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By John Nagy

Dust explosion data obtained in laboratory studies by the Bureau of Mines are presented for activated carbon, asphalt, charcoal, carbon black, coal, coke, gilsonite, graphite, lignite, miscellaneous carbons, pitch, tunnel dust, and mixtures of these materials with other ingredients. The explosion hazard is shown to increase as the volatile content of the dusts increases.

Jan 1, 1965

By Robert M. Becker

This report (part 3 of a five-part series) presents computer programs for evaluating moments and moment relationships of the generalized probability distributions extended or developed in parts I and 2. The principal program is for evaluating the first three moments and moment relationships of the compound-multinomial distribution for finite as well as for infinite populations. This is the generalized distribution for sampling to some amount of items per sample. Another program is for evaluating the first four moments, the moments of the mean, and the moment relationships of the multinomial and generalized hypergeometric distributions. This is a general moment program in sampling to some number of items per sample or for sampling to some number of samples. This program will accept either ungrouped data, frequency data, or probability data.

Jan 1, 1965

By H. Dolezal

An investigation was made on the use of magnesium for the direct reduction of rutile to make low-cost, offgrade titanium which could be upgraded to an acceptable grade of metal by electrorefining. Reductions made with charges containing magnesium chloride under hydrogen yielded products with oxygen con-tests close to the theoretical equilibrium composition. Two reduction products were made from rutile for use in electrorefining amenability tests: (1) a product from reduction in an inert atmosphere which contained 88.9 percent titanium and 4.42 percent oxygen, and (2) a product from reduction in a hydro-gen atmosphere which contained 92.5 percent titanium and 2.40 percent oxygen. Reduction products obtained under both of these conditions were amenable to electrorefining.

Jan 1, 1965

By A. A. Sonnek

A simple, portable helium analyzer was developed primarily for field use. Its utility lies in making preliminary surveys before exact analyses are required. The analyzer is based upon chromatographic principles; that is, separation of gas mixtures resulting from variable retention times of the components with respect to a separation medium (column-packing material). It uses thermistors for sensing detectors, a dry battery as source of power, and a micro-ammeter for indicating helium concentration. The absolute accuracy of the instrument depends upon the recency and care with which the instrument is calibrated with a standard gas. The unknown gas should be analyzed immediately after calibration, and another calibration should be made before another unknown sample is analyzed. The instrument is simple to operate, requiring approximately 15 minutes, after calibration, to determine the helium content of a natural gas sample. Although developed primarily for helium determination, the analyzer possibly can be used for other analyses that can be performed at ambient temperatures.

Jan 1, 1965

By J. G. Eisele

Solvent-extraction characteristics of dodecyl phosphoric acid (DDPA) were investigated to determine its potential as a fractional or selective extract-ant for individual elements in a rare-earth-yttrium mixture. The DDPA is an effective extractant for splitting rare-earth mixtures into light and heavy subgroups. Yttrium normally extracts with the heavy rare-earth elements but may be shifted toward an extraction sequence with the light rare-earth elements by increasing the pH. Elements in the light and heavy ends of the rare-earth series can be separated from middle-group rare-earth elements by using diethylenetriaminepentaacetic acid (DTPA) as an aqueous phase counter-extractant. Hydrogen-ion dependency of the distribution coefficients differs from that reported for similar systems at tracer-level concentration.

Jan 1, 1965

By George L. Gates

The Bureau of Mines developed a rapid instrumental method of analyzing oil well scales containing primarily barium sulfate. After removal of oil and water by carbon disulfide) the scale was dissolved in strong hydrochloric acid. The cations, barium, calcium, strontium, magnesium, and iron, were determined with the flame photometer using the method of additions. Sulfate was deter-mined colorimetrically after separation by selective adsorption on an alumina column. Phosphate was determined colorimetrically and carbonate titrimetrically. The method was reasonably accurate, although iron and magnesium were found to have mutual interference.

Jan 1, 1965

By Jr. Frank Parrish

This report describes the performance of 17 selected water-injection projects producing from Pennsylvanian-and Permian-age reservoirs. Illustrations depict reservoir structure and thickness, and production and injection history. A selected bibliography of publications pertaining to area oil recovery and geology is included. Tabulations of field and reservoir data reveal marked differences in the projects. Increased oil recovery resulted from injecting water in most cases; however, seven projects recovered less oil than the operators anticipated. Oil recovery by water injection ranged from 0.2 to 262 bbl per acre ft, or 0.1 to 22.5 pct of the initial stock-tank oil in place. Major reasons suggested for poor performance include: (1) Adverse directional horizontal permeability, (2) channeling of injected water through fractures or zones of high permeability, and (3) lack of containment of injected water. One 330-foot-deep project is among the first successful shallow water-floods in north Texas. Another project is the first successful Canyon sand-stone waterflood reported in the area. Previous gas injection in two Cisco sandstone projects did not prevent the reservoirs from responding favorably to waterflooding.

