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By George E. Fish

This report describes investigations conducted by the Bureau of Mines from 1957 through 1959 in the Roseland anorthosite-titanium belt of Nelson and Amherst Counties, Va., for the purpose of studying the titanium resources of the area. Three titanium deposits containing much saprolite ore derived from the decomposition of anorthosite and diorite were selected for detailed study Following a reconnaissance of the reported titanium occurrences in the belt. These three deposits occur in or are associated with anorthosite. Most of the occurrences are situated on or near the contact between the anorthosite and the gneissic country rock. The saprolite deposits are as much as 1.5 miles long, 1,000 feet wide, and 100 teat deep and contain significant reserves of titanium-bearing material estimated in excess of 20 million tons. Where it was penetrated by drilling, the unweathered rock beneath the saprolite contains nearly the same titanium values as the saprolite.

Jan 1, 1962

By F. B. Petermann

The Bureau of Mines conducted electric furnace smelting tests on sintered flotation concentrate and siliceous log-washed are. The flotation concentrate was derived from the Maggie Canyon deposit of the Artillery Mountains area, Mohave County, Ariz., and contained, before sintering, 35.6 percent Mil and 19.4 percent Si02 + A1203. The log-washed ore was from the McGregor deposit of the Artillery Mountains area, Mohave County, Ariz., and contained 31.2 to 33.6 percent Mil, 19.5 to 27.6 percent Si02 + A1203, and 2.5 percent Pb. This work was undertaken to determine the most effective smelting technique for producing standard products from such nonspecification ore and concentrates. The objective was to collect data, using a small furnace, which would be reasonably accurate and permit extrapolation to large-scale practice for comparing with results on specification-grade are.

Jan 1, 1962

By Charles Zahn

Direct mass spectrometric determination of alcohols in the presence of hydrocarbons has not been possible because of the similarity of hydrocarbon and alcohol mass spectra. Experiments have demonstrated that by converting the alcohols to their trimethylsilyl derivatives, characteristic mass spectra are obtained free of interference from hydrocarbon ion fragmentation. Hexa- methyldisilazane is the reagent selected for the conversion, An improved method of preparing the reagent is given, Mass spectrometric determination of alcohols as trimethylsilyl ethers now is not only possible without prior separation from other materials, but the range of the room-temperature mass spectrometer is also extended to include the C10 alcohol region. Water does not interfere because it is converted to hexamethyldisiloxane, which has its own distinctive mass spectral peak, Experience indicates that other compounds such as glycols, amines, and phenols probably could also be determined by mass spectrometry of their trimethylsilyl ethers. Studies on the similar detemination of phenols in coal oils have been started, When mass spectrometry is not available, gas-liquid chromatography of alcohols before and after their conversion to the trimethylsilyl derivatives probably could be performed. The preparation and properties of the trimethylsilyl derivatives of 23 alcohols, 2 glycols, 3 amines, and 1 mercaptan are detailed. INRODUCTION During investigations by the Bureau of Mines at the Pittsburgh Coal Research Center relative to the development of Fischer-Tropsch processes, complications were encountered in the mass spectrometric analysis of alcohols in hydrocarbon oils. The fragmentation peaks of the alcohols and the hydrocarbons were so similar that an accurate analysis was not possible, Since involved separation techniques are necessary to isolate alcohols from hydro-carbons for separate determinations, efforts were turned to the search for a

Jan 1, 1962

By Harold L. Riley

This Bureau of Mines paper describes the methods and practices used at the Peck quarry of the Crab Orchard Stone Co., Inc., one of the leading producers of dimension stone in the Crossville, Tenn., area. The product is marketed under the registered trademark "Crab Orchard Stone". Another large producer of stone from the Crossville district sells its product under the registered trademark of "Tenn-Quartz". Both companies, and a number of other companies and individuals who quarry and process dimension stone from the same general geological formation, are members of the Quartzite Producers Association of Tennessee. The salable product is shipped throughout the country for use as architectural building stone. In 1959, 653,008 cubic feet of stone was produced in the Crossville area and was sold for $1,414,405. Terms and descriptions used in this report are those of the quarry and building trades. The offices, pitching sheds, wire saws, railroad siding, and storage areas of the Crab Orchard Stone Co., Inc., are on a side road 0.3 mile north from a point 2.2 miles east of Crossville, Tenn., on U.S. Highway 70. The quarry is on this same side road 2.0 miles south of Highway 70. Crossville is 62 miles west of Knoxville and 65 miles northeast of Chattanooga, Tenn.

