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By L. Weyher, H. L. Lovell

This discussion is restricted to a very specific application of the cyclone - its use as a hydro-cyclone in the cleaning of fine coal. It is hoped that the development of the present data will assist in the further elucidation of existing qualitative models, and also in an enhanced application of the hydrocyclone and provide a base for further research. Discussed are the mechanisms of gravity separation in hydro-cyclones, test procedures, experimental observations, and industrial applications from these studies. Within the general area of unit operations, a considerable effort has been expended in theoretical and empirical research associated with cyclone operations. The motivation involves the industrial requirement for devices and techniques to manipulate small particles at low operating costs, a situation required in coal preparation. There are good reasons why the cyclone helps to satisfy this demand, because it combines operational simplicity (no moving parts) with versatility and high throughput capacity per unit area. The cyclone is one of the most widely applied tools in the process technologies. There are areas for potential cyclone application which have been only meagerly explored or not considered at all. This discussion is restricted to a very specific application of the cyclone - its use as a hydrocyclone in the cleaning of fine coal. It represents an initial presentation of a more comprehensive report. Coal preparation can appropriately claim the hydrocyclone since most of its predominant industrial uses have originated in this area and have spread into other applications, including the broad field of ore dressing, the petroleum industry, chemical processing, nuclear engineering and food technology. There is one operational principle common in all cyclones: A fluid is tangentially introduced into a cylindrical or conical container under pressure. A predominantly irrotational flow field1 is established within the cyclone (Fig. 1). The uniqueness of this flow is indicated by the variation in tangential velocity across the cyclone radius, which reaches a maximum a short distance from the center and decays toward the cyclone wall. In contrast, the tangential velocity in a centrifuge increases uniformly toward the wall. Usually two products are discharged from the cyclone. They differ in that one discharge consists predominantly of that portion of the feed fluid which moves along the wall axially away from the feed inlet, while the other consists predominantly of fluid spiralling along the central regions of the cyclone, in an axial direction opposite to that of the wall current. Fig. 2 indicates these discharge points schematically. The latter product may be termed the vortex-product, since it is discharged with the central vortex-current. In the case of conical cyclones, the former product may be referred to as the apex-product. Although the names "over- and underflow" are widely used, many cyclones are operated from extreme angular positions thus the proposed terms are less ambiguous. The cyclone feed fluid can be laden with solid particles or nonmiscible fluid drops. Such a feed component is discharged from the cyclone, after some residence time, into the one or the other product. Yet, the orifice through which a particle will leave the cyclone is dependent upon a number of factors. These factors, in a statistical sense, determine the path of the particle within the cyclone. Thus, different separation phenomena are possible and different process results attainable by the controllable variation of the particle path. It is then, to attain a fuller understanding of this particle path, to which this study is ultimately directed. It is anticipated that the detailed study of the data being developed will allow further elucidation of existing qualitative models. However, the development of a quantitative description of cyclone operation in terms of a mechanism is not currently feasible. The flow conditions in a cyclone are not fully understood even for a pure fluid, without the added complexity of the inclusion of multiple size-density particles. It is hoped that the development of the present data will also assist in an enhanced application of the hydro-cyclone and provide a base for further research. Some practical applications drawn from the data are suggested. Cyclone operations have been classified according

Jan 1, 1967

By A. Vifian, I. lwasaki

Several samples of copper-nickel ore from the Duluth Gabbro were studied to relate their mineral-ogical characteristics with their amenability to concentration by flotation. The most common rocks in the samples were norites, gabbros, and troctolites. The texture of the rocks varied from coarse pegma-titic to very fine. The copper contents ranged from 0.2-0.7% and the nickel contents from 0.07-0.15%. The ore minerals were chalcopyrite, cubanite, pyrrhotite, and pentlandite. Most of the ore minerals occurred in interstices between laths of plagioclase, but some were included in the gangue grains. The samples responded readily to xanthate flotation. After a 65 to 100-mesh grind about 95% of the copper and 85% of the nickel were recovered in a bulk sulfide concentrate. Such recoveries remained constant even with grinds as fine as 270 mesh due to the extremely fine inclusions of sulfides in the silicate gangue. A finer grind than 270 mesh was necessary to free the copper-iron sulfides from the nickel-iron sulfides. A combination of time and British gum* was quite effective in producing concentrates analyzing 25-30% copper. The nickel concentrate averaged 1.5% nickel. Most of the nickel lost in the tailing was present as un-liberated sulfides and not as nickel in the olivine structure. The nickel content of the olivine was only about 0.05 or 0.08%. Western world nickel usage in 1967 is expected to be the second highest on record, amounting to 825 million lb. Despite a rise in mine production, however, demand is expected to exceed supply in 1968. ' Hence, exploration, development, and production expansion projects are being accelerated on a world scale. In Minnesota the copper-nickel bearing Duluth Gabbro is receiving much attention. During the past year 11 companies have been granted leases in the region, and the 1967 Minnesota legislature enacted a tax law designed to encourage the development of a copper-nickel industry. Although it is only during the past few years that mining companies have shown an active interest in the Minnesota copper-nickel deposit, copper-nickel minerals have been known to exist in northeastern Minnesota since 1899.3 At the 28th Mining Symposium, Dr. P. K. Sims, from the Geological Survey of Minnesota, gave a review of copper-nickel exploration in northeastern Minnesota,4 in which he emphasized that the potential of the Duluth Gabbro complex is large. Tests on samples from the Kawishiwi River area were reported by the United States Bureau of Mines in 1955.' In 1964, the Mines Experiment Station described tests on samples from the Gunflint Trail: and in 1966 the Minnesota Geological Survey published a geological map of the Gabbro Lake Quadrangle. The Mines Experiment Station published a study of the concentration of a Minnesota copper-nickel ore in 1967.7 The present paper is divided into three parts. The first describes the mineralogy of some rock samples from the Kawishiwi River area of northeastern Minnesota; the second summarizes the results of numerous flotation tests that were made on the samples, and the third explains the loss of nickel in the flotation tailing. MINERALOGY OF KAWlSHlWl ROCKS Recently five samples of mineralized gabbro from the Kawishiwi River area, a few miles east of Ely, were received at the Mines Experiment Station. One of the samples was a 175-lb composite, which was designated Ore 1556. The other four samples were 7-lb grab samples that had been obtained from four different exploration pits. They were designated Ore 1626, Lots 1 through 4. Basic Mineralogy: Many authors have reported that the rocks of the so-called gabbro of the Duluth Intrusion vary widely in composition.8-9 The samples on which our studies were based also contained a wide range of rocks. A gabbro, olivine-gabbro, anorthosite-gabbro, norite, and a troctolite were represented. The essential minerals in the samples were plagio-clase, pyroxene, and olivine, in variable proportions.