Jan 1, 1965

By Robert L. Marovelli

The thermal conductivities of six rocks were measured by the transient line source method over the temperature range of -850 to 1,500° F. Close-fitting ceramic probes were used in 0.065-inch-diameter holes drilled through 5-to 6-inch-thick rock specimens. Taconite, granite, quartzite, and basalt were used in the tests. The method yields absolute data and is applicable to both laboratory and in situ measurements.

Jan 1, 1965

By S. J. Gasior

A method for destroying the caking properties of bituminous coal was developed by the Bureau of Mines. Coal is treated in a fixed bed by heating through its plastic range under controlled temperatures in mildly oxidative atmospheres composed of inert gas and/or steam containing about 1 volume-percent oxygen. High-volatile A (hvab) and high-volatile B (hvbb) and low-volatile bituminous (lvb) coals in the size range 1/8 to 1-1/2 inches were successfully treated at 0 (atmospheric pressure) to 300 psig in static beds 6 to 18 inches deep. Conditions of treatment depended on the coal and ranged from 80 to 200 minutes at 350° to 510° C. Char produced in this manner from hvab coal was gasified with steam at 800° C and 100 psig in a fixed bed in one series of tests and in other tests was exposed to hydrogen in a dilute co current free-falling-bed system at 750° C and 3,000 psig without agglomerating.

Jan 1, 1965

By Albert W. Deurbrouck

The performance of four sand cones was evaluated by the Bureau of Mines in three preparation plants that utilized cones in various flow schemes. The cone at plant A was a simple two-product one that provided clean coal and refuse. Plant B had two cones; one cone made a primary separation and the other a secondary separation. The primary cone separated salable coal from heavy rejects. The secondary cone separated a low-ash metallurgical coal and an intermediate-ash product suitable for plant fuel or steam markets. In plant C the sand cone was equipped with a middlings draw Which continually removed an intermediate specific-gravity product below the surface of the cone. The three primary separations of raw coal effected between floats and sinks were excellent. The recovery efficiencies for the plus 1/4-inch material ranged from 99.8 to 97.6 percent, the error areas ranged from 19 to 23 square centimeters, and the probable errors in specific gravity ranged from 0.033 to 0.024. The performance data of the two secondary separations varied from excellent in plant B, where the separation was on a par with the primary separations, to somewhat inferior in plant C, where the secondary separation was effected at the middlings draw.

Jan 1, 1965

By Manuel Gomez

The heat contents of thermally dried lignite, subbituminous B coal, and their corresponding low-temperature chars were determined at various temperatures below the highest temperature to which these materials had been exposed before testing. Similar studies were made on high-temperature char and coke, spent shale, and ash prepared from both coal and spent shale. Heat content of the carbonaceous materials tested correlated well with temperature. Heat con-tent results for spent shale compared well with the published results. Statistical analysis of experimental data together with published information showed moisture, volatile matter, carbon content, and temperature to be the principal variables influencing the specific heat of coal. The specific heat of devolatilized carbonaceous substances, char and coke, approached that of graphite as the carbonization temperature was increased. The elemental specific heats of coal constituents, estimated from the ultimate analysis and the specific heat of coal, compared favorably with published elemental specific heats.

Jan 1, 1965

By W. S. Landers

This report presents a detailed study of low temperature, entrained-bed carbonization of an Australian coking coal. The coal studied was high-volatile B bituminous from the Foybrook mine, an open-cut operation in the Liddell seam, New South Wales, Australia. Carbonization was conducted in an 8-inch diameter, continuous vertical reactor at several temperatures from 960° to 1,300° F. It was demonstrated that this bituminous coal can be carbonized within this temperature range to produce tar and a nonagglomerated char, without prior oxidation or char recirculation. Carbonization rates from 138 to 287 lb/hr (as-carbonized basis) were investigated. It was found that the carbonization temperature and the air-to-coal ratio must exceed minimum values to insure continuous operation. At the higher air-to-coal ratios employed, all or most of the carbonization heat was provided by internal combustion with air in the reactor. At the lower air-to-coa1 ratios, part of the heat for carbonization was supplied externally. On the moisture-and ash-free basis, the yield of tar plus light oil ranged from about 26 to 44 gallons per ton, and the char yield ranged from approximately 1,160 to 1,370 pounds per ton. The heat in the gas ranged from about 900 to 3,000 Btu/lb of moisture-and ash-free coal. Carbonization product yields correlated well with air-to-coal ratio and carbonization temperatures. The volatile matter in the char was found to be temperature dependent. At 1,300° F carbonization, the volatile matter in the char was 8.7 percent (dry basis), whereas at 9600 F carbonization, the residual volatile matter was about 16 to 18 percent (dry basis).

