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By Alton B. Cook

The practice of using partly depleted oil reservoirs for gas-storage operations is proving successful. Moreover, this practice provides a method of secondary oil recovery when gas is cycled at full-storage reservoir pressure. Because of the relative newness of this operation, a study was undertaken to assist engineers in developing improved gas-injection and production procedures and in calculating the amount of gas needed for completely repressuring reservoirs. This paper is the third in a series reporting the progress of a study by the Federal Bureau of Mines of reservoir performance during complete gas repressuring and gas cycling. A procedure for estimating secondary oil recovery by this method is also under study. One report (7)3/ describes the laboratory equipment. The other report (8) gives (1) data on the New York City field, Clay County, Tex., which has been converted to gas-storage operations; (2) laboratory data from research with a model oil reservoir, in which primary production, complete gas repressuring, and gas cycling for the New York City field were simulated; and (3) theory to explain reservoir performance during gas repressuring.

Jan 1, 1961

By E. Morrice

This report of the Federal Bureau of Mines presents a laboratory procedure, with the requisite equipment, for electrowinning ingot (liquid) cerium metal from a fused-fluoride bath, the metal purity being about 99.9 percent. Physicochemical studies, including bath properties and electrochemistry, are included, with a speculative model of the mechanisms involved. An historical review of the methods used for electrowinning misch metals and yttrim-group metals, as well as individual rare-earth metals, is presented. The electrolytic preparation of metal from fused salt and nonaqueous media is summarized, along with the unsuccessful attempts at depositing the metals from aqueous solutions.

Jan 1, 1961

By Gordon Jackson

"There are two accomplishments of air and gas drilling: a new series of economic and mechanical challenges; and, acceptance as a standard drilling and completion tool.The new challenges are related to the concept of using a gaseous circulating medium in drilling for oil or gas. For purposes of discussion, a two part division has been made: the challenge of fluid invasion control and that of equipment and tools. Great strides have been made in the development of materials and techniques to combat formation fluid invasion. Chemicals and the ""mist drilling"" technique, now in use, have the versatility to cope with a wide range of downhole fluid entry conditions.Equipment and tools have been developed to meet the challenges of better, more economic drilling and completion possible with a gaseous circulating fluid. Economic and operational challenges remain.Acceptance of air and gas drilling as a normal operating tool was reached with difficulty. It is now established as a means of reducing costs in exploratory and develop-mental well drilling, exemplified in a recent study of 226 wells covering 419,407 feet of hole in the United States. Air reached the projected depth in 85 per cent of the operations, although formation water was encountered in 48.7 per cent of the holes. Slim hole bit performance and cost all compared for overall bit averages as part of analysis."

Jan 1, 1961

By A. E. J. Gallagher

This report summarizes the results of flotation studies conducted by the Federal Bureau of Mines on samples of extremely fine-grained lead-zinc sulfide ores. Samples from five ore deposits in the Pine Creek area, Coeur d'Alene district, Idaho, and one deposit in the Metaline district, Washington, were studied at the Albany Metallurgy Research Center to determine the recovery of sulfide lead and zinc by flotation. During the investigation it was found that flotation could be effectively applied to the selective recovery of exceedingly fine-grained lead and zinc sulfide minerals. Separation of galena and sphalerite was obtained on pulps ground through 1,600-mesh, in which most of the particles were smaller than 5 microns. Selectivity and recovery of minerals in this fine size range were enhanced by use of a chemical dye, diphenylthiocarbazone, as a galena promoter. Although unsuccessful on one ore, application of the dye in treatment of two other very fine-grained ores yielded lead concentrates containing over 62 percent Pb at recoveries in excess of 85 percent. More than 55 percent of the lead in these concentrates occurred as particles smaller than 2 microns.

