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By A. Gene Collins

Some of the geochemical relationships that exist between subsurface fluids and the associated geologic strata in petroleum producing areas of Louisiana have been determined. Samples of petroleum-associated water were obtained from 126 wells in Louisiana that produced from sediments of three geologic ages: Tertiary, Cretaceous, and Jurassic. The samples were trans-ported to a central laboratory for analysis of chemical composition, using standard methods, to determine if the compositions varied with the geologic strata of their source and, if so, why. The dissolved constituents were com-pared with those of a brine that was concentrated by evaporation. The concentrations of bromide, calcium, and strontium were useful in distinguishing the brines produced from sediments of a late age from those of an earlier age. The concentration ratios of Mg' (total equivalent magnesium) and bromide indicated that dolomitization probably had occurred and altered the composition of the brines. A principal-components analysis of the data indicated an inverse relationship between depth and concentrations of bromide, strontium, calcium, and lithium.

Jan 1, 1970

By F. S. Karn

Conditions necessary to obtain optimum yield of useful products when coal is rapidly heated to extreme temperatures by laser irradiation were determined by the Bureau of Mines. Product distribution and yield were investigated as functions of several variables. Low-rank coals with high-volatile matter gave highest total gas yields. Medium-rank coals gave the highest yields of H2 and CA and low-rank coals gave highest yields of CO and C02. Macerals gave gases of approximately the same composition, but the total gas yield increased in the order fusinite, micrinite, vitrinite, and exinite. Total gas and C2H2 yields varied inversely with particle size. The addition of nominally inert gases such as Ar, He, N2 increased yields of H2, C2H2, and total gas. Metals such as nickel and platinum had little influence on the rate of coal decomposition. Total gas yield increased with total energy of irradiation, and the ratio of C2H2-CH4 increased with concentration of energy. A study was also made of the irradiation temperature, and a material balance was calculated.

Jan 1, 1970

By Thomas R. Bur

The order of identification and in same cases the magnitude of the elastic constants of an anisotropic material depends on the orientation of the cartesian coordinate axes with respect to a set of reference coordinate axes within the material; thus confusion will result unless standard orientations are used. In this paper the relationship between the cause (the internal fabric) and the effect (the elastic properties in this case) is discussed for single crystals and for polycrystalline and amorphous materials. While reference axes based on the cause are used in the IRE (Institute of Radio Engineers) standard for piezoelectric crystals) it is shown that a reference coordinate system that would be suitable and practical for all anisotropic polycrystalline and amorphous materials must be based directly on a three-dimensional expression of the effect. The conventions offered are similar to the IRE standards for piezoelectric crystals) but use the elastic coordinates of the wave surface which can be quite readily established experimentally as the reference coordinates.

Jan 1, 1969

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove, grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions 2 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1970

By D. A. Keefe, O&apos

The electrowinning of beryllium from beryllium oxide (BeO) using a molten-salt electrolyte composed of 56 LiF-37 BeF2-7 BeO (mole-percent) was investigated. Anodes made of porous carbon were found to be superior in current-carrying capacity and gave a lower cell voltage than other types of anode material tested. When porous carbon anodes were used) the resultant increase in anode area prevented anode passivation. The cell voltage was 3.3 volts) and electrode current efficiencies of 50 to 70 percent were obtained. The electrodeposited beryllium was recovered as beryllium powder or was coalesced to metal beads by heating to 1,300° C.

Jan 1, 1970

By Lester J. Crow

This study advances the use of elemental sulfur in structural materials by demonstrating its value in bonding high-strength, well-graded basalt aggregates to form sulfur-basalt concretes. Sulfur is an excellent bonding agent, and the strength of a thermoplastic sulfur-aggregate mixture depends, to a large degree, on the strength and grain-size distribution of the aggregate used. A 3-cubic-foot, electrically powered mixer with heat applied to the barrel was used to mix the sulfur and aggregate. Sulfur content of several mixtures was varied to obtain the best workability with a minimum of sulfur in excess of that necessary to fill the voids. The average grain sizes and grain-size distributions were also varied to determine their effects on strength. Unconfined compression tests of forty-five 6-by l2-inch cylinders yielded average strendths of 3,348 psi to 10,398 psi. The highest strength single cylinder was 10,717 psi. The cylinders were tested from 24 hours to 6 days after pouring; after 24 hours the rise in strength was very slight. From the results obtained it appears that sulfur can be a useful construction material. An evaluation was made of a high-vacuum application for sulfur concrete. Sulfur has a high vapor pressure at elevated temperatures, 50° to 100° C; consequently, significant losses by sublimation can be expected. At lower temperatures the losses are not significant; however, this factor will limit its use at a higher temperature.