Jan 1, 1965

By A. J. Forney

Recent experiments used catalysts of plate assemblies in synthesizing high-Btu gas and gasoline indirectly from coal. A gas with a heating value of 925 to 943 Bt-: per cubic foot has been prod u la the hot-gas-recycle pilot plant from synthesis gas (3H2+100) with lathe turnings used as catalyst in the first reactor, and assemblies of parallel sprayed plats of nickel in the second. Solid plates made of Raney nickel, and steel and aluminum plates sprayed with Raney nickel or nickel oxide were tested. Those catalysts had very low resistance to gas flow; 90 percent lower than nickel granules used in previous experiments. In a single stage of synthesis thee nickel plates were only partially successful. Although the heating values of the product gas ranged from 856 to 941 Btu per cubic foot, the carbon monoxide content of he gas was above 0.1 percent. Both steel and wrought turnings were tested in single-stage synthesis, but the conversion of hydrogen and carbon monoxide was too low to attain the desired heating value of 900 Btu per cubic foot in the product gas. Assemblies of plates thermally sprayed with fusel iron were tried in an experiment to make gasoline. A gasoline yield of 52 percent (of the hydro¬carbons produced) was obtained using a 1H2-10O feed These sprayed assemblies were in service for 1,500 hours, the longest that this type of catalyst has been used. When a second reactor containing Raney nickel catalyst was added in series with the first reactor, complete utilization of the feed gas was obtained because in addition to the liquid product, a high-Btu gas with a heating value of 800 Btu per cubic foot was made.

Jan 1, 1965

By John W. Buch

Hydraulic cutting tests made on samples of Pennsylvania anthracite (3,700 psi and 260 gpm) were promising enough for the Bureau to establish a full scale experiment in an anthracite mine. Water pressure and quantity for mining anthracite were arbitrarily established at 5,000 psi and 300 gpm (1,000 hp). For full-volume flow, hydraulic pressure is controlled by orifice size with the displacement pump. The hydraulic jumbo was designed for maneuvering on pitches from 0° to 20° in any direction and for a coalbed ranging in thickness from 10 feet 6 inches to 15 feet. All motions of the jumbo are by oil hydraulics. Jet flow is controlled (start-stop) at the face, through an interlocked pushbutton system. One button is in the operator's cab; one, at the pump station; and one (a safety shutoff), near the mining face. To December 1962, 7,400 tons of bed material had been mined at an average rate of 0.800 ton per minute, with an average power requirement of 14.125 kilowatt-hours per ton. In January 1963, the objective was changed from an engineering-development basis to a research basis--to determine, ultimately, the most efficient level of operating characteristics for maximum response, as measured by mining-out rate. This research phase of the project is not yet complete, but conclusions, and the method of arriving at them, will be made the subject of another Bureau publication. It should be noted that as of December 1963 nearly 13,000 tons of bed material had been mined, at rates as high as 1. 3 tons per minute for a complete face advance.

Jan 1, 1965

By C. C. Popoff

This report reviews the phosphate deposits, mines, and industry, and prospects in 10 districts covering most of the Montana phosphate field. These districts are discussed individually, and an evaluation of the resources and potential of each is presented. Phosphate rock produced from underground mines in the Garrison district is shipped to Canada for processing to fertilizers, utilized locally for production of animal feed supplement, and pulverized and sold for direct application to the soil. Production from the Melrose district is shipped to Silver Bow and processed to elemental phosphorus. The Maxville-Philipsburg district is destined to become a major producer with the development of the Douglas Creek mine and beneficiation plant by Montana Phosphate Products Co. Montana ranks fourth after Florida, Tennessee, and Idaho in total annual production in the United States. Production him increased from about 60,000 long tons of acid-grade phosphate rock in 1940 to more than 660,000 tons of acid-, beneficiation-, and furnace-grade ore in 1961. Montana has the second largest potential resources in the Western field; in the area south of Butte there are approximately 1.2 billion tons of phosphate rock (+18 to +31 pct P2O5) available above and within 100 feet below entry level; and in the northern part of the field there are about 67.6 million tons available above entry level. In contrast to Idaho, most of the phosphate deposits in Montana are best suited to underground mining.

