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By W. R. Purcell

An apparatus is described whereby capillary pressure curves for porous media may be determined by a technique that involves forcing mercury under pressure into the evacuated pores of solids. The data so obtained are compared with capillary pressure curves determined by the porous diaphragm method, and the advantages of the mercury injection method are stated. Based upon a simplified working hypothesis, an equation is derived to show the relationship of the permeability of a porous medium to its porosity and capillary pressure curve, and experimental data are presented to support its validity. A procedure is outlined whereby an estimate of the permeability of drill cuttings may be made with sufficient acuracy to meet most engineering requirements. INTRODUCTION The nature of capillary pressures and the role they play in reservoir behavior have been lucidly discussed by Lev-rett', Hassler, Brunner, and Deah12, and others. As a result of these publications the value of determining capillary pressure curves for cores has come to be generally recognized within the oil industry. While considerable attention has been directed toward the subject in an effort to provide a reliable method of estimating percentages of connate water, it has been recognized that capillary pressure data may prove of value in other equally important applications. This paper describes a method and procedure for determining capillary pressure curves for porous media wherein mercury is forced under pressure into the evacuated pores of the solids. The pressure-volume relationships ob- tained are reasonably similar to capillary pressure curves determined by the generally accepted porous diaphragm method. The advantages of the method lie in the rapidity with which the experimental data can be obtained and in the fact that small, irregularly shaped samples, e.g., drill cuttings, can be handled in the same manner as larger pieces of regular shape such as cores or permeability plugs. Based upon a simplified working hypothesis, a theoretical equation will be derived which relates the capillary pressure curve to the porosity and permeability of a porous solid, and experimental data will be presented to support its validity. This relationship aplied to capillary pressure data obtained for drill cuttings by the procedure described provides a means for predicting the permeability of drill cuttings. METHODS FOR DETERMINING CAPILLARY PRESSURES Several techniques have so far been employed in determining capillary pressure curves and these fall into two principal categories: (1) Liquid is removed from, or imbibed by, the core through the medium of a high displacement pressure porous diaphragm (2) Liquid is removed from the core which is subjected to high centrifugal forces in a centrifuge4,'. There are? however, certain limitations inherent in both methods. The greatest capillary pressure which can be observed by method (I), above, is determined by the maximum displacement pressure procurable in a permeable diaphragm which at the present time appears to be less than 100 psi. An even more serious limitation of the diaphragm method is imposed hy the fact that several days may be required to reach saturation equilibrium at a given pressure; hence, the time re- quired to obtain a well-defined curve may be measured in terms of weeks. Furthermore, to date, no suitable technique for handling relatively small, irregularly shaped pieces of rock, such as drill cuttings, has been reported and, therefore, measurements must be made, in general, on cores, or portions thereof. The centrifuge method offers the distinct advantage over the porous diaphragm method of arriving at saturation equilibrium in a relatively short time by virtue of the elimination of the transfer medium for the liquid. The calculation of capillary pressures from centrifuge speeds is somewhat tediousa, however, and the equipment required is fairly elaborate. While there exists the possibility that this method might be adaptable to the determination of the capillary pressures of cuttings, this particular ramification has not been investigated, as far as is known. In view of the limitations of the two principal methods for determining capillary pressures, the apparatus described in the following sections has been devised in order that difficulties previously encountered might be circumvented. MERCURY INJECTION METHOD FOR DETERMINING CAPILLARY PRESSURES Theory The methods described above for determining capillary pressures are characterized by the fact that one of the fluids present within the pore spaces of the solid is a liquid which "wets" the solid, i.e., the contact angle which the liquid forms against the solid is less than 90" as measured through that phase. For these "wetting" liquids the action of surface forces is such that the fluid spontaneously fills the voids within the solid. These forces likewise oppose the withdrawal of the fluid from the pores of the solid.

