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By R. A. Vandermeer, J. C. Ogle

The preferred crystallographic orientations (texture) developed in randomly oriented, poly crystalline niobium during rolling were studied by means of X-ray diflraction techniques. The evolution of texture at both the surface and center regions of the rolled strip was carefully examined as a function of increasing defamation throughout the range 43 to 99.5 pct reduction in thickness. Certain aspects of the center texture development in niobium are in agreement with the predictions of a theory by Dillamore and Roberts, but others cannot be explained by the theory in its present form. Above 87 pct reduction by rolling, a distinctly different texture appeared in the surface layers which was unlike the center texture. The present results are compared with previous results obtained from other bcc metals and alloys. RANDOMLY oriented, poly crystalline metal aggregates when plastically deformed to a sufficiently large extent develop preferred orientations or textures. In a recent review article, Dillamore and Roberts1 pointed out that the nature of the developed texture may be influenced by a large number of variables. These include both material variables such as crystal structure and composition and treatment variables such as stress system, amount of deformation, deformation temperature, strain rate, prior thermal-mechanical history, and so forth. From a practical point of view, the control of preferred orientation may often be important for the successful fabrication of metals into usable components. During the past few decades many experiments have been devoted to the study of deformation textures. This work, however, has been confined in large part to metals and alloys that have an fcc crystal lattice. By comparison, bcc metals and alloys have received much less attention, and consequently our understanding of preferred orientations in these materials is only shallow. This state of affairs worsens when it is realized that almost all of our present howledge about this class of materials derives from studies on irons and steels.' The bcc refractory metals, which are relative newcomers to the industrial world, have, on the other hand, been given at best only passing glances in the area of texture development. Our understanding of the evolution of preferred orientations in bcc metals can only remain fairly limited until systematic studies of metals and alloys other than the irons and steels have been carried out and the influence of the many variables has been determined. To that end a program was initiated to investigate in detail texture development in niobium. The present paper reports some of the results of this study. Textures were determined at both the center and surface of strips rolled variously to as much as 99.5 pct reduction in thickness at subzero temperatures. Emphasis in this paper is on texture description and on texture evolution during rolling to progressively heavier deformation. EXPERIMENTAL PROCEDURE The niobium was purchased from the Wah Chang Corp. as a 3-in.-diam electron-beam-melted billet. Chemical analysis indicated the impurities to be less than 300 ppm Ta, 40 ppm C, 10 ppm H, 170 ppm 0, and 110 ppm N. All other impurities were below the limits of detection by spectrochemical analysis. This large-grained billet was fabricated into specimen stock so that a fine-grained randomly oriented grain structure resulted. This was accomplished in three deformation steps alternated with recrystalli-zation anneals of 1 hr at 1200°C in a vacuum of low 10"6 Torr range after each deformation step. The first step was to alternately compress the billet 10 to 20 pct in each of three orthogonal directions. The second step was to compress in only two directions 90 deg apart to produce a 2-in.-sq bar. The final step was to roll this bar 50 pct to give a 1-in. by 2-in. cross section. After the final anneal, metallo-graphic examination showed the material to have an average grain size equivalent to ASTM No. 5 at 100 times (i.e., 0.065 in. diam). Specimens cut from the center and edges of this bar gave no indication of detectable preferred orientation when examined by X-ray diffraction. Samples 1.5 in. long, either 0.625 or 0.750 in. wide, and approximately 0.400 in. thick were machined from this fabricated ingot. The surfaces corresponding to the rolling planes were ground so as to be parallel. The samples were chemically polished in a solution of 60 pct nitric acid and 40 pct hydrofluoric acid (48 pct solution) prior to rolling to remove any cold work introduced in the machining operations. Rolling was accomplished with a 2-high hand-operated laboratory rolling mill that had 2.72-in.-diam rolls. Prior to operation, the rolls were polished with 600 grit paper, cleaned with acetone, and then soaked in a container of liquid nitrogen for several hours. The samples were also soaked in liquid nitrogen prior to rolling and were recooled between each pass. While some slight heating of the samples occurred during rolling, this procedure maintained the sample temperature well below 0°C at all times. The samples were rolled unidirectionally, and the rolling plane surfaces were not inverted during any phase of the operation. The draft per pass averaged between 0.010 to 0.012 in. After 96 or 97 pct reduction the draft was reduced to 0.001 to 0.002 in. per pass. Samples were rolled to various reductions in thickness between 43 and 99.5 pct.

Jan 1, 1969

By T. H. Weldon, L. V. Whiton, R. R. McNaughton, J. H. Hargrave

R. H. McNAUGHTON*—The Smelting Co. and Mr. Reid and his men at Selby are to be congratulated on the job they have done on sinter gas recircula-

