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By E. S. Messer

A knowledge of the magnitude of the irreducible inter.;titial water in a porous medium is so important to petroleum engineering that its determination has become routine in core analyses. The method of determination, being a production problem, should encompass the basic requirements of simplicity in technique and calculations, with reproducible results obtainable in a short interval of time. The results of the evaluation tests outlined in this report indicate that the evaporation method for determining the irreducible water is a technique which meets the requirements. The procedure consists, as the name implies. of permitting the saturant in the pore spaces to evaporate until only an irreducible volume remains. The determination of this volume can be made either graphically or by a mathematical comparison of fluid flows; the time required for each determination being dependent on the fluid used. When fluids other than those having reservoir characteristics were used, a volume factor had to be calculated which was based on the relative volume of various liquids adsorbed on grain surfaces and retained in pores. This factor made possible the calculation of an irreducible water volume when more volatile fluids such as toluene and benzene were used as the saturants. Also presented is the theoretical discussion necessary for the calculation of the capillary pressure as determined from the evaporation curve. A comparison is made between the calculated values and those obtained by experimental means. INTRODUCTION In all geological formations there exists, in the pore spaces of the rock structure, water that is held in a state of equilibrium between capillary and hydrostatic forces. "Interstitial water" is the term given to this water and is defined as that water coexisting in the pore space with the oil prior to exploitation. The term ''connate water" has often been used synonymously with this term; however, this can be true only by a specific definition since, geologically, it means the water in place at the time the rock structure was formed. The quantity of the interstitial water is a variable factor in any formation, since it depends on the hydrostatic forces present in any multiple-phase system. These forces may become unbalanced by the introduction of an extraneous force such as the raising or lowering of the "water table" or the migration of oil into a water-filled formation. Any unbalanced force results in a change in the interstitial water. There exists, however, an irreducible interstitial water. for a particular sand, that is the fraction of the pore space occupied by water when the capillary pressure at the particular point in question is at an equilibrium with the hydrostatic head of the oil sand in the reservoir. For this discussion the term "irreducible water saturation" will be used in place of "irreducible interstitial water saturation" for the sake of brevity; however, they are understood to be identical. A great amount of work has been devoted to the theory and methods for studying the irreducible water saturation and its related capillary pressure. As a result of the publications of Leverett;' Hassler, Brunner and Deahl;2 Calhoun and Lewis;3 and others, the role of capillary pressure studies is being accepted by the industry as a tool for studying suhsurface phenomena. Many techniques have been developed and published for determining the capillary pressure and irreducible water. In general, these techniques may be grouped into three classifications. One of the first was the capillary pressure method described by Leverett1 and expanded by Bruce and Welge.4 The experimental results were compared with water saturation of cores obtained using oil-base mud. Thornton and Marshall compared the irreducible water saturation of core samples determined by the capillary pressure method and by salinity and reported good agreement between the two methods. The second classification for determining the irreducible water and capillary pressure may be referred to as the "centrifugal force method." The general technique is similar to the capillary pressure method except that the force driving the reservoir fluid from the sample is of a centrifugal nature. A complete description of this method was presented by J. J. . McCullough and F. W. Albaugh.6 A process, the reverse of the capillary pressure method, was presented by W. R. Purcell.7 Mercury under pressure is driven into the pores of the rock and the saturation of the core determined at each applied pressure. The resulting capillary pressure curve is used to evaluate the irreducible water saturation. The techniques mentioned are singular in their approach to the irreducible water saturation. In all cases. an external force was applied to the core. The forces employed in the evaporation method are the vapor pressure of the liquid causing evaporation, the kinetic diffusion forces. adsorptive forces and. to a lesser degree, the viscous forces resisting flow to the surface. The basic definition of irreducible water is that water held in a state of equilibrium between capillary and hydrostatic forces This water has been described by previous investigators as being held in the microcapillaries too small to support fluid flow. Actually, this fluid volume is made up of the water in the microcapillaries and as a film adhering to the surface of the crystals. All capillaries. therefore, possess some liquid as a film, the thickness of the film being dependent on the properties of the fluid and solid. A discussion of experiments with references pertaining to the measurement of this immobile layer next to the solid surface can be found in the text by J. J. Bikerman.8 Eversole and Lahr calculated the thickness of this layer to be in the order of 10 ' to 10' cm for aqueous solutions and glass. Between two quartz surfaces they found the thickness to be 2 x 10 cm. The work of Volkova, on the capillary movement of water and toluene in quartz grains, indicated the thickness of the Immobile layers to be near 10' cm. Since any measurement is an average value, it is easy to understand that an absolute value would depend on the roughness of the surfaces involved and the complexity of the system. A calculated effective pore radius of 2 x 10 cm is obtained at the, irreducible saturation of a porous media in a water-air system when a capillary pressure of 100 psi is applied. Since the separation of the sand grains is of the same approximate magnitude as the immobile layer.

