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By D. Bienstock

The use of alkalized alumina in removing sulfur dioxide from a coal-combustion flue gas at 625° F was investigated on a pilot plant scale. The absorber was 26 feet long and 1.6 inches ED. Counter-current gas-solids flow at gas velocities of 8 to 15 ft/sec in the presence and absence of baffles, as well as solids entrainment at gas velocities of 20 to 23 ft/sec with solids recycle, were employed. The spent absorbent as regenerated as fixed bed with the reducing gases--reformed natural .7.7d hydrogen. Of absorption-regeneration were successful completed using the alkalized alumina rolled into spherical granules 10 to 16 mesh. There was no loss in activity of absorbent toward SO2 with a modest attrition equivalent to 0.l percent of the solids feed. Supporting studies were conducted on the effect of the sodium content in the absorbent, the composition of the reducing gas, thermal treatment to increase absorbent hardness, and removal of absorbed chlorine from the absorbent. A mathematical model was formulated to describe the removal of SO2 by alkalized aluminum from fixed and falling beds.

Jan 1, 1967

By George H. K. Schenck

Diminishing returns in management's fight to lower manufacturing expenses have added luster to savings that can be achieved in delivered costs through creative management of the distribution function. This is especially true for companies engaged in the production of bulk commodities, for which transport costs may represent 25 to 50% or more of total delivered price, A. E. Cascino, vice president of International Minerals and Chemical Corporation, recently gave an example of why top management in his firm is concerned with distribution: "The price of a ton of phosphate rock, f.o.b. mine, is about $7. The cost of warehousing, freight, and handling frequently totals an additional $11 . . . . If one of our competitors . . . discovers a way in which he can cut his distribution costs by $3, we're dead! Even if we wanted to offset our competitor's more efficient means of shipping with reduced f.o.b. price for our product-we don't have that much profit margin . . . ." In a special report on the revolution now occurring in transportation of goods, Business Week stated in its September 24 issue: "Moving and storing goods on their way from mine and mill through various sub-assemblies to their final markets costs anywhere from $50 billion to $75 billion a year- $100 billion if paperwork costs are included.

Jan 1, 1967

By A. L. Service

In 1965 the Western phosphate industry ranked third after Florida and Tennessee in total mine and marketable production of phosphate rock and phosphate rock products. It has become an important regional industry and, since the close of World War II, it has become important in the national phosphate economy. This report includes an evaluation of the trends and outlook for the Western phosphate industry through 1975 as part of the Bureau's program to determine the rate at which the Nation's mineral resources are being utilized. The first part of this report is concerned with the relationship between the Western phosphate industry and that of the United States and the world. It describes the principal phosphate deposits and discusses production, export, and import of phosphate rock and marketable products. The second part of the report is concerned with the Western phosphate industry and discusses trends and outlook through 1975. Projections for the utilization of phosphate rock, phosphate fertilizers, and elemental phosphorus have been developed and extended through 1975 in an effort to provide data and information pertaining to the rate of depletion of the Nation's phosphate resources.