Jan 1, 1970

By D. E. Kirby

The electrochemical reduction of AlC13 was investigated as a process for the production of aluminum. An externally heated, single-compartment cell with a rammed refractory lining was used with molten KCl-NaCl-AlC13 electrolyte. Aluminum was deposited qt 700° to 760° C with a current of 100 to 200 amperes on a molten aluminum cathode. Chlorine was evolved at a graphite anode and collected and measured to provide a quantitative evaluation of the AlC13 reduction. Aluminum was removed from the cell by siphoning or ladling. Granular AlC13 was added periodically to replenish that depleted from the electrolyte. Concentrations of 7.5 to 17.5 percent AlC13 in the electrolyte were optimum for operation. Anode current efficiencies of 83 to 85 percent were attained, using anode current densities of 5.9 amperes per square inch and an anode-cathode distance of 4 inches. The chemically bonded, alumina liner was resistant to attack by aluminum and chlorine but susceptible to erosion at the surface of the electrolyte. Titanium diboride proved suitable for the electrical connection to the molten aluminum cathode. Aluminum of a purity equal to or better than 1100 series metal was electrowon continuously from commercial AlC13 for a period of 4-1/2 months.

Jan 1, 1970

By G. T. Brow

An experimental method is described for testing diffusion of gases in crude oils at pressures and temperatures up to 3,000 psia and 200° F. A sampling technique was developed to withdraw by constant-pressure mercury displacement about 60 µl of oil from the diffusion cell through any of several 1/2-in vertically spaced capillary tubes and to trap about 4 µl of the oil in a specially designed microsampler. Oil trapped in the microsampler can be completely inserted in the sample inlet of a chromatograph. From analysis in a three-stage chromatograph (GLC), gas concentration in a sample is determined from the ratio of gas peak heights to area of peaks of reference components (hexanes or heptanes) in the oil. A diffusion coefficient is calculated from measured concentration profiles with known equations for diffusion in finite or semi-infinite systems, depending on whether the gas has or has not reached the end of the oil column. Results are given for a test of methane diffusing at 2,560 psia and 160° F in crude oil from the Weber Sandstone reservoir in the Rangely field, Colorado. A constant diffusion coefficient of 3.34 X 10-5 cm2 per sec was obtained which gives a good fit between calculated and experimental profiles determined at six times after start of diffusion. The maximum standard error of gas concentration determinations experienced with this method was ±0.88 ml per ml of gas-free oil.

Jan 1, 1970

By A. R. Rule

Laboratory tests were conducted to study removal of magnesium impurities from western phosphate rock concentrates by selective leaching. The systems evaluated included leaching with dilute sulfuric acid, with ammonium sulfate, and in an aqueous medium with sulfur dioxide gas. Set standards for the magnesium impurity level of phosphate rock concentrates are not available, but industrial practice has indicated that magnesium in excess of 0.3 percent MgO causes problems in phosphoric acid manufacture. Removal of magnesium was accomplished with all three systems. With dilute H2S04 the magnesium level was reduced to less than 0.1 percent MgO with an accompanying P205 loss of 6 percent. Magnesium oxide levels from 0.3 to 0.2 percent were obtainable with ammonium sulfate. However, the system requires concentrate roasting at temperatures of 900° C or higher, heated pulps (100° C), and large quantities of ammonium sulfate. Selective leaching was obtained using S02 gas in an aqueous concentrate slurry. Magnesium oxide content was reduced to less than 0.1 percent without loss of phosphate.

