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By Robert C. Johnson

Water-swelling fluormicas and fluormontmorillonoids were synthesized and described. They were found predominantly in the system Mg0 - MgF2 - Si02, with varying amounts of Li+ or Na+, Some water-swelling synthetic minerals were prepared with only strontium or lead in the twelvefold position, Water- swelling compounds containing either K+ or Ba+ were not found. The synthesized water-swelling products were shown by electron microscopy, X-ray diffraction, and chemical analysis to be typically two-silica-layer, platy compounds, Except for the complete substitution of fluoride for hydroxyl, the compounds were similar to the natural micas or montmorillonites. The stability and properties of the compounds were further established by electrodialysis, by differential thermal analysis, and by anion and cation exchange methods. Fluoride in the interlayer positions was nonexchangeable except through decomposition of the product. Exchanging the sodium or the lithium of the synthetic fluormicas or fluormontmorillonoids with potassium ion, particularly those derived from KOH provided a product from which a completely inorganic paper of extraordinary flexibility was fabricated. This paper had excellent mechanical and electrical properties except for water adsorption and a high power factor. Neither of these problems was solved during this investigation. However, papers with dielectric strength from 1,500 to 5,000 volts per mil were readily fabricated, particularly from the lithium containing fluormicas or fluormontmorill onoids.

Jan 1, 1963

By Glenn L. Cook

Correlations between mass spectra and molecular structures of 186 organic sulfur compounds are discussed. The olefinic ions, the alkyl ions, the CnE2n+1 ions, the m/e 61 ions, and the m/e 35 ions in the spectra of thiols are related to molecular structure. In the spectra of sulfides, the olefinic ions, the m/e 61 ions, the m/e 35 ions, the CnH2n+1S+ ions, and the CnH2n+1SH+ ions are correlated with molecular structure. For disu1fides, the correlations relate HSSF+& and RSSH+ ions to molecular structure. Base peaks of alkylthiophenes are correlated to their molecular structures. Some unimolecular reactions of sulfur compounds in the mass spectrometer are considered. A cyclic intermediate is suggested for the reaction which produces m/e 47, CH3S+, and m/e 48, CH4S+, ions in the spectra of sulfides. An expanded ring is suggested as a possible intermediate in the reactions of thiophenes. Heats of formation of sulfur-containing ions and their appearance potentials are presented in tabular form. Ionization potentials for sulfur-containing radicals and molecules are also given. Discussion of the spectra, tabulated in the appendixes, provides an insight into the relationship of the molecular structure of a compound to the mass-to-charge ratios and the intensities of the ions in its mass spectrum. Correlations of the mass spectra with molecular structures are empirically developed by observing regularities in the spectra of the reference compounds. Correlations extend the usefulness of mass spectra because they can be employed to determine the molecular structure of an unknown compound.

Jan 1, 1965

By Árpád B. Palotás, Adel F. Sarofim, John B. Vander Sande, Lenore Rainey Christian, J. Feldermann

