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By G. K. Burgess

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

Jan 10, 1913

By T. K. Prentice

The January-February number of the Journal of the Chemical Metallurgical and Mining Society of South Africa, 1943, is made up entirely of a discussion of Ball Wear in Cylindrical Mills. Following the principal paper by T. K. Prentice are several remarkably pertinent and carefully prepared discussions. Few persons in this country would be likely to see this publication, and since the information presented is new and of current interest, it seems desirable to abstract and review this publication for the benefit of the members of the A.I.M.E. The purpose of the investigation is stated in the first two paragraphs of Prentice's paper, as follows: Early in 1941, The Chamber of Mines Steel Products, Limited, initiated a series of tests under semi-working scale conditions to determine, if possible, those physical and chemical properties of a ball which make it resistant to wear when used in a cylindrical mill as a grinding medium, with the primary object of incorporating those beneficial qualities in the balls being produced at their works. This paper describes the tests carried out and discusses the results obtained. From these results it was possible to formulate a new theory relating to ball wear in cylindrical mills. This theory is presented in the second portion of this paper. Practical Ball-mill Tests in a Cylindrical Mill Part I of the paper begins with a discussion of the methods used for the manu- facture of grinding balls in South Africa. The following paragraph is of particular interest. The cast steel ingots, 4¼ in. square by 3 ft. 6 in. long, are re-heated in a gas-fired sloping stationary-hearth furnace and then rolled in a six-pass continuous mill into 25/8 in. round billets. Some of these billets are then removed and cut into suitable lengths for forging into 4 in., 3¼ in. , 3 in. or 2½ in. balls by means of three Drop and two Beche hammers, but the greater number, whilst still at about 1,000, pass directly into a set of scroll rolls which produce, in an ingenious manner, finished 3 in. balls direct from the 25/8 in. billets. Except in special cases, all balls are allowed to cool in the atmosphere and are not water quenched. Details of the Tests In order to enable the reader to evaluate properly the results and conclusions in the rest of the paper and in the discussions following the paper, most of the information presented by the author under this heading is quoted: The testing unit was a nominal 30 in. diameter and 18 in. long centre discharge Denver Ball Mill. The ore pulp to the ball mill comprised a small portion of the normal feed to one of the fourteen City Deep 5 ft. 6 in. X 22 ft. tube mills, and the grinding media consisted of the balls under test plus other balls to give the desired load. The running time of the test-mill was divided into approximately equal periods of five days 13½ hours each. The usual procedure was to examine and make up the load

Jan 1, 1947

By T. K. Prentice

The January-February number of the Journal of the Chemical Metallurgical and Mining Society of South Africa, 1943, is made up entirely of a discussion of Ball Wear in Cylindrical Mills. Following the principal paper by T. K. Prentice are several remarkably pertinent and carefully prepared discussions. Few persons in this country would be likely to see this publication, and since the information presented is new and of current interest, it seems desirable to abstract and review this publication for the benefit of the members of the A.I.M.E. The purpose of the investigation is stated in the first two paragraphs of Prentice's paper, as follows: Early in 1941, The Chamber of Mines Steel Products, Limited, initiated a series of tests under semi-working scale conditions to determine, if possible, those physical and chemical properties of a ball which make it resistant to wear when used in a cylindrical mill as a grinding medium, with the primary object of incorporating those beneficial qualities in the balls being produced at their works. This paper describes the tests carried out and discusses the results obtained. From these results it was possible to formulate a new theory relating to ball wear in cylindrical mills. This theory is presented in the second portion of this paper. Practical Ball-mill Tests in a Cylindrical Mill Part I of the paper begins with a discussion of the methods used for the manu- facture of grinding balls in South Africa. The following paragraph is of particular interest. The cast steel ingots, 4¼ in. square by 3 ft. 6 in. long, are re-heated in a gas-fired sloping stationary-hearth furnace and then rolled in a six-pass continuous mill into 25/8 in. round billets. Some of these billets are then removed and cut into suitable lengths for forging into 4 in., 3¼ in. , 3 in. or 2½ in. balls by means of three Drop and two Beche hammers, but the greater number, whilst still at about 1,000, pass directly into a set of scroll rolls which produce, in an ingenious manner, finished 3 in. balls direct from the 25/8 in. billets. Except in special cases, all balls are allowed to cool in the atmosphere and are not water quenched. Details of the Tests In order to enable the reader to evaluate properly the results and conclusions in the rest of the paper and in the discussions following the paper, most of the information presented by the author under this heading is quoted: The testing unit was a nominal 30 in. diameter and 18 in. long centre discharge Denver Ball Mill. The ore pulp to the ball mill comprised a small portion of the normal feed to one of the fourteen City Deep 5 ft. 6 in. X 22 ft. tube mills, and the grinding media consisted of the balls under test plus other balls to give the desired load. The running time of the test-mill was divided into approximately equal periods of five days 13½ hours each. The usual procedure was to examine and make up the load

