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By F. R. McDonald

This report presents a discussion of the spectra of 39 condensed thiophenes in which the structure includes at least 1 benzene ring. The vibrational bands present in three regions of the infrared spectra of these thiophenes were interpreted by comparing the similarities of the spectra of condensed thiophenes with the spectra of substituted benzenes. In the overtone-combination region 23 of the 39 condensed thiophenes had spectra which contained sufficient detail to be usable for correlating this region of the spectrum with the appropriate benzene spectrum. In the in-plane deformation region it was possible to make correlations for the vibrations of 18 of the 39 condensed thiophenes whose infrared spectra were studied. In the out-of-plane deformation region the C-H out-of-plane vibrations for hydrogen on benzene rings in the condensed thiophenes can be correlated using known data from substituted benzenes.

Jan 1, 1967

By R. J. Heemstra

A continuous flowing paper electrophoresis cell was used to separate petroleum and petroleum extracts into characteristic patterns. The electrophoresis of Bachaquero, Lagunillas, Boscan, and Gibson petroleums in nitro-benzene and acetic acid-based electrolytes was investigated. The extent of separation in the patterns was studied by measuring the metal and porphyrin contents of the effluents. Qualitative separations were achieved in some systems, whereas either system demonstrated only a high degree of electrophoretic migration.

Jan 1, 1967

By Russell E. Griffin

Dielectric constants and dissipation factors were measured for six rocks over the 20-to 100-megahertz frequency range by means of the susceptance-variation method. Results for both dry and moist specimens are presented and compared with data reported by others. Loss factors calculated from the data presented are important to the Bureau's study of rock fragmentation by means of dielectric heating.

Jan 1, 1967

By Jr. Hill

Laboratory metallurgical treatments of three high-iron bauxite ores from Arkansas were conducted to determine the relative effectiveness of experimental methods for recovering alumina and a commercially acceptable iron concentrate. The standard for evaluating recoveries from experimental processes was the Al2O3 recovery from Bayer digests of the crude ores; recoveries from digestion of the three ores were 74.1, 87.4, and 88.7 percent. Flotation, magnetic separation, or various combinations of digestion, calcination, and reduction-sintering, leaching, and magnetic separation of leach residues failed to produce Al2O3 recoveries as high as the standard. A high-iron-bearing fraction, containing between 68 and 78 percent of the total iron, was produced in a three-phase treatment involving a caustic, lime reduction-sinter of the crude ore, water extraction of Al2O3 from the sinter, and magnetic separation of the leach residue.

Jan 1, 1967

By F. W. Hoertel

Near-optimum parameters were determined by the Bureau of Mines for vapor deposition of rhenium on heated copper substrates by hydrogen reduction of rhenium hexafluoride (ReF6). High-purity deposits of nearly 90-percent theo¬retical density were obtained with the reaction chamber at 250° C, with an H2 to ReF6 volume ratio of 25 to 1, and with an ReF6 flow rate of 5 grams per hour. Some rhenium deposited as a loose, black powder. When the established near-optimum parameters were carefully followed, this could be minimized but never completely avoided. Varying the reaction chamber pressure, both above and below atmospheric, yielded excessive quantities of rhenium powder. Deposition efficiencies, based on only the coherent metal, ranged between 70 and 75 percent. Massive deposits contained only spectrographic traces of impurities. The average microhardness (Knoop, 100-gram load) of vapor-deposited rhenium was 907. Limited research on the deposition of rhenium-tungsten alloys by reduction of the mixed hexafluorides produced deposits in which linear composition gradients were pronounced; this nonhomogeneity was attributed to the wide variation in optimum hydrogen-reduction temperatures of the two hexafluorides (250° C for ReF6 and 550° C for WF6). Using deposition temperatures between 250° and 550° C did not eliminate the composition variations.

Jan 1, 1967

By John S. Berber

To improve the economics of low-temperature carbonization of coal, the Bureau of Mines is conducting research on the upgrading of the product tar to marketable chemicals. This report describes experiments on the catalytic hydrodealkylation, followed by catalytic vapor-phase oxidation of the dealkylate to phthalic and maleic anhydrides, of mixed residues from the urea adduction of lignite-neutral oil fraction and on the catalytic thermal dealkylation of high-boiling tar acids. The hydrodealkylation experiments were conducted at pressures from 1,000 to 1,750 psig and at temperatures from 600° to 1,000° F. The oxidation was, in all cases, at atmospheric pressure and 9500 F. Maximum yield of maleic anhydride, based on the liquid feed to the hydrodealky1ation unit, was 12.2 percent at 750° F and 1,500 psig; that of phthalic anhydirde was 6.9 percent at 650° F and 1,500 psig. Maximum yield of combined anhydrides was 18.8 percent at 650° F and 1,500 psig. The non-dealkylated feed material, upon oxidation, yielded 8.9 percent and 3.8 percent maleic anhydride and phthalic anhydride, respectively.

