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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 Richard C. Ballance

Fly ash from four sources and in certain proportions was shown to assist chemical coagulation of turbid water and settling of chemically induced floc. Fly ash reduced the time required to form the first visible floc, promoted more uniform flocs about 2 mm in diameter, and increased the mean settling rate of floc particles. Also, the addition of fly ash produced denser sludges than those obtained with alum alone. Final turbidities were independent of fly ash particle size and carbon content. Optimum proportions of fly ash additive are given.

Jan 1, 1966

By C. Ortuglio

The Bureau of Mines developed equations to determine the relationship of yields and products obtained from BM-AGA carbonization in 13-and l8-inch-diameter retorts. The developed equations indicate that results of carbonization in l8-inch-diameter retorts can be predicted from results obtained with l3-inch-diameter retorts.

Jan 1, 1966

By D. E. Wolfson

Twenty-two samples of West Virginia coals 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. Eighteen samples represented the Coa1burg, No. 2 Gas, No. 2 Gas and Peerless, Powellton, Eagle, Big Eagle, Lower Eagle, Sewell, Fire Creek, and Pocahontas No.6 beds in Fayette County, and four samples represented the Sewell and Fire Creek beds in Greenbrier County. Expansion characteristics of the majority of samples were determined in the Bureau of Mines sole-heated oven. Chemical analyses were determined for all coals. The coals in Fayette County are high-volatile A, medium-volatile, and low-volatile in rank, and the Greenbrier coals are medium-volatile in rank. Most of the coals are chemically suitable for metallurgical coking. All coke strength indices are within acceptable limits for metallurgical coking coals. All the high-volatile A coals contracted and the medium-and low-volatile coals expanded in the sole-heated oven expansion test.

Jan 1, 1966

By R. Barany

The heats of formation of seven substances were determined by solution calorimetry. At 298.15° K, the heat of formation of lithium sulfate from lithium, rhombic sulfur, and oxygen was -343.1 ± 0.7 kcal/mole, and the heat of formation of lithium sulfate monohydrate from lithium, rhombic sulfur, oxy-gen, and hydrogen was -414.3 ± 0.7 kcal/mo1e. For the silicates, the heats of formation at 298.15° K from the elements were kaliophilite, -503.8 ± 0.5 kcal/mole; leucite, -721.6 ± 0,8 kcal/mole; eucryptite, -505,2 ± 0.6 kcal/mole; alpha-spodumene, -727.9 ± 0.9 kcal/mole; and beta-spodumene, -721.1 ± 0.9 kcal/mole. The corresponding heats of formation at 298.15° K from the constituent oxides were kaliophilite, -42.7 ± 1.1 kca1/mole; leucite, -42.8 ± 1.1 kcal/mole; eucryptite, -16.1 ± 0.7 kcal/mole; alpha-spodumene, -21.0 ± 0.7 kcal/mo1e; and beta-spodumene, -14.3 ± 0.7 kcal/mo1e.

Jan 1, 1966

By A. W. Deurbrouck

The Bureau of Mines analyzed 13 samples collected from three Randolph County coalbeds. The Peerless and Sewell bed samples were generally of metallurgical quality as received from the mines or could be easily upgraded. How-ever, the Lower Kittanning coa1bed samples proved to be quite inimical to upgrading to metallurgical quality.

Jan 1, 1966

By E. K. Kleespies

The Bureau of Mines demonstrated a technique for electrowinning titanium from titanium nitride and titanium dioxide. Titanium-nickel-copper metal solutions containing 26 to 61 weight-percent titanium were prepared by electrolyzing titanium nitride in molten mixtures of potassium fluotitanate) and sodium chloride or barium chloride and depositing titanium on nickel-copper cathodes. A titanium-nickel alloy was prepared by electrolyzing titanium dioxide in an electrolyte of potassium fluotitanate) sodium fluoride) and calcium fluoride and depositing titanium on solid nickel cathodes. This alloy contained 21 weight-percent titanium and had a combined oxygen-carbon content of less than 0.1 weight-percent. A compartmented cell confined the oxide feed near the anode and inhibited oxygen contamination of the metal.

