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By James Norman, O. C. Ralston, John Dasher

Most mineral products are used in the finely divided state, but some are sold in larger sizes. Coal, gravel, metallurgical fluorspar, phosphate rock, hematite, chro-mite, and other products are sold in sizes coarser than can be treated by many mineral-dressing methods. Gravity separation of coarser sizes by log washing and jigging is probably as ancient as any process now in use. The performance of jigs on a feed with sufficient difference in density of the minerals is excellent, but many families of minerals are too similar in density to be separated effectively by this method. The use of heavy suspensions of fine solids to separate coarse coal from bone and slate has been in use for some years. This separation by sink-and-float was limited until recently to light minerals. Development of galena and ferrosilicon as suspension media, by Minerals Beneficia-tion, Inc., at Mascot, Tenn., Pitcher, Okla., and Crosby, Minn., under patents granted during and since 1938, has permitted excellent results to be obtained on minerals of very similar densities up to 3.3. This process has been put In the hands of American Cyanamid Co. for exploitation, and further research now in progress may increase the density of suspension obtainable so that separations at a density of 4.0 may be practicable before this is published. The Huntington-Heberlein dense-medium process, developed in England, is also being commercialized in the United States by Sink and Float Corporation. Du Pont has developed a sink-and-float separation using halogenated hydrocarbons as parting liquids; at this writing, the method is used commercially only on coal but has been successful in the pilot plant on many other minerals using tetrabrom-ethane at densities up to 2.95. While these processes were being developed to extend the range of separation by difference in density to the coarser sizes, the Bureau of Mines was engaged in developing a process that will extend the range of separation by difference in wettability up to 2-in. size. War work has pushed aside its further development indefinitely. The results are published here with the hope that some use may be suggested that will justify post-war development, and so that readers that may be able to make immediate use of the scheme may have the information. Earlier Work It has been known since the time of Herodotus (B.C. 484(?)-425) that water-repellent particles will adhere to sticky surfaces. That early historian reports the recovery of gold from the mud of a lake

Jan 1, 1943

By James Norman, O. C. Ralston, John Dasher

MOST mineral products are used in the finely divided state, but some are sold in larger sizes. Coal, gravel, metallurgical fluorspar, phosphate rock, hematite, chromite, and other products are sold in sizes coarser than can be treated by many mineral-dressing methods. Gravity separation of coarser sizes by log washing and jigging is probably as ancient as any process now in use. The performance of jigs on a feed with sufficient difference in density of the minerals is excellent, but many families of minerals are too similar in density to be separated effectively by this method. The use of heavy suspensions of fine solids to separate coarse coal from bone and slate has been in use for some years. This separation by sink-and-float was limited until recently to light minerals. Development of galena and ferrosilicon as suspension media, by Minerals Beneficiation, Inc., at Mascot, Tenn., Pitcher, Okla., and Crosby, Minn., under patents granted during and since 1938, has permitted excellent results to be obtained on minerals of very similar densities up to 3.3. This process has been put in the hands of American Cyanamid Co. for exploitation, and further research now in progress may increase the density of suspension obtainable so that separations at a density of 4.0 may be practicable before this is published. The Huntington-Heberlein dense-medium process, developed in England, is also being commercialized in the United States by Sink and Float Corporation. Du Pont has developed a sink-and-float separation using halogenated hydrocarbons as parting liquids; at this writing, the method is used commercially only on coal but has been successful in the pilot plant on many other minerals using tetrabromethane at densities up to 2.95. While these processes were being developed to extend the range of separation by difference in density to the coarser sizes, the Bureau of Mines was engaged in developing a process that will extend the range of separation by difference in wettability up to 2-in. size. War work has pushed aside its further development indefinitely. The results are published here with the hope that some use may be suggested that will justify post-war development, and so that readers that may be able to make immediate use of the scheme may have the information. EARLIER WORK It has been known since the time of Herodotus (B.C. 484(?)-425) that water-repellent particles will adhere to sticky surfaces. That early historian reports the

Jan 1, 1942

By S. Suphi Yavasca, A. M. Gaudin

THIS paper is intended as a contribution to our knowledge of the mechanism of comminution and of the work of crushing. In a previous paper' it was shown that with quartz comminution proceeds as follows I. The size distribution of broken fragments made by a single fracture is such that the new surface on each grade is the same. 2. Multiple fracturing results in a size distribution such that in the fine sizes the surface per grade is the same in every grade; in coarse sizes the surface per grade decreases gradually with increasing size. In that paper it was mentioned that determinations on minerals other than quartz were in course of completion in order to establish the generality of these observations. In this paper, condensed data2 are presented for galena, pyrite and glass. Galena and pyrite are crystalline material and glass is noncrystalline. Galena has excellent cubic cleavage. Pyrite, although cubical, does not have marked cleavage. Quartz, on which the original determinations were made, does not cleave and although crystalline (hexagonal) breaks conchoidally. Glass breaks much like quartz. It is apparent, therefore, that the minerals selected represent some range in character of the solid without covering all possible types. GLASS Fifteen glass marbles were crushed individually in the pendulum crusher described in the preceding paper,1 then subjected to careful screening for 30 min. Six sized fractions were selected and cleaned in a hot 0.12 N solution of hydrochloric acid, washed with distilled water and dried on a hot plate. This was followed by an examination with a binocular microscope, to remove foreign matters not eliminated in cleaning as well as to eliminate "compacts" of fine particles. These compacts are groups of fine iragments that seem to be mechanically stuck together as a result of localized compacting during the comminution operation. The presence and the abundance of these compacts may be related to the amount and direction of the forces applied in different crushing devices. Since, properly, such compacts should be entirely eliminated in the sizing analyses, it is necessary to remove them to the last before making surface determinations on sized fractions. For example, with a - 28 + 35-mesh glass the surface areas of two samples, one cleaned with acid and under the binocular, the other only washed, were 102 and 172 sq. cm. per gram, respectively. Examination of the samples under an Ultropak microscope showed that washing alone failed to remove the compacts and also that it fails to remove certain fine dusts attached to the particles. Cleaning with acid loosens the fine dusts and

