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By A. Martens

When I was honored with an invitation from the American Institute of Mining Engineers to present a paper at the Chicago meeting on the microstructure of iron, I hesitated about accepting, as the short interval that would remain at my disposal, after other pressing matters had received attention, could not but seriously affect the work of preparing such a paper. Unfortunately my fears have been realized and my work is neither completed, nor yet as comprehensive as I should desire. Mindful of my promise, however, and recognizing that 1 have reached a point where the results of my researches may prove suggestive, I am led to present them now, trusting that this brief explanation map secure indulgence for whatever deficiencies the paper may disclose. So far as my knowledge of published memoirs and treatises extends, microscopy cannot yet be said to possess a really firm foundation. In few cases only has any systematic development of the methods of investigation been undertaken, and broad gaps remain to be filled. It is not yet possible, therefore, to give a complete survey of the field, or, indeed, to supply a text-book on microscopic metallography. As Mr. F. Osmond, of Paris, a distinguished member of our profession, has undertaken to prepare for the Chicago meeting a historic review of the work actually accomplished I need not touch on that branch of the subject; but before entering upon my special theme, it may not be out of place for me to introduce certain explanations, as furnishing reasons for the course 1 have hitherto pursued, and to offer some suggestions for the further development of the methods of microscopic investigation. In microscopic metallography, the examination has to be conducted principally with incident light. Objectives of low power, in which the distance between the front lens and the abject is considerable, are adapted for directly incident light, and in such cases the relatively great depth of the image renders it possible to examine

Jan 1, 1894

By E. S. Bardwell

Each of the three refining furnaces in use at Great Falls is provided with a waste-heat boiler. The general arrangement of furnace and boiler is as shown in Fig. 1. Two of the furnaces have hearths 45 ft. 7 in. by 14 ft. 6 in.; the third has a hearth 46 ft. 101/2 in. long and of the same width as the other two. The furnaces at present are equipped for firing with natural gas. As originally constructed two of the furnaces had hearths 36 by 14 ft., and were designed to use coal on grates, but these furnaces were lengthened and fired successively with pulverized coal and oil. The third furnace was added in 1926 and was oil-fired until 1928. Since that year natural gas has been in use on all of the furnaces. The changes that have occurred in connection with furnace design and the comparative performance of the furnaces with various fuels were described1 by the author in 1932. Two of the furnaces are provided with Stirling class A-30 boiler. rated at 400 hp. and having 4008 sq. ft. of heating surface. The thir furnace has a class A-21 Stirling waste-heat boiler rated at 300 hp. with 2805 sq. ft. of heating surface. The boilers are not baffled. The waste-heat boilers are placed on a platform 17 ft. 3 in. above the level of the furnace charge floor. The waste gases from the furnace pass by a vertical uptake flue, 4 by 3 ft. inside at the point where it enters the chamber, to a brick chamber from which the gases pass over a bridge wall and into the boiler setting. The uptake flue and chamber are constructed of silica brick. Each furnace has a steel stack 125 ft. high, measured from the boiler floor. The stacks have a 41/2-in. firebrick lining and are 5 ft. in diameter

Jan 1, 1934

By W. L. Prehn, Adele Chambers, R. L. Slobod

The centrifuge has been found to be an extremely useful tool for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. The use of the centrifuge for determining the properties of small core plugs has been discussed in the literature,',' but practically no experimental evidence has been presented justifying the use of this method in preference to other methods (mainly disc method) now in use. Data have been accumulated and are now presented demonstrating the advantages of the centrifugal method, some of which are: (1) rapid establishment of equilibrium, (2) excellent precision yielding very reproducible results, (3) availability of high pressure differences between phases, (4) simple operational procedure, and (5) ability to establish connate water, residual oil, or to obtain complete capillary pressure curve in one day or less. A commercially available centrifuge capable of speeds up to 3,800 rpm, and a high speed attachment providing a maximum rate of rotation of 18,000 rpm were used in this work in conjunction with core holding tubes designed specifically for this application. In view of the outstanding advantages associated with the use of the centrifuge the conclusion has been drawn that this method should be used in place of the more tedious, slower, and less reliable disc method for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. INTRODUCTION The need for accurate values of connate water, residual oil, and capillary pressure curves in reservoir engineering has been recognized for many years, and the extent of the effort devoted toward solving these problems is reflected in the large number of papers3-" which have appeared in the literature during the past decade. Most of the methods discussed in the recent literature employ a porous disc as a semi-permeable membrane to separate two immiscible phases and make pos-ible the application of an explicit difference in pressure between two phases in the core. Thus, in the determination of the capillary pressure curve the wetting phase (water) is displaced by the non-wetting phase (air or oil). Several investigators1,2 have used centrifugal forces to develop pressure differences between phases. As a result of the first work' in this field the conclusion was reached that "the more rapid centrifugal method for measuring irreducible saturation may have equal value, (compared to use of discs) but more work is required to establish this point." This work was followed in 1945 by a more detailed study2 in which the concepts of this experimental work were more clearly enunciated. A method for calculating saturation for any given speed of rotation based on the observed volume of water displaced was developed and a wider application of the method was suggested. The absence of any subsequent pertinent literature on this subject is interpreted as indicating that no additional work has been completed to substantiate or deny the earlier claims and suggestions of promise contained in the original papers on this subject. One purpose of this report is to provide evidence designed to establish the practical value of centrifugal methods in determining core properties such as connate water and capillary pressure curves. It is also our purpose to suggest a broadening of the scope of this tool to include determinations of residual oil by gas or water drives. THEORY AND PRACTICE IN USE OF CENTRIFUGE Hassler and Brunner2 have clearly presented the basic concepts involved in the use of the centrifuge by relating the performance of a small core in a field of high acceleration to the