Jan 1, 1951

By E. S. Messer

A knowledge of the magnitude of the irreducible inter.;titial water in a porous medium is so important to petroleum engineering that its determination has become routine in core analyses. The method of determination, being a production problem, should encompass the basic requirements of simplicity in technique and calculations, with reproducible results obtainable in a short interval of time. The results of the evaluation tests outlined in this report indicate that the evaporation method for determining the irreducible water is a technique which meets the requirements. The procedure consists, as the name implies. of permitting the saturant in the pore spaces to evaporate until only an irreducible volume remains. The determination of this volume can be made either graphically or by a mathematical comparison of fluid flows; the time required for each determination being dependent on the fluid used. When fluids other than those having reservoir characteristics were used, a volume factor had to be calculated which was based on the relative volume of various liquids adsorbed on grain surfaces and retained in pores. This factor made possible the calculation of an irreducible water volume when more volatile fluids such as toluene and benzene were used as the saturants. Also presented is the theoretical discussion necessary for the calculation of the capillary pressure as determined from the evaporation curve. A comparison is made between the calculated values and those obtained by experimental means. INTRODUCTION In all geological formations there exists, in the pore spaces of the rock structure, water that is held in a state of equilibrium between capillary and hydrostatic forces. "Interstitial water" is the term given to this water and is defined as that water coexisting in the pore space with the oil prior to exploitation. The term ''connate water" has often been used synonymously with this term; however, this can be true only by a specific definition since, geologically, it means the water in place at the time the rock structure was formed. The quantity of the interstitial water is a variable factor in any formation, since it depends on the hydrostatic forces present in any multiple-phase system. These forces may become unbalanced by the introduction of an extraneous force such as the raising or lowering of the "water table" or the migration of oil into a water-filled formation. Any unbalanced force results in a change in the interstitial water. There exists, however, an irreducible interstitial water. for a particular sand, that is the fraction of the pore space occupied by water when the capillary pressure at the particular point in question is at an equilibrium with the hydrostatic head of the oil sand in the reservoir. For this discussion the term "irreducible water saturation" will be used in place of "irreducible interstitial water saturation" for the sake of brevity; however, they are understood to be identical. A great amount of work has been devoted to the theory and methods for studying the irreducible water saturation and its related capillary pressure. As a result of the publications of Leverett;' Hassler, Brunner and Deahl;2 Calhoun and Lewis;3 and others, the role of capillary pressure studies is being accepted by the industry as a tool for studying suhsurface phenomena. Many techniques have been developed and published for determining the capillary pressure and irreducible water. In general, these techniques may be grouped into three classifications. One of the first was the capillary pressure method described by Leverett1 and expanded by Bruce and Welge.4 The experimental results were compared with water saturation of cores obtained using oil-base mud. Thornton and Marshall compared the irreducible water saturation of core samples determined by the capillary pressure method and by salinity and reported good agreement between the two methods. The second classification for determining the irreducible water and capillary pressure may be referred to as the "centrifugal force method." The general technique is similar to the capillary pressure method except that the force driving the reservoir fluid from the sample is of a centrifugal nature. A complete description of this method was presented by J. J. . McCullough and F. W. Albaugh.6 A process, the reverse of the capillary pressure method, was presented by W. R. Purcell.7 Mercury under pressure is driven into the pores of the rock and the saturation of the core determined at each applied pressure. The resulting capillary pressure curve is used to evaluate the irreducible water saturation. The techniques mentioned are singular in their approach to the irreducible water saturation. In all cases. an external force was applied to the core. The forces employed in the evaporation method are the vapor pressure of the liquid causing evaporation, the kinetic diffusion forces. adsorptive forces and. to a lesser degree, the viscous forces resisting flow to the surface. The basic definition of irreducible water is that water held in a state of equilibrium between capillary and hydrostatic forces This water has been described by previous investigators as being held in the microcapillaries too small to support fluid flow. Actually, this fluid volume is made up of the water in the microcapillaries and as a film adhering to the surface of the crystals. All capillaries. therefore, possess some liquid as a film, the thickness of the film being dependent on the properties of the fluid and solid. A discussion of experiments with references pertaining to the measurement of this immobile layer next to the solid surface can be found in the text by J. J. Bikerman.8 Eversole and Lahr calculated the thickness of this layer to be in the order of 10 ' to 10' cm for aqueous solutions and glass. Between two quartz surfaces they found the thickness to be 2 x 10 cm. The work of Volkova, on the capillary movement of water and toluene in quartz grains, indicated the thickness of the Immobile layers to be near 10' cm. Since any measurement is an average value, it is easy to understand that an absolute value would depend on the roughness of the surfaces involved and the complexity of the system. A calculated effective pore radius of 2 x 10 cm is obtained at the, irreducible saturation of a porous media in a water-air system when a capillary pressure of 100 psi is applied. Since the separation of the sand grains is of the same approximate magnitude as the immobile layer.

Jan 1, 1951

By T. A. Rickard

From time immemorial the fissure-vein has been held the simplest type of ore-deposit. The prominence given to it by Cotta and his disciples, from their study of the mines of the Erzgebirge, is impressed upon technical literature; and, in consequence, the ores which carry the valuable metals have been supposed to occur mainly in fissures, cleaving the rocks in diverse directions, and the noblest type of vein has been deemed that which cut across the country independent of its structure, whether evidenced as bedding, foliation or cleavage, and which was identified with rents produced in the rocky crust of the earth. As so conceived, the vein was a fissure filled with ore, extending through the country for a varying distance, and continued downward to a depth more or less proportionate to its longitudinal extent. The vein-material was bounded by an encasement of rock, and those immediate surfaces which limited it on either aide were called " walls." These primary conceptions have become modified by the experience of modern mining in widely separated regions. The study of lode-formations has led to the recognition of notable departures from the supposed normal structure of the veins of Saxony and Cornwall, the two classic homes of early economic geology. Typically the walls of a vein are conceived as parallel rockplanes enclosing the ore; the upper one being called the " hanging-," and the lower the "foot-wall."* Walls are rarely alike. Even where a vein traverses a homogeneons formation, such as a massive crystalline rock, it is usually found that the surface which bounds it underneath

Jan 1, 1897

By R. B. Rosene, G. L. Foster, A. R. Hendrickson

he properties of some of the common fracturing oils, such as sand-falling rate, fluid loss and viscasity, are a function of the three major constituents of the oil. These are: asphaltic material, parafin waxes and a base oil. The base oil can be either high or low viscosity. Asphaltic material increases viscosity by thickening the oil, decreasing the rate of fall of sand through the oil. at temperatures up to 200" F. When large arnorrnts of parafin wax are present, much of the wax i.s not dissolved, but is present in the form of rnicroscopic crystals. 7'his, of course is limited to temperatures below the melting points of waxe.s. As a result, parafin waxes clo not function primarily as thickener.7, but rother as bullting materials. The functiori of wax, without asphaltic material, in a low viscosity base oil is uniquely unlike that of wax with asphalt coexistent in the oil. The resulting difierence in wax crystal size governs the sand-falling rate to a large extent. An ideal type of fracturing oil is one containing neither asphalt nor waxes. In such cases, the viscosity and resulting low sand-falling rate are apparently due to soluble resin- ous hydrocarbons, which are compatible with formation oils. INTRODUCTION Since the introduction of hydraulic fracturing as a method of stimulating production from oil and gas wells, a variety of fluids have been employed to open the fractures and carry the propping agent. Such fluids include gels, emulsions, and oils. In the latter category, the use of refined oils has increased tremendously, and it is probably safe to assume that such oils represent more than one-half of the total fluid used in fracturing. The general acceptance of refined oils for fracturing can be accounted for on the basis of their relatively low cost and general applicability. To minimize transportation costs, such refined oils are generally obtained within the local areas of operation. As a result there are several kinds of oil used in different areas, with a wide variation in the basic composition. These types may vary from a fair grade of lubricating stock to a highly viscous cut-back asphalt. or road oil. Originally, little attention was paid to the composition of the oils used for fracturing, and any oil which would carry sand was considered satisfactory. Recently, however, service companies and well operators have become more concerned with the type of oils used for fracturing. With this in mind, the present work was undertaken to evaluate and compare many widely used fracturing oils to determine which constituents were most desirable for fracturing purposes. Some of the important properties of fracturing fluids are sand-falling rate, viscosity, and fluid loss. Other properties, that are actually of no less importance, include flash point, pour point, emulsifying tendencies with formation brines, and compatability with the formation oils. This discussion has been limited, however, to the first mentioned properties in order to give some idea of the general composition of the refined oils, how they function, and why. PROPERTIES OF FRACTURING OILS The properties of fracturing oils are a function of the three major constituents of the oil. These may be designated as: (1) asphaltic material, (2) paraffin waxes and (3) a base oil, which may be of either high or low viscosity. The asphaltic material clas-

