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By Robert B. Sosman

The chance that a Howe Memorial Lecturer will be able to refer back to a personal contact with the distinguished metallurgist for whom this lectureship is named grows steadily I I did not have the pleasure of his personal acquaintance, but I did receive from him in 1916, quite unexpectedly, a letter commenting On a paper that I had recently published27 On "Types of Prismatic Structure in Igneous Rocks." The paper was written for geologists and petrologists, but it had an application, naturally, to the crystallization of iron and steel in a mold. The letter impressed me at the time, and still does, with the breadth of of Howe's interests and his perseverance in keeping up with the progress of any branch of knowledge that had metallurgical connotations. Scope of the Lecture During several years preceding the date mentioned I had worked in collaboration with Arthur L. Day and E. T. Allen8 at the Geophysical Laboratory, Carnegie Institution of Washington, on the temperature scale as defined by the nitrogen thermometer at high temperatures. Later (1928-1947) I had the opportunity of helping to apply this experience to the pyro-metric problems of the steel industry. Because of the range of its temperatures, the multiplicity of the methods used, and the variety of its purposes, pyrometry in the open-hearth process has always offered a fertile field for both research and development. I am therefore devoting an hour to the subject of temperatures in the basic open-hearth furnace, the furnace that makes most of our steel in the united States. I would direct your attention particularly to the choice of the first two words in the title of the Lecture. One sometimes hears or reads of the ((temperature of such-and-such a furnace," as if it were a single, measurable, characteristic quantity. I need hardly emphasize to any one who has ever operated a furnace or a kiln that " temperature of the furnace " is a meaningless phrase. Even if we confine our attention to the space enclosed by the roof, walls, and hearth of an open-hearth furnace, it is doubtful whether any such space has ever been so uniform in temperature that the phrase would have a meaning. In any furnace, there are many different temperatures, capable of being measured at many different places, and actually being measured for several different purposes. These pyrometric purposes, methods, and results, if given in detail, would expand this lecture into a book on the basic open-hearth process. I must therefore confine myself to a statement of the range of temperatures as they have been observed in various parts of the furnace, indicating in a general way why they are measured, and mentioning the methods that are available without attempting to describe these

Jan 1, 1949

By Robert B. Sosman

The chance that a Howe Memorial Lecturer will be able to refer back to a personal contact with the distinguished metallurgist for whom this lectureship is named grows steadily I I did not have the pleasure of his personal acquaintance, but I did receive from him in 1916, quite unexpectedly, a letter commenting On a paper that I had recently published27 On "Types of Prismatic Structure in Igneous Rocks." The paper was written for geologists and petrologists, but it had an application, naturally, to the crystallization of iron and steel in a mold. The letter impressed me at the time, and still does, with the breadth of of Howe's interests and his perseverance in keeping up with the progress of any branch of knowledge that had metallurgical connotations. Scope of the Lecture During several years preceding the date mentioned I had worked in collaboration with Arthur L. Day and E. T. Allen8 at the Geophysical Laboratory, Carnegie Institution of Washington, on the temperature scale as defined by the nitrogen thermometer at high temperatures. Later (1928-1947) I had the opportunity of helping to apply this experience to the pyro-metric problems of the steel industry. Because of the range of its temperatures, the multiplicity of the methods used, and the variety of its purposes, pyrometry in the open-hearth process has always offered a fertile field for both research and development. I am therefore devoting an hour to the subject of temperatures in the basic open-hearth furnace, the furnace that makes most of our steel in the united States. I would direct your attention particularly to the choice of the first two words in the title of the Lecture. One sometimes hears or reads of the ((temperature of such-and-such a furnace," as if it were a single, measurable, characteristic quantity. I need hardly emphasize to any one who has ever operated a furnace or a kiln that " temperature of the furnace " is a meaningless phrase. Even if we confine our attention to the space enclosed by the roof, walls, and hearth of an open-hearth furnace, it is doubtful whether any such space has ever been so uniform in temperature that the phrase would have a meaning. In any furnace, there are many different temperatures, capable of being measured at many different places, and actually being measured for several different purposes. These pyrometric purposes, methods, and results, if given in detail, would expand this lecture into a book on the basic open-hearth process. I must therefore confine myself to a statement of the range of temperatures as they have been observed in various parts of the furnace, indicating in a general way why they are measured, and mentioning the methods that are available without attempting to describe these

Jan 1, 1949

By S. A. LoPilato, J. T. Smith

SEVERAL techniques have been evaluated for cooling the throat area of rocket-nozzle inserts to prevent erosion or fracture of the inserts during exposure to high operating temperatures and pressures. Self-cooled composites, such as infiltrated tungsten, have shown considerable promise for these applications. These composites can be fabricated by infiltrating the refractory matrix with a lower-melting metal or non-metal which is insoluable in tungsten. During firing, the lower-melting substance undergoes a series of continuous endothermic phase changes which absorb sufficient heat to maintain the nozzle matrix material at or below a safe operating temperature. At present, the state-of-the-art has reached a point where the refractory matrix density and microstruc-ture have been established as the critical parameters to be controlled for optimum self-cooled performance.'" Nondestructive testing has been utilized to ensure that porous tungsten billets were of uniform density and free from cracks or other defects prior to fabrication into rocket nozzle inserts. Ultrasonic-velocity techniques have been employed because of their reliability and reproducibility. The purpose of this note is to present and interpret the test data developed for porous tungsten matrices. For evaluation purposes, tungsten powders with Fisher subsieve sizes of approximately 4 and 18 p have been obtained for study from four commercial sources: the General Electric Co., Wah Chang Corp., Fansteel Metallurgical Corp., and Kennametal, Inc. Porous tungsten matrices were fabricated from the powders by hot pressing in induction-heated graphite die assemblies. Typical billets ranged from 3 in. diam, 2 in, high to 5 in. diam, 5 in. high. The ultrasonic-velocity measurement technique employed was through transmission, pulse echo at a frequency of 1.0 mc using matched barium titanate crystal transducers. The testing equipment included a pulsed ultrasonic generator, an amplifier, a specimen holder, and an oscilloscope, as shown in Fig. 1. The porous tungsten thickness was measured to i 0.0005 in, with precision micrometers while the oscilloscope achieved 0.02 psec time measurement accuracy. The time for a sound wave to pass through the billet, the bulk wave velocity, was calculated to 0.5 pct using Eq. [l]: V-} where V = bulk wave velocity, in. per psec, T = specimen thickness, in., and / = time, psec. To develop inspection standards, the bulk density of a porous tungsten billet was determined by the ASTM water-immersion technique.3 The ultrasonic-velocity measurements were completed at seventeen positions for each billet and averaged to develop a characteristic standard velocity for a particular tungsten powder at several density levels. A plot of ultrasonic velocity vs density is presented in Fig. 2 for six different tungsten powders. This graph has been established as

