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By H. P. Leighly, J. W. Marx, H. L. Walker

A relationship between recrystallized grain size and prior deformation is predicted from elementary statistical considerations, and reasonable agreement with experiment is obtained. RECRYSTALLIZATION phenomena have received much theoretical and experimental attention, and very adequate discussions of the various mechanisms suggested have been given by Anderson and Mehl,' Cook and Richards,' and Burgers," and others. It suffices to note here that the initial concepts fitted one of two general hypotheses: I—The new crystals are nucleated within microscopic regions at which there is a concentration of internal stress, i.e., volume elements of maximum strain energy. 2—The new crystals have their inception in volume elements of minimum strain energy. In a comprehensive early review of the subject, van Arkel' considered both possibilities and came to the conclusion that hypothesis 2 was inconsistent with the experimental fact that the number of nu-cleations increased with increasing deformation. He suggested that, if allowance was made for a preliminary atomic rearrangement at the points of large internal strain, hypothesfs 1 provided the more reasonable concept. Following the initial observations of Collins and Mathewsonb nd Crussard,Y he systematic X-ray investigations of Cahn' and Guinier and Tennevin" established the existence of a polygonized structure in metals that had been cold-worked, and subsequently annealed, under conditions such that re-crystallization did not occur. This new experimental evidence by no means disproved the first nucleation hypothesis, a fact recognized by both Beck" and Cahn,10 who independently suggested nucleation mechanisms based on the idea that regions of large strain might polygonize before the bulk of the less deformed material. These mechanisms, together with others recently proposed," are dependent upon the prior existence of some degree of polygonization in the deformed material. On the other hand, a critical examination of the published data leads to the supposition that polygonization may not be the necessary precursor of recrystallization, but merely its favored energetic competitor. In regions where the lattice distortion is not too severe, the limited adjustment afforded by polygonization may permit the lattice to drop to a relatively stable low energy state in which the nucleation of a new crystal becomes improbable, even at elevated temperatures. Such structures, of course, might provide a fertile field for the growth of nuclei, if these could be introduced. In regions of concentrated lattice distortion, polygonization alone may not be able to accomplish an adequate strain reduction, and in these volume elements sufficient thermal activity permits the more drastic atomic rearrangement involved in nucleation. Completely polygonized structures are known to withstand extended heating close to their melting points," with no other effect than a slow enlargement of some of the subgrains at the expense of others. Once started, macroscopic recrystallization might be expected to go to completion in a matter of minutes under similar heat treatment. Crussard12 and his coworkers have found that recrystallization may occur in single crystals of impure (about 99.7 pct) aluminum without any detectable prior polygonization. The indication here is that large Cottrell impurity atmospheres inhibit dislocation movement, thus suppressing polygonization to such an extent that the alternative process, recrystallization, dominates the lattice restoration. Experimental studies relating recrystallization directly to stored energy have not, at the present time,

Jan 1, 1954

By Donald Jaffe, Michael B. Bever

The solidification of Al-Zn alloys (2 to 70 pct Zn was investigated at different rates of solidification. The resulting structures were studied; the amounts of nonequilibrium eutectic were measured and compared with the amounts calculated on the assumption of no diffusion in the solid. The compositions of the cored primary constituent were investigated by quantitative autoradiography after activation of the zinc by neutron irradiation. These compositions were also determined from microhardness values. IN a recent investigation of the soltdification of aluminum-rich AI-Cu alloys,' the amounts of non-equilibrium eutectic were measured and compared with the amounts calculated on the assumption of no diffusion in the solid. The compositions of the cored primary constituent were investigated by quantitative autoradiography. The work reported here extends the investigation of nonequilibrium solidification to the Al-Zn system in the range from 2 to 70 pct Zn. In addition to autoradiography, microhard-ness values were used to determine compositions on a micro scale. Solidification Experiments The alloys contained approximately 2. 6, 12, 20, 30, 50, and 70 wt pct Zn and the balance aluminum. According to published diagrams the eutectic reaction occurs at 382°C between the eutectic liquid (95 pct Zn), a (82.8 pet Zn), and $ 498.9 pct Zn). Solid-state reactions at lower temperatures (due to the miscibility gap between 350" and 275"C, the eutectoid at 275'C, and the precipitation from supcrsaturated a) did not affect this investigation. Even if they occurred to any appreciable extent, they did not alter the evidence pertaining to the solidification structures. The alloys had to be of high purity to avoid radioact~ve contamination during activation. The aluminum analyzed 0.015 pct Si, 0.009 pct Fe, less than 0.004 pct Cu, and less than 0.006 pct Mg with traces of sodium and titanium; the zinc was reported to be at least 99.99 pct pure with traces of iron and magnesium. The alloys were prepared under argon in an induction-heated, bottom-pouring furnace, and poured into a coated steel mold, which could be preheated to temperatures up to 700°C in order to control the rate of solidification. The pouring temperatures ranged from about 40" above the liquidus for 2 pct Zn alloys to about 130°C above the liquidus for 70 pct Zn alloys. As soon as the melt entered the mold, the readings of a thermocouple placed % in. above the bottom of the mold were recorded by a recording potentiometer. Cooling at the rate induced by the initial temperature of the mold was continued to a temperature 100°C below the liquidus; the mold with its contents was then quenched in icy brine. Quenching from a fixed interval below the liquidus was used to provide a standardized procedure, since the solidus and liquidus temperatures and the interval between them vary greatly over the composition range investigated. The temperatures from which the samples were quenched were below the equilibrium solidus, but under nonequilibrium conditions some liquid was still present. This residual liquid solidified during the quench. The samples measured 314 in. diam and 11, in. height. Drillings for chemical analysis were taken

Jan 1, 1957

By Lawrence B. Wright

The Republic district, Washington, is of new interest because of the discovery of new gold-silver ore within a unique structural pattern. The camp was revived in 1937 fol1owing installation of a plant to treat low-grade disseminated ore at Knob Hill and further stimulation followed discovery of "cross vein" breccia ores in 1939. Previous writers 1-2 ascribed the quartz veins to a latite porphyry stock, but are in disagreement as to its precise location and extent. This study leads to the conclusion that the ores have a more profound parentage linked to a broad system of thrust faults and folds, the mechanical origin of which is related to a southward trending (Sanpoil) syncline connecting with the Lewis and Clark zone of shift described by Billingsley and Locke3 in 1939. The Republic anticliue and a cross anticline recumbent against Cretaceous granodiorite. and involving some 4000 ft of Eocene andesite flows and early Miocene lake beds, localize the ores, mainly along the east flank, in a series of openings simulating drag folds and steeper than the folded flows. These broad structural features no doubt reach deeply into the basement rocks, where at appropriate crossings and junctions it is suggested that heat effects gave rise to ore-making materials, including, in this instance, intrusive breccias that later were mineralized, and comprising the broader bodies of new ores. The breccia ore is seen crosscutting the earlier narrow quartz veins with a welding of the two at junction areas by a second surge of ore minerals. The ore mined and developed since 1937 equals district production from 1896 to 1937 The ores are typified by cherty quartz, adularia and some barite, with fine pyrite and marcasite, polybasite, pyrargyrite, tetrahedrite and gold. Selenium is present, possibly with gold, as a normal selenide. The disseminated ores, as well as the vein and breccia ores, are localized principally in one 500-ft flow (Knob Hill andesite), which has been traced around the crest of the low northward-plunging Republic anticline. The gold-silver ratio in the earlier narrow veins is about I to 4 and in the disseminated and breccia ores, I to 7. The latter higher silver ratio is deemed to reflect the character of the second surge of mineralization. Sills and dikes of the Columbia River (Miocene) basalt cut the folded structure and ore, thus placing the mineralization in the middle Miocene. Introduction The Republic district of north central Washington is of new interest because of the discovery, development and extraction of new gold-silver ore; also, because of a unique local structural pattern believed to be integral with the broader tectonic mechanism of the continental framework. This district had 40 years of modest rating following its discovery in 1896. Its narrow ore bodies, complex mineralogy. and early inadequate metallurgy, together with the apparent bottoming of ore near 1000 ft, limited production to 300,000 oz of gold and 1,000,000 oz silver between 1897 and 1914. The camp was then reduced to lease Life until 1937, when the gold price increase of 1933 to $35 per ounce