Jan 1, 1956

By D. N. Seidman

In the course of a study of the electronic and thermodynamic properties of Pb-Se alloys it was found necessary to have an accurate knowledge of the phase diagram. However, the literature is in disagreement as to whether or not a monotectic reaction occurs in the lead rich portion of the phase diagram. Pelabonl reported only a two-phase region consisting of lead-rich liquid and solid PbSe extending from almost pure lead to the compound PbSe, and gave the melting point of PbSe as 1065°C. The data of Friedrich and Leroux2 are in general agreement with this type of diagram, with the melting point of the compound being 1088°C. However, Nozato and Igaki by inverse rate thermal analysis observed a monotectic reaction isotherm exlacing at 860°C with a monotectic composition of 20.5 at. pct Se. The miscibility gap in the liquid state extends from 7.5 to 20.5 at. pct Se. Hansen and Anderko4 accepted Nozato and Igaki's phase diagram in the region of the lead-rich monotectic. To reinvestigate this portion of the phase diagram, both thermal analysis and metallographic examination of various compositions were performed. The thermal analysis apparatus was constructed according to the specifications of the National Bureau of Standards. A t/t-l pct Rh thermocouple was calibrated against the melting point of copper (NBS), zinc (NBS), and antimony (A. D. Mackay), the emf being measured with a Rubicon Type B potentiometer sensitive to lpv. The absolute accuracy of the thermal analysis obtainable with this system is ± 0.5oC. Starting materials were semiconductor grade lead and selenium purchased from the American Smelting and Refining Co. Both elements were 99.999 pct pure with only trace impurities detected upon spectroscopic examination. One hundred galloys were sealed in quartz crucibles with a central thermocouple well under a vacuum of less than 1 p. This procedure prevented any composition change due to vaporization during the run. Cooling curves were obtained on the alloys listed in Table I. Data was taken by the direct method at cooling rates ranging between 1/2 to 2°C per min. The alloys were heated well above the liquidus and shaken vigorously to insure homogeneity. No evidence of an arrest indicative of the monotectic reaction was observed, and the two-phase region reported by Pelabonl and Friedrich and Leroux? was confirmed in general, although our data give higher liquidus temperatures than Friedrich and Leroux. The melting point of stoichiomet-ric PbSe determined for two different samples was 1080.7 0.5oC. The results of this investigation are compared with Nozato and Igaki's data in Fig. 1. To Complement the thermal analysis data, an 86 at. pct Pb specimen was examined microscopically. This composition was in the center of the miscibility gap reported by Nozato and Igaki.3 The alloy was heated to 1000°C, held for 1/2 hr, and water quenched. The specimen was polished using standard metallographic techniques for lead. The alloy was etched with an acetic-nitric acid etchant for 10 min at 45°C. Microscopic examination did not indicate the existence of two separate layers or solidified droplets imbedded in a matrix, as would be expected if a miscibility gap were present. The mi-crostructure shown in Fig. 2 consists of uniformly dispersed, dendritic PbSe in a lead-rich matrix.

Jan 1, 1962

By Henry J. Joesting

During the past year and a half, the Territorial Department of Mines in Alaska has conducted a modest experimental program for the purpose of determining the extent to which magnetic and resistivity methods can be used in interior Alaska in connection with prospecting, mining and geological studies. Since little information is available concerning previous work,l,2 and since conditions differ considerably from those in most other regions, it was considered advisable to make a general study of the possibilities and limitations of the two methods, rather than a detailed study of any single problem. Problems One of the most serious handicaps to prospecting and geological study in interior Alaska, especially in the mature regions, is a cover of unconsolidated deposits ranging in thickness from a few feet to several hundred feet. These deposits, some of which are permanently frozen, consist of silt with varying proportions of vegetation and windblown material in the valleys and of residual deposits on the hills.3'4 The problems treated here are caused by the existence of this overburden: I. Location of buried placers. 2. Determination of depth and areal distribution of permanently frozen and of thawed unconsolidated deposits. 3. Location of water-bearing beds under unconsolidated deposits. Instruments and Methods Magnetic and direct-current resistivity methods were used because they are relatively simple, rapid and inexpensive and because generally they are well suited to the study of the problems indicated. The instruments used were a vertical Schmidt-type magnetometer and a direct-current resistivity instrument similar to those used by the Geophysical Branch of the U. S. Geological Survey. For placer surveys with the magnetometer, a sensitivity of about 25 gammas per scale division was found suitable. For resistivity studies of frozen and thawed overburden and of underground water, the Lee partitioning method6 was found to be most generally suitable. In the Lee method a central potential electrode is placed midway between the two potential electrodes of the Wenner four-electrode configuration.7 Nonpolarizable electrodes were made from unglazed porcelain pots about 10 cm. high and 5 cm. in diameter. In order to retard evaporation of the electrolyte the sides of the pots were glazed, inside and out, with clear Duco lacquer. For resistivity work in cold weather, a nonfreezing electrolyte consisting of equal parts of ethylene glycol and a saturated water solution of copper sulphate proved satisfactory. Stainless steel rods of 3/4-in. diameter made excellent current electrodes because their bright finish enabled good ground contacts to be made.