Jan 1, 1967

By Margaret Dienes, Karl L. Fetters

It is recognized that ingot structure is important in determining the quality of finished steel. Such elements of ingot structure as the size, shape and distribution of primary crystals; the size, shape and distribution of shrinkage cavities; the degree and kind of segregation (both macro and micro); the distribution of nonmetallic impurities and gas cavities are each the result of solidification phenomena. 'These structural features vary with variations in ingot practice. Their control requires a knowledge of their correlation with the variables of ingot practice. The structures of full-sized commercial steel ingots have been studied extensively by the Steel Ingots Committee of the Iron and Steel Institute.l This work has contributed much to our knowledge of ingot structure and the factors that control it. These investigations of necessity have been limited in scope because of their costliness and the great amount of time required. Studies of the structure of small steel ingots have not been very satisfactory because of the rapid rate of freezing of the ingots. Their structures are thus difficult to resolve and to interpret. Medium sizes of steel ingots in the ranges of 150 to 500 lb. do offer opportunity for study, but their cost also becomes greater and their use less expeditious. Experimental models for the study of steel-ingot structure have been made of nonferrous metals. Gathmann2 used lead-tin alloys and reported that they were satisfactory for determination of the location of the major shrinkage cavities and the Liplanes of weaknessv resulting from the pattern of crystallization. Certain features of mold design have been illustrated by these results. Bezdenezhnihk3 has used copper and aluminum ingots similarly and has shown the effect of mold-wall thickness on the depth of columnar grains. These studies of nonferrous models have been useful, but their results have been limited because the analogy with steel ingots obviously is not a close one. Model wax ingots have also been useful in pointing out important features of mold design. Gathmann4 watched the solidification of wax ingots, through a glass-walled mold, and has reported the effects of mold type on the location of the shrinkage cavities. Segregation was simulated by using a mixture of paraffin and stearine and adding a red dye that on freezing segregated preferentially to the stearine. Brearley5 also used wax models to determine the effects of some of the principal features of mold design. Carlsson and Hultgren6 dsed stearic acid to show that the columnar crystals of ingots tend to slope upward progressively from the mold wall toward the center of the ingot. As with the nonferrous ingots, the wax ingots have

Jan 1, 1943

By Margaret Dienes, Karl L. Fetters

It is recognized that ingot structure is important in determining the quality of finished steel. Such elements of ingot structure as the size, shape and distribution of primary crystals; the size, shape and distribution of shrinkage cavities; the degree and kind of segregation (both macro and micro); the distribution of nonmetallic impurities and gas cavities are each the result of solidification phenomena. 'These structural features vary with variations in ingot practice. Their control requires a knowledge of their correlation with the variables of ingot practice. The structures of full-sized commercial steel ingots have been studied extensively by the Steel Ingots Committee of the Iron and Steel Institute.l This work has contributed much to our knowledge of ingot structure and the factors that control it. These investigations of necessity have been limited in scope because of their costliness and the great amount of time required. Studies of the structure of small steel ingots have not been very satisfactory because of the rapid rate of freezing of the ingots. Their structures are thus difficult to resolve and to interpret. Medium sizes of steel ingots in the ranges of 150 to 500 lb. do offer opportunity for study, but their cost also becomes greater and their use less expeditious. Experimental models for the study of steel-ingot structure have been made of nonferrous metals. Gathmann2 used lead-tin alloys and reported that they were satisfactory for determination of the location of the major shrinkage cavities and the Liplanes of weaknessv resulting from the pattern of crystallization. Certain features of mold design have been illustrated by these results. Bezdenezhnihk3 has used copper and aluminum ingots similarly and has shown the effect of mold-wall thickness on the depth of columnar grains. These studies of nonferrous models have been useful, but their results have been limited because the analogy with steel ingots obviously is not a close one. Model wax ingots have also been useful in pointing out important features of mold design. Gathmann4 watched the solidification of wax ingots, through a glass-walled mold, and has reported the effects of mold type on the location of the shrinkage cavities. Segregation was simulated by using a mixture of paraffin and stearine and adding a red dye that on freezing segregated preferentially to the stearine. Brearley5 also used wax models to determine the effects of some of the principal features of mold design. Carlsson and Hultgren6 dsed stearic acid to show that the columnar crystals of ingots tend to slope upward progressively from the mold wall toward the center of the ingot. As with the nonferrous ingots, the wax ingots have