Jan 1, 1945

By S. Suphi Yavasca, A. M. Gaudin

This paper is intended as a contribution to our knowledge of the mechanism of comminution and of the work of crushing. In a previous paper1 it was shown that with quartz comminution proceeds as follows: 1. The size distribution of broken fragments made by a single fracture is such that the new surface on each grade is the same. 2. Multiple fracturing results in a size distribution such that in the he sizes the surface per grade is the same in every grade; in coarse sizes the surface per grade decreases gradually with increasing size. In that paper it was mentioned that determinations on minerals other than quartz were in course of completion in order to establish the generality of these observations. In this paper, condensed data1 are presented for galena, pyrite and glass. Galena and pyrite are crystalline materials and glass is noncrystalline. Galena has excellent cubic cleavage. Pyrite, although cubical, does not have marked cleavage. Quartz, on which the original determinations were made, does not cleave and although crystalline (hexagonal) breaks conchoidally. Glass breaks much like quartz. It is apparent, therefore, that the minerals selected represent some range in character of the solid without covering all possible types. Glass Fifteen glass marbles were crushed individually in the pendulum crusher described in the preceding paper,' then subjected to careful screening for 30 min. Six sized fractions were selected and cleaned in a hot 0.12 N solution of hydrochloric acid, washed with distilled water and dried on a hot plate. This was followed by an examination with a binocular microscope, to remove foreign matters not eliminated in cleaning as well as to eliminate "compacts" of fine particles. These compacts are groups of he irag-ments that seem to be mechanically stuck together as a result of localized compacting during the comminution operation. The presence and the abundance of these compacts may be related to the amount and direction of the forces applied in different crushing devices. Since, properly, such compacts should be entirely eliminated in the sizing analyses, it is necessary to remove them to the last before making surface determinations on sized fractions. For example, with a — 28 + 35-mesh glass the surface areas of two samples, one cleaned with acid and under the binocular, the other only washed, were 102 and 172. cm' per gram, respectively. Examination of the samples under an Ultropak microscope showed that washing alone failed to remove the compacts and also that it fails to remove certain fine dusts attached to the particles. Cleaning with acid loosens the fine dusts and

Jan 1, 1947

By S. Suphi Yavasca, A. M. Gaudin

This paper is intended as a contribution to our knowledge of the mechanism of comminution and of the work of crushing. In a previous paper1 it was shown that with quartz comminution proceeds as follows: 1. The size distribution of broken fragments made by a single fracture is such that the new surface on each grade is the same. 2. Multiple fracturing results in a size distribution such that in the he sizes the surface per grade is the same in every grade; in coarse sizes the surface per grade decreases gradually with increasing size. In that paper it was mentioned that determinations on minerals other than quartz were in course of completion in order to establish the generality of these observations. In this paper, condensed data1 are presented for galena, pyrite and glass. Galena and pyrite are crystalline materials and glass is noncrystalline. Galena has excellent cubic cleavage. Pyrite, although cubical, does not have marked cleavage. Quartz, on which the original determinations were made, does not cleave and although crystalline (hexagonal) breaks conchoidally. Glass breaks much like quartz. It is apparent, therefore, that the minerals selected represent some range in character of the solid without covering all possible types. Glass Fifteen glass marbles were crushed individually in the pendulum crusher described in the preceding paper,' then subjected to careful screening for 30 min. Six sized fractions were selected and cleaned in a hot 0.12 N solution of hydrochloric acid, washed with distilled water and dried on a hot plate. This was followed by an examination with a binocular microscope, to remove foreign matters not eliminated in cleaning as well as to eliminate "compacts" of fine particles. These compacts are groups of he irag-ments that seem to be mechanically stuck together as a result of localized compacting during the comminution operation. The presence and the abundance of these compacts may be related to the amount and direction of the forces applied in different crushing devices. Since, properly, such compacts should be entirely eliminated in the sizing analyses, it is necessary to remove them to the last before making surface determinations on sized fractions. For example, with a — 28 + 35-mesh glass the surface areas of two samples, one cleaned with acid and under the binocular, the other only washed, were 102 and 172. cm' per gram, respectively. Examination of the samples under an Ultropak microscope showed that washing alone failed to remove the compacts and also that it fails to remove certain fine dusts attached to the particles. Cleaning with acid loosens the fine dusts and

