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By J. F. Fidiam, T. F. Ford, A. G. Loomis

It is only within the past 10 years that serious attempt appears to have been made to improve rotary drilling fluids by the application of the principles of colloid chemistry, although the use of chemicals to control the rheological properties of clay slips has long been known in the ceramic industry. The main difficulty apparently lay in the lack of a complete analysis of all of the functions of a drilling fluid in the drilling of the well, together with the lack of adequate consideration of how colloid science could be applied to secure these ends, and particularly how apparent antithetical properties of the fluid could be compromised. Thus one analvsisl of the many requirements of a drilling fluid proved conclusively that the viscosity should be low, in order that cuttings and entrained gas might be eliminated effi-ciently in the settling ditch, while the loss in carrying capacity accompanying low viscosity could be regained by increasing either the density of the mud or the upward velocity of the mud stream in the annular space of the well, and the danger of sticking of the drill stem due to rapid settling in case of enforced suspension of drilling operations could be eliminated by enhancing the thixotropic properties of the fluid. The desired properties of the drilling fluid having thus been established, it was a natural step to treat the fluid with vis-cosity-reducing chemicals, such as salts of weak organic acidsl for example, sodium tannate or gallate—and to adjust the pH to the alkaline side to such a degree of thixo-tropy as would give low viscosity and low yield point under the conditions of flow prevailing in the settling ditch, but rapid gelation and high yield point when quiescent in the annular space during shutdowns. In fact, flow in the settling ditch should be just short of turbulent while flow in the well, together with the flow of mud past the cuttings, is practically always turbulent. The use of chemicals other than those mentioned, such as Calgon (sodium hexametaphosphate) and certain other phosphates together with sodium tannate, has now become standard practice and it is the consensus that this method of treatment has proved to be an important step in the development of the art of drilling oil wells. It is safe to assume that the application of colloid chemical principles can also help in solving other outstanding problems of drilling fluids, such as the development of cheaper and more efficient viscosity reducers ; the development of chemicals that do not lose their effectiveness in a short time during drilling operations; the finding of chemicals to preserve the plastering properties of muds when concentrated brines are encountered or in drilling through salt beds; improvement in the plastering properties of poor muds by further defloc-culation, and, conversely, the prevention of excessive deflocculation of certain marine shales sometimes encountered; the preparation of muds suitable for the successful drilling of heaving shale formations; the finding 0f chemicals to treat the mud to prevent or to diminish lost circulation; the development 0f muds that will not impair 6

Jan 1, 1941

By T. F. Ford, J. F. Fidiam, A. G. Loomis

It is only within the past 10 years that serious attempt appears to have been made to improve rotary drilling fluids by the application of the principles of colloid chemistry, although the use of chemicals to control the rheological properties of clay slips has long been known in the ceramic industry. The main difficulty apparently lay in the lack of a complete analysis of all of the functions of a drilling fluid in the drilling of the well, together with the lack of adequate consideration of how colloid science could be applied to secure these ends, and particularly how apparent antithetical properties of the fluid could be compromised. Thus one analvsisl of the many requirements of a drilling fluid proved conclusively that the viscosity should be low, in order that cuttings and entrained gas might be eliminated effi-ciently in the settling ditch, while the loss in carrying capacity accompanying low viscosity could be regained by increasing either the density of the mud or the upward velocity of the mud stream in the annular space of the well, and the danger of sticking of the drill stem due to rapid settling in case of enforced suspension of drilling operations could be eliminated by enhancing the thixotropic properties of the fluid. The desired properties of the drilling fluid having thus been established, it was a natural step to treat the fluid with vis-cosity-reducing chemicals, such as salts of weak organic acidsl for example, sodium tannate or gallate—and to adjust the pH to the alkaline side to such a degree of thixo-tropy as would give low viscosity and low yield point under the conditions of flow prevailing in the settling ditch, but rapid gelation and high yield point when quiescent in the annular space during shutdowns. In fact, flow in the settling ditch should be just short of turbulent while flow in the well, together with the flow of mud past the cuttings, is practically always turbulent. The use of chemicals other than those mentioned, such as Calgon (sodium hexametaphosphate) and certain other phosphates together with sodium tannate, has now become standard practice and it is the consensus that this method of treatment has proved to be an important step in the development of the art of drilling oil wells. It is safe to assume that the application of colloid chemical principles can also help in solving other outstanding problems of drilling fluids, such as the development of cheaper and more efficient viscosity reducers ; the development of chemicals that do not lose their effectiveness in a short time during drilling operations; the finding of chemicals to preserve the plastering properties of muds when concentrated brines are encountered or in drilling through salt beds; improvement in the plastering properties of poor muds by further defloc-culation, and, conversely, the prevention of excessive deflocculation of certain marine shales sometimes encountered; the preparation of muds suitable for the successful drilling of heaving shale formations; the finding 0f chemicals to treat the mud to prevent or to diminish lost circulation; the development 0f muds that will not impair 6