Jan 1, 1947

By C. C. Wright, T. S. Spicer

A characteristic property of bituminous coal is that upon being heated the coal becomes plastic, evolves volatile gases, and finally solidifies into coke. This fundamental characteristic is of utmost importance and is utilized in the production of the high-temperature coke upon which the steel industry is so dependent; but from the standpoint of operation in the domestic underfeed stoker this coking tendency seriously interferes with efficient combustion. When the coke formed has too strong a structure, certain difficulties result, such as low rate of burning, slow response to heat demand, and, in extreme cases, extinction of fire. The plastic mass prevents uniform distribution of air through the fuel bed and, with strongly coking coals, large dense pieces of coke are produced which have much less reacting surface than was possessed by the original coal. In both ignition and combustion of solid fuels, the extent of the reacting surface is an accelerating factor. Poor combustion permits a surplus of fuel to accumulate in the furnace because the rate of feed and the rate of combustion are not in equilibrium, and this produces an unbalanced condition detrimental to continued automatic service. In order to bum strongly coking coals satisfactorily in a conventional stoker during the three requisite types of operation—continuous, intermittent and hold-fire, frequent attention is necessary. Domestic stokers are defined by the industry as residential stoker heaters that burn 60 lb. of coal or less per hour. With a few exceptions, these units employ the underfeed principle of combustion in which both air and coal move in the same direction up and through the fuel bed. Domestic combustion equipment has difficulty in meeting the problems presented by the several variations in ash and volatile matter, in ash-clinkering tendencies, in coking properties, and in the particle size of bituminous coals. The work of Bituminous Coal Research Inc. at Battelle Memorial Institute has shown that, of these, coking characteristics and the clinkering tendencies have the greatest effect upon the operation of the conventional clinkering type of stoker. Typical coke formations in a clinkering type of underfeed domestic stoker are illustratcd in Fig. I, which shows (A) the ideal fuel bed obtained with a noncoking or free-burning coal; (B) the type of fuel bed formed with a coal that produces a weak coke; and (C) the type of fuel bed obtained with a strongly coking coal. C is characteristic of the fuel bed developed when the average Pennsylvania bituminous coal is burned in an underfeed stoker of conventional type. It is apparent from these pictures that the formation of coke trees will seriously interfere with the efficient automatic combustion of Pennsylvania bituminous coals.

Jan 1, 1942

By T. S. Spicer, C. C. Wright

A characteristic property of bituminous coal is that upon being heated the coal becomes plastic, evolves volatile gases, and finally solidifies into coke. This fundamental characteristic is of utmost importance and is utilized in the production of the high-temperature coke upon which the steel industry is so dependent; but from the standpoint of operation in the domestic underfeed stoker this coking tendency seriously interferes with efficient combustion. When the coke formed has too strong a structure, certain difficulties result, such as low rate of burning, slow response to heat demand, and, in extreme cases, extinction of fire. The plastic mass prevents uniform distribution of air through the fuel bed and, with strongly coking coals, large dense pieces of coke are produced which have much less reacting surface than was possessed by the original coal. In both ignition and combustion of solid fuels, the extent of the reacting surface is an accelerating factor. Poor combustion permits a surplus of fuel to accumulate in the furnace because the rate of feed and the rate of combustion are not in equilibrium, and this produces an unbalanced condition detrimental to continued automatic service. In order to bum strongly coking coals satisfactorily in a conventional stoker during the three requisite types of operation—continuous, intermittent and hold-fire, frequent attention is necessary. Domestic stokers are defined by the industry as residential stoker heaters that burn 60 lb. of coal or less per hour. With a few exceptions, these units employ the underfeed principle of combustion in which both air and coal move in the same direction up and through the fuel bed. Domestic combustion equipment has difficulty in meeting the problems presented by the several variations in ash and volatile matter, in ash-clinkering tendencies, in coking properties, and in the particle size of bituminous coals. The work of Bituminous Coal Research Inc. at Battelle Memorial Institute has shown that, of these, coking characteristics and the clinkering tendencies have the greatest effect upon the operation of the conventional clinkering type of stoker. Typical coke formations in a clinkering type of underfeed domestic stoker are illustratcd in Fig. I, which shows (A) the ideal fuel bed obtained with a noncoking or free-burning coal; (B) the type of fuel bed formed with a coal that produces a weak coke; and (C) the type of fuel bed obtained with a strongly coking coal. C is characteristic of the fuel bed developed when the average Pennsylvania bituminous coal is burned in an underfeed stoker of conventional type. It is apparent from these pictures that the formation of coke trees will seriously interfere with the efficient automatic combustion of Pennsylvania bituminous coals.

Jan 1, 1942

By J. H. Brophy

Experimental evidence in recent years shows that nickel coated hydrogen reduced tungsten powder can be sintered to 98 pct of theoretical density at 1100°C. New data indicate that the sintering rate is the same for nickel contents ranging from 0.125 wt pct (mon-atomic layer) to 5.0 wt pct Ni coated on 0.561. tungsten powder. Nickel tungsten made by coreduction from oxides sinters in a kinetically similar way, but the rate tends to increase with higher nickel contents. The activation of sintering can be accomplished with a minimum amount of nickel if coated powder is used. Transverse rmpture strength was found to increase in specimens containing 0.25 pct Ni as density increased during the initial stage of the carrier-phase sintering process. Upon the onset of grain growth in the final stage, strength was found to decrease. With increasing nickel contents up to 4 pct, strength increased. Maximum strengths in three-point loading were observed at 73,000 psi for 0.25 pct Ni and 93,000 psi for 5 pct Ni. These were comparable to that of massive tungsten recrystal-lized in the presence of nickel and tested in the same way. The results were sensitive to the mode of powder treatment and ductility was negligible in all cases. The study and application of sintered bodies of nickel and tungsten is not new; however, the analysis of the mechanism by which small additions of nickel increase the sintering rate of tungsten promises to Contribute new information regarding sintering theory in general. Initial experimental evidence was presented by the authors showing that nickel-coated hydrogen-reduced tungsten powder may be sintered to 98 pct of theoretical density at 1100°C in 16 hr.' Simultaneously, a kinetic analysis of the process showed that it took place in two distinct stages. In the first stage, nickel evidently served as a carrier phase through which tungsten atoms could move. This stage was kinetically similar to the 'solution-precipitationo step postulated when the carrier phase is liquid3 although in the nickel tungsten case, there is no evidence of the existence of a liquid phase either in equilibrium phase relationships or in mi-crostructures at the temperatures under consideration. In the present work, new data for nickel-coated tungsten powder are offered in support of the proposed mechanism, and a more explicit study of the second stage of densification is presented. Concurrently, the sintering kinetics of these coated powders are compared to Ni-W powder made by coreduction of oxides. In this way the present work can be compared to earlier results in nickel activated sintering of tungsten in which the coreduction process was emplyed. The ultimate utility of such an activated sintering process will be determined to some extent by the mechanical and physical properties of the final prod-