"Interest in the fine structure of soots and carbon blacks is motivated by a variety of possible applications. The structure provides information on the origins of the particles and on their adsorptive and reactive properties. This paper describes a method for quantification of the structure of soots and carbon blacks based on direct electron microscopic observation followed by image analysis of these materials. High-resolution transmission electron microscopy (HRTEM) provides a very detailed observation of particle structure. The differences in soot structure, because of its complexity, may not be easily quantifiable with the human eye; therefore, high-level computer software has been used to manipulate HRTEM images. This technique involves the application of fast Fourier transforms (FFT) to single particles and the measurement of characteristic parameters such as interplanar spacings and crystallite sizes from these particles. The methodology and application of this characterization technique are presented here. Results are shown for dif¬ferent samples obtained from soot and carbon black particles selected to illustrate the capabilities of the methodology. Quantitative information can be obtained on structural characteristics, e.g., interplanar spacing, circularity, orientation, elongation, and length distribution of lattice fringes, as well as on the fractional coverage of the extracted pattern. c 1996 Wiley-Liss, Inc.This paper presents a combination of techniques for recognizing and classifying different carbonaceous materials, using their structural morphology. A new method to assess and quantify the parameters which define such structures is proposed and discussed. The technique is based on the use of HRTEM (high-resolution transmission electron microscopy) and computational image analysis.It is well-known that carbonaceous materials like graphite, soots, coals, cokes, chars, etc. possess characteristic structural appearances which can vary from mostly random or amorphous to a perfectly ordered graphitic crystalline structure (Buseck and Bo-Jun, 1985; Buseck et al., 1987). The carbon structure has been variously described as turbostratic (Oberlin, 1989) or as crumpled sheets (Rouzaud et al., 1991) to indicate that parallel layering, reminiscent of graphite, is observed over dimensions of nanometers, but that these planes or crystallites show disorder over larger scales. The degree of order of such structures is strongly dependent on the thermal treatment of the material as well as on the composition of the source of the carbonaceous material. The value of the electron microscope in studying the morphology of such materials has been well-established, and abundant information is available (Ishiguro et al., 1991; Lahaye and Prado, 1978; Buseck, 1992).The use of HRTEM has brought further insight into this matter. Qualitative assessment of the structural order of such materials has been attempted over a long period of time in order to differentiate between various sources or treatments. There is, to date, no successful method available for quantifying the structural characteristics of various carbonaceous materials. This paper presents a technique which is able to recognize dif-ferent materials and to quantify the structural parameters of those materials using HRTEM and computational image analysis, including pattern recognition techniques.In the case of perfectly ordered graphitic crystals, electron diffraction is widely used for obtaining details on structure. Analysis of diffraction patterns can reveal parameters such as interplanar spacing, d002, crystallite size along the c-axis, Lc, crystal size in the plane of the layers, L., mean number of crystallites, Nc, etc.Complicated electron microscopy methods such as defocusing, tilted illumination, axial illumination, etc., often have to be used in order to characterize complex materials such as randomly oriented crystals in soots and carbons. Obtaining the right fo"

Jan 1, 1998

By D. Bienstock

Using a nitrided fused-iron catalyst, the Bureau of Mines investigated the Fischer-Tropsch reaction in the oil-circulation process. The nitrided iron was quite stable and permitted the longest run obtained thus far in the oil-circulation process without the need for reactivating the catalyst--3,700 hours of operation. The effects of several operating variables--temperature, pressure, gas-recycle ratio, space velocity, synthesis-gas composition, and synthesis with and without reflux of oil to the reactor--on the production of oxygenates were studied. The importance of removing reflux oil and of high gas recycle in increasing the oxygenate content was shown. A finished gasoline containing 28 percent by weight alcohols was produced. The research octane number (RON) was 92.9 clear, increasing to 98.5 with the addition of one milliliter of tetraethyl lead (TEL). INTRODUCTION The Federal Bureau of Mines has been engaged since 1944 in a research and development program on the synthesis of gasoline from coal. Gasification of coal with steam and oxygen to yield a "synthesis gas"--a mixture of carbon monoxide and hydrogen--is being investigated at Morgantown, W. Va., and the synthesis of gasoline by catalytically reacting carbon monoxide and hydrogen over iron by the Fischer-Tropsch reaction is being investigated at Bruceton, Pa.

