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By L. G. Jones, A. S. Odeh

A theoretical developtment is presented which provides a straightforward method of handling the drawdown analysis for both oil and gas wells flowing at variable rates. In the past our inability to analyze variable-rate drawdowns has been a major obstacle in using them for formation evaluation. This method should permit wider use of these tests in the future. INTRODUCTION Pressure build-up analyses are widely used to obtain reservoir data such as the effective flow capacity of the formation. On the other hand. although pressure drawdowns have been run for a long time, they have not been used extensively to evaluate reservoirs because they are difficult to analyze. One of the difficulties in analyzing pressure drawdowns has been that the theory developed until now has required the test to be run at a constant rate. For both oil and gas wells this is a difficult requirement to satisfy. especially during the early period of a well's life when drawdown tests are usually run. In spite of this limitation, drawdown tests are often run with build-ups as a check. In this paper a theory, which handles the drawdown analysis for variable rates, is presented for both oil and gas wells. Thus, one of the biggest deterrents to running drawdowns is removed, and they should become a much more useful engineering tool in the future. THEORETICAL CONSIDERATIONS 011, RESERVOIRS The general equation used for describing the unsteady-state radial flow of slightly compressible fluids in homogeneous porous media can be written in cylindrical coordinates as where r is the radial distance in cm, t is the time in seconds, p is the pressure at r and t in atmospheres, + is the fractional porosity, p is the viscosity in cp, c is the compressibility in vol/vol/atm, and k is the permeability in darcies. There are a number of solutions of Eq. 1 for various boundary conditions. One of these is the so-called "point-source" solution, which approximates the case of an infinite oil reservoir with a well located at r = 0 and produced at a constant rate. The point-source solution of Eq. 1 is

Jan 1, 1966

By C. E. Reistle

All crude oils become more viscous when chilled, but the only oils that congeal and precipitate paraffin to such an extent as actually to cause production troubles are those that contain an appreciable amount of wax. In handling these oils of high wax content, three distinct problems may be encountered before the oil reaches the refinery. The first problem is the precipitation and accumulation of paraffin in the well, either in the oil string or on the face and in the pores of the sand. The second problem is the accumulation of paraffin and the congealing of oil in the transportation lines. The third problem is the precipitation of paraffin and the formation of tank bottoms. Factors That Control the Solubility of Paraffin in Crude Oil Two main factors, possibly three, govern the solubility of wax in crude oil. The first of these is temperature. The solubility of wax in crude oil increases with an increase in temperature, and as the temperature approaches the melting point, the wax becomes soluble in all proportions in the crude oil. The higher the melting point of a wax, the less soluble it is in crude oil below its melting point. All crude oils containing wax can be chilled to a point where the oil is saturated with wax. If the temperature is decreased below this point, some of the wax will crystallize from solution. Fig. 1 shows the effect of temperature on the solubility of crude paraffin in oil. The second factor is the amount of volatile constituents and gas removed from the crude oil. Evaporation of the volatile constituents and gas lessens the volume of the oil and concentrates the solution of wax in the oil; therefore less wax can be held in solution at a definite temperature. As the natural amount of wax present in the oil is constant, this results in the oil becoming saturated with wax at a higher temperature than if the volatile constituents and gas were still in the oil. As an example of this, a fresh sample of crude oil having a gravity of 39.8

