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By C. S. Tout

While investigating methods for determining the best temperatures for hot-working experimental stainless steels, the Bureau of Mines Albany Metallurgy Research Center developed a machine in which hot-twist tests could be made in a few minutes. This machine is similar to some used previously except that specimens are heated by induction instead of by radiation, and their temperature is measured by a calibrated radiation-detection unit instead of by a thermocouple. In. developing the technique for using the new machine, tests were made on specimens of medium-carbon steel, mild steel, and AISI (American Iron and Steel Institute) type 304 stainless steel. Tests also were made on as-cast specimens and preworked specimens of experimental AISI type 202, low austenitic stainless steel, and as-cast specimens of AISI type 301 experimental stainless steel. The optimum hot-working temperatures were determined for all types of steel tested. Also, data were gathered on the effects of test speed and temperature on torsional strength and the effect of twisting on tensile stress in the specimen.

Jan 1, 1962

By C. J. Thompson

In the course of the work currently conducted by the Bureau of Mines in cooperation with the American Petroleum Institute Research Project 48 on identifying sulfur compounds in petroleum, a micromethod was developed (12)5 for catalytically removing the sulfur atom from sulfur compounds. The product is the residual portion of the molecule; the structure otherwise was unaltered except for hydrogenation of any unsaturated bonds that were present in the original compound. Positive identification of sulfur compounds isolated from crude oils is a difficult problem. Direct comparison of properties of the unknown with those of reference compounds is often impossible because of the limited number of reference sulfur compounds available. However, a relatively large number of pure hydrocarbons is available, and the conversion of the sulfur compound to a hydrocarbon enhances the possibility of identification. The technique also can be used to prepare microquantities of scarce hydrocarbons by hydrogenating compounds that are readily available.

Jan 1, 1962

By R. E. Perry

To develop new or improved flotation methods for beneficiating low-grade red iron ores, the Bureau made many bench scale and continuous anionic flotation tests on ferruginous sandstones and calcareous iron ores from the north-eastern part of the Birmingham, Ala., iron district. The ores contained about 21 to 36 percent iron, a to 11 percent lime, and 22 to 64 percent silica. Production of iron concentrates containing 48 to 52 percent iron was technically feasible in batch tests, and the iron recoveries ranged from 85 to 92 percent. In continuous tests 49 to 51 percent iron products were obtained with 80 to 90 percent recovery.

Jan 1, 1962

By M. Clair Smith

This report is one of a series being prepared by the Bureau of Mines on exploration, development, mining methods, and costs at various open-pit mines in the United States. These reports have been prepared in cooperation with various mining companies. A similar program, conducted from 1928 to 1939, was generally conceded to have contributed to improving the efficiency of mining operations. The purpose of these reports is to promote development and conservation of our mineral resources by disseminating technological information on mining methods and practices. This report describes exploration, development, equipment, and mining by open-pit methods of the remainder of an ore body that had been previously worked by underground methods. The Tripp pit of the Consolidated Coppermines Corp. is located at Kimberly, Nev., a small mining company town having an elevation of 7,250 feet, 9 miles by road west of Ely, Nev. (fig. 1). The pit extends over the area formerly mined by underground methods from the Morris and Brooks shafts.

Jan 1, 1962

By Gerald V. Gibbs

As a part of the Bureau of Mines long-range program in asbestos, synthetic asbestiform compounds and minerals were prepared and described. Fundamental structural data on two such compounds are given in this report. Crystallographic data are provided for the synthetic isotypic compounds potassium-lead silicate, K2.Pb4 -Si8021 (I), and lead-aluminum silicate, Pb2. Pb4 .Al2Si6O21 (II). The space group symmetry 14/mmm was assigned provisionally to I and II on evidence of single crystal and piezoelectric measurements. A statistical evalua¬tion of indexed powder diffraction data revealed the cell edtes of I to be a 11.816 and c 7.932A and those of II to be a 11.723 and c 8.044A. The phases are uniaxial with observed refractive indices eD 1.790, an ?D,699 and eD 1.884, cusp 1,807, respectively. The atomic structure of I and II may be based on a complex of chains of silicon-oxygen tetrahedra lying along the c cell edge similar to the type of chain structure postulated by Pauling for scapolite. K2.Pb4.Si8021 and Pb2.Pb4 Al2Si6021 were first described by Geller and Bunting (5, 6)4 as fibrous compounds similar in crystal habit to asbestos. These authors gave powder diffraction data, although no attempt was made to find the cell edges or to index the powder diffraction patterns. Later, Shell and others (9) conducted a crystallochemical study of these fibrous silicates in search of a substitute for strategic asbestos. Their single crystal data revealed K2.Pb4 -Si8021 to be tetragonal body-centered with cell edges a 11.66, c 7.95 A. Pb2.Pb4 Al2Si6021 was concluded to be isotypic with K2.Pb4 -Si8021 on the basis of similar powder diffraction patterns, chemistry, and physical properties. No attempt was made, however, to index the powder diffraction record nor to determine the appropriate space group of either compound.