Jan 1, 1961

By F. E. Armstrong

This report describes development and application by the Bureau of Mines of techniques and instruments for using radioactive inert-gas tracers to determine flow paths through petroleum reservoirs that have natural fracture systems and for which water injection has been selected as the stimulative production method. A field test was made to prove the techniques and evaluate instrumentation. The feasibility of applying the techniques and instruments to the solution of reservoir problems in other stimulative methods of production also is discussed. Oil commonly is displaced from sandstone host rocks by the action of a driving force that causes the oil to move through interstices of the rock and into production wells. In addition to the requirements of oil being trapped within the sand pores and the presence of an effective displacement mechanism, the rock itself must have adequate permeability to permit flow of oil and other fluids.

Jan 1, 1961

By R. A. Wood, R. I. Jaffee, H. R. Ogden, D. N. Williams

Dispersion-containing titanium-copper alloys were prepared having mean free paths varying from 1.0 to 9.7 P. Tensile studies at room temperature and at 1000°F showed that little or no strengthening occurred when the mean free path exceeded 3 p. However, at lower values of mean free path appreczable strengthening was observed. A considerable amount of strengthening also resulted from copper in solid solution. DURING the past several years, an increasing amount of study has been devoted to dispersion hardening, an alloying process in which increased strength is obtained through the addition of a ran-

Jan 1, 1961

By M. J. Ackerman

This study was undertaken to make a comparison between the cost of mining coal under roof bolt and under conventional timber methods of roof support. Studies were made at 14 mines in Pennsylvania, eastern Ohio, and northern and southern West Virginia. At each mine data were obtained for sections of the mine where the physical conditions, mining equipment, and mining systems were similar. Coal, recognized as one of the basic industrial fuels, is very competitive with other fuels, and management, in order to protect and enlarge its market, must be continually alert to find more efficient methods of production. Continuous production of coal is desired by all operators but never obtained. In mechanized mining the performance and production vary with operating time, which can be interrupted by many variable factors, such as condition of the roof, method of roof support, condition of equipment, water, ventilation, power, transportation, efficiency of operating crew, and supervision.

Jan 1, 1961

By Donald F. Smith

This report describes the construction and calibration of two ice calorimeters and includes results of high-temperature heat-content measurements, made by the Federal Bureau of Mines, on rubidium fluoride, hafnium tetrafluoride, cesium chloride, and cesium iodide. The heats and entropies of fusion of rubidium fluoride, cesium chloride, and cesium iodide have been calculated at their respective melting points using equations derived from the experimental heat-content data. Hafnium tetrafluoride did not melt within the range of temperatures investigated. Heat and entropy of transition of cesium chloride from the alpha to the beta form were also determined. INTRODUCTION Free-energy data usually afford the cheapest and quickest means of determining the feasibility of experimentally untested reactions. For known reactions, free-energy data show the variation of the equilibrium constant with temperature and make it possible to calculate, without experiment, the maximum ratio of product to raw material for a given chemical process.

Jan 1, 1961

By Francis J. Quinn

The Natural Gas Act, of 1938, which put interstate pipelines under the jurisdiction of the Federal Power Commission, did not place a protective competitive shield around such companies - nor does any provision of the act guarantee them a profit. Natural-gas pipelines are competitive with each other and also with the coal and oil industries. Gas distributing companies must compete not only with the coal and oil industries, but also with the electric industry. Natural gas has captured markets from oil, which had taken them from coal. Oil men contend that gas prices have: been, held to an artifically low level by regulation. The electric industry is moving into the space-heating market, which pleases the coal people because the coal industry's largest customer since losing the railroads to dieselization has been the electric companies. The coal industry is attempting to monopolize the industrial and electric generating market through government intervention, and this is being done under the guise of concern for the national welfare through advocation of a "National Fuels Policy purporting to, further the cause of fuel conservation. Such a policy is contrary to American principles and would result in the individual's loss of freedom of choice and ultimately, in less reserves of preferred fuels because of diminished exploration efforts.

Jan 1, 1961

By J. B. Gayle

During the past several decades, there has been a steady increase in the number and size of experimental ovens used for carbonization research. Although many were originally intended principally for studies of coal expansion, current practice usually includes determinations of the properties of the experimental cokes. With respect to size and shatter characteristics, the cokes from the larger experimental ovens closely approximate those from duplicate charges carbonized in commercial ovens; however, they are consistently lighter and frequently less resistant to degradation by abrasive forces. To minimize these differences, some operators dry the experimental charges before carbonization. The resulting higher dry coal charge densities do, in fact, yield cokes with gravities closely approximating those produced commercially from the same coal or blend but without drying. The drying of the experimental charges may be criticized on the grounds that it represents a departure from commercial practice and may result in oxidation of the samples; for these reasons, the practice has not been universally adopted.