Jan 1, 1949

By W. R. Purcell

An apparatus is described whereby capillary pressure curves for porous media may be determined by a technique that involves forcing mercury under pressure into the evacuated pores of solids. The data so obtained are compared with capillary pressure curves determined by the porous diaphragm method, and the advantages of the mercury injection method are stated. Based upon a simplified working hypothesis, an equation is derived to show the relationship of the permeability of a porous medium to its porosity and capillary pressure curve, and experimental data are presented to support its validity. A procedure is outlined whereby an estimate of the permeability of drill cuttings may be made with sufficient acuracy to meet most engineering requirements. INTRODUCTION The nature of capillary pressures and the role they play in reservoir behavior have been lucidly discussed by Lev-rett', Hassler, Brunner, and Deah12, and others. As a result of these publications the value of determining capillary pressure curves for cores has come to be generally recognized within the oil industry. While considerable attention has been directed toward the subject in an effort to provide a reliable method of estimating percentages of connate water, it has been recognized that capillary pressure data may prove of value in other equally important applications. This paper describes a method and procedure for determining capillary pressure curves for porous media wherein mercury is forced under pressure into the evacuated pores of the solids. The pressure-volume relationships ob- tained are reasonably similar to capillary pressure curves determined by the generally accepted porous diaphragm method. The advantages of the method lie in the rapidity with which the experimental data can be obtained and in the fact that small, irregularly shaped samples, e.g., drill cuttings, can be handled in the same manner as larger pieces of regular shape such as cores or permeability plugs. Based upon a simplified working hypothesis, a theoretical equation will be derived which relates the capillary pressure curve to the porosity and permeability of a porous solid, and experimental data will be presented to support its validity. This relationship aplied to capillary pressure data obtained for drill cuttings by the procedure described provides a means for predicting the permeability of drill cuttings. METHODS FOR DETERMINING CAPILLARY PRESSURES Several techniques have so far been employed in determining capillary pressure curves and these fall into two principal categories: (1) Liquid is removed from, or imbibed by, the core through the medium of a high displacement pressure porous diaphragm (2) Liquid is removed from the core which is subjected to high centrifugal forces in a centrifuge4,'. There are? however, certain limitations inherent in both methods. The greatest capillary pressure which can be observed by method (I), above, is determined by the maximum displacement pressure procurable in a permeable diaphragm which at the present time appears to be less than 100 psi. An even more serious limitation of the diaphragm method is imposed hy the fact that several days may be required to reach saturation equilibrium at a given pressure; hence, the time re- quired to obtain a well-defined curve may be measured in terms of weeks. Furthermore, to date, no suitable technique for handling relatively small, irregularly shaped pieces of rock, such as drill cuttings, has been reported and, therefore, measurements must be made, in general, on cores, or portions thereof. The centrifuge method offers the distinct advantage over the porous diaphragm method of arriving at saturation equilibrium in a relatively short time by virtue of the elimination of the transfer medium for the liquid. The calculation of capillary pressures from centrifuge speeds is somewhat tediousa, however, and the equipment required is fairly elaborate. While there exists the possibility that this method might be adaptable to the determination of the capillary pressures of cuttings, this particular ramification has not been investigated, as far as is known. In view of the limitations of the two principal methods for determining capillary pressures, the apparatus described in the following sections has been devised in order that difficulties previously encountered might be circumvented. MERCURY INJECTION METHOD FOR DETERMINING CAPILLARY PRESSURES Theory The methods described above for determining capillary pressures are characterized by the fact that one of the fluids present within the pore spaces of the solid is a liquid which "wets" the solid, i.e., the contact angle which the liquid forms against the solid is less than 90" as measured through that phase. For these "wetting" liquids the action of surface forces is such that the fluid spontaneously fills the voids within the solid. These forces likewise oppose the withdrawal of the fluid from the pores of the solid.

Jan 1, 1949

The Carlin gold deposit is located in northeastern Nevada about thirty-five miles by road from the town of Elko. Following the staking of six square miles 'of ground, a drilling program outlined a fine ore body mineable by open pitting. The resulting mine turned out to be the largest open-pit gold operation in the world, until the Rosario Pueblo Viejo operation was started in 1975. Because of the high profitability forecast at the then $35 gold price, construction of a 2000 stpd mill was commenced on a crash program and was completed for Newmont Mining Corporation by Bechtel Corporation in ten months. Production was started in early 1965. The gold mineralization occurs in marine-type sediments, chiefly silt- stones and limey shales, and the ore characteristics make for a difficult materials-handling problem. At 5% to 6% moisture the ore is dusty during crushing, but even a light rain or snowfall virtually turns the material into a slurry. Crushing this sticky ore below 314 in. (19 mm) in the dry season and 1 in. (25.4 m) during the winter is extremely difficult and leads to problems with conveyors, chutes, and fine ore storage. The initial flowsheet for Carlin's crushing plant used a 5 ft by 22 ft (1.52 m by 6. 7 m) vibrating feeder -grizzly under the 60 -ton dump pocket for feeding the 42 in. by 48 in. (1067 mm by 1220 mm) single toggle jaw crusher and a 5 ½ ft (1.52 m) standard cone crusher in closed circuit with a 6 ft by 12 ft (1.83 m by 3.66 m) vibrating double - deck screen. Because continual packing of fines in the vibrating feeder pan would cause frequent plant shut-downs to remove the fines with jack hammers, the decision was made to replace the vibrating unit with an apron feeder and stationary grizzly ahead of the jaw crusher. A dribble belt was also installed under the apron feeder. This installation has greatly improved the feeding of the pit run ore to the .primary jaw crusher. Mining at Carlin is done by a 5 yd shovel and 7 ½ and 10 yd front-end loaders, and ore transport is by several sizes of trucks from 30 to 75 tons capacity. These pit haulage trucks dump onto stockpiles adjacent to the primary crusher. Ore is then fed to the dump hopper by front- end loaders only when the crushing plant is operating. This extra handling procedure is necessary because plant delays caused by problems with wet ore in the secondary crusher resulted in the ore setting up or packing in the dump pocket. Solidified material in the dump pocket would in turn delay truck haulage. The substitution of an

