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By J. B. Rosenbaum

This report presents new findings and consolidates previously published data to provide a single reference containing a concise and comprehensive description of the Bureau's work on electrolytic chromium. Two separate systems for electrolytic-chromium recovery were developed, one designated as the oxidized system the other as the reduced system. The electrowinning of chromium metal follows the dissolution of chromium from the ore or from ferrochrome and its separation from gangue and metallic impurities. Chromite was first solubilized by pressure digestion at slightly elevated temperatures in an oxidized acid solution using Na2Cr2O7 as an oxidizing agent. Later it was found that a sodium-free electrolyte was preferable, using return-cell anolyte containing H2SO4 and Cr03 as the oxidizing agent. Gangue materials were separated from the soluble metallics by filtration; and, after the Cr+3 had been stabilized, the metallic impurities were separated as crystalline ammonium salts by vacuum crystallization.

Jan 1, 1957

By F. N. Bender

Percolation leaching of wad-type manganese ores was investigated, using a novel system of alternate upward passage of sulfur dioxide gas through moistened ore and downward percolation of wash solutions to extract solubilized manganese. Bench and large-scale tests designed to simulate vat and heap leaching were made on four wad ores from Arizona and Nevada and on a pailomelane ore from Arizona. Three of the wad ores required prebaking at 500° to 600° C. to produce a permeable agglomerate that would not slake during percolation washing. The hard-type ore and one of the wad ores that contained a large amount of granular gangue did not require prior roasting. The deportment of the different ores toward leaching and percolation was studied with particular reference to the influence of the sulfur dioxide - oxygen ratio and the effect of gas dilution on the rate of manganese dissolution, dithionate formation, and acid production. Crushed charges of the ores, as coarse as 1 inch and as fine as 1/4 inch, were treated for periods of 5 to 11 days. Percolation of the gas and leach solutions through the charges was achieved without difficulty. The manganese extractions varied between 78 and 97 percent and depended upon the size and type of ore leached. The average quantity of sulfur dioxide required in the larger scale tests was about 2.6 pounds per pound of manganese recovered. The dithionate formation varied from 0.35 to 0.9 pound per pound of manganese extracted depending upon the strength of leaching gas.

Jan 1, 1957

By T. A. Evans

The Bureau of Mines conducted a Laboratory and pilot-plant investigation of the flotation of iron sulfides from zinc-lead mill tailings near Platteville, in south-western Wisconsin, at the North Central Experiment Station, Minneapolis, Minn. The procedures used and the results obtained in this investigation are described in this report. Samples for laboratory tests were obtained from each mill in the district, namely, Calumet & Hecla, Inc., Eagle-Picher Co., Vinegar Hill Zinc Co., and Tri-State Zinc, Inc. The sample fat pilot-plant work was obtained from the Davis Mining Enterprises mill.

Jan 1, 1957

By Wilbur A. Haley

One of the purposes of the investigation was to determine and report on how coal augers are used to mine bituminous coal that is near outcrops and may not be mined otherwise by any other present-day method. Such increased overall recovery results in the conservation of coal resources. Other reasons for the investigation were to determine and report the production rates of such operations and the types of equipment used. Auger mining of coal as a means of coal recovery supplementary to strip mining has been introduced and developed since World War II. This type of coal mining has grown rapidly, and bituminous-coal production by auger mining has been estimated at 6,000,000 tons in 1955. Mines were selected for study to give reasonably representative information on auger mining in different types and thicknesses of coal beds in different geographic areas and on different types and sizes of equipment operated under various conditions. This report is based on field studies of 8 auger-miming operations in Pennsylvania, West Virginia, and Ohio and in 5 different coal beds. Operations were observed in active strip mines, in strip mines reopened for auger mining, and along benched coal-bed outcrops. At the time of this study, no augers were reported to be operating in underground mines. The diameters of holes drilled ranged from 26 to 52 inches, and the lengths of holes ranged up to 208 feet. At some operations auger holes often penetrated abandoned underground mine workings.

Jan 1, 1957

By Effie T. Kurt, Jack Wright, J. W. Watkins, Cynthia Pearson

"The analysis of water produced with crude petroleum has interested oil producers since inception of the industry. Records of the first analysis of mineralized water produced from an oil-productive formation are obscure, and references to the first use of brine analyses to assist in solving problems of petroleum production are not available in the technical literature. However, many early reports of the Federal Bureau of Mines 5-8/ and. Federal Geological Survey, 9-11/ as well as articles in engineering and geological placed special emphasis on journals ,12-l4/ the importance, interpretation, and application of water analyses.One of the earliest applications of water analyses, and still a major one today, is for identification of intrusive waters in oil wells. This may be done by comparing the chemical constituents of a sample of water indigenous to the oil-productive formation with those of samples from upper, water-bearing formations within the same general area. Some earlier investigators recognized the need for analyzing samples of all waters encountered in drilling operations. Ambrose15/ stated, in part, ""In wells being drilled, the engineer should grasp every opportunity to get a true sample of water from each sand. . .,"" and, ""The waters of each oil field are chemically different from those of another field."" The validity of the latter observation and the importance of the former one have been borne out by comparing the results of analyses of many samples and noting the differences in relative concentrations of like constituents of waters from the same geological formation in different localities or oil pools."