Jan 1, 1962

By Reed W. Hyde

SOME information has been published on the sulphur dioxide concentration of gases from Dwight-Lloyd machines sintering lead ores but most of this relates to the customary practice in which the charge is relatively high in lead and is sintered in two passes over the machine. It is thought, therefore, that the following observations on sintering in one pass a low-lead, low-sulphur charge may be of interest. The data were obtained in sintering lead sulphide flotation concentrates mixed with minus 20-mesh oxide ore, the mixture carrying 16.8 per cent Pb and 5.3 per cent S. No returns were used because of the limited amount of sulphur available as fuel, but the mixture pelletized readily to make a satisfactorily permeable bed on the sintering machine. As there was a possibility that the SO2 might be utilized, a series of runs was made to determine the concentration of SO2 in the gases at different points along the wind box, and the effect on this concentration of changes in the wind-box vacuum. Several runs each were made with vacuums (as measured in inches of water at the wind box) of (1) 2 to 1 3/4 in., (2) 4 to 3 1/2 in. and (3) 6 to 5 1/8 in. The averages of the determinations from each series are platted on the graph (Fig. I). The vertical scale shows the percentage by volume of SO2 (as determined by the Reich method), and the horizontal scale shows the time expressed as percentage of the total sintering time. Sintering was considered to be complete when no SO2 could be detected in the gases. In all cases the depth of bed was 4 1/2 in. and the weight of dry charge per square foot of hearth area was 45.2 lb. Other data are given in the table. The volume of gases corresponding to the several points along the wind box at which SO2 determinations were made could not be measured, but has been calculated from the SO2 content and sulphur elimination on the assumption that the volume is uniform throughout the sintering period. This is not strictly true, as with a given vacuum the volume will usually drop slightly toward the middle of the period and increase toward the end. However, this assumption is a reasonable approximation. Several interesting features are brought out by these data. In general, the published data on SO2 concentration in sintering under ordinary conditions show a high SO2 concentration in the early stages followed by a rapid decrease in concentration and with relatively little SO2 in the gases from the last half or third of the operation. In other words, the greater part of the sulphur elimination is obtained in the first third or half of the period. In these runs, the 6-in. vacuum, which approximates the usual operating condition, gives a curve that follows this customary pattern. Maximum SO2 concentration is obtained 2 ½ min. after

Jan 1, 1942

By P. R. Schmidt, N. J. Themelis

A study zvas made of the deoxidation of copper at 1170°C by injecting a jet of carbon monoxide vertically upwards into the melt. The effects of submersion depth (2 to 20 cm), orifice diameter (& to 5 in.), and gas velocity (100 to 3650 ft per sec) were examined. In the oxygen range 0.1 to 1.0 pct 0, the overall rate was conlrolled by gaseoLcs mass Lransfer. The results were interpreted in terms of a rate coefficient per unit depth which was found to be constant with distance along the jet axis and nearly proportional to the orifice Reynolds number in the range 1000 < NReo < 9100. AS the gas flow rate through an orifice submerged in a liquid is progressively increased, at least three regions of bubble formation may be distinguished. At very low rates, the formation of bubbles is practically a static phenomenon, depending on the orifice diameter, the liquid surface tension, and the densities of the two phases. In this region, the bubble size is constant while the frequency of bubble formation increases with gas flow rate.&apos;-3 At higher flows (500 < NR~, < 2100), the frequency of bubble formation reaches a steady value and the bubble size increases with gas flow rate; when the bubbles issuing from the orifice become so large that they start coalescing to form larger bubbles, the turbulence induced in the liquid by the passage of previous bubbles shatters them into small bubbles of varying size. Finally, for gas velocities in the intermediate and turbulent regions of flow (NR,, > 2100) a tangential separation surface is created around the jet and momentum transfer takes place between it and the surrounding liquid medium. The entrainment of liquid and the resulting deceleration of the gas-liquid dispersion causes the jet to expand forming a characteristic jet cone. The large velocity and density differences between the jet and the liquid result in a high degree of instability and the jet envelope fluctuates rapidly.The characteristic jet cone can be observed by means of time exposure photographs such as those shown in Fig. 1 for an air jet introduced vertically upwards in a water bath. High-speed photography has showns that the gas-liquid dispersion within the cone consists of small bubbles the size of which depends mainly on the jet orifice diameter and Reynolds number. In the laminar region of flow, the following correlation was obtained by Leibson: The results of Liebson et a1.&apos; are plotted in Fig. 2. It can be seen that the region 2000 < NReo c 10,000 is not well-defined experimentally. In the entrance to the fully turbulent region of flow (NR,, = 10,000), the mean bubble diameter decreased to about 0.4 cm and varied only slightly from there on according to the correlation:

Jan 1, 1968

By W. O. Philbrook, A. H. Jolly, T. R. Henry

IN the course of a study of slag-control methods, the authors devised a laboratory technique by which the basicity of basic open-hearth furnace slap could be estimated with sufficient accuracy to make the method of possible interest for slag-control purposes. The process consisted of measuring the slight basicity of an extract of the powdered slag in water. The procedure was presented, for the benefit of those who might care to experiment with it, in a paper submitted in the 1944 McKune Award Contest and presented at the 1944 Open-hearth Conference in Pittsburgh.1 Interest expressed at that meeting and favorable operating experience with the method at a neighboring plant, as described in a related paper by Michael Tenenbaum and C. C. Brown,2 have encouraged us to present further details of the development, technique, and pitfalls of the method and some additional data not included in our first report. At the outset it must be admitted that this method of estimation of slag basicity is not perfect; neither is any other that we know of. It is subject to somewhat greater errors than would be desirable, but compares favorably with other techniques in this respect. It has the disadvantage that it places the final determination of slag basicity in the hands of a laboratory technician rather than the furnace operator, although it can be operated in a control laboratory adjacent to the furnaces. It requires close attention to certain details, as do most laboratory procedures. On the favorable side, it eliminates the "human factor" of personal judgment inherent in estimation from pancakes or powdered samples. The procedure can be placed in practice much more rapidly and presents much less of a training problem than visual methods of estimation. The principle and operation of the method are so simple that it would not be surprising if others have experimented with the same or similar procedures, but we are not aware of any prior publication of details. Our own shop has been operating fairly successfully for several years with the aid of slag pancakes. Since the past year or two have not been favorable for the expenditure of time and energy where the need was not urgent, we have not introduced the new practice for actual slag control and hence do not have extensive operating data. In presenting this method, therefore, we make no claims as to theoretical justification nor guarantees as to practical applicability, but offer it as an empirical observation. We believe it has sufficient merit to warrant its investigation by those just instituting a slag-control program or in search of supplementary methods for judging slag basicity PRINCIPLE OF THE METHOD It is well known that when burnt lime or slaked lime is shaken up with water it

Jan 1, 1945

By W. O. Philbrook, A. H. Jolly, T. R. Henry

In the course of a study of slag-control methods, the authors devised a laboratory technique by which the basicity of basic open-hearth furnace slags could be estimated with sufficient accuracy to make the method of possible interest for slag-control purposes. The process consisted of measuring the slight basicity of an extract of the powdered slag in water. The procedure was presented, for the benefit of those who might care to experiment with it, in a paper submitted in the 1944 McKune Award Contest and presented at the 1944 Open-hearth Conference in Pittsburgh.&apos; Interest expressed at that meeting and favorable operating experience with the method at a neighboring plant, as described in a related paper by Michael Tenenbaum and C. C. Brown,; have encouraged us to present further details of the development, technique, and pitfalls of the method and some additional data not included in our first report. At the outset it must be admitted that this method of estimation of slag basicity is not perfect; neither is any other that we know of. It is subject to somewhat greater errors than would be desirable, but compares favorably with other techniques in this respect. It has the disadvantage that it places the final determination of slag basicity in the hands of a laboratory technician rather than the furnace oper- ator, although it can be operated in a control laboratory adjacent to the furnaces. It requires close attention to certain details, as do most laboratory procedures. On the favorable side, it eliminates the "human factor" of personal judgment inherent in estimation from pancakes or powdered samples. The procedure can be placed in practice much more rapidly and presents much less of a training problem than visual methods of estimation. The principle and operation of the method are so simple that it would not be surprising if others have experimented with the same or similar procedures, but we are not aware of any prior publication of details. Our own shop has been operating fairly successfully for several years with the aid of slag pancakes. Since the past year or two have not been favorable for the expenditure of time and energy where the need was not urgent, we have not introduced the new practice for actual slag control and hence do not have extensive operating data. In presenting this method, therefore, we make no claims as to theoretical justification nor guarantees as to practical applicability, but offer it as an empirical observation. We believe it has sufficient merit to warrant its investigation by those just instituting a slag-control program or in search of supplementary methods for judging slag basicity Principle of the Method It is well known that when burnt lime or slaked lime is shaken up with water it

Jan 1, 1945

By Sylvan Z. Beer

The factors that determine the yield and crystal size in the two-temperature synthesis of A lp were examined. Low yields and small crystals were associated with low temperatures and pressure. Attempts to grow large crystals in the critical and supercritical region of phosphorus were unsuccessful. Crystal size increases markedly at elevated temperatures. Crystals grown at temperatures as high as 1450° C fluo-resced, under uv excitation, at energies close to the estimated band gap of about 2.4 ev, while crystals grown at lower temperatures tended to fluoresce in the red region of the spectrum. Those grown in the supercritical region showed no ALP fluorescence. Heating the high-temperature-grown ALP under vacuum greatly increased its fluorescence efficiency and moved the emission peak to higher energies. I HE III-V compounds, with few exceptions, have been prepared by the two-temperature method. In its classic form this technique is applicable to closed systems where at least one of the components, in this case the column V element, is a liquid or a solid with a high vapor pressure. One advantage of this method over flow systems is in its simplicity. In addition, because it is a closed system, it can, under the circumstances to be described later, be run at higher pressures of the volatile species than in flow systems. In instances where the III-V compound is soluble in the parent III metal to about 1 mol pct or higher, solution growth can be made to take place by slow cooling. This, for instance, is one way in which single-crystal GaP1 and Inp2 have been grown. Initial attempts to synthesize and grow A1P by this technique were not too successful; the yield was low and the crystals obtained were exceedingly small. The conditions required for improving the yield and growth by this technique were, therefore, sought. Two obvious conditions which could be controlling were examined. These were the temperature of the aluminum and the pressure of the phosphorus. The range of temperatures studied extended from about the melting point of aluminum, 660° to about 1450°C. The latter is dictated by the vapor pressure of aluminum which reaches about 1 Torr at that temperature and the limitations of the materials of construction as described in the next section. The pressure range of interest covers from below 1 atm to above the critical pressure of phosphorus, 82.2 atm. EXPERIMENTAL The Temperature of Aluminum as a Variable. A series of experiments were run in the conventional two-temperature manner. All refractories and quartz were dried by heating at 800° to 900° for a minimum of 24 hr, and usually much longer, before use. The aluminum