Jan 1, 1943

By A. H. Geisler, J. H. Keeler

Preferred orientations in unalloyed zirconium were determined by the Geiger-counter spectrometer X-ray diffraction technique. With increasing P-annealing temperature the following textures were obtained: l—a retained a-annealing texture, 2—additional orientations predictable from the a-p (Burgers) relationship, and 3—a texture derived from a cube texture in the p phase. Earlier work on cold-worked and a-annealed zirconium was reappraised to show a quantitative dependence of rotations on temperature and to identify spurious areas of some of the pole figures. IN a previous paper,' the preferred orientations of high purity zirconium sheet were described for cold-rolled and annealed samples. Annealing temperatures up to 900°C, which is slightly above the allotropic transformation temperature, were explored. Of interest was the observation that the orientation of the hexagonal-close-packed material after annealing in the temperature range of the stable body-centered-cubic phase was similar to that of the material which had been annealed in the a temperature region, although a change in texture would be expected because of the many new orientations based on an orientation relationship between the two forms of zirconium. The reversion to an original orientation after an allotropic transformation cycle is not unusual. It has been found for titanium,"* for thallium," and for cobaltB among the hexagonal metals. Burgers found in his original work7 that, when zirconium was cooled through the allotropic transformation and then reheated, the body-centered-cubic phase reverted to the original orientation. Additional experimental work has been carried out to further explore the textures of zirconium after annealing in the temperature range above the allotropic transformation. In addition, a reappraisal was made of the earlier results for zirconium' in light of recent work on titanium4 which has shown that the texture type depends quantitatively on the temperature of annealing and that spurious areas may be encountered in the pole figures of hexagonal metals determined by the X-ray spectrogoniometer technique of analysis. Experimental Procedure Crystal-bar zirconium prepared by the iodide process was the material used in this investigation. The major impurity was hafnium which was less than 0.3 pct. The composition obtained by spectro-graphic analysis is given in Table I. Cold-rolled specimens were prepared from crystal bar by a series of reductions of approximately 0.010 in. until the sheet reached a thickness of 0.010 in., after which it was cold rolled to 0.001 in. thickness between sheets of alloy steel. The total cold reduction amounted to about 99.8 pct. Specimens were annealed for % hr at 1000" to 1100" to 1200°C or 1 hr at 1400°C in an evacuated Vycor or quartz tube. The transmission pole figures were obtained by

Jan 1, 1956

By C. R. Dodson, D. Goodwill, E. H. Mayer

The paper summarizes the historical background of the pressure-volume-temperature analyses of reservoir fluids, the errors involved in both the sampling and testing of reservoir fluids, the type of information required of a PVT determination, and the field conditions that limit the application of any one analysis. Particular emphasis is placed on the necessity for approximating as closely as possible the liberation sequence occurring in the producing formation, flow string, and surface separators. A combined differential and flash or "composite" liberation is suggested as the best means of approximating this liberation sequence. HISTORICAL BACKGROUND Petroleum reservoir engineering commonly is considered to be one of the newest fields of petroleum science, yet much work of a theoretical and intuitive nature was done many years before the modern techniques of reservoir analyses were developed. The period 1910-1924 saw considerable work in the field of reservoir behavior done by the U. S. Bureau of Mines. This work:.' although entirely theoretical, pointed out the importance of gas in the recovery of oil from the reservoir. The statement by J. 0. Lewis that 20 per cent or less of the oil originally in place in a pool was recovered from the ground under uncurtailed production conditions caused some operators to re-examine and modify their production methods. However, though these works showed methods of production that have subsequently resulted in greater oil recoveries, they in general went unnoticed, even though there was a fear that the nation's petroleum resources were being exhausted. The period 1924-1933 saw the industry take considerably more interest in reservoir behavior because of an unfounded fear of its inability to replace oil reserves, the possibility of government regulation, and the energy of one man, Henry L. Doherty. Doherty aroused heated discussions in the industry concerning conservation. To prove or disprove his theories the first experimental work on the reservoir behavior of petroleum was undertaken. The papers of Dow and Calkin,' Beecher and Parkhurst," and Mills and Heitheckere are classics although their experimental procedures were crude. These papers proved that the properties of petroleum in the reservoir are quite dissimilar to the properties measured at the well head. Gas dissolved in the oil phase was recognized as having considerable importance as had been predicted by the earlier theorists. Slightly later Miller and his co-workers assembled the first text correlating all the known data on the reservoir behavior of petroleum and used, these data to show the economic value of conservation. Quantitative application of pressure-volume-temperature analyses of reservoir fluids was given in the paper of Coleman, Wilde, and Moore"; this work showed that with sufficient laboratory and production data prediction of reservoir behavior was possible. The refined sampling and labora-

Jan 1, 1953

By William Klement

THIS note reports the results of some attempts to metastably extend the primary solid solubilities of tin, antimony, and silicon in silver by rapidly quenching these binary alloys from the melt. The procedures employed for alloy preparation, quenching, and Debye-Scherrer X-ray diffraction measurements have been described elsewhere. The lattice parameters obtained for the fcc structures in Ag-Sn and Ag-Sb alloys are presented in Fig. 1, together with the results of Owen and Roberts.4 Alloy compositions are believed to be within ± 0.2 at. pct on the basis of negligible weight losses during preparation and reproducibility of the lattice spacings. Diffraction lines from hcp phases were also detected: the relative visual intensities of the fcc (200) and hcp (10.2) lines were estimated as shown in Table I. The intensities were m for the (200) and w for the (10.2) in a quenched 13.6 at. pct Sn alloy: a lattice spacing for the fcc structure could not be reliably obtained, however. As seen from Fig. 1, the lattice parameters vary linearly with composition up to 8., at. pct Sb and 13." at. pct Sn, respectively, which may be compared with the maximum equilibrium solid solubilities5 of 7.2 at. pct Sb and 11.5 at. pct Sn, respectively. The presence of the hcp phases, which were found together with the fcc phases, is a consequence of the competition1,3 in the nucleation and growth processes during solidification. Both the fcc and hcp phases must be of the same composition for those alloys in the range where lattice parameters increase linearly with solute concentration. Despite much effort with quenched alloys of several silicon concentrations, it has not been possible to obtain lattice spacings of sufficient precision to establish the variation of lattice parameter with composition or the maximum metastable solid solubility: the equilibrium data5 suggest little primary solid solubility of silicon in silver. For alloys containing less than 16 at. pct Si, the Si (111) diffraction line was not observed. For alloys containing 10 to 25 at. pct Si, faint low-angle lines were detected and these could be indexed as the (10.0), (00.2). and (10.1) reflections of an hcp structure with a = 2.87 + 3A. c = 4.52 ± 3A, and c/a = 1.57 ± 2. The 16 at. pct Si alloy was quenched to, and examined at. liquid nitrogen temperatures without any change observed in the proportion of the hcp phase. These experiments were jointly supported by the Atomic Energy Commission and Office of Naval Research under a program directed by Professor P. Duwez. The assistance of H.-L. Luo and A. Abu-Shumays is acknowledged. as is the support afforded