Jan 1, 1962

By H. D. Kline

This paper is one of a series being prepared by the Bureau of Mines on methods, practices, and costs in various mining districts in the United States. The paper describes mining and ore recovery methods common to the Batesville manganese district, Independence County, Ark., and gives the costs of producing merchantable ore by three operators whose methods were more or less typical of those of many other local manganese producers. The operating costs reported were those of Leonard Baxter at mines on Brooks Hill for the calendar year 1958 and Arkansas Mining and Exploration Corp. at Section 16 mine and the Searcy group of mines and Miller-McGee Corp. at the Diener mine during the first 6 months of 1959. Manganese are was mined in the district as early as 1849 and almost continuously thereafter until August 1959, when termination of the Government's domestic manganese purchase program resulted in complete cessation of mining activity. During those years, production came from more than 189 mines and properties, of which only a few produced as much as 30,000 tons of merchantable ore.

Jan 1, 1962

By Robert F. Stewart

The oxidation of structural materials at high temperatures in gas-cooled systems can be greatly retarded by the addition of small amounts of hydrogen to the inert coolant. In experimental equipment for gasifying coal with heat transferred by helium, the oxidation of graphite and metals (molybdenum, tungsten, and certain stainless steels) by trace impurities in the coolant helium was virtually eliminated by adding 0.1 to 1.0 percent hydrogen. The reaction of hydrogen with praphite does not preclude its use to retard oxidation; at 2,400° F. only 0.2 pound of graphite per square foot per year is lost for each percent of hydrogen in the helium. The addition of hydrogen appeared to prevent the mass transfer of carbon often associated with oxidation of graphite, without causing noticeable embrittlement of stainless steels and molybdenum or other damaging effects. This method has been tested in precision gas-recycle systems and applied successfully for more than a year in a pilot-scale unit operating at 250 pounds per square inch gage and 2,400° F. It is now used routinely and can be applied to many gas-cooled systems operating at high temperatures.

Jan 1, 1962

By Willard L. Hunter

The research described in this Bureau of Minus report was conducted to improve the chromium-iron ratio of offgrade chromite. Two methods were used: (1) Iron was selectively reduced from chromite by carbothermic reduction in an electric-arc furnace, and (2) a mixture of carbon, chromite, and sometimes fluorspar was chlorinated to remove a substantial part of the iron. Chromite concentrate from the Mouat deposit in Montana and from northern California was used in the test work. Chromium-bearing slag and chromite that had been beneficiated by a roast-leach process were each smelted to produce high-carbon ferrochromium. Iron was selectively reduced in a laboratory-scale., electric-arc furnace. Carbon additions to the smelting charges varied from 40 to 100 percent of the stoichiometric requirement, and slag basicities were varied from 0.4 to 1.0 chromium-iron ratios of more than 4:1 were obtained with 89 percent recovery of chromium in a chromium-bearing slag.

Jan 1, 1962

By T. T. Campbell

Research conducted by the Bureau of Mines demonstrated the feasibility of preparing columbium and tantalum metals by the application of Kroll-process techniques. Yields in excess of 95 percent were obtained in a modified Kroll-process reduction apparatus constructed from nickel and Inconel.4 Operating conditions during reduction and distillation were determined. Optimum temperatures during sodium reductions ranged from 650° to 750° C and for magnesium from 700° to 800° C with retort pressures ranging from 3 to 7 psig. Undesirable vapor phase reactions occurred when temperatures exceeded 750° C during sodium reductions or 850° C with magnesium. Vacuum distillation at 850° C effectively removed volatile salts and excess reductant from the reduced metals. Calculations based on the results obtained in small scale tests indicate that reaction rates of up to 34 lb/hr could be obtained during columbium reductions and up to 60 lb/hr during tantalum reductions in production scale reac¬tors. The small, laboratory-scale techniques used in this study could be adapted to commercial practice. The reduced powder or sponge metals can be consolidated by conventional arc-melting techniques, and the arc-melted metals can be fabricated into ductile sheet at room temperature. Analyses of arc-melted buttons prepared from Kroll-process tantalum or columbium showed that tantalum of greater than 99.8-percent purity was obtained and that columbium purity exceeded 99.7 percent. A significant purification of the reduced metals occurred when they were consolidated by electron-beam melting, and the purity and ductility of electron-beam-melted Kroll-process tantalum and columbium compared favorably with the commercial metals. After electron-beam melting, the purity of the tantalum exceeded 99.95 percent, and columbium purity was approximately 99.9 percent.

Jan 1, 1962

By E. D. Calvert

The objective of this research was to examine variations in melting and forging practice for four titanium-base alloys and to determine their effect on the resultant product. Of particular interest was the evaluation of the skull-casting technique. The data should serve as a guide to producers and consumers of titanium products. Physical properties of four titanium-base alloys in ingot form and in sheet form were evaluated and correlated, where possible, with variations in the melting and casting procedure. Consumable-electrode melting was used throughout, but arc current and furnace backfill pressure were varied, and ingots were formed both by melting directly into a water-cooled copper mold and by skull melting followed by pouring into a graphite mold. Alloying metal additions for the alloys tested were (1) 8 percent manganese, (2) 6 percent aluminum and 4 percent vanadium, (3) 6 percent molybdenum and 2 percent aluminum, and (4) 16 percent vanadium and 2.8 percent aluminum.