Jan 1, 1969

By Walter Craft, John L. Lamont

Adequate hardenability has long been recognized as one of the first requirements for producing desired mechanical properties in a heat-treated steel. Since the introduction of the Jominy end-quench test' and the development of correlative information to expand its use, industry has had an effective measure of hardenability. Prediction and control of the hardenability have been made possible by Grossmann's principle2 for calculating hardenability from chemical composition; and Field's conversiona from depth of half-martensite hardening to Rockwell C hardness has made the relation more quantitative. These developments have facilitated the design of new steels and the control of standard grades to the extent that it has been possible to establish tentative hardenability bands for some of the more commonly used alloy steels.4 As the depth of hardening of the Jominy test specimen is usually measured by Rockwell C hardness, it was considered that it should be possible to predict the hardness by a more direct calculation. It has been found that this can be accomplished by the addition of Rockwell C units proportional to the carbon and alloy content, grain size, and position in the Jominy test specimen. The calculation has been found to be fairly accurate, and because of its additive character is relatively simple to use. In principle the method of calculation is somewhat similar to the expressions developed by Herty, McBride, and Hollen-back,5 Burns, Moore, and Archer,= and Burns and Riege1.l The calculation is started from a base that includes the effects of carbon content and position in the Jominy test speimen. Rockwell C units are added to the base in proportion to the alloy content and grain size. This sum represents the Rockwell C hardness up to the level at which a disproportionate increase of hardness is caused by the formation of martensite, and above this level an increment for martensite hardening is added. The effects of alloys are directly proportional to the amounts present and are independent of each other, the carbon content, and the position in the specimen. Furthermore, the factors for determining the martensite increment are dependcnt only on carbon content and are independent of cooling rate and alloy content. It is this absence of interrelation between the different factors that makes it possible to calculate the hardness and makes the method of calculation consistent with the principle that the character of the hardening reaction is governed primarily by carbon and that alloys exert their effect chiefly through control of the critical cooling rate. The principle of the calculation, and the effects of alloys on the critical cooling rate,

Jan 1, 1947

By John L. Lamont, Walter Craft

Adequate hardenability has long been recognized as one of the first requirements for producing desired mechanical properties in a heat-treated steel. Since the introduction of the Jominy end-quench test' and the development of correlative information to expand its use, industry has had an effective measure of hardenability. Prediction and control of the hardenability have been made possible by Grossmann's principle2 for calculating hardenability from chemical composition; and Field's conversiona from depth of half-martensite hardening to Rockwell C hardness has made the relation more quantitative. These developments have facilitated the design of new steels and the control of standard grades to the extent that it has been possible to establish tentative hardenability bands for some of the more commonly used alloy steels.4 As the depth of hardening of the Jominy test specimen is usually measured by Rockwell C hardness, it was considered that it should be possible to predict the hardness by a more direct calculation. It has been found that this can be accomplished by the addition of Rockwell C units proportional to the carbon and alloy content, grain size, and position in the Jominy test specimen. The calculation has been found to be fairly accurate, and because of its additive character is relatively simple to use. In principle the method of calculation is somewhat similar to the expressions developed by Herty, McBride, and Hollen-back,5 Burns, Moore, and Archer,= and Burns and Riege1.l The calculation is started from a base that includes the effects of carbon content and position in the Jominy test speimen. Rockwell C units are added to the base in proportion to the alloy content and grain size. This sum represents the Rockwell C hardness up to the level at which a disproportionate increase of hardness is caused by the formation of martensite, and above this level an increment for martensite hardening is added. The effects of alloys are directly proportional to the amounts present and are independent of each other, the carbon content, and the position in the specimen. Furthermore, the factors for determining the martensite increment are dependcnt only on carbon content and are independent of cooling rate and alloy content. It is this absence of interrelation between the different factors that makes it possible to calculate the hardness and makes the method of calculation consistent with the principle that the character of the hardening reaction is governed primarily by carbon and that alloys exert their effect chiefly through control of the critical cooling rate. The principle of the calculation, and the effects of alloys on the critical cooling rate,

