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By J. P. Hansen

Wustite beds were reduced with carbon monoxide and mixtures of hydrogen and nitrogen in the temperature range 900° to 1,300° C to determine the effect of temperature, gas flow, and surface area on the rate of reduction to iron. The composition of the gas stream as it passed through the wustite bed was continuously measured with infrared absorption cells and heated-wire methods. The change in composition was used to calculate the reaction rates. Arrhenius plots of the data give heats of activation of 34 kcal for particles using CO, 27 kcal for particles using H2, 24 kcal for pellets using C8, and 6 kcal for pellets using H2. The velocity of reduction is dependent on the area of reacting interface and the driving potential of the gas (reducing gas concentration minus equilibrium concentration) as well as the exponential temperature effect. The reaction rate was independent of the gas velocity over the range of conditions studied.

Jan 1, 1965

By J. G. Donaldson

Cobalt-tungsten binary deposits were formed in laboratory experiments by hydrogen reduction of the anhydrous mixed vapors of cobaltous chloride and tungsten hexachloride. The materials were sublimed in seperately heated zones of reaction tube and were transported in a stream of purified helium into the deposition section of the tube where the chloride gases were reduced to metal by a countercurrent flow of hydrogen. Heattreating of the near stoichiometric binary metallic deposits converted nearly all to the intermetallic compound Co3W, however, small quantities of both cobalt and tungsten remained. Mechanical tests showed that the tensile strength of heat-treated 75 percent cobalt-25 percent tungsten deposits was twice as high as that of similarly treated deposits of cobalt.

Jan 1, 1965

By W. L. Acherman

Molybdenum, tungsten, and vanadium were found by the Bureau of Mines to possess generally superior chemical and galvanic corrosion properties in many aqueous corrosive media at temperatures up to the boiling point. The corrosion resistance of vanadium in certain solutions was further improved by alloying it with such metals as columbium, tantalum, and titanium. was susceptible to a type of crevice corrosion in mercuric chloride solutions, but no other instances of crevice corrosion were encountered. With few exceptions, molybdenum, tungsten, and vanadium were not adversely affected when coupled with dissimilar metals in galvanic corrosion experiments; in some cases one or both members of a couple were protected by contact. When exposed to aqueous ammonia spray at 60° C, all three metals were attacked, but they were moderately resistant in spray environments of substitute ocean water and ammonium dihydrogen phosphate.

Jan 1, 1966

By E. A. Loria

The Bureau of Mines analyzed the effects of oxygen, nitrogen, and carbon on the tensile properties of electrorefined vanadium in terms of the Petch equation. The effects of the different impurities and grain sizes on the yield and flow stress between 2730 and 770 K were studied. For specimens of like composition, the values of the Petch parameters 01 and ky obtained by two different methods, extrapolation and grain size, were nearly the same. For high-purity electrorefined vanadium, the 01 value at 2730 K was 10,300 psi (5,150 psi shear). The 01 values for this metal at 1950 and 2730 K were lower by factors of 3 to 4 than for three less pure samples of commercial vanadium metal of equivalent grain size. Nitrogen was more effective than oxygen in increasing 01' the increase being about twice as much for the same impurity level. Carbon produced a slight increase in 01 up to 0.024 percent and then a gradual decrease in 01 to 0.11 percent, the maximum carbon content studied. The corresponding ky values followed the same trend in regard to oxygen and nitrogen additions, whereas the addition of carbon produced no variations at either temperature. Dislocations in vanadium are anchored by carbon, oxygen, and nitrogen with increasing firmness in that order. The high purity of electrorefined vanadium was confirmed by low yield stress and high ductility throughout the low temperature range. The metal also exhibited profuse twinning with high ductility at 1230 and 770 K. The effective surface energy for fracture, y, was found to lie between 3.3 and 3.6 x 1()4 erg cm-2?

Jan 1, 1966

By R. T. Sorensen

Research and testing in a small scale equivalent of a commercial flota-tion plant was completed on four low-grade, iron-bearing materials from the western Mesabi range. Closed circuit-flotation of calcium-activated silica with fatty acid collector developed data for comparison with the batch process and highlighted problems not evident from previous bench testing. The four ore samples contained from 27 to 39 percent Fe and were equally represented by nonmagnetic taconite and semitaconite type materials. Iron concentrates containing 6.0 percent, or less, SiO2 were made 5, all four samples. Of the two material types, the semitaconite was the ore amenable to treatment, yielding iron recoveries of about 90 percent as cc pared with 70 to 80 percent for the other. Pilot plant tests showed that concentrate grade made in batch tests could be duplicated in the closed circuit and demonstrated that the amount of recoverable middling iron varied considerably between ore samples. The continuous tests also showed that water temperature strongly influenced results in the treatment of one ore but apparently was of indifferent consequence in another. Progress in thickening and filtration of flotation concentrates was made through introduction of tapioca flour to serve the dual role of iron mineral depressant and flocculant.