Jan 1, 1962

By Leonard Obert

Between 1927 and 1957, sodium borate minerals were mined by underground methods in the Kramer District, Kern County, Calif. In 1957, surface mining methods were initiated, and during the next two or more decades it is probable that most of the production from the district will be obtained from open pits. However, part of this borate deposit is sufficiently deep that surface mining may not be economical and, hence, at some future date underground methods may again be employed. This report was prepared to document the underground mining methods employed in the district before 1957. The general geology of the district and the detailed geology of each of four mine sites are presented, together with a mineral and mechanical description of the ore and enveloping rock. The report also describes the stoping, extraction, pillar support, methods of artificial support, and other factors that affect the structural characteristics of these mines.

Jan 1, 1962

By G. H. Gronhovd

This report describes the design and initial operation of a slagging gasification pilot plant installed by the Bureau of Mines at the Lignite Research Laboratory, Grand Forks, N. Dak., in 1958-59. The tests covered in this report were conducted over a period of about 2 years, beginning in April 1959. The pilot plant was designed for eventual operation at pressures ranging from 400 to 600 p.s.i.g. (pounds per square inch gage); however, for the preliminary test reported here, the gasifier was fitted with a low-pressure slagging section and operated at atmospheric pressure and at 80 p.s.i.g. The reason for using a low-pressure slagging section for initial operation was to facilitate modifications in design during the development of a reliable slagging procedure.

Jan 1, 1962

By Kenneth M. Earl

This report describes the results of a field study conducted by the Bureau of Mines during 1956 and 1957 on manganese-and iron-bearing mineral deposits in the southern district of Aroostook County, Maine. The work was undertaken to determine the extent of deposits largely concealed under glacial drift and to obtain subsurface samples for manganese mineral identification and research in ore dressing and extractive metallurgy. The investigation was confined to the Westford Hill-Daggett Hill area in Hodgdon Township and to the Stewart prospects and vicinity in Linneus Township. Over 50 magnetic anomalies were mapped by magnetometric surveys in the Westford Hill-Daggett Hill area, Hodgdon Township. The largest anomaly, as outlined by the 1,000-gamma contour, indicates a deposit 3,200 feet long with a maximum width of 350 feet. The smallest anomaly measures about 10 feet wide by 25 feet long.

Jan 1, 1962

By M. M. Wong

Beryllium possesses attractive properties for use in the nuclear and space fields. Since fused-salt electrorefining can be employed to produce this metal in high-purity form from low-grade or scrap metals, the Bureau of Mines investigated electrorefining of beryllium in electrolytes composed of a LiC1-KC1 eutectic mixture plus varying amounts of BeC12. Results showed a 99- percent or better reduction of oxygen and magnesium and a substantial reduction of other minor metallic impurities. Extremely pure beryllium metal was produced. Operating variables, including BeCl2 concentration in the bath (3.5 to 16.5 mole-percent), temperature of operation (450° to 550° C.), and cathode current density (45 to 770 a,/sq, ft.), were studied; their effects on the deposition of metal, working condition of the bath, and purity of the refined metal are discussed. The safety precautions used in handling beryllium in the laboratory are also described.

Jan 1, 1962

By J. R. Welty

High-temperature thermodynamic data have, in recent years, become increasingly important for the extractive metallurgist. The extraction of metals from their ores previously was based on trial and error methods, involving hours of testing and often costly equipment fabrication. Using thermodynamic data it is frequently possible to predict the feasibility of a proposed metallurgical process as well as the optimum operating conditions for the process with reasonable accuracy. Such predictions can save consider-able tim~ and expense. Widespread use of thermodynamic analyses has been handicapped by lack of dependable experimental data. Investigators, notably K. K. Kelley (4)4. have devoted many years to determining and compiling such data. These investigators, although prolific in their production of thermodynamic values, have been unable to meet all the needs of industry and other branches of science. This becomes obvious when one considers the aeronautical and nuclear fields, in which previously unimportant, therefore uninvestigated, substances have become of prime importance.