Jan 1, 1951

By R. L. Slobod, W. L. Prehn, Adele Chambers

The centrifuge has been found to be an extremely useful tool for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. The use of the centrifuge for determining the properties of small core plugs has been discussed in the literature,',' but practically no experimental evidence has been presented justifying the use of this method in preference to other methods (mainly disc method) now in use. Data have been accumulated and are now presented demonstrating the advantages of the centrifugal method, some of which are: (1) rapid establishment of equilibrium, (2) excellent precision yielding very reproducible results, (3) availability of high pressure differences between phases, (4) simple operational procedure, and (5) ability to establish connate water, residual oil, or to obtain complete capillary pressure curve in one day or less. A commercially available centrifuge capable of speeds up to 3,800 rpm, and a high speed attachment providing a maximum rate of rotation of 18,000 rpm were used in this work in conjunction with core holding tubes designed specifically for this application. In view of the outstanding advantages associated with the use of the centrifuge the conclusion has been drawn that this method should be used in place of the more tedious, slower, and less reliable disc method for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. INTRODUCTION The need for accurate values of connate water, residual oil, and capillary pressure curves in reservoir engineering has been recognized for many years, and the extent of the effort devoted toward solving these problems is reflected in the large number of papers3-" which have appeared in the literature during the past decade. Most of the methods discussed in the recent literature employ a porous disc as a semi-permeable membrane to separate two immiscible phases and make pos-ible the application of an explicit difference in pressure between two phases in the core. Thus, in the determination of the capillary pressure curve the wetting phase (water) is displaced by the non-wetting phase (air or oil). Several investigators1,2 have used centrifugal forces to develop pressure differences between phases. As a result of the first work' in this field the conclusion was reached that "the more rapid centrifugal method for measuring irreducible saturation may have equal value, (compared to use of discs) but more work is required to establish this point." This work was followed in 1945 by a more detailed study2 in which the concepts of this experimental work were more clearly enunciated. A method for calculating saturation for any given speed of rotation based on the observed volume of water displaced was developed and a wider application of the method was suggested. The absence of any subsequent pertinent literature on this subject is interpreted as indicating that no additional work has been completed to substantiate or deny the earlier claims and suggestions of promise contained in the original papers on this subject. One purpose of this report is to provide evidence designed to establish the practical value of centrifugal methods in determining core properties such as connate water and capillary pressure curves. It is also our purpose to suggest a broadening of the scope of this tool to include determinations of residual oil by gas or water drives. THEORY AND PRACTICE IN USE OF CENTRIFUGE Hassler and Brunner2 have clearly presented the basic concepts involved in the use of the centrifuge by relating the performance of a small core in a field of high acceleration to the

Jan 1, 1951

By W. A. Backofen, A. T. English

The kinetics of re crystallization were determined metallographically for a 3-1/4 pcl Si-Fe rapidly compressed at temperatures of 710° to 911°C, and held for various times at the working temperature. As in re crystallization following cold wwk, the time for re crystallization was reduced by increased temperature and strain. Nucleation occurred chiefly at grain edges, although other pre-existing interfaces, notably inclusions, also served as nucleation sites. The importance of intragranular nucleation to grain refinement in hot working is pointed out, together with some possible techniques by which nucleation might be induced within the grains. The observed isothermal growth rates are quite accurately described by the equation G = 4 x 10-'/t (cm per sec), independent of temperature and strain at all but the shortest times. Changes in G during recrystalliza-tion can exceed two orders of magnitude. It is argued that release of stored energy associated with lattice defects cannot adequately explain the time dependence. A suggested alternative involves processes of solute segregation and desegregation in the unrecrystallized matrix and at the moving boundary, respectively. EFFORTS to improve hot-working practice are hampered by an incomplete understanding of the fundamental metallurgy involved. Research directed at establishing the required basic foundation falls into two categories, the first concerned with measurement of mechanical properties under the conditions of high temperature and strain rate which characterize such processing, the second focused on structure and its relation to the deformation conditions. Rossard,' Rossard and Blain,2 and Hardwick and Tegart have conducted many high-speed, high-temperature torsion tests on various metals. One of their objectives was interpretation of stress-strain curves in terms of the structures of specimens rapidly quenched following interruption of twisting. They showed that appreciable hardening occurred in the early part of the test, and that this hardening reflected the concurrent development of an increasingly dense substructure within the grains. The detailed nature of this substructure was observed to depend on the ease of polygonization which, at least in fcc metals, varies with the stacking-fault energy.= By holding specimens after interruption but before quenching, the nucleation and growth of new grains could also be studied. Some success has been realized in relating the microstructure of hot-rolled steel to its temperature:strain rate:strain history with such testing.' The same general observations have been made by others investigating rolling4f5 and drop-hammer forging.~-~ Incident to these experiments, some efforts were made to determine the kinetics of re-crystallization as well as the velocity of the migrating boundaries. The results have been largely qualitative, owing to difficulties of interpreting hardness measurements5 and microstructures. The work described here was undertaken to obtain more quantitative information from tests on a material having suitable metallographic properties, and, in this way, to provide further insight into the fundamentals of this practically most important kind of deformation processing. I) MATERIALS AND EXPERIMENTAL TECHNIQUES Materials. Electrolytic etching of a Si-Fe alloy reveals dislocations and substructure in unrecrystallized grains.8'9 This unique characteristic makes possible a precise determination of the extent of recrystallization. For that reason, it was the material selected for all experiments in the present work. The two particular alloys that were used are identified in Table I. A major difference between "A" and "B" is the number of inclusions, as noted in the table. Most of the experiments were made with material "A". It was received as hot-rolled plate 1 in. thick, sawed to 2-in. widths, hot-forged at 1200°C to 5/8-in. rounds, and finally annealed in a mechanical vacuum at 1000°C for 24 hr. The result was substructure-free grains of mean diameter 0.05 cm.*