Jan 1, 1978

By A. Yoshikawa, T. Sugeno

To detenmine the origin of the sharp fatigue limit in many ferrous metals, S-N curvces were determined in push-pull fatigue at 18.6 kc per sec at room temperature and - 67°C for various kinds of iron. These differed in carbon and nitrogen content and grain size (25 and 2500 grains per sq mm). Sharp knees appeared in the S-N curves of fine-grained specimens with high interstitial content at both temperatures. In coarse-gruined specimens, knees were not sharp .regardless of the interstitial content and the testing temperature. It is concluded from these results that the controlling factov for the appeavance of the sharp fatigue limit is not strain aging but grain size. It has already been mentioned that iron and some iron alloys show fatigue curves characterized by a more or less sharp knee and a fatigue limit.' Explanations of the origin of this characteristic behavior of fatigue in iron appear to fall into two broad classes. One is concerned with interstitial impurities through the aging or locking effect and the other is based on intrinsic plastic properties of iron. Levy and sinclair2 and Lipsit and Horne3 have suggested that the fatigue limit observed generally in iron and steel is due to interstitial solute aging during the course of fatigue. On the other hand, Thompson and wadsworthl have suggested that the fatigue limit may be analogous to the sharp yield point, in the sense that alternating stresses above the fatigue limit are necessary to break down the dislocation locking. However, there are some experimental results which cast doubt on the general validity of these suppositions.4-8 Ferro and Montalenti' have recently suggested that the typical form of the fatigue curve of iron seems to come from an intrinsic plastic characteristic of the iron structure. This suggestion is based on the experimental result that pure iron containing an insufficient amount of interstitial solute to alldw appreciable strain-aging effects still showed a fatigue limit at room temperature. Although systematic investigations on the effect of grain size are scarce, it is thought that this effect is important in relation to the sharp fatigue limit. In fact, sensible differences were observed by Oates and Wilson4 in fatigue behaviors of a low-carbon steel depending on grain size. Ideally, the fatigue limit will be defined as the upper limit of stress amplitudes at which the life is infinite. This ideal fatigue limit can never be determined because of the limited time available for experiments, and moreover scattered data points often leave the construction of S-N curves somewhat arbitrary. And, it is usually stated that a material has a fatigue limit when its statistical S-N curve becomes apparently parallel to the N axis with a more or less sharp knee. The meaning of the fatigue limit and the sharp knee will be discussed in detail in relation to the construction of S-N curves. The origin of this sharp knee was investigated by determining S-N curves of iron for various interstitial contents, testing temperatures, and grain sizes. EXPERTMENTAL PROCEDURE The material as received was a commercial-grade low-carbon steel in the form of 4-mm-diameter rods with the following composition in weight percent: C, 0.09; Si, 0.017; Mn, 0.43; P, 0.006; S, 0.012; Cu, 0.11. Five different groups of specimens were tested. The grain sizes and interstitial contents in each group are given in Table I. The specimens of group C-02 were decarburized by annealing for 100 hr at 700°C, followed by an additional 100 hr at 850°C in wet hydrogen. Specimens of groups N-2 and N-9 nitrided in a mixed atmosphere of ammonia and hydrogen after an initial treatment identical to group C-02. The specimens of group C-9 were prepared in a manner similar to those of group C-02, except heat treatment was carried out in a vacuum. After polishing their surface with emery paper, the specimens of all groups were given a final anneal for 30 min at 930°C and air-cooled in an evacuated quartz tube. For group C*-9 this