Jan 1, 1962

By Eugene L. Grumer

High-expansion foam was applied to the flames of six fuels burning in a 1-foot-diameter tray. The flames of three hydrocarbon fuels were more readily extinguished than the flames of methanol, acetone, or unsymmetrical dimethyl hydrazine. The result is rationalized on the basis that heat transfer from flame to fuel surface is primarily radiative with the hydrocarbons and more largely convective with the nonhydrocarbons. INTRODUCTION Equipment for producing high-expansion foams has been developed by the Bureau of Mines to control coal mine fires.5 Recently such equipment has been redesigned for portability and has now been produced commercially for other fire-fighting applications. In May 1961, a 50-by 50-foot gasoline fire was extinguished within 2 minutes by a trailer-mounted foam unit that produced 12,000 cu.ft./min. of high-expansion (1,000:1) foam.6

Jan 1, 1962

By F. E. Brantley

Blister copper was successfully deoxidized with any of a variety of reducing gases; lancing techniques or a vertical-column furnace were used to contact the copper and gases. Of the gases tested, butane, when used to lance molten copper at about 1,200° C, reaction temperature, was slightly more effective than propane, natural gas, carbon monoxide, or reformed gas for deoxidizing copper from about 1.0 to less than 0.1 percent oxygen content, Laboratory-scale tests revealed that the vertical furnace, composed of a heated column packed with silicon carbide chips or hollow carbon cylinders, was significantly faster and more efficient than the lancing technique for deoxidizing molten copper with any of the gases tested. Comparison of the gaseous-reduction method with the conventional poling method suggests that the gaseous method has important technical and economic advantages for deoxidizing blister copper to any readily controlled amount of residual oxygen content.

Jan 1, 1962

By A. G. Starliper

The report covers studies by the Bureau of Mines on the removal of metallic values in two waste products from the Longhorn tin smelter at Texas City, Tex. One product was a slag that contained tin, tungsten, iron, tantalum, and columbium. The other product was a spent acid solution that contained tin, tungsten, iron, lead, copper, zinc, and silver and that came from presmelting treatment of impure tin concentrates. Molten slag was treated with sulfur or sulfur compounds and with coke, calcium carbide, or gaseous reductants to form tin sulfide that volatilized from the charge and to reduce tungsten along with iron and silicon to form a carbon-bearing metallic layer. The metallic layer was treated by an oxidizing alkali roast and then was water-leached to extract the tungsten. The waste acid was used in other experiments to dissolve an iron-tin- tungsten alloy (hardhead) obtained by direct reduction of the slag. An insoluble fraction containing tungsten, silver, silicon, columbium, and tantalum was removed, and copper was cemented on metallic iron, Tin was recovered by cementation on zinc plates, and lead was precipitated by adding sulfate ion. Iron was precipitated by increasing the pH which left a solution containing principally zinc. Slabs of hardhead were electrolyzed in an electrolyte consisting of waste acid to plate out groups of metals at different pH?s. The time did not permit thorough exploration of this method of treatment.

Jan 1, 1962

By D. J. Bauer

A pure scandium solution was concentrated from 10-4 mole per liter to 0.5 mole per liter by continuous foam fractionation in a spaced, packed column. Recovery in the foam was 77 percent using a spaced, packed draining column with sodium n-methyl-n-"coconut oil acid" taurate as the surfactant. The technique was first studied batchwise in a small unpacked column to determine the more important variables. Optimum surfactant concentration was found to depend on scandium concentration. Extraction and, in general, enrichment ratios were highest in the 2.5 to 3.5 pH range at temperatures ranging from 50° to 70° C. An airflow rate of 136 ml./min. was satisfactory in the equipment used.

Jan 1, 1962

By John C. Machisak

The National Safety Competition is sponsored and conducted annually by the Bureau of Mines, U.S. Department of the Interior, to give greater impetus to the building of programs safeguarding the employees of the mineral industries from disabling work injuries. The results of the 1960 National Safety Competition are presented in this publication. Mines and quarries that were awarded the Sentinels of Safety trophy for the best safety record in their competitive group and those mineral operations that ranked second, third, fourth, and fifth in the competition are listed with a summary of their achievements in preventing disabling work injuries. In addition, this publication presents statistical data on disabling work-injury experience in all other mines and quarries participating in the annual competitions.

Jan 1, 1962

By Donald E. Redmon

Industrial engineering departments perform staff duties and are most effective when sincerely supported by management. In accordance with the needs and desires of the mining companies involved, various industrial engineering functions have been adopted widely at western metal mines during the period 1950-60. Newly organized departments usually conduct method and equipment studies, work-measurement programs, and establish and maintain production standards. Supervisor-training programs and courses are effective in showing the relationship between supervisory responsibility and the purpose for which industrial engineering is practiced. Industrial engineering staffs of western metal mines are composed predominantly of personnel from within the companies. Experienced industrial engineers, not necessarily experienced in mining, frequently are hired by a company to help establish the department. Management consultants frequently are called upon to advise management and instruct department personnel in industrial engineering practices. Some departments have developed satisfactory industrial engineering programs without benefit of formal industrial engineering training or advice.

Jan 1, 1962