Jan 1, 1967

By D. L. Archer, W. W. Owens

Conventional waterflooding often is uneconomic in highly fractured reservoirs because of the gross bypassing of the reservoir oil by injected water. Imbibition and pressure pulse flooding have been used in at least one fractured reservoir in an attempt to achieve better oil recovery performance. This paper presents the results of laboratory flow tests conducted on large cores to evaluate the possible applicability of these methods (particularly pressure pulse flooding) to different types of reservoir systems. Test data were obtained on both water-wet and oil-wet systems, and on systems having two widely different levels of compressibility and flow capacity. Results indicate that pressure pulse recoveries from fractured reservoirs will likely not exceed 5 to 10 per cent pore space with maximum response achieved during the first pulse cycle. Improved recovery by this method is possible from both oil-wet and water-wet reservoirs. Comparable saturation distributions during imbibition and pressure pulse production suggest that an initial pressure pulse cycle to speed production response would not interfere with subsequent imbibition flooding in water-wet reservoirs. INTRODUCTION There is a steady increase in the number of fluid injection projects being initiated each year to improve oil and gas recovery over that obtained by primary production mechanisms. Experience gained in different geographical areas and with different recovery methods is teaching that reservoir anatomy is one of the more important factors controlling the success or failure of such projects. Fractured formations appear to be the rule rather than the exception, especially in carbonate reservoirs. Conventional methods of fluid injection, whether it is waterflooding, gas injection or miscible flooding, have limited applicability to highly fractured reservoirs because of the severe bypassing of reservoir fluids. The result is early breakthrough of the injected fluid and rapidly increasing ratios of injected to in-place fluid with an undesirable effect on return on investment. Thus, innovations to conventional methods must be developed if recovery from fractured reservoirs is to be optimized. One new method proposed for application to highly fractured reservoirs is pressure pulse waterflooding. Although pressure pulsing with gas has been suggested' and rested in at least one reservoir; the Sohio Oil Co. is generally credited with the development and testing of pressure pulsing in conjunction with waterflooding. Publications" of Sohio's waterflood operations in the Spra-berry Trend indicate that the idea for pressure pulse flooding evolved from a critical analysis of the disappointing early performance of their flood initiated in a portion of the trend in April, 1961. This flood was planned to take advtantage of imbibiltion and high pressure gradients across the reservoir matrix blocks (unfractured Mocks of the reservoir rock which are visualized to be generally surrounded 'by the fracture system) evaluated in pilot tests by the Atlantic Richfield Co.5 and Humble Oil & Refining Co.' However, the early recovery and pressure performance of this flood indicalted that high pressure gradients induced between the fracture system and the centers of the matrix blocks were forcing water into the periphery of the blocks and temporarily interfering with the counter-current flow of oil due to imbibition. Fill-up in the blocks was occurring with re-solution of the free gas phase as pressures climbed above the original reservoir bubble point. It appeared that cessation of water injection to permit the capillary forces to become dominant and that expansion of the rock and its contained fluids during pressure reduction might aid in expulsion of oil from the rock matrix into the fractures. Subsequent production performance. aflter cessation of injection, proved this hypotheslis correct. Thus, pressure pulse waterflooding was born. Pressure pulse flooding appears to have several advan'tages over imbibition type flooding in highly fractured reservoirs. First, all wells may be used for water injection which should hasten fill-up and achieve a more rapid increase in reservoir pressure. Second, because of increased injection pressures and rates, flooding gradients will force water into the reservoir matrix more rapidly than would be achieved by imbibition alone. Third, during the pressure depletion cycle of the flood, the compressibility of the system, which has been increased by resolution of the free gas phase, provides energy for the displacement of oil at a rate greater than would correspond to countercurrent flow during imbibition. Fourth, during depletion all wells may be put on production, thus contributing to higher oil withdrawal rates on a reservoir-wide basis. One possible disadvantage of pressure pulse flooding as compared to imbibition floodling, however, is that the outer periphery of each matrix block is flooded to a residual or near residual oil saturation during the Water lnjection stage. This zone of reduced permeability to oil m'ay offer greater restriction to the production of

Jan 1, 1967

By Lowell Stroud

Ten natural gases containing from 0.023 to 8.4 percent helium were investigated. In seven high-helium samples, the isotopic abundance of Ne21 was greater than in the atmosphere, being supplemented by 33 to 85 percent of "excess" or "radiogenic" Ne21. The ratio of He4/Ne21(rad) in these gases was evaluated and found to vary between 2.9 x 107 and 5.9 x 107 , a factor of approximately 2. Argon concentrations were determined by the isotope dilution method. The isotopic ratios of Ar40/Ar36 in the high-helium gases were from 5 to 75 times the atmospheric value, with the Ar40 being about 80 to 99 percent radiogenic in nature. The ratios of He4/Ar40(rad) in all 10 gases were evaluated and found to range from 4 to 18. The isotopic ratio of N14/N15 in four of the high-helium gases was essentially the same as in the atmosphere; in three cases it was approximately 5 percent higher than the atmospheric value of 272.0. The genesis of nitrogen and the relationship of nitrogen to helium in natural gases were reviewed and are discussed in terms of a theory for the concurrent generation of nitrogen, helium, radiogenic neon 21, and petroleum (hydrocarbon gases and liquids).