Jan 1, 1941

By B. H. Sage, R. T. Carter, W. N. Lacey

The phase behavior of a number of binary systems consisting of parafin hydro-carbons has been determined in recent years. In addition, the composition of the coexisting phases of mixtures of crude oil and natural gas has been investigated.~ However, the latter study did not include information concerning the influence of the concentration of a component upon its distribution between two coexisting phases. Owing to the paucity of such information it was considered desirable to investigate in some detail the composition of the coexisting phases in the methane-propane-n-pentane system throughout the greater part of the two-phase region at a tempera-ture of 100°F. Information of this nature also permits the establishment of the critical behavior of this ternary system. Method The compositions of the coexisting phases in this ternary system at 100°F. were deter-mined by withdrawing samples from a pres-sure vessel containing a heterogeneous mixture of the three components that had been brought 10 equilibrium by mechanical agitation at the desired pressure and tem-perature. The samples were withdrawn under such conditions that the equilibrium was not disturbed and the composition of each of the phases was ascertained by means of the conventional low-temperature fractionation procedure. The apparatus employed in this investi-gation was nearly the same as that utilized in an earlier study of the methane-pentane system.~ Several minor modifica-tions in the arrangement of the apparatus were made in the interest of simplifying the procedure and avoiding the possibility of condensation in the tubing connecting the equilibrium apparatus with the analyti-cal equipment. The pressures were meas-ured by means of a pressure balance with a precision of 0.5 lb. per sq. in. It is believed that the equilibrium pressure was ascer-tained with an uncertainty of not more than 2 lb. per sq. in., even though small varia-tions in pressure obtained during the withdrawal of the samples. The tempera-ture of the equilibrium equipment was maintained by use of an automatically controlled oil bath. The bath temperature was determined by means of a copper-constantan thermocouple, the electromo-tive force being determined by means of a potentiometric circuit of such a nature as to reduce the uncertainty of the tempera ture to less than O.I f. The fractionating column employed in the determination of the composition of the gas phase had a diameter of 0.12 in. and was approximately 4 ft. long, while the column employed in the analysis of the liquid phase was 0.18 in. in diameter and about 5 ft. long. Each column was equipped with the conventional constant-volume receivers, which were maintained at a constant temperature by means of an automatically controlled oil bath. In nearly every case the distillation in thr neighborhood of the transition between

Jan 1, 1941

By W. N. Lacey, R. T. Carter, B. H. Sage

The phase behavior of a number of binary systems consisting of parafin hydro-carbons has been determined in recent years. In addition, the composition of the coexisting phases of mixtures of crude oil and natural gas has been investigated.~ However, the latter study did not include information concerning the influence of the concentration of a component upon its distribution between two coexisting phases. Owing to the paucity of such information it was considered desirable to investigate in some detail the composition of the coexisting phases in the methane-propane-n-pentane system throughout the greater part of the two-phase region at a tempera-ture of 100°F. Information of this nature also permits the establishment of the critical behavior of this ternary system. Method The compositions of the coexisting phases in this ternary system at 100°F. were deter-mined by withdrawing samples from a pres-sure vessel containing a heterogeneous mixture of the three components that had been brought 10 equilibrium by mechanical agitation at the desired pressure and tem-perature. The samples were withdrawn under such conditions that the equilibrium was not disturbed and the composition of each of the phases was ascertained by means of the conventional low-temperature fractionation procedure. The apparatus employed in this investi-gation was nearly the same as that utilized in an earlier study of the methane-pentane system.~ Several minor modifica-tions in the arrangement of the apparatus were made in the interest of simplifying the procedure and avoiding the possibility of condensation in the tubing connecting the equilibrium apparatus with the analyti-cal equipment. The pressures were meas-ured by means of a pressure balance with a precision of 0.5 lb. per sq. in. It is believed that the equilibrium pressure was ascer-tained with an uncertainty of not more than 2 lb. per sq. in., even though small varia-tions in pressure obtained during the withdrawal of the samples. The tempera-ture of the equilibrium equipment was maintained by use of an automatically controlled oil bath. The bath temperature was determined by means of a copper-constantan thermocouple, the electromo-tive force being determined by means of a potentiometric circuit of such a nature as to reduce the uncertainty of the tempera ture to less than O.I f. The fractionating column employed in the determination of the composition of the gas phase had a diameter of 0.12 in. and was approximately 4 ft. long, while the column employed in the analysis of the liquid phase was 0.18 in. in diameter and about 5 ft. long. Each column was equipped with the conventional constant-volume receivers, which were maintained at a constant temperature by means of an automatically controlled oil bath. In nearly every case the distillation in thr neighborhood of the transition between