Jan 1, 1949

By Donald L. Katz

THE Oklahoma City Wilcox sand, discovered on March 26, 1930, has produced 394 million barrels of crude oil and 819 billion cubic feet of natural gas as of July 1, 1941. The 100,000-bbl. wells, pressures of 2600 lb. per sq. in., and flows of "Wilcox" sand caused exciting moments in the early life of the field. Today the reservoir is substantially at atmospheric pressure and produces 75,000 bbl. of crude oil daily through 466 pumping wells. Early estimates of the initial crude-oil content of the "Wilcox" sand' indicated that about 600 million barrels of crude oil would remain after the pumping wells ceased to produce economically. The Oklahoma City Wilcox Secondary Recovery Association was organized in March 1939, to study the possibilities of recovering a portion of this oil. Only a very brief summary of the information available can be presented in a paper of this nature. Some simplification and generalizations are necessary to give the over-all picture in so short a space and statements made may not apply to a specific well or small area. Since the area under consideration by the Association is that north of the south line of section 22-11-3, some information will be presented for areas A, B, C, r, 2, 3 and part of 4 of Fig. 2, and some will be for the entire Wilcox zone west of the fault. This paper is essentially an abstract of an engineering report made by A. D. Small, B. T. Murphree, M. C. Sons and the author for the Oklahoma City. Wilcox Secondary Recovery Association on Sept. 5;.1940. Some information is taken from a report to the Association by C. V. Sidwell on March 1, 1940, and some data are from a recent report by A. D. Small. It gives a brief history of the Wilcox zone, estimates of the initial oil contents of the reservoir, present conditions in the reservoir, and probable results from several programs of "secondary recovery." HISTORY OF WILCOX ZONE The Wilcox sand lies on the flank of the general structure, as shown by cross section of Fig. 12.1 .4 and areal map of Fig. 2. The sand is of Ordivician age and is composed of well assorted, rounded' sand grains with no apparent cementing material. The loose texture of the sand is shown by the enormous quantities of sand production from the wells and from the soft cores. The productive sand varies from zero thickness on the east to 220 ft. maximum and to zero thickness on the west because of water. The development of the pool4 was dependent upon drilling restrictions within the city limits, which accounts for the spacing of drilling operations listed in Table I by years. In 1931, areas I through 7 of Fig. 2 were open for drilling with the exception of some west-edge properties, and all wells drilled before Feb. I, 1935, were in this portion of the field. Nearly all wells drilled from 1933 to 1937 were in areas A, B and C. Since 1939, the newly drilled wells have gradually enlarged the producing area toward the west in the northern portion.

Jan 1, 1941

By C. C. Herrick

The vapor pressure of indium has been measured by the torque-effusion technique, as a function of temperature between 1102o and 1422oK. For liquid indium, the vapor pressure (in atmospheres) can be represented by the equation -R In P = 5.782 x104/T - 25.29from 1000o to 1422oK. Extrapolation yields a calculated normal boiling point of 2329°K and a heat of vaporization at 298 oK of 58.09 kcal per mole by the third-law method and of 58.39 kcal per mole by the second-law method. Calculations indicate that the free-energy functions of Hultgren are to be preferred to those of Guruich. BECAUSE of the potential uses of liquid metals, it is important that convenient experimental methods be developed which will lead to a sufficient body of thermodynamic data so that reasonable estimates of properties of liquid metals can be made. Indium is particularly well-suited to investigation, since it remains liquid over a long temperature interval, it alloys readily, suitable containers for it are easily procured, and relatively few investigations of its thermodynamic properties in the region above 1000°K have been made. PREVIOUS RESEARCH The first determination of the vapor pressure of indium was made by Anderson,' using the Knudsen method and silica-lines stainless-steel cells. Kohlmeyer and spandau2 determined the normal boiling point, and a mass-spectroscopic investigation has been made by Lyubimov and Lyubitov.3 (Unfortunately, only an equation representing the data of the latter investigators has been available to us.) Hultgren et al.4 and Gurvich5 have published discordant tables of the free-energy functions for indium. EXPERIMENTAL METHOD The torsion-effusion principle has been described amply in the literature.8,7 With this method, one observes the angular deflection induced by effusion of vapor from a multihole effusion cell which is suspended from a filament producing a small rotational restoring force. The pressure within the effusion cell can be computed from the relation ziaifiai where k is the torsion constant of the filament, 6 is the observed angular deflection, and ai, fi, and qi are the area, force factor, and moment arm of the ith effusion orifice. The force factor f is analogous to the Clausing factor,' and corrects for the reduction in effusive force attributable to the finite geometry of the effusion orifice. Schultz and Searcy' have tabulated the force factors for various tube geometries. EXPERIMENTAL APPARATUS The physical arrangement employed in this study is shown in Fig. 1. The furnace elements are six Globar heat rods with 15-in. hot zones. Temperature is maintained to * 1°K by a Beck mechanism driving two 26-amp Powerstats in parallel. A Pt (Pt, Rh 10 pct) thermocouple serves as the sensing element. Four inner tubes act as vibration isolators; the air pressure required for maximum isolation was determined empirically, and is maintained by a solenoid valve. The tungsten fiber, 9 by 0.002 in., is joined to an 0.008-in. tungsten wire or graphite rod via a machined lightweight chuck.

Jan 1, 1964

By S. R. Mitchell, M. Weissman, J. H. Brown

It has been demonstrated that for fine grinding operations, the energy input (E) and the product size modulus (k) are related by an equation of the form E = Ak1-n (1) where "A " and "n" are constants.(1) Also, it was suggested that "A" is determined by the comminuting device and that "n" depends primarily on the rock. It was the purpose of this investigation to study these constants by determining the form of an energy-size reduction relationship over an extreme range of energy inputs, and at the same time, to evaluate the minimum particle size produced during grinding. The comminution system consisted of a stainless steel laboratory ball mill in which quartz was ground at 60% solids for times ranging from 1 minute to 700 hours. The mill which measured 10" diameter by 12" long was loaded with about 60 pounds of balls ranging in diameter from 3/8" to 1-1/8" and was driven at 55 r.p.m. Quartz was selected for the tests because it is a brittle material for which size distribution data were expected to show a constant distribution coefficient regardless of product size.(1) This permitted specification of product size by a size modulus alone. The quantities measured were the time of grind (measure of energy input) and the specific surfaces of the products. Since no accurate method is available yet for determining particle size directly in the very fine size ranges specific surface data were used for this purpose. The relationship between these two quantities may be expressed as where Cis a constant which includes a shape factor, p is the specific gravity of the solid,_S is the specific surface and D is an equivalent particle diameter. For a material in which the distribution coefficient does not change with size the term (l/S) may be substituted for k in equation L if the proportionality constant "A" is changed correspondingly. This substitution was made in this work but in addition, screen analyses were made on several products to verify the equivalence of the two methods of size specification. EXPERIMENTAL DETAIL QUARTZ Quartz from two sources was tested. One series of tests was made on a clear, high purity crystalline quartz from Brazil and Arkansas, and another series was run on massive quartz fromNewHampshire. Grinding charges of the high purity material consisted of 2000 gram samples of -3-8 mesh particles, while the charges of the New Hampshire quartz were 500 gram samples of a -35+48 mesh screen fraction. The difference in the sizes of these two series of charges was not significant in view of the extreme size reduction accomplished, and the New Hampshire samples were smaller to permit ginding to finer sizes in shorter times than required for 2000 gram lots. SAMPLING AND ANALYSIS Separate charges were ground for all tests in which the grinding times were less than one hour and for all tests on New Hampshire quartz since these products were difficult to sample accurately without affecting the entire charge. During the long time grinding tests the mill was