Jan 1, 1965

By Benny J. Nelson

AS a part of the fundamental research program of Aluminum Research Laboratories, some data were obtained on the ternary system Mg-Al-Mn. As very little information on the magnesium corner of this diagram has heretofore been published, it seems desirable to make available the values found for the liquidus and solidus surfaces of this system. Procedure The settling procedure was used for the determination of the liquidus compositions. Metallo-graphic examination of quenched samples, and stress-rupture upon incipient melting, were used for the solidus determinations. The settling procedure has been described in a previous paper.' Briefly, this method involved saturating the alloy with manganese at a temperature substantially above that at which the sohbility was to be determined, then cooling the melt to the latter temperature, and holding it at that temperature for a substantial period of time. Samples for analysis .were carefully ladled from the upper portion of the melt at hourly intervals during the holding period. After the ladling of each sample, the melt was stirred to redistribute some of the manganese that had already settled, because it appeared that when the latter particles of manganese again settled, they aided in carrying down more of the manganese and thus hastened the attainment of equilibrium. The melts were prepared and held in a No. 8 Tercod crucible holding approximately 4 lb of metal. The manganese was added either in the form of a prealloyed ingot (Dow M) containing about 1.5 pct Mn or by the use of a flux (Dow 250) containing manganese chloride. In calculating the flux additions, it was assumed that the manganese introduced would be equal to 22 pct of the total weight of the flux. Temperatures were measured with an iron-constantan thermocouple enclosed in a seamless steel tube, the lower end of which was welded shut. This protection tube also served as a stirring rod. The samples ladled from the upper portions of the melts at the various intervals were analyzed for aluminum, manganese, and iron. When making the alloys which were to be used for the determination of the solidus, 2½ in. diam tilt mold ingots were cast, scalped to 2.0 in. in diam, and extruded into ? in. diam wire. The principal impurities in the melts for this investigation were iron and silicon; their total not exceeding 0.03 pct. Portions of the wire, approximately 2 in. in length, were enclosed in stainless steel capsules for protection from the atmosphere. Bundles of these capsules, with a dummy capsule containing an iron-constantan thermocouple, were heated inside a large steel block (acting as a heat reservoir) in a closed circulating-air type electric furnace. At ap- propriate times, the capsules were removed and quenched in water. The wires were examined metallographically to determine the temperature of initial melting. Short times at temperature were used at the beginning for wire specimens of all alloys to obtain quickly the approximate temperatures at which melting could be first observed. When approximate solidus temperatures had thus been determined, equilibrium heating was attempted. This equilibrium heating consisted of an 8 or 16 hr period at a temperature, about 50 °F below the lowest temperature at which melting occurred when short heating cycles were used, followed by further heating for 1 hr periods at consecutive 10" higher temperatures. The theory for the method of stress-rupture at incipient melting has been well covereda and its limitations are recognized. Thus, if the interfacial tensions are such that the first minute quantity of liquid is "bunched up" at the grain boundary junctions instead of spreading out along the grain boundaries,³ temperatures higher than the solidus are required before melting will be manifested by rupture of the specimen. This point will be elaborated later. Specimens of the wires with a reduced section (approximately 1/16 in. diam) were suspended vertically in a tubular furnace. The setup used is shown in Fig. 1. The clamp holding the specimen was made from alumel thermocouple wire and the thermocouple was thus completed across the specimen by attaching a chrome1 wire to its lower end. Temperatures were read from a Speedomax recorder used in conjunction with a calibrated thermocouple. The small weight attached to the specimen and a vibrator attached to the furnace tube, to aid in distributing the molten constituent along the grain boundaries, were used to bring about rupture at a temperature closely approximating the solidus. The specimens were heated at a rate of about 5°C per min. The rupture of the specimens was indicated both by sound and by the action of the recorder. An argon atmosphere containing a small amount of SO² was used for protection of the specimen. The assembly was taken out of the furnace immediately following rupture and the specimen removed. Some of the broken specimens were examined metallographically and will be referred to later. Results and Discussion Fig. 2 shows a set of typical time-composition curves for liquid samples of the Mg-Al-Mn alloys used for the settling tests. The data as presented

Jan 1, 1952

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 T. Egleston

AT the Dover meeting of the Institute, Mr. F. A. Canfield showed some of the members a machine which he had invented for dressing mineralogical and geological specimens, which he has since modified and brought to such a high state of perfection, that after having used it for several months in preparing specimens for the cabinet of the

Jan 1, 1876

By T. Egleston

At the Dover meeting of the Institute, Mr. F. A. Canfield showed some of the members a machine which he had invented for dressing mineralogical and geological specimens, which he has since modified and brought to such a high state of perfection, that after having used it for several months in preparing specimens for the cabinet of the

By Edward B. Walker, Michel Grosmangin

The geological and economic conditions peculiar to the Greater Oficina area are presented to demonstrate the necessity of a low-cost, well-site method of distinguishing gas-bearing formations. The method of gas detection with the neutron log is briefly discussed and its limitations are explained. A new method is described which consists in running a second neutron log with a larger source-to-detector spacing. Field data indicate that under favorable conditions the larger spacing response is proportionately more influenced by the virgin gas zone than is the shorter spacing response. One important condition is that the gas sands be invaded, with a diameter of invasion equal to about two to three times the hole diameter. The calibration of the longer spacing log is made so that the two logs read the same deflection in shale and in a known water or oil sand. Under such conditions, gas is indicated by a positive separation, i.e., the curve for the longer device is displaced to the right of the curve for the shorter device. Because of the non-linearity of the long spacing response, low porosity formations also show positive separations. In sands with large porosity variations, the gas sands can no longer he located visually. They can be detected on a plot of shorter spacing vs longer spac-ing deflections. INTRODUCTION In the Greater Oficina area of Eastern Venezuela, the rapid and accurate detection of gas from well logs is of primary importance because of a combination of economic, geologic, and operational conditions. Briefly, these conditions are: economic—there is no market for gas at the present time; geologic—a single well may contain as many as 30 or more oil or gas sands for which intervals -to be tested must be selected; opera-tional—first, once opened to the casing through perforations, gas sands are extremely difficult and expensive to squeeze off, and second, gas detection must be rapid because the geologist must decide immediately, at the well, which sand to perforate. During the early period of exploitation in Greater Ofi-cina, when clay base muds were used, sidewall samples, together with electric logs, gave fairly good distinction between oil and gas sands. When exploitation became concentrated on deep fields of poorer sidewall sample recovery, and after the advent of oil emulsion muds, now the standard drilling fluid in Greater Oficina, the regular neutron log became the most reliable indicator of gas. In 1953, R. Norelius devised the dual-spacing neutron technique for gas detection. The dual-spacing neutron log has proved to be highly successful in detecting gas and has been adopted as a regular survey by all of the oil companies of the area. Several hundred dual-spacing neutron logs have been run in Eastern Venezuela and several tests per well are available for positive evaluation of the logs. The findings outlined below are based upon this extensive field experience. GEOLOGICAL CONDITIONS OF THE GREATER OFICINA AREA The Greater Oficina area lies on the south flank of the Eastern Venezuela Basin (Fig. 1). Nearly all accumulations of oil and gas in the area are trapped, in whole or in part, against normal faults. All known oil and gas reservoirs in Greater Oficina occur in the Ofi-cina formation (Miocene-Oligocene) or in the "U" sands. The U sands are the lithologic equivalent of the Merecure group (Otigocene-Eocene), which contains oil in many fields north of Greater Oficina. Most of the petroleum produced in Eastern Venezuela is from the Oficina formation.