Jan 1, 1967

By Theodore Kessler

The purpose of this Bureau of Mines investigation was to determine what new organic compounds or high concentrations of a particular organic species can be formed by exposure of coal derivatives to ultrasonic energy. Tetralin, l-methylnaphthalene, and pyridine were used as model compounds. Gaseous and solid reaction products resulting from the ultrasonic irradiation of these coal derivatives were determined using mass spectrometry. Products from the irradiation of tetralin were studied as a function of time, atmosphere, and sample size. The sonolysis (chemical reactions produced by ultrasonic energy) of tetralin and l-methylnaphthalene produced C2H2, HCN, CH4, H2, CO, and CO2, depending upon the experimental conditions. The ultrasonic irradiation of tetralin also produced diacetylene under certain experimental conditions. The cleavage of organic chemical bonds by ultrasonic cavitation in the absence of water was also observed in this study.

Jan 1, 1967

By A. A. Brant

"Improving geological and geophysical evaluation should serve to reduce the early-stage risk assessment and there-by contribute to exploration expenditure stimulation. The limitations of present-day methods are reviewed, particularly as to anomaly causes, depth penetration and quantitative physical interpretative abilities. Some of the problems now under study are discussed. Future developments expected include the treatment of quantitized geologic and geophysical data, as well as continuing attempts toward computerized interpretation."

Jan 1, 1967

A process was developed based on the thermal hydrolysis and precipitation of iron from solutions resulting from the leaching of zinc plant residue. A study was made of the hydrolysis of iron, at temperatures in the range 140-220°C, in both pure solutions of ferrie sulphate and in leach solutions derived from plant spent electrolyte.At 200°C hydrolysis of pure ferric sulphate solutions results in the precipitation of ferric oxide, Fe2O3, at low acid. concentrations, and a basic salt, Fe2O3.2S03.H20, at hIgher acid concentrations. At 180°C ferric oxide is precipitated at low acid concentrations, but at higher acidities. carphosiderite, 3Fe203.4SO.3.9H20, is the stable phase. Frequently a mIxture of ferric oxide and carphosldente IS produced at 180°C, the ratio of phases being dependent on the non-equilibrium experimental conditions.With solutions derived from plant spent electrolyte hydrolysIS at elevated temperatures results in the precipitation of jarosite compounds of the type NaFe3(S04)2(OH)6 The precipitation of natrojarosite jarosite, and ammonio-jarosite was studied in detail. Temperature, free acidity, and the concentration of sodium potassium, and ammonium ions are critical factors which affect the extent of precipitation.A process based on ammonio-jarosite precipitation was tested in a pilot plant.An alternative method of iron removal based on the addition of zinc oxide calcine, to neutralize excess acidity, and the precipitation of ferric oxide was also tested in the pilot plant. Both processes appear economically favourable...

Jan 1, 1967

The flolation behaviour of some Australian uranium ores was investigated. Although uraninite and pitchblend float readily with fatty acids, selective concentration to produce an economically discardable tailing has not yet been achieved. This is attributed to the presence in the ores of a quantity of uranium mineral in finely dispersed form which is very difficult to liberate. For some of the ores, at least, the proportion of this material decreases with increase in head assay.Flotation may be a useful concentrating method for some Australian ores if uranium oxide is to be sold in a free competitive market.