Jan 1, 1950

By William M. Boorstein, Robert D. Pehlke

The rates of solution (of hydrogen in liquid pure iron and in several liquid binary iron alloys were meas-ured using a constant volume technique. The rates of absorption and desorption were found to be equal un-der all experimental conditions. increasing concen-trations of S, Si, or Te decrease the rate of hydrogen uptake but additions of Al, B, Cr, Cu, or Ni have no measurable effect up to concentrations normally en-countered in steelmaking practice. No relation ship was found between the effect of an alloying element on the equilibrium solubility of hydrogen in liquid iron and its effect on the solution rate constant. Mathe-rnatical analysis of the data indicates that under the present experimental conditions the rate of reaction of hydrogen with liquid iron is controlled by transport of gas solute atoms in the metal phase. Comparison of the present resuts with data on nitrogen taken un der similar conditions establishes that the hydrody-nurnic conditions which exist near the surface of a metal bath are best approximated mathematically by a surface renewal model for the case of rapid in-ductive stirring and by a boundary layer model for more quiescent melts. HYDROGEN has long been recognized as being a detrimental constituent in steel. If dissolved in the molten metal in excess of its solid solubility, hydro-gen can be evolved during solidification and cause bleeding or porosity in ingots and castings. In the solid metal, lesser amounts play a definite role in causing other defects such as hairline cracks, blisters, and embrittlement. For significant refinements to be made in metallurgical procedures designed to control or eliminate hydrogen from liquid iron or steel dur-ing processing, available equilibrium solubility data must be supplemented with reliable fundamental in-formation pertaining to the kinetic factors involved in the transfer of hydrogen to or from the metal. The scarcity of such information in the literature prompted the present investigation. PREVIOUS RESEARCH Whereas much of the existing data on the solution kinetics of gases such as nitrogen were obtained during the course of thermodynamic investigations, the solu-tion rate of hydrogen has been found too rapid to be accurately determined by conventional solubility meas-urement techniques. Consequently, little work on hy-drogen solution kinetics has been reported in the lit-erature. Carney, Chipman, and crant1 attempted to study the rate of solution and evolution of hydrogen from liquid iron by employing a newly devised sampling method. Although no significant quantitative data could be obtained, it was observed that the rate of solution was approximately equal to the rate of evolution of hy-drogen from the melt. Karnaukov and Morozov2 stud-ied the rate of absorption and Knuppel and Oeters3 the rate of desorption of hydrogen from molten iron by measuring pressure changes with time in a constant volume system. Karnaukov and Morozov determined the hydrogen pressures over their inductively stirred melts with the aid of a McLeod gage and therefore, were forced to work at pressures not in excess of 40 mm of Hg. Their experimental data conformed to a mathematical correlation based on diffusion control: and the rate coefficients calculated on this basis were shown to be independent of the initial absorption pres-sure. These authors reported the solution rate of hy-drogen to be eight-to-ten times higher than they had found for nitrogen in a previous study. They also re-ported that under identical conditions, hydrogen dis-solves somewhat more slowly in iron-columbium alloys than in pure iron. Knuppel and Oeters found that the desorption of hydrogen from pure iron at 1600°C was controlled in all cases investigated by diffusion in the metal bath as long as bubble formation was sup-pressed. This was substantiated by Levin, Kurochkin, and umrikhin4 who studied the kinetics of hydrogen evolution from liquid (technical) iron while applying a vacuum. Salter5 measured the rate of hydrogen ab-sorbed by iron buttons, arc-melted by direct current, as a function of hydrogen partial pressure in a hy-drogen-argon atmosphere. A carrier gas technique was used for analysis of the hydrogen absorbed. The initial rate of absorption was found to increase di-rectly with the square root of the partial pressure of hydrogen. EXPERIMENTAL METHOD Because of the rapid uptake and evolution of hydro-gen by iron-base melts, a constant volume technique was devised in order to obtain meaningful kinetic data over the entire course of the solution process. Apparatus. A schematic view of the experimental apparatus is given in Fig. 1. The hydrogen-liquid iron reaction system consisted of a gas storage bulb con-nected to a meltcontaining reaction chamber through a normally-closed solenoid valve. The gas storage bulb, an inverted 250 ml round-bottomed Pyrex flask was joined to the inlet port of the solenoid valve by a glass-to-metal seal. A more detailed illustration of the reaction chamber is shown in Fig. 2. The design of the Vycor reaction bulb was essentially that de-scribed by Weinstein and Elliott6 with the exception of a shorter, larger diameter gas inlet for this kinetic study. In position, the reaction bulb was closely by an eight-turn coil of water-cooled copper tubing which, when energized by a 400-kc oscillator, provided the inductive heating source. The walls of the bulb were maintained relatively cool by circulating cold water along their outer surface, thus preventing

Jan 1, 1970

By Harlowe Hardinge

THE sound made by ball, pebble and rod mills has long been used by the operator as the "telltale " of their operation. The nature of this sound depends upon local conditions and the type of mill used. By experience an operator can tell whether the mill is running properly or not. Some operators are able to detect the difference in sound much better than others and get better results running the same mill under the same conditions. The automatic operation of a mill using sound as the fundamental means for maintaining control presents many problems. The satisfactory solution of these problems requires, for given operating conditions, a greater average output, with improved product for subsequent processing, than can be obtained by manual control. RELATION OF SOUND TO USEFUL GRINDING ENERGY Experience has taught us that there is a difference in character as well as in intensity of sound between a mill grinding wet and one grinding dry, in open or closed circuit, to obtain a coarse or fine product, on the same material, to say nothing of the effect with a variety of different materials. Broadly speaking, a wet-grinding mill operates best at a lower sound level than the same mill grinding dry, with other conditions the same. Several reasons for this variation in sound intensity under these conditions can be advanced, but the important point is that there is a difference, based upon practical results. Since these reasons may be more or less involved, and may be subject to much discussion, only one will be considered here. It is apparent that two balls hitting together or a ball striking the lining, if there is no intervening material, will produce the maximum sound. If a complete cushion of material is placed between the balls or ball and liner, so that the energy is dissipated without doing useful work, the balls will be unable to create enough pressure or force to fracture the particles, and the sound will be at a minimum. At some point in between-that is, where there is sufficient material between the balls or ball and liner so that the ball will fracture the particles without mashing them unduly-the sound