Jan 1, 1962

By Mary F. Koehler

Continuing a program of thermochemical investigation of compounds of to ferroalloy elements, this paper contains ins values of the heats of formation of two sodium molybdates (Na2Mo04 and Na2Mo207) and three sodium tungstates (NO2W4, Na2W207, and NA2W207, and Na2W4013). The experimental method was solution calorimetry. The solution medium was sodium hydroxide solution, except that hydrofluoric acid solution was used for sodium tetratungstate. The heat of formation values are given with reference both to the constit¬uent elements and to the constituent oxides. These data are of prime impor¬tance in the thermodynamic consideration of these substances, as their accumulation includes the most difficult and time-consuming steps toward evaluating the free energies of formation and thus the potential reactivities and thermal stabilities. Except for values for sodium monomolybdate and monotungstate, no previous similar data were contained in literature sources.

Jan 1, 1962

By John C. Machisak

THIS CHAPTER of the Minerals Yearbook (Volume III) contains overall injury experience for coal mines, both anthracite and bituminous, coke plants, petroleum and natural gas, peat, and asphalt and related bitumens (native); metal mines, their metallurgical plants, including ore-dressing plants and primary nonferrous reduction plants and refineries; nonmetal mines; nonmetal mills; sand and gravel operations; slag (iron blast-furnace) plaints; and stone quarries and their related pants. Volume I of the yearbook contains a chapter showing injury experience and employment data treated separately by metal mines, nonmetal mines, quarries and their related plants, metallurgical plants (ore-dressing plants and primary nonferrous reduction plants and refineries are shown separately), nonmetal mills, sand and gravel plants, and iron blast-furnace slag plants. Volume II contains injury and employment experience in the fuel industries (coal, coke, petroleum and natural gas, asphalt and related bitumens (native), and peat. Injury and employment data are submitted voluntarily for the mineral operations through an industry canvass made by the Bureau of Mines, except for the coal industry, whose reports are mandatory. Information published in this chapter is the result of this canvass. Figures presented in this chapter for 1961 are preliminary except for anthracite, peat, coke, petroleum and natural gas, asphalt and related bitumens, and slag. These preliminary data, with the exception of bituminous coal, are a summation of reports received by May 31, 1962, from the operators showing their injury and employment experience. Estimations of injury and employment experience are not included in these preliminary data.

Jan 1, 1962

By V. T. Dow

This report describes construction details and methods used in driving the 5490 tunnel at the Kennecott Copper Corp, property, Bingham, Utah. The tunnel will provide railroad access to the world-famous open-pit copper mine at the projected 5490 level. This publication is one of a series prepared by the Bureau of Mines to depict mining operations and techniques in various mining districts in the United States. Utah Construction and Mining Go. (formerly Utah Construction Co.), contractor on the tunnel project, began work during September 1956 and completed the project in February 1959. The tunnel is 18 feet wide, 24 feet high, and about 18,000 feet long, It will accommodate a railroad locomotive on standard- gage track. With the exception of the last 1,700 feet, the tunnel is supported by steel sets embedded in concrete lining. The 1,700-fact segment of the tunnel is supported by timber sets that will eventually be removed as the pit is deepened.

Jan 1, 1962

By Henry E. Blake

The purpose of this Bureau of Mines investigation was twofold. The first phase of the work was to determine the technical and mechanical feasibility of defluorinating low-grade siliceous fluorspars on an intermediate scale by high-temperature pyrohydrolysis in a rotary kiln. The second phase was to react the liberated hydrogen fluoride (HF) offgas with alumina monohydrate to produce commercial-grade aluminum fluoride (85 percent AIF3). The two phases of the work were to be integrated into a single continuous process. Evaluation of the data shows that low-grade siliceous fluorspars can be successfully defluorinated, either in a solid or a molten state, in a gas-fired rotary kiln in the presence of water vapor at 1,250° to 1,350° C. The water produced by combustion of propane was sufficient to yield defluorinatians of 75 to 85 percent.