Jan 1, 1967

By Leo A. Schrider

A prediction for oil recovery from a pilot waterflood in the Kane oil- field, located in Elk, Forest, and McKean Counties, Pa., was made and compared to actual field performance. Water-injection and production histories, well logs, other field data, and results from laboratory tests of core material were used in this analysis. Performance of the pilot waterflood, initiated in January 1963, was predicted using a modified Craig, Geffen, and Morse calculation technique. Maximum recovery from this low permeable, preferentially oil-wet formation was predicted to be about 22,500 barrels of oil after 300,000 barrels of water had been injected into the pilot waterflood area. After additional field data were collected it became necessary to reevaluate the pilot waterflood area. The gas saturation prior to the waterflood was estimated to have been 20 percent, based on an assumption regarding the required volume of water injected to initiate oil production. In view of the actual field performance, a gas saturation of 13 percent is indicated. When this gas saturation and the method originally proposed by Craig and others are used) the predicted results are more representative. In December 1965, field performance was further analyzed using a hyperbolic-decline curve as presented by Arps. Based upon this evaluation method, the pilot water flood in the Kane sand should produce 37,000 to 42,000 barrels of oil with the injection of 300,000 barrels of water into the pattern. By continuing this secondary-recovery project to a reasonable economic limit, ultimate oil recovery may be as much as 50,000 to 55,000 barrels, or 129 to 142 barrels per acre-foot from 36.5 acres.

Jan 1, 1967

By W. P. Haynes

To evaluate the potential use of battery-powered vehicles, the Bureau of Mines studied the performance of a battery-powered truck propelled by a 9.6 kw dc motor in considerable detail under various driving conditions. Some of the factors investigated were: Gear ratios, payload (1,468 lb maximum), road grade, stops made per mile, and charging time. With the exception of some difficulty with brush wear, operation and maintenance of the truck was generally trouble-free. On range tests carrying an 868-lb payload a distance of about 50 miles at an average speed of about 19 mph in normal driving, the Bureau's battery-powered truck averaged 1.6 to 1.9 miles per ac kwhr input. Stop-and-go tests indicated that prospects for the use of battery-powered trucks in house delivery service within city limits are good; performance of the Bureau truck was sufficiently high for that type of service. The estimated power cost of 2.65 cents per mile while making 10 stops per mile was attractively low from the standpoint of fuel costs.

Jan 1, 1967

By Jack Smith

New turbine blades designed to resist ash erosion were tested by the Bureau of Mines in a pilot-scale coal-fired gas turbine. After a total of 1,963 hours, the rotor blades were only slightly eroded; and they had an estimated useful life of 20,000 to 30,000 hours. Changes in aerodynamic design of the blades successfully concentrated the ash at the outer casing, but stepped sidewalls for the rotor drum and wear strips at the bases of the rotor blades are still needed to minimize wear at these points. Stepped sidewalls and wear strips did not adequately protect the stator blades. Ash slightly eroded their leading edges, above the inserts, and cut notches into their trailing edges near the bases. Stator blade life was estimated at 5,000 to 7,500 hours. Blade erosion in these tests was less severe than with previous designs, but more efficient combustors and ash separators are required to reduce the amount and size of ash entering the turbine, to achieve acceptable blade life for commercial operation.

Jan 1, 1967

By David E. Nicholson

In a Bureau of Mines investigation of the dynamic compaction of mine hydraulic backfills, two basic forms of mechanical vibration inducers were used and compared for effectiveness of compaction. Internal compaction, using concrete probe vibrators of various sizes, and external compaction, using plate vibrators} were studied and evaluated for use in underground stopes. An aluminum plate, which was light and displaced sufficient volume to remain afloat in fluid fill, and a steel plate were both used in the external compaction tests. Efficiency of compaction was better in studies conducted with internal probe vibrators. Tests were conducted in an underground backfilled stope with three different-sized probe vibrators (2-, 4-, and 6-inch-diameter) to determine an approximate area of influence. Results showed the areas of influence to be approximately 3, 4, and 5 feet in diameter, respectively, for the three different probes. Physical properties of hydraulic slurries were determined; preferred grain-size distributions, water exudation properties, and water contents of hydraulic slurries are reported. The best compaction results were obtained with moderately well-graded, fully saturated backfills, with slow rates of water exudation, which were capable of remaining in a semifluid state during the compaction process.