Jan 1, 1928

By R. L. Orr, J. D. G. Masse, Ralph Hultgren

The relative partial molar enthalpies of gold and tin in liquid Au-Sn alloys have been measured from Xsn = 0.474 to 0.510 at 696°K, slightly above the melting point of solid AuSn. Within an average precision of 6 cal per g-atom, the data are represented by two smooth curves, which satisfy the Gibbs-Duhem relationship and which do not show any anomalous behavior in the range of composition studied. The results give no support to the hypothesis that atomic associations in the equiatomic liquid alloy resemble those in solid AuSu. LITTLE has been firmly established as to the nature of atomic distribution in liquid metallic phases. A favored hypothesis assumes the existence of atomic groupings in the liquid phase which are similar to those in solid phases occurring at lower temperatures. Beginning with this hypothesis, it is often possible to adjust the values of certain parameters (such as degree of association) so that approximate agreement is achieved with certain features of the X-ray diffraction pattern of the liquid, even though many other possible structures might satisfy the data equally well. Thus, in this manner, the structure of liquid tin has been described as a dispersion of fragments of gray tin in a matrix of metallic tin.1 Four X-ray diffraction studies2"5 have been made of the liquid alloy of composition AuSn at temperatures slightly above the melting point of the solid. Each investigator concluded, on somewhat different grounds, that the liquid consisted to a large extent of arrays of atoms similar to the solid, with admixture of more disordered arrays. Solid AuSn has the nickel arsenide crystal structure: each tin atom has six nearest neighbors, all gold atoms; and each gold atom has six tin and two gold atoms as nearest neighbors. It remains highly ordered to the melting point. The liquid alloy has a large exothermic (?H700° K = -2700 cal per g-atom6) enthalpy of formation, favoring ordering and making the hypothetical molecular association not unreasonable. The possible existence of such solidlike arrays, or of a high degree of order that occurs preferentially at a specific composition in a liquid alloy, might also be revealed by thermodynamic behavior somewhat analogous to that in highly ordered solid alloy phases. The latter often exist over wide composition ranges, within which the highest degree of order occurs at the ideal composition for which the atomic fractions are equal to the fractions of sites which are "right" for each kind of atom. On departing from the ideal composition, the excess atoms occupy "wrong" positions, raising the internal energy and making it progressively easier for additional atoms to occupy "wrong" positions. Thus, on either side of the ideal composition, there should be a pronounced rise in the entropy and enthalpy, which would be shown particularly by the change in the relative partial molar enthalpies, ?Hi, since they depend strongly on d?H/dx. In the one case where accurate measurements have been made, the solid AuCu ordered phase, the structure becomes much less ordered as the composition deviates from the ideal, and relative partial molar enthalpies change sharply as shown by the data6 given in Table I. This suggests the possibility of finding similar pronounced changes in the relative partial molar enthalpies of gold and tin in liquid alloys near the composition AuSn if the postulated solidlike ar-

Jan 1, 1967

By A. J. Boyer, T. R. Meadowcroft

An experimental determination has been made of the efject of surface diffusion on the vapor pressure obtained in a Kwudsen cell. The results show that a knife-edge orifice in a molybdenum lid may give erroneous results for the vapor pressure of silver. when a correction suggested by winterbottom and Hirth is made, the results become meaningful. Experimental work with cylindrical orifices in molyhdenz~m lids and knife-edge orifices in ceramic lids shows that good vapor-pressure results may he obtained when the orifice is designed so that ejfusion is the only significant source of weight loss. THE Knudsen effusion cell technique has been used by many investigators to study relative and absolute vapor pressures over metals and alloys at elevated temperatures. As a result of this interest, some theoretical studies have been made of geometric factors affecting effusion from the orifice of a Knudsen cell. A review of these studies has been made by Margrave.1 Recently, Winterbottom and Hirth2 have suggested that a physical effect, that of condensation, surface diffusion, and re-evaporation, may seriously affect Knudsen cell measurements, especially when a knife-edge orifice is used. Inasmuch as many of the present vapor-pressure data have been obtained using knife-edge orifices. it was felt that an experimental evaluation of the effect of surface diffusion on Knudsen cell measurements would be of value both in the design of the cell orifice and in establishing realistic estimates of the limits of error for existing data. The experimental program was in two sections. Firstly, measurements of the vapor pressure of silver were made in cells with cylindrical and conical orifices in which the surface-diffusion contribution to the weight loss should be negligible. These results were correlated with existing data to give a reliable measure of the real vapor pressure of silver. Secondly, measurements made using knife-edge orifices were corrected using the surface-diffusion theory of Winterbottom and Hirth2 and were then compared to the real values. The experimental arrangement is shown in Fig. 1. The balance was an Ainsworth RV-AU-1 automatic recording microbalance capable of measuring weight changes of ±0.02 mg on a total load of up to 100 g. The temperature was measured by an optical pyrometer signted on the bottom of the suspended crucible. The temperature readings were calibrated in a separate experiment in which pyrometer measurements were made while at the same time thermocouple readings were taken of the temperature at the inside top and bottom of the crucible. The range of reproducibility with this technique was ±4°C. A constant voltage source maintained a temperature of ±2°C at 1200°C over 10 hr. Silver of 99.99 pct purity was used in nonporous alumina crucibles. Lids of molybdenum, tantalum, or magnesia were cemented to the crucible using a sodium silicate cement. Table I shows the characteristics of the lids used. The vapor pressure is obtained using the basic Knudsen formula:

Jan 1, 1965

By Norris Johnston, Carrol M. Beeson

For many years the permeability of reservoir sands has been measured by flowing air through a cleaned and dried core sample. This differs from the true reservoir permeability in one important respect: the rock particles in the reservoir are surrounded by interstitial water, not air, and their physical shape and condition of hydration are greatly dependent thereon. Permeability as defined must be measured with a single-phase fluid. Since no means exist for removing the oil and gas from a core sample by simply flowing water through it, the sample must be cleaned and then resatu-rated with water before testing. The present discussion attempts to show that after the cleaning process a considerably different permeability is determined with salt or fresh water than is obtained with air. The postulate is made that the salt-water permeability is probably closer to the true reservoir permeability than is the measurement with air. This is discussed in relation to both physically possible and economically feasible measuremerits. Data On more than 1200 core samples are given to show the nature of the effects observed, and a plea is made for others to consider water permeability measurements as a routine necessity, eventually replacing air permeability in regions where the differences are great. Introduction Permeability is defined1 as a "a measure of the capacity of a porous medium to transmit fluids, when there is no interaction between the solids and the fluid." Darcy's law of liquid flow in porous media states: kA?P QµL/A?L [I] where Q represents milliliters of liquid of viscosity p centipoises passed per second through a porous medium of permeability k darcys and cross-sectional area A sq. cm. under a pressure gradient ?P/L atmospheres per centimeter, the flow being understood to be laminar or viscous, not turbulent. This equation defines the darcy. For the case of radial flow in a uniform sand, such as usually exists in the neighborhood of a well in an oil or gas sand, Darcy's law becomes:2 Here h is the net sand thickness in feet, Pe and Pw are pressures at the drainage radius4 and well radius, and re and rw are these radii, respectively. The productivity index3 is defined as the barrels of liquid produced per day per pound per square inch mean pressure differential between ferences and well bore, and is thus: By further definition, the specific productivity index is: or in terms of practical units, and allowing for shrinkage:

Jan 1, 1945

By M. H. Waxman, M. Gondouin, H. J. Hill

Streaming-potential experiments were conducted within the Muddy- and Dakota-sandstone interval of a Denver basin well. Analysis of the data shows that, for this case, streaming potentials opposite sands were higher than those opposite shales when the mud was fresh. Streaming potentials opposite shales, however, were of sufficient magniiIlde to be important in SP interpretation. They were linearly dependent upon pressure differential, and they increased with mud filtrate resistivity. The magnitude of streaming potentials opposite sands was influenced by the characteristics of the original mud cake formed at the time of drilling. Use of mud samples taken at the time of logging may not always be satisfactory for determining streaming-potential corrections. Both the streaming and electrochemical potentials were found to be affected by the previous history of the borehole system. Following a change in mud characteristics, several days were required for SP stabilization. This was, in part, due to the mud cake acting as an imperfect shale membrane. INTRODUCTION Laboratory investigations by Wyllie,1 Salisch,2 Moore," Sen Gupta and Bannerjee,0 and Hill and Anderson' have shown that streaming potentials developed across mud cakes deposited on permeable filter beds are of sufficient magnitude to be critically important in SP interpretation. Streaming potentials across shales have been reported by Schenck,' Gondouin and Scala; and Hill and Anderson." The magnitude of the shale streaming potentials obtained by Schenck and by Gondouin et a1 led these authors to conclude that in many cases the shale streaming potential would approximately equal the mud-cake streaming potential. Hill and Anderson, however, obtained somewhat lower magnitudes of shale streaming potential. The field experiment described in the present paper was a cooperative project carried out by the respective operations and research departments of Schlumberger Well Surveying Corp., Shell Development Co. and Shell Oil Co. The primary objective of the experiment was to determine in the borehole the streaming-potential behavior of both shales and mud cakes under conditions approaching, as nearly as possible, those normally encountered in logging practice. METHODS AND EQUIPMENT WELL A Muddy- and Dakota-sandstone vie11 in the Denver basin was chosen for the experiment. Both sandstones were water-bearing and, since reservoir pressures in these sandstones are abnormally low (gradient of approximately 0.25 psi/ft), it was expected that studies of streaming potential could be conducted from low-pressure differentials (approximately 200 psi) to about 27000 psi by bailing mud from the hole, filling up and then applying wellhead pressure. The selected well encountered the Muddy sand-