Jan 1, 1961

By A. N. Fried

With the growing importance of fluid injection in recent years, the petroleum industry has been investigating and field- testing a variety of new methods designed to modify the physical properties of reservoir oil to improve the efficiency of gas and water injection. These procedures include condensing-gas drive, LPG (liquefied petroleum gas) injection, alcohol-slug process, high-pressure-gas displacement, detergent-solution flooding, and in situ combustion (30, 37).3 A new and different method to increase the effectiveness of gas and water injection has been tested by the Bureau of Mines, Consideration of both fundamental and practical factors that operate to limit the oil recovery attain- able by conventional oil-displacement mechanisms led to the concept of a displacement mechanism called the foam-drive method. This report describes the experimental study that tested this concept in the laboratory.

Jan 1, 1961

By E. G. King

An earlier Bureau of Mines report4 provided low-temperature heat-capacity and entropy data for three sodium vanadates. This report continues the study of vanadates by presenting analogous data for three crystalline calcium vanadates - calcium metavanadate (CaV206), calcium pyrovanadate (Ca2V2O7), and calcium orthovanadate (Ca3V208). No similar data for these compounds have been published previously. MATERIALS All three vanadate samples were prepared by the Bureau of Mines by heating stoichiometric mixtures of reagent-grade calcium carbonate and vanadium pentoxide.5 Calcium metavanadate was prepared at 610° to 660° C. A stoichiometric mixture was heated for 17 days with intervening grindings, mixings, and adjustments of composition, as shown necessary by chemical analysis. The final analysis gave calcium oxide, 23.48 pct. (theoretical, 23.57 pct.) and vanadium pentoxide, 76.32 pct. (theoretical, 76.43 pct.). The sample also contained 0.11 pct. acid-insoluble matter. The X-ray diffracton pattern showed no lines of free calcium or vanadium oxides. No X-ray diffraction patterns were found in the literature for any of these substances.

Jan 1, 1961

By William H. Dresher

A study has been made of the reaction mechanisms occurring during the salt-roast process to form water-soluble sodium vanadate compounds from the vanadium oxide compounds present in vanadium-bearing ores and concentrates. Two reactions have been identified, either of which lead to water-soluble compounds--oxidation of sodium chloride by water vapor and. oxidation of sodium chloride by oxygen. The former reaction has been found to be predominant in the salt-roast process. A kinetic treatment of the data has shown that for the formation of sodium metavanadate the rate-controlling step in the reaction, in which sodium chloride is oxidized by water vapor is the decomposition of a species containing water and sodiumm chloride, on the surface at the gas-solid interface. For the formation of sodium pyrovanadate, the rate-controlling step is the decomposition of a species containing water and sodium metavaradate on the surface. The transportation of water through the system, perhaps as a sodium chloride-water complex or a sodium metavanadate-water complex, and the actual chemical reaction are relatively fast compared to the initial surface decomposition step. A similar treatment on the data for the oxidation, of sodium chloride by oxygen has shown that the rate-controlling step, is the actual transportation of oxygen from the gas-solid interface to the reactive site. This transportation is by a sequence of two diffusion processes. Transportation during the early stages of the reaction is by the diffusion of oxygen through a continuous layer of reaction product. After, the first few minutes of reaction time a second diffusion process begins and is continuous for the remainder of the reaction. This second diffusion process involves the diffusion of oxygen, through a layer of reaction product that has developed voids around which the oxygen must diffuse. The hindering, nature of this latter process causes the rate of transportation of oxygen to the reaction site to be considerably slower than by the simple diffusion mechanism initially followed. A thermodynamic treatment of the data has shown that the energy of activation for the decomposition of the water-sodium chloride species on the surface is -12.1 Kcal. per mole. For the decomposition of the water-sodium metavanadate species on the surface' the energy of activation is -15.1 Kcal. per mole. The results of this study indicate the limiting mechanisms of the basic reactions occurring during the salt-roast process. These results suggest what variables should be examined in applying this information to actual plant operations.