Jan 1, 1939

By Erwin S. Sperry

The oxidation of metals melted in contact with air takes place with dissimilar results. Tin, lead or zinc are examples of a class, the oxides of which float on the surface of the melted metal. First a film is produced, which covers the surface; then, if agitation from any cause exposes new metal to the action of the air, additional oxidation takes place, and the film is increased in volume. This change goes on until a considerable quantity of oxide (or " dross," as it is technically called) is formed; depending, of course, upon the duration of the exposure of the metal to the atmosphere. When such metals are poured, the dross may be skimmed off; and clean metal will be left underneath. The removal of such oxides is, therefore, merely a mechanical process. In the case of copper, however, the result is quite different. The sub-oxide of copper (Cu2O) is readily soluble in molten copper; and therefore, instead of the formation of a film of oxide, to be finally removed as dross, the surface of the metal remains bright and clear, because the oxide has been dissolved as soon as it was produced. It is customary in the process of copper-refining to leave a small quantity of oxide in the metal, in order to oxidize any traces of bismuth, arsenic or antimony which have not been entirely removed. As a result, these metals exist in the commercial product as oxides, and not as metals, which would form an

Jan 1, 1901

By R. J. Watson

In an earlier paper, Ehrenburg and Watson1 published the develop ment for a potential function by which it is possible to obtain the electric potential at points on the surface of the ground when a current I passes between two electrodes and the subsoil is composed of parallel, homogeneous layers. In view of the continued interest in the resistivity method of electrical prospecting, the author has considered it desirable to publish the results of a number of theoretical studies making use of this potential function, and also the results of a considerable number of tests with models designed to show the soundness of the mathematical theory. It is hoped that these results will prove how erroneous the various empirical rules for depth determination may be. It has always seemed puzzling to the author that one can find, in papers published comparatively recently, statements upholding empirical rules for depth determination, and attributing most of the irregularities of resistivity curves to vertical discontinuities in resistivity in the subsoil. It would indeed be fortunate for the geophysical investigator if such a simple rule held. However, numerous investigators have proved both theoretically and by the success of their field work that such a rule does not hold, even by a "rough approximation" in many cases. On the other hand, as is shown in the development to follow, if the underground conditions are favorable it is possible for such empirical rules to give a satisfactory depth determination. Authors should be more careful about making such sweeping statements about the accuracy of these empirical rules because the relative simplicity of the field work places the method in the hands of any interested experimenter, and he is likely to become completely disgusted with the method after he has made several obviously wrong interpretations by empirical rules. There are simple and rapid methods for finding out whether the ground beneath the electrodes is sufficiently similar to the conditions

Jan 1, 1934

By H. D. Hoskold

DuRing the last few years, various persons have been put forward as originators of some mechanical device for the purpose of finding distances without the use of a chain or other linear measuring-instrument, and among these, the Englishman, Gascoigne, 1639, is prominent as the first in England; while James Watt, 1771, and William Green, 1778, are also included in the list of inventors. It is possible that this useful and important problem occupied the attention of others prior to the date cited, and, consequently, it is difficult to decide what nation first gave birth to the inventor of an instrument for the object under consideration. A very important work appeared, not long since, in Paris, devoted to a history and discussion of some of the older and newest forms of surveying-instruments,* and at page 79 of that work a curious old instrument is exhibited, called Bigonometre, i. e., an instrument for finding distances and solving trigonometrical problems. in surveying. A copy of the diagram of the instrument exhibited in the book referred to is represented in Fig. 1. Having had an occasion to read the French work referred to, I communicated with the author of it, and he was good enough to reply that he found a diagram of this old instrument in a book published in 1597, by Danfrie, existing in the library of the Academy of Sciences, in Paris. Col. Laus-

Jan 1, 1904

By Edward Wisser

The Pachuca silver district, situated about 100 kilometers northeast of Mexico City (Fig. l), covers roughly the southeastern half of the Sierra de Pachuca. The latter is a mountain range with northwest trend, and forms a part of the northeastern rim of the topographic basin known as the Valley of Mexico. The length of the Sierra proper is about 50 km., its greatest width about 9 km., and it rises to a maximum of 600 meters above the general level of the basin floor. The Pachuca district consists of two contiguous subdistricts, the Pachuca area and the Real del Monte area. The center of the Real del