Jan 1, 1967

By Edna A. Dancy, Gerhard J. Derge

The specific conductance of FeOx,-CaO melts in contact with iron was found to decrease from 200 ohm-1 cm-1 for FeO, to 40 ohm-1 cm-1 for a melt containing 26.3 pct CaO at 1400°C. The temperature coefficient was positive at all compositions, but became smaller at high CaO contents. Current efficiencies for electrolysis increased from 2.5 pct in FeOx to 17.3 pct at the high CaO composition, indicating a change from predominantly electronic conduction to conduction with a substantial ionic contribution. It was shown that Ca++ ions as well as Fe++ ions carry the ionic current. A subsidiary investigation on the apparent effect of atmospheres of argon, helium, and nitrogen on the electrical conductivity showed that this could be correlated with surface temperature losses, which varied with the thermal conductivities of the gases and resulted in precipitation of metal by the reaction 3 Fe++ = 2 Fe+++ + Fe. The work described in this paper is offered as a contribution to the general fund of knowledge concerning metallurgical slags. Measurement of electrical conductivity and electrolysis are comparatively trouble -free methods for investigating molten materials, but, although these methods had been used for complex slags, it was not until the work of Bockris et al.1 that the approach of examining simple binary slag systems was employed, and CaO-SiO2, MnO-SiO2, and Al2O3-Si9 were studied. Two groups have performed work of particular relevance to the present investigation. Inouye, Tomlinson, and chipman2 studied the conductivity of wustite as a function of temperature and of the addition of 5 mol pct of a number of oxides, including CaO. They concluded that molten FeOx in equilibrium with iron is a semiconductor. Simnad, Derge, and ceorge3 demonstrated the ionic nature of liquid iron silicate slags and also concluded that, although the conductivity of FeOx in equilibrium with iron is predominantly electronic in nature, there is a small ionic contribution. The work reported here on FeOx,-CaO slags consists of three main parts, namely, the determination of the specific conductance over a wide composition range, an investigation into the nature of the conductivity through current-efficiency measurements over the same composition range, and an attempt to identify the current-carrying ions, as well as a subsidiary investigation on the apparent effect of the nature of the inert atmosphere on the conductivity. EXPERIMENTAL Materials. The slags, varying in composition from FeOx to 27 pct CaO, were prepared by heating reagent- grade Fe2O3 in an ingot iron crucible with a suitable amount of CaCO3 and, in some cases, powdered iron, in air. This prefused material was then used for the runs. At the end of each run the cell was removed from the furnace and quenched by immersing the bottom half in water. After crushing, the slags were analyzed for calcium and total iron by the usual wet methods. The oxygen content was obtained by difference. Specific Conductance: Apparatus and Method. Fig. shows the experimental setup, with the conductivity cell and leads of ingot iron. The standard four-probe method for measuring high conductivities was used. In this, the potential drop across the unknown resistance is compared with the potential drop across a known resistance connected in series, i .e., same current through both resistances. Thus there are both current and potential leads to the center electrode and to the crucible, which acts as th other electrode. Both ac and dc circuits were available for the measurements; they have been described in earlier work performed in this laboratory.4,5 The geometry of the cell was such that the center electrode was equidistant from the bottom and sides of the crucible. This ensured that the current path was the same irrespective of the magnitude of the conductivity of the material in the cell. Cell constant were measured with KC1 or NaCl solutions, which have considerably lower conductivities (0.0013 to 0.25 ohm-' cm) than the slags, and this precaution in design made sure that the determined cell constants applied to the cells with contents of any conductivity. The cell-constant determinations were made with the ac measuring circuit to prevent polarization. The four-probe method eliminates lead resistance but not the resistance of those parts of the center

Jan 1, 1967

By Webster S. Anderson

The design, development, and testing of hydraulic props to provide a lightweight, high strength, recoverable unit is described. Modifications in design incorporating threaded components resulted in the development of a lightweight hydraulic prop fabricated from aluminum alloy tubing. This new design facilitates interchange and replacement of component parts, and the physical properties of the material are not changed as they are when welding is required. The new prop is 65,000 pounds and has a maximum load capacity of a lower weight-to-load capacity ratio than the hydraulic props now available.