Jan 1, 1961

By Samuel G. Vera

INTRODUCTION The Climax Mine is a property of Climax Molybdenum Company, a division of AMAX Inc. Climax is located in the central part of the Colorado Mineral Belt on the west slope of the Tenmile Range, Lake County, Colorado at 3,425' m. above sea level. Climax Mine, the largest single producer of molybdenum in the free world, has been a cornerstone of mining in the State of Colorado for many years. Before molybdenum was known, the early hunters of gold and silver laid their hands on the outcrops of the Climax deposit and left it as low quality lead or graphite without much value. Today, 44,000 TPD of ore is extracted from the heart of Bartlett Mountain. The molybdenum, separated from the ore, is vital for mankind, being used for everything from fertilizer to fine components of aerospace ships, because of its valuable physical and chemical properties. The operations at Climax have never remained static. Constant demand for the "gray gold", and technological advancements, have converted Climax into an "open book of technology", where learning the still-hidden secrets of mining is a continuing process. (All figures related to tons are metric tons) BRIEF HISTORY The mine produced its first molybdenum ore in 1918. It was shut down in 1919, resumed production in 1924, and has been in continuous production since that time. During World War 11, a peak of 20,000 tons per day was reached, then tonnage dropped from 1945 to 1950. Since 1951, production has been in- creasing, reaching a peak of 46,000 tons per day during the month of June, 1980. Early mining used shrinkage stoping. Block caving using the grizzly system was introduced in the early 1930's. Caving methods were improved through empirical studies of rock behavior and by trial and error, evolving a very efficient mining method by the late 1940's. This form of continuous retreat panel caving, with small modifications, is still used today, and has made the Climax Mine one of the biggest underground mines in the world. The Climax Mine, synonymous with molybdenum, was essentially an underground mine until 1973 when the open pit was introduced. Since then, both mining methods have operated successfully. Current production is 60% from underground, and the remaining from the open pit. Climax has been in continuous operation for 56 years, and as of December 31, 1980, more than 386 million tons of ore have been mined. The orebody is not fully defined, and at the present mining rate, the known life span of the mine will be to the year 2020. GEOLOGY The Climax deposit is a large low-grade porphyry molybdenum deposit somewhat similar to porphyry copper deposits, with a well- mineralized quartz molybdenum stock work sys- tem. It lies within the pre-Cambrian granites and schists and the Tertiary Climax porphyry. The age of mineralization is thought to be mid-Tertiary and is characterized by fracture filling and replacement through silicification. The main economic mineral is molybdenum, with pyrite, cassiterite and wolframite as by-products. Fluorite and topaz also occur, but are not recovered at this

Jan 1, 1981

By P. Marier, T. R. Ingraham

When cylindrical powder compacts of nickelous oxide (NiO) are heated in an equilibrated stream of SO3, SO,, and 02, in the temperature range 500°to 800°c, tlickelous suljate (NiSO4) is formed as an adherent layer on the oxide. The reaction is diffusion-controlled, with an activation energy of 13 ± 3 kcal per mole. When cylindrical powder compacts of NiSO4 are heated in a stream of dry nitrogen in the temperature range 1000 0to 11500C, NiO is formed at a well-defined interface between the sulfate and oxide. The interjhce migrates into the sulfate at a constant rate at a constant temperature and gas flow. The reaction rate increases with increasing gas flow and decreases with increasing partial pressure of SO3 in the gas stream. Resolution of the partial-pressure data with a Lang-itzliir Adsorption Isothern suggests that about 80 pct of the NiO interface is covered with SO3. The heat of adsovption is about 68 kcal per mole. The activation energy of the decomposition process is 61 ± 3 kcal per mole. MOST of the work reported on the formation and decomposition of nickel sulfate is related to thermodynamics.1-3 No quantitative work has been reported on the decomposition process. The only kinetic work reported on the formation is that by Fletcher and shelef.4-6 whose main purpose was to study the effects of alkali metal sulfate additions on increasing the rate of nickel sulfate formation. They found that, in the absence of an additive, only small amounts of sulfate were formed and the kinetic data were difficult to interpret. However, they suggested that the sulfa-tion of nickel oxide is a diffusion-controlled process for which the activation energy is approximately 17 kcal per mole.6 In this paper, both the formation and decomposition reactions will be examined; and based on the effects of temperature, flow rate, interfacial area, and partial-pressure of sulfur trioxide, mechanisms and activation energies will be suggested for both processes. EXPERIMENTAL Material. The nickel source material used in all experiments was Baker and Adamson Reagent Grade NiSO4. 6H2O, for which the following analysis was supplied by the manufacturer: C1, 0.001 pct; NO3, 0.005 pct; Co, 0.02 pct; Cu, 0.005 pct; Pb, 0.002 pct; Fe, 0.001 pct: insol, 0.005 pct. The anhydrous sulfate was prepared by heating the hydrate at 420°C in a muffle furnace for 5 hr. Nickel oxide was prepared by decomposing the sulfate at 950°C over a period of 10 hr. Method. The technique used for measuring the rates of formation and decomposition was developed earlier in these laboratories.7-8 The method is based on the observation that the kinetic parameters of a reaction can be established in a flow system, with specimens prepared by compacting powder to a uniform pellet shape. The results are identical with those established with solid polycrystalline specimens or single