Jan 1, 1964

By Henry F. Adams, Guy H. Ruggles

IN this paper the authors aim to chronicle the experience and salient points brought out in changing flotation reagents at a concentrator which had probably been using a mininium amount of oil at a minimum cost per ton, to a more complicated system requiring a partial chemical control. The original oils were coal tar and pine oil. The new reagents are lime, xanthate and pine oil. It was found that there were no insurmountable difficulties and eventually the cost of the new reagents per ton of ore proved to be very little more than that of the old. LIME PLANT When the question of handling lime came up there were two propositions open: (1) to handle the lime dry; (2) to handle it wet in the form of an emulsion. Granting that a dry lime feeder would function properly, delivering lime uniformly, the chief objection was the dust that would be raised when these feeders were being charged or operated, as the only possible location was on a gallery beneath which men were working. With this objection the handling of lime as an emulsion seemed to be the better scheme. The lime plant which was first installed was for experimental work on one section. This was gradually changed and developed until it was of sufficient size to accommodate 20 sections. The various changes will not be discussed and the following description deals only with the fully developed plant. Crude as it is, and perhaps somewhat expensive to operate, the lime-handling plant has been quite successful. Much has been learned which will pave the way for a better installation in the future. Burnt lime is received loose in standard gage box cars. This is the product of the kilns and has had no screening or sorting. A grab sample is taken from each car as it is unloaded. An average of the analyses of samples from 44 cars gave the following: [ ]

Jan 1, 1928

By E. S. Hutchinson

The subject of the influence of coal-dust in mine-explosions has received considerable attention both in England and on the continent of Europe, but until the recent disaster at Pocahontas, Va., it seems not to have been of special interest to engineers in this country. The reason, perhaps, is that most of our bituminous mines are worked by short shafts, slopes and drifts; few have been specially dry; and the explosions that have occurred could readily be traced to fire-damp with 110 complicated circumstances. The object of the present paper is to bring together, for the convenience of members of the Institute, the principal English opinions upon this important subject. Messrs. Lyell and Faraday, in their report to the Home Secretary," in England, on the Haswell Colliery explosion in 1844, seem to have been the first to point out that dust fed the flame originating in a

Jan 1, 1885

By Walter J. Johnson

The coals in northern Wyoming and Montana are free-burning and non-caking and range from lignite to bituminous C in rank. Strip and underground mining are employed to supply railroad, utility, industrial, and domestic fuel. The market area includes Iowa, Nebraska, Minnesota, North and South Dakotas, Wyoming, Montana, the Pacific Northwest, and western Canada. THE larger producing coal mines in northern Wyoming are located in the Powder River Basin lying between the Black Hills region of South Dakota, eastern Wyoming, and the Big Horn Mountains in north central Wyoming, see Fig. 1. The mines are located particularly in the area along the route of the Chicago, Burlington & Quincy Railroad from Gillette, Wyo., to a point approximately 15 miles northeast of Sheridan, Wyo. Fig. 2 is a graph of coal production in the state of Wyoming from 1918 to 1951. Across the Big Horn Mountains lies the Big Horn Basin, situated between the Big Horn Mountains and the Rocky Mountains proper. Mining in the Big Horn Basin is almost entirely confined to a small area known as the Gebo Field, near the town of Kirby, which is located on the Chicago, Burlington & Quincy Railroad. This paper will describe present operating areas, making only brief reference to the history of mining and marketing primarily because of the large area to be discussed. The coal beds presently mined in the Powder River Basin are all of Tertiary age and are of Fort Union and Wasatch formations of Paleocene and Eocene ages, see Fig. 3. The Fort Union formation, consisting of 2000 to 3200 ft of alternate sandstone, shale, and coal, is divided from oldest to youngest into the Tullock, Lebo Shale, and Tongue River members. Most of the mineable coal is in the Tongue River member, which is 500 to 800 ft thick. The Carney coal bed, varying from 7 to 20 ft in thickness, is considered the base of the Tongue River member. About 85 ft above the Carney is the Monarch bed, ranging from 18 to 42 ft in thickness. At approximately 210 ft above the Monarch is what is locally known in the Sheridan district as Dietz No. 3 bed, which varies from 12 to 30 ft in thickness. One hundred feet above the Dietz No. 3 is Dietz No. 2 bed, which is 7 to 12 ft thick. At about 100 ft above the Dietz No. 2 is Dietz No. 1 bed, 7 to 15 feet in thickness. Two hundred and fifteen feet above Dietz No. 1 is the Smith bed, approximately 5 ft thick. One hundred twenty-five feet above the Smith is the Roland bed, which is estimated to be approximately 13 ft thick. The Roland bed is considered the base of the Wasatch formation, which in the Powder River Basin is 1000 to 3500 ft thick and is composed largely of shale, sandstone, and coal. The foregoing measures are the only ones above the Tongue River member that have been mined in the Sheridan field. To the east of the Sheridan field, particularly in the area of Gillette, the Roland bed is considerably thicker and is considered the thickest and most extensive coal bed in Wyoming, reaching a maximum thickness of 106 ft. From 125 to 225 ft above the Roland lies the Arvada bed, average thickness 9 ft. Three hundred seventy-five to four hundred feet above the Arvada is the Felix bed, which reaches its maximum thickness of 30 ft near Echeta on the Chicago, Burlington & Quincy Railroad. East of the Powder River the bed averages more than 10 ft in thickness, but it thins in a northwesterly direction. The highest mineable coal in the Powder River field is the Healy bed, about 400 ft above the Felix bed and exposed only in the highest parts of the area where much of it has been burned along the outcrop. Where it has not been burned, the thickness at most of the outcrops is 10 to 15 ft.