Jan 1, 1966

By Richard F. Link

A statistical technique, useful to analyze assay and other data characterized by location in three dimensions, is described in this Bureau of Mines report. If present, trends in the data are defined for the purposes of improving ore estimation, predicting ore beyond existing workings, and aiding geological interpretation. The technique is to fit linear and quadratic polynomial equations to the data through the statistical method of regression analysis. The fitted linear equations have the geometric form of hyperplanes; the fitted quadratic equations have the geometric form of ellipsoids or elliptic hyperboloids of one or two sheets. To visualize these three-dimensional forms, contour maps of a series of plane sections through the fitted surfaces are plotted. Both the fitting of the polynomial equations and the plotting of the con-tour maps are done by electronic computer to facilitate calculations and to obtain accurate results. Computer programs are described in appendixes. Methods employed are illustrated by an example analysis) based on data from a part of the Fresnillo mine) Zacatecas, Mexico.

Jan 1, 1966

By Robert K. Koch

The Bureau of Mines investigated separating HF from HF-SiF4-H2O mixtures by passing the mixed gases through a sodium fluoride slurry in an airlift scrubber and forming a mixed precipitate of NaHF2 and Na2SiF6. The oven-dried precipitate was thermally dissociated in two stages. The first stage was carried out at 400° C and dissociated NaHF2 to NaF and HF. Condensation and analysis of the evolved HF proved it to be 97 to 99 weight-percent HF containing 0.79 to 0.99 weight-percent H2O and 10 to 93 ppm silicon. The second stage was carried out at 700° C and dissociated Na2SiF6 to NaF (for recycle) and SiF4. The quantity of HF recovered from gaseous HF-H2O-air mixtures decreased with increasing relative H2O concentrations. Air was beneficial when scrubbing extremely dilute wet HF gases. At HF partial pressures of 0.24 and 0.013 mm Hg in the scrubber entrance gases, HF partial pressures of 6.2 x 10-4 and 9 x 10-6 mm Hg were obtained, respectively, in the scrubber exit gases. Scrubber efficiencies were 99.7 and 99.3 percent.

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

This report shows the feasibility of predicting drillability, analytically, by using regression analysis techniques. The approach is new in diamond-drilling research. Further, the study shows that this technique may be of value to drill manufacturers and others in mathematically delineating performance characteristics of new drills in specific rock types. Another application might be the prediction of penetration speeds in extraterrestrial material based on the physical properties of the materials as samples become available. Prediction equations for penetration rates are presented for 9 rocks drilled in the laboratory and for 20 rocks drilled under field conditions. The prediction equations are based on drill operating parameters and on characteristics of the rock penetrated. No single physical property appeared consistently in the best predictor equations, and all the physical properties were found to be highly correlated with each other.

Jan 1, 1966

By Ralph Husack

The Bureau of Mines investigated the effect of gamma radiation on reactions between Pennsylvania anthracite and fluorine and chlorine. In the tests with fluorine about 90 percent of the coal reacted at 350° C to form volatile products whether or not irradiation was employed. Up to 0.8 ml of liquid products per gram of anthracite was collected. Among the 25 com-pounds indicated by gas chromatography, fluoroform and l,l-difluoroethylene were tentatively identified from their relative retention times and perfluoro-cyclopentane from its infrared spectrum. In addition, a clear, hard, wax, probably a fluorocarbon, was formed at 45° C in both the presence and absence of radiation. With chlorine there was no significant difference due to radiation, and preliminary tests indicated that the chlorine reacted more with the organic matter of anthracite at 200° C than with inorganic matter. At 400° C the results were inconclusive because of excessive corrosion in the reaction vessel.

Jan 1, 1966

By E. S. Shedd

The Bureau of Mines investigated electrowinning and tapping lanthanum metal from lanthanum oxide in a fluoride bath. The electrolyte was composed of LaF3, BaF2, and LiF. Metal containing 0.2 percent impurities was produced at a rate of over 2 pounds per hour. Principal impurities were carbon, aluminum, and silicon. Low-carbon metal was produced by continually discharging the carbon oxide gases and maintaining 0.1-atmosphere pressure. Anode reactions and cell design were found to be important factors in cell operation. Both frozen electrolyte skulls and tungsten metal crucibles proved satisfactory for collecting the metal and did not react with the molten lanthanum.

Jan 1, 1966

By John Ward Smith

Variations in specific gravity of oil retorted from oil shales of the Eocene Green River Formation in northwestern Colorado were evaluated statistically, demonstrating that these variations are very strongly associated with stratigraphic position and less strongly but still significantly associated with geographic location. Specific gravity of oil retorted from these oil shales apparently varies with the carboxyl group content of the oil shale's organic matter. Higher temperatures accompanying increasing depth of burial probably progressively decarboxylated oil shale's organic matter producing the decrease of oil specific gravity associated with deeper stratigraphic position. The geographically associated oil-gravity variations were probably produced by regional variation in the original thickness of late Cenozoic extrusive rocks once overlying the Green River Formation.