Jan 1, 1969

By E. W. McAllister

THE decision of the California Oil Umpire&apos;s1 office to accept well potentials established from subsurface-pressure data has brought to the attention of many operators for the first time the application of such data to production problems. This paper reviews the development and application of subsurface-pressure data in Kettleman Hills, where these data have been used in production work since 1932. The Kettleman Hills field was discovered in October 1928. The first subsurface-pressure surveys were made early in 1932 and by the middle of 1933 the two major operators in the field were making routine pressure runs in their respective wells. Shortly thereafter, these companies agreed to exchange pressure data, and later a third company entered into the agreement. This made it possible to analyze the effects upon the reservoir pressure of past production practices, which are discussed in the latter part of the report. It is interesting that many of the applications of subsurface-pressure data discussed herein were anticipated by C. L. Clarks and C. B. Kimberlin‡ in a reports dated March 1933. PRODUCTIVITY INDEX In the majority of individual well problems involving the use of subsurface pressure data, it is necessary to use a factor known as the "productivity index," which indicates the ability of a well to produce and represents the number of barrels of oil or oil and water per day that will enter the well bore for each pound per square inch pressure drop made opposite the producing interval of the well. The productivity index may be determined from pressure and production data for one or more rates of flow and a static or shut-in pressure survey or from production and pressure data for two or more rates of flow. Productivity indices may be based upon either net oil or total fluid production. All indices referred to in this report are based upon net oil. The value of the productivity index for Kettleman Hills wells decreases generally with time and it is not uncommon for the index to vary in value at any specific time for various rates of flow. The decline of the productivity index may be attributed partly to the loss of reservoir pressure. As. the reservoir pressure decreases, gas originally in solution is released from the oil, congesting the flow of fluids through the formation and increasing the viscosity and surface tension of the oil; thus the flow resistance of the fluids through the formation is increased, resulting in a decrease of the productivity index. For convenient reference, the productivity indices for each well are plotted against time and a curve is drawn through the points showing the trend of the average index value. Plotted on Fig. I are index values for five

Jan 1, 1941

By E. W. McAllister

The decision of the California Oil Umpire&apos;s&apos; office to accept well potentials established from subsurface-pressure data has brought to the attention of many operators for the first time the application of such data to production problems. This paper reviews the development and application of subsurface-pressure data in kettleman Hills, where these data have been used in production work since 1932. The Kettleman Hills field was discovered in October 1928. The first subsurface-pressure surveys were made early in 1932 and by the middle of 1933 the two major operators in the field were making routine pressure runs in thcir respective wells. Shortly therefter, these companies agreed to exchange pressure data, and later a third company entered into the agreement. This made it possible to analyze the effects upon the reservoir pressure of past production practices, which are discussed in the latter part of the report. It is interesting that many of the applications of subsurface-pressure data discussed herein were anticipated by C. L. Clark and C. B. Kimberlint in a report2 dated March 1933. PRODUCTIVITY Index In the majority of individual well problems involving the use of subsurface- pressure data, it is necessary to use a factor known as the "productivity index," which indicates the ability of a well to produce and represents the number of barrels of oil or oil and water per day that will enter the well bore for each pound per square inch pressure drop made opposite the producing interval of the well. The productivity index may be determined from pressure and production data for one or more rates of flow and a static or shut-in pressure survey or from production and pressure data for two or more rates of flow. Productivity indices may be based upon either net oil or total fluid production. All indices referred to in this report are based upon net oil. The value of the productivity index for Kettlcman Hills wells decreases generally with time and it is not uncommon for the index to vary in value at any specific time fur various rates of flow. The decline of the productivity index may be attributed partly to the loss of reservoir pressure. As the reservoir pressure decreases, gas originally in solution is released from the oil, congesting the flow of fluids through the formation and increasing the viscosity and surface tension of the oil; thus the flow resistance of the fluids through the formation is increased, resulting in a decrease of the productivity index. For convenient reference, the productivity indices for each well are plotted against time and a curve is drawn through the points showing the trend of the average index value. Plotted on Fig. I are index values for five

Jan 1, 1941

By E. W. McAllister

The decision of the California Oil Umpire&apos;s&apos; office to accept well potentials established from subsurface-pressure data has brought to the attention of many operators for the first time the application of such data to production problems. This paper reviews the development and application of subsurface-pressure data in kettleman Hills, where these data have been used in production work since 1932. The Kettleman Hills field was discovered in October 1928. The first subsurface-pressure surveys were made early in 1932 and by the middle of 1933 the two major operators in the field were making routine pressure runs in thcir respective wells. Shortly therefter, these companies agreed to exchange pressure data, and later a third company entered into the agreement. This made it possible to analyze the effects upon the reservoir pressure of past production practices, which are discussed in the latter part of the report. It is interesting that many of the applications of subsurface-pressure data discussed herein were anticipated by C. L. Clark and C. B. Kimberlint in a report2 dated March 1933. PRODUCTIVITY Index In the majority of individual well problems involving the use of subsurface- pressure data, it is necessary to use a factor known as the "productivity index," which indicates the ability of a well to produce and represents the number of barrels of oil or oil and water per day that will enter the well bore for each pound per square inch pressure drop made opposite the producing interval of the well. The productivity index may be determined from pressure and production data for one or more rates of flow and a static or shut-in pressure survey or from production and pressure data for two or more rates of flow. Productivity indices may be based upon either net oil or total fluid production. All indices referred to in this report are based upon net oil. The value of the productivity index for Kettlcman Hills wells decreases generally with time and it is not uncommon for the index to vary in value at any specific time fur various rates of flow. The decline of the productivity index may be attributed partly to the loss of reservoir pressure. As the reservoir pressure decreases, gas originally in solution is released from the oil, congesting the flow of fluids through the formation and increasing the viscosity and surface tension of the oil; thus the flow resistance of the fluids through the formation is increased, resulting in a decrease of the productivity index. For convenient reference, the productivity indices for each well are plotted against time and a curve is drawn through the points showing the trend of the average index value. Plotted on Fig. I are index values for five