Jan 1, 1967

By J. W. Town

Recrystallization studies on chrome-bearing spinel materials were made by the Bureau of Mines to determine the effects of certain fluxing agents and cooling rates on the chromium-to-iron ratio of recrystallized spinel. Statistically designed and evaluated tests showed that the ratio of chromium to iron in naturally occurring chrome spinel could be increased from 1.5 to 1 to over 7 to 1 and that the ratio of chromium to iron in the chrome-spinel in a stain-less steel slag could be raised to over 18 to 1. Silica, magnesia, and lime had significant positive effects, while alumina had a significant negative effect. Cooling rates of 200 C per hour in a programmed spiral globar electric furnace were satisfactory for growing crystals of recoverable size.

Jan 1, 1967

By Robert E. Barieau

General expressions for evaluating practically all the thermodynamic properties of a fluid from a single equation of state are derived. Most of the formulas are expressed in terms of the compressibility factor, with this factor being an explicit function of the temperature and the molal density. Similar expressions are given using reduced variables.

Jan 1, 1967

By T. Estelle Gardner

Heat-capacity measurements were made over the range 8° to 350° K on beryllium sulfate dihydrate and beryllium sulfate tetrahydrate using an adiabatic calorimeter. No anomalies were noted in the curve for either compound. Smooth values of heat capacity, entropy, enthalpy function, and free-energy function were calculated from the heat-capacity data at 10° K intervals and at 273.15° and 298.15° K. The entropy values calculated at 298.15° K were 39.01 ± 0.12 entropy units (eu) for the dihydrate and 55.68 ± 0.17 eu for the tetrahydrate.

Jan 1, 1967

By J. B. F. Champlin

The continuing development of the nuclear industry in the United States requires a program of waste disposal that insures against the release of large amounts of radioactivity to the environment. This paper describes research on one proposed means of disposal of this waste, that of injection into geologic formations at depth. Nuclear production plant wastes were simulated and injected into samples of sedimentary rock obtained from outcrops, quarries, and deep wells. Changes in the chemical and physical characteristics of the rocks caused by the interaction of ions and suspended particles in the waste solutions with the cementing material and claylike particles in the rock are discussed. Laboratory tests show that nuclear wastes can be injected into many natural porous, permeable geologic formations. Injectivity can be maintained over a longer period by monitoring the ionic balance and particle-size distribution of waste streams. The combination of permeability and porosity with low cation-retention capacity, as exhibited by most sandstones, would satisfy the engineering requirements for the subsurface disposal of nuclear waste. Shales and clays with their low permeability and high cation-retention capacity would make excellent confining formations. The amount of cation retained by sedimentary rocks increases with increasing valence or concentration of the cation or decreasing brine concentration. The use of rock cores as model reservoirs had proved successful in determining some of the parameters that need to be considered in full-scale field disposal of wastes.

Jan 1, 1967

By Frank A. Peters

An evaluation is made of a lime-soda sinter process for extracting alumina from clay. In this process, alumina is extracted by sintering clay with soda ash and limestone and then leaching the sinter with a dilute sodium carbonate solution. The sodium aluminate solution formed during leaching is separated from the residue and treated with lime in autoclaves to remove dissolved silica before alumina trihydrate is precipitated with carbon dioxide. The tri-hydrate is then calcined to a-alumina. Two options, dry grinding and wet grinding, are used in the sintering step. The fixed capital costs for plants producing 1,000 tons of alumina per day are $72 million for the dry grinding option and $66 million for the wet grinding option on a Marshall and Stevens chemical equipment index basis of 240.0. Specific geographic locations of plant and raw material sources are not assigned, but, since this process requires large quantities of both lime-stone and clay, the plant site is considered as variable with relation to the clay mine and limestone quarry. A nomograph is given to find operating costs at various delivered costs of clay and limestone. If the plant is located nearer the limestone quarry so that the delivered cost of clay is $2 per ton and the delivered cost of limestone is $1 per ton, the operating costs are $76.47 and $71.61 per ton of alumina for the dry grinding and wet grinding options, respectively. On the other hand, if the plant is located nearer the clay mine so that the delivered cost of clay is $1 per ton and the delivered cost of limestone is $2 per ton, the operating costs are $80.15 for dry grinding and $75.34 for wet grinding.

Jan 1, 1967

By Arcy R., D&apos George

A process for removing sulfate from Great Salt Lake brines and other natural brines, including sea water, has been developed. Sulfate is quantitatively removed by precipitation as barium sulfate in a cyclic process employing ion-exchange techniques. Barium is continously recovered and recycled, and sodium carbonate and sulfur or sulfuric acid are produced as byproducts in quantities sufficient to more than defray the cost of desulfation.

