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By Albert W. Deurbrouck

Twelve samples from six Barbour County coal beds were analyzed for this report. The samples collected were generally high sulfur content coals, frequently exceeding 3 percent in the raw-coal sample. Many of them could not be upgraded to acceptable metallurgical standards even by rigorous preparation procedures. The production of coal in the county in 1963 amounted to almost 3 million tons of which 44 percent was mechanically cleaned.

Jan 1, 1965

By L. B. Pankratz

Heat contents, measured above 298.15° K, and derived entropy increments are presented in tabular and equation form for the two crystalline forms of zinc sulfide (sphalerite and wurtzite) and for four solid solutions of iron and zinc sulfides having the compositions Zno.,,6Fe0.302S, Zno.750Fe0.250S, Zno.650Fe0.3505, and Zno.498Feo.502S.

Jan 1, 1965

By J. G. Walters

Analyses of light oils produced from the fluidized carbonization of coal at 485°, 550°, 600°, and 660° C are presented. Tar vapors from 485 C fluidized carbonization were thermally treated at 600°, 700°, and .800° C, and the analyses of light oils produced by this treatment are also presented. Procedures were developed for analysis of coal carbonization light oil by gas chromatography to permit a more definitive analysis than can be obtained by the conventional distillation procedure. An increase in low-boiling olefins, benzene, and toluene, a decrease in low-boiling paraffins, and little change in the remainder of the aromatics was observed with increased temperature of carbonization.

Jan 1, 1965

By Henry M. Harris

The Bureau of Mines investigated a glass containing approximately 17 percent lithia and 83 percent silica to establish a method of devitrifying cast and rolled shapes. Glass shapes with high strength were made by melting, forming, and rapid cooling of the composition, and the shapes subsequently were converted to a crystalline condition by heat treatment. The best devitrification schedule included rapid cooling of the glass to below 300° C, followed by reheating at a rate of 50° to 400° C per hour, depending on the size of the shape, followed by a of 60 to 70 hours at 500° C and another period of 15 hours at 800° C. attempts to use faster heating rates or slow cooling to accomplish devitrification in deformation of the shapes. The crystalline shapes had flexural strengths that averaged over 33,000 psi, achieved with an annealing time of 60 to 70 hours at 500° C.

Jan 1, 1965

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 John D. Corrick

The environmental and nutritional characteristics necessary for maximum copper extraction from a low-grade ore by Ferrobacillus ferrooxidans have been explored as have many of the limiting parameters. Criteria considered were oxygen consumption, copper extracted, soluble copper concentration, temperature, pH, particle size, nutrients, and other inorganic salt concentrations. A set of environmental and nutritional conditions were developed for E. ferrooxidans Which supported cell reproduction and maximum microbial oxidation of a low-grade copper sulfide ore. Percolator tests conducted under these optimum conditions resulted in an 18 percent increase in the quantity of copper microbially extracted over that extracted under conditions considered to be standard. Manometric tests determined those extremes of environmental conditions and nutritional factors Which were detrimental to the extraction of copper by E. ferrooxidans.

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 P. L. Woolf

An investigation was conducted to evaluate the use of a formcoke as the total fuel in the Bureau of Mines experimental blast furnace. The formcoke performed very satisfactorily, and comparisons made with a metallurgical coke showed that the performance with the formcoke was somewhat superior under the experimental conditions used.

Jan 1, 1966

By A. W. Deurbrouck

Four samples of Pittsburgh-bed coal, of various size consist and ash content were dewatered in a pilot-size vacuum-disk filter partially enclosed with a steam jacket. Steam fed at 2.5 to 12.5 pounds per minute reduced the moisture content of the filter cakes from 2.8 to 13.8 percentage points more than normal vacuum dewatering. Approximately 1.5 pounds of steam was required to remove 1 pound of water.

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 Jr. Taylor

The following heats of solution have been measured in 1.160 molal H2SO4 at 25° C: AH298, kcal./mole Be(c) + 77.44(H2SO4?47.849 H2O) H2(g) + BeSO4 (soln) -92.83 ± 0.11 BeSO4 ?(c) + 77.44 (H2SO4?47.849 H2O) BeSO4(soln) -16.45 ± 0.02 BeSO4?2H2O(c) + 77.44(H2SO4?47.849 H2O) BeSO4?2H2O(soln) -5.395 ± 0.019 BeSO4?4H2O(c) + 77.44 (H2SO4?47.849 H2O) BeSO4?4H2O(soln) 1.513 ± 0.010 Combining these data with other experimental results and data taken from National Bureau of Standards information yielded the following heats of formation at 298° K:

Jan 1, 1966

By R. W. Dalzell

The performance characteristics, efficiency, and operating pressure of jute line-brattice systems were studied under varying underground conditions; various fabric grades and installation methods were used. The test results indicate that line-brattice system efficiency is dependent upon the method of ventilation the method of installation, porosity of fabric, and size of tight rib area.

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 E. G. Davis

The Bureau of Mines made laboratory-scale experiments to examine the technical possibilities of reclaiming manganese from slags produced by oxygen lancing of high-manganese pig iron. Ferromanganese was added to molten pig iron to yield a 4-to 5-percent manganese hot metal, which simulated a product obtainable from the blast furnace. This was injected with oxygen to reduce the metal to 1 percent or less manganese and form a slag containing about 40 percent manganese. The molten slag was water-quenched, treated with H2SO4) roasted at 660° C, and water-leached to give soluble manganese and iron sulfates. The sulfates were precipitated as hydroxides, converted to the oxide form, and smelted to produce a standard ferromanganese containing 74.6 percent Mn and 0.01 percent P. As an alternate method of manganese recovery, a manganese cell feed was prepared from the leach solutions and electrolytic manganese was produced. Direct smelting of the high-manganese slag resulted in 74.2 ferromanganese meeting ASTM specifications except for phosphorus content. The high phosphorus content of the metal and high slag-to-metal ratio obtained made this approach unattractive.

Jan 1, 1966