Jan 1, 1941

By D. T. MacRoberts

This paper embodies the results of theoretical studies concerning gas reservoirs, especially the effect of drilling programs of various intensities upon pressure depletion and ultimate recoveries. The primary objective has been to determine the net quantity of recoverable gas that could be obtained as a result of each additional well, in comparison with the gas . that might be secured from a single well ideally placed with respect to both acreage and geological structure. No method is yet known whereby the relative merits of intensive and sparse drilling can be compared experimentally; a reservoir must either be drilled closely or developed with wide spacing, but both programs cannot be conducted simultaneously. Hence, the analytical method seems to be the only approach to the problem. While the present state of our theoretical knowledge does not offer a precise solution to the problem of gas flow in sand bodies, it takes such appropriate cognizance of the limitations of the methods used as to restrict any answer obtained to the realm of engineering accuracy. In solving the problem for the average gas field, it was found that practically the same answers resulted as to pressure distribution, regardless of the size of the drainage radius, even though the latter was assumed to vary from a few feet as a minimum to that of the entire reservoir as a maximum. Such limits represent extreme possibilities; therefore, the practical conditions that are associated with normal development programs, in which wells are placed in the center of tracts varying in size from 40 to 640 acres, will of necessity result in less extreme variations than those indicated in the tables accompanying this paper. Stated more concisely, the amount of gas unrecovered at abandonment (of the particular field used for illustrative purposes) will lie somewhere between 4.6 and 6 per cent of the total original content, no matter how intensively the field is drilled. Gas reservoirs may be divided into two general types, those in which the energy is intrinsic, and those of which the energy is extrinsic. † The first type contains energy in the form of a compressed gas, which expands

Jan 1, 1938

By H. H. Evinger, M. Muskat

Although the shooting of oil wells for the purpose of increasing production has been practiced since 1866, present-day shooting technique has been arrived at almost wholly by a process of trial and error. The difficulties attending either a theoretical analysis of the problem or an experimental attack become apparent when one actually embarks on a theoretical investigation or attempts to formulate an intelligent experimental program. The literature on the subject consists mainly of descriptions of current practice, scattered eye-witness accounts of events following the shooting of a well, and vague speculations on the mechanical processes involved. In contrast to quarry blasting, the results of oil-well shooting cannot be determined by means of visual inspection, and it is perhaps for this reason that only one attempt at what approaches a direct experimental attack has been reported in the literature.' In these experiments, charges of liquid nitroglycerin were exploded in holes drilled in a sandstone outcrop. In order to observe the character and extent of the resulting fractures, the rock was blasted away so as to expose the original shot holes. After all this had been done it was found impossible to distinguish the fracturing due to the original shots from that due to the subsequent blasting. The enlargement of the holes due to the pulverizing action of the shots was measured and an attempt was made to determine the effectiveness if sand tamping. Only five shots were made and few definite conclusions could be drawn. Some small-scale experiments to deter-mine the effect of tamping were performed by Snelling and IIalL2 Small charges (zo grams) of dynamite were detonated at the bottom of a cylindrical hole in a lead block and the resulting enlargement of the hole was taken as a measure of the effectiveness of the explosion. It was found that when the shot was tamped with a sufficient amount of sand or clay, the volume enlargement was approximately double that found when no stemming had been used. The properties of the explosives have been the subject of much study by the manufacturers, the U. S. Bureau of Mines, and various other agencies. For example, velocities of detonation for many commercial explosives are to be found in the Blasters' Handbook, issued by the Du Pont company. Many other properties are given in a treatise on the subject by Naoum.~ The shock wave that accompanies the detonation of high explosives has been studied photographically by Payman4 and others. The hydrodynamical theory of the shock wave has received much attention, and an extended theoretical treatment is given by Bateman.6 Two aspects of the well-shooting problem will be considered in this paper; namely, the fracturing of subsurface strata, and possible damage to casing. With respect to the former of these, several calculations have been made giving the stresses in the rocks surrounding the shot. In order to arrive at numerical results at all, however, it is necessary to introduce a great many simplifying