Jan 1, 1954

By C. H. Cheng, C. E. Birchenall

The fundamental problem in the thermodynamics of solid solutions is the determinatiorl or calculation of the activities of the components as a function of temperature and composition. Since the theory of metals is not suficiently developed to allow a priori calculation of these quantities, they must be obtained from experiment. C. Wagner1 has reviewed the literature of this subject for the period before 1940. Although several important and extensive studies have been made in the meantime, the number of systems to which any sort of quantitative information can be assigned is vanish-ingly small. These data have become of great potential importance in studies of the structure of solid solutions2 and intermetallic compounds, the nature of the diffusion process,3,4 and perhaps even the mechanism of mechanical deformation.5 For these reasons, it. seems very worthwhile to extend the experimental data in this field. Although there is little use in duplicating Wagner's review, attention should be directed to the most recently reported investigations. A brief enumeration of the methods of measurement previously employed also should be valuable. The most direct method is the determination of the partial pressure of the components in the vapor phase in equilibrium with the solution. Both equilibrium and kinetic methods have been tried in metal systems, but almost exclusively on liquid phases. Only in the ease of carbon in iron alloys and in the copper-zinc system have extensive measure- ments been made which include solid phases. When one of the components is an element, such as nitrogen or carbon, which forms compounds which are very volatile and stable at normal temperatures and pressures (CH4, Co2, CO NH3), it is frequently possible to equilibrate mixtures containing these (such as CH4-H2, CO2-CO, NH3-H2) independently with the elernents (C, X) and with the metal (Fe, Ni, etc.). Such measurernents have been made for carbon in iron, iron-silicon, and iron-manganese alloys by Smith6 and in iron and iron-nickel alloys by Toensing.7 Differences between carbon activity values at the same temperature and carbon content when carboil is introduced from CH4-H2 rnixtures or CO-CO. mixtures indicate that the effects of hydrogen and oxygen in the system are not negligible, and one can only hope that the true value lies somewhere between these sets of results, probably nearer the CH4-H2 data since hydrogen is less soluble in iron than oxygen. This is essentially an equilibrium method, although flowing gas is employed. A kirletic method has been employed which consists of sweeping an inert gas (generally hydrogen) over the alloy at a series of rates, condensing the metal vapor out,, and analyzing it. The metal content can be extrapolated to zero flow rate (equilibrium). Wejnarth's8 work on Cd-Mg and Zn-Mg is a good example of this frequently used method. A variant of this consists of equilibrating a known volume of inert gas with the alloy, sweeping it out quickly, and analyzing for metal. In common with the above method, it has the disadvantage that the "inert" gas is generally somewhat soluble in the alloy. Moreover, the former continuously displaces the system from equilihrium and may give low values if solid diffusion is involved. The dew point method applied by Hargreaves9 to the alpha and beta brasses and by Schneider and Stolll0 to A1-Zn avoids the introduction of another component to the system, but is useful only in systems in which one component is much more volatile than the other. The alloy sealed in one end of an evacuated silica tube is heated to the desired temperature. The temperature of the other end is lowered until droplets of the volatile component condense. When the temperature is raised slightly, the droplets will evaporate. By careful adjustment of temperature, the range between evaporation and condensation can be narrowed appreciably. An independent determination of the vapor pressure of the . pure volatile component is necessary to give the partial pressure over the alloy. This is the method employed here to determine the vapor pressures of zinc and cadmium over their silver alloys up to 34 pct in cadmium and 76 pct in zinc. The former involves only the a solid solution, but the latter covers the a, ß, y, and e fields. In recent determinations, Herbenar, Siebert, and Duffenbarkl1 used the

Jan 1, 1950

By Ralph E. Esarey, George V. Cohee

In Indiana, 349 wells were drilled for oil and gas in the year 1942. Of this number, 125 oil wells and 21 gas wells were successfully completed and 203 were dry holes. Drilling activity declined 37 per cent as compared with that of the year 1941. This reduction was brought about largely by Federal Conservation Order M-68, restricting drilling to one well on 40 acres, in order to save steel. This Order was later supplemented to permit closer spacing of wells drilled to sandstone formations in southwestern Indiana. Most of the drilling in 1942 was in the southwestern part of the state. Posey County ranked first, with 94 completions and 44 producers; Gibson County, second, with 77 completions and 38 producing oil wells and 2 gas wells. There were 58 drilling operations in the state at the end of the year. During 1942 a total of 589,734 ft. of hole was drilled, of which 231,702 ft. was wildcat footage. The total initial production of the oil wells completed was 9974 bbl. and of the gas wells, 11,148,000 cu. ft. (Table 2). Of the 349 wells completed, 122 were wildcat wells (Table 3); 26 were completed as oil wells; 17 were extensions to proven fields and 9 discovered new pools. Posey County was foremost in wildcat drilling, with 37 wells completed (Table 6). Thirty-five per cent of the wells drilled in 1942 were wildcat, as compared with 25.5 per cent in 1941. It is anticipated that the percentage of wildcat wells drilled in 1943 will be greater, although the total number ol ,wells drilled in the state will probably be less. The new discoveries in Indiana in I942 were, for the most part, one-well pools in the southwestern part—in Posey, Gibson and Spencer Counties (Table 4). Most of the development in pools took place in the . Hazelton and Kirksville pools in Gibson County, Mr. Vernon pool in Posey County and the Vernon Heights pool in Vander-burgh County. Deeper production was obtained from the Osage limestone in the Hazelton pool at a depth of 2402 ft., 650 ft. below the productive McClosky limestone. The well had an initial production of 140 barrels. Extensions to 17 pools in the southwestern part of the state were successfully completed (Table 5). An interesting development during 1942 was new production from the Devonian limestone in the Dodds Bridge pool, Sullivan County. The Ohio Oil Co. deepened one of its wells, which had been producing from a shallow sand, to the,Devonian, and it was completed for an initial production of 77 bbl. Five other Devonian producing wells were completed in that area. Crude-oil production in Indiana in 1942 was 6,609,000 bbl. (Table I). The Griffin field, Gibson and Posey Counties, which produced approximately 3,550,000 bbl., accounted for more than half of the state's production. The Mt, Vernon and New Harmony fields were next in importance of production, with 684,000 and 523,000 bbl., respectively. The price of crude oil was $1.22 a barrel for the old

