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By J. C. Febles

HISTORY. THE use of iron for the precipitation of copper was known at least as early as the fifteenth century. Both Paracelsus and Basil Valentine refer to it in their writings, as early as 1500 A. D. It was used in Peru, for this purpose prior to 1637, and at Rio Tinto, Spain, as early as the sixteenth century. The statement has been made repeatedly that in the early history of the mining industry at Butte, the practicability of this method of recovering copper from solution was overlooked, and that enormous quantities of copper-bearing water were allowed to go to waste, the copper in which might easily have been recovered at small cost; and that this oversight on the part of the mine operators was due to ignorance of this method of recovering copper. As a matter of fact, very little copper-bearing mineral was encountered in the mines of Butte until a depth of 400 or 500 ft. bad been reached, and in many cases much greater depths were necessary to reach the copper-bearing zone. The water encountered in the upper levels (although in most cases quite highly mineralized) contained little or no copper, and it was only after considerable areas of copper-bearing ore had been uncovered and developed that copper sulphate began to. appear in the mine water in any considerable quantity. In fact, the first water that was observed to contain copper carried it in such small amounts as to be of little or no importance. It was only after years of underground work had opened extensive areas of stopes, drifts, and other underground workings, these being subsequently filled with waste, nearly all of which contained small copper values, which became oxidized by exposure to the air and were acted upon by the slowly percolating mineral water, that the recovery of copper from mine water became commercially important.

Jan 7, 1913

By Hsun Hu, R. S. Cline

A detailed studj) of texture formation in 2 pet Al-Fe single crystals with initial orientations of approximately (111) [112], (112) [111], and (112) [111] was made by examining the textures developed on the surface and at various interior sections of the crystal after rolling to various amounts. Depending' upon the initial orientation of the crystal, the surface and interior textures may differ only in sharpness, or may differ essentially in orientation. The orientation of the (111) [112] crystal does not change upon rolling up to 70 pet, but after rolling more than 90 pet a distinct component of (001) (110] orientation is developed. The texture formed in the two (112) (1111 type crystals consists of (111) (1121 and (001) (1101 components. The latter, however, is largely confined to the surface layers. The textures formed on both sides of the crystal are identical, and the texture composition profile is approximately symmetrical with respect to the central section of the strip thickness. The formation of these texture components is analyzed. DURING the past seven or eight years, deformation and recrystallization textures in rolled Si-Fe single crystals have been extensively studied by various investigators.1-7 From these studies, much knowledge on texture formation in bee crystals of various initial orientations was obtained. However, these results also raised many questions, regarding particularly the correlation between deformation and recrystallization textures, as well as the deformation texture itself of some particular crystals. To take a (111) [112] type crystal as an example, it was shown by Dunn and Koh2, 3 that this orientation does not change during deformation by rolling. This finding is consistent with the conclusion reached by Barrett and Leven-son8 with respect to iron crystals that (111) [112] is one of the stable end orientations. However, different recrystallization textures were observed by Dunn and Koh3 in (111) [112] type crystals of different initial thickness, which widened differently during rolling even though their deformation textures were identical. Another interesting example, also from the results of Dunn and Koh2'3 is that of texture formation in a (112) [111] crystal. This crystal developed a two-component deformation texture of (111) [112] plus (001) [110]. Its recrystallization texture, however, was found to be predominantly (110) [001], which is related to the (111) [112] component by a simple [110] rotation. This crystal, therefore, behaved as if the other deformation texture component, (001) [110], were not present. There are also discrepancies among the results of different investigators, as well as numerous unexplained fine features of the deformation texture of crystals of various initial orientations. In order to have a better understanding of all of these points, a detailed study of deformation textures is greatly needed. One of the obvious things that has been completely overlooked in previous texture studies is the possible effect of surface texture. All past work on the texture of Si-Fe single crystals was conducted in a rather simple manner, i.e., the rolled crystals were etched to a very thin sheet; then their textures were examined by transmission X-ray techniques. For recrystallization texture studies, unless precautions are taken by etching off a sufficient amount of the surface layer before annealing, the texture developed in the interior may be affected by the surface layer, which may well have a different initial texture and which may have undergone recrystallization earlier than the interior of the specimen. Because of this effect, it is now planned to reexamine the texture of various rolled and annealed single crystals at the surface, and at various sections below the surface by using reflection techniques. In some cases, both surfaces of the rolled crystal will be examined. In one of Dunn's early papers,9 he noted that at an early stage of rolling the crystal seems to divide roughly through the middle to become a sample which in effect consists of two layers having some what different orientations. This effect has never been further explored. The investigation described in the present paper constitutes the beginning of a series of thorough investigations of texture formation in deformed bee single crystals designed to clear up some of the uncertainties which have been discussed. We have chosen a high-purity 2 pet Al-Fe alloy for this investigation. It is known that the allotropic transformation of iron is eliminated by alloying with approximately 1petAl. Such an alloy, being very similar to silicon ferrite, can be heated to the solidus temperature without phase transformation. One reason for choosing A1-Fe instead of Si-Fe for the present investigation is that we have been able to make single crystals of a vacuum-melted high-purity A1-Fe alloy by the strain-anneal method without much difficulty, but were not successful in doing so with a vacuum-melted high-purity Si-Fe alloy. For many research purposes,