Jan 1, 1958

By James M. Schopf

Coal petrology is the study of the lithologic composition and texture of coal and includes megascopic as well as microscopic differentiation. Coal petrography is a quantitative study, principally (but not exclusively) microscopical in nature. The distinction between coal petrologic and coal petrographic studies usually is not important, but it is important to recognize that these studies differ materially from other types of petrology that deal primarily with minerals. The petrologic entities of coal are less clearly distinguished than most minerals and the basis of distinction is not always clearly expressed. The relation of coal petrology to geologic, mining, and technologic problems is most evident when results of coal petrologic studies can be stated quantitatively. The chemical and physical composition of coal and the determination of its quality and properties are continuing problems. The source of these problems lies in the heterogeneity of coal and in its almost complete insolubility in ordinary solvents at normal temperatures.

Jun 1, 1956

By H. C. Ray

ABOUT the beginning of 1930, coal preparation had reached the stage where the cleaning of coal by liquid or air had become the order of the day. Since that time many new preparation plants have been installed in spite of the years of depression in the coal industry, and this is indicative of a trend wherein the coal producer found it expedient to manufacture a cleaner product in order to compete with other fuels. It was also about 1930 that, because of the difficulties encountered with fine coal in cleaning plants, dust collectors came into use. Both cleaning plants and dust collectors, therefore, were much discussed at the engineering meetings of the early 1930's. During these meetings the many advantages to be gained through the use of dust- collecting systems were pointed out by Hebley,1 Appleyard2 and others. The great possibilities of new markets for this product were emphasized and discussed at the same time; however, the disposal of the collected dust remained a problem. Since the purpose of dust collecting is to improve the preparation and, consequently, the salability of the coal, it seems illogical to return the collected dust to any of the coal being prepared for market use, as is done in preparation plants that include dust-collecting systems. The logical thing is to dispose of the dust in some useful and practical manner outside of the tipple. As a practical matter, this can be done in one or both of two ways; either by consuming the dust at the mine's own power plant or by marketing the dust direct to the consumer. The latter method not only offers the greatest opportunities, but is the most important, because of inequalities that may exist between the quantity of dust collected and the consuming capacity of the mine's power plant. In considering the more important marketing possibilities, we are confronted immediately with the problems connected with the handling and transportation of so fine a material. It is this problem, rather than the problem of finding new markets, that has been responsible for the lack of progress in the matter of dust disposal. It is the purpose of this paper to point out again some of the potential market out- lets, and also to describe an existing system of handling and transporting coal dust. To the best of the writer's knowledge, this is the first and only operation in this country that has handled fine-mesh coal in bulk so-ton lots direct to the consumer. POTENTIAL MARKETS FOR FINE- MESH COAL DUST In general, the potential market outlets would include any operation of which the pulverization of coal is a necessary part. To be more specific, a few of the better known operations of this type must include: colloidal-fuel plants, briquetting plants, “sea coal” distributing plants, water-purification plants and obviously, pow-