Jan 1, 1946

By Henry J. Joesting

During the past year and a half, the Territorial Department of Mines in Alaska has conducted a modest experimental program for the purpose of determining the extent to which magnetic and resistivity methods can be used in interior Alaska in connection with prospecting, mining and geological studies. Since little information is available concerning previous work,l,2 and since conditions differ considerably from those in most other regions, it was considered advisable to make a general study of the possibilities and limitations of the two methods, rather than a detailed study of any single problem. Problems One of the most serious handicaps to prospecting and geological study in interior Alaska, especially in the mature regions, is a cover of unconsolidated deposits ranging in thickness from a few feet to several hundred feet. These deposits, some of which are permanently frozen, consist of silt with varying proportions of vegetation and windblown material in the valleys and of residual deposits on the hills.3'4 The problems treated here are caused by the existence of this overburden: I. Location of buried placers. 2. Determination of depth and areal distribution of permanently frozen and of thawed unconsolidated deposits. 3. Location of water-bearing beds under unconsolidated deposits. Instruments and Methods Magnetic and direct-current resistivity methods were used because they are relatively simple, rapid and inexpensive and because generally they are well suited to the study of the problems indicated. The instruments used were a vertical Schmidt-type magnetometer and a direct-current resistivity instrument similar to those used by the Geophysical Branch of the U. S. Geological Survey. For placer surveys with the magnetometer, a sensitivity of about 25 gammas per scale division was found suitable. For resistivity studies of frozen and thawed overburden and of underground water, the Lee partitioning method6 was found to be most generally suitable. In the Lee method a central potential electrode is placed midway between the two potential electrodes of the Wenner four-electrode configuration.7 Nonpolarizable electrodes were made from unglazed porcelain pots about 10 cm. high and 5 cm. in diameter. In order to retard evaporation of the electrolyte the sides of the pots were glazed, inside and out, with clear Duco lacquer. For resistivity work in cold weather, a nonfreezing electrolyte consisting of equal parts of ethylene glycol and a saturated water solution of copper sulphate proved satisfactory. Stainless steel rods of 3/4-in. diameter made excellent current electrodes because their bright finish enabled good ground contacts to be made.

Jan 1, 1946

By N. E. Rogen, N. J. Grant

WHILE direct measurements of the growth of precipitate particles during aging is of fundamental value, few such measurements have been made. Direct measurements by means of optical or electron-microscopy and X-ray techniques are preferred, however, many of the aging studies have been based on indirect methods such as electrical resistivity and hardness. Because of the minute size of most precipitate particles (less than 1000A) the light microscope is of limited use while electron microscopy is subject to slowness, etching problems and consequent resolution problems. It is fortunate that alloys of the Nimonic type, based on Ni-Cr-Ti-Al, lend themselves to accurate and relatively easy particle size measurements. With proper balance of titanium and aluminum, the only aging precipitate is the gamma prime (r') Ni3,(Al, Ti)2 phase and this phase is the basis of the high-temperature strength of these allos.3-6 The Ni3(Al, Ti) phase is a face-centered-cubic, ordered structure with nickel atoms occupying the cube faces. Titanium atoms can replace three out of every five aluminum atoms and when substituting do so preferentially.2 Electron microscopy has shown that during aging of most of the commercial alloys of this type, precipitate particles are unusually uniform in size and distribution, and that the volume of (r') phase is large (20 pct).4,7 The aim of this investigation was to measure the growth of (y') phase during aging. In so doing, it was hoped that a clearer understanding of the aging process would be attained. X-ray line broadening was used as the measure of precipitate particle size. This technique was selected because it can measure and average the diameter of thousands of particles in one operation. The variations in hardness and matrix lattice parameter with aging were also studied and related to the particle size. EXPERIMENTAL PROCEDURE An alloy of the following composition was studied: Cr Ti A1 C Ni Wt pct 20.71 2.98 1.43 0.04 bal. At. pct 22.06 3.47 2.95 0.18 bal. The alloy, a 15- lb vacuum melt, was forged to 1/2-in. diam at a temperature of 1900" to 2200°F; was solution heat treated for 4 hr at 2000°F and water quenched; and was then aged in various ways. The ASTM grain size was 4 to 5. No (7') phase could be detected by X-ray analysis after solution treatment and electrolytic extraction. Aging was performed on 2-in. long specimens at 1400°, 1500°, and 1600°F for increasing times. One-half inch sections were removed after each time increment and were then electropolished in a solution of H3P04 saturated with chromium trioxide at a potential of 30 v and rectified with a tantalum electrode. Rockwell hardness measurements were taken using one side of the polished specimen. Matrix lattice parameter determinations were made on the other side using filtered chromium radiation references with the position of the (220) line of a silicon standard. To enable the precipitate particles of the (y') phase to be measured using X-ray line broadening techniques, it is first necessary to separate and concentrate this phase by electrolytic extraction. Extraction is necessary because the difference between matrix and precipitate lattice parameters is only approximately 0.5 pct and intensities of.the (y') phase lines are very weak relative to those of the matrix. The extraction techniques employed have been described before and found to produce a reasonably quantitative separation.398 A water solution of 15 pct H3Po4 is used at a current density of 0.5 amp per sq in. at 6 v. The precipitate particles are separated from the liquor by centrifuging and decanting and are then washed, dried and repowdered. A plot of the X-ray intensity vs diffraction angle for the (111) line of the precipitate particles was used as a measure of particle size. The intensity curve approximated the shape of Gaussian distribution function and its breadth was measured at the half height. The (220) line of a silicon standard was used to correct the measured line breadth for instrumental and other broadening errors. The Scherrer formula was used to calculate particle