Jan 1, 1941

By R. E. Reed, C. J. McHargue

Poly crystalline aluminum specimens having random and diffuse (001) initial orientations were reduced 90 pct in area at room temperature by drawing, extruding, and swaging. Although each procedure produced the duplex (001)- (111) texture, there were marked dqferences in the relative amounts of each component. This also produced variations in the tensile properties of the aluminum rods. It is generally agreed that the fiber texture found in aluminum rods consists of a strong (111) and a weak (001) component after reductions in area of 90 pct or more. An examination of data summarized in recent reviews&apos;-3 shows much spread in the values for the relative amounts of the two components reported by different investigators. That the initial orientation has a marked influence on the final texture even after reductions in area greater than 90 pct is well-documented.4-7 Another factor which may influence the relative amounts of the two components is the method of fabricating the wires or rods. Barrett and ~assalski&apos; state that the center of wires formed by rolling, swaging, and drawing have the same textures. The data cited in support of this conclusion came from qualitative X-ray techniques. In recent years there has been renewed interest in correlating the type of preferred orientation with such parameters as stacking fault energy and onset of mechanical twinning.&apos;&apos; Since these analyses have often used many sources of data, it is essential that the data be evaluated for the effect of fabrication variables. In this study we have produced aluminum rods by drawing, swaging, and extruding and have quantitatively determined their textures. All specimens had the same purity and fabrication temperature, and the amount of deformation and the starting textures were determined. We have compared our results with published studies on similar materials and fabricating parameters. We have also compared results from the same three fabricating procedures for single-crystal specimens in three instances. EXPERIMENTAL PROCEDURE The aluminum was 99.99+ pct with the only detected impurities being (by weight) 0.002 pct Cu, 0.001 pct Si, and 0.001 pct Mg. Cylinders a in. in diam by 1 in. long with a fine-grain random texture were made by the following method. Cubes 1+ in. on a side were machined from 2-in.-diam ingots. These cubes were slowly pressed about 30 pct in each of the cube directions. The material was recrystallized by annealing 1 hr at 350°C. Three deformation-anneal cycles produced the desired material. Polycrystalline specimens with a diffuse (001) texture were made by casting into a graphite tube 1 in. ID, li in. OD, by 8 in. long which had been preheated to 900°C. One end of the tube was placed on a water-

Jan 1, 1969

By M. H. Caron

BASIC U. S. Patent 1,487,145 on ammonia leaching of nickel ores was issued to the author on March 18, 1924. Equivalent patents in other countries were obtained later. The Dutch Syndicate Brikcarbo became interested in the process in 1935; and a couple of years later the late Dr. H. Foster Bain sent samples of Surigao laterite iron ore to Delft and witnessed tests made there on this material for the Philippines Commonwealth. As a result, the author was asked in April 1940 by Dr. Bain to go to the Philippines to erect and take charge of a pilot plant for the process. The World War prevented carrying out this proposal. The Dorr Co. also became interested in the process at about the same period. The investigations by the Freeport Sulphur Co. on the process as applied to the Cuban nickeliferous laterites, which resulted in the Nicaro enterprise, and the results of this operation have been well described elsewhere.1,²,³,4,5 This Nicaro plant was, in operation for almost two years, and during this period produced about 10 pct of the world nickel production from laterites containing 1.35 pct nickel. This plant and its operation were war measures and, in view of this, activities were suspended in April 1947. The results obtained fully demonstrated the technical feasibility of the process and its economical aspects on a commercial scale. In this respect, it should be understood that it is probable that improvements may be made by further development, and that there are possibilities for advantageous application of the process to garnierite and similar ores with higher values in nickel than the laterite iron ores at Nicaro. While the articles cited above have given a certain amount of information, no general article containing all the important process data has been pub- lished. Since the process is of more than local interest, a fuller knowledge of the fundamental and practical factors of the method may be welcome to those interested in this new field of metals technology. The author, accordingly, takes pleasure in submitting this article to the AIME as it represents in a condensed form the results of many years of research. The brief outlines of the fundamental and other factors and the explanation of observed phenomena are presented with as little discussion of details as possible, consistent with clarity. It is a special satisfaction to the author to make some contribution of his own in return for the benefits of the many valuable publications issued by the Institute during his thirty years of membership. Ores Adapted for Ammonia Leaching: All nickel and cobalt ores which originate from weathering of peridotites or similar basic rocks having sufficient values are suitable for treatment by the ammonia leaching process after a preliminary reduction under proper conditions. The formation of these deposits was probably as follows: In the course of time the basic rocks were attacked by atmospheric agencies; MgO and SiO2 were gradually leached out, and secondary nickel minerals formed, such as garnierite, a hydrated silicate of nickel and magnesia. These secondary products are, however, not stable. They decompose in a further stage of weathering and ultimately only a relatively small residue of insoluble oxides remains, known as laterite iron ore with a small nickel content and very little cobalt. Under these mantles of laterite, richer nickel values may be found, usually indicated by the occurrence of garnierite. The more the ore is disintegrated by nature, the higher the iron content and the better the nickel extractions that may be expected therefrom. Table I shows extractions that may be expected from different types of ores, assuming treatment of -200 mesh products and that all precautions have been taken for obtaining maximum extractions. As for the distribution of the various nickel minerals and compounds that may be present, great variations may occur from locality to locality as well as vertically in a deposit. From such "run of