Jan 1, 1941

By M. Muskat, H. H. Evinger

Although the shooting of oil wells for the purpose of increasing production has been practiced since 1866, present-day shooting technique has been arrived at almost wholly by a process of trial and error. The difficulties attending either a theoretical analysis of the problem or an experimental attack become apparent when one actually embarks on a theoretical investigation or attempts to formulate an intelligent experimental program. The literature on the subject consists mainly of descriptions of current practice, scattered eye-witness accounts of events following the shooting of a well, and vague speculations on the mechanical processes involved. In contrast to quarry blasting, the results of oil-well shooting cannot be determined by means of visual inspection, and it is perhaps for this reason that only one attempt at what approaches a direct experimental attack has been reported in the literature.' In these experiments, charges of liquid nitroglycerin were exploded in holes drilled in a sandstone outcrop. In order to observe the character and extent of the resulting fractures, the rock was blasted away so as to expose the original shot holes. After all this had been done it was found impossible to distinguish the fracturing due to the original shots from that due to the subsequent blasting. The enlargement of the holes due to the pulverizing action of the shots was measured and an attempt was made to determine the effectiveness if sand tamping. Only five shots were made and few definite conclusions could be drawn. Some small-scale experiments to deter-mine the effect of tamping were performed by Snelling and IIalL2 Small charges (zo grams) of dynamite were detonated at the bottom of a cylindrical hole in a lead block and the resulting enlargement of the hole was taken as a measure of the effectiveness of the explosion. It was found that when the shot was tamped with a sufficient amount of sand or clay, the volume enlargement was approximately double that found when no stemming had been used. The properties of the explosives have been the subject of much study by the manufacturers, the U. S. Bureau of Mines, and various other agencies. For example, velocities of detonation for many commercial explosives are to be found in the Blasters' Handbook, issued by the Du Pont company. Many other properties are given in a treatise on the subject by Naoum.~ The shock wave that accompanies the detonation of high explosives has been studied photographically by Payman4 and others. The hydrodynamical theory of the shock wave has received much attention, and an extended theoretical treatment is given by Bateman.6 Two aspects of the well-shooting problem will be considered in this paper; namely, the fracturing of subsurface strata, and possible damage to casing. With respect to the former of these, several calculations have been made giving the stresses in the rocks surrounding the shot. In order to arrive at numerical results at all, however, it is necessary to introduce a great many simplifying

Jan 1, 1941

By W. L. Fink, L. A. Willey

This paper is the nineteenth of a series from the Aluminum Research Laboratories, presenting the results of the investigations of equilibrium relations in aluminum-base alloys made from electrolytically refined aluminum. In previous papers equilibrium relations have been determined and correlated for 12 binary systems. Equilibrium relations have also been determined for portions of the aluminum corners of three ternary systems (aluminum-iron-silicon, aluminum-magnesium-silicon and aluminum-copper-magnesium). The object of the present paper and those to follow is to increase our knowledge of the aluminum corner of the more important ternary systems. In 1926 Dix and Keith † suggested a new method for designating the phases encountered in alloy systems. The system has been used to a very limited extentl,2,3 The system has since been slightly modified and will be used in this and future papers. In the system as modified, a phase is designated by placing in parentheses the chemical symbols of the elements essential to the formation of that phase. The symbols in the parentheses are separated by dashes in order to clearly distinguish them from a chemical formula. Elements that are not necessary to the formation of the phase in question, but which may be present in solid solution, are not indicated in the designation. If two or more phases would have the same designation according to these rules, they are distinguished by prefixing Greek letters, and are definitely identified by X-ray diffraction patterns. Previous Investigations The solid solubility of magnesium in aluminum has been well established by the work of Dix and Keller4, Schmid and Siebe15, and Saldau and Sergeev6. There is no agreement as to the composition of the magnesium constituents at the aluminum end of the binary aluminum-magnesium system. Hanson and Gayler7 report Mg2Al3; Boyer8 found that the alloy