Jan 1, 1944

By R. W. Heins, N. Street

An investigation was made of the Rehbinder-Kuznetsov pendulum as an instrument to aid in the study of rock drillability and of the effect of surface active agents on rock drillability. The "critical weight", i.e., the pendulum weight at greatest sensitivity, was determined for several solids and it was shown that a change in surface environment changed the maximum value of the apparent hardness but not the critical weight, and the critical weight increased with increase of hardness of the solid used. Using silver halides as the solid material, and solutions of either silver nitrate or the appropriate alkali halide, it was shown that there is a hardness maximum at the zero point of charge of the particular silver halide. INTRODUCTION The development of relative hardness measurement by the method of damped oscillations, or what has been called the pendulum sclerometer, is due largely to the Russian workers P. A. Rehbinder and V. D. Kuznetsov and their co-workers.1,2 The apparent simplicity of the method has led to its use in a number of fields, particularly those where relative hardness has to be determined on a brittle solid. As will be shown, the simplicity of the method belies its complexities. THEORY OF THE PENDULUM SCLEROMETER The operation of the pendulum is quite simple. Make a sharp point such as a diamond, hardened steel or tungsten carbide, as the fulcrum of a pendulum, with the center of gravity of the system below the point of support. The attenuation of this pendulum is a function only of air friction, provided no fragmentation, breakage or other work is performed by the point. However, when the solid surface breaks or disintegrates under the point, and the latter penetrates the solid, part of the energy of oscillation is absorbed in the work of creating new surface, and the rate of attenuation increases. In the case of brittle solids, the point of the pendulum produces fragmentary particles, whereas the point produces plastic deformation in a plastic solid; but in both cases damping occurs. This pendulum damping is a function of the hardness or strength of the solid. Whereas a pendulum oscillating on a hard material attenuates primarily by air friction, in the case of a soft material, the points penetrate the surface of the solid, producing new surface, and the pendulum damps much faster. Thus the attenuation rate is a function of the hardness or strength of a material in both plastic and brittle substances. Russian workers initially used a single support for the pendulum, but this created many problems because of oscillation of the pendulum in more than one plane. A revised version used two points, or sometimes a prism as support, successfully confining oscillation to one plane. The version using two points was constructed and used throughout this investigation, making the recording of the attenuation as a function of time relatively easy. That both points should be in contact with the solid during the damping is implied. Rehbinder (c.f. Kuznetsov2) proposed that the hardness H as measured by this method could be expressed by a quantity which is inversely proportional to the relative initial rate of attenuation of amplitude. where H = hardness parameter (arbitrary units) a, = initial amplitude da/dt = rate of attenuation of amplitude with time. In the simplest case of damping with a constant logarithmic decrement, H can be regarded as a constant for the duration of the whole damped oscillation process. That is

Jan 1, 1966

By P. Greenfield, C. C. Smith, A. M. Taylor

The Mg-Zr alloy ZA and Mg-Mn alloy AM503(S) are shown to have a markedly improved resistance to creep deformation after suitable heat treatments. This improvement makes them suitable for certain stress-bearing fuel element components in nuclear reactors. The extent of strengthening is described and an explanation of the behavior of both materials is given, based on a combination of strain-aging and grain growth. The increase in operating temperatures of fuel element components in Calder Hall type nuclear reactors has necessitated the development of magnesium base alloys with a very high resistance to creep at temperatures up to 500°C. Such alloys are not required for fuel element cans, which require high-creep ductility rather than strength, but for can supporting and stabilizing components, which are needed to support the imposed loads without deforming more than about 1 pct in times of up to 40,000 hr. The amount and type of alloying addition made to magnesium for these parts is limited by the necessity of keeping the cross-section to thermal neutrons as low as possible. The alloys must also possess a high resistance to oxidation in CO2. Alloys which have been developed for this application include ZA, an alloy of magnesium with 0.5 to 0.7 pct Zr and AM503(S), an alloy of magnesium with 0.5 to 0.75 pct Mn. In the as-extruded condition these alloys are very weak and ductile in creep but it has been found that they can be strengthened to a significant extent by heat treatment. This paper describes the method of developing a high-creep resistance in ZA and AM503(S), the extent of the strengthening produced and discusses the probable mechanisms of strengthening. TEST MATERIALS Specimens were taken from typical casts of ZA and AM503(S) alloys extruded into 2 1/4-in.-diam bars, supplied by Magnesium Elektron Ltd. Typical analyses of the bars were as follows: The as-extruded mean grain diameter was 0.001 to 0.002 in. for the ZA alloy and 0.003 in. for the AM503(S) alloy. EXPERIMENTAL METHODS Extruded bars of ZA alloy, 2 1/4 in. in diameter and 9 in. long, were heat treated in electrical resistance furnaces in an atmosphere of flowing CO2 containing 50 to 300 ppm water, thereby reducing the extent of oxidation compared with that which would have occurred in air. Heat treatments were carried out at 600oc for times of 8, 24, 48, 72, and 96 hr and material was subsequently both furnace cooled and water quenched. In order to measure the effect of time of heat treatment, specimens were creep tested at 400°C and 336 psi for about 1000 hr. Subsequently, the behavior of material heat treated for 96 hr at 600°C and furnace cooled was tested at a variety of stresses from 200° to 500°C. Tests were also conducted at 200o and 400°C on material in the as-extruded condition for comparative purposes. With the AM503(S) alloy, only the effect of heat treatment at 565°C for 4 hr was examined. It has been shown1 that such a heat treatment produces marked strengthening in this alloy. Tests on this material were conducted at a variety of stresses at 200°, 300°, and 400oc with comparative tests on as-extruded material at 200o and 400°C. The creep tests were carried out on machines using dead-weight loading and direct micrometer strain measurements on specimens 5 in. long and 0.357 in. diameter. At temperatures of 400° C and below, the creep tests were conducted in air, but at higher temperatures an atmosphere of CO2 was used. Grain size measurements were made on ZA in the extruded and heat treated states and on each specimen after creep testing. This was done by a line count of a minimum of 20 grains in two or three random fields in the longitudinal and transverse directions. The same method was used for measuring the grain size of as-extruded AM503(S), but the grain size of the heat treated material was so large that this method could not be employed. For heat-treated AM503(S) the large grained characteristics (between 0.1 and 1 in.) were confirmed by the measurement of individual grains. In the case of the ZA alloy, specimens taken from various stages in the program were analysed for hydrogen by a combustion method. Material in various states was also analysed for the soluble and insoluble zirconium content by dissolving in dilute hydrochloric acid. This technique has been useda for the determination of amounts of zirconium present