Jan 1, 1960

By Benjamin W. Haynes

Analytical procedures are described for the quantitative determination of 16 elements (As, Ba, Be, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Se, TI, and Zn) and 7 ionic species (NH4, C032-, CI-, F-, NO3-, P043-, SO42-), identification of major and minor mineral components, and measurement of physical properties associated with manganese nodules and nodule processing reject waste materials. Compound identification methods discussed include X-ray diffraction, infrared spectroscopy, scanning and transmission electron microscopy, selective area electron diffraction, and optical and reflected light microscopy. Methods for elemental analysis include atomic absorption spectrophotometry, inductively coupled plasma emission spectroscopy, neutron activation analysis, fluorescent X-ray spectrography, and ion chromatography. Thermal gravimetric analysis, ultraviolet-visible spectrophotometry, ion specific electrodes, and standard wet chemical procedures are briefly discussed. Physical properties determined in manganese nodule materials include grain size distribution, specific gravity, triaxial shear, permeability, maximum density, Atterberg limits, and slurry density. The results of a round-robin analysis of an ammonia process waste material and manganese nodule standards demonstrate the applicability of the discussed methods. Tests discussed for the evaluation of the waste materials for disposal options include the Environmental Protection Agency (EPA) EP toxicity test, the ASTM shake extraction test, and the U.S. Army Corps of Engineers EPA seawater elutriant test.

Jan 1, 1983

The principal activities of the Bureau of Mines Explosives Research Center (now Safety Research Center) during fiscal year 1968 (July 1, 1967, to June 30, 1968) are reviewed in part 1. Part 2 presents short abstracts of the publications issued during this period in the Bureau series and in other media. Part 3 describes a short study on the thermal decomposition of RDX and HMX not destined for publication elsewhere. ACKNOWLEDGMENTS The Bureau gratefully acknowledges the support received through cooperative agreement in fiscal year 1968 from The Manufacturing Chemists Association.

Jan 1, 1970

By Galen G. Waddell

Dilation and contraction of the rock surrounding horizontal access open-ings of a deep mine were analyzed during stope advance to determine what type of measurements, made with relatively inexpensive instrumentation, would best reflect the rock behavior. A variety of instruments, mostly mechanical extensometers, were used. Detailed descriptions are given of Down-the-hole extensometers, floating rockbolt clusters, transit surveys, and other instruments and measuring techniques. Although all of the radial-deformation-rate graphs illustrated useful rock behavior data, the most informative graphs were compiled from data procured with the radial extensometers that penetrated, to various depths, the rock around the access openings. An analysis is given of measurement data on the rock around lateral drifts and across and adjacent to the nearly vertical vein of the Star mine, Burke, Idaho. Several useful relationships were found between the rock deformation rate and the stoping process. Information was produced on the elastic state of rock around an underground opening, effectiveness of stope support, rheology of rock, zone of influence around stopes, effectiveness of rockbolts, axis of maximum strain in a plane perpendicular to the long axis of the lateral, and other phenomena. This information could be of particular value in determining location, design, and support of underground openings.

Jan 1, 1966

By C. W. Owings

"Coal may be and has been hauled safely at approximately the same cost with permissible2 storage-battery locomotives as with trolley, cable-reel, crab-reel, or nonpermissible storage-battery locomotives. While in general, thinking mining men readily admit the relative safety of the permissible storage-battery locomotive there are some persons who question the safety of this type; however, the greatest opposition to the widespread use of storage-battery locomotives is from those who believe them to be more expensive to operate and to be more expensive in first cost than the trolley or cable-reel locomotive. Data collected during a comprehensive study- of storage-battery and wired transmission of power in some Pennsylvania and West Virginia coal mines indicate that there is but little difference between the cost of hauling with cable-reel or with storage-battery locomotives. It would appear that if this fact were mere generally known mine operators of the more progressive type would install such equipment and avail themselves of greater safety in hauling coal.The need for greater safety in haulage in coal mines is readily understood when it is considered that during the 12 month period, July 1, 1929 to June 30, 1930, trolley or cable reel gathering locomotives caused four explosions in which 407 lives were endangered, 11 persons were injured, and 30 lives were lost. Still another disaster was averted by the vigilance of a fire boss, who discovered a stratum of gas 3 feet thick at the top of an entry into which a gathering locomotive was about to enter. Other explosions not resulting in any fatality probably have not been reported. In addition numerous fires have been caused by trolley or cable-reel locomotives, and these fires probably would have been avoided had permissible storage-battery locomotives been used."