Jan 1, 1937

Page Laboratory Methods...........................127 Special Analytical Methods.......................127 Improvements in the Accuracy of the Vacuum-fusion Method for the Determination of Oxygen in Steel....................127 Quantitative Spectrochemical Analysis of Mixtures of Gases.......131 Oxygen Samples from Open-hearth Bath...............133 Rapid Analysis of Sample for Alumina.................139 Accurate Carbon Analyses in Low-carbon Steel.............139 Laboratory Technique for Study of Reactions Involving Liquid Metal. . . . 142 Rotating Liquid Crucibles......................143 Stationary Crucibles.........................145 Jones and Laughlin Experimental Furnace...............148 Vacuum Melting..........................149 Measurement of Temperature of Liquid Iron and Steel;..........149 Pouring and Teeming Temperatures..................149 Bath Temperatures.........................151 Plant Methods.............................154 Methods of Studying Slags.......................154 Sampling Slag in the Open Hearth..................155 Viscosity of Open-hearth Slags....................155 Petrographic Examination of Slag...................156 Statistical Methods Applied to Study and Control of Chemical Relations in Bath...............................166 Rapid Method of -Correlation Applicable to Study of Steelmaking Reactions............................166 INTRODUCTION On Thursday morning, Feb. 16, 1939, a round table discussion was held on the subject of Experimental Methods in the Study of Steelmaking. Dr. John Chipman, Professor of Metallurgy at the Massachusetts Institute of Technology, and chairman of the A.I.M.E. Committee on Physical Chemistry of Steelmaking, presided. In opening the meeting, the chairman said: "The purpose of this round table is to discuss methods of study by which more and better information on the fundamentals of steelmaking can be obtained. It was thought that a round table discussion rather than a symposium would furnish the best opportunity for those actually using various methods of study to get together and discuss their common problems. For this reason attention will be focused upon methods of study rather than upon their results. We want new and current and up-to-date discussion.

Jan 1, 1940

Page Laboratory Methods...........................127 Special Analytical Methods.......................127 Improvements in the Accuracy of the Vacuum-fusion Method for the Determination of Oxygen in Steel....................127 Quantitative Spectrochemical Analysis of Mixtures of Gases.......131 Oxygen Samples from Open-hearth Bath...............133 Rapid Analysis of Sample for Alumina.................139 Accurate Carbon Analyses in Low-carbon Steel.............139 Laboratory Technique for Study of Reactions Involving Liquid Metal. . . . 142 Rotating Liquid Crucibles......................143 Stationary Crucibles.........................145 Jones and Laughlin Experimental Furnace...............148 Vacuum Melting..........................149 Measurement of Temperature of Liquid Iron and Steel;..........149 Pouring and Teeming Temperatures..................149 Bath Temperatures.........................151 Plant Methods.............................154 Methods of Studying Slags.......................154 Sampling Slag in the Open Hearth..................155 Viscosity of Open-hearth Slags....................155 Petrographic Examination of Slag...................156 Statistical Methods Applied to Study and Control of Chemical Relations in Bath...............................166 Rapid Method of -Correlation Applicable to Study of Steelmaking Reactions............................166 INTRODUCTION On Thursday morning, Feb. 16, 1939, a round table discussion was held on the subject of Experimental Methods in the Study of Steelmaking. Dr. John Chipman, Professor of Metallurgy at the Massachusetts Institute of Technology, and chairman of the A.I.M.E. Committee on Physical Chemistry of Steelmaking, presided. In opening the meeting, the chairman said: "The purpose of this round table is to discuss methods of study by which more and better information on the fundamentals of steelmaking can be obtained. It was thought that a round table discussion rather than a symposium would furnish the best opportunity for those actually using various methods of study to get together and discuss their common problems. For this reason attention will be focused upon methods of study rather than upon their results. We want new and current and up-to-date discussion.