Jan 1, 1967

By A. A. Cochran

Bureau of MinesThe Bureau of Mines studied the development of practical methods for recovering manganese from the extensive domestic resources of low-grade ores and open hearth slags. A one-step operation was developed on a laboratory scale in which manganese and iron compounds are treated with chlorine, volatilized, and separated by selective condensation. Manganese recoveries of 90 to nearly 100 percent were obtained from 9 of the most important domestic ores. Analyses of the manganese chloride product indicated that it was suit-able for aqueous electrolysis with little additional purification. A complete, integrated process that provides for the recovery and recycling of chlorine is proposed. This process appears to have distinct advantages over previously proposed manganese recovery processes, and, in sharp contrast to leaching procedures, it is applicable to practically any manganese-bearing material.

Jan 1, 1967

By W. F. Brace, James D. Byerlee

Although prediction of failure of rocks may be ultimately possible without knowing in detail how failure occurs, understanding of this process is certainly of fundamental interest in rock mechanics. Of the various failure mechanisms, probably brittle fracture is of greatest interest. Recent reviews have brought this subject nearly up to date (Hock,1 Price,2 and Jaeger 3) and here, we summarize certain recent developments. As our understanding of brittle fracture is derived almost solely from laboratory studies this will amount to a review of certain laboratory experiments. New studies in four areas are pertinent; these concern 1) the volume changes which accompany brittle fracture, 2) the propagation of cracks in compression, 3) certain frictional characteristics of rocks and minerals at high pressure, and 4) the law of effective stress for crystalline rocks. Our objective here is less to present an entirely consistent, complete picture of how a rock fractures than it is to emphasize gaps in our understanding and, thus, suggest areas that need further study. Progress is still painfully slow in this field and perhaps this approach will stimulate new work. OBSERVATIONS Although the behavior of large rock masses is most often the concern in rock mechanics, the number of large-scale experimental tests is still vanishingly small. Our experimental observations arc, by and large, still made on small, relatively flaw-free, rock samples. Here also we report the behavior of small samples.

Jan 1, 1967

By Harry Perry

By 1980, the free world's need for economic sources of energy is expected to double. As a result, there will be a tremendous potential for all energy sources working together to supply the demand. For coal to continue its dominant role as a low-cost energy source, means must be found for it to meet the challenge of nuclear power and to overcome obstacles placed on its use by air and water pollution regulations. As the more limited reserves of gas and oil diminish, economic ways are also required for converting coal to synthetic liquid and gaseous fuels, and to chemicals, thus resulting in optimum utility of the most abundant low-cost fuel resource. The means for accomplishing these ends can only come about by a vigorous research and development program. Successful efforts by industry and government working together, both in America and abroad, will assure the continued use of coal to meet the world's energy demands. This paper discusses the emerging patterns of energy sources throughout the world and the role that research and development on coal will play in supplying future energy requirements.

Jan 1, 1967

By R. Stauffer, S. Lindsay

"Sherritt Gordon Mines Limited utilizes pressure hydro-metallurgical techniques to recover nickel, copper and cobalt from su1phidic concentrates, mattes and various other metal-bearing materials.A brief description of the nickel refinery operation is given. In the nickel refinery process, an ammonia pressure leach is employed to treat the feed materials to dissolve the non-ferrous metals as their respective ammine complexes. The resulting leach solution goes through a series of steps which removes copper as copper sulphide and further purifies the solution prior to nickel precipitation by hydrogen reduction. The reduction end solution, containing the cobalt which was originally present in the leach solution as well as residual nickel, is treated with hydrogen sulphide. The resulting nickel-cobalt sulphide precipitate feeds the soluble cobaltic ammine process, which separates the nickel and cobalt and recovers the cobalt as a pure powder.A detailed description of the cobalt recovery process is given. Included are the various steps, comprising: acid leaching of the mixed sulphides, solution purification, ammine complex formation and cobaltous oxidation, two-stage nickel precipitation, cobalt conversion and reduction. A brief description of cobalt powder handling is included, along with typical physical properties and chemical analyses of the cobalt product. In general, the purpose of this paper is to describe the present plant practices employed in the recovery of cobalt as a by-product of the nickel refinery operations."

