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By L. O. Bacon

This Bureau of Mines report summarizes the results of laboratory work in the design of instrumentation for obtaining the dynamic tensile strength of rock at minimum loading. Minimum loading is defined as the lowest tensile loading by pulse reflection to cause fracturing. The instrumentation for obtaining dynamic tensile strengths of rock cores evolved into the use of a compressed-air pellet gun to impact one end of a rock core, suspended by wires, at increasing increments of air pressure. Maximum strain was measured on most or all of the impacts, and the strain at fracture of the core was obtained by extrapolating the pellet velocity-strain curve to the pellet velocity at fracture. Stress at tensile fracture was obtained from the maximum s train, and the dynamic Young's modulus was calculated from the rod velocity by using simple rod theory.

Jan 1, 1962

By Charles B. Kenahan

Application of ultrasonics in the electrolytic deposition of metallic manganese and manganese dioxide from sulfate electrolytes had several effects. Ultrasonics produced finer-grained deposits of electrolytic manganese at all current densities than obtained in normal cell operation, but at high current densities it resulted in less adherent deposits. Ultrasonic radiation did not affect cell voltage or cathode current efficiency. In the electrodeposition of manganese dioxide at 70° C., ultrasonic-; increased the current efficiency and decreased the cell voltage at a current density of 9 amperes per square foot, but it had little effect at current densities above this. The decrease in cell voltage was caused by the depolarizing action of ultrasonics at both anode and cathode. Ultrasonic radiation produced a smooth, glossy, adherent, and pit-free deposit at all current densities and at each temperature. Radiation had no effect on current efficiency or cell voltage at 90° C. Ultrasonics was more effective than conventional agitation in producing all of these effects.

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 S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions 5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1962

By David Burgess

Natural gas is a general term applied to the gas obtained from oil or gas wells. It is the most widely used of all gaseous fuels. The principal disadvantage in the use of this and other gaseous fuels is the difficulty encountered in the storage and transportation of large quantities in the gas state. Handling in the liquid state is possible, but reduced temperatures are required since methane (table 1) is the principal component of most natural gases that are used as fuels. Actually, liquid storage has been utilized both here and abroad;3 however, the Cleveland disaster4 has pointed out the need for a critical evaluation of the hazards involved in the storage of this cryogenic fuel. Accordingly, a program was undertaken to obtain basic data that could be used to assess these hazards. In this report, the factors to be considered in an evaluation of the fire and explosion hazards associated with any fuel are each discussed briefly. These factors are then used to assist in the design of experiments for the evaluation of the hazards associated with liquefied natural gas (LNG) relative to those associated with other common fuels. Experiments have been conducted on the vaporization of LNG, the mixing of LNG vapors with air, the effect of temperature and nitrogen dilution on the limits of flammability of methane in air, the burning rates of LNG and other fuels, flame radiation, and extinguishment of fires above liquid pools. Based on the results of these experiments, LNG can be stored safely in suitably designed above-ground tanks surrounded by earthen dikes in much the same manner as gasoline.

Jan 1, 1962

By R. V. Lundquist

This report describes results of tests on the desilication of solutions resulting from the leaching of lime-soda sinters. Desilication was accomplished by heating the solutions in an autoclave. A liquor relatively free of silica was obtained after 30 minutes of heating at 200 p.s.i.g. in the presence of lime. The addition of lime improved desilication, but the rate and efficiency of desilication was effected by the quality of lime used. The optimum quantity of lime for effective desilication was about 6 grams per liter. A lesser quantity gave poorer desilication, and a greater quantity increased the alumina loss without improving desilication. The alumina loss was approximately proportional to the lime added. A complex structure, called artificial noselite in this report, was the only silica bearing compound detected in the desilication precipitate. Other compounds present were Ca(OH)2 (calcium hydroxide), CaCO3 (calcium carbonate), and Ca [A1(OH)6]2 (hydrated tricalcium aluminate). Sodium carbonate in the leach liquor retarded the formation of the calcium aluminate; hence it decreased the alumina lost to the precipitate. The extraction of alumina from aluminum silicate materials by the limestone soda-sinter process has been investigated by the Bureau of Mines for many years. The process consists of the following major operations: Blending the aluminum silicate with limestone and soda ash in such proportions that dicalcium silicate and sodium aluminate are formed on sintering; leaching the sinter in a carbonated caustic solution to extract the soluble alumina; purifying the leach liquor by the precipitation of soluble silica (this precipitate is designated desilication precipitate in this paper); precipitating alumina trihydrate from the purified liquors by carbonating with carbon dioxide gas; and calcining the trihydrate to alumina. Commercial grades of