Jan 1, 1940

By Gerhard Derge, J. Warren Stewart

Extrusion processes are used in the commercial production of a wide variety of products, as indicated by the review presented a few years ago by D. K. Crampton.' Most writers have confined themselves to a general description of the equipment and products and the engineering aspects of the process. The few studies that have dealt with the metallurgical side of extrusion have been concerned primarily with an examination of the mode of flow of the metal during extrusion. This has been accomplished by the use of composite billets, by scribing grids on symmetrical sections of billets and observing the change of dimensions in the gridwork, or by examining microstructures in extruded sections.2"8 Ariotlier limitation of these original studies is that they were confined to the extrusion of very simple shapes, usually rods having a diameter of about one-fourth that of the billet. Tin is particularly well suited to the extrusion of collapsible tubes and similar shapes in which the extruded section is very small in comparison to the diameter of the billet or slug. In modern production, impact extrusion methods are generally employed, therefore the thickness of the slug is small compared to its diameter. Under these conditions the process differs considerably from the processes that have been most fully described in the literature, and it is known that the quality of the product is very sensitive to slight variations in any one of the many variable factors involved, such as coinposition and structure of the alloy, rate of extrusion, temperature, shape of punch and die. An exhaustive examination of all of the above-mentioned problems promises to produce so many data that it seems advisable to initiate the reports at this time, even though all of the factors outlined have not been examined fully, and to confine this paper to a description of the apparatus and method. Only tin and its alloys with small amounts of copper have been considered. These are the alloys most commonly used in this country for the production of the type of articles already described.

Jan 1, 1940

By Gerhard Derge, J. Warren Stewart

Extrusion processes are used in the commercial production of a wide variety of products, as indicated by the review presented a few years ago by D. K. Crampton.' Most writers have confined themselves to a general description of the equipment and products and the engineering aspects of the process. The few studies that have dealt with the metallurgical side of extrusion have been concerned primarily with an examination of the mode of flow of the metal during extrusion. This has been accomplished by the use of composite billets, by scribing grids on symmetrical sections of billets and observing the change of dimensions in the gridwork, or by examining microstructures in extruded sections.2"8 Ariotlier limitation of these original studies is that they were confined to the extrusion of very simple shapes, usually rods having a diameter of about one-fourth that of the billet. Tin is particularly well suited to the extrusion of collapsible tubes and similar shapes in which the extruded section is very small in comparison to the diameter of the billet or slug. In modern production, impact extrusion methods are generally employed, therefore the thickness of the slug is small compared to its diameter. Under these conditions the process differs considerably from the processes that have been most fully described in the literature, and it is known that the quality of the product is very sensitive to slight variations in any one of the many variable factors involved, such as coinposition and structure of the alloy, rate of extrusion, temperature, shape of punch and die. An exhaustive examination of all of the above-mentioned problems promises to produce so many data that it seems advisable to initiate the reports at this time, even though all of the factors outlined have not been examined fully, and to confine this paper to a description of the apparatus and method. Only tin and its alloys with small amounts of copper have been considered. These are the alloys most commonly used in this country for the production of the type of articles already described.

Jan 1, 1940

By John J. Egan, A. B. Kinzel, Walter Crafts

The demands of the petroleum and chemical industries for steels to be used in pressure vessels and similar structures at artificially low temperatures are continually increasing, and the writing of proper specifications with suitable tests becomes increasingly important. Likewise, the selection of suitable steels for such applications is of increasing concern to the metallurgist. It is generally recognized that highly alloyed steels of the austenitic stainless type retain their properties even at very low temperatures and represent the best technological solution of the low-temperature steel problem. However, in many instances less expensive carbon or low-alloy steels suitable for service within limited temperature ranges are available. The problem thus becomes one of defining the various factors involved in the production and fabrication of these less expensive steels and determining the temperature ranges in which their properties justify engineering application. Most of the applications involve welded structures, and the heat effect of welding as well as the nature of the weld metal are matters of prime concern. The first problem that the metallurgist faces is the determination of the type of test to be used as a criterion of the performance of the steel in low-temperature service. It has been generally recognized that the static properties of steel as determined in the ordinary tensile test undergo a gradual and relatively slight change as the temperature of test is lowered in the range of current interest; i.e., from room temperature to minus 120' C. It is further generally recognized that the behavior of steel under impact involving notch sensitivity is definitely affected at the lower temperatures. While the major subject of this paper is the effect of grain-refining deoxidizers, of low-alloy additions and of welding on the low-temperature notched-bar impact properties, an inquiry into the general behavior of steel under low-temperature impact testing is included. This is a pertinent portion of the investigation and the results thereof are