Apr 1, 1957

By Jack Wright

The analysis of water produced with crude petroleum has interested oil producers since inception of the industry. Records of the first analysis of mineralized water produced from an oil-productive formation are obscure, and references to the first use of brine analyses to assist in solving problems of petroleum production are not available in the technical literature. However, many early reports of the Federal Bureau of Mines5-8 and Federal Geological Survey,9-11/ as well as articles in engineer and geological journals12-14/ placed special emphasis on the importance, interpretation, and application of water analyses. One of the earliest applications of water analyses, and still a major one today, is for identification of intrusive waters in oil wells. This may be done by comparing the chemical constituents of a sample of water indigenous to the oil-productive formation with those of samples from upper, water-bearing formations within the same general area. Some earlier investigators recognized the need for Analyzing samples of all waters encountered in drilling operations. Ambrose15/ stated, in part, "In wells being drilled, the engineer should grasp every opportunity to get a true sample of water from each sand. . .," and, "The waters of each oil field are chemically different from those of another field." The validity of the latter observation and the importance of the former one have been borne out by comparing the results of analyses of many samples and noting the differences in relative concentrations of like constituents of waters from the a geological formation in different localities or oil pools.

Jan 1, 1957

By H. Kenworthy

The investigations described in this report were undertaken to demonstrate, on a laboratory scale, the possibility of recovering several million pounds of tin plus tungsten contained in stockpiled and currently rejected slags from the Longhorn tin smelter at Texas City, Tex. At the same time, it was anticipated that the treatment procedures developed might be applicable to slags from other tin-smelting operations. Results of the laboratory work show that it is possible, by pyrometallurgical means, to separate the tin and tungsten into products of intermediate grade that may be returned to the smelter circuits for further upgrading. Several methods of treatment were investigated. The methods that proved effective were: Fusion reduction, chloride volatilization, sulfide volatilization, and carbide formation. Over 90 percent of the tin and tungsten could be removed from the slat by any of these methods. Each type of treatment has advantages and disadvantages, and it could not be determined from the small-scale work which method was the more meritorious. Tungsten and (in some types of treatment) tin-bearing products were diluted by iron, the separation of which will require additional studies. Prevention of a portion of the iron from reporting with the tin or tungsten is a distinct advantage and possibility that will require inure laboratory work to develop the needed techniques for its accomplishment. Tin products from single treatments of stag ranged up to 75 percent in tin content but were more generally under 35 percent. Tungsten products were usually under 15 percent; but segregated portions could be selected, at a sacrifice in recovery, that contained up to 50 percent tungstic oxide equivalent.

Jan 1, 1957

By H. E. Peterson

A study was undertaken by the Bureau of Mines to develop a simple, reliable test for field detection of selenium in rocks and soils. Two methods are described for qualitative detection of selenium, dependent upon its form of occurrence and the presence of interfering constituents in the sample. Both methods involve fusion of the sample in a test tube to form elemental selenium that will volatilize and condense as a red deposit on the cooler upper portion of the test tube. The methods are sensitive to 10 parts per million, (p.p.m.) equivalent to 0.001 percent, and can be made semiquantitative by using suitable standard samples. INTRODUCTION Although selenium is widely distributed in the United States, the known deposits are either so small or so low grade that they cannot be processed economically for selenium alone-4/ At present, commercial production is a byproduct of the smelting and refining of base-metal ores, particularly copper.5/ About 0.75 pound of selenium is recovered per ton of electrolytic copper, and small amounts are recovered by special treatment of assorted smelter dusts and fume products. Since selenium is a strategic metal in short supply, new sources are being sought by both Government and private interests.

