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By E. J. Kloos

The Bureau of Mines devised a new machine-test method for measuring carbon dioxide inspired by a wearer of self-contained breathing apparatus. The new method compares favorably in speed and precision with standard man-tests in which the apparatus is tested while actually worn, and is scheduled for use in future approval tests for facepiece carbon dioxide 'measurements. However, man-tests will still be used to measure the efficiency of the carbon dioxide sorbent materials in closed-circuit breathing apparatus.

Jan 1, 1966

By C. W. Schultz

The vapor pressure of manganese in equilibrium with a series of liquid iron-manganese alloys was determined by the carrier gas method over a broad range of alloy composition. From these data the activities of manganese in the iron-manganese system were calculated. The system appears to be ideal.

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 Jr. Koch

Statistical methods applied at the Bureau of Mines Denver Mining Research Center to data from metallic ore bodies were used to evaluate lignite reserves from core data and to predict the extent of lignite horizons in some Texas lignite beds. Six lignite seam units were studied using data from 361 drill holes. The data indicate a total of 214.2 million tons of lignite in the area examined, and probable reserves of 113 million tons in an area 2,000 feet beyond the limits established by the drill holes. It was demonstrated that lignite reserves present in lenticular beds could be reliably determined by statistical techniques, and that core drilling could be optimized to maximum information with minimum drill holes. The technique described is applicable to other coal beds.

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 Albert F. Baker

Techniques were developed and circuitry was assembled for measuring the total and volume resistances to the flow of electric current through solid specimens of anthracite. The two-, three-, and four-terminal test methods demonstrated the extreme sensitivity of resistivity to differences in anthracite characteristics and showed response to changes resulting from variations in structure, temperature, and moisture content.

Jan 1, 1966

By Jr. Sharkey

The Bureau of Mines investigated gases from flash and laser irradiation of Pittsburgh seam (hvab) coal to determine the action of high temperatures on coal. Temperatures in excess of l,000° C were reached with both types of irradiation. Craters about 300 microns in diameter were produced in the coal with millisecond pulses from the laser unit rated at 1.7 joules' output. Gaseous products from laser and flash irradiations in vacuum contained 21 and 8 percent acetylene, respectively. Diacetylene, vinylacetylene, and other products to molecular weight 130 were indicated in the mass spectrum of the gas from the laser study. Single experiments were also conducted in which the laser energy, particle size of the coal, and atmosphere were varied. The results indicated that the distributions of products obtained from the flash and laser irradiations of coal were different from that produced in high-temperature carbonization.

Jan 1, 1966

By J. E. Zeilinger

The technical feasibility of using energy from explosive ignitions of coal dust to pump water was .demonstrated in an exploratory investigation. Ignition of small amounts of pulverized coal that were dispersed in air over columns of water pumped up to 5.3 gallons of water per cycle when operated against a head of 30.75 feet. Water displacement was accomplished by either manual or automatic operation through a single cycle, and by automatic operation through a continuous series of cycles of I-minute duration. Operating through single cycles, slurries containing up to 3 pounds of coal and 4.6 gallons of water were also pumped. Possible uses of an efficient coal-fired pump would include pumping water for irrigation purposes, removing water from mines, transporting coal from mines in the form of a slurry, and pumping water to elevated reservoirs at electric powerplants so that it could be used to generate electricity during peak periods of demand.

Jan 1, 1966

By Alvin Kaufman

To aid industry and Government in planning water developments the Bureau of Mines in 1963 canvassed mineral producers to determine water use in 1962. Water use by the mineral industry comprises only 2 percent of the water withdrawn by industry as a whole. The major water-using mineral industries are natural gas processing, phosphate rock, sand and gravel, and iron ore. Analysis indicated the following conclusions: 1. Total water use and new water intake is dependent on the quantity of material processed and the process water requirements of the particular industry or commodity. 2. Recirculation is dependent on the processing requirements of a particular commodity, the manner in which the water is used, cooling and condensing requirements in certain large industries, the quality of new water intake, and the need to treat new and discharged water. 3. Consumed water is dependent on the quantity of water recirculated, the temperature and humidity in the area, and the proportion of water used for cooling and condensing. 4. A threefold increase in water use by the mineral industry by 1985 is forecast.