Jan 1, 1961

By Tell Ertl

TODAY'S mining industry is witnessing a transition in labor utilization. The drill-jumbo operator, the mucking-machine operator, the blasting crew, the scaling and timbering crew are all specialists. The all-around miner is rapidly disappearing. As mechanization has resulted in a higher order of underground skills; specialization of labor has been a natural consequence, as has the need for more supervision and engineering. Mines now are cleaner, neater, safer, and have a greater productivity per man-shift than ever before. Nothing spectacular like the continuous miner has yet come to the underground metal mines, but t a gradual improvement in methods, equipment, and technical knowledge is achieving the increased efficiency. With the exhaustion of the rich ores and large profits and who-cares-about-the-costs, mining has become a business; that of producing low value ores at costs below selling price. Charles A. Chase, patriarch of Colorado mountain mining men, manager of the Shenandoah-Dives, was one of the first to preach and prove his preachings that mining is a business. He has been mining a lead-copper-zinc-gold-silver ore, much from elevations above 1.3,000 ft, for a quarter century without a shutdown.-The ore is of such low value that most engineers and investors still would consider it foolhardy. Yet he has kept Silverton, Colo., alive, has paid wages without a lapse, has produced $25 million of new wealth and maintained a steady return to the investors. This type of responsibility is increasingly apparent in the mining business and is one feather that can be worn proudly. .Much emphasis is being placed on improving, the productive mining operations-breaking, loading and transportation. Breaking in underground metal mining is done by drilling and blasting. To the writer's knowledge, no chain or rotary-type machine has been developed for mining strong, abrasive rock. Drilling Percussion drills are still the standard drilling machines underground. Diamond drills, that: were the rage a decade ago for drilling long holes, are being superseded by the rock drill. The development of the hard abrasion-resistant carbide bit permits full-gage long holes to be drilled by percussion drills at a lower cost than diamonds. The change in the use of percussion drills is chiefly in the method of mounting. The column and arm are disappearing and the jackleg and rubber-tired or track-layer jumbo mountings are taking its place. At the Homestake mine .lightweight jackhammers mounted• on pneumatic legs using 7/8-in. hexagonal drill. rods and 1 1/2-in, tungsten-carbide detachable bits have been found more portable and maneuverable. They have less air consumption, lowered, dynamite consumption, and more footage and tonnage per man-shift than with 3 1/2-in. drifters on a column mounting. Drills now are mounted on longer feed carriages, drilling up to 20 ft without changing steel. These mountings result in great savings because the driller can set up quickly, drill the entire depth of the hole without changing the drill rod or bit using carbide and one-use bits, and can move his machine quickly to the next hole. One man to the machine is becoming general practice. The result is longer rounds rounds drilled at a lower cost than the previously used short rounds. A jumbo developed in the Tri-State can be extended to mine ore left in the roof up to 65 ft above the floor. Drill-rod life was formerly considered to be about 250 min of actual use. The increase in the drilling time per rod per day has gone up considerably with the development of the jumbo and the long-feed carriage, resulting in which is apparently more rod breakage., Consequently, a great deal of research is being done in the attempt to develop an alloy-steel rod with longer service life to offset the greater cost. Some reports indicate that alloy steel or Swedish steel results in cheaper drilling than conventional drill rod. However, several tests have shown only slightly increased life for alloy drill rod. Undoubtedly, the blow of the rock drill, the length of the drill rod, and the resiliency of the rock being drilled are important factors in the life of drill rod, so it follows that alloy steel might work well in some mines and result in no savings in others. The bit forged on the drill rod is seldom encountered and steel detachable bits are not as common as in the recent past. The one-use bit is gaining popularity because of. the difficulty in rehardening reconditioned steel bits satisfactorily. It is thought that the, carbie-insert bit is most applicable to drilling hard 'rock' where the steel bit is unable to drill out a full change, for instance, in extremely abrasive

Jan 1, 1952

By F. M. Lewis, J.F. Myers

The Tennessee Copper Company's operations are in the Ducktown Basin, in the extreme southeast corner of Tennessee. The ore is of the heavy sulphide type, the predominating sulphides being pyrite, pyr-rhotite, chalcopyrite and sphalerite. The gangue is a micaceous schist, with varying amounts of free quartz. The mining operation develops two classes of ore, each of which is concentrated by the flotation process in separate mills. Table 1 shows a typical analysis of the ore treated in each mill. The London mill was built in 1922, with a capacity of 400 tons per day. This was gradually increased to 600 tons by 1926, to 900 tons in 1928, and to 1350 tons in 1938. Fig. 1 shows the crushing and grinding flowsheet in 1928, when the capacity was 900 tons; Fig. 2, the crushing and grinding flowsheet that was developed by 1938, for the treatment of 1350 tons per day. A comparison of these flowsheets reveals that this increase in tonnage, with a subsequent improved operation, was accomplished with identically the same major equipment. Improving a concentrator's capacity, metallurgical results, and costs as time goes by is a commonplace practice, and is accomplished in various ways, depending upon the local conditions. The reason for presenting the data of how this was accomplished in the mills of the Tennessee Copper Co. is that a fast-running rod mill plays such an interesting role

Jan 1, 1943

By J. F. Myers, F. M. Lewis

The Tennessee Copper Company's operations are in the Ducktown Basin, in the extreme southeast corner of Tennessee. The ore is of the heavy sulphide type, the predominating sulphides being pyrite, pyr-rhotite, chalcopyrite and sphalerite. The gangue is a micaceous schist, with varying amounts of free quartz. The mining operation develops two classes of ore, each of which is concentrated by the flotation process in separate mills. Table 1 shows a typical analysis of the ore treated in each mill. The London mill was built in 1922, with a capacity of 400 tons per day. This was gradually increased to 600 tons by 1926, to 900 tons in 1928, and to 1350 tons in 1938. Fig. 1 shows the crushing and grinding flowsheet in 1928, when the capacity was 900 tons; Fig. 2, the crushing and grinding flowsheet that was developed by 1938, for the treatment of 1350 tons per day. A comparison of these flowsheets reveals that this increase in tonnage, with a subsequent improved operation, was accomplished with identically the same major equipment. Improving a concentrator's capacity, metallurgical results, and costs as time goes by is a commonplace practice, and is accomplished in various ways, depending upon the local conditions. The reason for presenting the data of how this was accomplished in the mills of the Tennessee Copper Co. is that a fast-running rod mill plays such an interesting role