Jan 1, 1947

By James Norman, O. C. Ralston, John Dasher

Most mineral products are used in the finely divided state, but some are sold in larger sizes. Coal, gravel, metallurgical fluorspar, phosphate rock, hematite, chro-mite, and other products are sold in sizes coarser than can be treated by many mineral-dressing methods. Gravity separation of coarser sizes by log washing and jigging is probably as ancient as any process now in use. The performance of jigs on a feed with sufficient difference in density of the minerals is excellent, but many families of minerals are too similar in density to be separated effectively by this method. The use of heavy suspensions of fine solids to separate coarse coal from bone and slate has been in use for some years. This separation by sink-and-float was limited until recently to light minerals. Development of galena and ferrosilicon as suspension media, by Minerals Beneficia-tion, Inc., at Mascot, Tenn., Pitcher, Okla., and Crosby, Minn., under patents granted during and since 1938, has permitted excellent results to be obtained on minerals of very similar densities up to 3.3. This process has been put In the hands of American Cyanamid Co. for exploitation, and further research now in progress may increase the density of suspension obtainable so that separations at a density of 4.0 may be practicable before this is published. The Huntington-Heberlein dense-medium process, developed in England, is also being commercialized in the United States by Sink and Float Corporation. Du Pont has developed a sink-and-float separation using halogenated hydrocarbons as parting liquids; at this writing, the method is used commercially only on coal but has been successful in the pilot plant on many other minerals using tetrabrom-ethane at densities up to 2.95. While these processes were being developed to extend the range of separation by difference in density to the coarser sizes, the Bureau of Mines was engaged in developing a process that will extend the range of separation by difference in wettability up to 2-in. size. War work has pushed aside its further development indefinitely. The results are published here with the hope that some use may be suggested that will justify post-war development, and so that readers that may be able to make immediate use of the scheme may have the information. Earlier Work It has been known since the time of Herodotus (B.C. 484(?)-425) that water-repellent particles will adhere to sticky surfaces. That early historian reports the recovery of gold from the mud of a lake

Jan 1, 1943

By R. F. Stahl, W. A. Martin, R L. Huntington

A marked gravitational segregation of liquid has been observed to take place in a number of volumetric fields toward the later stages of their oil-producing periods. This phenomenon has been pronounced in thick, highly permeable sand formations such as those of the wilcox zone in Oklahoma City. This observation has prompted considerable research directed toward the semiquantitative determination of the equilibrium saturation distribution of oil vertically throughout a formation at final depletion. In this paper, data are also presented showing the transient distribution of liquid at different stages of the depletion period. Other experimental results show the effect of temperature on the drainage rates of water, Wilcox crude oil, and a close-cut heptane fraction. Intermittent drainage of liquid produced saturation gradients that might well be expected from the flow theories involved, Yields of the various liquids varied from 50 to 75 per cent of the original fluid content of the sand-packed (4 in. by 8 ft.) vertical tube. Introduction In certain volumetric Oil fields the performance of the reservoir during the latter part Of its producing life is governed to a large extent by the downward movement of liquid due to the force of gravity. This is especially true of formations having thick or tilting beds of uniformly high permeability, free of shale breaks. Laverett4 and Katz3 have presented original data and discussed the theory relating to the capillary and gravitational forces acting On liquids contained in a sand body. These investigators have pointed out the importance of such studies in the estimation of future reserves as well as the original fluid content of a reservoir. In this previous work, no data have been reported showing the history of saturation distributions during the drainage period. Since a knowledge Of these transients is helpful in obtaining crude Oil from such a reservoir, the authors have obtained these data during this investigation. Experimental Apparatus The drainage tests were carried out in two vertical tubes, 8 ft. high and consisting of 2-in. and 4-in. standard wrought-iron pipe, respectively. Each tube was equipped with a water jacket, which could be kept virtually isothermal ( ± 1.0ºF.). A diagrammatic sketch of the 4-in. tube and its auxiliaries is shown in Fig. 1. At 6 in. above the base of the tube, and at every foot above this point, core nipples were inserted through the water jacket. These nipples were closely fitted with steel-plug inserts during each drainage run. At the end of the run, these inserts were removed so that cores could be obtained from the sand-packed tube.

Jan 1, 1943

By Charles R. L. Oder, Howard W. Miller

Approximately 5000 tons of zinc ore a day was mined during 1943 in the Mascot-Jefferson City district in East Tennessee. This ore came from the Kingsport formation, a part of the Knox dolomite, of Ordovician age. The Kings-port is composed of 350 to 400 ft. of limestone and dolomite. Thin cherts, sandy layers and shales are numerous. Frequently, the limestones are altered to crystalline dolomite. The Kingsport is divisible into four main lithologic zones. These divisions are illustrated in an accompanying table, which gives detailed sections of the ore-bearing beds as found in the mines and shows the exact positions of the various ore zones within the formation. Key beds are described and the practical applications of stratigraphy in mapping, prospecting and mining are discussed. Introduction The Mascot-Jefferson City zinc district is in Knox and Jefferson Counties, in the Great Valley of East Tennessee. It extends from Mascot, I3 miles northeast of Knoxville, to Jefferson City, about 30 miles northeast of that city. The American Zinc Company of Tennessee is producing from five mines in the district, in which it has operated for more than 30 years. The only other important producer is the Universal Exploration Co. The approximate daily production of the district in 1943 was 5000 tons of sulphide ore, grading from 2.5 to 6 per cent zinc. Small amounts of oxidized ore are mined intermittently. The Knox dolomite has been described by various geologists,'-' but no detailed descriptions of the rock sections revealed by mining have been published. Rock units are not conspicuously different and careful study is required to distinguish them. Nevertheless, familiarity with the stratigraphy of the mineralized zones is essential to successful exploration and extraction of the ores; therefore the purpose of this paper is to give detailed stratigraphic sections as measured in the mines, to discuss their important features and to show their relationship to the stratigraphy of the district. Generalized Section Table I gives the most characteristic general features of the major stratigraphic units. The formation names given in parenthesis are locally and widely used terms, the correlations of which are not necessarily established. For this reason they are put in quotation marks and are replaced by more restricted terms. The names "Mascot" and "Kingsport" were adopted from local towns. They were chosen jointly by Josiah Bridge, of the Federal Geological Survey, and the senior author for use in their separate unpublished manuscripts describing the Knox dolomite in East Tennessee. Descriptions of the type sections may soon be published. The name "Longview" was first applied by Butts6 in Alabama.