Jan 1, 1962

By H. H. Campbell

Many attempts have been made to write a formula by which to calculate the strength of steel from its chemical composition, but most of these endeavors have failed because there were too many disturbing conditions. It is idle to collect from the pages of trade-papers, books, or the proceedings of scientific societies, a multitude of observations. The combination of such results will simply show that steel of the same composition will vary in tensile strength through wide limits—a fact that has been known for generations. That cold-working, overheating, and many another form of heat-treatment alter fundamentally the strength of steel, is ancient history, although it is only recently that the microscope has pointed out the road to an explanation of the phenomena. It mag be urged that the microscopic structure must betaken into consideration in any formula giving the ultimate strength, but from the standpoint of the present investigation this is unnecessary. We are trying to determine primarily, not what changes in ultimate strength may be made by variations in the condition of carbon, but what effect is produced by changes in the amount of carbon, when its condition remains constant. For such an inquiry, in order that the condition of the carbon should remain as nearly uniform as possible, it is essential that all testrpieces be made under the same conditions; and it is believed that the tests described in this paper satisfy that requirement. The investigations were made at the works of the Pennsylvania Steel Company, Steelton, Pa.; the ingots from which the tests were made were 6 in. square in every case; they were heated in the same furnace and forged at the same ham-

Jan 1, 1905

[Appalachian Petroleum Section: James M. Kimbrough, chairman; John H. Adair, first vice-chairman; Walter L. Diddle, second vice-chairman; Byron M. Finch, secretary-treasurer. Balcones Section: Robert V. West, chairman; Frank W. Jessen, first vice-chairman; Zane V. Morgan, second vice-chairman; Brantley G. Myers, secretary-treasurer. Meets 4th Wed., Petroleum Club (San Antonio) or Terrace Dining Room (Austin) Billings Petroleum Section: Charles B. Evans, chairman; L. M. Lyon, first vice-chairman; Gordon E. Lansford, second vice-chairman; Fred. A. Haddenhorst, secretary-treasurer. Meets 3rd Tues., Billings Petroleum Club. California Coastal Section: Robert L. Richardson, chairman; David K. Hayward, first vice-chairman; W. Jackson Bransford, secretary; William N. Harwell, treasurer. Meets 3rd Thurs., Pierport Inn, Ventura. Caracas Petroleum Section: Edwin A. Moo re, chairman;. Jose Cirigliano, vice-chairman; Frank B. Davis, secretary; Robert N. Powers, treasurer. Meets 2nd Tues., Caracas Theater Club.]

Jan 1, 1961

By L. N. Brown

The use of sheet and strip metal has increascd rapidly during the last few years and manufacturers have been called upon for an ever-increasing tonnage, better drawing quality, and better surface. The automobile industry is probably the most insistent in striving for a better product and a desire to reduce costs. Confronted by these demands, the mills have directed their efforts toward the delivery of material. Their personnel has been occupied largely with the problems incident to production, as any increase forced the use of new sources of raw material with their problems. These problems, combined with those met in the daily routine, have demanded immediate attention, with the result that the standardizing of heat treatments, quality, or temper, etc., have been neglected. Considerable work in standardizing has been done by many companies, but no acceptable method has been developed. The following method, therefore, is given with the hope that some method that can be accepted by the manufacturers and users may be developed. The problem of selecting a material with such properties that the losses in processing are a minimum is interesting and difficult. A description of the properties required is likewise difficult, largely because of loose terms. Another handicap is the number of methods of testing which have not been standardized and concerning which little information is available. In the selection of drawing or forming stock, it is advisable to eliminate as many variables as possible; consequently the method of testing the material is of the utmost importance. The method should be rapid and comparatively easy of application, as it is more important that a large percentage of the stock be tested with reasonable accuracy than that