Jan 1, 1965

By A. W. Henderson

This investigation was performed to develop chlorination methods for extracting tungsten from scheelite and from an ore concentrate containing a mixture of scheelite and wolframite. On a laboratory scale with proper temperature control using elemental chlorine, over 90 percent extraction of tungsten is achieved. Carbon and sulfur dioxide were studied as reducing agents. The effects of salts such as calcium fluoride and sodium chloride were studied as additives to increase extraction and to reduce impurities in the volatile tungsten chloride product. Sodium chloride reacts with ferric chloride to form a nonvolatile double salt; whereas the chlorides and oxychlorides of tungsten are volatile and consequently condense free of iron. Separation of tungsten from molybdenum from an equal molar mixture was successful by fractionally distilling the oxygen-free chlorides and by selectively condensing the oxychlorides. Yields of 60 and 80 percent, respectively, were achieved for separating the less volatile tungsten chlorides containing less than 0.5 percent molybdenum.

Jan 1, 1965

By Lars Osen

This investigation was undertaken to contribute to the understanding of underground pull tests by conducting laboratory tests under closely controlled conditions. Steel bolts, instrumented with electrical resistance strain gages, were anchored in an aluminum block, a granite block, and a steel sleeve, and were subjected to pull tests. The bearing plates used were either flat7 dished, or embossed. In pull testing a bolt that is prestressed, there is a range of loading during which bolt load is greater than the jack-applied load, This study showed that preload, the size, shape, and type of bearing plate; and the geometry of the system determine the point at which bolt load and applied load become equal. The effects on bolt load of both a theoretical solution and actual pull tests were analogous and led to similar results.

Jan 1, 1965

By John W. Sweeney

Shales and clays from Illinois were sampled, tested, and evaluated to determine feasibility of producing lightweight aggregate by rotary-kiln methods. Sampling procedures and the 1 ,,,y of the Pennsylvanian shale units are discussed. Chemical, X-ray spectrographic and X-ray petrographic analyses were run on the samples to determine if a correlation existed between chemical mineralogic composition and expansion. Preliminary expansion testing was conducted in a muffle furnace. Rotary-kiln tests were conducted in a 16- inch by 14-foot rotary kiln. The weight of the aggregate ranged from 27 to 59 pounds per cubic foot. Concrete cubes employing the aggregate were tested to determine the qualities of the concrete. Compressive strength of the concrete using the 7-bag of cement cement per cubic yard mix, after autoclave curing for 6 hours, ranged from 2,950 to 6,750 psi. No correlation was found between the chemical, X-ray spectrographic, and X-ray and petrographic analyses and expansion, Sixteen samples made suitable lightweight aggregates in the laboratory rotary kiln. The expansion temperature range of eight of the samples was extremely narrow, and difficulties would probably be encountered in processing these materials commercially.

Jan 1, 1965

By G. W. Birge

Fifteen coal samples, representing the Winifrede, Chilton, Alma, No. 2 Gas, Powellton, Eagle, Douglas, Sewell, Beckley, Pocahontas No.4, and Pocahontas No.3 beds in Wyoming County, and five samples, representing the Fire Creek, Pocahontas No.6, and Pocahontas No.3 beds in Mercer County, W. Va., were carbonized at 9000 C by the Bureau of Mines-American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Expansion characteristics of the majority of samples were determined in the Bureau of Mines sole-heated oven. Chemical analyses and agglutinating values were determined for all coals. The coals were mostly strongly coking and low in ash and sulfur content. Dry, mineral-matter-free fixed-carbon content of the Wyoming County coals ranged from 63.0 to 83.4 percent. The Mercer County samples were all low volatile in rank. Yields of carbonization products were generally in accord with yields from similar rank coals of the Appalachian region. Because of their expanding tendencies, most of the medium-and low-volatile coals would require blending with lower rank coal for normal coke production.

Jan 1, 1965

By Stephan Stecura

Crystallographic modifications and kinetics of solid-state phase trans-formations were determined for five rare-earth" sesquioxides--La2O3, Nd2O3, Sm2O3, Eu2O3, and Gd2O3. Oxides used for crystal modification studies were prepared by thermal decomposition of the following high-purity salts of the five rare-earth elements--carbonates, chlorides, fluorides, nitrates, oxalates, and sulfates. X-ray diffraction patterns of the cubic and hexagonal oxides were indexed by a graphical method and patterns of the monoclinic oxides by Ito's method. The kinetics of crystallographic transformation were determined by high-temperature X-ray diffractometry. The kinetic data were interpreted using a shrinking sphere model. All of the transformations followed first order kinetics. Activation energies were calculated by application of the Arrhenius equation. These solid-state phase inversions were concluded to occur by a reconstructive transformation mechanism.

Jan 1, 1965