By D. K. Deardorff, Earl T. Hayes

An improved technique is described for the accurate determination of melting points of metals in the temperature range 1500' to 2500°C. The improvements consist of gradient heating and refinements in cavity preparation to obtain true black-body conditions. The melting point of hafnium, as determined by this method, is set at 2222°±30°C. This is over 200°C higher than one of the values reported earlier. Discrepancies in the previously reported values for the melting point of hafnium are explained. The melting points of zirconium and titanium are found to be 1855O±15OC and 1668°±10°C, respectively. Reproducibility of results was ±3OC. PRIMARILY, this report is being made to correct a 1975o±25oC1 value for the melting point of hafnium, and to present an improved method for melting point determination. As a matter of interest, the technique was also applied to determining the melting point of zirconium and titanium. There is a wide difference in the melting point of hafnium as reported by competent investigators. DeBoer and Fast' reported a value of 2230°±500C, and later work of McPherson, as reported by Aden-stedt, placed the melting point at 1975o±25oC. Zwikker" calculated that the melting point was 2430°C. In resolving this discrepancy, improvements were made in the procedure for determining the melting points of refractory metals in the range 1500" to 2500°C. Special techniques are necessary to determine the melting point of these metals accurately. Since the metals oxidize in air above 900oC, the determinations must be carried out in an inert gas or vacuum. Also, every known refractory contaminates them to some extent. In addition, the attainment of true black-body conditions is always difficult. DeBoer and Fast actually determined the melting point of Hf-Zr as-deposited iodide process alloys and extrapolated to 100 pet Hf. McPherson employed a tungsten wire suspension similar to that described by Schramm, Gordon, and Kaufmann,1 and used hafnium metal produced by the iodide process. There was no apparent reason for the wide spread in melting points, since the quality of the metal was very good and the work was under the direction of highly competent investigators. Retracing some of this work revealed one understandable error in the case of hafnium, and led to development of an improved technique for determining melting points of reactive metals in the range 1500" to 2500°C. Material Crystal bar hafnium, zirconium, and titanium were used for this work, with analyses as shown in Table I. The hafnium was of the highest purity that has been prepared, though not as pure as the zirconium and titanium. At the instigation of the Pittsburgh Area Office of the AEC, a special lot of Hfo2 was purified, converted to the tetraflouride, and bomb-reduced with calcium, all at the Iowa State College Laboratories. This crude hafnium metal was then refined by the iodide process at the Foote Mineral Co. All specimens were cut with a Sic wheel, ground, pickled, and dried carefully before use. Procedure General Tungsten Suspension Method—In this method, a small specimen is suspended by a fine tungsten wire in a slender, induction-heated tungsten or tantalum cylinder, all under vacuum. The melting point is determined by heating the specimen slowly while observing it with an optical pyrometer focused upon a portion of the specimen that radiates as a black body. This means that there should be no reflected radiation, either from colder objects near the pyrometer or from hotter surfaces. The induction heater would be the only hotter object and, if it is slender enough, the specimen will attain the same temperature. Often a slender hole is drilled into the specimen as a source of black-body radiation. This was the general method used by McPherson in obtaining his value of 1975°C for the melting point of hafnium. In trying to repeat this work, it was found that the points of contact between the