Jan 1, 1923

By L. N. Brown

The use of sheet and strip metal has increascd rapidly during the last few years and manufacturers have been called upon for an ever-increasing tonnage, better drawing quality, and better surface. The automobile industry is probably the most insistent in striving for a better product and a desire to reduce costs. Confronted by these demands, the mills have directed their efforts toward the delivery of material. Their personnel has been occupied largely with the problems incident to production, as any increase forced the use of new sources of raw material with their problems. These problems, combined with those met in the daily routine, have demanded immediate attention, with the result that the standardizing of heat treatments, quality, or temper, etc., have been neglected. Considerable work in standardizing has been done by many companies, but no acceptable method has been developed. The following method, therefore, is given with the hope that some method that can be accepted by the manufacturers and users may be developed. The problem of selecting a material with such properties that the losses in processing are a minimum is interesting and difficult. A description of the properties required is likewise difficult, largely because of loose terms. Another handicap is the number of methods of testing which have not been standardized and concerning which little information is available. In the selection of drawing or forming stock, it is advisable to eliminate as many variables as possible; consequently the method of testing the material is of the utmost importance. The method should be rapid and comparatively easy of application, as it is more important that a large percentage of the stock be tested with reasonable accuracy than that

Jan 1, 1923

By John A. Gann

The following investigation constitutes a brief réumé of the more important binary magnesium alloys from the standpoint of metallo-graphic technique, and the effect of heat treatment on structure and properties. The comparative newness of the subject justifies this procedure as a preface to a more detailed study of each individual series of alloys. The work was started with the idea of practical application in the industry rather than as a theoretical investigation. The alloy compositions studied were selected as those most likely to show whether heat treatment would produce beneficial results. Furthermore, it was considered satisfactory to use commercial 99.9 per cent. magnesium, the best commercial grade of alloying ingredients, and to limit the time of heat treatment at the expense of incomplete equilibrium. These facts must be kept in mind when examining the results obtained, and the conclusions drawn. Preparation of Alloys All melts were made in an oil-fired cast-steel pot, approximately 12 in. dia, by 12 in. deep. Approximately 15 lb. of flux and 50 lb. of magnesium were melted and the calculated amount of alloying metal was added. After thorough alloying and puddling, the metal was chill cast in a graphite mold with four 1/2 by 1/2 by 4 in. bars fed from a common sprue and runner. The next higher composition alloy in a given series was made by adding the calculated amount of metal to the heel from the preceding cast. The pot was thoroughly cleaned after each series and new flux then introduced, thus avoiding possible contamination from earlier melts. The percentage compositions given in Table 1 are the calculated values. While not all alloys were analyzed, enough were checked to indicate that the reported compositions are correct to a few tenths of one per cent. A more detailed description of the foundry methods employed has been given in a previous paper. 1

Jan 1, 1929

By John A. Gann

The following investigation constitutes a brief réumé of the more important binary magnesium alloys from the standpoint of metallo-graphic technique, and the effect of heat treatment on structure and properties. The comparative newness of the subject justifies this procedure as a preface to a more detailed study of each individual series of alloys. The work was started with the idea of practical application in the industry rather than as a theoretical investigation. The alloy compositions studied were selected as those most likely to show whether heat treatment would produce beneficial results. Furthermore, it was considered satisfactory to use commercial 99.9 per cent. magnesium, the best commercial grade of alloying ingredients, and to limit the time of heat treatment at the expense of incomplete equilibrium. These facts must be kept in mind when examining the results obtained, and the conclusions drawn. Preparation of Alloys All melts were made in an oil-fired cast-steel pot, approximately 12 in. dia, by 12 in. deep. Approximately 15 lb. of flux and 50 lb. of magnesium were melted and the calculated amount of alloying metal was added. After thorough alloying and puddling, the metal was chill cast in a graphite mold with four 1/2 by 1/2 by 4 in. bars fed from a common sprue and runner. The next higher composition alloy in a given series was made by adding the calculated amount of metal to the heel from the preceding cast. The pot was thoroughly cleaned after each series and new flux then introduced, thus avoiding possible contamination from earlier melts. The percentage compositions given in Table 1 are the calculated values. While not all alloys were analyzed, enough were checked to indicate that the reported compositions are correct to a few tenths of one per cent. A more detailed description of the foundry methods employed has been given in a previous paper. 1