Jan 1, 1970

By Ted C. Briggs

A removable-jacket distortion apparatus was constructed and used to measure distortion coefficients for two high-pressure vessels. The measured distortion coefficients were used to compute distortion coefficients for volumes VI and (V1+V2) of a 1,000-atmosphere Burnett compressibility apparatus for the temperature range 0° to 75° C. Young?s modulus for Armco 17-4 PH stainless steel, heat treated to condition H1150-M, was computed from experimentally determined distortion coefficients. A 10-to 14-percent correction to the values obtained for Young's modulus may be required because pressure vessel end effects were neglected. The distortion coefficients of the compressibility apparatus are believed to be accurate to about 1 percent.

Jan 1, 1970

By Edward A. Mihok

This paper presents plant design and cost estimates for limestone treatment of acid mine water covering a wide range of quality and quantity conditions. The treatment process consists of limestone neutralization, aeration, solids settling, and concentration. The design criteria for the various operation functions are based on pilot plant performance, laboratory data, and established mine water treatment standards. Unit costs have been assumed and are related to general market prices and conditions. These estimates serve as preliminary indicators of what it would cost to construct and operate a mine water treatment plant.

Jan 1, 1970

By E. G. King

Low-temperature heat capacity determinations of the minerals goethite and pyrophyllite were made in the temperature range from 510 to 298° K. The entropies at 298.15° K were evaluated as 14.43 ±0.15 cal/deg mole for goethite and 56.6 ±0.5 cal/deg mole for pyrophyllite. The entropies of formation from the constituent oxides are -4.4 ±0.2 cal/deg mole for goethite and -12.3 ±0.6 cal/deg mole for pyrophyllite. The standard free energy of formation of goethite from its oxides is ?G°298.15 = 0.16 ±0.20 kcal/mole.

Jan 1, 1970

By Alfred E. Schwaneke

The surface tension from 240° to 844° C and the density from 236° to 583° C of 99.999 percent purity liquid tin has been measured using the maximum-bubble-pressure method. Results for surface tension (y) show y (dynes/em) = 566.84 -4.76 X 10-2 T (° C) with a standard error of 1.9 dynes/cm. Results for density (p) show p (g/cm3) = 7.16 -6.3 X 10-4 T (° C) with a standard error of 0.012 g/cm3. Comparisons with other data found in the literature are discussed. The experimental results are considered to be as good as any data presently available.

Jan 1, 1970

By R. Newman

An inexpensive slow-speed data acquisition system has been adapted to digitally record multiple parameters simultaneously at intervals of 15 seconds. The system was built for use with standard soils testing equipment to automatically record load and displacement parameters at predetermined instants in time. Simultaneous readout is achieved by the use of special signal conditioner and sample-and-hold circuits which read the multiple signals simultaneously and hold them until the slow acting system can print out. Three channels of a 10-channel system have been converted and found to operate successfully during a series of direct shear tests. A unique feature of the system, which significantly reduced its cost, is the power supply units. Dummy circuits are used to maintain a constant power demand during sampling) thus eliminating the need for a costly power supply with rapid response characteristics. The entire system, having an overall accuracy of 0.25 percent, was put in operation for a cost under $2,500.

Jan 1, 1970

By R. B. Tippin

To study continuous operation of the heavy liquid separation (HLS) of minerals, the Bureau of Mines concentrated spodumene from a typical ore. The studies included heavy liquid concentration, removal of the heavy liquid from the mineral products, and recovery of the heavy liquid for reuse. The research program examined the influence of feed moisture, steam consumption, stripping time, and condition of steam. Operation of multiple cyclones in series resulted in spodumene concentrates assaying 92 to 95 percent spodumene and indicated mineral recoveries of 86 to 89 percent. Continuous filtration and steam stripping produced mineral products containing less than I pound of heavy liquid tetrabromoethane (TBE) per ton of material. Problems unique to this process are discussed, including heavy liquid properties and viscosity, toxicity, material handling hazards, and safety precautions.