Jan 1, 1937

By T. R. Ingraham

The thermal decomposition of Nickel (II) sulfate was examined by determining the total pressure of SO3, SO2, and O2 developed over a sample when it was heated in an evacuated system fitted with a Pyrex-bellows mercury manometer. The equilibrium pressures were combined with previously published data on the oxide and sulfide systems to establish a predominance volume diagranz for the Ni-S-O system over the normal range of roasting temperature and gas composition used in the treatment of nickel minerals. The protective coating of NiSO4 which forms on the oxide during roasting, and which causes the sulfation reaction to almost cease, may be disengaged readily by temperature cycling. When nickel sulfide is roasted in air, either nickel sulfate or nickel oxide may be formed by altering the experimental conditions. Because of the differing stabilities of various metal sulfates and oxides, possibilities exist for separating some of the constituents of mineral mixtures by the technique of selective sulfation and oxidation roasting. The experimental information required to make reasonable predictions of the possibilities of this technique is incomplete and, in some cases, in conflict. As part of a general program of providing some of the required information, a study EXPERIMENTAL Materials, Apparatus, and Procedure. Fisher certified reagent-grade nickel sulfate hexahydrate was used in the source material for both nickel sulfate and nickel oxide. The manufacturer's analysis indicated: 0.001 pct Fe, 0.005 pct Cu, 0.003 pct Co, 0.001 pct C1, other 0.15 pct. The material was dehydrated, before use, by heating at 420°C for 5 hr. The oxide was prepared by roasting the sulfate in an open tray in a muffle furnace for 10 hr at950°C. Preliminary experiments which were made by thermogravimetric analysis and X-ray diffraction analysis established that only one crystal form of nickel oxide and one of nickel sulfate were involved in the equilibrium shown in Eq. [I]. The apparatus used in the experiments was described previously.1,3 The main feature is a corrosion-resistant, flexible Pyrex bellows which is used to protect the mercury in a u-tube manometer. Before a run was begun, the apparatus was washed thoroughly with hot hydrochloric acid and water and dried by heating under vacuum. The mixed sulfate -oxide sample was contained in a platinum bat rest-

Jan 1, 1967

By J. O. Betterton, W. M. Spicer

The solubilities of antimony in the a and ß-forms of zirconium were determined between 750" and 1300°C. The a-phase forms by a peritectoid reaction, and the a/(a + ß) and ß/(a + ß) phase boundaries rise in temperature with in- ' creasing antimony. Impurities in the 99.95 pct zirconium were sufficient to influence the phase boundaries and the variation reported is approximate. The restricted solid solubility of the terminal zirconium phases, which is especially characteristic of this system, is thought to result from the low free energy of the Zr2Sb phase. ZIRCONIUM-antimony alloys are important in zirconium alloying studies since antimony is one of the highest valent elements which can be used to make zirconium alloys. The dilute alloys are of further interest as they have somewhat better corrosion resistance' than pure zirconium. The first investigation of the phase diagram was made by Russi and wilhelm2 who found a eutectic reaction, liquid (- 17.5 at. pct Sb) = ß zirconium (- 11 at. pct Sb) + Zr2Sb, at 1430°C'. The Zr2Sb phase was of complicated hexagonal structure, and by thermal analyses of the relatively impure alloys then available, Russi and Wilhelm found evidence for the peritectoid formation of the a-phase. EXPERIMENTAL In the present work, the phase diagram was re-investigated in the region 0 to 5 at. pct Sb and 750" to 1300°C using iodide-zirconium alloys. Details of the procedure have been described earlier. Essentially the alloys were prepared by arc casting and were then examined by the annealing and quenching method. The times of annealing varied from 1 hr at 1300°C to 30 days at 760°C. As in other zirconium phase-diagram studies1"5 the impurities in the zirconium were still sufficient to affect the results, and the experiments will therefore be described in 3 parts. The results from the first 2 parts of the work are shown in Fig. 1. Here the ß/(ß + Zr2Sb) and a/(a + ZrzSb) phase boundaries were determined with alloys made from 99.9 pct zirconium,* and cast under such conditions that the Vickers hardness of a alloys extrapolated to 95 to 110 VPN at 0 at. pct Sb. Such alloys were not suitable for investigations of the (a + ß) region, and the results shown in Fig. 1 near the (a+ ß) and (a +ß + Zr2Sb) regions were determined with purer alloys. These alloys had an extrapolated hardness range of 75 to 85 VPN and were made from 99.95 pct zirconium. A deviation from binary equilibrium occurs in Fig. 1 as indicated by the (a + ß) region of pure

Jan 1, 1959

By David B. Reger

The exhaustion of oil and gas in the United States is proceeding at a rapid pace. This is especially true in fields where the light oils that furnish the most fuel for internal-combustion engines arc found, leading to a late estimate by Arnold that the petroleum resources are 36 per cent. exhausted.l The further remark by Dr. David T. Day at the New York meeting of the Institute, in February, 1916, that the operators of the country are now scarcely able to supply the ever-increasing demand for gasoline, leads the writer to believe that a determined effort will soon be made to secure deeper producing horizons in those regions that now furnish high-grade oil, and in which pump stations and pipe lines offer convenient means for the economical handling of new production. A study of Arnold's table shows further that the States that produce paraffin oil exclusively are 45 per cent. exhausted, this figure being much higher than the average of paraffin and asphalt States altogether. The most extensive of all the paraffin-oil-producing areas is the Appalachian Field, extending with the Appalachian Geo-Syncline from western New York southwestward through western Pennsylvania, western West Virginia, Ohio, Kentucky, and Tennessee, where oil of high gravity is always secured. Of these States, Pennsylvania and West Virginia rank highest in the quality of their product. In West Virginia, the oil sands dip to a lower level than in any other locality in the Appalachian Geo-Syneline, the Pittsburgh Coal of the Pennsylvanian being only 50 ft. above sea level along the Nineveh Syneline at Wileyville, Wetzel County.² The very significant fact that the sands of the Mississippian and Upper Devonian Measures furnished the richest oil pools of the State along this