Jan 1, 1965

By Donald B. Hunter

The Ti-Be system up lo 10 wt pct Be with cortlmercialll' pure titanium has been determined using metal-lographic techniques. Beryllium forms the p eutec-toid type of dinqarz with titanium; the eutectoid occurs at 0.5 xt pct Be azd 1500 F, while an eutectic is foritled at 1887°F containing between 5 and 7.5 rt pct Be. The solubility of beryllium in a titanium does not exceed 0.05 zvt pct and the maximum solubility of Beryllim in 0 titanium is 1 wt pet. PREVIOUS work on the Ti-Be phase diagram indicated that additions of beryllium to titanium resulted in a marked lowering of the melting point,''' and it was also observed that the solubility of beryllium in both a and p titanium was retricted.- With the limited data available, McQuillan and McQuillan constructed a partial hypothetical diagram of the Ti-Be system,= assuming that beryllium formed the 0 eutectoid type of system with titanium. Subsequently Bedford published a tentative diagram of the entire Ti-Be system: although he did not investigate alloys containing less than 10 wt pct Be. This diagram included several compounds described by other authorities.'-l3 The following account describes work directed toward determining the form of the titanium-rich portion of the phase diagram up to 10 wt pct Be. MATERIALS AND METHODS Titanium sponge and a master alloy containing 25 wt pct Be were used in the formulation of the alloys; the chemistry of these materials is detailed in Table I. The alloys were prepared as 250-g compacts which were melted into buttons by arc melting under purified argon on a water-cooled copper hearth. Results of analyses for beryllium are shown in Table I but no determination of other elements was made at this stage. The alloys were hot-rolled at 1650°F to produce 0.1-in.-thick sheet. Alloys containing up to 1.5 pct Be were fabricated without trouble; samples containing 2 pct cracked initially upon hot rolling, but thereafter rolled satisfactorily to sheet. The 5, 7.5, and 10 pct were hot short and could not be rolled. Surface contamination was removed from samples by sandblasting and pickling in a 5 pct HF-35 pct HNOs solution. For metal log raphic examination, heat-treated specimens were mounted transverse to the rolling direction, ground on silicon carbide papers of increasing fineness to 600 grit, and electropolished at 20 v using a solution containing 600 ml of methanol, 60 ml of perchloric acid, 360 ml of butyl cellosolve, and 2 ml of Solvent "X". Difficulty was experienced in obtaining good electropolished surfaces with samples containing more than 1 pct Be, the degree of difficulty in-

Jan 1, 1967

By R. W. Heckel

A method is described whereby the relationship of both the "at-pressure" powder compact density and the "zero-pressure" compact density to the applied pressure may be obtained from continuous measurements of punch movement during a single compaction operation. The rate of density increase with applied pressure for the metal powders is found to be proportional to the volume fraction of pores for pressures exceeding a lower limit which varies from 15,000 to 30,000 psi, depending on the powder. 1 HE compaction of powdered materials is carried out primarily to increase the density of the material. If the ultimate goal of the over-all process is the attainment of minimum porosity, compaction is responsible for most of the densification. For example, loose powdered metals have porosities of about 65 to 75 pct. Axial loading in a die or hydrostatic pressure may effectively reduce the porosity of most powders to 20 pct or lower with pressures of 50,000 psi and greater. The relationship between the density of a powder compact and the pressure needed to achieve that density is most commonly obtained by pressing several compacts, each at a different pressure. Measurement of the densities of the individual compacts when they are removed from the die then provides the density-pressure relationship. However, this method suffers from several disadvantages. Because a large number of compacts and pressing operations are required, it is inherently slow. Furthermore, since density measurements are made after the specimens are removed from the die, data obtained refer only to pressures greater than those necessary to form a coherent compact. The third disadvantage is the inability of this method to provide information about the compact density at the applied pressure in the die. Because the determination of density-pressure relationships has been a slow, tedious process, investigators have sought to express the compaction behavior of powders by other means. The general terms "comparability" and L'compressibility" have been used to rank powders qualitatively according to their compaction characteristics. To restore a quantitative nature to the subject and to prevent confusion, Schwarzkopf1 has proposed that compac-tibility be defined as the minimum pressure needed to produce a given green strength, while compressibility should be used to indicate the extent to which the density of a powder is increased by a given pressure. Probably the most widely used of the compaction parameters is the "compression ratio,'' which is generally defined as the ratio of the compact density obtained by pressing at a given pressure to the apparent density of the loose powder.2 However, the description of the compaction behavior of a powder by these parameters provides only limited information about the process because of their applicability to just one specific condition such as a given green strength or a given pressure. The method of obtaining density-pressure relationships which will be described in the present paper was designed to eliminate the shortcomings of the previous techniques while maintaining equivalent accuracy and precision. EXPERIMENTAL TECHNIQUES The general principle employed makes use of the fact that the linear movement of the punch during a