Jan 1, 1949

By John Chipman, Eric R. Jette, O. B. Ellis

IN the study of the chemical reactions occurring in the open-hearth furnace, it is frequently assumed that a condition of equilibrium between slag and metal is attained. In order to test this assumption it is necessary to have dependable operating data as well as an exact knowledge of the equilibrium state. Considerable progress has already been made in the study of slag-metal equilibria, notably in the earlier work of Herty1 and of Oberhoffer and Schenck2 and in the more recent researches of Krings and Schackmann3 and of Koerber and Oelsen.4 None of these investigators, however, have employed basic slags comparable to those encountered in basic open-hearth practice, so that up to the present time our only information regarding the equilibria of these slags is based upon observations drawn from steelmaking practice in which there is little assurance that actual equilibrium was attained. The original plan of this investigation was to secure simultaneous slag and metal samples at intervals during the making of an open-hearth heat, recording the heat history in detail and obtaining complete analyses of slag and metal, then to bring these slag samples into equilibrium with liquid iron in the laboratory induction furnace and thus to determine directly whether or not the observed relationships in the open hearth represent conditions approaching equilibrium. This plan was only partly successful. While slags were obtained from the open hearth under satisfactorily recorded conditions and these were remelted in the laboratory under equilibrium conditions, changes in slag composition, which accompanied the remelting operation, were so great that the final slag from the induction furnace bore little resemblance to its open-hearth parent and the direct comparison was therefore abandoned. The results, however, lie within a range of slag composition that is of interest in the making of low-carbon steel. As far as we are aware, they represent the first published laboratory study of equilibria involving slags that contain all the constituents of basic open-hearth slag. EXPERIMENTAL HEATS The first set of measurements on slagmetal equilibrium was made in the Research Laboratories of the American Rolling Mill Co. at Middletown, Ohio. This will be known as series A. The second set was made in the Metallurgical Research Laboratories at Massachusetts Institute of Technology, and will be referred to as series B. Series A.-The induction furnace used has been described.5 Approximately I kg. of a special ingot iron containing less than

Jan 1, 1941

By W. S. Stahmann, F. W. Bowdish

Previously published experimental data showing that both collectable and non-collectable sulfide films may be formed on chrysocolla were analysed, and chemical mechanisms were proposed for the formation of the films. A special technique was developed by which the quantity of sulfur adsorbed was determined for samples sulfidized under different conditions of pH and soluble sulfide concentration. The data on sulfur adsorption were used together with the expression for the equilibrium constant for the proposed reaction to indicate the validity of the chemical mechanism theory. A recent paper 1 about contact angle studies on chrysocolla reported the effects of pH value and sodium sulfide concentration during sulfidization upon the character of the surfaces produced. In each experiment the surface of a specimen of chrysocolla was prepared by grinding it with fine abrasive and washing it in tap water. The specimen was then placed in the sulfidizing solution for 10 min, rinsed in tap water, treated for 15 min in a solution containing 30 mg of potassium amyl xanthate per liter, rinsed in distilled water, and tested for air adhesion in a contact angle apparatus. The results, when plotted as in Fig. 1, showed an island representing conditions giving air adherent or collectable surfaces surrounded by conditions giving non-collectable surfaces. Particular interest may be attached to the region of non-collectability to the right of and above the island in Fig. 1, and to the boundry curve separating these two regions. It is apparent that at any pH from 4.0 to 6.0, where a collectable surface may be produced, a sufficient increase in the sulfide concentration results in a non-collectable surface. Thus it appears that too much soluble sulfide has a depressing effect upon the mineral, just as it has in sulfide flotation. This paper presents some speculations regarding the chemical mechanisms by which the collectable and non-collectable sulfide films may be formed and reports on a physical-chemical study intended to support these speculations. THEORETICAL CONSIDERATIONS The experimental results presented in the previous paper were analysed in several ways in an attempt to understand better the chemical mechanisms involved. For several points on the boundary to the right of the region of contact in Fig. 1, molar concentrations of H+, OH-, HS-, and S= ions, as well as various ion concentration products, were calculated. Following the reasoning of Wark and Cox, 2,3 no single kind of ions may be credited with causing depression of the surface because none of them have a constant con-

