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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 Roger L. Williams

The Bureau of Mines investigated northern New Jersey as a potential future source of yttrium and the rare-earth elements. The studies, consisting of geophysical surveying, sampling, and exploratory drilling, began in the spring of 1959. A total of three and one-half months were spent in the field collecting data. Thirty-three deposits were investigated, of which five demonstrated some potential resources of yttrium and rare-earth minerals. Results indicate that the deposits examined do not contain quantities of yttrium and the rare-earth elements recoverable under present economic conditions. Detailed studies conducted at the Scrub Oaks mine, near Dover, N. J., delineated a yttrium and rare-earth-bearing zone within the magnetite-hematite ore body that represents a potential low-grade deposit. Beneficiation studies on this deposit indicate that a final product, averaging 31.3 percent rare-earth oxides including yttrium, could be produced through amine and fatty acid flotation procedures with 77 percent recovery. Two hundred and eighty-five feet of diamond drill core was obtained from exploration studies conducted at the Bemco prospect in Sussex County. The deposit averages 2.30 percent rare-earth oxides (including yttrium), 0.45 percent uranium and 0.24 percent thorium. Low-grade deposits were identified at the Canfield phosphat2 mine and the Tanners Brook Monazite placers in Morris County, and the Marble Mountain prospect in Warren County.

Jan 1, 1967

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 M. S. Oudenhoven

The Bureau of Mines conducted an investigation to determine the theoretical stress distribution in the vicinity of explosively expanded rock bolt anchors independent of their bolts. Plane-strain solutions applicable to this problem were obtained by combining the field pressure with the uniform pressure that would be produced by vertically placed anchors having 2-, 3-, and 4-foot spacings. High rock stress which would be produced by an anchor was localized, as would be expected from St. Venant's effect, and increased as the field pressure decreased.

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

By Raymond P. Maloney

The Bureau of Mines investigated the White Mountain mercury deposit, in the Kuskokwim River Basin, to better determine the extent of mercury mineralization and to encourage its development by private industry. A program of diamond drilling, augering, bulldozer trenching, and sampling was carried on during four field seasons, from 1960 to 1963, inclusive. Significant amounts of cinnabar, with only trace amounts of arsenic and antimony, occur in dolomite over an area about 4,000 feet long and 1,500 feet wide. The deposit differs from other mercury deposits in the Kuskokwim River Basin by the absence of silica-carbonate and rhyolite intrusives. Small-scale mining was started in 1963 as the result of Bureau investigation and continued during the summers of 1964 and 1965. The investigations indicate that open pit mining might be the most feasible method of working this deposit.

Jan 1, 1967

By Ernest L. Corp

First in a projected series on the use of flexible liners for support of underground mine openings, this report presents information obtained from an extensive review of the literature on this subject. It also includes results of some preliminary test work by the Bureau of Mines. Investigations thus far indicate that flexible liners offer numerous advantages over rigid-type sup-ports, By deforming in the direction of the applied stress, the stresses are redistributed from the liner to the surrounding material. The corresponding buildup of passive resistance in the direction of diametric extension causes an equalization of stresses around the liner, thereby enabling the liner to carry loads in a more efficient manner. However, additional experimental data are needed to establish design criteria that will permit maximum utilization of the flexible liner concept in mining. Testing of small-scale models, accompanied by measurement of free-field stresses in material surrounding the model, is recommended as the most suit-able approach to the problem. The experimental procedures necessary to such an approach are outlined in detail and a statistical design for the experiments is proposed. The report also describes a device developed by the Bureau for measuring free-field soil pressures to 1,000 psi and a technique for evaluating the response of the device.

Jan 1, 1967

By J. D. Marchant

The Bureau of Mines studied solid-state electromigration to determine the value of the technique as a method of purifying cerium metal. Cerium metal in bars 6 inches long and 1/2 inch in diameter was refined at 600° C by solid-state electrolysis to remove iron, copper, and manganese. Iron and manganese were electrotransported to the anode and copper was electrotransported to the cathode. The concentration of iron at the anode of a cerium bar was 800 times greater than the concentration at the cathode. The concentration of manganese at the anode was twice the value at the cathode. The concentration of copper was 170 times greater at the cathode than at the anode. A radiotracer technique was used to follow the iron migration in the cerium metal. Molybdenum, silicon, and aluminum impurities were not electrotransported.

Jan 1, 1967

By L. F. Heising

The Bureau of Mines evaluated 42 composite samples from selected Michigan-Wisconsin iron formations by reductive roasting-magnetic separation and flotation at minus 325 mesh. Samples having poor to marginal response on initial examination by conventional methods were reevaluated by finer grinding, by reagent suite modifications, and by selective flocculation-desliming techniques. Results ranged from excellent on Menominee Range samples to relatively on Gogebic Range ores. Marquette Range samples ranged from responsive to nonresponsive, depending upon grain size and mineral association.

Jan 1, 1967

By Robert E. Wood

The compressibility factors, Z, of helium, nitrogen, and helium-nitrogen mixtures in the three-dimensional space of temperature, pressure, and gas composition have been related to the Leiden form of the virial equation of state. The dependency of virial coefficients through the fifth on temperature and gas composition has been established for the temperature range 133.15° to 748.15° K. Compressibility factors, Z, have been computed from the equation of state and tabulated as functions of gas composition, pressure, and temperature. Tabular values of Z are presented for 30.00 through 100.00 percent helium for temperatures from 240° through 700° R for pressures from 14.696 through 3,050 psia and for temperatures from 720° through 1,300° R for pressures from 14.696 through 1,500 psia. Tabular values of Z are presented at increments of 5.00 percent helium and 20° R, and, for pressures greater than 50 psia, at increments of 50 psi.

Jan 1, 1967

By Jr. Koch

As a means of investigating the distribution and variability of gold in ore from the Homestake mine, Lead, S. Dak., the Bureau of Mines performed a designed sampling experiment, and assay results were statistically interpreted. Fifty-six feet of diamond-drill core from five boreholes was sawed into l-inch-long cylinders, which were sampled randomly and were assayed. Analyses of variance of the assay results were used to compare and assess the different types of variation: within drill holes, among paired drill holes, among unpaired drill holes, and among furnace runs. The extreme variability in gold mineralization found is the natural variability on the smallest scale that can be detected by fire assay; most of the variability is associated with among-feet rather than within-feet sample intervals. Because of the extreme variability, one-half of the gold is in 3 percent of the samples.

Jan 1, 1967

By Richard F. Link

The objective of this report is to explain a statistical method for the summarization, organization, and classification of multivariate assay and other data from the mineral industry. Multivariate data are those characterized by several measurements at each data point, such as assay data from a mixed metal mine, or blast furnace data. A specific method of linear discriminant analysis, the Mahalanobis d2 procedure, is explained, starting from elementary principles; the d2 procedure enables many measurements at many data points to be studied by investigating the interrelationships among the data. The relation of linear discriminant analysis to other statistical methods for treating multivariate data, in particular the eigenvalue technique of factor analysis, is also explained. Example analyses are made on data from the Frisco mine, San Francisco del Oro, Chihuahua, Mexico. The data comprise assay values for silver, lead, copper, and zinc taken at some 19,000 sample points distributed into 91 groups.

Jan 1, 1967