were derived for each substance. These equations are [Y (c): HT-H298.15 = 1.2041T 1 3.393 x 10-3T2- 0.4176 x 10' T"1 + 739.9 cal/mole Cp = 1.2041 + 6.786 x 10-3T + 0.4176 x 106-T-2 cal/deg mole Fe (CO) E, (1) : HT - H298.15 = 55.636T - 16,588 cal/mole Cp = 55.636 cal/deg mole]

Jan 1, 1963

By R. O. Dannenberg

Exploratory research was conducted to ascertain the feasibility of recovering beryllium from Spor Mountain, Utah, ore by the sodium fluosilicate (Na2SiF6) method used industrially for processing beryl. Na2SiF6 requirements to form water-soluble salts of beryllium were determined for three different samples--two clayey ores containing 0.6 and 1.3 pct BeO, respectively, and a calcareous ore containing 0.6 pct BeO. The ores were sintered with Na2SiF6 at 750° C for 3 hours. About 80 pct of the beryllium was rendered water soluble by sintering the 0.6-pct BeO ores with 30 and 40 lb Na2SiF6 per lb BeO contained in clayey and calcareous ores, respectively. The higher grade 1.3-pct BeO clayey ore required only 20 lb Na2SiF6 per lb BeO to solubilize over 80 pet of the beryllium. As the 0.6-pct BeO clayey ore was possibly the most representative of the deposit as presently delineated, leach liquor prepared from this sample was treated to recover beryllium salts. About 60 pet of the beryllium contained in the ore was recovered as beryllium hydroxide, which then was calcined to yield a 99-pct BeO final product by means of the following operations: (1) Sintering with Na2SiF2, (2) leaching with water, (3) precipitating crude Be(OH)2 by adding NaOH, (4) filtering to separate the hydroxide from the NaF solution, (5) redissolving the crude Be(OH)2 in excess NaOH, (6) filtering to reject caustic-insoluble impurities, and finally (7) boiling the Na2BeO2 filtrate from (8) to precipitate pure Be(OH)2. Reagent consumption was 49 lb Na2SiF6 per lb BeO recovered and 17 lb NaOH per lb BeO.

Jan 1, 1963

By A. R. Taylor

Low-temperature heat capacities of cesium chloride (7° - 300° K) and cesium iodide (13° - 300°K) were measured with an adiabatic calorimeter. The heat-capacity measurements were analyzed graphically to determine smooth values of heat capacity, entropy, enthalpy function, and free-energy function at 10° K intervals and at 273.15° and 298.15° K.

Jan 1, 1963

By Richard F. Hewlett

The mining industry utilizes a vast store of knowledge, wisdom, and engineering talent in designing mining systems. However, the complexity of the required systems and the presence of numerous variables frequently necessitates raking important decisions without having adequate accurately detailed information. That many of the decisions made in the past were nearly correct, in the long run, is substantiated by the number of successful mining enterprises that exist in the world today. Subsequent to 1940, the disciplines of operations research and systems engineering were developed. The disciplines have produced methods of providing better information to persons responsible for making decisions.

Jan 1, 1963

By P. T. Brooks

The selective recovery of nickel and cobalt from impure raw materials is being investigated by the Bureau of Mines as part of a program to develop improved procedures for preparation of pure metals. A combination solvent extraction-electrolytic process has been developed in the laboratory that enables preparation of high-quality nickel and cobalt from nickel oxide containing, in percent, 76 nickel, 0.8 cobalt, 0.5 magnesium, 0.2 iron, and lesser quantities of copper, zinc, and other metals. The oxide was smelted, using carbon as reductant, and cast into anodes. These anodes subsequently were dissolved in diaphragm-type electrolytic cells. Nickel and cobalt were deposited separately from appropriate electrolytes, concurrent with dissolution of the impure anodes. Anolyte containing nickel and cobalt in the form of chlorides and sulfates was treated for removal of impurities and separation of nickel and cobalt. First, iron and aluminum were removed as hydroxides by adding nickel hydroxide to raise the pH of the anolyte from 2.3 to 4.5. Next, the pH was adjusted to 2 by adding hydrochloric acid, and the solution was treated by solvent extraction to separate nickel and cobalt.

Jan 1, 1963

By Charles Prasky

This report describes and appraises recent progress in the development of a differential sulfatizing process for recovering a ferrograde manganese oxide from low-grade manganiferous ferruginous materials in the Cuyuna range. Individual process steps were carried out successfully using a 20-inch-diameter shaft for continuous countercurrent sulfatization of the manganese, a multiple-compartment rotary drum for leaching the water-soluble manganese sulfate, a submerged-combustion evaporator for the recovery of monohydrate crystals of manganese sulfate, and a shaft furnace for the thermal decomposition of sulfate crystals for production of a ferrograde manganese oxide and a sulfur dioxide gas suitable for sulfatization of fresh are. Of the two general kinds of Cuyuna manganiferous materials--the carbonate slates and the oxidized ores--only the slates were studied at pilot scale.