Jan 1, 1968

By Howard W. Miller, Charles R. L. Oder

Approximately 5000 tons of zinc ore a day was mined during 1943 in the Mascot-Jefferson City district in East Tennessee. This ore came from the Kingsport formation, a part of the Knox dolomite, of Ordovician age. The Kings-port is composed of 350 to 400 ft. of limestone and dolomite. Thin cherts, sandy layers and shales are numerous. Frequently, the limestones are altered to crystalline dolomite. The Kingsport is divisible into four main lithologic zones. These divisions are illustrated in an accompanying table, which gives detailed sections of the ore-bearing beds as found in the mines and shows the exact positions of the various ore zones within the formation. Key beds are described and the practical applications of stratigraphy in mapping, prospecting and mining are discussed. Introduction The Mascot-Jefferson City zinc district is in Knox and Jefferson Counties, in the Great Valley of East Tennessee. It extends from Mascot, I3 miles northeast of Knoxville, to Jefferson City, about 30 miles northeast of that city. The American Zinc Company of Tennessee is producing from five mines in the district, in which it has operated for more than 30 years. The only other important producer is the Universal Exploration Co. The approximate daily production of the district in 1943 was 5000 tons of sulphide ore, grading from 2.5 to 6 per cent zinc. Small amounts of oxidized ore are mined intermittently. The Knox dolomite has been described by various geologists,'-' but no detailed descriptions of the rock sections revealed by mining have been published. Rock units are not conspicuously different and careful study is required to distinguish them. Nevertheless, familiarity with the stratigraphy of the mineralized zones is essential to successful exploration and extraction of the ores; therefore the purpose of this paper is to give detailed stratigraphic sections as measured in the mines, to discuss their important features and to show their relationship to the stratigraphy of the district. Generalized Section Table I gives the most characteristic general features of the major stratigraphic units. The formation names given in parenthesis are locally and widely used terms, the correlations of which are not necessarily established. For this reason they are put in quotation marks and are replaced by more restricted terms. The names "Mascot" and "Kingsport" were adopted from local towns. They were chosen jointly by Josiah Bridge, of the Federal Geological Survey, and the senior author for use in their separate unpublished manuscripts describing the Knox dolomite in East Tennessee. Descriptions of the type sections may soon be published. The name "Longview" was first applied by Butts6 in Alabama.

Jan 1, 1949

By A. J. Shaler, J. Prieto Isaza, J. Wulff

Tantalum metal has a number of unique properties which give it widespread application in modern technology and in research. In electronic apparatus involwing high temperatures in vacuo some of the refractory metals 6ecome brittle. Tantalum retains its ductility at elevated temperatures, and this property, together with its low vapor pressure and its ability to absorb gases, make it important in this field. Its chemical inertness in the presence of acids, halogens, and other corrosive media, makes it useful in chemical apparatus and in neuro and orthopedic surgical applications. As an addition to tungsten carbide in steel-cutting grades of cemented-carbide tools, the carbides of tantalum and of its sister element colum-bium have found considerable use. The present-day method1 of manufacturing tantalum is to sinter a powder compact of the metal in vacuo. Because tantalum-columbium alloys are difficult to work and since tantalum ores almost always contain columbium, the two metals must be separated chemically, the products of the separation being generally in the form of potassium tantalum fluoride and potassium columbium oxyfluoride. These salts are used in fused-salt electrolytic baths from which coarse metallic powder is deposited as a sponge at the cathode. Finer powder can be made from the coarse product or from tantalum scrap by first submitting it to an embrittling heat treatment in hydrogen and then crushing it. The fine hydrogen-containing powder may subsequently be degassed in vacuo at a high temperature. Prompted by the success of others2,3 in the magnesium reduction of titanium and zirconium halides; one of the authors undertook4 an investigation of the thermochemistry of the reaction between solid magnesium and gaseous tantalum penta-chloride, a subject which had not previously been studied. He found that the heat of formation of tantalum pentachloride is approximately 364,250 cal per mol at temperatures lower than the melting point of magnesium. A value of 83 units was found for the standard entropy at these temperatures. With these values, it was shown that magnesium and tantalum pentachloride are capable of reacting exo-thermically at temperatures less than the melting point of magnesium, and that no great violence is to be expected when these substances are heated together. The exothermic nature of the reaction indicated that the Drocess should be efficient and should not require much externally applied energy. Tantalum pentachloride is not commonly made commercially, and any process using it therefore involves the subsidiary problem of producing and handling this substance. A series of experiments was carried out in which dried chlorine saturated with carbon tetrachloride was passed over heated tanta-