Jan 1, 1962

By N. S. Wagner

The production of lightweight aggregates in Oregon is a new industry, and, like all new enterprises, it is suffering from growing pains characterized by numerous, small operations some of which flourish for a short time and then cease altogether. Normally all industrial mineral products are produced in a highly competitive atmosphere. At the present time this condition does not exist to a very marked degree in the state because as yet producers have not saturated the constantly expanding market. This paper has been prepared with the intention of outlining very briefly the current status of the various products now being used as lightweight aggregates in Oregon. The present picture will surely change, perhaps quite radically within even a short space of time.

Jan 1, 1949

By Samuel J. Sims

The Grace mine magnetite deposit, located 2 miles north of Morgantown in Berks County, Pennsylvania, was discovered in 1948 by an aerial magnetometer survey. It is situated on the southern border of the Triassic lowlands section of the Piedmont province. Cambrian sandstones, shales, and limestones overlie Precambrian crystalline rock and were folded and thrust-faulted during the late Paleozoic Appalachian revolution. Late Triassic continental sediments were deposited on the deformed basement rocks and were intruded by Late Triassic diabase dikes and sills before regional tilting and normal faulting occurred. The Grace mine magnetite ore is characteristic of the Cornwall type. The ore has replaced a Cambrian limestone lens isolated between Triassic diabase footwall and Triassic sedimentary rock hanging wall. The ore body is roughly tabular in shape, dips 20° to 30°NE and plunges about 20°N80°E. The ore is granular, fine- to medium-grained, typically consisting of unevenly distributed magnetite in a matrix of light green to white serpentine gangue. Magnetite is the major ore mineral, pyrite and chalcopyrite are common accessory minerals, and pyrrhotite occurs locally. Sphalerite, marcasite, galena, hematite, digenite, and goethite are uncommon. Serpentine, talc, and chlorite are the major gangue minerals; calcite and dolomite are common, and phlogopite, tremolite, and biotite are present locally. Apatite is a common accessory; sphene is rare. Calcium-magnesium silicates were formed first by contact metamorphism of impure limestone by the intruding diabase. Later, the silicates were altered hydrothermally to the serpentine- talc-chlorite assemblage now present. Magnetite, the first ore mineral, formed by replacing serpentine and was followed by pyritepyrrhotite and then by chalcopyrite-galenasphalerite. Marcasite, secondary pyrite, goethite, and hematite are secondary minerals resulting from alteration of pyrrhotite and magnetite. It is estimated that confining pressure was about 1500 bars and the temperature range was 500° to 675°C during ore formation.

Jan 1, 1968

By D. A. Koss, R. O. Gordon

Changes in the ultrasonic attenuation in steel specimens have been observed during tensile tests. Samples of AISI 1020, 1045, and 1095 steel quenched and tempered to a spheroidized condition have been used. Both attenuation and microstrain measurements fail to reveal preyield dislocation motion in the as-tempered specimens. Upon reapplication of the load to samples in the strain-aged condition there is a large preyield attenuation increase but no observable micvostrain up to 90 pct of the flow stress. These and other observed changes can be related to changes in the free disloca-tion density and the average dislocation segment length. The results show that the increase inflow stress in the strain-aged condition is caused by increased fric-tional stresses rather than by dislocation pinning. Strain aging is found to proceed through three distinct stages. The second of these follows the t2,3 law and is characterized by an activation energy of 20 kcal per mole. RECENT years have seen substantial progress in the understanding of the sharp yield-point phenomenon in metals; the influence of solute atom pinning of dislocations, of dislocation multiplication, and of the stress dependence of dislocation velocity on the stress-strain curve has been investigated. Evaluation of the relative importance of these factors in the various metals and alloys is not complete, however, because observation of the stress-strain curve alone is not sufficient to determine the yield mechanism. In the experimental study of the sharp yield point it would be desirable to be able to directly observe the dislocations in a bulk specimen. Ideally, the observations should be made during deformation because of the rapidity of recovery processes in lightly strained metals. While direct observation of dislocations under these conditions is not possible, certain physical properties sensitive to the dislocation structure can be observed while a test specimen is undergoing deformation. Of these properties, one of the most useful is the ultrasonic attenuation. The total observed attenuation, a, is due to a number of causes: acoustic diffraction, scattering by inhomogeneities in the structure, heat flow, magnetostriction, and dislocation damping. Satisfactory measurements of the absolute a are difficult to make because all of these factors cannot be evaluated in any given specimen, but changes in a due to changes in the dislocation contribution alone can be reliably observed by appropriate technique. Because dislocation damping is sensitive to small concentrations of long, free dislocation segments, observation of acoustic attenuation due to dislocations is particularly useful in the study of the early stages of plastic deformation. In the experiments to be described, acoustic-attenuation measurements have been made on steel samples as these were pulled through their yield in tension. While many details of dislocation-damping phenomena in the bee metals remain obscure, the main characteristics of this type of internal friction are established. At low strain amplitudes and at frequencies well below that of dislocation resonance (the conditions of these experiments) the dislocation contribution to a is given by1 where A is the density of freely oscillating dislocation segments, L is the average segment length, B is the damping constant for a moving dislocation, w is the frequency, O is an orientation factor, C is the dislocation line tension, and t is a numerical factor relating average segment length to the distribution of lengths. Because of its fourth-power dependence on L, a is highly sensitive to changes in dislocation free segment length such as might arise from unpinning, recovery, jog formation, or dislocation intersection. The above equation is not valid near the resonant frequency of dislocations, but the segment length in steel is believed to be much too short to cause over-damped resonance near 10 Mc; this will be discussed later. In the present experiments plastic-strain measurements with a sensitivity of 2 x 10-5 were also made during the early stages of loading in order to detect preyield strain. The general plan of the experiments is to observe