Jan 1, 1962

By R. C. Bates

Uranium mine workers? daily exposure to radon daughters was estimated by two methods of sampling, detailed and spot-check. Both methods involve time- weighting measured exposure levels to arrive at an average exposure figure. Random sampling, or sampling without regard for the duration of exposure, has proved inadequate for estimating average exposure levels. During the first phase of the study, the breathing zones of eight workmen in three underground uranium mines were sampled for an entire shift; 20 to 36 radon-daughter samples were collected per man-shift, Analysis of these data indicated that a suitably accurate estimate of the full-shift exposure could be made by time weighting a considerable lesser number of representative radon-daughter samples. This analysis led to the spot-check method of estimating full-shift exposures to radon daughters. Additional detailed studies were made in seven mines to Learn more about the full-shift radon-daughter exposures and to test the spot-check method, In all, 617 radon-daughter samples were taken in 10 underground uranium mines during 26 man-shifts, and the spot-check method was tested 35 times.

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 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 J. D. Brown

The electron optics, vacuum system, and sample stage assembly for the Bureau of Mines? electron probe X-ray spectrograph were purchased. Four scanning curved-crystal spectrometers, two reflection- and two transmission-type, were designed and constructed by the authors. The reflection spectrometers are placed in a vacuum chamber for measurement of long-wave-length X-radiation. Detection, pulse-amplitude discrimination, and recording circuits are provided for the simultaneous measurement of four X-ray spectral lines. Minimum spot size is approximately 2 microns in diameter at 30 kilovolts and a sample-to-ground current of 5 x 10-8 ampere. At this voltage and current the limit of detection with reflection spectrometers is less than 0.05 weight-percent for most elements. The limit of detection for elements determined by transmission-type spectrometers, evaluated at 35 kilovolts and 5 x 10-8 ampere, is approximately 0.1 weight--percent for all elements having excitation voltages below 20 kilovolts. In general, reflection spectrometers exhibited satisfactory but poorer resolution than the transmission type, resolution of the spectrometers being limited primarily by crystal imperfections, with greater mosaic structure being introduced by the grinding process for the reflection crystals. Several applications of the electron probe X-ray spectrograph are described. Analysis of a uranium-steel is discussed in detail to illustrate calculation of composition from measured X-ray intensities.

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 William J. Campbell

Evaluation by the Bureau of Mines of published expansion values for magnesium oxide shows significant variation in values, which may be attributed to sample variables, experimental errors, or systematic differences between measuring techniques. To eliminate the sample variable in measuring expansion, thermal expansion characteristics of a high-purity polycrystalline magnesium oxide were determined by 21 cooperating laboratories using one or more of the following techniques; X-ray camera, X-ray diffractometer, dilatometer, interferometer, and telemicroscope. All expansion values were corrected by the author to a single reference temperature of 25° C. Linear expansion was expressed as a power series in the form of the following equation. Expansion (percent) = [[ A + B (?t) + C (?t)2] ?t 104] The constants, A, B, and C, were determined by least square techniques for X-ray camera, X-ray diffractometer, and dilatometer data separately, and for combined data of all five techniques. Expansion values are tabulated from 26° C. to 1,400° C. in 2° C. intervals using constants derived from X-ray camera data. Below approximately 500° C., expansion values obtained by dilatometric and interferometric methods are significantly lower than those by X-ray methods; above 500° C., this bias decreases rapidly. Comparison of results within methods showed the least variance for X-ray camera results; dilatometer and X-ray diffractometer results have about the same variance. The average deviations, in percent, between observed and calculated expansion values among methods were approximately 10 percent from 100°C. to 300°C., 5 percent from 300°C. to 500°C., and 2 percent from 500°C. to 1,400°C. Maximum deviations were approximately twice as large in most instances.

Jan 1, 1962

By D. F. Walsh

A study of damping capacity was made on a number of magnesium-base alloys, commercial types and experimental compositions. Hardness and tensile properties were determined, and the microstructure of each alloy was examined. Alloys of low yield strength, in general, possessed high damping ability. A correlation was established between damping capacity and composition.

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 Richard D. Graves

Pitch from low-temperature carbonization of bituminous coal was hydrogenated at cracking conditions in a continuous bench-scale unit to produce low-molecular-weight oils and tar acids. The pitch contained 15.6 pct benzene-insoluble material, 4.0 pct hexane-soluble oil, and 80.4 pct asphaltene by weight. At 475° C, 7,500 psig, and 1.5 hours residence time, hydrogenation products, based on the weight of pitch, were about 36 pct oil boiling below 325° C, 24 pct hexane-soluble heavy oil, 17 pct asphaltene, 1 pct benzene insolubles, and 12 pct hydrocarbon gases. The yield of tar acids boiling below 250° C was 4.3 pct, and the yields of C6 to C8 paraffins, naphthenes, and aromatics were each less than 1.0 pct. The yield of tar acids was within the range of yields obtained by hydrogenation or high-temperature carbonization of bituminous coal (2 to 5 wt pct). Yields of oil boiling below 325° C increased with increased residence time or temperature. There was little or no effect of residence time on yields of alkali- soluble material which contained tar acids. Yields of hydro-carbon gases increased markedly with an increase in temperature from 475° to 500° C. Lowering the hydrogen pressure to 4,500 psig resulted in yields similar to those obtained at 7,500 psig.

