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By Frederic Dewey

HAVING shown1 the difficulty of assaying so-called cyanide bullion and the extreme variations often found in the results, an investigation was undertaken to discover if possible the causes of these variations by a series of tests upon the specific action of various metals during cupellation. Zinc.-In order to test the effect of zinc, 48 assays were made in sets of 6, 2 rows of 3. The charge for the middle cupels consisted of 500+ mg. Au, 1,125 mg. Ag, 10 mg. Cu. To the end cupels 50, 75, 100 and 125 mg. Zn were added, and a set of each proportion was cupelled with 4 and 8 grants Pb. The cupels were assayed and showed the following gold contents in milligrams, the figures being arranged as the cupels stood in the muffle: TABLE 1 50 Mg. Zn 75 Dig. Zn 100 Mg. Zn 125 Mg. Zn 4 grams, Pb 0.2S 0.25 0.2S 0:29 0.27 0.34 0.33 0.28 0.41 0.31 0:30 0.36 0.30 0.33 0.34 0.31 0.31 0.29 0.35 0.37 0.42 0.41' 0.34 0.38 8 grams, Pb 0.40 0.43 0.42 0.38 0.36 0.43 0.35 0.34 0.41 0.33 0.37 0.37 0.54 0.17 0.59 0.44 0.43 0.43 0.38 0.39 0.41 0.57 0.38 0.46 _ In many instances the zinc does not appear to affect the cupel gold, but various exceptions are apparent, generally in the cupels in the back row. With 100 and 125 mg. Zn, in some cases the Zn burned with its characteristic flame before it could alloy with the other metals. Also, less fusible oxidized lumps were observed during the cupellation and some cupels showed a scum. In order to lessen the premature burning out of the Zn, an alloy of 2 parts Ag to 1 part. Zn was used. A uniform charge of 500,+ mg. Au,

Jan 7, 1917

NEW MEMBERS The following list comprises the names of those persons who became members during the period Mar. 10 to Apr. 10, 1914. Members ADAMS, DANIEL T., Mining 1416 Westminster Bldg., Chicago, Ill. BLICKENSDERFER, FRANK CLEVELAND, Sampler Morenci, Ariz. CAVERS, THOMAS WILLARD, Met Copperhill, Tenn. CLAPP, CHARLES H., Geol Univ. of Arizona, Tucson, Ariz. CLARK, PATRICK T., Pres Bullwhacker Mine, Spokane, Wash. COMSTOCK, HARRY, Mining Mineville, Essex Co., New York. COOKE, JOSEPH H., Gen. Mgr Mono Dev. Co., Gisborn, Tooele Co., Utah. COOPER, DEXTER P., Civ. and Hyd. Engr 101 Park Ave., New York, N. Y. DEGOLYER, E. L., Geol Apartado 269, Tampico, Mexico. DESHAYES, ERNEST F., Mine Foreman Baldy, N. M. DOUGLASS, WILLIAM CRAWFORD, Min. Engr 107 Leonard Hotel, Butte, Mont.

Jan 5, 1914

NEW MEMBERS The following list comprises the names of those persons who became members during the period May 10 to June 10, 1914. Members ABE, ASAKA, Chief Min. Engr., Yamagano Gold Mine, Satsuma-Gori, Satsuma, Japan. ANDERSON, FRANK M., Geol Cartagena Refining Co., Cartagena, Colombia, S. A. BACON, MAURICE W., Genl. Mgr Stewart Mining Co. Butte, Mont. BACON, RAYMOND F., Chem Director, Mellon Institute, Pittsburg, Pa. BAKER, HAMILTON WALLACE, Min. Engr Fernley, Nev. VON BAYER, AUGUST HECTOR, Supt Kentucky Solvay, Coke Co., Ashland, Ky. BISHOP, WHEELER SCOTT, Research Chem Care Braden Copper Co., Rancagua, Chile, S. A. BOWEN, CHARLES GILMAN, Timekeeper 208 School St., Grass Valley, Cal. BOYER, SAMUEL L., Mine Operator, Mgr., Mike. Horse Min. Co., W. 2808 Boone Ave., Spokane. Wash.