Jan 1, 1943

By George V. Cohee, Ralph E. Esarey

In Indiana, 349 wells were drilled for oil and gas in the year 1942. Of this number, 125 oil wells and 21 gas wells were successfully completed and 203 were dry holes. Drilling activity declined 37 per cent as compared with that of the year 1941. This reduction was brought about largely by Federal Conservation Order M-68, restricting drilling to one well on 40 acres, in order to save steel. This Order was later supplemented to permit closer spacing of wells drilled to sandstone formations in southwestern Indiana. Most of the drilling in 1942 was in the southwestern part of the state. Posey County ranked first, with 94 completions and 44 producers; Gibson County, second, with 77 completions and 38 producing oil wells and 2 gas wells. There were 58 drilling operations in the state at the end of the year. During 1942 a total of 589,734 ft. of hole was drilled, of which 231,702 ft. was wildcat footage. The total initial production of the oil wells completed was 9974 bbl. and of the gas wells, 11,148,000 cu. ft. (Table 2). Of the 349 wells completed, 122 were wildcat wells (Table 3); 26 were completed as oil wells; 17 were extensions to proven fields and 9 discovered new pools. Posey County was foremost in wildcat drilling, with 37 wells completed (Table 6). Thirty-five per cent of the wells drilled in 1942 were wildcat, as compared with 25.5 per cent in 1941. It is anticipated that the percentage of wildcat wells drilled in 1943 will be greater, although the total number ol ,wells drilled in the state will probably be less. The new discoveries in Indiana in I942 were, for the most part, one-well pools in the southwestern part—in Posey, Gibson and Spencer Counties (Table 4). Most of the development in pools took place in the . Hazelton and Kirksville pools in Gibson County, Mr. Vernon pool in Posey County and the Vernon Heights pool in Vander-burgh County. Deeper production was obtained from the Osage limestone in the Hazelton pool at a depth of 2402 ft., 650 ft. below the productive McClosky limestone. The well had an initial production of 140 barrels. Extensions to 17 pools in the southwestern part of the state were successfully completed (Table 5). An interesting development during 1942 was new production from the Devonian limestone in the Dodds Bridge pool, Sullivan County. The Ohio Oil Co. deepened one of its wells, which had been producing from a shallow sand, to the,Devonian, and it was completed for an initial production of 77 bbl. Five other Devonian producing wells were completed in that area. Crude-oil production in Indiana in 1942 was 6,609,000 bbl. (Table I). The Griffin field, Gibson and Posey Counties, which produced approximately 3,550,000 bbl., accounted for more than half of the state's production. The Mt, Vernon and New Harmony fields were next in importance of production, with 684,000 and 523,000 bbl., respectively. The price of crude oil was $1.22 a barrel for the old

Jan 1, 1943

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

Mzasurements of the surface diffusion coefficients of metals have been made. Diffusion profiles for the Ag-Ag system were obtained by means of a radioactive point source and a precision auto-radiographic technique. The activation energy for silver self diffusion (=8.1 kcal per mole) is lower than that previously reported (-10 kcal per mole) on poly crystalline wire by Nickerson and Parker. The bresent data indicate an effect due to parasitic volume diffusion at temperatures above 500°C. RELATIVELY few measurements have been made of the surface self-diffusion coefficients of metals. Nickerson and arker' measured the diffusion of silver over the surface of poly crystalline wires and estimated that the activation energy was 10.3 kcal per mole. Winegard and chalmers2 carried out measurements on both polycrystalline and single crystal surfaces but did not report a value of the activation energy. They found, however, that at temperatures between 250" and 400°C the diffusion coefficients were on the order of lo-' sq cm per sec and that there was an acceleration of the migration of silver on the polycrystalline sample when a change of surface shape occurred. Winegard and Chalmers used an autoradiographic technique, hereafter designated ARG, and Nickerson and Parker used a surface scanning geiger counter in order to determine the diffusion profiles. More recently, Hackerman and simpson3 measured the surface self-diffusion coefficient of copper at a single temperature (750°C), and the value of the diffusivity (- 10-5 sq cm per sec) is in agreement with that given by jostein from his thermal grooving measurements. This paper reports the results of an investigation of the surface self-diffusion coefficients of silver over a large temperature range and describes the adaptation of autoradiographic (ARG) techniques for the determination of diffusion profiles obtained from a radioactive point source. EXPERIMENTAL PROCEDURE The experimental procedure is a modification of the method employed by Hackerman and simpson3 in their measurements on copper. A brief description of their technique is as follows: A radioactive needle which sinters to the surface during the diffusion an- neal serves as the source of diffusing atoms. After the diffusion run the needle is removed and the surface is scanned with a shielded counting arrangement. The diffusion profiles reported in this paper were obtained by a modification of the above procedure which employs a precision ARG technique. Previous investigations in this laboratory and elsewhere51B have shown that under carefully controlled developing conditions and by the use of calibration sources a linear relation exists between the concentration of the isotope and the photographic density for values below unity. The use of ARG under these conditions has advantages over the counter scanning method in that cumbersome shielding and requirements for great mechanical precision of the scanner are eliminated. Also the ARG gives a complete picture of the surface which is advantageous in studies of anisotropic diffusion. A recording microdensitometer having a 0.1 p wide slit was employed. At low temperatures the disturbing effects of subsurface radiations are negligible. The diffusion anneals are carried out in the cell shown in Fig. 1. The needle is formed by grinding down a 1.0 mm rod of high-purity silver until a tip of 0.2 mm radius or smaller is formed. This tip is plated withA"' which becomes the source of the diffusing atoms that are detected by ARG. The needle carrier and the crystal holder, Fig. 1 are constructed of quartz and ports are provided in the holder pedestal which allow free vapor circulation ((2.0 oz) and the carrier apron fits snugly over the crystal holder cap, insuring that the needle does not move and scratch the surface. Temperatures are provided by a stabilized tubular furnace which can be quickly positioned around the cell, thus bringing the crystal up to temperature in a time that is short compared to the diffusing times. The diffusion anneals range from 2 hr for the high-temperature samples to about 25 hr for those at the lowest temperature. The possibility of vapor transport of the radioactive metal as a contributing factor in the diffusion profile was investigated in two ways. One method was to suspend the needle directly over a dummy sample, raise the temperature, for periods of time equal to the diffusion times, and then take an auto-radiograph of the surface. Negligible radioactivity appeared. In the second method a thin slot in the crystal face on one side of the source provided a "cong path" for surface diffusion. If evaporation was the primary source of surface atoms the region of radioactivity around the source would be symmetrical. This was not the case. The profile dipped abruptly at the edge of the slot but on the other side of the source the usual diffusion profile appeared.