Jan 1, 1962

By T. P. Papazoglou, N. A. D. Parlee, W. C. Phelps

HE high vapor pressures of metals such as lead, calcium, lithium, bismuth, and magnesium at steel-making temperatures present experimental problems which have thus far rendered it almost impossible to obtain really reliable data for their solubilities in liquid iron. Many investigators have attempted to equilibrate liquid iron in the same crucible with the undissolved liquid phase of such volatile metals. The published results,l-6 although useful, are often questionable on the grounds of not being obtained under true equilibrium conditions. Such information is not always of practical value in any case since the equilibrium vapor pressure is often several atmospheres and steel is not currently made at these pressures. Solubility measurements at lower partial pressures (< 1 atm) appeared to be more practical and easier to make. These data could be used to calculate solubilities at other pressures where Henry&apos;s Law is obeyed, and to estimate solubilities under other conditions of temperature and pressure with useful accuracy. This note outlines the development of a general technique for the measurement of solubilities in systems of this kind. The method involves equilibration of the high-boiling metal at known temperatures with the vapors of a low-boiling metal at known partial pressures. Analyses of quenched samples provide vapor pressure-solubility data and make calculations of alloy thermodynamics possible. The principle involved is similar to the closed-system diffusion-transport method which is difficult to apply with most high-melting liquid metals like iron, due to closure problems. A two-zone horizontal (molybdenum wire element) tube furnace, Fig. 1, provides two constant-temperature zones in a reaction tuve (3/4 in. ID by 1 in. OD by 36 in.). A high-boiling metal sample, 9, introduced in the higher-temperature zone, is maintained at temperature T1, and a volatile metal sample, 7, in the lower-temperature zone, is held at T2. A stream of argon with 10 pct hydrogen is passed via flowmeters, 1, and mixing-drying towers, 2 and 3. through the reaction tube at a favorable flowrate and acts as a carrier gas which entrains vapor from the volatile liquid metal at a specific constant partial pressure. The gas mixture passes through a system of constrictions, 6 and 8, to the higher-temperature zone, establishes intimate contact with the high-boiling liquid sample, 9, and exits through a small condenser tube. The entire system is at (nearly) atmospheric pressure and the volume of carrier gas passed is measured with a wet gas meter. When the high-boiling sample attains equilibrium with the vapor phase, both samples are removed and quenched. Analysis of the high-boiling sample for solute content reveals its solubility for the low-boiling metal at a vapor pressure calculated from carrier-gas volume and either a) weight loss of volatile metal or 6) weight gain of high-boiling sample plus condenser (which collects the undissolved vapors). To test the capabilities of the method, liquid silver at 1403&apos;C was equilibrated with lead vapor at various partial pressures. The relatively simple Pb-Ag system was particularly suitable for uncovering experimental problems and providing the first step toward investigations with more volatile metals and more difficult combinations.

Jan 1, 1965

By R. P. Abendroth

The hydrogen-water vapor ratio at which Fe-Cr alloy, chromium oxide, andiron chromite coexist in equilibrium was determined between 900" and 1200°C. A thermogravimetric method was used to determine equilibrium conditions. The results fit a straight-line relationship in the temperature region studied, and are given by Reduction experiments were also performed to confirm the results of the equilibrium investigation. ThE oxygen pressures at which Fe-Cr alloy, chromium oxide, and iron chromite coexist in equilibrium have been previously determined by Boericke and angert,&apos; Morozov and Novokharski,&apos; and Katsura and uan. Only one determination (at 1300°C) was made by Katsura and Muan, but it agrees with the results of orozov and Novokharski. The results of Boericke and Bangert, however, differ appreciably from the results of these investigators. Previous studies have assumed that the equilibrium metallic phase is pure iron, but Dahl and Van vlack have shown that the iron contains from about 1 wt pct Cr at 1000°C to over 2 wt pct above 1300°C. The chromium oxide also contains a small amount of iron in solid solution. In the present study, hydrogen-water vapor mixtures were equilibrated with the condensed phases, using a therrnogravimetric method to determine equilibrium conditions. The reaction can be written EXPERIMENTAL General Procedure. The starting material was a sintered pellet of Fe2O3-Cr2O3 solid solution with a hole in the center, and was placed on a fused silica hook. This assembly was raised into the preheated hot zone of the furnace in a helium atmosphere, hooked onto a fused silica hangdown suspended from one arm of an Ainsworth Model RV-AU-1 recording balance, and the starting weight determined. A flowing hydrogen-water vapor atmosphere was then exchanged for the helium by evacuation, and the sample reduced until the weight loss indicated the sample composition to be in the alloy-Cr2O3-chromite field. The tem- perature was adjusted incrementally until constant sample weight was achieved for several hours, to within 0.02 mg. A hydrogen-water vapor atmosphere of different composition was then admitted, and the same procedure carried out. At the end of a series of determinations, the sample was examined by X-ray diffraction to verify the presence of the desired phases. Microscopic examination of the silica hook showed no interaction with the sample, nor did it lose any weight. Several criteria were used to insure equilibrium besides constancy of weight. For a given hydrogen-water vapor composition, equilibrium was approached from both oxidizing and reducing sides by varying the furnace temperature slightly. The resulting slow weight loss or gain was observed for several hours. Constant weight could be re-established by returning to the original furnace temperature. The last criterion used was varying the relative amounts of the phases by further reduction or oxidation, and observing any changes in temperature required for constant weight for a given hydrogen-water vapor atmosphere. None were observed. This procedure was essentially the same as approaching the equilibrium from oxidizing and reducing sides, but larger weight excursions were carried out. Sample Preparation. Reagent-grade Fe2O3 and Cr83 powders were mixed in the desired proportions and heated in air at 1250°C for 2 hr. The mixture was re-ground and heated in air overnight at 1250°C. X-ray diffraction showed complete solid-solution formation as a result of this procedure. The solid solution was then pressed into l/2-in.-diam pellets using Carbowax 4000 as a binder. The hole was drilled in the center, and the pellets were sintered 24 hr at 1250°C in air on a bed of Fe2O3-Cr2O3 of the same composition, contained in an alundum boat. After cooling, the pellet surfaces were abraded with 310 paper to remove any surface compositional differences, such as loss of Cr2O3. Chemical analysis of the sintered pellets was 67.16 wt pct CrP3 and 33.02 wt pct Fe203. Atmosphere Generation and Control. The hydrogen-water vapor atmospheres were generated by passing Matheson ultrahigh-purity hydrogen, with no further purification, through two water bubblers contained in a constant-temperature water bath. Since the water-vapor dew points required in this study were below room temperature, the bath was insulated, and was cooled by thermoelectric-immersion devices. The bath temperature was controlled to 0.0l0C. Since rather high flow rates of about 900 ml per min were used through the furnace tube, an independent check of the dew point was made to insure saturation of the hydrogen by the water vapor. Although the dew point could only be determined to within 1/2"C, the determined dew points agreed with the water-bath temper-