Jan 7, 1914

By Oscar E. Harder, H. A. Grove

It is now just a quarter of a century since Fred W. Taylor§(23) pub-lished his classical paper On the Art of Cutting Metals, describing his researches in which he, in cooperation with Maunsel White, had developed what is essentially the modern method of heat-treatring high-speed steels. Regarding this research, Dr. Sauveur,(22) in his address on Steel Wizards, Past and Present, at the annual banquet of the American Society for Steel Treating in Philadelphia in 1920 said, "The discovery of high-speed steel, or if you prefer, of the treatment imparting high-speed properties to certain steels by Taylor and Maunsel White I am inclined to consider as our one epoch-making contribution to the metallurgy of steel." It was at about that same time (1900) that Taylor exhibited high-speed steels, heat-treated by the improved process, at the World's Exposition in Paris and attracted much attention by showing that the steels would operate at such feeds and speeds that the tips of the tools were visibly red hot. This observation must have started metallurgists to wondering regarding the relative hardness of the various steels at red-heat temperatures. Considerable work has indeed been done in an effort to measure the hardness of high-speed steels and related materials in the red-heat range, using various methods. The result's, however, have been only partly satisfactory, owing to experimental difficulties. The present investigation had as it's immediate inception an address by J. V. Emmons, of the Cleveland Twist Drill Co., to the Columbus Chapter of the American Society for Steel Treating in 1931, in which he deplored the fact that comparatively little was known with regard to the hardness of high-speed steels at elevated temperatures, in spite

Jan 1, 1933

By J. B. Austin

It is now well established, chiefly through the work of Davenport and Bain,' that the influence of temperature upon the rate of transformation of austenite to ferrite at constant temperature is represented by a curve of the type shown in Fig. 5 on page 295 and the reasons for this general shape have been discussed by them in a qualitative way. Thus, the upper part, or nose, of the curve is the resultant of two factors of which the rate of change with temperature is not the same, and by analogy with other like cases it is almost certain that these factors are: (1) the chemical potential, or driving force, of the transformation, which is zero at the equilibrium temperature and increases rapidly as the temperature falls below this point; and (2) a factor analogous to viscosity, or resistance of the crystal lattice to a change in structure, which also increases as the temperature is lowered. Just below the equilibrium temperature this virtual "viscosity" of the metal is relatively low—that is, the metal offers little resistance to a change in lattice—but the driving force is also small, and the net result is that the reaction proceeds slowly. As the temperature is lowered the magnitude of both factors increases; but at first the driving force increases more rapidly than the resistance and the reaction is observed to proceed more rapidly. At lower temperatures, however, the resistance begins to increase faster than the driving force, and eventually, at the nose of the curve, overbalances it, causing the reaction to proceed more and more slowly thereafter. This concept is somewhat, though not completely, analogous to that employed in certain electrical cases where the precise factors are known and are separately measurable. The current I (in amperes or coulombs per second) flowing through a given wire is proportional to the impressed potential, or driving force E, and is inversely proportional to the resistance R of the wire; that is, I = E/R. Stated in a slightly different way, the time required for one coulomb to pass a given point (1/I) is equal to R/E. If the temperature of the whole circuit is changed, the resultant change in 1/I will depend on the relative rates of change of R and of E,

Jan 1, 1935

By J. B. Austin

It is now well established, chiefly through the work of Davenport and Bain,' that the influence of temperature upon the rate of transformation of austenite to ferrite at constant temperature is represented by a curve of the type shown in Fig. 5 on page 295 and the reasons for this general shape have been discussed by them in a qualitative way. Thus, the upper part, or nose, of the curve is the resultant of two factors of which the rate of change with temperature is not the same, and by analogy with other like cases it is almost certain that these factors are: (1) the chemical potential, or driving force, of the transformation, which is zero at the equilibrium temperature and increases rapidly as the temperature falls below this point; and (2) a factor analogous to viscosity, or resistance of the crystal lattice to a change in structure, which also increases as the temperature is lowered. Just below the equilibrium temperature this virtual "viscosity" of the metal is relatively low—that is, the metal offers little resistance to a change in lattice—but the driving force is also small, and the net result is that the reaction proceeds slowly. As the temperature is lowered the magnitude of both factors increases; but at first the driving force increases more rapidly than the resistance and the reaction is observed to proceed more rapidly. At lower temperatures, however, the resistance begins to increase faster than the driving force, and eventually, at the nose of the curve, overbalances it, causing the reaction to proceed more and more slowly thereafter. This concept is somewhat, though not completely, analogous to that employed in certain electrical cases where the precise factors are known and are separately measurable. The current I (in amperes or coulombs per second) flowing through a given wire is proportional to the impressed potential, or driving force E, and is inversely proportional to the resistance R of the wire; that is, I = E/R. Stated in a slightly different way, the time required for one coulomb to pass a given point (1/I) is equal to R/E. If the temperature of the whole circuit is changed, the resultant change in 1/I will depend on the relative rates of change of R and of E,