Jan 1, 1957

LIST OF MEMBERS AND ASSOCIATES ARRANGED ACCORDING TO STATES AND TOWNS. ALABAMA. Aldrich, Aldrich, W. F. Anniston, Noble, A. E Bessemer, Fergusson, V. Bir¬mingham, Aldrich, T. H., Jr, Bowron, C. E, Bowron, J., Davis, F H, Dimmick, F. D., Hillman, Ludwig, C. P., McCarthy, M. E, McCormack, G B., McCrery, Ramsay, E, Shook, A. M. Ensley, McDonald, S., Shook, J. W. Gadsden, Lee, R. H., Jr. Gannts Quarry, Hiller, E Helena, Squire, J. Huntsvalle, Moss Le¬high, Toulmin. Ozmoor, Greenamyer, A. G. Rock Run, Garvin, J M. Selma, Saylor, B. F. A. Sheffield, Miller, D, I. Tuscaloosa, Lodge, J. Woodward, Wood¬ward, A. H. ALASKA Coppermount, Wiswell, H. J. Douglas Island, Macdonald, J Ellamar, Stevens, B. Fairbanks, Hamilton, A L Haines, Le Wald, E A. Jualin, Hoggatt, W. B. Juneau, Denby, Hampton, W. H , Thane, B L , Whipple, J. R. Ketchikan, Bar¬ber, J C , Parker, J. L., Reid, G D Nome, Garfield, C D. Snettwham, Tisdale. Teller, Hirshberg, M. R. Treadwell Caty, Kinzie, Stow, H. P. Valdez, Esterly, G. M, Hazelet.

Jan 1, 1910

TO THE. BOARD OF DIRECTORS AND MEMBERS OF THE AMERICAN INSTITUTE OF MINING AND METALLURGICAL ENGINEERS GENTLEMEN Submitted herewith are the report of the Treasurer for the year 1945 and reports for the same year of the following committees: Membership, Admissions, Papers and Publications, Mining and Metallury (Magazine), and Library. In this review of the year by the Secretary reference frequently will be made to the "Paul" Committee and to the "hotter" Committee. The first is the special committee on Divisional Relationships and the second the special Committee on Ways and Means. These two important committees, appointed by President Harvey S. Mudd under authorization of the Board of Directors on March 21, 1945, were composed as follows:

Jan 1, 1946

By Jonathan Ludlow, Paul J. Guay

Based on two studies that were funded by the U.S. Department of Energy, the authors provide an overview of the benefits expected from mining deeper webs on United States longwalls. The first study, completed in November 1979, identified the limits and potential gains from taking deeper webs with presently available equipment. The second on-going study discusses the conceptual design and benefits of a future system for taking very deep webs.

Jan 1, 1981

By Robert L. Marovelli

A recent reorganization placed the health and safety research activities of the Bureau of Mines under a director, Division of Minerals Health and Safety Technology. The new health and safety research organization and its position in the Bureau hierarchy is shown in Table 1.

Jan 11, 1979

Jan 1, 1908

By Frederic Benard

PRIOR to 1936, the Ontario Refining Co. received all incoming blister copper from The International Nickel Company's smelter in the usual form of 460-lb. cakes, or slabs. These were received in open cars in lots of 250 pieces. At the refinery the cakes were unloaded onto narrow-gauge cars, for convenient handling and pickup by charging cranes. In March 1936, an investigation was started on the feasibility of trans-ferring converter copper in the molten state from the smelter to the refinery anode furnaces, a distance of 114 miles. Although common in steel practice, the transportation of blister copper in this form had not previously been attempted and a preliminary study of the various factors involved was therefore necessary. For this purpose, a series of experiments was made in which molten copper, removed at different stages during the furnace cycle, was held in a small portable holding furnace. This vessel was essentially a refractory-lined steel cylinder provided with ports for filling and emptying, heated by an oil burner. Dimensions of the steel shell were 3 ft. 10 in. diameter by 7 ft. 3 in. long, and thickness of refractories depended oil the design and combination used for the particular experiment. The vessel was filled with approximately 2 ½ tons of copper at a predetermined temperature, the lining having been preheated to a definite point by means of an oil burner. All openings were well luted and temperature readings were made every 15 min. by means of an immersion-type thermocouple. In this manner the rate of heat loss resulting with different refractory design could be developed. The ratio of exterior surface to weight of metal was taken into consideration in comparing the experimental results with what might be expected for a full-sized unit, and observations were also made on type and degree of slag accretion. It was not possible to get as much information on this latter point as desirable, but all evidence showed that the problem would be control of slag build-up rather than attack oil refractories.