Jan 1, 1967

By D. L. Katz

The Oklahoma City Wilcox sand, discovered on March 26, 1930, has produced 394 million barrels of crude oil and 819 billion cubic feet of natural gas as of July I, 1941. The 100,000-bbl. wells, pressures of 2600 lb. per sq. in., and flows of "Wilcox" sand caused exciting moments in the early life of the field. Today the reservoir is substantially at atmospheric pressure and produccs 75,000 bbl. of crude oil daily through 466 pumping wells. Early estimates of the initial crude-oil content of the "Wilcox" sand1 indicated that about 600 million barrels of crude oil would remain after the pumping wells ceased to produce economically. The Oklahoma City Wilcox Secondary Recovery Association was organized in March 1939, to study the possibilities of recovering a portion of this oil. Only a very brief summary of the information available can be presented in a paper of this nature. Some simplifications and generalizations are necessary to give the over-all picture in SO short a space and statements made may not apply to a specific well or small area. Since the area under consideration by the Association is that north of the south line of section 22-11-3, some information will be presented for areas A, B, C, 1, 2, 3 and part of 4 of Fig. 2, and some will be for the entire Wilcox zone west of the fault. This paper is essentially an abstract of an engineering report made by A. D. Small, B. T. Murphree, M. C. Sons and the author for the Oklahoma City Wilcox Secondary Recovery Association on Sept. 5, 1940. Some information is taken from a report to the Association by C. V. Sidwell on March I, 1940, and some data are from a recent report by A. D. Small. It gives a brief history of the Wilcox zone, estimates of the initial oil contents of the reservoir, present conditions in the reservoir, and probable results from several programs of "secondary recovery." History of Wilcox Zone The Wilcox sand lies on the flank of the general structure, as shown by cross section of Fig. I2,3,4 and areal map of Fig. 2. The sand is of Ordovician age and is composed of well assorted, rounded sand grains with no apparent cementing material. The loose texture of the sand is shown by the enormous quantities of sand production from the wells and from the soft cores. The productive sand varies from zero thickness on the east to 220 ft. maximum and to zero thickness on the west because of water. The development of the pool4 as dependent upon drilling restrictions within the city limits, which accounts for the spacing of drilling operations listed in Table I by years. In 1931, areas I through 7 of Fig. 2 were open for drilling with the exception of some west-edge properties, and all wells drilled before Feb. I, 1935, were in this portion of the field. Nearly all wells drilled from 1933 to 1037 were in areas A, B and C. Since 1939, the newly drilled wells have gradually enlarged the producing area toward the west in the northern portion.

Jan 1, 1942

By D. L. Katz

The Oklahoma City Wilcox sand, discovered on March 26, 1930, has produced 394 million barrels of crude oil and 819 billion cubic feet of natural gas as of July I, 1941. The 100,000-bbl. wells, pressures of 2600 lb. per sq. in., and flows of "Wilcox" sand caused exciting moments in the early life of the field. Today the reservoir is substantially at atmospheric pressure and produccs 75,000 bbl. of crude oil daily through 466 pumping wells. Early estimates of the initial crude-oil content of the "Wilcox" sand1 indicated that about 600 million barrels of crude oil would remain after the pumping wells ceased to produce economically. The Oklahoma City Wilcox Secondary Recovery Association was organized in March 1939, to study the possibilities of recovering a portion of this oil. Only a very brief summary of the information available can be presented in a paper of this nature. Some simplifications and generalizations are necessary to give the over-all picture in SO short a space and statements made may not apply to a specific well or small area. Since the area under consideration by the Association is that north of the south line of section 22-11-3, some information will be presented for areas A, B, C, 1, 2, 3 and part of 4 of Fig. 2, and some will be for the entire Wilcox zone west of the fault. This paper is essentially an abstract of an engineering report made by A. D. Small, B. T. Murphree, M. C. Sons and the author for the Oklahoma City Wilcox Secondary Recovery Association on Sept. 5, 1940. Some information is taken from a report to the Association by C. V. Sidwell on March I, 1940, and some data are from a recent report by A. D. Small. It gives a brief history of the Wilcox zone, estimates of the initial oil contents of the reservoir, present conditions in the reservoir, and probable results from several programs of "secondary recovery." History of Wilcox Zone The Wilcox sand lies on the flank of the general structure, as shown by cross section of Fig. I2,3,4 and areal map of Fig. 2. The sand is of Ordovician age and is composed of well assorted, rounded sand grains with no apparent cementing material. The loose texture of the sand is shown by the enormous quantities of sand production from the wells and from the soft cores. The productive sand varies from zero thickness on the east to 220 ft. maximum and to zero thickness on the west because of water. The development of the pool4 as dependent upon drilling restrictions within the city limits, which accounts for the spacing of drilling operations listed in Table I by years. In 1931, areas I through 7 of Fig. 2 were open for drilling with the exception of some west-edge properties, and all wells drilled before Feb. I, 1935, were in this portion of the field. Nearly all wells drilled from 1933 to 1037 were in areas A, B and C. Since 1939, the newly drilled wells have gradually enlarged the producing area toward the west in the northern portion.

Jan 1, 1942

By C. F. Lucks, W. D. Wood, H. W. Deem

Electrical ad thermal-conductivity measurements have been made on titanium and 6 titanium alloys. The following expression was derived for calculating thermal conductivity from electrical conductivity: K = 0.626 s T x 10-8 + 0.00497 where K = thermal conductivity, cal sec-1 cm-2 cm0C-1 s = electrical conductivity, ohm-]cm-1 T = temperature, deg Kelvin This expression gives calculated thermal conductivities that are not in error by more than 10 pct from the experimental values for A-55 titanium and the 6 alloys measured; namely, A-110AT, C-110M, C-130AM, Ti-6A1-4V, Ti-140A, and Ti-155A, which are representative of the presently available commercial a and a-ß titanium alloys. THERMAL conduction in a gas, liquid, or amorphous solid is accomplished by energy diffusion from molecule to molecule, a relatively slow process. For this reason, such materials have a low thermal conductivity. When a material is crystalline, there is in addition a heat transfer by a vibratory motion of the crystal lattice. It is the contribution of this lattice conduction that makes a crystal a much better conductor than a gas, liquid, or amorphous solid. Lattice conduction, however, does not account for the relatively enormous thermal conductivity of a metal. This is explained by the freedom of movement of valence electrons. These valence electrons drift in a metal in a direction toward a drop in electrical potential and, to a lesser degree, in the direction of a temperature drop in the metal. Since both the electrical and thermal conductivities of a metal depend upon the presence of free electrons, there should be some relatively simple relation between the two. Wiedemann and Franz in 1653 first discovered an approximate empirical relation between the electrical and thermal conductivities of metals at the same temperature. This ratio varies appreciably with temperature, and Lorenz later showed that by adding a temperature factor to the Wiedemann-Franz ratio the value of K/(s T) is constant, where K is the thermal conductivity, a the electrical conductivity, and T the absolute temperature. This Lorenz constant shows a greater variation for alloys than it does for pure metals, the ratio increasing slightly as the proportion of alloying elements increases. It has been found that a closer correlation between electrical conductivity and thermal conductivity can be obtained by means of an equation of the form K - A s T + B [1] where A and B are constants. In this equation the term AsT is the contribution of electronic conduction and B is the contribution of lattice conduction to the total thermal conductivity. EXPERIMENTAL MEASUREMENTS Electrical-resistivity and thermal-conductivity measurements on titanium and 6 titanium alloys serve as the basis for determining an equation of the K = AsT + B type for titanium alloys. Specimens—Table I shows nominal compositions of the 7 metals on which electrical and thermal conductivities were measured. The electrical and thermal-conductivity specimens for each alloy were taken from stock of the same heat and usually from adjacent sections of the same bar. All of the metals measured were in a mill-annealed condition. Methods—Electrical-resistivity measurements