Jan 1, 1917

By G. L. Tufford, R. L. Bleifuss

Low-grade manganiferous iron ores of Minnesota's Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite with subsequent magnetic separation and flotation have not given satisfactory results because, in many instances, concentrate grade and manganese recovery are low. Metallization of iron and concurrent reduction of higher manganese oxides to MnO, as in the R-N process, followed by recovery of iron by magnetic separation and manganese by leaching, seems to be a technically feasible process. High-temperature x-ray diffraction studies show that solid-state reactions between iron and manganese, with the formation of intermediate iron-manganese oxides, occur during reduction and affect recovery of both iron and manganese from the final product. Solid state reactions also occur between FeO, MnO, and SiO, at temperatures as low as 900°C. The kinetics of these reactions are such that they become an important factor in the treatment of ores by the R-N process. These investigations suggest a temperature and gas composition cycle that would maximize both iron and manganese recovery. During the past ten years, iron ore shipments from the Cuyuna Range of Minnesota have decreased sharp1y. Because of adverse grade, structure, and cost, many Cuyuna ores are no longer competitive with high-grade foreign ores and domestic pellets. The low-grade manganiferous iron ores from the Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite for subsequent magnetic separation and flotation has not given satisfactory results because concentrate grade and manganese recovery are often low. However, a technically feasible process appears to be metallization of the iron and concurrent reduction of manganese oxides to MnO with recovery of metallic iron by magnetic separation and extraction of manganese from the tailings by leaching. In 1962 the R-N Corp., with a grant from the Area Redevelopment Administration, conducted an amenability study of the metallization of manganiferous iron ore from the Cuyuna Range. The results of this preliminary investigation were sufficient to interest the Economic Development Administration in sponsoring further studies of the process with emphasis on secondary recovery of manganese from the nonmagnetic tailings. Inasmuch as the metallization process has considerable influence on the final form of the manganese - its texture and distribution between the magnetic concentrate and nonmagnetic tailings-the investigation included a study of metallization of the ore as well. Therefore, the investigation conducted at the Mines Experiment Station covered three interrelated phases: (1) laboratory R-N roasting studies and magnetic separation tests, (2) laboratory chemical extraction experiments of the nonmagnetic tailings, and (3) a mineralogical study of the crude ores and their various roast products. High-temperature x-ray diffraction investigation of the Fe-Mn-Si0,-0, system is the main topic of this paper and an extension of the mineralogical work. GENERAL GEOLOGY The Cuyuna Range is known for its complicated geologic structure, complex orebodies, and generally indifferent response to attempts at conventional beneficiation. Several geologists have made intensive studies of the Cuyuna Range, including Leithl (1907), ~darns' (1910), Zapffe3 (1925), Grout and Wolff4 (1955), and schmidt5 (1963), whose study was the most comprehensive of all. The Range is covered with glacial deposits - till, out-wash, and lake sediments -up to 250 ft thick. Bedrock stratigraphic units of the Cuyuna Range consist of three tightly folded Precambrian sedimentary formations. The lower unit is the Mahnomen formation, composed of 2000 or more feet of argillite, slate, siltstone, and quartzite. The middle unit is the Trommald formation, which varies from 45 to 500 ft in thickness and comprises the major iron-bearing formation. The upper unit is the Rabbit Lake formation, consisting of over 2000 it of argillite, slate, and interbedded lenses of lean iron formation. In the central part of the Cuyuna Range, the units have been folded into a series of

Jan 1, 1969

By Edgar Dunn

PART I.-DETERMINATION OF GASES IN SMELTER FLUES. IN 1907, upon arriving in Anaconda to take up work in the testing department of the Washoe Reduction Works, the. following problem was met at the car step, so to speak: complete and. exact analysis of gases, not only at the stack, but also in all departmental flues. Taken up to employ time not otherwise needed for regular testing department work, instructions were extremely liberal for a commercial plant, to the effect that accuracy should not be sacrificed to speed. In December, 1907, the work was temporarily transferred to the Great Falls Smelter, and some of the methods here given were there worked out. Differences in smelting operations at Great Falls and Anaconda, however, necessitated further investigations and the development of a new method for S03 determinations at the latter plant, where work was resumed in July, 1908, and completed about a year later. At the time of inception of the work, data (not only on percentages, but even on methods) were found to be meager in the extreme, for one or the other of two reasons: either entire lack of experiment at a large proportion of smelters, or disinclination on the part of the managements to divulge data of any description pertaining to either results or methods. In making determinations of gaseous constituents of flues, two methods are open to consideration: 1, the drawing out of a sample, and collection of the same as a whole, to be removed to the laboratory for later analysis; and 2, the absorption in situ on the flue of one certain constituent, disregarding others for the time being, or perhaps combining two or three in one determination. The first is generally the more rapid, but it is also the more inaccurate, method of analysis, even with special type absorption apparatus, being the more largely subject to error, both of reading, and also because of leakage during complicated manipulation in the laboratory. The amount used for analysis must also, because of limit of container, be small for the first method, and an average gas is very seldom obtained, necessitating for a fair average result a large number of determinations. Consequently, when we balance the time spent in a dozen determinations of short-time samples as against the time employed in making two or three long-time determinations of various constituents in situ, we are not so certain in our statement as to the relative speed of the two methods. Moreover, the method of analysis in the laboratory of 100 cc. of flue gas is satisfactory only when constituents thus determined are present in considerable quantity, results being simply approximate when determining such compounds as sulphur dioxide, sulphur trioxide, carbon monoxide and dioxide, and arsenic trioxide and water vapor, none of which are carried in all smelter flues in amounts in excess of (or even approaching) 1 per cent by volume. Special condi-