Jan 1, 1967

By R. D. Longyear

[Some Problems Involved in the Interpretation of Diamond-drill-hole Sampling and Surve ing (paper by J. J. Collins, Mining Tech., Jan. 1946). ............... I Geologic Interpretation of Magnetic Exploration on the Mesabi Range, Minnesota (paper by R. H. B. Jones, Mining Tech., July 1946) ................... 2] DISCUSSION R. D. LONGYEAR.*-Mr. Collins is to be commended very highly for the brief summary he has made of the currently used methods of taking diamond-drill sludge samples and the principles involved in evaluating the results. This paper should stimulate further discussion and research on this vitally important problem. It is particularly imperative that geologists and engineers know when assay results on sludge recovery can be accepted quantitatively and when they must be considered only qualitatively. In most cases where the sludge recovery is less than 95 per cent or more than 125 per cent, it is safest to consider the assays as of qualitative value only. Certain cases, however, are known where a relatively small proportion of the sludge sampling will give a reasonably accurate measure of the value of the total sample. One such case is ore in which the valuable mineral is of approximately the same specific gravity as the waste mineral, such as chalcopyrite in a massive pyrite body. The essential point is to determine the degree of accuracy of sludge sampling in any given drilling project and to weigh the results accordingly. It should be emphasized, however, that sludge sampling can be made reliable in many localities where careless practice produces unreliable results. In many instances, it is desirable to empty the core barrel in the core shack instead of at the drill, so that the engineer can examine the core as it first comes from the core barrel. It should be pointed out, however, that the drill * E. J. Longyear Co., Minneapolis, Minnesota. runner should be permitted to study the core to guide his future drilling. It is hoped that with the return of more normal conditions after the war geologists, engineers, contractors, and manufacturers will be able to carry on more research along the lines of improved core-barrel design and drilling technique with the objective of increasing core recovery so as to eliminate as far as possible the necessity of relying upon sludge samples. H. M. ROBERTS.*-Whoever in the future will have to do with the search for ore bodies and their exploration will have frequent occasion to refer to the clear and comprehensive summary on diamond-drilling methods by John Collins. His review of the experience of the last 40 years in this technique is invaluable. As Dr. L. D. Ricketts wrote in 1932, "The principles on which an art is founded are usually few and necessarily basic in nature, but he who wishes to achieve the power to select his aides and give success to important undertakings that may be intrusted to him in the future must ordinarily undergo years of drudgery in order to gain the experience that will enable him to distinguish such fundamentals through the haze of reinforcing detail that clothes and tends to disguise them."[t] Ricketts went on to say that since the beginning of the century there has been much

Jan 1, 1946

1. How Does One Determine Whether an Ore Body Will Block-cave? Page Mark A. Smith......... 122 Harry A. Leidich........ 122 McHenry Mosier ...,.. 22 R. W. Hughes ........ 122 Sherman R. Burdick ....... 123 R. T. Gallagher........I 23 Benjamin F. Tillson...... 123 Lucien Eaton...........123 C. F. Jackson..... . .. 123 Philip B. Bucky........... 126 2. How Does One Determine the Block Dimensions and the Development Work Necessary to Make an Ore Body Cave? Mark A. Smith... 125, 127, 129 Harry A. Leidich..........126 McHenry Mosier......126, 127, 132 R. W. Hughes...........126 Sherman R. Burdick.........127 R. T. Gallagher...........127 Benjamin F. Tillson......127,131 L. E. Young............127 Robert D. Hoffman.......128, 132 Gerald Sherman..........128 Philip B. Bucky......130, 131, 132 K. S. McClellan..........132 Tell Ertl.............132 3. How Do the Forces Act and What Are the Stresses Developed in a Block That Cause It to Block-cave? Mark A. Smith.........132, 135 Harry A. Leidich........133 McHenry Mosier . .. 133 R. W. Hughes ....... 133 Sherman R. Burdick..... . 133 R. T. Gallagher..........134 C. F. . Price, Jr. ........134 Benjamin F. Tillson.........134 C. F. Jackson......134, 135,137 R. Taborelli...........135 Frank A. Ayer ... .....136 Philip B. Bucky . .........136 Rollin Farmin . . .......136 . . . Weysser.....135, 136, 137 George S. Rice...........137 4. What Determines the Procedure in Removing Caved Ore? Harry A Leidich...........137 McHenry Mosier........137,141 R. W. Hughes...........137 Sherman R. Burdick........138 R. T. Gallagher...........138 Mark . Smith...........138 Philip B. Bucky......140,141,143 C. F. B. Price, Jr..........140 R. H. Bennett...........141 C. F. Jackson..........141, 143 Gerald Sherman..........141 Tell Ertl.............141 .. .. ..................143 C. H. Shoemaker..........143 5. What Are the Criteria for Determining the Efficiency of a Block-caving Operation? Harry A. Leidich.......... 143 McHenry Mosier......... 144 R. W. Hughes........... 144 Sherman R. Burdick.......144 R. T. Gallagher . ......... 144