Jan 1, 1947

By Robert W. Metcalf

THE name "tripoli" is used to designate a number of more or less similar types of silica of sedimentary origin. Usually they are spoken of as "soft" silicas, and are light, very fine grained, porous, and friable. Structure is microcrystalline or cryptocrystalline. The deposits are the residual product of weathering and occur in massive form, either blocky or in friable masses. Tripoli is the end product of the weathering of siliceous Limestones, cherty limestones, or cherts. Weathering removes the calcium carbon- ate, leaving a finely divided siliceous residue to which the name "tripoli" has been applied. Authorities differ as to whether the chert accumulates first and is converted into tripoli or the tripoli is derived by direct decay from various forms of silica during initial weathering of the Limestone. It has also been asserted that tripolis were formed in situ in essentially their present condition as a flocculent, colloidal silica, but it is now believed by most geologists that varying degrees of pressure, combined with one or more methods of origin, have influenced the characteristics of the deposits. Considerable confusion has existed as to what constitutes tripoli. Owing to the similarity of names, tripolite, a type of diatomaceous earth found originally in Tripoli in northern Africa, has been erroneously called tripoli. Tripoli, however, contains no diatoms, the distinguishing characteristic of diatomaceous earth. The material mined in the Missouri-Oklahoma area has been considered by the trade to be the type material, and many feel that the term "tripoli" should more properly be restricted to the product of this region. Although also designated as soft silica, it would be less misleading, perhaps, if the siliceous material mined in southern Illinois were called amorphous silica. Both the Missouri-Oklahoma and Illinois materials are very high in silica. Different in composition, as it is very much lower in silica content than tripoli or amorphous silica, yet included under the classification of tripoli in Bureau of Mines statistical data, is the small but important output of rottenstone in Lycoming County, Pennsylvania. The principal justification for grouping these three types of silica is similarity of use.

Jan 1, 1949

By Frank E. Hauser, Philip R. Landon, John E. Dorn

The flow and fracture strengths of polycrystalline aggregates of high purity magnesium and a solid solution of aluminum in magnesium were determined as functions of temperature and grain size. Magnesium was found to obey two distinct fracture laws. Over the high temperature range, the fracture stress decreased with increasing test temperatures in a manner that closely paralleled the flow stress-temperature relationship. However, over the low temperature range, the fracture stress was independent of the test temperature though highly dependent on grain size, following the trend that is typical for the low temperature brittle fracturing of polycrystalline aggregates of body-centered-cubic and close-packed-hexagonal metals. Even at 78°K, however, plastic strains of 1 to 7 pet were obtained preceding onset of brittle fracturing. Over the brittle fracture range of temperatures, the fracture stress increased linearly with the reciprocal of the square root of the mean grain diameter, while over the entire range of temperatures investigated, the flow strength was observed to increase linearly with the reciprocal of the square root of the mean grain diameter. PREVIOUS investigations', 'have shown that deformation of coarse grained aggregates of high purity magnesium is interrupted by fracturing at very small strains. Such tendency toward brittle fracturing increased with increasing grain size and decreasing test temperature. In several respects, however, low temperature fracturing of magnesium appeared to differ from the truly brittle type exhibited by zinc, molybdenum, tungsten, and iron, so often characterized as a cleavage mode of fracturing. The absence of a well-defined cleavage mechanism for fracturing and the fact that some plastic deformation precedes fracturing might suggest that magnesium does not exhibit the same kind of brittle fracturing that is common to body-centered-cubic metals and to other close-packed-hexagonal metals. But, as will be shown, the low temperature fracture laws for magnesium are analogous to those that apply to iron, molybdenum, tungsten, and zinc in spite of differences in mechanisms and in plastic strains to fracture. In view of these observations. the low temperature fracturing of magnesium will also be called brittle fracturing. This, of course, does not imply that the brittle fracturing of metals is synonymous with the brittle fracturing of glass or other nonmetallics. Whereas the brittle fracturing of glass probably obeys Griffith's law, the low temperature brittle fracturing of metals arises from stresses induced by a series of dislocations piled up at an opaque grain boundary. Experimental Results All tests were made on tensile bars having gage sections that were 2 in. long and 0.375 or 0.25 in. wide. In order to develop a series of grain sizes, the

Jan 1, 1957

By A. A. Rauth

In this paper, the author derives a series of formulas from basic principles and illustrates the application of these formulas to practical grinding charge problems. The paper establishes the nearly proportional relationship of mill power to charge level and shows how this relationship can be used to advantage in the design, manufacture and operation of grinding mills. The procedures outlined offer a rapid means of anticipating the power requirements for a given charge or determining makeup charges for a given power reading. The theories which have been developed concerning the dynamics of grinding have been motivated largely by the desire to derive workable formulas for the accurate determination of grinding mill power. This accurate determination has always been handicapped by the large number of variables to be considered, some of which are mill diameter, length, speed, liner design, grinding charge and material density, volumetric mill loading, internal friction, and charge size and gradation. In efforts to determine mill power, attempts have been made to utilize torque concepts. The formulas derived consider the grinding mass as a rigid body and utilize factors that are based on empirical data so that the movement of the charge within the mill is compensated for. These formulas are of principal interest to the mill designer since he is charged with the responsibility of analyzing all of the variables and from them predicting a mill size and a motor size which are compatible both with each other and with the grinding job for which they were intended. The mill operator, on the other hand, has an entirely different problem. The mill dimensions are already established and so is the driving motor. The operator's main concern is to obtain maximum performance from the mill he already has. For him, the many variables which perplex the mill designer are fixed values. Mill diameter, length and speed are set and, to a large extent, so are the conditions inside the mill from which the torque formula advocates derive their empirical data. It is conceivable that if the major mill dimensions which affect power demand are held constant, and if the variables influencing empirical factors are held fairly constant, as they are in an operating mill, then the only major variable remaining which affects power is the level of the charge itself. Under this condition.