Nov 1, 1930

By Louis A. Panek, John A. Stock

A flat slot is created in rock to cause stress relief effects in a pair of hydraulic borehole pressure cells (previously installed in drill holes above and below the slot ) , which act as sensing devices . This relief is annulled by repressuring the slot by means of a flat hydraulic cell . The slot pressure at annulment is taken to be the existing ground stress at right angles to the plane of the slot . A number of trial installations in the rib of a mine drift showed that for a valid determination of ground stress the sensing devices that respond to relief and repressuring must be within a specified zone close to the pressure transmitter ; otherwise the indicated ground stress may be excessive . By using an additional pair of borehole pressure cells , installed a few feet away , the existing rock stress can be redetermined at intervals , irrespective of a change of stress intensity subsequent to the initial installation . Based on these findings , equipment and procedures have been developed that make possible the installation and operation of a permanent rock stress monitoring station for observing mining - induced stress changes . The station consists of a 12 - in - wide hydraulic pressure cell cemented in a flat slot and four 2- by 8 - in flat hydraulic pressure cells in nearby drill holes . All drilling for the installation can be done with an air leg drill and conventional bits . Once the installation is completed , all required information is obtained by Bourdon pressure gage readings . The apparatus is simple , relatively inexpensive , and reliable under operating conditions in a wet mine . Unlike most methods of rock stress determination , this scheme permits periodic remeasurement of absolute rock pressure over several years , without additional drilling or instrumentation . Similar to other flat slot procedures , stress measurements are obtained without making auxiliary tests to determine elastic

Jan 1, 1964

By Michael E. Henderson

The U.S. Bureau of Mines (BOM) constructed the Hydraulic Transport Research Facility (HTRF) to investigate the hydraulic parameters relating to the transport of coarse coal. To achieve these goals in a timely and efficient manner, the Bureau contracted to Boeing Services International, Inc. (BSI) the responsibility of operating the HTRF and providing technical support. This data report is a summary of the testing and data results for the period from 6 September to 9 September 1983. The testing covered herein is for coarse 2-in by 0 (minus 50 mm) Pittsburgh Seam run-of-mine (ROM) coal in a 12-in (300 mm) pipeline, at velocities ranging from 8 to 16 ft/s (2.4 to 4.9 m/s) and at concentrations ranging from 15 to 50 pct.

Jan 1, 1985

By Charles S. Allbright

To develop a method for predicting the stability of a fuel during long-term storage from rapid aging tests at 200° F, the Bureau of Mines determined the stabilities of three gasoline base stocks and an alkylate blending stock in both sealed storage and aerated storage at 110° F for periods extending to 32 weeks. Stabilities of samples containing gasoline-additive compounds were compared by aging, using two methods--rapid aging in a bomb at 200° F for intervals up to 16 hours and storage at 110° F. The additives used were an uninhibited tetraethyllead motor mix, N,N'-di-sec-buty1-p-phenylenediamine and 2,6-di-tert-butyl-4-methylpheno1. Results were related by graphs that enable predictions of gum and sediment formation during storage from data obtained in bomb tests. A premium-gasoline base stock and the alkylate proved to be stable, but the two regular-grade gasoline base stocks were found to be unstable. Addition of the diamine antioxidant improved the stability of both of the regular gasoline base stocks, while the phenol antioxidant improved only one of them. The presence of the tetraethyllead decreased the storage stability of all four fuels, both with respect to formation of gum and precipitation of inorganic sediment. The rapid test at 200° F appears to offer promise as a basis for a method of predicting gasoline stability in long-term 110° F storage.

Jan 1, 1968

By Robert D. Ewing

The computer program described in this user's guide provides for the static, three-dimensional, linear and nonlinear analysis of structural and geological systems by the finite element method. The guide describes the capabilities and general features of the program and shows how input is prepared. A number of recent advances in finite element theory and computer technology are incorporated in the program. Nonlinear material properties are provided for, including isotropic, anisotropic, and time-dependent material properties, gravity loading, simulation of a sequence of excavation or construction, and a slip or joint element. The finite elements include beam, rod, axisymmetric and plane quadrilateral, hexahedron, thick shell, and axisymmetric and plane joint. The program also has an automatic mesh generator to minimize user input preparation for continuum finite element meshes.