Jan 1, 1929

By J. J. Pye, J. B. Drew

The surface-diffusion coefficients of Ni63 diffusing on low-index planes of nickel single crystals have been measured over the temperature range from 400° to 1000°C using a precision autoradio-gvaphic technique. The activation energy for sur -face diffusion appears to he the same on the {111}, {110), and (100) planes and amounts to -0.60 ev. This is in good agreement with the value (-0.62 ev) reported for (111) planes obtained by mass-transport techniques. In an earlier paper, the authors have reported self surface-diffusion coefficients on silver.' In that work, a deviation of the diffusion coefficients from linearity in the Arrhenius plot was observed at high temperatures. This effect was attributed to a loss of tracer atoms into the bulk by volume diffusion. The purpose of the present work was to extend the technique developed to the nickel surface-diffusion system up to the point where volume diffusion would come into play. The nickel system especially lends itself to this technique due to the high efficiency of the isotope in darkening the film and the large absorption of the weak radiation (0.063 mev /3- particle of the trapped tracer atoms. The diffusion coefficients and ictivation energy for different orientations on nickel can also be compared with a report published by Blakely and Mykura 2 where a mass-transfer technique was used. This paper reports the self surface diffusion of nickel on the low-index planes over a wide temperature range using a precision autoradiographic technique. EXPERIMENTAL PROCEDURE The experiment is similar to that described in the earlier publication consisting of a radioactive needle as a source resting on a flat, smooth, chemically polished surface annealed in a dynamic dry-hydrogen atmosphere. The needle is held snugly on the surface by a holder fabricated from commercially pure nickel. The point source is made by grinding down a small-diameter nickel rod until a tip of approximately 0.1 mm radius is formed. It is then etched and the needle tip plated with the radioactive isotope Ni63. Nickel single crystals were used whose main impurities were spectrographically determined as Co 0.05, Fe 0.007, C 0.005, and S 0.003 pct. The surfaces, oriented to within 1/2 deg of the low-index planes, were carefully mechanically polished and etched in a 50-30-10-10 hot solution of acetic, nitric, sulfuric, and phosphoric acids giving a smooth polished surface. The crystals were then washed in distilled water and alcohol. Annealing temperatures ranged from 400° to 1000°C with a furnace arrangement in which the crystals could be brought up to temperature in times short compared to diffusing times. The temperature was maintained constant to ±10°C. In the temperature range investigated, the ratio of the surface-diffusion coefficient to the volume-diffusion coefficient (Ds/Du) was 105 or more and the mean bulk-penetration values, calculated from literature values of volume-diffusion coefficients,3 were on the order of 10-5 cm. After the diffusion anneal, the sintered needle is removed, and both the radius of the needle point and spot left on the crystal face are measured. The crystal is then placed on photographic film. Diffusion profiles are obtained by scanning the film with a recording microdensitometer which has a slit width of 10µ. DISCUSSION AND RESULTS The experimental conditions are such that the source strength and needle radius are essentially constant and the time is adjusted such that the mean bulk penetration is small. An exactly analogous heat-flow problem has been considered by Carslaw and Jaeger4 and the solution can be written in integral form as:

Jan 1, 1964

By Leo P. Tarasov

Magnetic torque studies of ferromagnetic single crystals have been carried out in a number of laboratories during the last decade&apos;s2 and some work has been reported on polycrystalline material showing preferred orientation. Goss3 used the method extensively in developing electrical sheet with desirable magnetic properties, but he used it as a control rather than as a means of studying the texture. Bozorth4 made a quantitative correlation of a torque curve he obtained from some cold-rolled iron with the texture as determined from X-rays, but did not extend his studies beyond the one specimen. Other studies, which have been reported from time to time2,5 have also been incomplete in the sense that no effort was made to study a whole series of samples, differing only in degree of cold reduction or in the annealing temperature, in order to ascertain the effect of such treatments on the texture as revealed by torque measurements. It is the purpose of this investigation to make such a study, mainly in order to see how useful the method can be made when used under favorable circumstances and to find what kind of a correlation can be expected between magnetic and X-ray studies of texture. Before proceeding further, it is desirable to say a little about single crystals, so as to make clear the concepts involved in magnetic torque measurements. Magnetic Torque Method It is fairly well known nowadays that single crystals of ferromagnetic substances have directions of easy magnetization and of hard magnetization. In Fig. 1 are reproduced typical magnetization curves for a single crystal of iron, which show that in a < 100 > direction saturation occurs at low fields compared to those required to saturate the same crystal in a <110> or a <111> direction. (The magnetization intensity I is defined by the equation B = H + 4pI.) At fields high enough to