Jan 1, 1970

By C. L. Mantell

ALTHOUGH SO common and well known a metal, tin is really a less abundant element than many of those less familiar and usually ranked with the scarce or rare elements, such as cerium, yttrium, lithium, beryllium., titanium, zirconium and vanadium. The color of tin is white, with a slightly bluish tinge. When it is compared with nickel, the latter metal is brown. When placed alongside of tin, chromium is definitely blue. Tin is whiter than silver or zinc. Exceedingly thin films of tin show various shades of brown by transmitted light. The metal has a brilliant luster, and when mirror-polished, has high light reflectivity. The luster depends to a large extent upon the pouring temperature at which the metal is cast. If the temperature be, too high, iridescent colors may show on the surface. These are the result of oxide film formation. If the pouring temperature be too low, the surface is dull. Small amounts of foreign metals, such as lead, arsenic, antimony and iron, decrease the luster of tin and impart a yellowish tinge to the metal. The structure is decidedly crystalline. The cast metal is a mass of crystals. When a bar of tin is bent, it emits a characteristic creaking sound. This is called the "cry" of tin, resulting from the grinding of the crystals one against the other during the bending of the metal. Tin metal may lose its crystalline structure by cold working, but grain growth occurs rapidly under the influence of heat. Metal which has been cast at a low temperature may become amorphous as the result of mechanical work. If such material be heated to temperatures well. below the melting point, say at 110° C. for a half hour or for a few minutes at 150° C. recrystallization occurs. If the surface of tinned plate, tin foil, or tin metal in cast form be etched with hydrochloric acid containing a little free chlorine, attack occurs at the intercrystalline faces. The surface shows patterns resembling the frost flowers on window panes in winter. The etched appearance is called moiré metallique. Fine dendritic surface crystals of tin may be obtained by casting the metal on a surface of polished steel. In commercial tin plate, the intercrystalline boundaries are shown by fine grooves or channels, which result from the method

Jan 1, 1929

By M. G. Corson

Information regarding the use of ixanganese alloys has hitherto been incomplete and available only from widely scattered sources. This paper attempts a systematic description of properties and uses of alloys other than manganese bronze, manganin and duralumin, which are probably the only non-ferrous alloys associated with manganese in the minds of most metallurgists. Properties of Manganese Manganese can react either acid or basic; it is hard to obtain in the pure state; it has two different crystalline lattice structures, both of the cubic system, one stable above 850" C. and the other below 650" C., both coexisting in the intermediate range. Although the commercial product is hard and brittle, the pure metal seems to be ductile. In fact Zhemchuzhny, in Russia, was able to obtain ductile manganese and draw it to fine wires by the simple expedient of adding about 3 per cent. copper to the alumino-thermic product. Copper most probably brings the sili-cides, aluminides, nitrides and carbides present in the commercial product into a much less harmful form of distribution. One industrial use that can be foreseen for wrought manganese articles is as anodes for electrolytic processes in sulfate and nitrate solutions, particularly with high voltages. A practically insoluble skin of manganese peroxide is likely to form in such cases and an insoluble and strong anode material will be available. Manganese as a Scavengek Because of its activity manganese might become the most efficient scavenger and refiner of copper, were it not for the fact that 0.01 per cent.

By Forrest K. Pence

BENTONITE deposits are known to occur in Texas within the Jackson group of formations. This group represents the uppermost Eocene age sediments found in the coastal plain area of Texas. It outcrops across this area of the state in a narrow band of some 4 to 20 miles width. The outcrop pattern roughly parallels the present Gulf of Mexico shore line and is some 100 miles inland from the Texas shore, Fig 1. The principal bentonite deposits are found in the areas where this outcrop pattern cuts across the south-central Texas counties of Karnes, Gonzales, and Fayette. In these deposits, the better quality bentonite is found in the lower or bottom layers of the volcanic ash deposits in which they occur. Some of these better quality bentonites develop very light colors upon firing and therefore justify their being classified as "white firing." The deposits in Karnes and Gonzales Counties apparently occur in commercial quantity, whereas the white firing strata so far uncovered in Fayette County have been too thin to be classified as yet as "commercial." A study of the ceramic properties of the weathered ash in Gonzales and Karnes Counties was reported in 1941.1

Jan 1, 1949

By G. K. Burgess

THE question of the allotropy of iron, in spite of a vast amount of experimental work and perhaps an even greater amount of theorizing, is not yet settled. That there is a definite transformation in iron near 900,° the A3 point, is generally recognized, as well as the fact that the temperature of this transformation is lowered by the addition of carbon and metallic elements. On heating, the transformation Ac3 is always found at a higher temperature than the transformation on cooling, Ar3. Whether the A3 transformation is sharp like the melting point of a pure substance, or extends over a considerable range of temperatures, embracing perhaps as a lower limit the A2 change, appears to be still an open question for pure iron. The nature and identity of the A2 transformation, it would appear from recent publications, has not yet been satisfactorily settled. In the present paper a critical, historical summary is given of the experimental investigations of the location of A2 and A.3 in pure iron, together with brief mention of some of the theoretical aspects of the subject, and an account is given of a series ?of experiments carried out with several samples of very pure iron which were studied by two methods of thermal analysis in the range from 5000 C. to 1,000° C., and which it is believed furnish a contribution of considerable interest as to the location and nature of the A3 and A2 transformations. Great attention has been given to the details of experimental manipulation and to the preparation of the samples, as it was soon found that some of the discrepancies noted in the work of many experimenters may be traced largely to lack of precautions which we have found essential. For example, to anticipate somewhat, it is necessary to provide a suitable practically gas-free furnace, the heating and cooling of which may be regulated to a nicety. To render a minimum the deforming effects on the cooling and heating curves of the poor conduction of the sample, it must be of a form and mass to pass on its heat rapidly and completely to the thermocouple; and finally the sample itself must be freed from gases which, if present, further mask the definiteness of the heating and cooling curves. We, have also varied within wide limits the several factors which may influence the determination of the exact location and shape of the transformation ranges, especially the mass and preparation of sample, rate of heating and cooling, design of furnace; and finally, as nearly as it is experimentally possible, we have worked with a substance approaching pure iron, free from occluded gases and other impurities, and contained within a vacuum.