Jan 1, 1949

By R. F. Stahl, W. A. Martin

A marked gravitational segregation of liquid has been observed to take place in a number of volumetric fields toward the later stages of their oil-producing periods. This phenomenon has been pronounced in thick, highly permeable sand formations such as those of the wilcox zone in Oklahoma City. This observation has prompted considerable research directed toward the semiquantitative determination of the equilibrium saturation distribution of oil vertically throughout a formation at final depletion. In this paper, data are also presented showing the transient distribution of liquid at different stages of the depletion period. Other experimental results show the effect of temperature on the drainage rates of water, Wilcox crude oil, and a close-cut heptane fraction. Intermittent drainage of liquid produced saturation gradients that might well be expected from the flow theories involved, Yields of the various liquids varied from 50 to 75 per cent of the original fluid content of the sand-packed (4 in. by 8 ft.) vertical tube. Introduction In certain volumetric Oil fields the performance of the reservoir during the latter part Of its producing life is governed to a large extent by the downward movement of liquid due to the force of gravity. This is especially true of formations having thick or tilting beds of uniformly high permeability, free of shale breaks. Laverett4 and Katz3 have presented original data and discussed the theory relating to the capillary and gravitational forces acting On liquids contained in a sand body. These investigators have pointed out the importance of such studies in the estimation of future reserves as well as the original fluid content of a reservoir. In this previous work, no data have been reported showing the history of saturation distributions during the drainage period. Since a knowledge Of these transients is helpful in obtaining crude Oil from such a reservoir, the authors have obtained these data during this investigation. Experimental Apparatus The drainage tests were carried out in two vertical tubes, 8 ft. high and consisting of 2-in. and 4-in. standard wrought-iron pipe, respectively. Each tube was equipped with a water jacket, which could be kept virtually isothermal ( ± 1.0ºF.). A diagrammatic sketch of the 4-in. tube and its auxiliaries is shown in Fig. 1. At 6 in. above the base of the tube, and at every foot above this point, core nipples were inserted through the water jacket. These nipples were closely fitted with steel-plug inserts during each drainage run. At the end of the run, these inserts were removed so that cores could be obtained from the sand-packed tube.

Jan 1, 1943

By L. P. Teas

Although 1930 has been a year of stagnation, proration and curtailment, the Gulf Coast has measured up to its tradition in the matter of interesting and significant discoveries. Only 2 domes and 7 new structural areas were brought into the producing column in 1930, whereas, in 1929, 13 domes and one structure were added to this list, yet a total of 14 new producing horizons were proved on various domes and structures. On 5 domes new flanks were successfully tested for commercial production. The year 1930 has shown at Barber's Hill that oil in commercial quantities may exist below salt or cap. Numerous wells have been drilled through cap, or even salt itself, into good producing sands. The past year has been particularly notable in the interest and in the number of deep holes drilled. Two wells have gone below 8000 ft. in each of the states of Texas and Louisiana, and in the two states together 14 wells have gone below 7000 ft At the beginning of the year only one well was producing below 6000 ft. in coastal Texas, while at its end, 19 wells were producing or had produced. Geophysical discoveries and activity on the Coast have waned and this type of work has moved further inland. The peaks of production at Pettus, Barber's Hill, Raccoon Bend, Refugio, Orchard and at Humble, in Texas; and at Lake Barre, Port Barre, Black Bayou, White Castle and Vinton in Louisiana, were seen this year. These were new peaks for Humble and Vinton, of course, these fields having previously gone through periods of peak flank production. In Table 1 the completions listed are for the entire month of December in both years. It is remarkable that in 1930, a year of overproduction and proration, there were actually more wildcat operations at its end than at the end of 1929; but it is gratifying that the operations in the proven fields were exactly one-half what they had been at the end of 1929. The price of A grade coastal crude, or oil below 25" Bé., has been cut from $1.30 at the beginning of the year to $1.00 at its close; and B grade, or oil above 25o Bé., has been reduced from a price range of $1.15 to $1.63 down to a range of from $0.75 to $1.22. In spite of these reductions there has been no proration program on the Coast. Systematic

Jan 1, 1931

By O. B. Ellis, Eric R. Jette, John Chipman

In the study of the chemical reactions orcurring in the open-hearth furnace, it is frequently assumed that a condition of equilibrium between slag and metal is attained. In order to test this assumption it is necessary to have dependable operating data as well as an exact knowledge of the equilibrium state. Considerable progress has already been made in the study of slag-metal equilibria, notably in the earlier work of Hertyl and of Oberhoffer and Schenck2 and in the more recent researches of Krings and Schack-mann3 and of Koerber and Oelsen.4 None of these investigators, however, have employed basic slags comparable to those encountered in basic open-hearth practice, so that up to the present time our only information regarding the equilibria of these slags is based upon observations drawn from steelmaking practice in which there is little assurance that actual equilibrium was attained. The original plan of this investigation was to secure simultaneous slag and metal samples at intervals during the making of an open-hearth heat, recording the heat history in detail and obtaining complete allalyses of slag and metal, then to bring these slag samples into equilibrium with liquid iron in the laboratory induction furnace and thus to determine directly whether or not the observed relationships in the open hearth represent conditions approaching equilibrium. This plan was only partly successful. While slags were obtained from the open hearth under satisfactorily recorded conditions and these were re-melted in the laboratory under equilibrium conditions, changes in slag composition, which accompanied the remelting operation, were so great that the final slag from the induction furnace bore little resemblance to its open-hearth parent and the direct comparison was therefore abnndoned. The results, however, lie within a range of slag composition that is of interest in the making of low-carbon steel. As far as we are aware, they represent the first published laboratory study of equilibria involving slags that contain all the con stituents of basic open-hearth slag. Experimental Heats The first set of measurements on slag-metal equilibrium was made in the Research Laboratories of the American Rolling Mill Co, at Middletown, Ohio. This will be known as series A. The second set was made in the Metallurgical Rescarch Laboratories at Massachusetts Institute of Techology, and will be referred to as series B. Series A.—The induction furnace used has been described. Approximately I kg. of a special ingot iron containing less than