Jan 1, 1961

By Mary S. Esfandiary

U.S. scientists attempting to maintain continuous surveillance of scientific information are confronted with two acute problems: The steady, even spectacular; increase in the volume of such information and the fact that much of it is published in unfamiliar foreign languages, According to the National Science Foundation, almost one-third of the world's scientific literature is published in languages that are read by less than 5 percent of U.S. scientists. Most scientists in the United States must rely on abstract journals and translations to obtain information on developments in research and investigations conducted in the non-English-speaking countries. However, there are problems involved in procuring suitable abstracts and translations and in obtaining such information as cheaply and rapidly as possible.

Jan 1, 1961

By R. B. Porter

Bench-scale tests were performed by the Federal Bureau of Mines on lignite and subbituminous coal at pressures to 1,000 p.s.i.g. (pounds per square inch gage) in atmospheres of hydrogen or nitrogen to obtain information concerning the influence of pressure on carbonization of normally noncaking coals. The distribution of gaseous, liquid, and solid products as a function of processing pressure was determined. Except for special experiments, the carbonization was at 940° F. In a hydrogen atmosphere above 400 p.s.i.g., agglomeration of the solid residue (especially with lignite) became noticeable and increased directly with the processing pressure. Although in some instances the solid particles fused together, the mechanical strength of the agglomerate was always low. On the basis of visual inspection, the coals agglomerated in the following order of decreasing intensity: (1) Steam-dried lignite; (2) lignite; and (3) subbituminous coal. Addition of lignite tar in quantities to 25 percent by weight of charge did not increase agglomeration or change the carbonization characteristics of the coal.

Jan 1, 1961

By J. G. Walters

In 1928, the Coal Carbonization Section of the Federal Bureau of Mines, in cooperation with the American Gas Association, began a survey of the carbonizing properties of American coals. A standard test method for evaluating the carbonizing properties of coals that met the following conditions was developed: To yield products similar to those obtained in commercial operations. To produce yields sufficient to permit analyses and tests of quality. To be laboratory size. To be convenient to operate. To permit reproducible control of test conditions and results. This test method has become known as the Bureau of Mines-American Gas Association (BM-AGA) test (53),3/ and more coals of greater variety have been tested in this apparatus than in any other of similar scale.

Jan 1, 1961

By Floyd G. Anderson

The Federal Bureau of Mines promotes the use of safe and effective dust-collecting devices for rock drilling in coal mines. To insure that such devices are available to the coal-mining industry, the Bureau issues certificates of performance for dust-collecting systems and certificates of approval for dust collectors and rock drills or other mining equipment with integral dust-collecting systems that meet the requirements of an established Schedule.4/ Investigations are conducted under the provisions of the current revision of this Schedule by engineers of the Branch of Health Research. This circular describes briefly the requirements and procedure for obtaining certificates of performance or approval and lists equipment that has been certified as permissible under Schedule 25 or its revisions as of January 31, 1961. The names and addresses of companies to which certificates have been issued are listed alphabetically at the end of this circular.