Jan 1, 1959

By Robert M. Funk, James E. Lawver

The development of a laboratory and pilot-scale high-tension electrostatic flowsheet for the production of iron-ore super concentrates having silica contents in the range of 0.1% is presented, A variety of hematite and magnetite ores were tested with this flowsheet, and the pertinent metallurgical data are given. The applications and limitations of this process are brought out in terms of both practical and theoretical considerations. There have been many new developments in the past few years that have required mineral beneficiation engineers to consider new techniques for iron-ore concentration. Developments in iron powder metallurgy, and particularly the making of sheet metal directly from high-purity iron-ore concentrates, and the concept of using metallized pellets as a substitute for scrap in electric-furnace steelmaking have created demands for what is commonly referred to as iron-ore superconcen-trates. In most cases, specifications for superconcentrates are that they contain less than 0.1% total gangue, with some applications requiring less than 0.05% gangue. To produce these concentrates, new and modified processes are being developed, and the three methods receiving attention as the primary concentrating methods are: 1) Magnetic separation in which dry rotor-type equipment is used for magnetite and the high-intensity magnets are used for hematite. 2) Amine flotation. 3) "High-tension" electrostatic separation (or, elec-trodynamic concentration). This paper examines the high-tension electrostatic process in terms of its limitations and abilities for the production of iron-ore superconcentrates. A technically effective and simple flowsheet was developed through laboratory and 5 and 100-ton pilot-plant studies for the production of concentrates containing from 0.02 to 0.20% SiO, with iron recoveries between 85 and 90%. The process is also shown to be economically feasible. Laboratory Test Program Separation Characteristics: The suitability of the electrostatic high-tension method for iron-ore supercon-centration stems from the fundamental mechanism governing the process, i.e., particles are separated on the basis of differences in electrical conductivities. This conductivity is a characteristic property of minerals, and if the difference between the conductivities of two min- erals is great enough, then their separation can be performed by a high-tension machine. As shown in Figs. 1 and 2, the critical factor is the time necessary for the particle charge density, which is established by a corona discharge field, to decay to a level such that the centrifugal force acting on the particle exceeds its electrostatic, or image, force. At this point, the particle can leave the rotor at some trajectory and fall into an appropriate product receptacle. This decay time is directly proportional to electrical conductivity, and the process variables, such as feed rate, rotor speed, electrode configuration, and rotor composition, are selected to optimize the ability of the separator to resolve different conductivities. Table 1 lists the measured conductivities for some of the iron and gangue minerals used in developing the flowsheet. These results were obtained by using the conductivity cell described by Lawver and Wright.' The discharge curve of most minerals that lend themselves to super concentration by high-tension is so fast that the

Jan 1, 1971

By F. O. Jones

The capabilities of small proportions of divalent cations, such as calcium or magnesium, for controlling clay blocking are reported. Potentially sensitive formations can be exposed to fresh water if at least one-tenth of the salts dissolved in both the native water and invading fresh water are calcium and magnesium salts. Often, even less suffices. The behavior evidently depends upon the cation exchange properties of the clays, which favor adsorption of calcium and magnesium over sodium. Clays having sufficient adsorbed calcium and magnesium resist dispersion by water and consequent blocking of permeability. An allied phenomenon, the dependency of clay blocking on salinity contrast, is also reported. Abrupt change from highly saline to fresh water can cause blocking which may not occur if salinity is lowered slowly. A process related to osmosis is thought responsible for this behavior. Applications of findings to drilling, fracturing and water flooding are discussed. INTRODUCTION Many formations, when exposed to fresh water, can lose permeability through clay effects.',' For example, drilling-mud filtrate can cause oil permeability decreases, which persist long enough to interfere with drill-stem testing and well completion.3 Ultimate productivity may suffer when clay damage is severe, especially if drawdown pressures are low.' The injection pressures and the time required for water flooding can increase if clay blocking occurs. Earlier work indicates that clay blocking is caused by obstruction of flow channels by clays or other mineral fines dispersed by fresh water.'!" It is well known that increasing salt concentrations in water tends to prevent clay blocking. Also it is well established, although perhaps not as widely known, that the nature of the dissolved solids is also important. If, for instance, formation clays are exposed to calcium chloride solution and then exposed to weaker solutions of calcium chloride or distilled water, considerably less permeability damage results than if the clays had been exposed instead to sodium chloride solutions. The reasons for this behavior are: (1) clays are cation-exchange, or base-exchange, materials similar in this respect to zeolites or exchange resins, and (2) clays in the calcium form do not disperse easily in fresh water, whereas clays in the sodium form do. The base-exchange form of a clay is easily altered by flowing a solution through it. For example, a sodium clay can be changed to a calcium clay simply by passing a calcium chloride solution through the clay bed. There is general agreement that the reason calcium and magnesium clays do not disperse easily in fresh water is because the calcium ions do not ionize easily from the clay surfaces.' Sodium clays, however, are believed to allow the sodium ions to ionize from the clay particle surfaces. In fresh water, this allows the particle to accumulate a net negative electrical charge great enough for the particles to repel one another and, therefore, disperse more easily. The foregoing suggests that, even in the presence of a large excess of sodium, a relatively small ratio of divalent cation, such as calcium or magnesium, might serve to prevent clay dispersion. The divalent ion probably adsorbs to a disproportionately large extent, because of being adsorbed more tightly, with the result that the proportion of divalent cation on the exchange positions of the clay might then be great enough for the clays to resist dispersion. Consequently, an investigation was conducted to find how mixtures of salts in solution influence clay blocking. APPARATUS AND PROCEDURE Water permeability tests were conducted using conventional techniques. The equipment is illustrated schematically in Fig. 1. Flow rates of solutions driven through small core samples at known temperatures and pressures were measured. Regulated compressed air, usually at 10 to 15 psig, was used to drive the solutions. Core samples 0.75 in. in diameter and 1 in. long were used for the most part. Cores were saturated by evacuating and then admitting a de-aerated solution. Tight core samples were first saturated with carbon dioxide gas and then evacuated and saturated with the test solution. After saturation, 140 psig pressure was imposed for several hours. Cores were tested to insure absence of gas saturation by a Boyle's

Jan 1, 1965

By M. A. Jones

Performance of a pilot flood in eastern Kansas indicates improved recovery and accelerated production resulting from mobility ratio control obtained by adding a high moleculur weight polymer to injected water. Ultimate pilot flood recovery of the 75-cp reservoir oil is anticipated to he 350 bbllacre-ft during the six-year flood life. Cumulative recovery to date totals 242 bbl/acre-ft after 30 months of injection. Reservoir parameters and flood performance are disc~rssed in detail to provide a case history relating to the feasibility of polymer flooding. INTRODUCTION The Vernon Polymer flood of the Brazos Oil & Gas Co., located in Sec. 2, 24 S., 16 E., Woodson County, Kans., was begun in late Oct., 1963. Injection of a 500 ppm solution of Pusher* polymer was initiated in a 15-acre pilot to determine feasibility of improving oil recovery by mobility ratio control. Performance to date and the anticipated recovery of 115,000 bbl from the 329 acre-ft pilot indicate efficient displacement of the viscous reservoir oil. Dependence of flood recovery on the displacing fluid-displaced oil mobility ratio has long been recognized. Displacement efficiency of the reservoir oil decreases with increasing mobility ratio. Therefore, economic reduction of this parameter is an attractive approach to improving oil recovery. particularly from viscous oil reservoirs where mobility ratios are often quite high. Waterflood mobility ratios can be controlled by dilute solutions of certain polymers'; which provide a displacing fluid with considerably reduced mobility. Reservoir parameters and flood performance are emphasized in this paper to provide data relating to polymer flood applicability. THEORY The polymer used in the Vernon pilot exhibits the property of unusually high resistance to flow through porous media.'.' A small concentration in injected water effects a mobility reduction considerably beyond that predicted from increases in bulk viscosity as measured in a capillary or rotating cup viscosimeter. Water mobility in the subject flood is reduced by a factor of 7.55 with the addition of 500 ppm Pusher chemical to injected water while the bulk viscosity is increased from 1.03 to only 1.40 cp at 75F. The exact flow mechanism causing resistance to flow has not been established; however, it is observed only in tortuous flow systems and appears to be influenced by brine properties, rock properties and oil saturation. Consequently, mobility reduction is estimated from flow studies for a given sample of reservoir rock and is expressed in terms of a "resistance factor".' This parameter is defined as the ratio of brine mobility to polymer solution mobility measured at residual oil saturation: RF= ?m/?p= (km/µm)/(kp/µp)M.......(1) where RF = resistance factor (dimensionless) k*. and A, = mobility of water and polymer solution, respectively k,,, and k,, = water and polymer permeability, respectively (darcies) µie and µp = viscosity of water and polymer, respectively (poise). Eq. 1 is similar to the expression commonly used to relate the relative mobility of the water bank at residual oil saturation to oil-bank mobility at irreducible water saturation: where M =mobility ratio of water to oil (dimension-less) A, = mobility of oil k, = permeability to oil (darcies) )i* = oil viscosity (poise). From Eqs. 1 and 2 it is apparent that the polymer-solution-to-oil-mobility ratio can be approximated by dividing the brine-to-oil ratio by the resistance factor RF: Mpn=M10/RF...........(3) where M,-, = mobility ratio of polymer solution to oil (dimensionless). This simplified presentation assumes no dilution of the polymer solution by connate water. Also, the presence of a connate water bank separating the polymer solution from the displaced oil is not considered. Displacement of oil by waterflooding is increasingly dominated by viscous forces as the viscosity of the oil displaced increases. When the oil mobility is less than that of the injected water, the oil-water interface is not a piston-like front.3,' Instead, instabilities occur at the flood front in the form of viscous fingers which tend to penetrate the less mobile oil bank. The magnitude of these protrusions, or the degree of channeling, increases