Jan 1, 1938

By H. M. Faust

THERE are a number of different types of power plants. Some use coal to generate steam, others use oil or gas either in the form of steam or internal combustion equipment, while still others avail themselves of water power as a source of energy. A general comparison of the relative power production with different sources of energy in the United States, for several different years is set up in Table 1. This table shows that coal was used to generate 85.6 per cent of the total heat power requirements of 1909, and only 59.2 per cent of the 1930 requirements. The increasing proportion of modern heat energy generated by the use of fuel other than coal is apparent. If coal is to maintain its importance as a source of heat energy, the necessity for its improved perform-ance, in which preparation plays an -important part, cannot be stressed too strongly.

Jan 1, 1933

By G. L. Oldright

THE upper limit of richness of concentrates that can be smelted by means of the blast furnace without added diluents is fixed by the opera-tion of sintering. A sinter feed with normal gangue constituents, con-taining more than about 50 per cent of lead, tends to fuse; as a result, air does not come sufficiently into contact with the sulphides at roasting temperatures, and sulphur elimination is poor. Since most lead con-centrates now contain 55 to 80 per cent lead, it is necessary to add diluents to lower the grade of such sinter feed to about 50 per cent or less. This not only entails the expense of providing barren diluents when adequate diluents containing precious metals are not available but also appreciably lowers the capacity of the blast furnace to produce lead and increases slag losses. Attempts to desulphurize rich lead concentrates by methods other than sintering have not proved successful. Flash roasting, for example, converts much of the lead sulphide to lead sulphate rather than to oxide. However, this suggested the possibility that deliberate flash roasting of the concentrates to sulphate, followed by sinter roasting of the resulting product, might prove promising, particularly inasmuch as the elimination of sulphur from lead sulphate requires heat alone and not contact with atmospheric oxygen. The sintering of lead sulphate products has additional interest because important amounts of such products are now treated by lead smelters. Considerable quantities of lead sulphate are present in rich lead flue dusts and other by-products; lead-chamber sulphuric acid plants and other

Jan 1, 1940

By J. O. Lewis

Oil wells usually reach their maximum daily output shortly after they are completed. From that time they decline in-production, the rapidity of decline depending on the output of the wells and on other' factors governing their productivity. The production curve of a well shows the mount of oil produced per unit of time for several consecutive periods; if the conditions affecting the rate of production are not changed by outside influences, the curve will be fairly regular, and, if projected, mill furnish useful knowledge as to the future production of the well. By the aid of this knowledge the value of a property may he judged, and proper depletion and depreciation charges may be made on the books of the

Jan 2, 1918

By Stanley F. French, Bruno F. Koch

Although the amount of dust that will be actually recovered in the six main dust-control systems cannot be accurately stated until the tests mentioned previously are carried out, it is estimated that the average air entering the wet collectors will contain around 5 grains of dust particles per cubic foot. This means that the six systems handling a total of about 133,000 cu.ft. of air per minute will return about 68 1/2 tons of dust to the concentrator per day and since the copper in this dust will average around 2 per cent, the total recovery is approximately 1.37 tons of copper every 24 hours. This important copper recovery is not due entirely to the dust-control system since in a plant without control only the duct that is dispersed to the atmosphere represents a loss. A conservative estimate of the recovery of copper solely due to the dust control system would be about half of the total or approximately 0.70 tons of copper per day.