Jan 10, 1913

By Donald E. Crowell

Due to falling metal prices and depletion of ore reserves, lead- zinc mining in the Leadville, Colo., area gradually came to a halt in the 1950's. Exploration work continued, however, and by 1969 sufficient ore had been blocked out to warrant sinking a shaft and erecting a new concentrator to treat 700 tpd. The new shaft and concentrator were to be located in Iowa Gulch several miles east of Leadville at an elevation of 11,100 ft. The Leadville project is a joint venture between Newmont Mining Co. and Asarco, with Asarco being the operator. Design work began in the fall of 1969. Engineering was done by Torkelson Engineering Co. of Salt Lake City in conjunction with the central engineering department of Asarco. The plant was constructed by Stearns-Roger Corp. Construction began in the spring of 1970 and the plant went onstream in April 1971.

Jan 11, 1972

By M. C. Udy, C. H. Lorig

THROUGH the years much interest has been centered in attempting to develop a direct method of iron-ore reduction, to replace or supplement the present indirect blast-furnace process. It would not be difficult to produce a list of more than 500 patents dealing with the direct production of iron and steel, but the few of this type of process that have proved successful do not produce in competition with the blast furnace; they produce special products. A survey of the literature reveals that the equilibrium conditions for the reduction reactions (iron oxides with carbon monoxide and with hydrogen) have been fairly well established but that data on the rate of reaction are discordant, although the general effects of the variables are known. This dissertation deals with the rate of reduction of a magnetite concentrate with hydrogen. The following variables have been studied: bed depth, gas velocity, particle size and temperature. The behavior of a single particle was also studied. LITERATURE Two general factors should he considered in a study of reduction of iron oxide: (1) equilibrium relations, and (2) rate of reaction. The first factor, equilibrium, has received the attention of many investigators and the equilibria Fe3O4-FeO-H2-H2O, Fe304-FeO-CO-CO2, FeO-Fe-H2-H2O, FeO-Fe-CO-CO2 are fairly well established. Of the second factor, the rate of reaction, much less is known. Data are comparatively scarce and there is very little concordance. The discordance probably results from the large number of variables influencing the reactions. However, the general effect of the variables is known. Among these variables are temperature, gas velocity, particle size, porosity, gas composition (distance from equilibrium), presence of impurities, greater or less prevalence of side reactions, and even design of the apparatus itself. Wetherill and Furnas1 published an excellent paper in 1934. They point out that any one or more of five processes (the chemical reaction, diffusion of the reactant through the gas film, diffusion of the reactant through the solid phase, diffusion of the reaction product through the solid phase, or diffusion of the reaction product through the gas film) may be the slow process, and thus the rate-controlling process. It is regretted that the work of these authors was limited to experiments at one temperature, and that the range of gas compositions was limited. Langmuir2 has shown that heterogeneous reactions take place at phase boundaries.

Jan 1, 1942

By G. Sachs, E. J. Ripling, S. I. Liu, J. J. Lynch

It is a generally recognized fact that by repeated straining the fracture stress of any metal is reduced to a fraction of its value for static loading. The value of this fatigue strength depends upon numerous factors, such as the states of strain and stress, the limits of straining, and the number of repeated loadings or cycles The large volume of previous investigations on fatigue is concerned entirely with large numbers of cycles, say exceeding 10,000 and up to 500,000,000. However, the changes in fracture stress and fracture strain occurring after a small number of repeated loadings have attracted little attention. Apparently the only investigations of this type are those byLudwik4.5 who subjected steel, copper, and aluminum wire to repeated torsion. In each test the torque was varied between identical values in the two directions of twisting. Depending upon the magnitude of the moment, fracturing occurred after a number of cycles, up to 10,000. The results of Ludwik's tests will be discussed later Such torsion does not readily yield actual stress and strain values. Therefore a pre- liminary study was made of the effects of repeated direct stresses, that is, tension and compression stresses. Because such tests are considerably more tedious than torsion tests, only high stresses were used in the preliminary work, yielding definite changes in metal properties after a few cycles. It was found in these tests that strains could be controlled more readily than stresses in the investigated range of high stresses. This paper, consequently, deals with the effects of strains of equal magnitude but different signs. The metal was first prestrained in static tension by a certain amount then subjected to compression to yield the same amount of strain after unloading. This loading cycle was repeated up to a maximum of seven times. After various cycles, the stress-strain curves in tension were determined, up to fracturing. As material for these tests, the aluniinum alloy 24ST was selected because it exhibits a comparatively small amount of necking in the tension rest This alloy permitted, therefore rather accurate cont.rol at the high strains necessary to produce fatigue failures at less than seven cycles. The results of this invest~gation appear sufliciently interesting to extend the method of attack in various directions It is intended to study (11 the effects of cycles up to a tew thousands and (2) the effects of strains of different magnitude in tension and compression respectively 'The latter variable also includes a. a special case the effects of compressive strains.