Jan 1, 1935

By Donald D. Carr, Lawrence F. Rooney

Perhaps no other mineral commodity in this volume has as many uses as limestone and dolomite. These carbonate rocks are the basic building blocks of the construction industry, the material from which aggregate, cement, lime, and building stone are made. Carbonate rocks, and their derived products, are used as fluxes, glass raw material, refractories, fillers, abrasives, soil conditioners, ingredients in a host of chemical processes, and much more. Although the use of limestone and dolomite goes back before recorded history, new uses and products are continually being found. Carbonate rocks form about 15% of the earth's sedimentary crust and are widely available for exploitation. Found extensively on all continents, they are quarried and mined from formations that range in age from Precambrian to Recent. Reserves of carbonate rock are large and will last indefinitely, although high-purity deposits may be absent or have limited availability in certain areas. Limestone and dolomite are so useful and so abundant that in 1981 about 644 million tons were produced in the United States. In fact, about 75% of all stone quarried or mined in the United States was carbonate rock. Sand and gravel was the only mineral commodity produced in greater quantity. In this chapter we have sought to provide the general reader an overview of carbonate rocks, their composition, distribution, production, and uses, with emphasis on developments since 1960. In doing so we borrowed extensively from our report on the applied geology of limestone and dolomite (Rooney and Carr, 1971). The literature on the limestone and dolomite resources of the United States and Canada is so vast and diverse that one can easily become mired down in print. We tried to list those references that are easily accessible and that provide the economic geologist with a starting point for more intensive study. The table listing selected references on limestone and dolomite resources in Canada and the United States reflects our attempt to be selective rather than exhaustive and to direct the reader to the best sources of detailed information. Geology Mineralogy The principal carbonate rocks used by industry are limestone and dolomite. Limestones are sedimentary rocks composed mostly of the mineral calcite (CaCO3) and dolomites are sedimentary rocks composed mostly of the mineral dolomite (CaCO3 • MgCO3). Aragonite (CaCO3), which has the same chemical composition as calcite but a different crystal structure, is economically important only in modern deposits, such as oyster shells and oolites. Aragonite is metastable and alters to calcite in time. Some other carbonate minerals, notably siderite (FeCO3), ankerite (Ca2MgFe (CO3)4), and magnesite (MgCO3), are commonly found associated with limestones and dolomites but generally in minor amounts. Because of their similar physical properties, the carbonate minerals are not easily distinguished one from the other. Specific gravity,

Jan 1, 1983

By Oswald J. Heinrich

THE origin of spontaneous combustion in collieries is, of course, chiefly due to bad system in laying out the pits, unclean workings, insufficient ventilation, and neglect in damming off works after they are exhausted of the main coal. This is particularly indispensable in the Richmond field, because it is difficult and dangerous here, on account of the inferior roof, to remove the last vestiges of coal ; and we are compelled also to retain all the slates and bands, as far as possible, in the pit, to help fill up, although such material is liable to fire. This, however, can be prevented to a great extent, as mentioned below. I am satisfied that the only system of working this thick coal is by cross-cutting (Querbau, ouvrage & travers) or working in benches, as practiced in France (Creusot, Rive de Gier, St. Etienne), in Silesia (Kiinigsgrube), which I have used as far as it is practicable in an old pit, almost torn to pieces by former workings. Modifications may, of course, be needed, even in the same pit, on account of irregularities in the seam. I am also satisfied for economical reasons (on account of the heavy cost for timbering) that pits here ought to be worked upwards, even if it requires a longer period of time to win the coal, and a greater outlay of capital to commence with. The various saddle-shaped " troubles " making natural minor basins in the main basin aid in the execution of this plan. A pit worked once ought to be worked out clean, given up, and dammed off forever. If sections of proper height are assumed, according to the required amount of production for a certain period of time, they ought to be worked out and filled in as much as possible, dammed off, and ultimately allowed to fill up with water, in order to protect the upper works in future from fire in the gob below. This I consider indispensable, because we may not be able profitably to fill in all the ground. To do so we have to use the waste of the mine, although it is liable to fire in time. In using this stuff, it ought to be surrounded by walls of rock not liable to take fire, laid firmly in clay, the gob being in the middle, and firmly covered and packed with clay on top. In