Jan 1, 1942

By Etienne A. Ritter

The Evergreen mine, located at Apex, in the northern part of Gilpin county, Colorado, has opened a very peculiar and interesting copper-deposit, in which both bornite and chalcopyrite occur as rock-minerals. The country-rocks are crystalline schists cut by dikes of granu-lite and of pegmatite. At the Evergreen property they have been cut by a dike of a uew kind of eruptive rock, to which I have given the name " Evergreenite." The rock is composed of quartz, alkali feldspars, orthoclase and albite (often interlocked as microperthite), with augite of the ægirine variety and long needles of enstatite and diallage. For reasons stated below, I believe the dike to be of Tertiary age. It is easily traced on the surface of the ground, from a point in the bottom of Pine creek, about a mile below Apex, to the top of Nevada hill, 1,500 ft. beyond and 600 ft. above it. (See Fig. 1.) It varies from 3 to 12 ft. in width, and is bounded on both sides by contact-zones about 60 ft. wide, in which the crystalline schists have been changed into pseudo-quartzites or pseudo-gneisees, according to the injection of an excess of quartz or of feldspars through the special layer of the schists. The most interesting feature is the presence of the pyroxenes, which are always found, though in very variable proportions from place to place, in the layers of these metamorphosed crystalline schists. The dike has torn from its walls a large number of fragments of the wall-rock. It must have been in a viscous state when that happened, because these fragments of the wall-rock do not show any sign of resorption or of assimilation by the magma. In places they are so distinct and so numerous that the rock looks to the naked eye like a pseudo-breccia, of which, never-

Jan 1, 1908

By C. D. Thompson, D. C. Violetta, C. A. Czako

The mechanics of the continuous sintering process are briefly reviewed and the application of this process for the beneficiation of principal minerals used in making cement is shown. Pilot plant tests using pyrobeneficiation techniques were conducted with mixtures of limestone and shale in various ratios. Results are illustrated and show the percentage removal of carbon, carbonates, sulfur, alkalies, and volatiles as a function of the limestone-shale ratio. Tests with varying quantities of solid fwls, added to mixtures containing limestone and shale in a 4 to 1 ratio, were made to attain optimum elimination of the volatile constituents. Experimental results show that 90 pct of these constituents were removed during the calcination sintem'ng process. The advantages of using the beneficiated material for making cement are discussed with regard to prepam'ng, handling, and clinkering operations. A sintering process for treating raw materials or kiln waste products which contain high amounts of alkaline materials is described. Tests were performed with a high alkaline waste dust mixed in a 1 to 1 ratio with raw cement meal. The data from these tests and others using different halides for aiding alkali removal are evaluated by the alkali content of the cement clinker. Test results showed that the Dwight-Lloyd process could be applied with facility in beneficiating raw materials for cement making. Substantial quantities of deleterious volutile constituents were removed by calcining and sintering techniques. The continuous sintering process has been applied for a number of years as a means of beneficiating minerals for subsequent conversion to merchantable products. The process was developed and first used for nonferrous metallurgical applicatfons. However, it has risen to prominence for ferrous metallurgical applications where last year in the U.S. and Canada nearly 40 million tons of iron ore were treated by grate firing processes. Through the years of process development many investigators have realized the versatility of the sintering process and have directed experiments toward the use of it for applications with nonmetallic minerals. These have included calcining limestone, carbonizing coal, expanding shale, and burning cement raw meal. Today commercial sintering plants produce cement clinker from mixtures of limestone and shale, lightweight aggregate from shale or clay, and calcined products from phosphate shale. The mechanics of the downdraft sintering process have been presented by many authors. In general practice the materials to be agglomated are mixed as moistened fines with a solid fuel and this mixture is spread uniformly on the grates of the sintering machine. The charge is then momentarily directed under an ignition furnace. After ignition a continuous downdraft of air promotes combustion of the fuel and through heat transfer particles become partially fused into a coherent mass. This is cooled from continued draft induced after combustion. Many investigators have shown that distinct zones are formed during the process of sintering iron ores. At the midway point of the sintering process these are prominent and are, respectively, from the top of the bed to the bottom, comprised of a cooling zone of sintered material, a combustion zone of sinter formation, a calcination zone, a drying zone, and a zone of unreacted materials. Completion of sintering occurs near the discharge end of the machine where the firing zone approaches either the grates or grate dressing material called hearth layer. Here the peak draft temperature usually can be noted in the windboxes. The zonal pattern has been illustrated with the use of graphs which show thermal gradients as they progress through the bed of materials during sintering. Fig. 1 shows, in simplified form, thermal gradients existing when clinkering cement on a sintering machine. The thermal gradients illustrated are for periods of initiation, midway and completion of the clinkering process. The occurrence of these zones has importance for the beneficiation of cement raw materials. A research program was performed at the Dwight-