Jan 1, 1967

By A. D. Rovig, D. W. McGlashan, Donald M. Podobnik

Crystal-chemical and stntctural properties of sulfide minerals are considered. The information gained is to be used to interpret (I ) freshly broken mineral surfaces, (2) modifications of the mineral surfaces, and (3) reactions at the mineral surfaces. From these basic disciplines, concepts with regard to the changes that surfaces undergo, reactions that might take place, the geometry of the interface, the state of different atoms and ions in the interface, and other physical and chemical properties of an interface must be developed, weighed and applied. The authors first deal with these conceptual considerations from which hypotheses are set forth to describe the environ men tal-interfacial relationships for several sulfide minerals. Qualitative and quantitative explanation of par-ticulate solid separations are unknown entities because of the lack of adequate models and mathematical relationships to explain the activity occurring between the solid and liquid phases. It is a transitional region in which it is difficult to ascertain the mechanisms of adsorption of ions, molecules, etc., on mineral surfaces, as well as other secondary reactions which occur in interfacial regions. Thus, in this paper the authors deal with conceptual considerations from which hypotheses are set forth to describe the environmental-interfacial relationships for sulfide minerals. GENERAL CONSIDERATIONS Interfacial Reactions:Interfacial reactions are the cruxes of flotation schemes as well as other processes such as thickening, filtration and hydrometallurgy. However, as noted by Klassen and Mokrousov: 1 "The problems concerning the surfaces of natural minerals, the laws governing simultaneous adsorption from aqueous solution on these surfaces of a whole series of reagents, the laws of the surface reactions and the properties of water layers separating the minerals, are all known to a first approximation only." An investigator has the privilege of postulating methods of solid-liquid interfacial reactions. REACTIONS WITH WATER - Water consists of hydronium (H3 O 4) and hydroxyl (OH-) ions in the ionized state. That this is so forms the basis for the postulated reaction of the hydrated hydrogen ion with net-negative mineral surfaces as depicted in Fig. 1. In this case water is bonded to mineral surfaces through hydrogen-bridge-type bonds - possibly hydrogen bonds. Although bonding of the van der Waal type may be responsible for this reaction, it is most likely that stronger bonds are involved. Once firmly bonded to the surface, the water layer is known to be quite tenacious. It is further speculated that a shear plane exists at some distance (see Fig. 1) away from the mineral surface. Exact location of this plane is not known, but in all probability it will be positioned across a weak bond of the hydrogen-bond type where the surface-attached water is coordinated to the original hydrated hydrogen ion. REACTION WITH METAL IONS - Klassen and Mokrousov ' state: "The presence of an ion in water leads to an immediate formation around that ion of a highly condensed atmosphere of water dipoles and thus to hydration of the ion." The fact is known that multivalent cations are strongly hydrated, usually by six or eight molecules of water, and that anions are not so strongly hydrated. Conceding the fact that thermodynamics, concentration, pH, and physical considerations are of utmost importance in truly explaining a mechanism of metal ions reaction with a hydrated mineral surface, it does seem logical that the mechanism illustrated in Fig. 2 is feasible. In this reaction, the metal ion (M) is coordinated in one dimension - to the mineral-surface hydration layer. Note also that explanation of this reaction requires that the shear plane move to a less stable bond configuration; that is, the shear plane has moved to a position between the metal ion and the other coordinated water molecules which are more free to dissociate. Reactions as depicted in Fig. 2 should cause the formation of an apparent mineral surface which is net-positive. Immediately, it must be noted that measurements of apparent-mineral surfaces serve - within limits - to indicate a degree of ion-surface reaction capability. The major limiting factor he re is one related

Jan 1, 1970

By F. S. Pettit

The oxidation of Ni-3 to 25 wt pd Al alloys has been studied in 0. 1 atm of oxygen at temperatures between 900° and 1300°C. These alloys have been found to oxidize by three different mechanisms which depend on the temperature of- oxidation and the alloy composition. Two of the three mechanisms do not permit a continuous layer of Al,0, to be formed on the alloy surface and the oxidation rates are greater than that for pure nickel. The third mechanism results in the formation of an external A1203 scale and lke oxidation rates are about three orders of magnitude smaller than those for pure nickel. The minimum amount of aluminum required for the formation of external scales of A L,0, has been determined. NICKEL-base alloys are currently the main source of materials for use at elevated temperatures in gas turbine engines. These alloys are usually coated to obtain oxidation resistance. Coatings on nickel-base alloys are frequently formed by reaction of the alloy with aluminum whereby alloyed nickel aluminides are formed. The alloyed nickel aluminides provide protection to the nickel base alloy because external scales of A1203 (alumina) are formed during oxidation and mass transport through A120, is slow in comparison to mass transport through most other oxides. In view of the protective properties of A1203, it is important to know how much aluminum is required in these alloys in order to form external scales of AlzO,. The present paper is concerned with the oxidation kinetics and the oxidation mechanisms of Ni-A1 alloys and the minimum amount of aluminum required in these alloys for the formation of external scales of Alz03. THEORETICAL CONSIDERATIONS When a Ni-A1 alloy is heated in oxygen at elevated temperatures, the following reactions can take place on the surface of the alloy where the oxide phases are assumed to be virtually pure: These oxide phases are in the form of nuclei scattered over the surface of the alloy and, in view of their rapid formation, they need not be in equilibrium with the alloy. As the oxidation process continues, equilibrium between the alloy surface and the oxide phases is approached and the stability of the oxide nuclei is determined by the composition of the alloy at the alloy/oxide interface because of the following reactions: 3NiA1204 + 2A1 (alloy) = 4AlzO3 + 3Ni (alloy) [41 4Ni0 + 2Al (alloy) = NiA120, + 3Ni (alloy) [ 5 1 Application of the mass-action law to Eqs. [4J and [5J yields the following equilibrium conditions for these reactions: where aA1 and aNi are the activities of aluminum and nickel, are the standard free energies of formation of NiO, A1203, and NA1204, respectively, R is the gas constant, and T is the absolute temperature. If the composition of the alloy at the alloy/oxide interface is such that (akl/ahi) is greater than the equilibrium values defined by Eqs. [6] and [7], then Reactions (41 and [5] will go to the right as written. Conversely, if the alloy composition is such that the activity ratio (aLl,/aki) at the alloy/oxide interface is less than the equilibrium values, then Reactions [4] and [5] will proceed to the left. The equilibrium activity ratios in Eqs. [6] and 171 can be calculated since values for the standard free energies of formation of the oxide phases are available. Standard free energies of formation for NiO and A1203 have been tabulated by Elliott and ~leiser.' The standard free energy of formation for NiA1204 can be obtained from the data of Tretjakow and Schmalzried.' The results of these calculations are tabulated in Table I. Table I shows that the following inequality is valid over the temperature interval 900" to 1300°C: (Reaction [5]) (Reaction [4]) « 1and therefore the aluminum activity for these compositions can be taken as equal to the square root of the activity ratios (i.e., aNi = 1). If equilibrium is estab-