Jan 1, 1957

By R. A. Meyer

A table that greatly simplifies determination of metastable transitions in mass spectra has been prepared. All the mathematically possible metastable transitions of any compound whose molecular weight lies between 26 and 150 can be determined from the table without calculation. The method of utilizing the table is described, using selected peaks from the spectrum of normal butane for illustration. In the mass spectrometer, ions are formed in the isatron and accelerated through a series of slits. Most of these ions reach the collector without further change, but a few dissociate in transit to form new ions. These ions appear in the mass spectrum at neither the mass--to-charge ratio (m/e) of the original ion nor that of the new ion. A formula that relates the appearance of these new ions to the ion from which they were formed is: [ ]

Jan 1, 1957

By Oren C. Baptist

[Several new oilfields have been developed in northwestern Wyoming during the past 10 years, production is obtained from discontinuous, permeable sands enclosed within impermeable shales. The energy to drive the oil to producing wells in supplied by gas in solution in the oil. Most of the wells had high-initial potentials, but rates of oil production have steadily declined, indicating a dissipation of the driving energy and the possibility that large volumes of oil will remain unrecovered in the reservoirs. The studies reported in this paper were undertaken to develop laboratory data of the type most likely to be needed by persons studying the susceptibility of the Newcastle sand reservoir to secondary-recovery methods.]

Jan 1, 1957

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions4/ issued by the Bureau of Mines, the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1957

By C. H. Schack

Although viscosity is known to be important in processing and handling finely ground urea, its effect has never been fully quantified. This report describes the methods used and the results obtained in the initial phases of a broad investigation of the influence of viscosity of water suspensions of minerals in flotation, thickening, filtering, and other mineral-dressing unit operations. Several types of vis-cosimeters were tested before reliable and reproducible results could be obtained on mineral suspensions. After the viscosimeter used in the research was calibrated and standardized, tests were made on six pure minerals to study the relationship of pulp density, particle size, crystallinity, and cleavage on viscosity. An orifice-type viscosimeter equipped with a mechanical stirrer gave as good results as other types and was more flexible, faster, and simpler to operate. The orifice-type viscosimeter, when calibrated and standardized with glycerin and water mixtures, proved satisfactory over a wide range of viscosities. The accuracy and reproducibility were reasonably constant between 1 centipoise and 200 centipoises, the anticipated range in common mineral-dressing unit operations.

Jan 1, 1957

By R. A. Hatch

This report summarizes the results of nearly 8 years research on and production of synthetic mica at the Electrotechnical Experiment Station of the Federal Bureau of Mines, Norris, Tenn. This program was undertaken at the request of the United States Department of the Navy and was financed mostly by the Army Signal Corps and the Navy Bureau of Ships through a contract with the Office of Naval Research, The original objectives included fundamental studies of fluor-phlogupite and other fluorine-micas and production of synthetic mica sheets on a pilot-plant scale. The first 3 years of this project were devoted mainly to a search for practical solutions of the many problems involved in designing and constructing a pilot plant for crystallizing fluor-phlogopite mica. The first and most urgent need was a suitable container for the corrosive mica melt. After extensive study, it was concluded that platinum, graphite, high-silica fire clay, and silicon carbide were the most promising refractories for crucibles; but none was perfect. Silicon car¬bide seemed to have the better combination of qualities, combining good corrosion resistance with oxidation resistance.

Jan 1, 1957

By S. M. Runke

The pegmatite investigations at the Rapid City, S. Dak., Experiment Station during; the pact 3 years have been primarily a study of recovering beryl from nonlithium-bearing pegmatite rock by continuous-testing methods. Beryl concentrates containing 25 to 88 percent beryl were produced from rock that ranged in beryl content from 0.1 to 2.5 percent. The beryl recovery ranged upward from 70 percent but averaged better than 80 percent. Although promising results have been obtained with flotation methods for upgrading these concentrates to standard specifications, additional work is needed to improve and simplify the procedure. In addition, it was demonstrated that several potentially useful coproducts could also be recovered from pegmatite rock. The principal coproducts were mica, feldspar, and quartz. A heavy-mineral product also was made from pegmatites containing tin, tantalum, and columbium. The recovery if these minerals in products meeting the specifications of the commercial users has been reserved for future study. The investigations also included studies on extraction of beryllium from both high-grade beryl and flotation concentrates of medium beryllium content. The procedure investigated consisted of sintering beryl or beryl flotation concentrates with limestone, acid curing the resulting sinter with sulfuric acid to dissolve the beryllium, and water leaching to extract the beryllium. Over 90 percent of the beryllium was extracted by this procedure. Most of the optimum conditions and quantities of reagents were determined for dissolving the beryllium. As aluminum and iron also were taken into solution by the acid, further research is needed on methods of recovering high-grade beryllium salts from the solutions containing these elements.

Jan 1, 1957

By B. H. Clemmons

A field method has been devised for rapid determination of heavy minerals occurring in the unconsolidatod beach and dune sands. The method has been proved practical by usage in field evaluations of several hundred beach- and dune-sand samples in the Florida area. The simple equipment required and the techniques involved are described. Other data show that the method is relatively insensitive to variations in the mineralogical content or size distribution of the mixed heavy minerals contained in the samples tested. A modification of this procedure, found to be suitable for plant use in determining the relative purity of heavy-mineral flotation concentrates, is also described. A specific application is determination of the amount of feldspar-quartz in spodumene flotation concentrates. The results of the rapid evaluation techniques closely approximate those obtained by more precise laboratory procedures.