Jan 8, 1913

By Bradley Stoughton, Henry M. Howe

This paper presents an experimental verification of some of the predictions made by one of us1 concerning the influence of certain conditions of casting upon the size and position of the pipe, and the position of the segregate, in steel ingots. The predictions which we have been able to verify are the following: A. That the pipe is shortened and the segregate raised: 1. By slow casting; 2. By casting with the large end up instead of down; 3. By retarding the cooling of the top, e.g., by means of a sinking-head. B. That the pipe is shortened by slow cooling. C. That the pipe and segregate lie in the last-freezing part. Our procedure was to cast ingots of wax (commercially pure stearic acid) containing a little bright green copper oleate (usually 1.5 per cent.) under varying conditions; to saw each ingot open along a longitudinal plane passing through its axis; and to examine the longitudinal section thus laid bare. In order to make the segregate or enriched part more distinct in color from the impoverished part, a very little red cerasine was added. An experiment which will be described later showed that the cerasine itself does not segregate markedly, if at all. Hence we may assume that the strong contrasts between the green and red shown in so many of our ingots are due, not to segregation of cerasine, but to that of the green oleate, in the wax which in itself is uniformly reddened with cerasine.

Jan 1, 1908

By G. L. Fisher, R. H. Geils

The effect of small amounts of columbium (<0.01 to 0.10 pct) on the ?-a transformation occurring during the continuous cooling of a low carbon Ni-Cu steel was investigated. Dilatometer specimens were aus-tenitized at 950" and 1068?C and cooled at 17? and 375 C° per min. Columbium caused a marked depression in the ?-a transformation temperature except when cooling at the slower rate from 950°C. The effec of columbium on the transformation temperature was greater the higher the austenitizing temperature and rate of cooling. A maximum depression of 92 C" was observed. Metallographic examination of specimens of <0.01 and 0.07pct Cb steels heated at 1200°C for 1 hr and cooled at various rates showed that columbium had a major effect on the ferrite morphology. The fer rite in the columbium -free steel remained equiaxed at cooling rates as high as 440 C? per min while the columbium-bearing steel exhibited mixed structures o equiaxed and bainitic ferrite at cooling rates as low as 130 C° per min. The ? grain boundaries in the columbium -free steel provided the ferrite nucleation sites in rapidly cooled specimens. There was a complete absence of nucleation at these sites in the colum bium-bearing steel. It is concluded that columbium depresses the transformation temperature by suppressing ferrite nucleation at the austenite grain bound-aries. In this respect the effects of columbium are analogous to those of boron in low C-Mo steels. It is well known that small columbium additions can substantially strengthen plain carbon steels. As little as 0.02 pct Cb can increase the yield strength of mild steels by 10,000 psi.1 A fine precipitate of CbC has been observed in columbium-bearing steels2 and is generally thought to be responsible for the strengthening. Little attention has been devoted to the effect of columbium on the ?-a transformation. Webster and woodhead3 have studied the effect of columbium on the isothermal proeutectoid ferrite reaction in mild steels. They found similar transformation behavior in steels both with and without columbium additions. However, as the austenitizing temperature increased, the incubation time for the start of the ferrite transformation became longer in the columbium-containing steel. Morrison1 found that the addition of 0.03 pct Cb to a C-Mn steel lowered the transformation temperature by 50 C° during cooling from 1200°C at a rate of 80 C" per min. The strengthening effect of columbium has recently been utilized in an age-hardenable, low-alloy steel containing copper and nickel.4 A small amount of columbium has a substantial effect on the as-rolled strength of this steel. By increasing the columbium level from <0.01 to 0.13 pct the as-rolled yield strength is increased by 15,000 psi. Columbium also significantly lowers the ?-to-a transformation temperature of this steel during continuous cooling from the austenitizing temperature. Because of the low carbon level in this steel (0.05 pct max), it is almost entirely ferritic. Thus, it offers the opportunity of studying the effect of small columbium additions on the proeutectoid ferrite reaction. Of particular interest in this study was the reason for the marked lowering of the transformation temperature by columbium during continuous cooling. EXPERIMENTAL PROCEDURE Materials. The compositions of the steels used in this investigation are shown in Table I. The steels were 30-lb air induction melts. They were forged to 4 by 8 by 1 in. plate at 1230°C, air cooled, and then reheated to 1230°C and cross-rolled in two passes to in. plates. Dilatometry. A Leitz Bollenrath dilatometer was used to record the transformation during continuous cooling from two different austenitizing temperatures. The dilatometer specimens were + in. in diam and 2 in. long. Oxidation and decarburization of the specimens was prevented by maintaining a small positive pressure of dry argon in the dilatometer furnace and by plating the specimens with 1 mil of Cu. For the lowest cooling rate, 17 C" per min, the temperature of the specimen was measured with a Pt-Pt 10 pct Rh thermocouple placed in a & in. diam well in the center of the specimen. During air cooling, 375 C° per min, this method of measuring the temperature interfered with the operation of the dilatometer. However, it was found that the temperature of the specimen could be measured accurately by placing a thermocouple in an identical specimen in a holder adjacent to the one being used to operate the dilatometer mechanism. The dilation-temperature curves were recorded on photographic film and then converted to volume percent ferrite-vs-temper-ature curves. The cooling rates obtained with the dilatometer are shown in Table 11. Cooling rates of