Jan 1, 1970

By Daniel C. Boteler

Five lignites from the northern Great Plains province were carbonized at temperatures from 500° to 1,000° C in a bench-scale unit. A replicated Greco-Latin square experimental design was employed to allow testing of four independent variables at five levels. Independent variables investigated were temperature, source of lignite (mine), weight of charge, and moisture content of charge. Dependent variables were char yield, tar yield, light-oil yield, tar plus light-oil yield, carbonization gas yield, and carbonization gas heat yield. An analysis of variance indicated that, at the 99-percent confidence level, the independent variables of carbonization temperature, source of lignite, and weight of charge were significant for yields of char, tar plus light oil, and carbonization gas, whereas moisture content was only significant for carbonization gas yields. At the 95-percent confidence level, moisture content significantly influenced the carbonization gas heat yield per pound of lignite charge and the yields of dry tar plus light oil. All dependent variables were determined on a moisture- and ash-free basis. Multiple regression equations for predicting seven different factors of carbonization yields as functions of carbonization temperature and initial composition were developed using computer techniques. Equations for yields of char, tar plus light oil, and carbonization gas were compared with equations previously developed by others at the 500° C level.

Jan 1, 1970

By B. H. Eccleston

The effect upon automobile emissions in changing from leaded to lead-free gasolines was studied in experiments by the Bureau of Mines in cooperation with the American Petroleum Institute. Typical U.S. leaded gasolines and prototype lead-free gasolines of comparable octane quality were used in eight vehicles operated to simulate city driving. The experiments were run at 70° and 95° F. Exhaust and evaporative emissions were measured and the photochemical effect of the emissions was experimentally observed in an artificial smog chamber. Results of the study reveal the manner and degree in which the changes in fuel composition alter the amount and characteristics of both exhaust and evaporative emissions. Briefly, it is shown that the compositional differences between leaded and prototype lead-free fuels resulted in higher photo-chemical pollution potential of the emissions from the lead-free fuels. The effect is attributed to the photochemical characteristics of high-octane fuel components that are used in greater quantity in the lead-free fuels.

Jan 1, 1970

By K. Robert Dorman

Spray-applied polyurethane foam was used to insulate the walls of heated rooms excavated in permafrost. The experiment was designed to determine whether polyurethane foam can be sprayed successfully on frozen ground under freezing conditions and to measure the effectiveness of the insulation in maintaining--at elevated temperatures for an extended period--a room excavated in frozen ground. Two manufacturers' foams were investigated in the laboratory. Subsequently, one of the foams was employed to insulate two small rooms, one in frozen gravel and one in frozen silt, in an experimental tunnel belonging to the U.S. Army Cold Regions Research and Engineering Laboratory (USACRREL) near Fairbanks, Alaska. Following insulation, heat was introduced into the two rooms. Heat migration across the insulating barrier into the walls, in addition to wall closures, was monitored over an 8-month period. The results show that polyurethane foam can be successfully sprayed on frozen ground in below-freezing temperatures. Given this type of insulation, together with winter cold to supercool the surrounding ground, it should be possible to maintain a shaft or heated room in permafrost for several years.

Jan 1, 1970

By G. H. Keith

A vanadium-base alloy consisting of the following elements in weight-percent--molybdenum, 20; titanium, 10; carbon, 0.1; silicon, 0.5; and yttrium, 0.5--had exceptionally high strength at temperatures up to 1,200° C. This alloy was capable of fabrication to sheet of ~ 1 mm thickness by a combination of hot swaging and hot and warm rolling. In the warm-rolled condition at ambient temperature, its ultimate tensile strength was 1,205 MN/m2. The strength at 1,200° C was 150 MN/m2. Within the temperature range of 25° to 1,200° C, the ductility of the alloy as measured by elongation increased from 4 to >90 percent. Strengthening was achieved by both solid-solution and dispersed-phase mechanisms. Alloys of 20 percent molybdenum and 10 percent titanium were stronger than the other molybdenum-titanium alloy compositions tested. Strength was increased 15 percent in the temperature range of 25° to 800° C, with no accompanying loss in ductility, by the addition of 0.5 percent silicon. Workability was improved by additions of 0.25 and 0.5 percent yttrium.

Jan 1, 1970

By W. R. K. Wu

This Bureau of Mines report presents a statistical study of the repeat abilities of coal-plasticity parameters obtained in the tests with the Gieseler plastometer and the Audibert-Arnu and Hoffmann dilatometers. Repeatability is expressed in terms of one or two standard deviations for the differences between duplicates. The statistical method employed here is summarized. Results are tabulated for the temperature and nontemperature parameters of the three tests.

Jan 1, 1970