By Oswald J. Heinrich

(with figures on plate V.) THE origin of spontaneous combustion in collieries is, of course, chiefly due to bad system in laying out the pits, unclean workings, insufficient ventilation, and neglect in damming off works after they are exhausted of the main coal. This is particularly indispensable in the Richmond field, because it is difficult and dangerous here, on account of the inferior roof, to remove the last vestiges of coal ; and we are compelled also to retain all the slates and bands, as far as possible, in the pit, to help fill up, although such material is liable to fire. This, however, can be prevented to a great extent, as men¬tioned below. I am satisfied that the only system of working this thick coal is by cross-cutting ( Querbau, ouvrage à travers) or working in benches, as practiced in France (Creusot, Rive de Gier, St. Etienne), in Sile¬sia (Königsgrube), which I have used as far as it is practicable in an old pit, almost torn to pieces by former workings. Modifications may, of course, be needed, even in the same pit, on account of irregu¬larities in the seam. I am also satisfied for economical reasons (on account of the heavy cost for timbering) that pits here ought to be worked upwards, even if it requires a longer period of time to win the coal, and a greater outlay of capital to commence with. The various saddle-shaped "troubles" making natural minor basins in the main basin aid in the execution of this plan. A pit worked once ought to be worked out clean, given up, and dammed off forever. If sections of proper height are assumed, according to the required amount of production for a certain period of time, they ought to be worked out and filled in as much as possible, dammed off, and ulti¬mately allowed to fill up with water, in order to protect the tipper works in future from fire in the gob below. This I consider indispen¬sable, because we may not be able profitably to fill in all the ground. To do so we have to use the waste of the mine, although it is liable to fire in time. In using this stuff, it ought to be surrounded by walls of rock not liable to take fire, laid firmly in clay, the gob being in the middle, and firmly covered and packed with clay on top. In

Jan 1, 1873

[The following discussion, comprising both remarks made at the Chicago meeting and contributions since forwarded to the Secretary, is based upon the following papers, presented at that meeting : "Segregation and its Consequences in Ingots of Steel and Iron," by Alexandre Pourcel, Paris, France. (See p. 105, mans. xxii.) " Microscopic Metallography," by F. Osmond, Paris, France. (See p. 243, Trans. xxii.) " Microstructure of Ingot-Iron in Cast Ingots," by Prof. A. Martens, Berlin, Germany. (See p. 37.) " Microstructure of Steel," by Albert Sauveur, South Chicago, Ill. (See p. -546, Trans. xxii.) "Farther Observations on the Relations Between the Chemical Constitution and Physical Character of Steel," by William R. Webster, Philadelphia, Pa. (See p. 113.) "The Heat-treatment of Steel," by H. M. Howe, Boston. Mass. (See p. 466.) Since all these papers were considered together, no attempt has been made to separate the discussion strictly under the several heads.] William R. Webster, Philadelphia, Pa.: I desire to say that in my first paper (Trans., xxi., 766) the actual ultimates were subtracted from the estimated ultimates, whereas in the paper submitted at this meeting the estimated ultimates are subtracted from the actual, thus giving contrary signs. The latter method corresponds with the direct effect. of low and high finishing-temperatures ; that is, a plus difference indicates low, and a minus difference high, finishing-temperature. I make this explanation to prevent confusion in comparing the two papers. Mr. Sauveur has shown that there is a close relation between the size of the grain and the ultimate strength, and also that the size of the grain depends on the temperature at which the material is finished in rolling, and on the chemical composition of the steel. I have shown that there is a close relation between the chemical