Jan 1, 1962

By W. W. Agey

This report summarizes results of bench-scale metallurgical studies by the Federal Bureau of Mines on three composite samples representative of the low-grade manganese ores purchased by the General Services Administration (GSA) and stockpiled at Deming, N. Mex., and Wenden, Ariz. Bench-scale flotation tests at the Salt Lake City Metallurgy Research Center showed that all three composites could be beneficiated by flotation to recover 88 to 90 percent of the manganese in concentrates that assayed from 38.5 to 39.0 percent Mn, 10 to 12 percent insoluble, 5 percent CaO, 3 to 5 percent Fe, and 1.3 to 1.7 percent combined Pb plus Zn plus Cu, Sintering studies indicated that specification-grade material could be made from these concentrates by sintering above 1,000° C, and adding either sodium or calcium chloride to the charge to insure removal of enough lead and zinc to meet the specifications.

Jan 1, 1962

By A. R. Taylor

This report describes the design, construction, and operation of a low temperature adiabatic calorimeter for measuring heat capacities of solids or liquids from 60° to 300° K. A brief discussion of the basic theory involved in chemical thermodynamics and the problems involved in obtaining accurate experimental data is presented. The operation of the calorimeter was tested by measuring the heat capacity of a sample of benzoic acid obtained from the National Bureau of Standards over a temperature range of 60° to 300° K. The measured heat capacity values of the benzoic acid compared favorably with similar values obtained by the Bureau of Standards, the maximum deviation being 0.5 percent. THEORY A brief discussion of the basic theory involved in chemical thermodynamics will illustrate the applications of heat capacity data and the problems involved in obtaining accurate experimental data.

Jan 1, 1962

By T. E. Gray

This report describes the preparation characteristics of the significant coalbeds in Nicholas County, W. Va. It is one in a series describing coals suitable for producing metallurgical coke, either as mined or after beneficiation. Almost 5 million tons of coal were produced in Nicholas County, W. Va., in 1960, of which over 2.6 million tons were cleaned in eight preparation plants. It has been estimated that over 6 billion tons remained in the county as of December 31, 1960, in beds 12 inches and more thick.

Jan 1, 1962

By D. Bienstock

As part of the development of the hot-carbonate scrubbing process by the Bureau of Mines, the corrosion rates of steel in boiling solutions of potassium carbonate saturated with carbon dioxide and hydrogen sulfide were determined, and the effectiveness of various inhibitors was evaluated by Bureau researchers. The highly corrosive solution of carbonate saturated with carbon dioxide can be inhibited with a 0.2-percent concentration of either potassium chromate or sodium metavanadate. Solutions of carbonate saturated with carbon dioxide and hydrogen sulfide are mildly corrosive, 0.01 inch per year. Complete absence of corrosion is obtained with 0.2 percent sodium metavanadate or 0.15 percent vanadium pentoxide. Oxidizing inhibitors such as potassium chromate are destroyed in the alkaline sulfide mixture, N-alkyl trimethylene diamines, at a concentration of 0.1 percent, lower the corrosion rate to about 0.005. Sodium metasilicate, at a concentration of 0.6 percent, completely inhibits the corrosion but may deposit free silica in the system. Commercial cladding materials such as the epoxy coatings also prevent corrosion.

Jan 1, 1962

By S. R. Borrowman

Physical beneficiation, leaching, and solvent extraction investigations were made to recover a high-grade thorium oxide product from Bald Mountain, Wyo., conglomerate. The monazite in the Bald Mountain deposit contains 8.8 percent Th02 and, therefore, is higher in thorium content than the usual domestic or foreign monazite. A sample of composited drill cuttings for the study contained 4.3 pounds of monazite per ton of are. The work showed that the monazite, although unusually fine grained and friable, could be concentrated by tabling and magnetic treatment to yield a product assaying 5.65 percent Th02 with a recovery of 61 percent of the thorium. Subsequent decomposition of the concentrate by treatment with sulfuric acid and solvent extraction of the resultant solution with a primary aliphatic amine yielded a thorium oxide product of 99-percent grade.

Jan 1, 1962

By A. C. Rice

Investigation of a variety of mines to determine efficiency for rare- earth extraction has resulted in a solvent extraction technique wherein Primene 81-R,4 N-benzylheptadeeylamine (BHDA), and Primene JM-T give favorable extraction from sulfate solutions. Extraction from chloride, nitrate, and perchlorate solutions is negligible. Distribution coefficients for 10 rare-earth elements with Primene 81-R establish an extraction sequence beginning with lanthanum and proceeding through lutetium according to atomic number. Yttrium and ytterbium are exceptions in the extract ion sequence.