Jan 1, 1943

By R. P. Rothwell

The milling of silver ores has arrived at a great degree of perfection in the mining districts of our Western States and Territories, and I hare thought the record of the practical results obtained at the present time, in a few of the principal districts, would prove of value arid interest to many of our members, both at home and abroad. An American silver mill is composed, in descending order from where the ore is dumped, of: 1st. A rock-breaker, usually of the Blake or Alden pattern; 2d. The battery of stamps, the number of which varies from 5 to 120, generally in batteries of 5 or 10 heads, so arranged that a single battery may stand while the others are running; 3d. The tanks where the crushed ore settles (if it is a met stamping-mill), or of a drying-floor if the crushing is done dry; 4th. Amalgamating pans ; 5th. Settling pans ; 6th. Agitators or pans in which mercury escaping in the tailings is caught; 7th. Blanket sluices, over which the tailings run, and where mercury and unamalgamated sulplides are saved. A reference to the engravings (see plate), which show one of the latest forms of an 80stamp silver-mill run by a turbine water-wheel, will show clearly the arrangement of the several parts. THE ONTARIO, UTAH, SILVER MILL. One of the best examples of a silver-mill, and at the same time one of the most successful concerns in the West, is the mill of the Ontario Silver Mining Company, near Salt Lake, in Utah. This mill treats the ore from the Ontario mine, ore which at present is very base, being composed of zinc, lead, and silver sulphides and silver chloride in a quartz gangue. This ore has become baser as the mine attained greater depth, though the vein holds its own, or rather increases, both in thickness and richness. The mill is managed in a skilful and economical manner, though the necessity for

Jan 1, 1880

By J. B. Austin

In considering so complex a process as the smelting of iron in the blast furnace, there is obviously no single method of calculating efficiency that gives a complete appraisal of the performance of the furnace in all its several functions; such a comprehensive view as is required to evaluate producing ability and manufacturing costs for a given furnace is obtained only by considering a group of efficiencies, each of which measures the performance of the furnace from a specific point of view. For instance, there is the rate of consumption of coke per ton of iron produced, which is probably the most frequently considered, and is certainly one of the most important of the group; there is the efficiency of recovery of iron charged; and there is the efficiency of utilization of energy, both chemical and thermal, in some respects related to the former two yet in other ways independent of either. In each of these cases, the calculation can be made on the basis of the actual input of material or energy, or it may be based upon a comparison with the minimum amount of material or energy that would be required by a "perfect" furnace; that is, an imaginary ideal furnace analogous to the perfect steam engine used in thermodynamic calculations, when this furnace is operating under optimum conditions. Moreover, the furnace itself can be considered either as an apparatus for smelting iron or, taking a somewhat less common point of view, as a gas producer yielding iron and slag as by-products. Some of these efficiencies are more useful than others, yet all are instructive; for a knowledge of them not only leads to good engineering practice from the standpoint of control but also discloses limits to possible improvement in performance and indicates the lines along which improvement is most likely to be profitable. Estimates of some of these efficiencies have appeared from time to time in the literature, but many of them are open to objection because they are based on data of uncertain accuracy or because they have been calculated without due regard to the thermodynamic principles involved. Moreover, so far as the author is aware, no general survey of the blast furnace comparing its performance in all the aspects mentioned has been made.

Jan 1, 1938

By R. J. Reynik

A semiempirial small flunctation theory of diff- sion in liquids is presented, which employs a fluctuation energy assumed quadratic for a small atomic or molecular displacement and Einstein's random-iralh model. The resulting diffusion equation is given by In these equations. D is the diffusivity, is the average liquid shite coordination number (at interatomic distance d. cm. T is the absolute temperature, xu. em, is (the diffusive displacement. K, is the quadratic fluctuation energy force constant, and rg, cm, are the radii oj diffusing atoms A and B, respectively. The quantities Xn and K are calculated from the computer-filled values of the slope and intercept. respectively. The radius of self-diffusing atom or radii and of diffusing atoms A and B are eta United and compared with values reported in the literature.. The predicted linear variation of diffusivity with. It tempera lure htm been observed in approximately thirty-iire metallic liquid systems, and in over seventy-fiee other liquid systems, including the organic .alcohols, liquified inert gases, and the molten salts, ALTHOUGH the average density within a macroscopic volume element of liquid is constant for fixed total number of atoms. pressure. and temperature, there exist microscopic: density fluctuations within the respective volume element. As such the microscopic volume available to an atom and its Z first nearest neighbors at any instant of time fluctuates above and below the average volume available to these atoms. If one assumes that liquid state atoms vibrate as in a solid. and further postulates that the mean position of any atom in the liquid state is not stationary. but shifts during every .vibration a distance 0 5 j 5 xo. then every atom in the liquid state continuously undergoes diffusive displacements which vary in the range 0 5 j 5 ro. Mathematically. for a binary liquid system consisting of atcrms A and B. the maximum diffusive displacement. .YO, is defined by the equation: where d is the average liquid state interatomic distance at specified liquid state coordination number Z. and v~ \ and vg are the effective radii of diffusing atoms A and B: respectively. For self-diffusion. r^ equals rg , and Eq. [I.] reduces to: It is interesting to note that Eq. [l] or [2] can be used to compute the radii of the diffusing atoms, provided one had an experimental evaluation of xo. As such. the computed radii could be compared with metallic or crystallographic ionic radii to ascerlain the electronic character of the diffusing atoms. Thus it is proposed that in the liquid state the n~otion of an atom relative to its original equilibrium position of oscillation represents the thermal vibration of any atom and its Z first nearest neighbors. while the small and variable displacements. 0 5 1 5 xc,. of the centers of oscillation represent the complex diffusive motions of the atoms at constant temperature and pressure. This is consistent with data obtained from slow neutron scattering by liquids1 ' and resembles an itinerant oscillator model of the liquid state.'" It is further postulated that the atomic displacements characterizing the liquid state diffusion process are essentially a random-walk process. As such. it nlay be described by Einstein's equation:' where D is the diffusivity. sq cm sec-'. j2 is the mean square value of the diffusive displacement. and i> is the frequency of density fluctuations giving rise to diffusion. FORMULATION OF DIFFUSION EQUATION The effective spherical volume occupied by an atom, as a consequence of a microscopic density fluctuation which enlarges the volume available to any atom, exceeds its average liquid state atomic volume by an amount: where AV is the enlarged spherical volume, v is the radius of the diffusing atom. and j is the elementary displacement distance from the original center of oscillation of the vibrating atom to a new center of oscillation position. For small atomic displacements. where c is a constant whose value depends upon the assumed geometry of the enlarged volume. For a spherical increase in volume, c equals 4nr2. Following the treatment of Furthl' and ~walin." assuming the enlarged volu~nes AL7 for the diffusing atoms are distributed in a continuunl. the probability of finding a fluctuation in the size range 0 5 j 5 xo defined by Where c includes the geometric constant cl and Eij) is the fluctuation energy causing the volume change. But the proposed model assumes all the Z first nearest-neighbor atoms are centers of oscillation. and hence the probability that any of these atoms is adjacent to a fluctuation of magnitude 05j5xo is unity. Thus:

Jan 1, 1970

By J. R. Low, M. Gensamer

During the course of an investigation into the drawability of automobile-body sheet steel, it became apparent that certain advantages would be possessed by a deep-drawing steel with a very low yield strength, but almost normal tensile strength, provided a reduction in yield strength could be accomplished without sacrifice of ductility and fine grain size. It would also be desirable to have this steel free from strainaging; that is, free from the tendency for the yield point to return after it had been eliminated by straining. It was known that wet hydrogen treatment acted to eliminate aging, but as carried out by other investigators, at relatively high temperatures, this treatment resulted in grain coarsening. It has been established by some of the experiments reported in this paper that all of these objectives can be accomplished by treatment in wet hydrogen at a low temperature, in the neighborhood of 720°C. The time of treatment is relatively short (about 3 hr. to completion with 20-gauge sheet) if the water content of the hydrogen atmosphere is made fairly high, say almost 30 per cent by volume. At this temperature, the grain size remains fine in the time required. After this treatment sheet reduced the usual amount by cold-rolling has a grain size of about A.S.T.M. No. 7. The yield point is completely eliminated, and the yield strength is reduced to a very low value, in the neighborhood of 15,000 lb. per sq. in. The stress-strain curve departs gradually from the straight-line elastic part after the fashion of nonferrous deep-drawing alloys. This elimination of the yield point is accompanied by a very low indentation hardness; for example, 32 Rockwell B or even lower. There is no aging as measured by increase in the yield strength upon aging at room temperature or for 3 hr. at 200°C., after stretching about 10 per cent in tension. Tensile strength is only slightly less than the box-annealed sheet, seldom dropping much below 40,000 lb. per sq. in. Elongation is practically unchanged, or increased slightly. The term yield point, as here used, refers to the phenomenon of heterogeneous deformation occurring at a substantially constant load, observed principally in annealed low-carbon steels. If such a steel is loaded in tension, the load increases steadily with elastic strain, suddenly falls, fluctuates slightly about some constant value for a time and then begins to rise again as deformation proceeds. The maximum initial load before the sudden drop is generally called the "upper yield point"; the value of the load where deformation proceeds at a

Jan 1, 1943

By C. L. Ray, R. E. Baarson, H. B. Treweek

As an example of nonmetallic mineral flotation, the separation of several pegmatite minerals will be discussed in considerable detail, from both the laboratory-testing and plant-operation standpoints. The pegmatites have been chosen to illustrate the practicality of the selective separations of the minerals in a complex nonmetallic ore and, in so doing, to set forth a summation of the flotation art and technology which is applicable in part to the beneficiation of several less complex nonmetallic ores. In addition, a brief summary of descriptions of other nonnietallic mineral flowsheets and separations is included. Some of the industrial minerals now being concentrated by froth flotation methods commercially, or in the laboratory, are listed in Table 1. GENERAL CONSIDERATIONS There are two classes of chemicals that are normally utilized as collectors in froth flotation separations of nonmetallic minerals. These are defined as anionic and cationic and are typified by the fatty acids and amines, respectively. The fatty acids are selective to those minerals that have a high concentration of positive surface charges, such as the various calcium minerals typified by calcite, phosphate rock, and fluorspar. The amines are selective to those minerals with a high concentration of negative surface charges, such as silica sand and silicates. It should be noted, however, that by using various inorganic chemicals, a new or synthetic surface can be placed on specific minerals which produces different characteristics, thereby reversing the flotation reagent required for separation. The polar end of the collector attaches to the mineral surface either by chemical or physical adsorption; the nonpolar unreactive end is oriented away from the mineral surface. The result is a hydrophobic coating at the mineral surface which causes attachment to air bubbles. It is this surface condition that permits the floating of minerals which normally sink in water. In order to utilize these fatty acids and amine derivatives, several conditions .must be fulfilled. Before there can be a selective flotation process,

Jan 1, 1962

L. D. Ricketts, New York, N. Y.-In recent years the metallurgical field of the copper industry has expanded greatly, the copper ores have become lean and diverse in character, and we are obliged to treat such ores on a very large scale. On the commercial side, the operating and consulting staffs of ,the great mining companies have been enlarged and organized, and no great capital expenditure is decided upon until it has been investigated and recommended by a highly organized force of specialists as a committee. I believe that in the scientific field and in the most valuable proceedings of our various societies the old idea of one-man point of view and one-man treatment of principle and detail together has been. splendidly developed and should continue, but for the advancement of our art we should deliberately discuss subjects among ourselves in order to do away with the idiosyncrasies of the individual and to gain a composite view representing the best thought of many men. In the development of new ideas leading to the introduction of new methods, the societies could enlarge their present great field of usefulness if such discussion be had, and in my opinion further great good could be done if a number of men of different qualifications and experience would join in preparing a joint book, each dealing with his particular problem, but consulting the other men. In this way individualism would be preserved and various processes would be described, and if properly reviewed the paper would be palpably capable of analysis, and the student would have at his command the associated efforts of a group of qualified engineers.

Jan 4, 1915

By William Ian Wark, Alwyn Birchmore Cox

DIFFERENT parts of the world in which mineral separation by flotation is practiced experience vastly different natural temperatures, and in some districts there is a big difference between summer and winter temperatures. It will be shown in this paper that the temperature is of considerable importance where it is desired to separate pyrite or arsenopyrite from other minerals. It is probable that some of the differences obtained in the flotation of these minerals at plants working under otherwise similar conditions are due to temperature variations. The influence of temperature on the flotation of galena, chalcopyrite and sphalerite by xanthates is less marked than its influence on pyrite flotation. EXPERIMENTAL METHOD The methods used have been described previously.1-4 In each test the clean mineral specimen was immersed in a solution prepared by adding the reagents in the following order: (1) sodium carbonate and hydrochloric acid as necessary to buffer the solution and to give approximately the pH value desired, (2) sodium cyanide, (3) copper sulphate, (4) ethyl xanthate, followed by (5) a final adjustment of pH value. After ½ hr. the mineral was tested for a xanthate film by bringing a bubble of air into apparent contact with the submerged polished surface. If true contact (spreading) was not obtained within ½ min. and after cleaning the surface by wiping with a small linen pad, it was concluded that the adsorption of a xanthate film had been prevented. Following the method already described (ref. 2), curves have been constructed such that for a solution ' composition corresponding to any point below the curve, contact between mineral and air is possible, whereas for a solution composition corresponding to any point above the curve, contact is impossible.