Jan 1, 1894

By Nathaniel Arbiter

THE separation of minerals by flotation can be regarded as a rate process, with the extraction of any one mineral determined by its flotation rate, and the grade of concentrate by the relative rates for all the minerals. So regarded, the significant variables for the process are those that control the rates. These variables are of two types, the first describing the ore and its physical and chemical treatment prior to flotation and the second characterizing the separation process in the cells. This paper will examine the variation in rates for a group of separations, will show that a simple rate law appears to govern, and will consider the relation of the control variables to the rates. The use of rate constants for evaluation of performance and efficiency will be discussed. Flotation involves the selective levitation of mineral and its transfer from cell to launder. The flotation rate is the rate of this transfer. It may be defined by the slope of a recovery-time curve for any cell in a bank, or at any time in batch operation. The objective in flotation rate study is an equation expressing the rate in terms of some measurable property of the pulp. This can be either the concentration of floatable mineral in weight per unit volume1,2 or a relative concentration, which will be a function of the recovery." A rate equation for an actual flotation pulp will contain at least two constants, both to be determined from the data. One of these, the initial concentration or proportion of floatable mineral, is not necessarily equal to the feed assay because of nonfloatable oversize or locked particles." The other, a rate constant, is a measure of proportionality between the rate and the pulp property on which the rate depends. The value of the rate constant will be determined by the values of all variables which control the process and will be changed by significant changes in any of them. It is, therefore, a direct measure of performance. Where recovery or grade change continuously with flotation time, the rate constant will be independent of time and will characterize the entire course of the separation. Development of Rate Equations Rate equations can be developed either by analysis of the mechanism of the process or by direct fitting of equations to recovery-time data. Sutherland's attempt by the first method' suggests that the effect of particle size variation on the rate complicates the derivation of a simple equation applicable to an ore pulp. A further problem with an ore is the concentrate grade requirement, which usually involves a variable rate of froth removal. Thus the final rate for any cell may depend on the froth character and froth height, as well as on the pulp composition. This does not imply that each cell cannot reach a steady state2 in which the rate will depend ultimately on pulp composition. The second method is the fitting of rate equations consistent with the necessary boundary conditions* to experimental recovery-time curves. On the assumption that under constant operating conditions the flotation rate is proportional to the actual or relative concentration of floatable mineral in the pulp, a generalized rate equation may be expressed as follows: Rate = Kcn [I] where K is the rate constant, c is some measure of the quantity of floatable mineral in the pulp at time t, and n is a positive number. In previous rate studies, the value of n has been taken as 1, either by direct assumption," or as a result of the hypothesis that bubble-particle collision is rate determining.' A first order equation results, which after integration in terms of cumulative recovery R, leads to Loge A/A-R = Kt [2] The quantity A is the maximum possible recovery with prolonged time under the conditions used. No conclusive proof for the validity of this equation in flotation has been advanced. The evidence cited in its support consists entirely in the demonstration that it appears to apply to a limited number of recovery-time curves."' It will be shown subsequently that this procedure is not sufficient to establish the order of a flotation rate equation. The possibility that the equation may be of higher order therefore requires examination. If, in particular, the exponent in eq 1 is assumed to be 2, then after integration there results R = A2Kt/1 + AKt [3] with K again a rate constant and A the maximum proportion of recoverable mineral. Eq 3 may be

Jan 1, 1952

By J. Burns Read

IT IS the purpose of this paper to summarize, as far as possible, the metallurgical information and experience gained by the Ordnance Department, during the War, in the manufacture of artillery cartridge cases, to describe the tests to which artillery cartridge cases were put, and to summarize the knowledge and experience gained in this testing. The authors wish to acknowledge the aid given by manufacturers, army officers, and civilian employees of the Ordnance Department in obtaining these data. Artillery cartridge cases are cold drawn from circular disks punched from strips of rolled brass. The manufacture involves from 25 to 30 main operations, which are done almost entirely on a punch press. Descriptions of the operations have appeared in various periodicals and, therefore, will not be given here. After each cupping, or drawing, operation, except the last, the cases are annealed at from 540° to 650° C. (1000° to 1200°F.), to remove all the hardening stresses set up in the metal and to allow complete recrystallization. After each annealing, the cases are pickled in niter cake or sulfuric-acid solution and then washed in water to remove all traces of acid. In some instances, the cases are then immersed in a cyanide-salt solution, and afterwards rinsed in water, to remove the thin layer of copper that forms on the surface of the cases during the acid pickle. The last cold-drawing operation is followed, by the heading operation which, by flattening the head of the case on the outside, causes the metal to flow on the inside to approximately the proper finished dimensions. The mouth, or open end, is then annealed at 430° to 480° C. (800° to 900° F.) by immersion in a salt bath or by gas flames. After being washed, the cases are tapered, when they are ready for machining, inspection, and testing.