Jan 1, 1967

By B. Russell, J. R. Tuffley

The stability regions of the normal sulfate and the various basic sulfates of lead in 02-SO2 and PhS-SO2 gas atmospheres were calculated from available thermodynamic data over the temperature range 600o to 1200oC. Roasting experiments were carried out on samples of synthetic lead sulfide at various temperatures and for various roasting times. Compounds in the oxidized surface layers were identified by X-my techniques. The order in which the various reactions occurred was determined by considering the experimental results in conjunction with the thermodynamic calculations. The results of these investigations were applied to the sintering of lead sulfide concentrates, and the extent to which each of the various reactions occurred in a sinter bed was determined. PRODUCTS which may be formed during the roasting of PbS are PbS04, PbSO4. PbO, PbSO4 . 2PbO, PbSO4 . 4PbO, PbO, and Pb.1, 2 The formation of some sulfates has been studied by a number of investigators3-' whose experiments have mostly been confined to the temperature range between 500" and 850°C. Culver, Gray, and spooner3 were able to isolate the reactions which formed PbSO4 and PbSO4. PbO by carefully controlling the compositions of the roasting gases. The kinetics of these reactions were studied within the temperature range 673" to 807°C. Gardner4 and Merrick5 also studied the kinetics of oxidation of PbS. Gardner disregarded the existence of basic sulfates and, as a result, misinterpreted some of his experimental data. Merrick recognized that most of the products of oxidation were mixtures of basic sulfates, but was unable to identify the individual components. Hoschek6 oxidized PbS in air at temperatures up to 800°C. The products were analyzed after roasting had proceeded for some minutes, but no attempt was made to follow the reactions in the initial stages. Consequently, no roasting mechanism was derived. He also showed that PbSO4 and PbSO4 - 4PbO decomposed slowly in air at temperatures in the region of 800°C. The stability regions of sulfates in the temperature range 500" to 850°C have been only partially determined, while practically no information is available for higher temperatures. In the lead sintering process, PbS concentrates are roasted at temperatures within the range 1000o to 1200°C. In order to investigate sulfate formation, it is necessary to determine the effects of temperature and gas composition upon the various oxidation reactions and upon the regions of stability of the various lead sulfates. Kellogg and Basu2 introduced an equilibrium diagram similar to those in Figs. 1 to 3 which provides a convenient medium for represent-

Jan 1, 1964

By T. Sterry Hunt

Jan 1, 1884

By Arthur Clark, Terrill

THE Tri-State field is now believed to be the largest zinc district in the world. It has a potential production sufficient to supply the entire zinc demands of the country. It is estimated that a train 70 miles long would be required to haul the district's 1919 output of 60 per cent. zinc concentrates. For many years,, including 1917, Missouri surpassed Oklahoma in zinc production. In 1918, however, Oklahoma led by a wide margin and, in 1919, Missouri produced less than one-sixth of the total for the three states, when Kansas replaced Missouri in second place in the production. The district is now producing one-third of the zinc of the world and twice as much as ever before at the present price.

Jan 1, 1920

By Edward Steidle

NOTHING stands still. We go forward or backward. As a distinct group of educators, our immediate concern is with the preparation of young men and women for participation in the mineral industries on a professional basis. I am going to have the temerity to state emphatically that for a long time as a whole we have remained in a static position. We are now confronted with the choice of advancement or retrogression. We are still in a position to make a choice and our ultimate fate will depend upon the course of action we elect to follow. Wars always have been great catalysts and social and scientific advancements mature under military stimulus in a fraction of the time normally consumed. We are now in the midst of a conflict whose duration or final effects cannot be estimated. However, the record already demonstrates that this war as never before is a mineral war in which incentive, strategy, and outcome are directly related to the distribution and utilization of minerals. The inevitable result is a drain upon our resources now reflected in our record production and a growing public consciousness of the importance of minerals in the role of human affairs. It is evident that we must seek new mineral frontiers beyond the borders of the United States and take every other precaution to forestall a "have-not" position in the world.

Jan 1, 1943