Jan 1, 1949

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

Unmodified disilicide coatirigs were applied to sheet-tensile specimens ofCb-Dg3 and Mo-TZM veJractovy- metal alloys. Coating thickness, degree of coating-substrate interdiffusion, and specimen geonzetry (notched and plain were included in the variables studied. Tensile tests were made to determine the ductile-lo-brittle transition temperature. The disilicide coating modestly increased the transition temperatlre of TZM, but had no effect on 043. Neither material condition (recrystallized or stress-velieved) nor specimen geometry (notched or unnotched) significantly altered the effects of coatings on the transilion temperatures of. the alloys. Cracks in the brittle coatings did not propagate into the substrate, and fracture modes appeared to be the same for both un-coated and coated specimens. MOST potential structural applications for refractory metals and alloys involve exposures to oxidizing environments at elevated temperatures. The general lack of oxidation resistance of these metals will require protective coatings to allow fulfillment of their potential. Currently preferred coatings for the oxidation protection of refractory metals are brittle intermetallic aluminides or silicides. These are typically formed on the surface of the refractory-metal substrate by a diffusion reaction between the substrate and a gaseous or liquid medium that is rich in aluminum or silicon. Because of the brittleness of these coatings, they will sustain no plastic deformation at low temperatures. They are frequently cracked by cooling from the coating temperature because of the thermal-expansion mismatch with the substrate alloy. Even if they survive cooling intact, they crack rather than sustain deformation under load at low temperatures. Thus, when a coated refractory metal is strained beyond the elastic limit of the coating at low temperatures, the mechanical environment of the substrate would include both static and dynamic cracks. These might be expected to influence the flow and fracture behavior of the substrate. This could be manifested in an altered fracture mode and/or an increase in the normal ductile-to-brittle transition temperature of the refractory-metal substrate. This paper presents the results of a research program that was conducted to determine the influence of the presence of a brittle surface coating on the low-strain-rate tensile behavior of typical refractory metals at low temperatures. EXPERIMENTAL PROCEDURES Material Preparation. Thirty-mil-thick sheets of molybdenum TZM alloy (Mo-0.5Ti-O.1Zr) and colum-bium D43 alloy (Cb-IOW-1Zr-O.1C) were obtained commercially. These alloys were selected as substrate materials representing two classes of materials important in current refractory-metal technology. The TZM was in the stress-relieved condition, and exhibited a heavily fibered grain structure. The D43 had been processed by the duPont "optimum" fabrication schedule,' and exhibited slightly elongated grains typical of this process. Tensile specimens of two geometries were prepared from these materials: 1) plain specimens with 0.2-in.-wide 1.0-in.-long gage sections; 2) specimens similar to above, but with a 0.06-in.-diam hole drilled in the center of the gage section, providing a stress concentration factor, Kt, of 2.5. The "notch" geometry was selected to represent a typical condition of a rivet hole or other geometric discontinuities as might be encountered in various applications. Machined specimens were degreased, with a final rinse in acetone, prior to the application of coatings. Specimens of each substrate and configuration were pack-siliconizedin a particulate mixture of 80 pct A1203, 17 pct Si, and 3 pct NaF. Specimens were embedded in this mix (contained in graphite retorts) and coated in an electrically heated argon-atmosphere furnace under time-temperature conditions to effect nominal 1- and 3-mil-thick silicide coatings: Coating Thickness, mils Thermal Treatment 0.6 to 1.4 24 hr at 982°C 2.4 to 3.2 48 hr at 1093°C Coating kinetics were similar for both the TZM and D43 substrates. These treatments had little or no visible effect on the substrate microstructure as determined by optical metallography. The coatings on TZM were essentially single-phase unmodified disilicides, while those on D43 showed substantial evidence of modification by proportionate reaction with the respective substrate elements or phases, as shown in Fig. 1. It was recognized that these coatings might not be particularly desirable regarding protective capability. However, it was desired to circumvent possible inter -ferring chemical interaction with the substrate by pack additives such as chromium, titanium, boron, aluminum, and other elements that typify the better protective coatings for these materials.' Thus, the results presented apply specifically to the simple silicide coatings investigated. They may not be rep-