Jan 1, 1941

By B. D. Crawford, S. A. Falconer

ONE of the outstanding achievements in connection with this country's war efforts has been the ability of our mining industry to supply from domestic sources many of the minerals of strategic importance that formerly were obtained principally from abroad. In order to meet the war-born demands for these scarce minerals, it has frequently been necessary to develop special methods for treating ores and waste products hitherto considered too low-grade to be workable; and to improve the efficiency of older beneficiation processes. Important in this respect have been the recent technological advances in the field of froth flotation of nonsulphide minerals. Because of the refractory nature of many of these domestic ores, and, in many cases, the limited available technical data regarding their treatment, much research work has been necessary. The following examples describe the procedures and reagents used, and the results obtained, in certain laboratory flotation investigations conducted by American Cyanamid Company's engineers at the Cyanamid Ore Dressing Laboratory on ores containing such minerals as scheelite, manganese oxides and carbonate, ilmenite, brookite, kyanite, garnet, spodumene, mica, feldspar, celestite, fluorite, chromite, corundum, and cassiterite. In presenting these data, we wish to point out that many of the minerals listed have previously been tested, and their amenability to flotation reported, by other investigators-notably those of the United States Bureau of Mines. In some instances the procedures and reagents used in the treatment of some of the following described ores follow rather well-established lines, and with one or two exceptions, the reagents used were well known. However, many of the ores tested did not respond well to simple conventional procedures and it was necessary to adopt special methods of conditioning and desliming, reversal of the usual order of floatability of some of the minerals, multiple cleaning, etc., in order to secure separations. Except where otherwise noted, all numbered and trade-marked reagents mentioned in this paper are marketed by the American Cyanamid Co. or the American Cyanamid and Chemical Corporation. TUNGSTEN ORES Tungsten minerals, vitally important in the war industries of the United States, rank high in the list of those we formerly had to import in order to supply our needs. Most of our domestic ores of tungsten contain scheelite as the valuable mineral. Today there are in the neighborhood of twelve tungsten operations in this country where flotation is used as the main or accessory form of benefication. It has, of course, been known for some time that scheelite and other tungsten minerals respond to treatment by flotation.

Jan 1, 1944

By John Chipman, Eric R. Jette, O. B. Ellis

In the study of the chemical reactions orcurring in the open-hearth furnace, it is frequently assumed that a condition of equilibrium between slag and metal is attained. In order to test this assumption it is necessary to have dependable operating data as well as an exact knowledge of the equilibrium state. Considerable progress has already been made in the study of slag-metal equilibria, notably in the earlier work of Hertyl and of Oberhoffer and Schenck2 and in the more recent researches of Krings and Schack-mann3 and of Koerber and Oelsen.4 None of these investigators, however, have employed basic slags comparable to those encountered in basic open-hearth practice, so that up to the present time our only information regarding the equilibria of these slags is based upon observations drawn from steelmaking practice in which there is little assurance that actual equilibrium was attained. The original plan of this investigation was to secure simultaneous slag and metal samples at intervals during the making of an open-hearth heat, recording the heat history in detail and obtaining complete allalyses of slag and metal, then to bring these slag samples into equilibrium with liquid iron in the laboratory induction furnace and thus to determine directly whether or not the observed relationships in the open hearth represent conditions approaching equilibrium. This plan was only partly successful. While slags were obtained from the open hearth under satisfactorily recorded conditions and these were re-melted in the laboratory under equilibrium conditions, changes in slag composition, which accompanied the remelting operation, were so great that the final slag from the induction furnace bore little resemblance to its open-hearth parent and the direct comparison was therefore abnndoned. The results, however, lie within a range of slag composition that is of interest in the making of low-carbon steel. As far as we are aware, they represent the first published laboratory study of equilibria involving slags that contain all the con stituents of basic open-hearth slag. Experimental Heats The first set of measurements on slag-metal equilibrium was made in the Research Laboratories of the American Rolling Mill Co, at Middletown, Ohio. This will be known as series A. The second set was made in the Metallurgical Rescarch Laboratories at Massachusetts Institute of Techology, and will be referred to as series B. Series A.—The induction furnace used has been described. Approximately I kg. of a special ingot iron containing less than