Jan 1, 1967

By J. M. Singer

This study was undertaken to obtain some fundamental information about hazardous mixtures of coal dust and methane (firedamp) likely to occur in mines. Fuel concentration limits for ignition of mixtures of coal dust, methane, and air have been determined by a hot-gas ignition method. The limiting concentration of each of the two fuels was usually less than that corresponding to its lean flammability limit in air. The lean limits of flammability of coal dust vary with the type and size of the dust; in this study coal dust concentrations were less than 80 mg/liter. Ignition jets were turbulent pulses (emerging from a channel of 0.5 cm diam) resulting from explosions of stoichiometric mixtures of methane, oxygen, and nitrogen, Temperatures of the ignition jets were varied by changing the oxygen index (OI) = O2/(02 + Nj2) of the primary methane-oxygen-nitrogen mixture (adiabatic flame temperatures from 2,000° to 3,000° K). The objectives of the study were to establish quantitative relations between concentrations of each fuel at ignition limits of hybrid mixtures and to study the mechanism of ignition of these hybrid mixtures by hot turbulent gases, Empirical equations were fitted to concentrations for four coals, namely) Pittsburgh Seam (sizes A, B, and C), Sewell No.2 Seam, pocahontas No.3 Seam, and anthracite. Equivalences of coal dust to methane were computed from these equations; equivalence being defined as -Ac/Am, where c is the coal dust concentration and m is the methane concentration, each in milligrams per liter of air. It was found that the equivalence increases as the temperature of the hot-gas jet decreases. In general, the equivalence is also an inverse function of volatile content of the coal and a direct function of the particle size, However, volatile con-tent in itself is not a sufficient correlating variable, nor is the specific surface area of the coal dust.

Jan 1, 1967

By R. C. Hickman

Preliminary evidence indicated that the Chattanooga Shale might constitute a potential vast low-grade source of uranium. Investigation by core drilling indicated that while the Chattanooga Shale may constitute a resource for the future, the very low (0.006 percent) average uranium content is not economic when compared with the relatively higher grade western ores. A total of approximately 12,000 feet of test drilling was done in 72 drillholes, and large samples were mined for extractive and metallurgical testing. An experimental mine site was selected on the basis of the drilling project.

Jan 1, 1967

By Sarkis G. Ampian

Extraction of alumina was correlated with the sinter and leach products from the lime soda sinter process for anorthosite. The effect of composition and grain size of reactants, time and temperature of sintering, and techniques of sample preparation were investigated. Greater than 90 percent Al2O3 extractions were obtained from dry-mixed minus 200-mesh anorthosite sinter mixes having mole ratios of CaO/SiO2 = 1.8 and Na2O/Al2O3 = 0.8. These sinter mixes were briquetted at 15,000 psi and fired between 1,200° C and 1,320° C for 20 to 60 minutes. The sinter phases that contribute to low alumina recovery were determined by X-ray diffractometry, optical microscopy, and electron probe X-ray spectrography. The mechanism of the sintering reaction was investigated by high-temperature X-ray diffractometry. The contrast in the lime soda sinter process for clays and for anorthosites are discussed. Explanations and suggested solutions are presented for problems such as gelation and variable alumina recovery encountered by previous investigations.

Jan 1, 1967

By J. S. Coffman

Wyoming is estimated to have more than 700 million tons and Utah more than 2.5 billion tons of +10 percent P2O6 phosphate rock considered to have some future economic potential. In Wyoming, the +24 and +18 percent P205 rock potential resources total nearly 250 and 450 million tons, respectively. In Utah, the +31, +24, and +18 percent rock total approximately 33 million, 222 million, and 2.2 billion tons, respectively. These resources are all located above the local drainage levels and do not include latent resources. All of the mining and beneficiation of phosphate rock in the two States is done by San Francisco Chemical Co. The facilities include open pit mines at Vernal, Utah, and Leefe, Wyo.; an underground mine in the Crawford Mountains, Utah, and beneficiation plants at Leefe and Vernal. One of the principal markets for the phosphate rock is Western Phosphates, Inc., fertilizer plant at Garfield, Utah. Recent exploration and development has been under-taken by different companies in the Southeastern Wind River Range, Sublette Range, and Crawford Mountains. The facilities at Leefe and Vernal are in the process of expansion. Some of the areas of western Wyoming contain vast quantities of phosphate rock in minable units, but, because of their remote location, are classed as latent areas. In these areas, there are estimated to be about 700 million, 2 billion, and 3 billion tons of phosphate rock in the +24, +18, and +10 percent P205 grade classes, respectively. The Snake River Range of Idaho and Wyoming is also estimated to contain roughly 21, 106, 177, and 214 million tons of potential resources in the +31, +24, +18, and +10 grade categories, respectively. This area also contains a large amount of latent rock in the more remote areas.

Jan 1, 1967