Jan 1, 1962

By Raymond W. Hiteshue

To aid in designing a continuous system for evaluating processes for converting coal to high-Btu gas] the Bureau of Mines determined the amenability of various coals and a char to hydrogasification at 800° C and 6,000 psig using a molybdenum catalyst. A lignite from Rockdale, Tex., an hvCb coal from Rock Springs, Wyo., a char from the low-temperature carbonization of the latter, an hvAb coal from Pittsburgh, Pa., and an anthracite from Luzerne County, Pa., were selected. Highest yields of gaseous hydrocarbons, 94 pet, based on maf feed, were produced from char, and lowest yields, 67 pct, were obtained from lignite. Hydrocarbon gases contained 82 to 92 pct methane, 8 to 15 pct ethane; and 1 to 3 pct propane.

Jan 1, 1962

By A. J. Forney

The hot-gas-recycle process, for the hydrogenation of carbon monoxide, was investigated in a 12-inch-diameter reactor. Initially because the distribution of gas was poor, hotspots developed in the catalyst bed. After the velocity profile of the gas flowing through the bed was studied, the method of packing the catalyst was altered. Because this change improved the distribution of gas, temperature control was excellent. The l2-inch-diameter reactor was operated successfully in the synthesis of gaseous and liquid fuels. When high-Btu gas was synthesized in two stages, parallel-plate assemblies of Raney nickel were almost as active as granular Raney nickel in the second reactor. The pressure drop through the second reactor, however, was reduced 90 percent by the use of these assemblies.

Jan 1, 1962

By James A. Whelan

The Bureau of Mines sponsored research studies of variables in rotary drilling, done in the Department of Mineral Engineering, University of Minnesota. By studying carefully controlled drilling with good instrumentation, it was hoped to obtain a better understanding of rock failure during drilling and of the stresses in drill bits during drilling. Experimental procedures and equipment are described. From these studies it was concluded that 1. Thrust requirements, other things being equal, are proportional to the total length of cutting edge in the bit. 2. Data from penetrating a wedge into rock under thrust only are not directly applicable to rotary drilling. 3, In rotary drilling the initial wear on a bit greatly decreases penetration rate under any given set of conditions; however, after initial wear the effect of wear on penetration rate is reduced. 4. An increase in rotary speed increases the overall penetration rate but decreases the penetration per revolution. 5. An increase in thrust increases the overall penetration rate and the penetration per revolution. 6, Torque on a drill bit is proportional to both penetration rate and bit diameter. 7. For small-diameter holes full-hole drilling will save both drilling time and energy compared with pilot drilling followed by reaming; for large-diameter holes pilot drilling-reaming is advantageous in both respects,

Jan 1, 1962

By W. W. Weller

This report provides low-temperature heat-capacity data and entropies at 298.15° K. for magnesium metavanadate (MgV206) and magnesium pyrovanadate (Mg2V207). The work completes low-temperature measurements planned for alkaline-earth vanadates; an earlier report dealt with calcium vanadates.4 No similar data for these compounds have been published previously. Free energy of formation values at 298.15° K. were derived by combination of the present entropy values with heat of formation data. MATERIALS The materials used in the measurements were portions of the samples described in a previous Bureau of Mines publication by King, Koehler and Adami.5 Methods of preparation, chemical analyses, and X-ray examinations are covered in this paper. The indicated purity of the samples was 99.9 pct.

Jan 1, 1962

By R. Barany

The heats of formation at 298.15° K of calcium tungstate, calcium molybdate, and magnesium molybdate were determined by solution calorimetry. For the heats of formation from the elements, the values obtained were calcium tungstate, -402.4 ± 0.5 kcal/mole, calcium molybdate, -369.5 ± 0.3 kcal/mole, -334.8 ± 0.2 kcal/mole. For the heats of formation from the oxides J the values obtained were calcium tungstate, -49.2 ± 0.4 kcal/mole, calcium molybdate, -39.6 ± 0.1 kcal/mole, and magnesium molybdate, -12.9 [ ] 0.1 kcal/mole.

Jan 1, 1962