Jan 1, 1963

By P. Chiotti, R. J. Hecht

Vapov pressure data of solid and liquid alloys along with phase diagram data WERE employed in calculating the thermodynamic properties for the Ca-Zn system. The relative excess partial molal free energy for zinc in the liquid alloys was fitted to the relation wnvre i is we tvmpvrutiirc in ucgrees neivtu ana in is the tr~ole fvaction. Relations for the standard free energy of fortnation for the eight cornpounds were developed. ThE phase diagram for the Ca-Zn system as determined by Messing et a1.' is reproduced in Fig. 1. Earlier work on the phase diagram has been summarized by Hansen and Anderko2 and the very limited thermodynamic information for this system has been reviewed by Hultgren et a1.3 The heat of fusion for the compound CaZn2 has recently been determined to be 9260 cal per mole.4 Solubility data for calcium in zinc for the temperature range of 650" to 725°C were fitted by the relation and reported by Johnson and Dilloon5 In the present investigation zinc vapor pressure data were obtained by both the dewpoint and Knudsen methods in order to calculate the thermodynamic properties for liquid and solid alloys. The dewpoint method as employed in this work requires that only one of the components be significantly volatile, in this case zinc, and that the vapor pressure of pure zinc be known. For calculation purposes the vapor pressure data for pure zinc3 were fitted to the relations; for temperatures below 692.7K, the melting point of zinc. The corresponding free-energy relations for vaporization and sublimation of pure zinc are respectively. Some of the calculations also required knowledge of the free energy of fusion of zinc and calcium and the free energy for the 721°K allotropic transformation of calcium. The free energy of fusion of zinc was taken to be the difference between Eqs. [4] and [5], or The free energy of fusion and transition for calcium were based on the enthalpy values of 2040 and 222 cal per g-atom, respectively, as reported by Chiotti et al. 4 and the heat capacity data given by Hultgren et a1.3 and are represented by the relations, In the latter expression the difference in heat capacity between the a and 0 forms of calcium was neglected. MATERIALS AND EXPERIMENTAL PROCEDURES The metals used in preparing the alloys were Bunker Hill slab zinc, 99.99 pct pure, and Ames Laboratory calcium. The average impurities in the calcium in parts per million by weight, ppm, were N-17, H—77, Ba—216, Mg-15, Si—7, C—157, and Fe—9. The zinc was cleaned in dilute nitric acid and the calcium was used as received. The calcium was stored and handled in an argon-filled glove box and when removed from the dry box it was kept in an argon-filled desiccator. Tantalum was found to be a suitable alloy container. The alloy components were contained in a 1-in.-diam cylindri-

Jan 1, 1968

By T. L. Joseph, G. Bitsianes

The gaseous reduction of dense iron ore is a topochemical process in which reduction takes place at distinct interfaces between solid phases or layers. Under normal conditions, these interfaces remain parallel to the exterior surface of the ore body as they move inward. Certain conditions, such as cracking, high porosity, impurities, entrapped residual oxides, may cause departures from normal topochemical behavior. THE gaseous reduction of dense iron ore proceeds at interfaces between several solid phases or layers.',' Under normal conditions, these interfaces progress inward and remain parallel to the exterior surface of the ore body. This topochemical behavior is clearly illustrated in Fig. 1 which shows partially reduced specimens of natural and synthetic hematite. Using a coordinated sequence of macro, micro, and X-ray examinations, the authors1-'2 found that the number of interfaces and participating phases was in agreement with the Fe-0 system. Above 570°C, reduction of the ore involved a maximum of three common boundaries between four solid phases: iron, wiistite (Fe,O), magnetite (Fe,O,), and hematite (Fe,O,). Below 570°C, reduction proceeded through two interfaces between three phases: iron, magnetite (Fe,O,), and hematite (Fe,O,). The decrease in the number of phases below 570°C was due to the instability of wiistite below this temperature. The sequence of phases was also consistent with the equilibrium requirements. For example, the layers of iron oxides that were formed in topochemical fashion were always orientated in the order of increasing oxygen content. Thus, in Fig. 1 an outer layer of metallic iron is followed in turn by a thick intermediate band of black wiistite, by a thin layer of light magnetite, and finally by a relatively large core of hematite. This arrangement of the oxide layers was due to restrictions in reducing conditions which were imposed by the physical structure of the solid. The highly reducing gas on the outside of the particle gradually lost its reducing power as it penetrated into the specimen. On a macro scale, the layers of the various oxides appeared to be sharply defined and uniform in composition. Microexamination of the sections, however, revealed that the interfaces did possess measurable widths which varied with the porosity and chemical activity of the oxide phase undergoing reduction. For example, Fig. 2 shows three interfaces in a dense hematitic ore which was partially reduced at 850°C. At the iron-wiistite interface where the greatest porosity developed, the reaction proceeded over a zone 25 to 30 microns in width. Toward the interior, the interfaces became progressively narrower until at the magnetite-hematite boundary the reaction zone was about 1 micron wide. In this region the structure was exceedingly dense; the hematite possessing a porosity on the order of 3 pct. A careful micro study across polished layers of the various oxides revealed generally homogenous and single-phase structures. As reported in a previous paper,' the wiistite layer was characterized by an increase in oxygen content with depth of penetration. The topochemical behavior of reduction was studied in six types of ore of different origin, composition, and physical structure. In most cases, reduction proceeded at the boundaries of well defined layers or phases, and this behavior may be regarded as normal for most dense fine grained ores. Deviations from Ideal Topochemical Behavior A number of deviations from the normal topochemical behavior were noted. In these cases, the continuity of the reduction interfaces was disrupted in one of four ways: 1—Cracking of the specimen interrupted the geometric configuration, and the interfacial advance was no longer parallel to the exterior surface. 2—As a result of high porosity, the interfaces were spread over an appreciable distance and all but obliterated. 3—Impurities in the ore promoted a variety of deviations, including cracking. 4—A residual oxide phase was entrapped in the reaction product and left behind the advancing macro interface. Results from Cracking: A crack leading into the interior of an ore specimen presents a path of least resistance for the counter-flow of reducing gases and gaseous reduction products. Higher reducing conditions can be maintained along such cracks and reduction accordingly will propagate well ahead of the normally advancing reduction interfaces. Cracking was caused by a number of factors, one of which was the thermal spalling of impurities in the massive form. A more general type of cracking was due to reduction and was found in all dense varieties of natural and synthetic hematite, particularly in the temperature range of 500" to 700°C. The effect is shown clearly in Fig. 3. In this case, a dense sphere of pure hematite was partially reduced at 650°C for 100 min. The macrosection shows that one large reduction crack had penetrated the specimen and disrupted the normal topochemical advance of the interfaces. The outer layer of iron was only slightly affected but the thin dark layer of wiistite, adjacent to the ferrite, had widened perceptibly as it progressed along the crack. Farther inward, the magnetite layer was greatly disrupted and had penetrated irregularly to form islands of unaltered white hematite. A great deal of internal cracking is evident in the magnetite phase. From a practical point of view, the cracking of dense ores in the blast furnace could lead to desirable as well as undesirable effects. The general result