Jan 1, 1976

By E. C. Tarpley, R. A. Drogowski, R. F. Abernethy

Three of the test methods frequently used for the determination of moisture in the analysis sample of coal were employed in analyzing a series of coals ranging in rank from anthracite to lignite . For most coals , the variation between the three methods are within the tolerances allowed between duplicate determinations by the same method . The processing variables studied included atmosphere , flow rate of atmosphere , inert atmospheres , oven temperatures , heating time , exposure of the dried coal to laboratory air , and surface area of the test sample . Unless close control is kept on these variables , erratic results will be obtained .

Jan 1, 1964

By C. Q. Cupps

n view of increased interest in secondary recovery of oil in the Cut Bank field, Montana, a review has been made of unpublished data obtained during a 1943-44 study of reservoir oil characteristics in this field. Considerable uncertainty was attached to interpretations of subsurface oil sample analyses from six Cut Bank zone wells, one Lander sand well, and one Moulton sand well, because of adverse sampling conditions and wide range in the data. Much of this uncertainty has been removed by this review which has shown two of the Cut Bank zone samples and the Moulton sand sample to be representative of the reservoir oils. Estimates of original reservoir oil characteristics derived from differential-liberation analyses of these samples show that the oil in the Cut Bank zone was initially saturated at the gas-oil contact pres-sure, 750 psia, and the oil in the Moulton sand was undersaturated with a saturation pressure of only 380 psia. The rest of the samples were indicated to be nonrepresentative of the reservoir oils because of a disproportional vaporization of heavier components of the solution gas. The vaporization of these components is believed to be a cumulative effect of contact of the oil with bypassing, light-gravity gas which had been liberated at higher pressures from solution in oil farther back in the formation, or which had come from the gas cap, rather than from the singular effect of gas evolution caused by excessively low bottom-hole pressures. Change of oil composition caused by the latter was found to conform closely to that occurring during a differential liberation of gas in the laboratory.

Jan 1, 1967

By Gregory J. Chekan

The U.S. Bureau of Mines is investigating longwall panel and gate road layouts to increase coal recovery and reduce multiple-seam interactive problems. This report presents design practices for longwall mining multiple seams to provide mine planners and operators with practical guidelines for designing productive longwall mines. Key aspects of mine design that control longwall interactions are examined, including sequencing of seams, design of gate road pillars, and orientation of gate roads and longwall panels. Theories that describe stress transfer between multiple scams and the mechanics of interaction are addressed in relation to geology. Common longwall designs were further investigated using a boundary element model, MULSIM/NL. The model provided insight into relative stress transfer and distribution that occurs between longwall operations in multiple seams. Findings from the model show that (1) a longwall panel should be mined from the gob to the solid coal of an overlying mine, because the stress concentrations are lower; the approach angle should be kept under 30°; and (2) when mining in descending order, superpositioning gate roads usually produces the worst stress condition. To prevent this, the overlying isolated gate roads should be positioned from the centerline toward the headgate side of the underlying panel.

Jan 1, 1993

By B. P. Martinez

A process for regenerating spent pickle liquor is proposed in which some of the water is evaporated at atmospheric pressure and ferrous sulfate is precipitated as monohydrate crystals..Equilibrium conditions are set for a slurry of crystals in a mother liquor containing 5 percent FeS04 and 45 percent E2S04, by weight, and boiling at about 235° F. The slurry is pumped continuously to a filter, and the mother liquor from the filter is pumped back for reuse in the pickling tanks. The net result of the process is to remove ferrous sulfate in the regeneration plant at the same rate ac it is produced in the pickling tanks. This process is integrated with the steel-pickling operation and controlled by the pickling requirements for particular steels. Spent pickle liquor is removed for regeneration continuously from both batch and continuous picklers at higher acid concentrations than would be dumped to waste because no acid is neutralized or discarded. However, the process is not designed to keep a sulfuric acid concentration stronger than 25 percent in any pickling tank. To retain flexibility in the pickling operation, all acid makeup is added to the pickling tanks. Rinse waters are used as water makeup for the pickling tanks. To further minimize waste of acid in the rinse waters, improvements of rinsing practices are outlined.