Jan 1, 1966

By Jr. Jacobson

Thermal reactions of l-methylpyrrole, l-butylpyrrole, and l-isopropyl-pyrrole were investigated by a flow method in the temperature range of 4500 to 5750 C. Those of I-butylpyrrole and l-isopropylpyrrole were also investigated in the 3400 to 4000 C range in a static system. The I-substituted pyrroles isomerize by an irreversible reaction to 2-substituted pyrroles. A reversible isomerization reaction shifted the alkyl group from the 2-to the 3-position on the pyrrole ring. All of the isomerization reactions are homogeneous, unimolecular, nonchain, first-order reactions having similar mechanisms and transition states. There is decomposition and cleavage of the longer alkyl side chain when it is in either the 2-or 3-position giving, as products, pyrrole, 2-and 3-methylpyrrole, 2-and 3-ethylpyrrole, pyridines, and hydrocarbons. The decomposition reactions appear to be by free-radical mechanisms. Pyridine homologs are formed by the expansion of the alkylpyrrole: butylpyrrole produces pyridine, and isopropylpyrrole produces 3-methylpyridine. Approximate Arrhenius equations are given for the formation of the decomposition products.

Jan 1, 1966

By W. H. Oppelt

Two exploratory gasification tests of limited duration were made at Dorsten, Germany, with strongly coking Pittsburgh-bed coal in a fixed-bed pressure gasifier. To reduce the coking potential of the Arkwright coal, ash refuse from the gasification of Dorsten (Leopold) coal was added to pre-pare coal-ash mixtures which contained nominal 20 and 30 percent ash. Major adjustments in principal process variables at the beginning of the tests resulted in wide fluctuations in the rate of gas production, gas offtake temperature, and carbon dioxide concentration in the gas. Because a higher steam-to-oxygen ratio was used in the tests than was customarily employed for routine operation, gas production was lower, and steam and oxygen consumption was higher. After operating conditions had been improved, the results of a 12~-hour-long test with addition of sufficient ash refuse to obtain a nominal 30 percent ash concentration indicated that operation is feasible with this coal mixture using a fixed-bed pressure gasifier equipped with a rotating coal distributor and stirrer.

Jan 1, 1966

By Foster Fraas

A separator for minerals of low magnetic susceptibility and fine particle size in a water suspension is described. A ring-shaped matrix of ferromagnetic fragments rotating so as to pass successively through magnetic-field and field-free regions provides for the separation. Application is illustrated in the separation of hematite and ilmenite from quartz.

Jan 1, 1966

By J. P. Morris

A diphenyl ether calorimeter for measuring high-temperature heat contents of ferrous alloys and iron-and steelmaking slags was constructed and calibrated with specimens of molybdenum, alumina, and platinum that were heated to temperatures ranging from 1,720° to 1,875° K. The standard deviation of the calibration measurements was 0.37 percent. By measurements of the enthalpy of delta and liquid iron, the heat of fusion of iron was found to be 3,298 ±100 cal per mole.

Jan 1, 1966

By Raymond L. Lowrie

Coal deposits in the Boulder-Weld County coalfield in Colorado are analyzed in relation to economic factors governing the growth, stability, and competitive potential of the coal industry. Recoverable reserves, estimated to be 571 million tons, are discussed in detail, particularly those in the Erie and Frederick Quadrangles. Geology of the coal measures, quantity and quality of water resources, and chemical and physical properties of the coal are described. Coal production factors, including mining techniques and equipment, labor requirements, transportation facilities and rates, and markets, are considered for coal's position in competition with alternate fuels. Growth of the fuels market, through increasing thermal-electric power generation in the Denver Metropolitan Area, will stimulate coal production in Colorado. Reserves of the contiguous Boulder-Weld coalfield, if mined in a sustained, year-round, high-tonnage operation, could be used to supply much of that fuel demand.

Jan 1, 1966

By Alla D. Mah

Compilation of data on materials of metallurgical interest is one of the important activities of the Berkeley Thermodynamics Laboratory of the Bureau of Mines. Recent renewed interest in metallurgy of vanadium renders the present compilation a timely guide for experimentation to improve present methods or to develop better methods of extractive metallurgy. Thermodynamic data for vanadium and its inorganic compounds have been critically surveyed, selected, and compiled into one convenient reference from which information can be readily obtained for evaluating heat balances, determining trends, and establishing limits of metallurgical processes. By indicating the direction of experimentation, this report enables the saving of time, effort, and expense which would otherwise be necessary for trial and error experimentation. Much of the data has been obtained experimentally at the Berkeley laboratory. Other data were collected through an extensive survey of worldwide literature through April 1965. Estimates were made when no data were avail-able. Data on the vanadium halides was sparse, and the results derived from existing data were at times divergent. Some of the selected values for the halides may need modification as more or better experimental data become available.