Jan 1, 1956

Discussion of the paper of, RICHARD H. RICE, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin No. 89, May, 1914, pp. 721 to 743. S. G. VALENTINE, Oxford, N. J.-In a paper read at the New York meeting of the Institute last February I presented some notes taken from our experience with the turbo blower operating on a blast furnace. In connection with Mr. Rice's very interesting paper there are a few items that might be of further practical interest. The question of the reliability of this type of blower will naturally be presented. In this connection we would say that our turbo blower has been in practically continuous use during the present blast, which was begun June 7, 1912, with only three interruptions for repairs of any consequence. Soon after blowing in there was developed a tendency of the blower to surge or pulsate. This occurred on operating at a point considerably below the normal capacity of the machine, and was checked with comparatively little trouble by throttling the intake slightly and taking up a small lost motion on the governor connections, a legacy of the previous blast that had not been attended to. All this required only a few hours' time. In. March, 1914, the furnace being banked on account of a blizzard that cut off our freight deliveries for five days, the opportunity was used to replace the carbon packing on the steam-turbine shaft and to repack the steam inlet valves. In June, 1914, the blower was off 8 hr. to replace an oil ring and scrape a bearing. With these exceptions we have made continuous use of the machine and find we can depend upon it with entire safety as a piece of machinery.

Jan 4, 1915

By H. F. Johnson, C. S. Harloff

The Nichols series system of electrolytic copper refining has successfully maintained its strong competitive position in the copper-refining industry of today; therefore the improvements made in accomplishing this result are of interest. While additional interest would lie in specific comparisons of results obtained in series operation with those in multiple, we have refrained from such a comparison because it can be fair to both only when they are operating under similar conditions on the same grade of materials. Historical The Nichols Copper Co. started a small refinery at Laurel Hill, using its present system, about 1892. The details of the process in its early stage of development were kept strictly secret, so that no information was published or interchange of ideas permitted with the staffs of other copper refineries, where the multiple system was being developed at the same time. However, the fundamentals of the process and type of cell used today differ very little from their earliest form. All operations including loading and unloading of tanks, and all transportation as well, were carried on by hand. The plant remained in this condition with a gradual expansion taking place until the World War forced such a rapid development that little time or thought could be devoted to modernization or mechanical improvement requiring careful design or detailed planning. Considerable progress was made, however. (1) Large refining furnaces were developed. (2) The old expensive air-lift type of circulation was abandoned in favor of the present system. (3) Operating technique was gradually developed to a high point of efficiency. (4) Tank construction and lining were greatly improved, the first concrete tank being installed in 1915. (This tank is still in operating condition.) (5) A new power plant was constructed. (6) Fuel oil was substituted for lump coal on the refining furnaces. (7) Mechanical casting of the finished product was accomplished. During this entire period the plant was particularly fortunate in receiving only high-grade, clean copper bullion coming principally from the Phelps Dodge mines in Arizona. This, together with the lack of

Jan 1, 1934

By R. B. G. Yeo

The effects of alloy additions on the M, and A, temperatures of an Fe-22.5 pct Ni alloy have been determined. Increasing amounts of titanium, colum-bium, vanadium, and silicon raise and then lower M,while raising A, cmtinuously. Cobalt raises both M, and A,. Aluminum has little effect on Ms but raises A,. Chromium md nickel lower M, and A,. It is proposed that elements raise M, in accordance with their effect on the Ae3 temperature of iron until the lattice becomes stiffened against the shear transformation so that M, is then lowered. An anomaly, first pointed out by Zener,1 arises in steels when the addition of elements, such as molybdenum and tungsten, which raise the Ae3 temperature, also lower the M, temperature.2'3 During the development of a series of martensitic precipitation-hardening (maraging) steels, the effect of several elements on the transformation of austenite to martensite was studied. The results show that under suitable conditions several elements which raise Ae3 also raise the M, and A, temperatures. PREPARATION OF MATERIALS STUDIED A series of alloys was made in which cobalt, titanium, columbium, vanadium, silicon, aluminum, molybdenum, chromium, and nickel were added to an iron base containing 22.5 pct Ni. The compositions of the alloys prepared are given in Table I. The residual manganese contents of the heats were in the range of 0.030 to 0.35 pct, silicon 0.05 to 0.1 pct, carbon 0.0008 to 0.009 pct, and nitrogen from 0 to 0.004 uct. The allois were made as 50-lb induction heats starting with electro-iron and electro-nickel, melted in air to oxidize impurities. Additions of silico-manganese and ferro-silicon were made after which the power was turned off to allow the products of deoxidation to rise and be skimmed from the surface of the melt. The furnace chamber was pumped down to a pressure of 5 p and the charge was heated to 2900°F for the addition of other alloying elements. The heats were poured into five 10-lb ingots, making successive alloy additions to each. The ingots were soaked for 2 hr at 2300°F and hot-worked to 3/4-in.-diam bars. This stock was heated to 1500°F for 1