Jan 1, 1957

By Robert L. Rough

The 1954 field tests consisted of six experimental shots in relatively deep holes in a sandstone similar to many oil-bearing sandstones. Water-injection measurements were made before and after each shot to establish the change in conductivity of the fluid caused by the shot. The pressure pulse produced by the shot was recorded in nearby holes to monitor the shot and to determine if any relation existed between the change in conductivity and the nature of the pressure pulse. The results of water-injection tests showed the range of conductivity of fluid before and after shooting with two different types of explosives. Because of the large spread in data for similar shots, not enough information was available to evaluate the differences in increased conductivity produced by the two explosives or any relation between the increased conductivity and the nature of the pressure pulse. However, these results, with the results of other tests involving explosive shots in rock, provide guidance for future research on the oil-well-shooting problem.

Jan 1, 1957

By Wallace E. Anable

This investigation by the Bureau of Mines was conducted chiefly on Cuban serpentine nickeliferous ores to determine whether these materials would be amenable to direct carbothermic reduction in an electric furnace to produce a low-carbon ferro-nickel. The project was carried out as one of several under a Memorandum of Agreement between the Bureau of Mines and the General Services Administration (Contract GS-OO-B (D)-152l). Two ore samples were received for this investigation. One was a mixture of nickeliferous serpentine from the North Ocujal, South Ocujal, and San Juan claims of the Nicaro Nickel Co. The other sample was a mixture of material from the Ramona and the Lorna Mulo claims of the Cuban Nickel Co. Most of the ore from the Ocujal-San Juan deposits and about 40 percent of the sample from the Ramona-Lorna Mulo deposits were calcined before smelting. The remainder of the sample from the Ramona-Loma Mulo deposits was smelted after drying to about 8 percent moisture. An arc-resistance, selective-reduction smelting technique was employed in these tests. Either bagasse alone or a mixture of bagasse and coke was used for reductants. No flux was used in the furnace charges.

Jan 1, 1957

By R. V. Lundquist

Aeration in water slurries and controlled drying of manganous hydroxide produced from dithionate leaching of Artillery Peak manganese ores from Arizona were investigated by the Bureau of Mines at its Electrometallurgical Experiment Station, Boulder City, Nev., to determine whether a simple process could be developed for converting this product into a battery-grade manganese dioxide. The properties of manganese dioxide prepared by the thermal decomposition of manganous nitrate were investigated also. Manganese dioxide suitable for use in batteries was not obtained from the dithionate leach product, but some of the factors controlling its oxidation were isolated. Aging of manganous hydroxide was of major importance in retarding its oxidation by aeration. Sodium hydroxide and sodium silicate promoted oxidation by drying. Optimum quantities were about 0.85 mol of sodium hydroxide and 0.2 mol of sodium silicate per mol of manganese, and drying temperatures of 200° C. produced yields of manganese dioxide up to 90 percent of the manganese present. Higher temperatures and concentrations of reagents carried oxidation of manganese beyond its tetravalent state.

Jan 1, 1957

By Robert H. Merrill

This report summarizes the first phase of studies to determine the design and behavior of an unsupported roof in an experimental room in limestone. The selection of a roof horizon and the design of the room were results of an investigation of the geology of the formation, the physical properties of samples from the proposed roof, and calculations from the theory of gravity-loaded beams. The design of the opening, some physical properties of the roof in place, and the behavior of the roof were checked by tests in a full-scale experimental room. The room was instrumented to measure roof deflection, separations in the roof strata, and incipient failure. The dimensions of the room before instrumentation was installed were 10 by 100 feet; the room was widened in successive increments to 40 by 100 feet. Between widening operations periods up to 6 months were allowed to provide a time test of the roof spans. The results of the measurements of deflection and separations showed that the lowest 6-inch layer in the roof became detached as the room was widened. This layer was eventually removed after standing without failure for about 4 months at room dimensions of 40 by 100 feet.

Jan 1, 1957

By V. A. Nieberlein

An extractive process was developed applicable to submarginal titanium deposits containing valuable minor constituents; such as columbium (niobium) and iron. The process consisted of reducing the mineral concentrate with coke at high temperature to form a carbide-suboxide sinter, chlorination in the 400° -500° C. range, and fractional condensation of the chlorides. The chlorination procedure recovered 97, 83, and 87 percent of the titanium from brookite, rutile, and ilmenite sinters, respectively, while simultaneous columbium recoveries on the same materials were 85, 50, and 87 percent.

Jan 1, 1957