Jan 1, 1966

By P. E. Churchward

The Bureau of Mines developed a process using amines for recovering tungsten as ammonium paratungstate from alkaline leach liquors without producing synthetic scheelite as an intermediate product. Over 90 pct of the tungsten in low-grade scheelite or ferberite concen-trate was recovered as ammonium paratungstate by (l) autoclave leaching the concentrate with Na2CO3, (2) solvent extraction of the acidified leach liquor with kerosine solutions of either a quaternary amine (Aliquat 336) or a primary amine (Primene JM-T), (3) stripping the tungsten values from the quaternary amine with ammoniacal NH4C1 or from the primary amine with NH4OH, and (4) crystallization of ammonium paratungstate from the strip liquor. Reagent consumption in pounds per pound of W03 recovered was, for the quater¬nary amine, 3 Na2CO3, 3.5 H2SO4 , 2.2 NH4Cl, 1 NH3, and 0.4 glacial acetic acid; for the primary amine, it was 3 Na2CO3, 3.5 H2SO4, .06 NH4Cl, and 0.9 NH3. Both reagents extract molybdenum along with tungsten. Silicate and phosphate are partly extracted and contaminate the product; leach liquors containing these impurities require preliminary purification.

Jan 1, 1966

By L. C. Marchont

This Bureau of Mines report tabulates data on nitrogen-gas reservoirs and isolated occurrences of inert gases in several Williston basin oilfields. Recoverable reserves of nitrogen gas in the Minnelusa nitrogen interval within the areas of five oilfields on the Nesson anticline in North Dakota are estimated at about 1.27 trillion standard cubic feet, based on computer analyses of logs from over 300 wells. This volume of nitrogen represents a large source of high-pressure inert gas and warrants consideration of possible application in oil-production operations. Drill-stem tests made in two of the fields indicated that nitrogen can be produced at rates up to 28 million cubic feet per day.

Jan 1, 1966

By H. J. Coleman

Knowledge of the types of naturally occurring sulfur compounds in petroleum is of both theoretical and practical interest to petroleum chemists and geologists. This knowledge has been extended by the identification of 77 sulfur compounds, including 36 thiols, 23 chain sulfides, and 18 cyclic sulfides in a 111° to 150° C boiling range distillate of Wasson, Texas, crude oil. The characterization procedure used in separating and identifying these compounds included isothermal distillation, vacuum fractionation, liquid-solid chromatography (alumina adsorption), chemical treatment, gas-liquid chromatography, microdesulfurization, and infrared analysis. The procedural steps described represent a systematic method of sulfur compound analysis considered applicable for determining the nature and concentration of the sulfur constituents present in any straight-run petroleum distillate of the above-boiling range.

Jan 1, 1966

By James W. Myers

The Bureau of Mines studied factors affecting ignition of coal mine refuse and on methods for control of burning. Laboratory experiments showed that air permeates more readily through segregated than through nonsegregated refuse and that air permeability is greater through coarse than through fine particle refuse. Minus 3-1/4-inch refuse ignites spontaneously more readily than minus 1/4-inch refuse. The burning of a 1,000-pound conical coal pile was con-trolled by capping with an 18-inch-thick layer of minus 1/4-inch refuse containing 37 percent combustible. In field trials, the burning of refuse at operating mines was controlled by capping with a layer of fine refuse. Water, applied as a spray or by injection, quenched surface flames and cooled the burning waste. Inspection of refuse piles at operating mines showed that the spontaneous ignition tendency is affected by the exposed surface relative to the total volume and the segregation of particles during dumping.

Jan 1, 1966

By Jerry W. Ramsey

The Bureau of Mines studied two Pennsylvania anthracites using low-temperature carbon dioxide adsorption. A modified form of the Brunauer-Emmett-Teller equation was used to calculate specific surface areas. Two mesh sizes of each anthracite were used to determine how gamma irradiation at 106 and 108 rads, both in vacuum and in the presence of air, affected the carbon dioxide surface areas. Results show that anthracites have a system of pores that are essentially all interconnected rather than isolated; that anthracites differ from one another in specific surface, which may correlate with density; and that irradiation in vacuum has no discernible effect on specific surface of anthracite, but irradiation in air does produce changes in specific surface.

Jan 1, 1966

By F. E. Griffith

Cost data are given for five methods of secondary backfilling of strip mines previously partially backfilled. The operations were conducted in north-central Pennsylvania; an average of 600 linear feet of highwall were backfilled in each trial. Major obstacles and the relative merits of the methods are discussed.