Jan 1, 1937

By Kenneth B. Ray, George R. Gardner

The application of wet cleaning processes for the beneficiation of bituminous coal has created in some localities a problem in the recovery and disposal of fine solids in the washery water. The maximum allowable concentration of these solids in the washery circuit that is consistent with satisfactory operation of the cleaning units remains a controversial point. It has, however, been generally recognized for a number of years that some degree of control should be exerted over the concentration of such material. Early methods of control involved intermittent or continuous discharge of a portion of the plant slurry into near-by streams or settling ponds, and this persisted even after the adoption of settling tanks or cones. The practice is not always economical, for two reasons: first, because of the waste of coal, and, second, because it is sometimes difficult and expensive to obtain an adequate supply of water. The latter condition often is aggravated by chemical treatment of the make-up water that is necessary to prevent excessive corrosion of plant equipment. The modern approach to this problem has been the adoption of continuous thickening devices. However, because such equipment occupies considerable plant space and is somewhat expensive to construct, the practice of loading these thickeners beyond their rated capacity is widespread, therefore often the performance of such units is not altogether satisfactory. In recent years, European washeries have increased the rate of settling of the fine coal from the slurry by the addition of specially prepared starch solutions. These reagents cause flocculation of the solid particles and thereby increase the rate of sedimentation. The first important work on the flocculation and clarification of coal slurry was done by Henry, who developed the Henry process and used it successfully in Belgian preparation plants. Soon after the initiation in Belgium, the process was introduced into England, where subsequent investigation developed similar processes, which were successfully used in

Jan 1, 1940

By George R. Gardner, Kenneth B. Ray

The application of wet cleaning processes for the beneficiation of bituminous coal has created in some localities a problem in the recovery and disposal of fine solids in the washery water. The maximum allowable concentration of these solids in the washery circuit that is consistent with satisfactory operation of the cleaning units remains a controversial point. It has, however, been generally recognized for a number of years that some degree of control should be exerted over the concentration of such material. Early methods of control involved intermittent or continuous discharge of a portion of the plant slurry into near-by streams or settling ponds, and this persisted even after the adoption of settling tanks or cones. The practice is not always economical, for two reasons: first, because of the waste of coal, and, second, because it is sometimes difficult and expensive to obtain an adequate supply of water. The latter condition often is aggravated by chemical treatment of the make-up water that is necessary to prevent excessive corrosion of plant equipment. The modern approach to this problem has been the adoption of continuous thickening devices. However, because such equipment occupies considerable plant space and is somewhat expensive to construct, the practice of loading these thickeners beyond their rated capacity is widespread, therefore often the performance of such units is not altogether satisfactory. In recent years, European washeries have increased the rate of settling of the fine coal from the slurry by the addition of specially prepared starch solutions. These reagents cause flocculation of the solid particles and thereby increase the rate of sedimentation. The first important work on the flocculation and clarification of coal slurry was done by Henry, who developed the Henry process and used it successfully in Belgian preparation plants. Soon after the initiation in Belgium, the process was introduced into England, where subsequent investigation developed similar processes, which were successfully used in

Jan 1, 1940

By O. C. Ralston, William C. Hunter

DUring experimental study on the separation of a zinc concentrate from the heavy sulfide ores of Jerome, Ariz., a great deal of attention has been given to proper activation of the sphalerite content of the ore. The sphalerite at Jerome contains enough iron to class it as a marmatite, as picked specimens have only about 60 per cent. zinc, whereas pure zinc sulfide contains 67 per cent. zinc. This marmatite in large pieces is black in color, but in dry powdered state is brown. A flotation froth made from it has a silvery black luster in comparison with a brassy luster caused by chalcopyrite which occurs in the same ores. The sample used in most of the experiments described below consisted of about 3000 Ib. of diamond-drill core from the zinc-bearing orebodies of the United Verde mine, and had the following analysis: Per Cent. Per Cent. Oz. peR Ton Cu............... 0.695 Al2O3............ 0.83 Ag................. 1.30 Zn............... 6.17 S................ 43.35 Au................ 0.02 Fe...............36.23 CaO............. 0.46 SiO2............. 9.27 Mineralogically, this analysis is calculated to the following, which is in agreement with the microscopic examination: Per Cent. Per Cent. Chalcopyrite................... 2.0 Schist........................... 3.2 Marmatite..................... 10.32 Quartz........................... 8.2 Pyrite........................ 73.0 Calcite.......................... 0.9 All samples were ground in a laboratory ball mill in order to leave about 3 per cent. on a 200-mesh sieve, fine grinding being essential to liberate the minerals in the ore. Most of the Jerome ores are so intimately crystallized that reasonably complete unlocking by grinding does not take place until 800 mesh is approached. Therefore, the 200-mesh grind adopted contains a considerable amount of locked mineral grains, but not so much as to render impossible the preparation of commercial grades of concentrate.