Jan 1, 1967

By Robert E. Barieau

General expressions for evaluating various thermodynamic properties applicable to the van der Waals equation of state have been derived. These formulas were subsequently used to evaluate various thermodynamic functions in the two-phase region. The results indicate that, for a van der Waals fluid, there is a finite discontinuity in the second derivative of the vapor pressure curve, in the second derivative of the chemical potential or Gibbs free energy at the critical point, and in the heat capacity at constant volume measured at the critical density. Numerical values are tabulated and graphs are presented for all functions calculated.

Jan 1, 1967

By J. D. Campbell

"Coal is one of Alberta's major fuel resources, but its distribution, especially in the flat plains region, has been somewhat obscured by surficial deposits. After a period of neglect, easily strippable plains coal is presently approaching a position of dominance in electrical power production, a position it is likely to retain for a number of decades in the face of strong competition from hydro and nuclear power. Accordingly, the Research Council of Alberta has undertaken an inventory survey of the province's supplies of this resource.In the southern part of the province and in the north-central forest-fringe area, some strippable coal is found in the Belly River Formation and its equivalents, but major strippable coal reserves in large areas of central Alberta occur within the Edmonton Formation. The survey is planned on a reconnaissance scale, drilling test holes at 2-mile intervals in selected large areas. It appears to show that, in well-settled regions, large reserves of strippable coal are only to be expected where they have long been known; major presently unknown bodies of coal must be sought in unsettled regions or at depths too great for strip mining. However, such bodies might still be economically competitive with hydro and nuclear power in the production of electric power for some time to come."

Jan 1, 1967

By A. Gene Collins

The Bureau of Mines undertook research to determine the bromide and iodide content of Mississippi and Alabama oilfield waters of the Tertiary and Cretaceous Period to determine genetic relationships of the ions, to determine their origin, and to determine their genetic relation to petroleum. The 280 samples were analyzed after a pretreatment to remove interferences. The iodide was oxidized to iodate and was titrated with thiosulfate. The bromide was oxidized to bromate and was determined iodometrically. A computer was used to calculate the correlation coefficients of iodide to bromide and to other ions. The other ions are sodium plus potassium, calcium, magnesium, chloride, bicarbonate, and sulfate. The mineral content of the samples ranged from 52 to 1,760 mg/l for bromide and from 2 to 65 mg/l for iodide. The mean bromide-to-chloride and iodide-to-chloride ratios were 0.0065 and 0.0002. The correlation coefficient matrix and linear plots indicated a definite bromide-to-calcium relationship for the brines investigated.

Jan 1, 1967

By Witold J. S. Ostrowski

Stabilization of water-bearing sediments by the freezing method for shaft sinking has been used for over 80 years on the European Continent. The real application of this method in Canada started with the development of the potash mines in Saskatchewan during the past fifteen years. The great depth to which it is applied creates a number of problems which have to be seriously considered by engineers in order to produce a safe and economical design. Freezing depth, thickness of the ice wall, number of the freeze holes, capacity of the freezing plant, pre-freezing time, etc., are the most important points which have to be established. Recent field experience in freezing to great depth in the Saskatchewan area is immensely interesting and important for further development of our potash mining and the application of the freezing method.

Jan 1, 1967

By V. R. Miller

The Bureau of Mines investigated methods for testing the tensile and sheer strength of cast specimens of bulk solder and of soldered joints in order to increase the strength and extend the useful temperature range of soft solders. A spread-area test for determining the wettability of solder on copper surfaces was developed. Mannitol was used as a flux in spread tests to control spreading and to avoid plating, etching, and other side effects of regular fluxes. Data on commercial and high-purity solders obtained by these methods show more consistency than those reported by others from similar tests.

Jan 1, 1967