Jan 1, 1966

By M. M. Wong

Salt mixtures consisting of KC1, BaC12, and HfCl4 with RbCl or CsCl were investigated as electrolytes for refining hafnium. The presence of RbCI or CsCl in the electrolyte appeared to suppress the volatility of. Best electrorefining was obtained with an electrolyte containing 50.7 percent KCl, 27.l percent BaCl2, 15.7 percent CsCl, and 6.5 percent HfCl4. In this electrolyte, hafnium metal with an average oxygen content of 470 ppm was produced from an anode feed containing l,600 ppm oxygen. All metallic impurities were lowered, except titanium, manganese, and tin.

Jan 1, 1966

By C. J. Thompson

This Bureau of Mines study describes the preparation of sulfur compound concentrates boiling from 225° to 400° C, and reports the sulfur types detected in these concentrates by low-voltage mass spectrometry (LVMS). Existing LVMS methods were extended; the procedures described should be generally applicable to high-boiling petroleum distillates and concentrates as a preliminary means of narrowing the number of factions to be considered for more detailed separation and identification studies. The following major sulfur compound constituents of petroleum are indicated by the data: benzothiophenes, dibenzothiophenes, naphthanothiophenes, naphthenobenzothiophenes, and homologs and isomers of these. Cyclic and chain sulfides comprise a significant portion of the gas-oil range sulfur compound types. The presence of some classes of sulfur compounds containing two sulfur atoms per molecule was indicated.

Jan 1, 1966

By James Paone

The Bureau of Mines studied the behavior of rocks at the initial state of crater formation that results from the stresses created under a drill bit to determine which mechanical properties of rock are important in rock fragmentation by drilling. Although a definite relation between the drilling strength and relevant mechanical properties has not been established, maximum yield strength of rock is apparently a parameter of drillability of rock. The strengths of rock were considered from the Mohr-Coulomb criterion from which the surface of failure was constructed. The results from previous tri-axial tests on Solenhofen limestone were adopted to verify the criterion of failure. Inelastic behavior of some rock types was observed under a low-velocity impact of a hemispherical bit and under static indentation with a similar bit. Quantitative determinations of strengths of Solenhofen limestone) Indiana limestone, and Tennessee marble were made under static indentation. The maximum yield strength estimated from the average stress over the indented area was used as the crushing strength of rock under a drill bit.

Jan 1, 1966

By R. W. Van Dolah

The Bureau of Mines t.ced its investigations into sympathetic detonation of ammonium nitrate (AN) and ammonium nitrate-fuel oil (AN-FO) to define the scaling law for safe separation from detonating AN-FO. Both missile- and non-missile-producing AN-FO donors, weighing up to 5,400 pounds, were employed with acceptors of the same size. The usual cube-root scaling law was not confirmed; exponents for the relationship S = f(Wx) for AN were 0.51 with non¬missile-producing donors and 0.61 for missile-producing donors. For AN-FO an exponent of 0.80 was indicated in the missile-producing case. AN-F0 in polyethylene bags appeared somewhat more easily initiated than bulk AN-FO. The efficacy of barricades in protecting AN charges was investigated. detonation distances were reduced from one-third to one-seventh when filled barricades were employed. The investigation was extended to dynamite with both types of donors. With 1,600-pound missile-producing donors and an equivalent weight of dynamite, initiation would be expected in 50 percent of the trials at 167 feet. The corresponding value in the non-missile case was 67 feet. The data developed in this program of sympathetic detonation will allow the development of a rational set of safe separation distances for AN, AN-FO, and explosives.

Jan 1, 1966

By H. R. Babitzke

To develop alloys suitable for use at elevated temperatures, columbium and tantalum were combined with tungsten, hafnium, vanadium, zirconium, and titanium, and the resulting alloys were evaluated with respect to fabricability, hardness, Electrical resistivity, strength at elevated temperatures, oxidation resistance, and bend transition. Of the 23 compositions tested, Cb-2OHf-5W-10Ti exhibited superior high-temperature properties. A recrystallized sample of this alloy was fabricable at room temperature, had a strength of 44,000 psi at 1,200° C, and had an oxidation rate of only 7.7 mg/cm2/hr at 1,000° C.

Jan 1, 1966