Jan 1, 1968

By P. J. Spencer, J. N. Pratt

The vapor pressure of manganese over liquid Mn-Sn alloys has been determined by a high-temperature torsion-effusion technique. Alloys containing from 8 to 100 at. pct Mn were investigated in the temperature range jrom 1280" to 1580" and the measured pressure values were used to calculate the partial and integral thermodynamic properties of the liquid alloys. The activities show small negative departures from ideality while the integral heats and excess entropies of mixing are asymmetric inform, changing from positive to negative with increasing manganese content. The possible contribution of various factors to the observed thermodynamic properties is discussed. COMPARATIVELY few thermodynamic data are available for manganese alloy systems.' Therefore, as part of a continuing program of studies of the thermodynamic properties of transition metal alloys, measurements have been made on various binary alloys involving this element. In recent publications,2~3 investigations of liquid Mn-Cu alloys and of the Mn-Au system in both solid and liquid states have been reported. For the first-mentioned system the work suggested that magnetic interactions may be responsible for the observed form of the thermodynamic properties, while in the second the influence of the electrochemical factor appears to be dominant. The present paper describes a similar study of liquid Mn-Sn alloys. Again the thermodynamic properties have been obtained from vapor pressure measurements made by use of a high-temperature torsion-effusion technique.4 A detailed description of the apparatus and of the experimental procedures used in alloy preparation and pressure measurement may be found elsewhere.2'4 EXPERIMENTAL RESULTS Sixteen alloys, ranging in composition from 8 to 100 at. pct Mn, were prepared from spectroscopically standardized manganese of 99.99 pct purity and tin of 99.999 pct purity, both supplied by Johnson-Matthey and Co., Ltd. One-gram samples of the alloys were obtained by carefully weighing appropriate amounts of the pure components into an effusion cell; this was then suspended in the apparatus and the metals melted together in situ by heating under vacuum to approximately 1550°K. After allowing sufficient time for a homogeneous liquid alloy to be formed, vapor pressure measurements were commenced. These were determined as rapidly as possible at a series of steady temperatures within the range of interest. The duration of experimental runs on individual samples was kept sufficiently short to ensure insignificant varia- tion of alloy composition during investigation. After completing pressure measurements, the alloys were rapidly cooled and their compositions checked by weighing or chemical analysis. All experiments were conducted using effusion cells machined entirely from boron nitride. Measurements were made using a variety of cells with orifice areas ranging from 0.0032 to 0.0075 sq cm and lengths of the order of 0.04 cm; the usual effusion correction factors for orifice geometry and molecular distribution were calculated using Freeman and Searcy's equation5 and had values between 0.6 and 0.75 for the orifices employed here. The vapor pressures of manganese over the alloys were measured at approximately 20°K intervals in the temperature range 1280" to 1580°K. In view of the close approximation of the measured pressures to Clausius-Clapeyron behavior in the experimental temperature range, the data for each alloy have been expressed by equations of the form: logp(atm) =-A/T + B A least-squares computer treatment was applied to the vapor pressure values in order to obtain the coefficients A and B with their associated error. The resulting equations are listed in Table I, together with the equation for pure solid manganese obtained from a previous study.4 To minimize the effect of possible apparatus calibration errors, the activities and partial free energies of manganese in the alloys were calculated by initial reference to the latter equation, obtained from identical torsion-effusion measurements. The immediately resulting thermodynamic quantities, based on a solid manganese reference state, were then converted to refer to the more appropriate supercooled pure liquid manganese standard; tabulated values of the free energies of solid and liquid manganese from Hultgren et al.' were used for this purpose. Partial entropies of solution of manganese were calculated from the temperature coefficients of the free energies and partial heats from the Gibbs-Helmholtz relationship.

Jan 1, 1969

By H. Habenicht, J. J. Scott

An experimental method is described to compare strain data for rock and rock bolts when exposed to shock waves released by blastings. Static and dynamic strains were measured. Bolt gage response indicated a static decay of the bolt anchorage coupled with a reaction due to blasting vibrations. A distinct loss of bolt tension was indicated during vibrations and this was accompanied by a smaller but steady loss of tension due to static loading. The strain losses were found to relate to the shock source distance and the vibrational amplitude in the rock and bolts. Millions of roof bolts are used each year to stabilize mine openings and prevent their failure. Frequently, bolts become loose and lose their effectiveness as reinforcement to the mine structure. Many attempts have been made to determine the cause of loosening, including observation of the bolt tension or bolt torque through the use of torque wrenches, compression pads, and load cells. Pull tests have been used extensively to determine anchorage characteristics.102 These investigations have shown that even when bolts are loaded below the nominal anchorage capacity of the rock under 'static' conditions they exhibit a decay of load through adjustments and slippage at the bolt anchor. Since bolts are quite often found with the plate hanging loose from the rock surface, this condition suggests that some additional mechanism may have played a part in loosening the anchorage. Vibration from blasting or shock loading have been suggested as one cause in this type of anchorage deterioration. This paper gives the results of an investigation carried on at the University of Missouri at Rolla to determine the influence of shock waves on rock-bolt anchorage stability. ROCK BOLT ANCHORAGE UNDER DYNAMIC LOADING CONDITIONS In this report dynamic loading conditions are defined as conditions under which rock and bolts are exposed to vibrations occurring as a consequence of blasting, machine vibrations, earthquakes, rock bursts, etc. Whatever the location of the shock source, the waves created suffer extensive alterations along their travel paths, depending upon the vibrational properties and geometric parameters of the transmitting media. Together with reflection, refraction and diffraction at material boundaries, waves suffer changes in their nature to form tensile, compressive and shear waves. They become polarized, retracted, accelerated, dispersed, so that the waves incident at a point in the material can be the result of either one or a combination of this wide range of processes. A certain fraction of the wave energy will be lost due to friction, deformation, and material failure at the anchor-rock contact. Thus, the physical nature of wave propagation is such that it inhibits an exact analytical solution. For this reason this investigation should be considered qualitative rather than quantitative even though numerical data have been used as a base. CONCEPT OF THE INVESTIGATION Experiments were designed to find, from a series of rock bolts installed in natural mine rock, whether or not, and to what extent, bolt tensions would be influenced when bolts were exposed repeatedly to shock waves such as those produced by blasting. Electronic instrumentation available in the rock mechanics laboratory of the University of Missouri at Rolla was used to observe wave development in the rock and vibrational reactions in the bolts. EXPERIMENTAL PROCEDURE Fig. 1 illustrates schematically the experimental equipment. Electric resistance wire strain gages were used as sensors for the strain response of the rock and the bolts. Bolts were 5 ft long and 5/8 in. in diam, equipped with two-leaf type expansion shells for 1 3/8 in. boreholes. The bolt gages were mounted by use of Du Pont Household Cement, covered with an epoxy insulation and then enclosed in a copper foil for electronic shielding. For details of placement and the wiring diagram see Fig. 2 and 3. The output of both the rock gages and the bolt gages was fed into cathode ray oscilloscopes from which the vibrational traces could be photographed. A static strain indicator was also used to read the output of all gages.