Jan 1, 1966

By G. E. Johnson

Batch tests of coals and coal-derived materials were made by the Bureau of Mines to determine their effectiveness in removing organic contaminants (COD or chemical oxygen demand, comprising those organic compounds that can be chemically oxidized, and ABS or alkylbenzene sulfonate, common household detergents) from the final effluent of secondary-treated waste waters. The adsorptive capacities of flyashes, coals, including at least one sample of each rank found in this country, pretreated coals, and miscellaneous materials including commercial chars and coke, were determined and compared with that of granular activated carbon. The coals, though not as effective as activated carbon, possess an economic advantage--they are relatively inexpensive, and they can still be burned as fuel without any loss of fuel value after use in waste¬water treatment. A hvcb coal was found to be one of the best, having about one-fourth the capacity of activated carbon for COD, adsorbing about 4 percent of its weight before it became saturated. Several coals contained constituents that added to the COD content of the treated water. Thus knowledge of the performance of the coal is necessary to insure selection of a proper coal as adsorbent.

Jan 1, 1966

By E. F. Foerster

The Bureau of Mines used a diphenyl ether calorimeter to determine the heat contents of natural and synthetic blast-furnace slags. For solid slags, enthalpy (HT-H298) at 1,448° to 1,680° K ranged from 282.1 to 348.5 cal/g (±3 percent); liquid slag values were 400.1 to 514 cal/g (±3 percent) in the temperature range between 1,626° and 1,890° K. Experimental results for liquid slags were 14.3 to 16.2 percent higher than the enthalpies calculated from thermodynamic tables; values for solid slags ranged from 5.3 percent lower to 3.9 percent higher than calculated values. Experimental results for liquid synthetic slags ranged from 14.9 to 24.3 percent higher than the calculated enthalpies; values for solid synthetic slags were from 1.0 to 3.4 percent higher.

Jan 1, 1967

By Robert W. Ageton

The Bureau of Mines investigated the in situ vertical component of the rock stress in the rib of the haulage drift on the 6100-level of the Star mine, Burke, Idaho, using the flatjack and borehole deformation methods. The estimate of the vertical component of stress about 2 feet into the rib at a station along the haulage drift on the 6100-level of the Star mine by the flatjack method is approximately 5,875 psi, whereas the borehole deformation procedure at this station yielded a value of 5,500 psi for the same depth into the rib. The test zone is approximately 5,625 feet below the surface.No attempt was made to extrapolate stress estimates beyond the depth of the flatjack installation.

Jan 1, 1967

By Thomas R. Bur

The strain and pressure gage methods for evaluating the relative performance of explosives in rock were compared. This comparison was based on a study of the responses of strain and pressure gages to explosion-generated seismic waves. Several explosives) representing a wide range of detonation pressures) were used. In general the relative performance of these explosives) as determined from amplitude) impulse parameter) and energy parameter measurements) is the same if the compressive portion of the strain pulse and the comparable portion of the pressure pulse are considered. Other similarities and differences of the two methods are also discussed.

Jan 1, 1967

By J. A. Ruppert

The Bureau of Mines investigated methods of refining iron-contaminated zinc to marketable quality and developed a laboratory-scale process in which aluminum, added as a refining agent, reacted with the iron, forming solid Fe2Al which floated to the surface of the melt. Solids were separated by both filtration and centrifugation, using a unique type of "dipping" centrifuge devised during the work. Typical zinc recovery was 95 percent, and iron content of the metal was lowered from 0.37 to 0.02 percent.

Jan 1, 1967

By E. A. Sondreal

The Bureau of Mines investigated the use of lignite char for producing carbon disulfide; CS2 production rates were as high as when wood charcoal was used as raw material. The maximum space velocity for CS2 produced in the bench-scale study was 9,280 hour-1, reacting sulfur and lignite char at 792° C. The reaction temperature and the temperature at which the char was carbonized were the two most important factors in determining CS2 production rates. Increasing the carbonization temperature in nitrogen from 400° to 900° C advanced the temperature at which carbon disulfide was first produced from 550° to 850° C. The average activation energy for reacting chars with sulfur was 44,000 cal/g mole. The reaction was first order with respect to the partial pressure of sulfur. Increasing the rate of sulfur admission caused a decrease in rate of production at otherwise similar conditions. Rates were not affected by either char size or sodium carbonate catalysis. High space velocities at moderate temperatures using inexpensive lignite chars could offer an economic advantage in the manufacture of carbon disulfide provided that yields were attractive.

Jan 1, 1967