Jan 1, 1951

By E. M. Elkin, J. H. Schloen

All known methods of treating and recovering the various components of copper refinery slimes are discussed. The slimes treatment processes presently used by five copper refineries are described and flowsheets are given. A bibliography is appended. THE recent increase in anode copper production at the Noranda smelter placed an additional load on the Montreal East plant of Canadian Copper Refiners Limited. The consequent increase in the amount of anode slimes led to a careful consideration of the various methods of slimes treatment. A critical review of these methods is presented here in the belief that it would be of interest to copper refiners. No such review has yet been published, although a number of individual flowsheets have been described. To make the information of greater value, a questionnaire was sent to all copper refineries. While the overall response to the questionnaire was not entirely satisfactory, the foreign refiners gave much detail in their answers and expressed willingness to cooperate further if needed. Although the data below do not cover all refineries, it is thought that examples of all flowsheets currently in use are included. A comparison of these flowsheets should prove of interest. The paper is divided into two parts. One part deals with a discussion of all known methods of treating and recovering the various components of the slimes. The second describes the processes now in use at various copper refineries for the treatment of raw slimes up to the production of Doré bullion. A brief description of the two main electrolytic methods of parting Doré bullion is appended. Since the first commercial application of electrolytic refining of copper by J. B. Elkington in 1865, the treatment of anode mud or slimes has undergone many changes. The object of treating slimes has always been the recovery and separation of precious metals. With the passage of time, increasing attention has been paid to improvement in recovery and quality of byproducts, mainly selenium and tellurium. The original methods of treatment were crude, although relatively direct. For example," the slimes were fused on a dolomitic clay bed in a reverbera-tory furnace; the slag was removed and the resulting metal cupelled to silver and gold. In another process, the dried slimes were oxidized and scorified on the lead bath of a cupelling furnace. Later, these pyrometallurgical methods were modified by sulphuric acid leaching, followed by fusion with niter in a reverb eratory furnace. A preliminary oxidizing roast improved the leaching step. Straight hydro-metallurgy has not found practical application. No matter what method is employed, the result is Dorb metal—a silver-gold alloy, with or without the metals of the platinum group. Characteristics of the Slimes Anode slimes are made up of those components of the anodes which are not soluble in the electrolyte. They contain varying quantities of copper, silver, gold, sulphur, selenium, tellurium, lead, arsenic, antimony, nickel, iron, silica, etc. The color of raw slimes is grayish black and the particle size is —200 mesh. However, Baraboshkin and Gaev (Ref. 1, p. 37), describe light gray colored slimes from the electrolysis of secondary copper which are composed predominantly of sulphates and of basic salts. In anode furnace practice primary and secondary metals are not usually segregated and such slimes do not commonly occur. Copper in the slimes originates to a large extent in the cuprous oxide of the anodes and is therefore dependent on the oxygen content of the latter: Cu2O + H2SO4 + CuSO4 + H2O + Cu [I] Opinions have been expressed that some of the copper is formed by decomposition of cuprous to cupric sulphate Cu2SO4 ? CuSO4 + Cu PI The product of either reaction is very finely divided. Depending on the slimes composition, much of the copper is combined with sulphur, selenium, tellurium, etc. The balance of the copper is in the free metallic state.

Jan 1, 1951

By J. W. Edington

THE Hopkinson bar has become a popular technique for the measurement of the mechanical properties of materials deformed at high strain rate. Maximum use of the equipment is made in the arrangement first used by Kolskyl in which a short compression specimen is sandwiched between two pressure bars and is loaded by a single pulse travelling through the system. The pressure bars are used both to apply the load to the specimen and as transducers to obtain continuous strain-time histories of three pulses, incident on, reflected, and transmitted by the specimen. The data measured by the pressure bars can be analyzed in terms of the stress/strain behavior of the specimen.2&apos;3 However, one of the assumptions of the analysis of the observed pulses is that the total stress and total strain do not vary significantly from point to point within the specimen at any given instant during the deformation process. Although this assumption is generally justified for very short disc-like specimens2 the situation is uncertain for larger specimens. For example, at small plastic strains (-0.01) Hauser et al.2 have some evidence of small flucations in the total stress within the crystal during deformation, even in relatively short aluminum specimens. In addition, Karnes4 has shown that the plastic strain, and by inference strain rate, is different at each end of a compression specimen tested in a Hopkinson bar, although the length of the specimen was not specified. Recently, the mechanical properties and the dislocation substructure have been investigated in single crystals of columbium5 (length 0.25 in., diam 0.19 in.), and copper6 (length 0.5 in., diam 0.5 in.) deformed at high strain rates. As part of this research program the assumption that the plastic strain is constant throughout the specimen has been checked by measuring the total dislocation density as a function of position in the specimen. Compression specimens of the same orientations and dimensions were tested as described previously5,6 sing a split Hopkinson bar. Since any discontinuity in strain distribution is most likely to arise during the initial stages of deformation the investigation was performed on specimens deformed to plastic shear strains of 0.054 (copper) at a strain rate 1.2 x l03 sec-1, and 0.06 (columbium) at a strain rate 1.5 X l03 sec-1. The orientation of the single crystals is shown in Figs. 1 and 3. Thin foils were taken parallel to the most highly stressed slip plane, i.e., (111) in copper and (011) in columbium, using conventional disc techniques. The dislocation densities were measured using first order reflections with compensation for invisible dislocations.5&apos;6 In the copper single crystals the discs were randomly distributed throughout the cross section of the specimen. However, the dislocation density obtained from each disc was plotted vs the disc positions relative to the ends of the specimen. The results for the copper specimens are shown in Fig. 1. Clearly the dislocation density is constant throughout the main portion of specimen within the experimental error. The error bars on the dislocation densities correspond to a shear strain variation of 0.015 on the basis of previous measurements% ± of the rate of increase of dislocation density with strain in copper single crystals of the same geometry. Thus within this experimental error the plastic strain can be concluded to be constant within the specimen and the assumptions used in the analysis of the stress/time curves are therefore reasonably valid. The higher measured dslocation density near the impact end and the lower dislocation density at the bar end of the copper specimen is in agreement with the results of Karnes4 who showed that this strain/time curve rose to a maximum more rapidly at the impact end compared with the bar end. Hauser et al.2 have also pointed out that at small plastic strains (-0.01) the strain at the impact end of the specimen may be greater than that at the bar end. Thin foils taken from different points within the columbium single crystals demonstrated that the dislocation density could vary significantly within the specimen, see Fig. 2. Large areas of some thin foils up to 30 µ sq contained very few dislocations, see Fig. 2(a). However, in other parts of the compression specimen dislocation configurations like those shown in Fig. 2(b) existed over large areas (-30 µ sq). As a result, when the average dislocation density in a thin foil is plotted as a function of the position of the thin foil relative to the ends of the specimen, considerable scatter is observed, see Fig. 3. In this material then, the local dislocation density, and consequently the