Jan 1, 1961

By W. W. Mullins

The development, by the mechanism of volume diffusion, of a grain boundary groove on an interface separating a solid phase and a saturated fluid phase is calculated under the following assumptions: 1) isotropy of the interfacial free energy 's, 2) applicability of the Gibbs-Thompson formula relating curvature and chemical potential, 3) a nearly planar groove surface. The groove profile is found to have a .fixed shape and linear dimensions that are proportional to (time)1/3. The constant of proportionality is evaluated and involves ?s in such a way that the latter my be evaluated from grooving kinetics. A grain boundary that intersects an interphase interface will tend to produce a groove along the line of intersection (Fig. 1). The ultimate motivation for the formation of the groove is the reduction in interfacial free energ that occurs as the grain boundary contracts. Smith has discussed the way in which the free energy of the interfaces determines their dihedral angles at the groove root and has given a detailed analysis of the effect of the dihedral angles upon the nature the microstructures developed in polyphase alloys. Herring2 has extended the considerations to the case in which the free energy of an interface depends on its orientation and has thus added torque terms to the condition for interface equilibrium. Although the grain boundary and the interphase interface may quickly achieve the proper equilibrium angles where they intersect, as determined by the balance of equivalent tensions and torques,"2 the groove will generally continue to grow (though with decreasing speed). Thermodynamically, this continued growth reflects the fact that the lowest free energy cannot be achieved until the entire grain boundary has been eliminated; mechanistically, the growth occurs in response to inhomogeneities of chemical potential that are caused by the constraint of fixed dihedral angles at the groove root. The latter point is illustrated in Fig. 1, which shows that atoms* near the groove are on the convex side of a cylindrically curved surface and therefore have a higher chemical potential than atoms on the flat interface beyond. Thus atoms tend to leave the curved groove shoulders and force the groove to deepen. When both phases are solid additional chemical potential gradient may arise from whatever strain fields are necessary to insure continuity of material across the interface. In the discussion that follows, this complication due to strain will not occur since we always assume one phase to be a fluid and the other a solid. The transport processes that may operate to permit growth of the groove are surface (interface)* diffusion, volume diffusion in the phase on either side of the interface, and evaporation-condensation when one phase is gaseous. (Also a melting-freezing process is responsible for groove enlargement on a solid-melt interface as discussed in Sec. VI). The theory of grain boundary grooving has been discussed in detail for the processes of surface diffusion and of one type of evaporation-condensation.3'4 The theoretical predictions for the mechanism of surface diffusion have been confirmed in an experimental study of grooving kinetics in copper.5 In this paper, the theory of groove development by volume diffusion will be presented. Volume diffusion can occur either by atomic migration in the solid S or by diffusion of S atoms in the fluid phase, or solvent, adjacent to the groove surface. As discussed in Sec. V, volume diffusion in the solid should be less important than surface diffusion in forming a groove. Apart from verifying this statement then, the main interest of the present analysis centers on diffusion in an external solvent. The solvent may be either a liquid (e.g., water, or-

Jan 1, 1961

By D. A. Pirttinen

The promotion of improved coal quality for thermal generation can benefit our national economy. The construction of electric generating facilities in Canada is expanding at a rapid rate to satisfy the demands of a rising population and new uses for electrical energy. With remaining economic water power resources in the process of development, generation from thermal sources continues to grow. The increase in thermal capability has been somewhat arrested by a de-pressed economy, widening of inter-provincial and state transmission networks and decisions to exploit certain water resources before high capital investment is further in-creased by rising construction costs. The introduction of extra high volt-age transmission lines will further delay thermal generation planning, but in due course, when the effects of restrictive factors have been dissipated, steam-electric generation from fossil fuels will rise to considerable proportions. In time, nuclear sources will contribute a growing share to thermal power, but, it is doubtful if nuclear participation will ever displace conventional fuels for steam rising, unless it can be adapted to operate efficiently for variable outputs in peaking service. It appears certain that fossil fueled

Jan 1, 1961

By R. B. McIntosh, S Ramanchuk

A brief description is given of the process used by Sherritt Gordon Mines Limited to recover cobalt metal from nickel-cobalt sulphides. A description of the equipment with the operating conditions is presented with an evaluation of the corrosion test results for various stainless steels and other acid resistant materials for the part of the process involving the sulphuric acid leaching of nickel-cobalt sulphide slurry under air pressure. SINCE 1954 the Sherritt Gordon ammonia leach process has been used at Fort Saskatchewan to recover nickel metal, copper sulphides and cobalt-nickel sulphides from nickel concentrate produced at Lynn Lake, Manitoba. 'To develop a process for recovering cobalt and nickel from the cobalt-nickel sulphides, studies were carried out in the Sherritt Gordon laboratory and pilot plant and, late in 1957, continuous acid leaching of sulphides was started in the refinery. In September 1958 the present equipment

Jan 1, 1961