Jan 1, 1961

By Nicholas J. Grant, Yoichi Ishida, Arthur W. Mullendore

An inert particle -marker technique was developed to provide a direct measurement of grain boundary sliding during creep in tile interior of aluminum specimens. Groin boundary sliding in the interior as measured by this technique was found to be nearly the same or slightly lower than that measured on the surface. These data disagree with those obtained by the grain-counting technique developed by W. A. Rachinger. In tests where both techniques were used, the grain-counting technique gave large and variable values of grain boundary sliding. It is shown that the grain-counting technique gines erroneozcs results because of a preferred direction of grain growth during creep. A question which has long plagued those who study grain boundary creep is whether or not surface measurements yield a true representation of the deformation in the interior of a specimen. The first attempt to measure grain boundary sliding in the interior of a creep specimen was made by Rachinger.1 His technique is based on the measurement of average grain diameters, both parallel and perpendicular to the tension axis, followed by a calculation of the grain elongation from these measurements. The difference between total elongation, Et, and the calculated grain elongation, Eg, is considered to be the result of grain boundary sliding, Egb. Surprisingly large values of Egb/ Et (90 pct) came out of creep tests of pure aluminum at temperatures above 250°C (480°F), utilizing the Rachinger technique. This value is very much larger than the values of 8 to 15 pct measured by numerous investigators on the surface of a specimen. Values obtained on the surface by Rachinger, however, were consistent with those measured by the displacement of reference scratches. Chaudhuri and Grant2 repeated the Rachinger method for A1-10 pct Zn, and found the same large values of Egb/Et inside the specimen. However, from purely geometrical considerations, grain boundaries cannot slide without grain deformation; therefore, they questioned the validity of Rachinger's grain-counting method. Several authors2,3 have suggested that grain boundary migration during high-temperature deforma- tion may tend to restore the equiaxed grain shape in order to minimize interfacial energy. Rachinger4 tested this hypothesis and found that it did not hold. Grains elongated by rapid extension retained their elongated shape during a subsequent slow creep test. It appears that some other factor was responsible for the abnormally high values of .Egb/El. McLean and Gifkins5 made a survey of the effect of grain size on the ratio Egb/ Et, and proposed that the high values were the consequence of a small grain size. They failed to explain the low value of Egb/Et which Rachinger observed on the surface of the small grain size specimens, and suggested that the surface effect on the value of Egb/Et does not always occur. Many of the disagreements arising from Rachinger' s work stem from the fact that there was only one method of estimating grain boundary sliding in the interior of a specimen, and that method was of an indirect nature. If a marker line of some sort could be introduced inside of the specimen, one could make measurements just as clearly as on the surface. In the present investigation, the technique utilizes a layer of finely dispersed oxide particles inside the specimen introduced by hot press-bonding of two pieces of aluminum. Rachinger attempted a similar technique but with the oxide distribution he obtained there was so much interference with grain boundary motion that quantitative measurements were not attempted. MATERIALS AND EXPERIMENTAL PROCEDURE A) Materials Preparation. Two pure aluminum rods (impurity content in percent: Si, 0.002; Cu, 0.004; Fe, 0.002; Mg, 0.000: Zn, 0.000; V. 0.001) 1 in. diameter by 2 in. high were jacketed end to end in a 4-in.-diam cylinder of commercial-purity aluminum, 4 in, high, which had a l-in.-diam hole. The l-in.-diam mating surfaces of the two pure aluminum rods had been electropolished initially. This interface provided the oxide-film internal -marker plane after the hot press-bonding process, see Fig. 2. The composite was annealed for 1 hr at 900 F and hot upset more than 50 pct reduction in height in one step. The resulting slab was then rolled to 1/2 in. thickness; the pure aluminum test material was cut out and annealed at 900°F for 1 hr and cold cross-rolled to 1/8 in. thickness. The sheet was machined into specimens with a 1/8-in.-square cross section and a 1/2-in. gage length. The following heat treatment was given the specimens: Specimen 5A series: annealed at 1000°F for 5 min for grain-size control and then cooled to 700°F and held for 15 hr for stabilization.

Jan 1, 1965