Jan 1, 1970

By M. H. Merriss

In the last few years, there have been developed at the plant of the Nichols Copper Co., Laurel Hill, &apos;Borough of Queens, New York City, improvements in electrolytic copper refining by the series system that have materially increased the flexibility and economy of that system. The purpose of this paper is to discuss, as of interest to refiners and to those who have copper to refine, as well as to the engineering profession in general, the changes&apos; that have taken place resulting in wider application and increased efficiency of the series system. Copper is electrolytically refined in two ways, which are spoken of as the "multiple system" and the "series system." In both systems, the electrolytic tanks are in series electrically. In the multiple system the electrodes in a single tank are in multiple or in parallel, thus: There are two important adaptations of the series process, one represented by the series electrolytic tank room at the Baltimore Copper, Smelting & Rolling Co., Baltimore, Md., and the other by that of the Nichols Copper Co.&apos;s plant. At Baltimore, the anode is rolled to perfect

Jan 1, 1926

By Joseph C. Platt

It is not the object of the present paper to give a description of the minerals found on Mine Hill, in Sussex County, N. J., nor even to touch upon all the forms of the ores named, but to place upon record and call to the attention of the Institute some interesting facts concerning them. In May, 1875, after the Dover meeting, some of the members visited this locality, and, no doubt, it is fresh in their memories, being one of the best known mineralogical points in our country. It will be only necessary to describe it very briefly. Mine Hill and Stirling Hill, in Sussex County, N. J.,—the former being at the village of Franklin Furnace, and the latter near Ogdensburg,—are the only localities in the State where zinc ores are found in workable quantities.* Mine Hill is the more northerly, and mineralogically differs from its neighbor, chiefly in having no hydrated ores to speak of, while at Stirling this deposit is considerable. At both points Franklinite, red oxide, and silicate of zinc occur in large quantities. Mine Hill lies on the east side of the Wallkill River, above which it rises to an extreme elevation of about 150 feet. On the summit the outcrop of the Franklinite vein appears, while the lowest worked points are perhaps 10 or 15 feet above the level of the stream. Cornmencing at the northern end, where the Hamburg Road crosses it, this outcrop runs along the northwestern brow of the hill a distance of about 2000 feet, in a general southwest direction, to a point where is a large, cavern-like opening, called the "Southwest Opening." " Double Rock," about the highest point on the hill, lies near the middle of this 2000 feet of outcrop, and over or near it passes a property line, to which allusion will hereafter be made. At the Southwest Opening the vein bends abruptly towards the east,—the angle between the two parts being perhaps 45°,—and this easterly branch continues some 700 feet. From the northern part of the Stirling Hill deposit to the southern part of the Mine Hill deposit is about two miles, and in this interval the vein carrying Franklinite

By L. J. Dijkstra

During the past several years an extensive study has been made of the internal friction of iron containing carbon or nitrogen in solid solution.1,2,3,4,5 It has been found that a sharp peak is observed in a plot of the internal friction vs. temperature of measurement. With a frequency of about one cycle per second, this peak occurs at 20°C for N and 36°C for C. The physical origin of this anomalous internal friction was traced by Snoekl to the local tetragonal symmetry of the interstitial positions in body centered cubic (bcc) iron. A change in stress induces a change in the equilibrium distribution of the interstitial atoms among the three types of interstitial positions, the three types corresponding to the three directions along which the tetragonal axis may lie. It is the continual striving of the interstitial atoms to maintain an equilibrium distribution that gives rise to a phase lag between strain and stress during oscillation, and hence, to internal friction. A similar type of internal friction has been observed in the bcc lattice of tantalum containing in interstitial solid solution C, N or 06. The theory of this anomalous internal friction leads to the prediction that its magnitude is strictly proportional to the concentration of either the carbon or the nitrogen in solid solution, provided the concentrations are small. This prediction has been verified3 for the range of solubilities ohtainable in alpha iron. This proportionality provides us with a new tool for the study of nitrogen and carbon in alpha iron. It thus enables one directly to follow the precipitation of either of these solute atoms from solid solution and also directly to measure their solubility as a function of temperature. A preliminary study of precipitation using this method has already been presented by the author.3 The purpose of this paper is to present more extensive observations upon the precipitation of N and C in alpha iron, as well as to present observations upon the solubility of N and C in alpha iron which, at least in the lower tempera- ture range, are believed more accurate than those previously obtained by other methods. The interpretation of the observations upon precipitation involves the use of the appropriate equilibrium diagrams. For ease of future reference in this paper the equilibriunl diagrams for the Fe-N and Fe-C systems are accordingly reproduced as Fig 1 and 2, respective]y. Experimental Procedure The specimens were made of West-inghouse Puron iron and consisted of wires 0.025 in. in diam and about 1 ft long. By a wet hydrogen treatment the specimens were purified of C and N. In