Jan 1, 1946

By George A. Colligan, John M. Lo

Electrical resistivity as a function of temperature was investigated in undercooled gallium and under-cooled Ga-In alloy of eutectic compositian to examine structural changes in undercooled melts. A continuous linear extension of the resistivity was determined for 99.999 pct pure gallium when undercooled below the stable Ga(l)-liquid, and the metastable Gafl)-liquid equilibria. In icndercooled Ga-In, a significant continuous negative departure from linear resistivity behavior was observed below the eutectic temperature. All resistivity measurements were made by the four-point probe technique. ThE temperature range for investigations into the physical properties of liquids before freezing has been greatly extended with the undercooling of massive melts of pure metals and alloys. Experimental determinations of thermal and transport properties and diffraction patterns in undercooled systems should throw further light on the structural behavior of liquids. Many measurements showing prefreezing anomalies in viscosity1&apos;5 have been regarded677 as evidence for structural groupings in the liquid state. However, the majority of viscosity results,~)~-~~ conforming to the law 17 =A exp(~/RT), do not support theories of atomic aggregation. For the system Cd-Sb, which exhibits a metastable solid phase, Fisher and Phillipsg reported that, in undercooled alloys, the activation energies for viscous flow below the stable liquidus are much higher than those above it. Similarly, Miller et a1." observed a doubling of the activation energies for electrical conductivity in undercooled Cd-ib alloys. These effects were suggested as indicative of atomic association and clustering in the liquids at lower temperatures. With the recent establishment of metastable phases in pure gallium22 and its alloys,23 attempts were made during this investigation to undercool bulk samples and to determine the temperature dependence of electrical resistivitv. Pure gallium, when undercooled below -17°C at atmospheric pressure, can crystallize to either a stable Ga(1) phase (mp, 29.78"C) or a metastable phase identi-

Jan 1, 1967

By Charles R. Austin, Carl H. Samans

In an earlier serics of studies on 18-8 stainless steel at 600º, 700º, and 800ºC.l one pretreatment was used throughout; viz., 15 min. in hydrogen at 950°C., followed by an air quench. Several manufacturers of this alloy since have expressed doubt as to the suitability of the temperature employed, recommending instead the more customary Strauss treatment as promising superior results. In this subsequent investigation on the effects of the temperature of pretreatment several interesting points have arisen, which are described in this paper. Previous work on our equipment had shown a marked difference between alloys of "similar chemical composition" that had been manufactured by different companies. Accordingly, one mill-bar length was selected from which to prepare all specimens. It could then be assumed that any marked differences in creep characteristics would be due to effects resulting from variations in the pretreatment of the alloy. The material was furnished by the Allegheny-Ludlum Steel Co. in the form of 5/16-in. dia. rod, finished by air cooling from a mill anneal at 1950°F. (1066°C.). It was analyzed only for the elements shown: carbon, 0.07 per cent; chromium, 18.73; nickel, 9.46; manganese, 0.40. Three pretreating temperatures were chosen, the specimens being held for 15 min. in hydrogen at either: (1) 1150°C., to conform to the recommended Strauss treatment; (2) 950°C., to compare with the results of previous tests; or (3) 75Q°C., to initiate precipitation of carbides in the material before testing. As the test cross sections were only 1/8-in. dia., air cooling followed the annealing treatment. These treatments permitted two direct comparisons: (1) between the 1150" and 950°C. treatments to indicate the effect of grain size when all carbides were probably in solution at the start of the test; and (2) between the 950" and 750°C. treatments to indicate the effect of carbide "nucleation" for similar grain sizes.

Jan 1, 1940

By P. V. Martin

Shortly after the middle of the nineteenth century, the invention of the regenerative open-hearth furnace and the development of the Bessemer process stimulated a rate of steel production whose magnitude created an unprecedented demand for pig iron. Revolutionary improvements in furnace design, auxiliary equipment, and operating technique enabled the blast furnace to keep abreast of the constantly increasing requirements of the steel mill. The development of improved blowing equipment, more adequate facilities for material handling, and particularly the general use of anthracitc and coke to replace the physically weaker charcoal, led to a rapid expansion in both the height and volume of furnaces. Beyond a doubt, however, the greatest single factor in blast-furnace improvement at this time was the use of the higher blast temperatures made available by the replacement of the recuperative iron pipe stoves by the regenerative Cowper brick stove. The increased blast temperature not only resulted in greater output but also reduced fuel consumption . far more than could be explained by the additional heat content of the blast. The progress of iron manufacturing was thus largely mechanical and thermal. Little attention was given the chemistry of the process until the publication of the investigations of Sir Lowthian Bell.1 Bell&apos;s painstaking experiments and investigations gave to the blast-furnace man his first real scientific conception of blast-furnace chemistry. Bell&apos;s recognition of the dual function of the carbon, the technical importance of reversible reactions and chemical equilibria, and his conception of the degree of oxidation of the carbon as shown by the analysis of the outgoing gases as a criterion of furnace efficiency, laid the foundation upon which has since been erected the structure of blast-furnace theory. Prominent among those availing themselves of Bell&apos;s data as .a basis of further study was M. L. Gruner,2 professor of the French School of Mines. His "Blast Furnace Phenomena," published in 1870, presented