Jan 1, 1967

By William A. Kapp

INTRODUCTION Coal is being mined from beneath residential areas, structures, bodies of water and other surface features in the coalfields to the north, south and west of Sydney. The particular problems faced by mine operators in these areas vary considerably due to differences in the overlying strata, the variation in the depths of cover and also depend on the number of seams being mined. Detailed subsidence work first commenced in the Southern Coalfield in 1965 and is now being carried out over areas of extraction at roost collieries. The analysis of the results of the early investigations and of the work which continues in other areas has shown that there is a consistent relationship between subsidence and mine geometry and has led to a reliable empirical method for the prediction of subsidence. In addition, particular aspects of each of the studies in the Southern Coalfield results in a clearer understanding of strata movements and of the resulting subsidence. The features of a subsidence trough apply generally to all areas but the magnitudes of specific features vary according to the stratigraphy of the particular coalfield. The aim of the subsidence work is to quantify the effects of subsidence for a range of mining geometries and mining conditions to enable the maximum safe recovery of coal from beneath surface features. The importance of local subsidence investigations is becoming more evident to mine operators and to authorities or organisations with surface interests. The subsidence work also provides important information on the stabilities of pillars of coal which remain unmined between panels of extracted coal. These pillars are not extracted either because of poor mining or geological conditions, or because pillar extraction is not part of the particular mining operation. Subsidence studies over these coal pillars clearly establish whether the pillars have remained stable or have failed to support the overlying strata. With subsidence studies continuing over several years, it is possible to assess the stabilities of these pillars on a long term basis. BACKGROUND TO THE STUDY OF SUBSIDENCE Geographical setting Most of the black coal production in Australia comes from the Sydney Basin. The coal seams extend for approximately 350 km along the coast of New South Wales and inland for distances up to 150 km. The City of Sydney is located near the centre of the coastal extent of the Basin where coal has been mined at a depth of 900 m. The Sydney Basin is part of the Main Coal Province of NSW and is divided into several coal- fields. The Southern Coalfield to the south of Sydney contained 15 operating mines and produced 12.7 million tonnes of raw coal during the 12 months to June 1981. The collieries discussed later are shown in Fig. 1. The prominent topographical feature of the area is the Illawarra Escarpment which rises to 400 m above sea level, or 300 m above the coastal strip along the South Pacific Ocean. The escarpment is mainly sand- stone and the weathering of the cliff line has resulted in a covering of talus material at its base. Several collieries are located near the seams which outcrop along the escarpment. The city of Wollongong is located in a scenically attractive area on the coastal plain. The suburbs of Wollongong extend north along the coastline, south to beyond Lake Illawarra and west to the lower slopes of the escarpment. The Illawarra Escarpment forms the eastern boundary of the Woronora Plateau. On a regional scale the surface dips gently to the west and thus forms a watershed for the rivers, most of which flow in a general north westerly direction, sometimes forming steep gorges in the sandstone. These rivers join the Nepean and Hawkesbury River system and flow into the Pacific Ocean north of Sydney. Seven dam have been constructed over the Southern Coalfield (Fig. 1) and with one large dam further to the west, their stored waters provide the needs of the Cities of Sydney and Wollongong and the surrounding districts. A large part of the area affected by mining is the undeveloped bushland of the associated catchment areas. In general no special precautions have been required with respect to subsidence with the exception of the dam structures and stored waters. With the increase in coal mining activities and the expanding residential development south of the City of Campbelltown in the outer Sydney Metropolitan area, subsidence is becoming an increasingly important area of research. Structures which have been affected or considered are townships and extensive residential areas, buildings of historical importance, major tollways, and a high pressure natural gas pipeline. The subsidence effects of mining beneath natural features within national parks is coming under study as mining approaches these areas. Geological setting The coal seams of the Southern Coalfield lie within the Illawarra Coal Measures. They contain high rank coking coal used in the local steel industry and for export. The Bulli Seam is mined extensively through- out the Southern Coalfield with the lower Wongawilli Seam being second in importance with regard to coal production. The top of the Bulli Seam is taken to be the marker horizon between the Permian Coal Measures

Jan 1, 1982

By F. A. Olson, J. S. Cho, M. E. Wadworth

An infrared study of the states of hydration of MgSO4 revealed a hitherto unreported metustable dehydration state in the temperature range just below that of the stable anhydrous salt. Infrared, thermogvavimetric, and X-ray studies indicated that the state had bisulfate and hydroxide characteristics. A formula fitting all of the experimental evidence is hydrogen-bonded Mg(OH)HSO4, or possibly the chemically equivalent 1/2 Mg(HSO4)2. Mg(OH)2 Infrared spectra of the 7, 6, 1, and OH2O states of hydration are given as well as the spectra of the newly found state which is called the bisulfate state in this paper. Thermogvavimetric studies as a function of water-vapor pressure gave an enthalpy value of 16 cal per mole, and 25 eu for the conversion of the bisulfate state to that of the anhydrous salt. The free energies of the transition varied from 1.76 to 0.18 kcal per mole as the transition temperature varied from 279° to 336°C. The bisulfate state is believed to be of importance in catalytic dehydration phenomena using MgSO4 and may be of interest because of properties in sulfating reactions differing from those of the monohydrate. Also, an analogous state may exist as a hydration state of other sulfates. ANHYDROUS magnesium sulfate is a catalyst with a high degree of specificity for the dehydration of secondary alcohols.1'2 The only product obtained at the usual operating temperature range of 360" to 400°C other than the corresponding olefin is water. Thus, the bonding of water to the anhydrous salt as well as an understanding of the hydration states of MgSO4 became of interest in attempting to understand the catalytic mechanism better. In the process of this study using infrared, X-ray, and thermogravimetric analyses a dehydration state not previously reported was found. Proof of its existence, the nature of the state, and its role, if any, in the catalytic mechanism then became of interest. This paper is concerned principally with the first two aspects of this problem. Magnesium sulfate forms many hydrates, of which the monohydrate and heptahydrate (Epsom salts)3 are most important. Other hydrates4 are known with 1-1/4,5 l-1/2, 5 2, 4, 5, 6, and 12 H2O's. The hydrates with 1-1/4, 1-1/2, 2, 4, and 5 HzO's are unstable. The anhydrous salt is very stable thermally and has a strong affinity for water. It can be heated without additional decomposition to about 800°C.' At 900°C noticeable decomposition takes