Jan 1, 1970

By G. C. Kuczynski

Two particles in mutual contact form a system which is not in thermo-dynamical equilibrium, because its total surface free energy is not a minimum. If such a system is left for a certain period of time, the bonding of the two particles will take place in order to decrease the total surface area, even though the temperature is lower than the melting point. This phenomenon of bonding of two or more particles with the application of heat only and at temperatures below melting point of any component of the system will be called sintering, although the powder metallurgists use this term in a broader sense, including the presence of molten phase and pressure. It is the objective of this paper to study this process and the mechanisms involved in it. This problem is of utmost importance to powder metallurgy and powder ceramics, and its technological aspects have been studied for a good many years. However, the powder metallurgical operations are too complex and include too many superimposing mechanisms, and too many variables for a direct study. It was therefore advisable for the purposes of this study to reduce the variables to a minimum. In this work the radius of the interface formed during bonding in a simple system composed of a spherical particle and a large block of the same metal was studied as a function of time and temperature. It is believed that the mechanism involved in this simple process is fundamental to any sintering operations. Previous Work J. Frenkell was the first to make a serious attempt to develop a theory of sintering. He assumed that the process consists of a slow deformation of crystalline particles under the influence of surface tension which reduces to a viscous flow where the coefficient of viscosity n is related to the self-diffusion coefficient D by the following equation 1 _ D D6kT [1] where 6 is interatomic distance, k the Boltzman constant, and T the absolute temperature. This type of viscous flow of a crystalline substance is essentially different from the ordinary plastic flow. The latter is a specific propcrty of crystals and cannot take place in amorphous bodies. According to Frenkel this viscous type of flow is due to the diffusion of the holes or vacancies arising in the lattice. He was able to derive an equation relating the growth of the interface between two spherical crystalline particles or between a particle and a semi-infinite crystal (Fig 1) to time t at constant temperature. This relationship can be written as follows: x²— 3/2 a/nt [2] where x is the radius of the interface assumed to be circular, a the original radius of the sphere and a surface tension of the material. The other assump- x tions are that x is less than 0.3 and that during the period 1 the original radius, a, of the metallic particle did not change appreciably. A. J. Shaler and J. Wulff2 followed closely the ideas of Frenkel in their theory of sintering of a mass of metallic powder. Neither Frenkel nor Shaler has validated his theoretical speculations with conclusive experimental data. Two measurements reported by

Jan 1, 1950

By Howard R. Keil

Reactor at Carlton mill successfully calcines pyrite-telluride flotation concentrate for cyanidation. CARLTON mill in the Cripple Creek district, 45 miles southwest of Colorado Springs, Colo., has been in operation for approximately three years, treating the custom sulpho-telluride ores formerly handled by the Golden Cycle mill in Colorado Springs. At the new mill the pyrite-telluride flotation concentrates have been roasted, prior to cyani-dation, in a Dorrco FluoSolids reactor, which has proved capable of yielding calcine readily amenable to cyanidation. Incoming ores are crushed at Carlton to % in. and sampled in 30 to 75-ton lots before the individual lots are mixed in the fine ore bin. The composite ore then goes to the grinding circuit. Classifier overflow from the grinding circuit is treated by flotation to produce a concentrate containing approximately 85 pct of the values in 5 pct of the weight. The flotation concentrate goes to the FluoSolids reactor prior to cyanidation. Cyanide solution values are recovered by zinc dust precipitation. Flotation tailings are thickened and cyanided, the values from this part of the circuit being recovered from solution by activated carbon. Gold values in the flotation concentrates consist of a small amount of finely divided metallic gold; the tellurides, sylvanite and calaverite; and gold very intimately associated with the pyrite. The metallic gold and a part of the telluride values can be extracted from the concentrates by cyaniding without roasting. However, extraction on the tellurides by this method is not satisfactory, and the pyrite values are so intimately associated with the pyrite that very fine grinding and cyanidation for a prolonged period under ideal laboratory conditions does not yield good recovery. Upon roasting, the tellurides are oxidized to very finely divided metallic gold which is readily soluble in cyanide. The pyrite is oxidized mainly to a porous iron oxide which allows cyanide solution to penetrate to gold particles and take them into solution. Feeding the Reactor Flotation concentrates move by gravity to a thickener. Thickener underflow is discharged at approximately 60 pct solids, by means of a diaphragm pump, into a storage and blending agitator. From here the concentrates are pumped to a disc filter. The filter cake, at 84 to 88 pct solids, drops directly into a repulper where it is repulped into a slurry of 78 to 80 pct solids. The repulped filter cake flows into a 6x6-ft slurry agitator from which it is fed directly into the reactor by the Moyno pump. The Moyno pump has eliminated a large number of difficulties that were first encountered in feeding a wet concentrate to the reactor. On the original installation in Canada a screw feeder was used to introduce the filter cake directly into the reactor. Since the reactor is under a slight positive pressure it was necessary to have a suitable seal to prevent gas escaping from the reactor at this point. When the concentrates produced in flotation were coarse or granular they could be readily fed to the reactor but when fine-textured, clayey concentrates were produced a great deal of trouble was encountered.

Jan 1, 1955