Jan 1, 1950

By J. R. Thoenen, M. C. Malamphy, G. K. Dale

The beginning of the war and the events leading up to it precipitated a near crisis in the aluminum industry. Demands for the metal reached proportions far beyond the prewar production capacities and, in addition, the submarine menace seriously curtailed the importation of bauxite from South America, hitherto a chief source of high-grade ore. The situation required an intensive search for domestic ore to augment the reserves and in October 1941 Congress directed the Department of the Interior to investigate the extent, mode of occurrence, and quality of bauxite in the United States. In December of that year the Bureau of Mines and the Geological Survey began the search for bauxite in Arkansas, where more than go per cent of the domestic ore had been produced and where the greatest amount of bauxite was known to occur. The program involves the geophysical and geological investigation of the Arkansas bauxite region and the core drilling of areas considered favorable for the occurrence of bauxite deposits. Cores taken from the bauxite-kaolin zone are sampled and analyzed in the Bureau of Mines laboratory in Little Rock. The information from each of the deposits discovered is then assembled, the bauxite is graded with respect to its possible utility, tonnage estimates are made, and the whole is presented in the form of a war minerals report. Thirty-eight new bauxite deposits had been discovered and investigated at the end of the calendar year 1944, and the presence of several others had been indicated by the drilling. More than 5000 holes had been drilled throughout the bauxite region, and more than 60,000 chemical analyses had been made of samples taken from the bauxite-kaolin zone. A study of the chemical analyses led to certain general conclusions not only with regard to the chemical composition of Arkansas bauxite, but also with regard to its component minerals. Charts and diagrams based on these conclusions have been developed for practical use by the Bureau of Mines: (I) to serve as a check against laboratory analyses, (2) to present tonnage estimates of ore bodies based on mineral composition, (3) to illustrate the relationship of tonnages of bauxite to the alumina, silica, and iron content, and (4) to serve as a control for mining operations by providing a means for quick estimates of the value of the ore from a partial analysis of its chemical constituents. The use of charts and diagrams similar to those discussed in this paper-- is not new. The use of the trilinear diagram for studying the ultimate analyses of coals as of proposed by Ralston in Bureau of Mines Technical Paper 93 (1915) showed that the various ranks of coal fell in different areas on the diagram and that volatile matter, calorific value and other properties could also be plotted by the use of contours. A considerable subsequent literature, largely on classification of coals, has accurnulated since then, showing the utility

Jan 1, 1948

By J. R. Thoenen, M. C. Malamphy, G. K. Dale

The beginning of the war and the events leading up to it precipitated a near crisis in the aluminum industry. Demands for the metal reached proportions far beyond the prewar production capacities and, in addition, the submarine menace seriously curtailed the importation of bauxite from South America, hitherto a chief source of high-grade ore. The situation required an intensive search for domestic ore to augment the reserves and in October 1941 Congress directed the Department of the Interior to investigate the extent, mode of occurrence, and quality of bauxite in the United States. In December of that year the Bureau of Mines and the Geological Survey began the search for bauxite in Arkansas, where more than go per cent of the domestic ore had been produced and where the greatest amount of bauxite was known to occur. The program involves the geophysical and geological investigation of the Arkansas bauxite region and the core drilling of areas considered favorable for the occurrence of bauxite deposits. Cores taken from the bauxite-kaolin zone are sampled and analyzed in the Bureau of Mines laboratory in Little Rock. The information from each of the deposits discovered is then assembled, the bauxite is graded with respect to its possible utility, tonnage estimates are made, and the whole is presented in the form of a war minerals report. Thirty-eight new bauxite deposits had been discovered and investigated at the end of the calendar year 1944, and the presence of several others had been indicated by the drilling. More than 5000 holes had been drilled throughout the bauxite region, and more than 60,000 chemical analyses had been made of samples taken from the bauxite-kaolin zone. A study of the chemical analyses led to certain general conclusions not only with regard to the chemical composition of Arkansas bauxite, but also with regard to its component minerals. Charts and diagrams based on these conclusions have been developed for practical use by the Bureau of Mines: (I) to serve as a check against laboratory analyses, (2) to present tonnage estimates of ore bodies based on mineral composition, (3) to illustrate the relationship of tonnages of bauxite to the alumina, silica, and iron content, and (4) to serve as a control for mining operations by providing a means for quick estimates of the value of the ore from a partial analysis of its chemical constituents. The use of charts and diagrams similar to those discussed in this paper-- is not new. The use of the trilinear diagram for studying the ultimate analyses of coals as of proposed by Ralston in Bureau of Mines Technical Paper 93 (1915) showed that the various ranks of coal fell in different areas on the diagram and that volatile matter, calorific value and other properties could also be plotted by the use of contours. A considerable subsequent literature, largely on classification of coals, has accurnulated since then, showing the utility

Jan 1, 1948