Jan 1, 1964

By Ralph W. M. Lai, D. W. Fuerstenau

This paper presents the results of a study of the principles which control the distribution of ultrafine particles between an oil phase and an aqueous phase. Alkyl sulfonates were used to control the wettability of fine alumina particles and to stabilize the water-isooctane emulsion system in the extraction process. The effects of sulfonate chain length, sulfonate adsorption, pH, and oil-water ratio on the recovery of solids in the oil phase were investigated. Higher extraction was found under conditions which yield higher hydrophobicity and large interfacial area of the oil-water emulsion. Today there is considerable interest in developing methods for the recovery of fine particles from disseminated ores. One such method might be the extraction of fine particulate solids from aqueous suspensions into an oil phase, and one example of a successful industrial process based on oil-water distribution phenomena is the emulsion flotation process used in concentrating manganese ore.' The oil agglomeration process of Farnand, Smith, and Puddington has been suggested for concentrating tin ore. Patents 3-4 for oil flotation processes extend back to that of William Haynes in 1860. The basis of all these processes is directly related to the stabilization of emulsions with solid particles. The first extensive study of oil-water emulsions stabilized by finely divided solids was made by Pickering. Later, Briggs,6 weston, 7 Chessman and King,8 and Leja and Schulman9 experimentally demonstrated how solid particles control water-oil and oil-water systems. Hildebrand10 suggested that fine particles can stabilize an emulsion because the fine particles are partially wettable by both oil and water, that is, that the contact angle must be finite. Takakuwa and Takamori 11 recently applied emulsion inversion to the study of collector adsorption in flotation systems. At the Royal School of Mines, Shergold and Mellgren12 are currently carrying out a comprehensive study of the extraction of fine particles into an organic liquid phase. In the present study of the liquid extraction or oil flotation of ultrafine particles, the recovery of hydro-philic alumina particles of 0.1-µ average diameter was determined after separating an isooctane-water mixture (emulsion) into its two phases. Alkyl sulfonates of different chain lengths were used to change the wettability of the alumina and to effect emulsifi-cation of the oil-water mixture. The effects of the oil-water volume ratio, sulfonate adsorption, and pH on the recovery of the fine particles were investigated. Since the surface charge on an oxide such as alumina is determined by the adsorption or interaction of H+ and OH- with the surface, pH control is extremely important. Furthermore, since the zero point of charge (zpc) of alumina13-14 occurs at pH 9 to 9.4, major adsorption effects with anionic collectors in these systems will occur below pH 9. The results of the foregoing investigation are discussed in terms of the recovery of the fine particles, the oil-water ratio, contact angles, surface tension, the adsorption of sulfonate onto the solid surface, and the emulsifica-tion of oil. MATERIALS AND EXPERIMENTAL METHODS Materials: The particulate solid used in all the experiments was Linde "A" alumina, a high-purity, readily available form of a-alumina. The surface area of the alumina, as evaluated from measurements of stearic acid adsorption from benzene, was 14.5 sq m per gm, based on a value of 20.5 sq Å for the cross-sectional area of stearic acid.13 All aqueous solutions were prepared from triply distilled conductivity water. Other materials included high-purity crystals of sodium alkyl sulfonates, isooctane, and, for pH adjustments, reagent grade hydrochloric acid and sodium hydroxide-Because sulfonic acids are strong acids, they are

Jan 1, 1969

By E. H. Jr. Dix

THE success of the Charpy impact test in the steel industry has led those interested in aluminum alloys to investigate the possible applica¬tion of this test to aluminum and its alloys. In this paper are set forth the results of a few preliminary tests made at the Lynite Laboratories of the Aluminum Manufactures, Inc. In order to study more thor-oughly the significance of the Charpy test, slow-bending tests have been made duplicating the arrangement of the impact machine. Tests have been made on both notched and unnotched specimens of a series of copper-aluminum alloys. APPARATUS The standard American-made Charpy impact machine delivering a blow of over 200 ft.-lb. was- much too large to test aluminum-alloy specimens of the same type used for steel, so that it was necessary either to adopt a larger specimen or to have a special light-weight hammer made. Since there is no known relation between specimens of different sizes, even though geometrically similar, it was decided to adhere to the 10 by 10 mm. specimen. Accordingly, Sauveur and Boylston, the American makers of the machine, were asked to construct a special light-weight pendulum adapted to their standard machine, this pendulum to have one-tenth the capacity of the standard. The writer wishes here to acknowledge his indebtedness to Mr. H. M. Boylston for the personal interest and care exercised in constructing this pendulum. The machine with, the light-weight hammer in place is shown in Fig. 1. It is mounted on a concrete foundation with the concrete covering the flange on the base of the machine. Vibration is further prevented by four 5/8 -in. (15.8 mm.) foundation bolts. The large standard hammer shown against the wall was also used for some of the unnotched bars that requited more than 20 ft.-lb. to rupture.

Jan 4, 1920

By John Wulff, David A. Stevenson

The rates of solution of copper, nickel, and three copper-nickel alloys in liquid lead were studied at 527° and 727°C under dynamic conditions. The relative velocity at the solid-liquid interface was varied from 8.65 to 125 cm per sec. Analysis of the data for the pure metals indicates that the solution rate is transport corztrolled at lower velocities, but a transition to mixed control occurs at higher velocities, higher temperatures, and higher percent saturation. 1 HE present work concerns the effect of relative velocity at a solid-liquid interface on the dissolution kinetics of pure solid materials in liquid metals. This general problem is of interest in electrode kinetics, in electrolytic processes, and more recently in the field of liquid metal corrosion. Considerable work has been done on dissolution kinetics in aqueous environments because of the obvious importance to electrolytic processes.1,2 In purely metallic systems investigation has been more limited. There are, of course, extensive data from loop tests which are used in an engineering evaluation of liq- uid metal corrosion. Here, however, the dissolution process is complicated by several interdependent processes. In general, one of two factors is considered to be rate limiting in the dissolution process: the transport of material from the solid-liquid interface into the bulk liquid, or an activation process directly at the interface. A number of studies of the dissolution rates of solid metals in liquid metals under static conditions have been published.3- Since the attendant hydrodynamic conditions imposed by thermal gradient convection and concentration gradient convection are difficult to analyze, it is doubtful if a clear interpretation of the experimental findings of these papers in terms of the mechanism involved in the dissolution process can be made. A clearer picture of the dissolution process is provided by

Jan 1, 1962