Jan 1, 1940

By Carl H. Samans, Charles R. Austin

In an earlier serics of studies on 18-8 stainless steel at 600º, 700º, and 800ºC.l one pretreatment was used throughout; viz., 15 min. in hydrogen at 950°C., followed by an air quench. Several manufacturers of this alloy since have expressed doubt as to the suitability of the temperature employed, recommending instead the more customary Strauss treatment as promising superior results. In this subsequent investigation on the effects of the temperature of pretreatment several interesting points have arisen, which are described in this paper. Previous work on our equipment had shown a marked difference between alloys of "similar chemical composition" that had been manufactured by different companies. Accordingly, one mill-bar length was selected from which to prepare all specimens. It could then be assumed that any marked differences in creep characteristics would be due to effects resulting from variations in the pretreatment of the alloy. The material was furnished by the Allegheny-Ludlum Steel Co. in the form of 5/16-in. dia. rod, finished by air cooling from a mill anneal at 1950°F. (1066°C.). It was analyzed only for the elements shown: carbon, 0.07 per cent; chromium, 18.73; nickel, 9.46; manganese, 0.40. Three pretreating temperatures were chosen, the specimens being held for 15 min. in hydrogen at either: (1) 1150°C., to conform to the recommended Strauss treatment; (2) 950°C., to compare with the results of previous tests; or (3) 75Q°C., to initiate precipitation of carbides in the material before testing. As the test cross sections were only 1/8-in. dia., air cooling followed the annealing treatment. These treatments permitted two direct comparisons: (1) between the 1150" and 950°C. treatments to indicate the effect of grain size when all carbides were probably in solution at the start of the test; and (2) between the 950" and 750°C. treatments to indicate the effect of carbide "nucleation" for similar grain sizes.

Jan 1, 1940

By P. V. Martin

Shortly after the middle of the nineteenth century, the invention of the regenerative open-hearth furnace and the development of the Bessemer process stimulated a rate of steel production whose magnitude created an unprecedented demand for pig iron. Revolutionary improvements in furnace design, auxiliary equipment, and operating technique enabled the blast furnace to keep abreast of the constantly increasing requirements of the steel mill. The development of improved blowing equipment, more adequate facilities for material handling, and particularly the general use of anthracitc and coke to replace the physically weaker charcoal, led to a rapid expansion in both the height and volume of furnaces. Beyond a doubt, however, the greatest single factor in blast-furnace improvement at this time was the use of the higher blast temperatures made available by the replacement of the recuperative iron pipe stoves by the regenerative Cowper brick stove. The increased blast temperature not only resulted in greater output but also reduced fuel consumption . far more than could be explained by the additional heat content of the blast. The progress of iron manufacturing was thus largely mechanical and thermal. Little attention was given the chemistry of the process until the publication of the investigations of Sir Lowthian Bell.1 Bell&apos;s painstaking experiments and investigations gave to the blast-furnace man his first real scientific conception of blast-furnace chemistry. Bell&apos;s recognition of the dual function of the carbon, the technical importance of reversible reactions and chemical equilibria, and his conception of the degree of oxidation of the carbon as shown by the analysis of the outgoing gases as a criterion of furnace efficiency, laid the foundation upon which has since been erected the structure of blast-furnace theory. Prominent among those availing themselves of Bell&apos;s data as .a basis of further study was M. L. Gruner,2 professor of the French School of Mines. His "Blast Furnace Phenomena," published in 1870, presented

Jan 1, 1940

By John B. Dilworth

In September, 1930, H. N. Eavenson, then Chairman of the Coal Division, appointed a Committee on Methods of valuing Coal Propelvties, with John B. Dilworth as chairman. The latter prepared a schedule&apos; of features for consideration under the general headings of Undeveloped and Developed Coal Properties. These subjects were divided among the members of the committee and during the next year written discussions of his allotted subjects were received from each member. Mr. Grimes and Mr. Eavenson discussed the entire list,. These discussions were mimeographed and a set sent to each member before the meeting of the Institute in February, 1932. There was a general discussion at that meeting. At the meeting in February, 1934, Mr. Dilworth submitted a report12 which summarized the accumulated opinions and data and presented the conclusions of the committee as a whole on the subjects embraced in it&apos;s schedule. Members of the committee expressed the desire that some of the individual opinions be published for reference. Mr. R. Damon Hall&apos;s abstracts of these papers arc therefore presentrd herewith.3 Personnel of Committee John B. Dilworth (Chairman), Consulting Mining Engineer, Edward V. D&apos;Invilliers Engineering Co., Philadelphia, Pa. Eli T. Conner, Consulting Mining Engineer, Seranton, Pa. W. G. Duncan, Jr., Superintendent, W. G. Duncan CoaI Co., Greenville, Ky. Howard N. EAveNson, Consulting Mining Engineer; Eavenson, Alford & Hicks. Pittshurgh, Pa. George Watkin Evans, Consulting Mining Engineer, Seattle, Wash. J. A. Garcia, Consulting And Constructing Engineer, Allen & Garcia Co., Chicatgo. III. John Alden Grimes, Valuation Engineer, Bureau of Internal Revenue, Washington, D. C. Otto Herres, Assistant Manager, United States Fue1 Co., Salt Lake City, Utah. J. R. Hicks, Consulting Mining Engineer, Eavensorl, Alford & Hicks, Pittsburgh, Pa. Robert D. Reeder, Mining Engineer, U. S. Bureau of Mines, Washington, D. C. Samuel, A. Taylor, Consulting Engineer, Pittsburgh, Pa. Bleeckee L.. WHeeler, Mining Engineer, Ford, Bacon & Davis, New York, N. Y.

Jan 1, 1934