Jan 1, 1939

By Leo P. Tarasov

Magnetic torque studies of ferromagnetic single crystals have been carried out in a number of laboratories during the last decade&apos;s2 and some work has been reported on polycrystalline material showing preferred orientation. Goss3 used the method extensively in developing electrical sheet with desirable magnetic properties, but he used it as a control rather than as a means of studying the texture. Bozorth4 made a quantitative correlation of a torque curve he obtained from some cold-rolled iron with the texture as determined from X-rays, but did not extend his studies beyond the one specimen. Other studies, which have been reported from time to time2,5 have also been incomplete in the sense that no effort was made to study a whole series of samples, differing only in degree of cold reduction or in the annealing temperature, in order to ascertain the effect of such treatments on the texture as revealed by torque measurements. It is the purpose of this investigation to make such a study, mainly in order to see how useful the method can be made when used under favorable circumstances and to find what kind of a correlation can be expected between magnetic and X-ray studies of texture. Before proceeding further, it is desirable to say a little about single crystals, so as to make clear the concepts involved in magnetic torque measurements. Magnetic Torque Method It is fairly well known nowadays that single crystals of ferromagnetic substances have directions of easy magnetization and of hard magnetization. In Fig. 1 are reproduced typical magnetization curves for a single crystal of iron, which show that in a < 100 > direction saturation occurs at low fields compared to those required to saturate the same crystal in a <110> or a <111> direction. (The magnetization intensity I is defined by the equation B = H + 4pI.) At fields high enough to

Jan 1, 1939

By L. R. Gremillion, G. H. McClellan

Chemical and mineralogical data on 25 apatitic phosphate ores of diverse origins from commerical deposits around the world were widely variable. From 14 to 18 chemical constituents of each sample were determined, and each sample contained four to ten mineral phases. Altogether there were 34 different mineral phases, many of which occurred in only one sample. Samples contained varieties of francolites, fluorapatites, and mixed hydroxyfluorapatites. The apatite compositions calculated from chemical data showed that certain types of substitutions were characteristic of different apatite varieties, but every variety had some degree of substitution of (CO3)2- for (PO4)3-, and the P205 contents of the apatites ranged from 35.1 %for a North Carolina apatite to 41.9% for a Missouri apatite. In a concentrate with a grade of 32% P2O5, the North Carolina sample should contain about 8.7% gangue and the Missouri sample about 23.7% gangue. To optimize the digestion process of a phosphate ore, it is necessary to consider the dissolution behaviors of different mineral phases during acidulation and their possible effects on chemical properties of a fertilizer intermediate. In the production of wet-process acids or superphosphates, acidulation of certain minerals may cause foaming and formation of sludge, filtration, corrosion, and handling problems.

Jan 1, 1982

Briefly, an open stope is one in which the ore is taken out and no filling is put in; the only support for the walls may be posts or pillars of ore. Such a method is limited to orebodies with strong walls and ore strong enough to stand unsupported over the back of the stope. Details vary and depend on the dip of the vein, mode of breaking ground, method of handling broken ore, and so forth. The examples given are the Beat-son, Birmingham district, Mineville district, and Cornucopia.