Jan 1, 1941

By A. A. Smith, J. S. Smart

THE elements silver, cadmium, tin, antimony and tellurium either are found as impurities in commercial coppers or are intentionally added to produce coppers for special uses, When present in small quantities, each of these metals exerts a significant effect on the properties of copper, but despite considerable experience and investigation much remains to be learned about their specific behavior. The presence of extraneous elements, particularly oxygen, complicates the study of individual additions of impurities in the range 0 to 0.05 per cent, and the use of high-purity copper has been found extremely helpful in circumventing these difficulties. It has also been found that individual behavior can be satisfactorily determined from measurements of two commercially important properties, conductivity and softening temperature, according to methods that have been described previously.1,2 Data of this type, obtained in the course of a general investigation of the effects of impurities on the properties of both oxygen-bearing and oxygen-free copper are presented herewith. All samples except those containing cadmium were prepared as 3/8-in. continuously cast oxygen-free rod from pure copper and weighed amounts of a similarly synthesized master alloy. Composition was checked by chemical methods, which in every case verified the calculated analyses. Test wires were cold-drawn one B. and S. number per pass on a string-up machine using four 30-min. 600°C. anneals at 0.3125, 0.257, 0.204 and 0.162 in. and a final cold reduction of 75 per cent to 0.081 in. Some oxygen-bearing samples were produced directly from the 3/8-in. oxygen-free rods by diffusion from a surface scale at 850°C. and drawn to size as listed above, but most of the alloys were remelted in pure graphite and cast through air into a I-in. round mold, The slugs were then hot-rolled to 5/16 in., drawn to 0.162 in., annealed as listed above, and drawn to 0.081 inch. Conductivity wires were annealed for I hr. at 100°C. intervals between 300° and 800°F., using a hydrogen atmosphere for oxygen-free samples and purified nitrogen for the oxygen-bearing type, All samples were quenched from the annealing temperature in 10 per cent H2SO4 and conductivity was measured on a Hoopes bridge that had been checked against a Kelvin bridge. The softening temperatures represent the half-hard stage of the annealing curve as determined by a standard procedure.1 EFFECT OF SILVER Numerous excellent studies of the argentiferous coppers are found in the literature, and these have been adequately

Jan 1, 1943

By L. Wahl, M. Allard, B. Trentini

REMOVAL of sulfur in steelmaking is presently a problem of utmost importance as requirements on final sulfur contents in finished steels become increasingly strict. This is in spite of often increased sulfur contents in the fuels used during the different stages of steel processing. According to local conditions or current economic factors, sulfur can be removed during one or more of the processing operations; for instance, in a blast furnace operated under high temperatures and with a high slag basicity ratio and also by means of high inputs of manganese into the burden. These methods of proceeding are, however, expensive and in contradiction with the acid practice which is gradually being developed owing to the fact that it allows coke and lime savings and usually permits an increase of productivity. In the melting-shop, desulfurization can proceed in the open-hearth or electric furnace with one or several very basic slags, or with special prefused slags (Perrin process) mixed with steels poured from the open-hearth, electric furnace, or converter. Liquid pig iron has also been treated separately before being used in the melting shop, in order to reduce high sulfur contents. This external desul-furization has been developed in Europe for the basic Bessemer Thomas process, which is again in favor owing to the great flexibility of such installations and to the fact that the steel produced is not polluted by impurities coming from the scrap. Since the basic Bessemer process, as usually practiced, has a low desulfurizing power, external desulfurization is generally carried out in ladles by means of alkalies such as soda ash. This method, which has the advantage of being simple and costing little, has only a medium desulfurizing power, which implies the necessity for repeating the operation several times when a substantial amount of sulfur has to be removed or when very low sulfur contents are desired. Thermal losses are high and there is a considerable decrease in output. Moreover, the resulting fluid and corrosive slag, which is extremely difficult to eliminate, attacks the refractory linings of the mixers and steel furnaces. Therefore, it seems necessary to devise a simple method for external desulfurization which would not only remove substantial quantities of sulfur from the hot metal coming from an acid blast furnace, but which would also bring the sulfur contents down to the low level required in the making of high quality steel and iron. Principle of the Process In this paper a new method will be described for desulfurizing hot metal. It has been perfected by

Jan 1, 1958

By S. A. Falconer

One of the outstanding achievements in connection with this country's war efforts has been the ability of our mining industry to supply from domestic sources many of the minerals of strategic importance that formerly were obtained principally from abroad. In order to meet the war-born demands for these scarce minerals, it has frequently been necessary to develop special methods for treating ores and waste products hitherto considered too lowgrade to be workable; and to improve the efficiency of older beneficiation processes. Important in this respect have been the recent technological advances in the field of froth flotation of nonsulphide minerals. Because of the refractory nature of many of these domestic ores, and, in many cases, the limited available technical data regarding their treatment, much research work has been necessary. The following examples describe the procedures and reagents used, and the results obtained, in certain laboratory flotation investigations conducted by American Cyanamid Company's engineers at the Cyanamid Ore Dressing Laboratory on ores containing such minerals as scheelite, manganese oxides and carbonate, ilmen-ite, brookite, kyanite, garnet, spodumene, mica, feldspar, celestite, fluorite, chromite, corundum, and cassiterite. In presenting these data, we wish to point out that many of the minerals listed have previously been tested, and their amenability to flotation reported, by other investigators—notably those of the United States Bureau of Mines. In some instances the procedures and reagents used in the treatment of some of the following described ores follow rather well-established lines, and with one or two exceptions, the reagents used were well known. However, many of the ores tested did not respond well to simple conventional procedures and it was necessary to adopt special methods of conditioning and desliming, reversal of the usual order of floatability of some of the minerals, multiple cleaning, etc., in order to secure separations. Except where otherwise noted, all numbered and trade-marked reagents mentioned in this paper are marketed by the American Cyanamid Co. or the American Cyanamid and Chemical Corporation. Tungsten ORes Tungsten minerals, vitally important in the war industries of the United States, rank high in the list of those we formerly had to import in order to supply our needs. Most of our domestic ores of tungsten contain scheelite as the valuable mineral. Today there are in the neighborhood of twelve tungsten operations in this country where flotation is used as the main or accessory form of benefication. It has, of Course, been known for some time that scheelite and other tungsten minerals respond to treatment by flotation.

Jan 1, 1947