Jan 1, 1953

By Richard L. Fischer

Constant-volume charges of precipitated PETN (pentaeythrite tetranitrate) at three specific gravities (0.50, 1.00, and 1.50) were used in laboratory tests to examine the effects of changes in explosive properties on free-surface displacement pulses and on crater dimensions. The tests were performed in large blocks of cement-mortar. The values for the detonation velocity, detonation pressure, specific energy, energy density, and energy release rate were calculated from the explosive loading density. Calculated explosive properties were correlated with free-surface displacement pulse measurements, strain energy, and measured crater dimensions. Increases in explosive properties resulted in increased free-surface displacement pulse parameters and crater dimensions. The loading density, detonation velocity, energy density, detonation pressure, and energy release rate were found to be best indicators of explosive performance. Simple acoustic relationships involving impedance ratios were examined and could not be used to predict peak displacement amplitude or strain energy. Data are presented in the customary English units as well as the International System of Units (SI).

Jan 1, 1970

By Albert L. Toenges

The fuel requirements for industrial and domestic consumers in New England, in normal times, are supplied almost entirely by fuel oil, anthracite, and bituminous coal. A shortage of these fuels occurred during the war. This shortage was caused by: (1) The diversion of oil to military uses; (2) the use of railroad and boat facilities that ordinarily would transport coal for the transportation of war material; (3) the inability of coal mines to apply the increased demand for coal which resulted from the conversion from oil to coal by domestic and industrial consumers; and (4) the increased demand of war industries for coal. Because of this Critical fuel situation, an investigation was made of possible sources of fuel nearer to points of consumption in New England.

Jan 1, 1948

By Gerald W. Elger

To determine the feasibility of removing nonferrous metal impurities from automobile scrap by thermal treatment in a rotary kiln, the Bureau of Mines conducted four series of tests with synthetic scrap mixtures heated at various temperatures under oxidizing and reducing conditions. The treated scrap mixtures were melted in an electric-arc furnace and cast into small ingots for impurity evaluation. Analyses showed that the ingots were essentially free of residual metal impurities except for copper. Test data indicated that in an oxidizing atmosphere the percentage of copper removed increased with treatment temperature. Percent of copper removed in a reducing atmosphere was found not to be temperature dependent. A significant finding was that copper was embrittled under some of the operating conditions and was mechanically removed by fragmentation.

Jan 1, 1968

By R. A. Busch, R. R. Backer, R. W. McKibbin

The Bureau of Mines conducted laboratory tests to determine the slur- ry transport and deposition properties of coal waste. A 188.5-ft pipe test loop was constructed with instruments to measure density, flow, and power and discharge, suction, and differential pressures. A 20-ton sample of Western coal waste was crushed and screened to 100 pct minus 1/2 in. Eight loop tests using this graded waste were run at slurry densities ranging from 1.15 (25 wt-pct solids) to 1.46 (60 wt-pct sol- ids). The resultant friction-pressure gradients ranged from 0.06 to 0.24 ft of water per foot of 4-in standard steel pipe. Particle-size degradation was significant. In a typical loop test lasting 25 min, the minus 200-mesh fraction increased from 19 pct to 34 pct. Deposi- tion tests showed that without the use of a flocculant, the slurries would not dewater when left to stand for 1 week. With flocculant, ad- ditional water was released; however, the settled slurries remained thixotropic. Further testing is necessary to determine their suitabil- ity for use as backfill material in active mines.

Jan 1, 1965