Jan 1, 1925

By Alan Morris

Season cracking of brass has received wide attention and there is a wealth of technical literature on the subject. Its causes arc fairly well understood and means for its prevention are inexpensive and effective, so that the frequency of failures from this source has diminished of recent years. But its sister phenomenon, the failure of annealed brass by reason of applied tensile stress plus a certain type of corrosion, has received less attention, though it has been responsible for occasional more or less troublesome cases of cracking of brass in service. The work described in the following pages was undertaken about two years ago to determine the relative resistance of various commercial brass mixtures to stress-corrosion cracking, and to learn something of the controlling factors. By stress-corrosion cracking we mean the cracking of brass free from internal stresses by reason of applied tensile stress and simultaneous attack by certain corrosive agents. Rogers,&apos; in discussing a paper by Hatfield and Thirkell, says: " He had also applied a solution of mercuric salt to tensile test pieces of brass whilst they were under stress in the testing machine. At very moderate stresses such test pieces cracked, and very readily broke." Moore, Beckinsale and Mallinson2 subjected test pieces to simultaneous corrosion and tensile stress. In order to determine the minimum stress detectable in brass by the mercurous nitrate test, tensile samples were placed under stress and treated with mercurous nitrate solution. They found that brass stressed below a minimum did not crack. Dr. McAdam3 has investigated the effect of corrosion on the fatigue limit of brasses, among other materials. He directed a stream of either fresh or salt water against the specimen while it was undergoing fatigue test. The corrosion-fatigue limits thus determined may be considerably lower than the endurance limit without coincident corrosion. The exact

Jan 1, 1930

By A. F. Taggart

THE following notes represent significant excerpts from a mass of records of experimental work done in the ore-dressing laboratory at the Columbia School of Mines during the years 1926 to 1928-inclusive. CLASSIFICATION OF EXPERIMENTAL WORK The experiments performed may be grouped for purposes of description under the following general -headings: I. Collecting agents. a. A method for quantifying collecting effect. b. Coating with undissolved collecting agents (oils) c. Action of dissolved collecting agents. II. Frothing agents. a. A method for quantifying frothing effect. b. Relation between frothing effect and chemical composition. III. Inorganic reagents. a. Methods of studying the effects of these reagents. b. Effect on slime dispersion. c. Effect on sulfides. SUMMARY OF THE ORIGINS OF PRESENT-DAY FLOTATION PRACTICE The first practicable, foolproof method of froth flotation was described in U. S. patent 835120, issued in 1906 to Sulman, Picard and Ballot, and in the equivalent patents in other countries. A number of less simple methods of producing the same result had been described previously in patent publications and otherwise.1 The reagents specified in all of these early patents were "oils" and, in addition, some inorganic substance, usually an acid. The quantities of reagents recommended and added were enormous when&apos; compared with those used today.

Jan 1, 1929

By H. G. Moulton

THE INCREASING scale of mining operations over the past decade, particularly in connection with the exploitation of large bodies of comparatively low-grade copper ores, has made necessary the study of the behavior of rock under failure. When extractions of as high as 40,000 tons a day are reached in steam-shovel operations and as high as 20,000 tons per day in underground mining operations, it is evident that excavations soon become of such size that the behavior of the rock will often be dependent on fundamental principles applicable to more or less homogeneous materials under stress, rather than on weathering or local planes of weakness. In the ordinary rock excavations encountered in civil-engineering practice, such as excavations for subways, highways, railroads, etc., rock faces are not carried to depths sufficient to develop any pressures, or consequently any failures, except those due to loose masses resulting from local planes of weakness. When, however, orebodies whose tonnage is measured by hundreds of thousands are to be extracted by steam-shovel operations in open pits, it is necessary to determine if possible in advance the slopes that the sides of the pits will assume, for these slopes influence the shape of the excavations and thereby the amount of ore that may be extracted by the open-pit method. When large orebodies are mined underground at depths of 300 to 500 ft. (91 to 152 m.) by caving methods, the surface subsiding as the ore is withdrawn, it is necessary to determine in advance the outermost limits of fracture in the subsiding surface, for on the delineation of these limits depends the location of surface improvements, mills, smelters, etc. and also the location of development work, such as hoisting shafts, main haulage levels, and all other underground openings that must remain undisturbed during the period of ore extraction. Heretofore, in civil-engineering practice, it has been assumed that earth and rock behave differently in failure. For the calculation of earth