Jan 1, 1966

By James S. Browning

Research by the Bureau of Mines demonstrated that organic heavy liquid adhering to or adsorbed on fine mineral particles can be effectively removed by a novel method embracing pulping or displacement washing with hot water alone or in combination with a detergent. Displacement washing with steam alone or in combination with a detergent also was effective for removing the heavy liquid. In tests of sized minus 48-plus 200-mesh mineral charges, both the hot water washing with detergents and detergent steaming effectively reduced the heavy liquid losses on the particles to about 0.2 pound per ton of mineral or less. Centrifuging of the wash solutions permitted an almost complete recovery of heavy liquid from the solution as a pure heavy liquid product.

Jan 1, 1966

By Frank A. Peters

The Bayer process treating Jamaican bauxite was evaluated from an economic standpoint, using standard estimating methods and published data, to present a reference point for cost estimates for nonbauxite alumina processes. The estimated operating cost for a plant producing 1,000 tons of alumina a day is $47.96 per ton of alumina when charging $8 per ton for bauxite and $2.30 per hour for direct labor. The estimated fixed capital cost is $46 million.

Jan 1, 1966

By Louis A. Panek

Determining the change of stress in rock based on measurements of the deformation of a drill hole is a procedure that is increasing in popularity. A closely related procedure involves the applicat10n of this principle to determine the existing stresses in a rock medium, by cutting free (core drilling) an annulus containing the drill hole. In this Bureau of Mines report, expressions are derived from which one can calculate the stress ellipsoid--the three-dimensional change of stress, or the existing three-dimensional stress field, as the case may be. Study of these equations shows that the stress components in three dimensions can be determined by measurements in only two drill holes, and yields general principles that are useful in planning an efficient program of drilling and measurement. Procedures are given for calculating the least squares estimates of the stress components and their standard errors, and for evaluating or comparing calculated values by means of standard statistical inferences.

Jan 1, 1966

By D. C. Crowell

This publication presents the results of a laboratory investigation of displacement of gas by injection or imbibition of water into sandstone models under essentially isobaric conditions. A brief discussion of scaling requirements is included. The influence on residual gas saturation of independently varying the parameters of dimensional ratios of the porous media, rates and methods of flooding, surface tension, initial water saturation, and permeability is shown. Of these variables, increased initial water saturation and decreased surface tension reduced residual gas saturation significantly, whereas variations in flooding rate and dimensional ratios had no apparent effect. No correlation was evident between absolute permeability and residual gas saturation.

Jan 1, 1966

By Bernard Porter

The rate of the heterogeneous reaction between high-purity uranium metal and uranium tetrafluoride in molten lithium fluoride was measured. The apparent heat of activation for the reaction is 16.91 kilocalories per mole of UF4. A surface-controlled mechanism is suggested in which UF4 is adsorbed on the uranium metal surface. Additional UF4 reacts with the adsorbed species and the metal site to form an activated complex that decomposes to the product UF3. The reaction is an important source of metal loss in the electrowinning of uranium metal.

Jan 1, 1966

By W. L. Falke

Procedures in which manganese compounds are reduced and the metal is volatilized and selectively condensed, a hitherto neglected area, were investigated. More than 95 percent of the manganese was recovered from high-melting-point ores whether vacuum volatilization or atmospheric pressure volatilization was used, but neither process is economically attractive under present price-cost conditions.

Jan 1, 1966

By W. L. Falke

This Bureau of Mines report illustrates critical path planning and scheduling techniques as applied to typical mining operations. Detailed examples of arrow diagramming and computer oriented applications of critical path methods are given. Program Evaluation and Review Technique (PERT) is discussed briefly in comparison to the Critical Path Method (CPM).

Jan 1, 1966

By Albert W. Deurbrouck

The preparation characteristics of the coals of Buchanan County, Va., are described in this Bureau of Mines report. Twenty-one samples ,,,ere collected from 9 coalbeds in the county. Of these samples 13 were of metallurgical quality as received, and 8 required some upgrading to provide acceptable products. In general, the coals were of low to medium ash and sulfur content, and ranked as medium-to high-volatile bituminous. In 1963, production in the county was in excess of 13 million tons, of which 2.2 million tons were mechanically cleaned.

Jan 1, 1966

By Norman G. Foster

The mass spectra of four tertiary butyl substituted thiophenes are reported. A comparison and contrast with earlier structure correlations made by API-RP48 mass spectroscopists is presented. The fragmentation routes of these types of molecules are discussed and explained in terms of existing theories in mass spectrometry. Low ionization voltage data are presented to support the mechanistic picture developed. Structures are inferred about some of the ions, and these are correlated with existing theories. Metastable peaks in the spectra are used to support the fragmentation paths. The presence of doubly charged ions in the spectra is noted and the possible implications toward mechanisms discussed. The general picture of simple, small fragments leaving the ion moiety upon further fragmentation is developed in detail. Some suggestions are presented for further work utilizing isotopically labeled molecules to establish firmly the general picture of fragmentations of the alkylthiophenes.

Jan 1, 1966