Jan 1, 1963

By M. B. Bever, A. M. Reti, A. K. Jena

The results of this investigation show that in the system SnTe-PbTe l) the solid solutions have small exothermic heats of formation relative to the binary compounds, 2) solid-solution hardening is almost absent, 3) the tin and lead atoms are .randomly distributed on the sublattice occupied by them and do not undergo an ordering transition during a thermal treatment designed to promote such a transition, and 4) the lattice parameter changes linearly with composition. These findings suggest that the solid solutions of tin telluride and lead telluride approach ideal behavior. THE binary compounds SnTe and PbTe form a continuous series of solid solutions.' Information on several physical properties of these solid-solution alloys has been published.1"3 In the work reported here, the heats of formation, microhardness, and lattice parameters of these alloys have been measured and the possibility of an order-disorder transition has been investigated. Order-disorder transitions occur in some solid solutions of binary compounds. In the system Bi2Te3-BizSes, for example, the electropositive bismuth atoms and the electronegative tellurium and selenium atoms always occupy separate layers. In the disordered alloy Bi2Te2Se, the tellurium and selenium atoms are randomly distributed on the layers occupied by them, while in the ordered alloy they occupy distinct layers.4 The NaC1-type (Bl) structure of SnTe-PbTe alloys consists of two sublattices, one of which is occupied by the electropositive tin and lead atoms and the other by the electronegative tellurium atoms; any ordering would be expected to occur in the sublattice occupied by the tin and lead atoms. PREPARATION OF SPECIMENS Polycrystalline specimens of PbTe and Sn1-xPbxTe (x = 0.25, 0.50, and 0.75) were prepared by melting stoichiometric amounts of lead (99.999 pct), tin (99.98 pct), and tellurium (99.999 pct) in evacuated and sealed Vycor tubes. Because of the deviation of tin telluride from the stoichiometric composition5 this compound was prepared by melting 49.8 at. pct Sn and 50.2 pct Te. The tubes containing the melts were quenched into water; the solidified ingots were removed from the tubes and annealed for 2 weeks in vacuum (PbTe approximately 100°C below its melting point, the three alloys 100°C below their solidus tem-

Jan 1, 1969

By R. D. Carnahan, J. E. White

ThE use of strain gages in the measurement of microplastic behavior of materials is well-known.'-3 Recently it has been suggested that similar techniques might be useful for determining stress relaation. It is the purpose of this report to comment on the use of strain gages in the measurement of strains in the vicinity of 10"6. We will also discuss observations of an anomalous anelastic behavior apparently associated with small temperature changes, which accompanies the unload portion of a load-unload microstrain test. The key to successful strain determinations at levels below 1 pin. per in. is a good gage-mounting technique and either precise ambient temperature control or a set of matched temperature-compensated gages. The importance of good mounting cannot be overemphasized, for example, as in the use of Eastman 910 contact cement. If the cement layer is not sufficiently thin and properly hardened, it is possible to observe anomalous negative stresses when small loads are removed, which relax back to zero in an orderly way with time. Such anomalous behavior, thought to be due to gage bonding, has been reported in microstrain experiments by Thomas and verbach' who observed a negative strain of -3 X lo-' upon unloading. This kind of behavior severely limits the over-all strain sensitivity which can be achieved in such tests. The relaxation of a small positive strain subsequent to unloading in a load-unload experiment is quite normal, however, and is to be expected. The occurrence of an apparent negative strain is also encountered in those instances where the elasticity of the bonding cement is exceeded—for example 0.5 pct or 5000 pin. for cured Eastman 910. An elastic strain of this magnitude can be encountered during load-unload type testing particularly in higher-strength materials (-150,000 yield strength). During the course of microplasticity studies on pure nickel and nickel alloys,' the authors have made the following observation. In a four-point bending test, two active gages are mounted one on each side of the beam as arms R1 and R z of a conventional strain-gage bridge circuit shown in Fig. l(a). This technique provides two advantages: the sensitivity is doubled because R1 and Rz experience opposite strains and temperature compensation is provided automatically because any ambient temperature change would cause both gages to see a strain of like sign whose signals would cancel in the circuit.

Jan 1, 1964

[Abstmct of remarks by R. II. Sweetser arid suhscqueut discussion at the New York Meeting, February, 1926. The Transactions mill ultimately contain a report of work resulting from these discussions. Need for a standard of ualuration.—There should be an accepted method for evaluating the different kinds of bituminous coals based on their carbon just as that for iron ores is based on iron. Variation in the classes of coals and their desirability fol the different industrial uses is analagous to the case of iron ores. The iron people have developed a standard. In the past coals have not been intelligently distributed because the public has not been informed as to its uses. Many operators have known nothing about the final disposal of the coal shipped from their mines. Sales agents and retailers have had no means of evaluating coals except to make the price as high as the market will stand. Producers and distributors need to know how much more valuable the coals would be if prepared so as to contain less objectionable material. Mr. Swectser cnlletl on the Goal and Coke Committee of the Institnte to organize a study through producers and users to develop a method scientifically and comnereially sound E. A holbrook said that the information exists but the public is unwilling to investigate. He praised Ashley's1 nomenclature of the different kind of coal which has been accepted by the Coal Mining Institute of America and recommended to the American Enginecring Standards Commitee. G. S. Rice pointed out the wider variety and distribution of consumption of coal compared to Iron ore. C'. M. Young approved Mr. Sweetser's remarks and hoped lor a research institution, probably endowed, to study utilization of coal after it comes from the ground. Mr. Sweetser cited incidents to prove his former statements. He said that a reduction of 1 per cent. ash in the coal would cut down the cost of pig iron at a blast furnace 30 c. a ton, that the coal men should tell what the iron men would have to pay to get better coal. H. J. Prryn endorsed the need of blast-furnace operators to know the kind of coal from which their- coke is made and the latler's ash content, as this affects coke consumption. A. C. Fieldncr explained that the difficulty of evaluating coal on the basis of chermical analyses for calorimetric tests is: (1) representativr

Jan 1, 1927