Jan 2, 1920

By Reinhardt Thiessen

During the last few years a type of coal called "splint coal" has been brought to the attention of the United States Bureau of Mines, through numerous inquiries concerning its nature. Until recent years it appears to have escaped general notice. The term "splint coal" is of long standing, but was thought to be merely another expression applied by the miner to coal having certain minor characteristics. When closely examined, however, these coals were found to form a marked and distinct type, with distinctive characteristics that cannot be mistaken. Because splint coals produce a hot cheerful flame, possess a clean blocklike nature, and have a high volatile content, they have lately become much valued for domestic, gas-producer and steaming purposes, and have attracted considerable attention. Mattkohle For many years we have heard from the Germans about Mattkohle and Streifenkohle, in contradistinction to Glanzkohle, but have not realized that they were of a different type from the coals with which we were most familiar. This type of coal was first brought to general notice by Muck, in 1881, who gave a good description of it.&apos; Because this coal is often intercalated with thin sheets of brightly shining cod, Schondorff, who was more familiar with the Saar coals, called it Streifernkohle. This term was later used by Muck also. Still later Potoné² used this term exclusively for the whole group in contradistinction to a class called Glanzkohle, and considered these coals to be composed alternately of Humuskohle and Faulkohle or Mattkohle (Pig. 20). Not knowing the nature of the German coals and not realizing that the term Streifenkohle was applied to a distinct class of coal, the terms of its components as used by Potonié and others were translated to "bright Coal" and "dull coal" and applied to the components of our

Jan 1, 1930

By A. S. Michaels, R. S. Timmins

A study of the effect upon oil recovery from an un-consolidated porous medium of chromatographic transport of selected reverse-wetting additives during water displacement is described. Flow tests were performed on hydrocarbon oil-saturated sand columns (containing connate water) into which small volumes of short-chain aliphatic amine solutions were introduced during water flooding. Concurrently, meusurements of oil-silica contact angles, oil-water interfacial tensions and oil-water distribution coefficients were measured us a function of additive concentration. Certain treatments were found to cause a slight reduction in oil recovery, while others produced a significant increase (up to 50 per cent of the normtzl irreducible rninimum oil saturation). Recovery eficiency was correlated most satisfactorily with the maximum degree of reverse wetting produced during additive transport; conditions which resulted in only mild oil wettability of the sand reduced recovery, while those favoring strong oil wetting increased recovery. A mechanism of reverse-wetting additive action during chromatographic transport is developed which ascribes the results to transient changes in oil-solid contact angle during flow, with consequent release of oil trapped by capillary forces. Implications of these observations with regard to improved waterflood efficiencies are discussed. INTRODUCTION The need for finding improved methods of oil production is amply illustrated by the large volume of oil considered economically unrecoverable by existing production practice. Water flooding has long been an excellent method of secondary recovery. However, even in those areas of a formation which are well swept by a water flood, 20 per cent or more of the oil remains trapped within the formation and is not recovered. This trapping of oil within the pores of the rock structure results primarily from interfacial forces. If these interfacial forces were altered, it is possible that the trapped oil could be released and recovered. The addition of surface-active agents to a water flood to alter the interfacial properties of the oil-water-solid system has received considerable attention as a method of increasing oil recovery. Studies of surfactant treatment have yielded varied and, in some cases, apparently conflicting results. Increased oil recovery using surface-active agents has been reported by a number of investigators. Others have found that use of surfactants in a water flood either has no effect upon oil recovery or decreases it. Since surface-active agents tend to alter the formation wettability and oil-water interfacial tension simultaneously, several investigators have tried to determine the role these two factors play in oil recovery. Data have been presented which indicate that the most desirable condition for the solid surface is strongly water-wet. Other results indicate that, although breakthrough recovery may be less, the greatest ultimate recovery is obtained when neutral wettability prevails.", " The desirability of low interfacial tension seems to depend upon the wettability of the formation. Reports of higher recoveries, when the interfacial tension is high in a water-wet system and low in an oil-wet system, are at odds with reports of increased recovery in water-wet systems when surfactants which decrease the interfacial tension are added to the water flood. A review of previous work studying the effects of using surface-active agents in a water flood shows that these agents produce widely different effects and that opinions as to the role of the various interfacial properties are diverse. The consensus, however, is that the interfacial properties are quite important in the displacement of oil from a porous medium by water. Even in those investigations where appreciable increases in oil recovery resulted from treatment with a surface-active agent, economic considerations generally made practical application of the treatment unattractive because surfactants tend to be adsorbed within the formation. This adsorption would necessitate using large quantities of surfactant if all of the flood water were treated to contain a given surfactant concentration, even if this concentration were quite low. Preston and Calhoun suggested that the principles of chromatography could be applied to the use of surface-active agents as a means of increasing oil recovery. A small volume of surface-active material is injec-

Jan 1, 1965

By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,&apos; was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951