Jan 1, 1963

By M. M. Wong

Electrolysis of titanium carbide and a material consisting of titanium, carbon, nitrogen, and oxygen as soluble anodes in Used electrolytes was investigated by the Bureau of Mines for the preparation of crude titanium metal. Tests made in all-chloride electrolytes showed only a low recovery of titanium as well as a substantial volatilization of titanium trichloride (TiC13) when present in the electrolyte. Electrolysis at 750° to 850° C in a mixture containing 85 percent NaC1-15 percent potassium floutitanate (K2TiF6) yielded as high as 91 percent recovery of titanium from titanium carbide and 62 percent recovery of titanium from the titanium-carbon-nitrogen-oxygen material. Problems associated with the preparation of crude metal by fused-salt electrolysis are discussed. The crude metals produced from both anode materials were electrorefined in a sodium chloride-titanium chloride (NaCl-TiC12) electrolyte, and ductile titanium metal was obtained.

Jan 1, 1963

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 M. E. Hawkins

Mineral analyses and electrical resistivity measurements of 324 representative samples of oilfield brines from 24 oil-productive counties in Mississippi and Alabama are presented in tabular form. Results of the mineral analyses, which include calcium, magnesium, carbonates, bicarbonates, sulfates, chlorides, sodium, and barium (with strontium if present), are reported in milligrams per liter. Electrical resistivity measurements in ohm-meter2 per meter at 75° F are reported in ohm-meters in the tables. Chemical analyses of formation waters are helpful to operators having water problems associated with petroleum recovery; electrical resistivity values are helpful in making interpretations from electric logs.

Jan 1, 1963

By David J. Kusler

A gravimetric method for the determination of carbon dioxide, carbon monoxide, hydrogen, methane, and oxygen in blast furnace top gas is described. Nitrogen may be determined directly by volume measurement or by difference. The method is direct, permits continuous as sampling, and provides an averaged analysis over a selected range of sampling intervals from 1/2 to 24 hr or more. Neither expensive equipment nor specialized personnel are required. The method is suitable for routine analysis, and the results compare favorably with those obtained by established methods.

Jan 1, 1963

By Albert J. Rambosek

The results obtained in a study of the stress conditions existing in a drill bit-point area and in the underlying rock, when the bit was in full but nonpenetrative contact with the rock, are presented. This investigation by the Bureau of Mines was the preliminary exploratory phase of a long-range program of research on rock drilling to establish criteria for the maximum economically feasible rate of rock penetration. The photoelastic technique of experimental stress analysis was the principal method used to obtain the data. Transparent models and transmitted light were employed to investigate patterns in drill-bit models and isotropic materials under the bit when subjected to a concentrated static load. Comparative stress data for anisotropic rock were obtained by the reflective photoelastic technique. Brittle lacquer and an extensometer were used obtain supplementary information wherever substantiating data were desired to check photoelastic results. The zone of maximum shear occurs along an arc near the contact face of the bit. The stress distribution pattern in an isotropic model rock near the area contacted by the bit was nearly a mirror image of that exhibited within a similar areal zone of the bit. The stress pattern in granodiorite specimens was similar, though not symmetric, to the pattern in the isotropic model rock. The asymmetry of the stress pattern in the granodiorite was attributed to the anisotropic characteristics of the constituent minerals of various sizes.

Jan 1, 1963

By R. L. Crosby

The effect of indium on the solid solubility of calcium and of silicon in magnesium was studied using metallographic, X-ray diffraction, and electrical resistivity techniques. The addition of 2 weight-percent or more of indium reduced the solid solubility of calcium in magnesium by forming a compound containing indium and calcium. Indium additions have no perceptible effect on the solid solubility of silicon in magnesium.

Jan 1, 1963

By Alla D. Mah

Combustion energies of barium and strontium were measured by means of the combustion bomb calorimeter. The heats of formation obtained for the oxides were ?H298.15 = -139,060 ± 700 cal/mole of barium oxide (BaO) and ?H298.15 = -144,440 ± 400 cal/mole of strontium oxide (SrO). Tables containing heats and free energies of formation from 298.15° to 2,000° K were prepared.

Jan 1, 1963

By Vernon F. Swanson

Several laboratory flotation tests were conducted by the Bureau of Mines on a sample of unweathered diorite from the B. F. Camden property, Amherst County, Va. Results showed that an ilmenite concentrate analyzing 45.5 percent Ti02 (titania), 0.07 percent P205 (phosphorus pentoxide), and 2.21 percent Si02 (silicon dioxide) could be produced from a feed containing 7.72 percent Ti02 and 3.94 percent P205. Ti02 recovery in the concentrate was 47.6 percent in a batch test. The weathered saprolite material overlying the diorite required scrubbing and desliming to remove argillaceous material and preliminary flotation of apatite followed by flotation of ilmenite. The resulting concentrate analyzed 47.3 percent Ti02, 0.19 percent P205, and 0.99 percent Si02 from a starting feed of 8.99 percent Ti02 and 3.37 percent P205; TiO2 recovery was 54.5 percent.

Jan 1, 1963