Jan 1, 1962

By A. A. Cochran

Methods of preparing small heats of steel containing radioisotopes were developed, and the techniques of stripping film autoradiography were used to detect and study the carbide and sulfide phases in titanium-bearing steels. Metallography had revealed areas of titanium sulfide and ferrite or pearlite adjacent to areas of titanium carbide and ferrite, and unidentified, irregular phases at the boundaries between these two areas. Sulfur 35 was used to deter-mine the extent of the titanium sulfide inclusions, and carbon 14 was used to delineate the titanium carbide phase. Individual radioactive areas were located with a resolution of approximately 10 microns. A general background exposure that was not correlated with microscopically visible phases was observed in the carbon 14 autoradiographs. The evidence from both sulfur 35 autoradiographs and carbon 14 autoradiographs indicated that the unidentified inclusions were sulfides rather than carbides. INTRODUCTION The use of radioisotopes to facilitate the work at the Rolla Metallurgy Research Center was expanded in fiscal year 1959 when the Bureau of Mines authorized the installation of an intermediate-level radioactivity laboratory. Before this time, sealed cobalt 60 sources had been employed for radiography, but no tracer work was done. The primary objective of the first experiments conducted in the new laboratory was to supplement physical metallurgy investigations of selected problems in steel research.

Jan 1, 1962

By William J. Campbell

The purpose of this investigation was to extend the analytical services which are required for Bureau of Mines programs in developing and evaluating high-purity materials. Determination of trace elements in minerals and ores as an aid in geochemical evaluation and prospecting was considered. Serious consideration should be given to the merits of using the avail- able fluorescent X-ray spectrographic instrumentation and techniques for determining trace elements. Limits of detectability for trace elements in metal, oxide, solution or mineral samples range from 0.1 to 100 p.p.m, depending on the element being determined, overall sample composition, and the complexity of the X-ray spectra; limits of detectability range from 0.01 to 1 microgram for elements that have been preconcentrated by a chemical or physical process, for example, by ion-exchange membrane.

Jan 1, 1962

By H. D. Kline

This publication describes methods and techniques of mining and crushing limestone at 3 of 11 small quarries operated by Anderson-Oxandale Rock Co. in northeast Kansas in 1959. It is one of a series of reports by the Bureau of Mines on methods and costs of mining in various mining districts in the United States. The three quarries selected for study -Bosse quarry, Pottawatomie County; Hansen quarry, Morris County; and Huston quarry, Dickinson County (fig. 1) -were in many respects similar to many others that had been developed solely to fill local and usually transitory demands for crushed limestone for use as concrete aggregate, roadstone, and soil conditioning. Factors governing the choice of quarry sites were quality of limestone, shallow overburden, and proximity to points of consumption of the crushed stone.

Jan 1, 1962

By J. G. Donaldson

Optimum conditions are given for chloridizing pyrite, marcasite, chalcopyrite, arsenopyrite, stibnite, and covellite with chlorine gas. The formation of metal chlorides is affected by the time and temperature of chloridizing, and by particle size of the sample. Chloridizing data also are given for chemically precipitated antimony (III) sulfide and copper (II) sulfide.

Jan 1, 1962

By L. F. Willmott

Pulverized high-volatile A bituminous coal was gasified with oxygen and superheated steam in a pressure-gasification pilot plant equipped for slurry feeding. The minimum ratio of water to pulverized coal that could be pumped satisfactorily as a slurry was about 1 to 1. Heating this slurry produced a suspension of coal in superheated steam having a steam-to-coal ratio greater than the 0.3 to 1 proportion that is considered optimum for pressure gasification of pulverized coal. A steam separator removed enough steam to provide ratios down to about 0.5 to 1, but a 0.3 to 1 ratio was not achieved. Gasification of Sewickley coal produced a synthesis gas containing about 36 percent H2, 46 percent CO, and 13 percent CO2, Gas output, gas composition, and coal and oxygen requirements were Virtually the same as for a pilot plant equipped for fluidized-coal feeding. Typical results from the slurry-fed plant at 300 psig were carbon gasified, 95 percent; coal requirement, 34 lb/M (thousand) std cu ft CO + H2 produced; oxygen requirement, 365 std cu ft/M std cu ft CO + H2 produced. The results showed that the two feeding methods are equally satisfactory from the standpoint of gasification. A choice between a fluidized-coal gasification process or a slurry gasification process depends on considerations relating to the coal-feeding phase itself, including capital and operating costs, manpower requirements, safety, and flexibility of operation.

Jan 1, 1962