Jan 1, 1938

By D. H. Polonis, M. B. Kasen

AN unusual thermal etching phenomenon has been observed on the surface of a Cu-Si alloy. The observations were made during studies of vacancy condensation pit formation which were reported in previous papers.1,2 Figs. 1 and 2 are photomicrographs of the surface of a Cu-4.8 pct Si alloy after heating in vacuo (3 x X mm Hg) to 525°C and subsequently holding at that temperature for 16 hr in an impure (air-contaminated) argon atmosphere. Under these conditions preferential removal of silicon from the matrix by oxidation results in a surface which is entirely a phase overlying an a plus y structure. The light areas of Fig. 1 are regions in which very little thermal etching has occurred, while the majority of the surface has experienced severe etching. Similar regions in Fig. 2 are seen as plateaus above contours produced by net transfer of material from the specimen surface. Twin boundaries are also visible in Fig. 2. The difference in matrix mi-crostructure between Figs. l and 2 reflects the par- ticular orientation of low-index planes with respect to the surface of observation. Thermal etching contours of this type have been studied in detail by Hondros and Moore Both of the photomicrographs show that one or more dark spots are located approximately at the center of every protected area; where two spots are in close proximity, the protected areas have merged. The microstructures indicate that the anomalous resistance to thermal etching is related to the presence of these spots. Williams and Hayfield have shown that local regions of unusually high oxidation resistance can be caused by a surface monolayer of atoms with a work function higher than that of the base material. The result is an inhibition of the rate of electron removal from the base material and a decrease in the oxidation rate. The source of the protected layer may be either surface diffusion from contaminants on the specimen surface or pipe diffusion of solute atoms followed by migration across the surface. In the latter case the driving force is a difference in chemical potential resulting in a Gibbs adsorption phenomenon. In the present case, chemical polishing of the specimen surface precluded contaminants of a strictly surface nature. Consequently, diffusion of impurity atoms from within the lattice appears to be the most tenable explanation of the observed phenomena. The authors propose that the structures of Figs. 1 and 2 reflect the diffusion of impurity atoms along extended dislocations within the individual a phase grains prior to surface oxidation. The central spots within the protected regions are seen as sites of dislocation emergence which have become locally decorated with oxide in the manner discussed in Ref. 1. Williams and Hayfield observed protected regions adjacent to the grain boundaries of iron-contaminated copper which they attributed to the segregation of iron to the grain boundaries coupled with high dif-fusivity along the complex dislocation array at such boundaries. No evidence of such grain boundary protection was observed in the Cu-Si alloy; this

Jan 1, 1964

By E. R. Buchanan, R. E. Reed-Hill

Cylindrical magnesium single crystals were deformed in torsion. The axis of torsion was the basal pole. Five crystals were deformed to different strains between 0.08 and 1.03 and then sectioned in order to determine their dislocation densities using the transmission electron microscope. The work hardening rate of all specimens was at least an order of magnitude higher than that normally associated with easy glide in a tension test and comparable to that obserzed in stage B of a tension test. The correspondence between stage B in a tension test and the initial stages of a torsion test is believed to result from the fact that in both cases deformation occurs in a structure containing roughly equivalent densities of the dislocations associated with the three basal slip vectors. THERE are three basic ways of changing the shape of a crystal using slip dislocations. The crystal can be sheared along a slip direction in a slip plane; it can be bent about an axis in the slip plane normal to the slip direction; and, if the slip plane contains multiple slip directions, it can be twisted or rotated about the slip plane normal. Of the three processes, generally known as translational, flexural, and rotational slip, only rotational slip has not been extensively investigated. The object of the present research was to obtain basic information about this phase of crystalline plasticity. This paper is concerned with some aspects of the stress-strain curves obtained by twisting magnesium crystals about their basal poles. Magnesium was selected for four reasons. One, its recovery rate at room temperature is relatively low. Two, single crystals may be easily grown. Three, at room temperature the critical resolved shear stress for basal slip is about two orders of magnitude lower than that for nonbasal slip, so that rotational slip might be expected to occur primarily by basal slip. Finally, relationships between flow stress, shear strain, and dislocation density have been determined for tensile deformation of magnesium crystals,' thereby providing a basis of comparison for the torsional results. EXPERIMENTAL PROCEDURES Crystals were grown from 0.5 in. diam extruded sublimed magnesium rod furnished by the Dow Chemical Co. who reported that it contained in weight percent less than 0.0003 Al, 0.01 Ca, 0.01 Cu, 0.0012 Fe, 0.001 Mn, 0.0005 Ni, 0.003 Pb, 0.001 Si, 0.01 Sn, and 0.02 Zn, with the balance magnesium. All crystals were grown in a dried argon atmosphere using Jill-son's2 modified Bridgman technique. Two different methods were used to obtain crystals with the basal plane normal to the specimen axis. These included direct growth from seeds of the proper orientation, and spark machining (trepanning) of 0.5 in. diam cylinders from larger (1.5 in. diam) randomly grown crystals. The crystals thus produced were polished in a 20 pct HC1 water solution and then etched in a 1 pct HC1 water solution to develop etch pits lying in rows parallel to the basal plane trace. The crystals were then revolved about their axes on the stage of a low-powered microscope. Torsion specimens were prepared only from those crystals whose axes were normal to the rows of etch pits. It is estimated that this simple orientation method was accurate to about 51 deg. 1.625 in. long cylinders were next cut from these selected crystals and then acid machined in a 20 pct HC1 water solution into torsion specimens with a 1 in. long by 0.30 in. diam reduced gage section. Following this, they were annealed in air at 400°C and furnace cooled to room temperature. The specimens were given a final polish in a 10 pct HC1 water solution, rinsed in ethanol, dried, and cemented into brass grips with an epoxy resin. In addition to the torsion specimens, several tensile specimens with their basal planes at 45 deg to the stress axis were also prepared with similar dimensions except that the gage sections were increased to 4 in. in length. The torsion specimens were tested in the apparatus

Jan 1, 1970