Jan 1, 1930

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By Donald W. Scott, Nathaniel Arbiter, A. C. Richardson

This paper describes the application of amine flotation to a specific problem—that of increasing the grade of magnetite concentrates derived from an iron ore requiring extremely fine grinding for mineral liberation. Experiments conducted on an iron ore from Wisconsin had shown that concentrates containing 60 to 62 per cent iron and 12 to 14 per cent silica could be produced by magnetic separation. The residual silica occurred as quartz and hornblende, either entrained or locked with magnetite. Most advantageous utilization of the concentrate, however, necessitated that the silica content be reduced to about 5 per cent, equivalent to an iron content of 67.5 per cent. It had been demonstrated that tabling of the magnetic concentrate removed sufficient quartz and hornblende to yield an acceptable concentrate, but disadvantages inherent in tabling dictated that flotation be investigated as a substitute. The goals set for the flotation investigation were: (I) the production of concentrates of about 68 per cent iron content from the magnetic concentrate; (2) an iron recovery of about 85 per cent of that in the feed to flotation; and (3) minimum reagent cost. Both batch and continuous flotation tests were employed; the former, to establish the procedure and the latter to verify it. Although the data were obtained on a specific ore, and with a commercial application in view, it is believed that they have a bearing on other problems where amine flotation is being used or is anticipated. Samples Two samples, designated "(minus 100-mesh magnetic concentrate" and "minus 150-mesh magnetic concentrate," were used for the batch experimental work. They differed only in the degree to which the crude ore was ground prior to magnetic separation. They were stored moist in steel drums in quantities sufficient for all the experimental work reported. This procedure had the advantage of allowing all tests to be made on common samples, but had the disadvantage that the individual flotation samples, because of the difference in storage time, were subject to various stages of surface alteration. Previous work had indicated that common samples were desirable for the batch studies, and it was decided that if these data appeared sufficiently promising the effect of surface alteration could be checked best by continuous tests. The size distributions and the assays of the samples are given in Table I. The minus 150-mesh magnetic concentrate, on which most of the flotation tests were made, assayed 60.9 per cent iron, 13.3 per cent silica, and 0.016 per cent phosphorus. The minus 325-mesh portion represented 78.I per cent of the sample by weight, and assayed 67.9 per cent iron. Thus, the insoluble, mainly silica, was concentrated

Jan 1, 1947

By Arthur F. Taggart

Some years ago, A. M. Gaudin and one of the authors published a paper showing removal of tar acids from solution by sulfides preferentially as compared to gangues (specifically by galena as compared to quartz).' The underlying phenomenon was classed as adsorption, and the paper went on to develop the general thesis that so far as water-soluble frothing and collecting agents in flotation are concerned, the phenomenon of adsorption is one of controlling importance. Adsorption was defined in that paper as "a process of rearrangement of a system, which results in establishing a difference in concentration, as between the interfacial layers and the bulk of the phases, of a substance or substances initially uniformly dispersed in one or several of the phases." The paper went on to develop the relation between adsorption and surface cnergy according to Gibbs' equation (which may be thrown into the form U/c = KdT/dc, where U = excess concentration in surface layer, c = concentration, T = surface tension, and K is a constant), and pointed out that, according to this equation, degree of adsorption and change in surface tension vary directly. The present paper offers a somewhat different definition for the term adsorption; and sets up, in sweeping terms, the generalization that simple chemical reaction underlies the functioning of the flotation reagents which control mineral collection, when these reagents are soluble in and act from solution in the water of the pulp. Adsorption According to the modified definition, adsorption means concentration at an interface between different phases in a heterogeneous system (thus far the definition runs as before), by the action of some mechanism, of which nothing is properly implied in the word, and concerning which the user of the word is probably in entire ignorance. Thus defined,

Jan 1, 1930

By Arthur F. Taggart

The following notes represent significant excerpts from a mass of records of experimental work done in the ore-dressing laborattory 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 agent's. 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.' 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 compared with those used today.

Jan 1, 1930