Jan 1, 1968

By L. R. Plitt, E. O. Lilge

Tests carried out with both kaolin and silica slurries show that flocculants of the polyacrylamide type can be used to improve the thickening performance of hydrocyclones. This thickening improvement demonstrates that contrary to previously held theories, flocs can be formed which are capable of resisting the shear forces in a hydrocyclone. For the 1.25-in.-diam cyclone used, optimum thickening occurs when the flocculant solution is injected into the slurry stream at or near the feed inlet. Hydrocyclones offer many distinct advantages over gravity thickeners. These advantages include simplicity, low initial and operating costs, small space requirements, and flexibility of operation. In spite of these advantages hydrocyclones have not been widely used as thickeners. The main reason for their lack of application is that hydrocyclones are unable to efficiently remove semicolloidal particles (less than 5 microns) from the suspending solution. In gravity thickeners, the fine particles can be induced to form particle aggregates, or flocs, which have the settling characteristics of large particles. In the hydrocyclone, however, it was always assumed that the existence of shear would prevent the formation of flocs.1-3 Thus, if no floc structure is retained, the thickening hydrocyclone must be designed so that its separation size is below the size of the smallest particle to be recovered. To obtain a very small separation size requires the formation of very high centrifugal forces, which necessitates the use of small-diameter cyclones. Small hydrocyclones have, in turn, very low throughput capacities which render them impractical for many industrial thickening applications. Thus, if the effects of flocculation cannot be utilized, the usefulness of hydrocyclones as thickeners remains limited to pulps which contain no very fine particles. It is well established that most substances acquire a surface electric charge when brought into contact with an aqueous medium. The repulsive interactions between similarly charged particles act to prevent flocculation. One method of flocculating a dispersion is to neutralize the repulsive surface charges by the addition of an electrolyte. The reduction of the electrostatic surface charge (Zeta potential) then permits the universal van der Waals attractive forces to operate between the atoms of the various particles and form particle aggregates. The lime additions used by thickener operators promotes flocculation by this mechanism. A second method of flocculating a dispersion is by the addition of long-chain macromolecules. In this case flocculation is brought about by a bridging mechanism in which the molecules are adsorbed with part of their length on two or more particles, thus forming a molecular bridge between the particles.4,5 The molecules also form bridges between themselves when a single particle is bonded to several polymer molecules. The type of bonding between the flocculant molecule and the particle may be hydrogen bonding, chemical bonding, or electrolytic attraction.6 The flour and glue which are used as thickener additives are believed to promote flocculation in this manner. In the past decade synthetic long-chain polymers with extremely high flocculating capabilities have been developed. The flocs formed by these new polymeric flocculants are larger and more shear-resistant than those formed by the presence of electrolytes.7 The advent of these flocculants raises the question: Are the flocs formed by these synthetic polymers stable enough to resist the liquid shearing forces in a hydrocyclone? The investigations reported in this paper were carried out in order to provide some answers to this question. EXPERIMENTAL WORK For the bulk of the test work a 5% slurry of commercially available kaolin with an average particle size of 5 microns was used. An initial evaluation of the available flocculants was carried out to determine which flocculant formed the most shear-resistant flocs. A combination of the techniques used by Healy7 and Booth8 was used for this purpose. This initial study revealed that the neutral high-molecular weight polyacrylamides produced the most shear-resistant flocs. One of these flocculants, Separan MGL*, was selected and then used for all the hydrocyclone tests. The flocculant was dissolved in water and added to the hydrocyclone as a dilute solution.

Jan 1, 1968

By D. C. Seidel, E. F. Fitzhugh

The cementation of nickel from acidic solutions by metallic iron is discussed. The cementation is carried out in pressure vessels at temperatures above 100°C. The results from bench scale studies on variables such as retention time, temperature, and solution pH are presented. A continuous processing flowsheet is proposed. Cementation is one of the oldest known hydrometal-lurgical reactions. The cementation of copper on iron was recorded by 'Paracelsus the Great' in about 1500,1 and by 1600 the technique was being used to recover copper at the Rio Tinto operations in Spain.2 At least one early author felt that cementation may have been one of the primary reasons for the alchemists' belief in the transmutation of metals.' The early writings state that when iron was placed in the clear waters from some mountain springs, the iron disappears and copper is found in its place. To the alchemists this may well have been one of the most convincing proofs that transmutation could and did occur. Since these early times the recovery of copper from acidic solutions by cementation has been practiced in plants throughout the world. Probably the cementation technique in some form has been common to more copper mining and milling operations than any other single recovery process. During current hydrometallurgical extraction studies, which were sponsored by the Republic Steel Corp. at the Colorado School of Mines Research Foundation, Inc., it was found that under the proper conditions, metallic nickel could be cemented from acidic solutions by powdered iron. The reactions are apparently similar to those that occur during the cementation of copper, but the nickel cementation had not been anticipated because iron and nickel are nearly adjacent in the electromotive series. The potential difference between iron and copper is approximately 0.78 v, while the potential difference between iron and nickel is less than 0.21 v. The cementation of nickel with iron at room temperature is almost negligible, but when the reaction is carried out in a closed vessel at temperatures in excess of 100°C, the nickel can be cemented almost quantitatively. The part played by this discovery in a practical method of nickel recovery is set forth in a separate paper.3 The following paragraphs are a discussion of experimental studies that were made to investigate this cementation reaction. The technique has been designated the HTC or High Temperature Cementation procedure. The cementation work was part of a study on hydrometallurgical techniques for the extraction of nickel from the garnierite or silicate type nickel ores. A hydrothermal extraction procedure had been developed, and this technique produced an acidic pulp or solution that contained both nickel and appreciable amounts of magnesium.3 Small quantities of ferric and ferrous iron were also present along with cobalt, manganese, and chromium. The potential for recovering the nickel from these acidic solutions by ion exchange or solvent extraction did not appear to be promising because of the relatively high magnesium content. The Ni ++ and Mg++ have nearly identical ionic dimensions and tend to be co-absorbed or extracted during ion exchange or solvent extraction treatments. Preliminary tests indicated that the nickel could be precipitated as a sulfide when using the high pressure H2S precipitation technique developed for the Moa Bay operations of the Freeport Nickel CO.4 This technique gave good recoveries, but the nickel sulfide product requires considerable additional processing before a marketable form of nickel is realized. The process also requires clarified feed solutions, and the solids-liquid separations on the garnierite residues are difficult. A program was initiated to investigate alternate procedures that might shorten the route to a marketable nickel product, and hopefully also permit bypassing the difficult solids-liquid separation steps required for the H2S precipitation technique. It was during these studies that the nickel cementation reaction with iron was encountered. EXPERIMENTAL EQUIPMENT AND PROCEDURES The bench scale precipitation tests which were conducted during this experimental program were made in 2-liter stirred autoclaves.* A photograph showing the form and arrangement of the autoclave

Jan 1, 1968