Jan 4, 1922

By John Blatchford, William T. Hall

The product obtained by roasting stibnite is likely to contain some unoxidized antimony trisulphide and a mixture of antimony trioxide and antimony tetroxide. It was desired to determine, as accurately as possible, the condition of the antimony as well as the total quantity present. Attempts were made to separate the trisulphide and the two oxides by methods based upon their varying solubilities in different solvents, but no satisfactory results were obtained in this way. It was found, however, that by determining the total antimony content, the antimony present as trioxide, and the antimony present as trisulphide, a good idea of the chemical composition of the roasted product could be obtained. The total antimony was determined by dissolving the sample in concentrated hydrochloric acid, reducing the antimony entirely to the trivalent condition by means of hydriodic acid and eventually titrating the antimony back to the pentavalent condition by means of iodine in the presence of sodium bicarbonate1* The details of the procedure are as follows: Weigh out 0.25 gram of the roasted product into a trapped flask (Fig. I), add 4 grams of powdered tartaric acid, 2 grams of potassium iodide and 40 c.c. of concentrated hydrochloric acid. Boil the solution gently f;r 5 min. and then cool to room temperature by shaking the flask while holding it under running water. Then, very carefully discharge the iodine color by the cautious addition of 0.05-normal sodium thiosulphate solution, adding a little starch toward the last. Nearly neutralize the acid with ammonia solution, but leave the solution distinctly acid. Pour the slightly acid solution into 200 c. c. of water containing an excess of sodium bicarbonate and titrate to a permanent blue color with standard 0.1-normal iodine solution.

Jan 1, 1916

By B. S. Hickman

Using primarily quantitative single crystal X-ray techniques studies have been made of the precipitation of the metastable w phase in alloys of titanium with Mo, Mn, Fe, Cr, and Nb. It is shown that, in agreement with earlier work on the Ti-V system, the composition of the w phase during aging approaches a constant; the value varies from one system to another in a systematic manner with the electron concentmtion. Results relevant to the mechanism of w precipitation during quenching and during aging are presented and discussed. Results are presented to confirm that the w phase is coherent and the nzorphology of the Necipitates is described and discussed. PRECIPITATION of the metastable w phase in alloys of titanium is of interest because of its severe embrittling effect and also because of the enhancement of the superconducting properties which accompanies precipitation.1 The general features of w phase precipitation have been discussed by cuillan and by Bagaratskii et d3 The work described in this paper forms part of a general study of w phase precipitation which was undertaken to elucidate various unknown or controversial features of the process, namely: i) What is the mechanism of formation of the phase ii) How does its composition, morphology, volume fraction, and particle size vary with the type and content of the alloying element and with the heat treatment conditions? iii) What is the relation between the w phase and the equilibrium a phase? In a previous paper4 the results of a detailed study of w phase in Ti-V alloys were presented. It was shown that: U During aging the composition of the w phase approached a saturation value of 13.5 to 14.0 at. pct V. ii) w precipitated as cube shaped particles and once precipitation was complete, particle coarsening did not occur. iii) a phase formed initially by direct conversion of w-phase precipitates. In this paper similar measurements are reported on Ti-Mo alloys and some more limited data given on the Ti-Cr, Ti-Fe, Ti-Mn, and Ti-Nb systems. The results i.1 the six systems are then compared. It has been shown previously by electron microscopy that the w precipitates as ellipsoids in both the Ti-Nb system,&apos; and in i-o.&apos; Blackburn and williamsz3 have reported the precipitates in Ti-Fe, Ti-Cr, and Ti-Mn are cubic, i.e., similar to the Ti-V system.476 EXPERIMENTAL METHODS 1) Specimen Preparation. Samples of the compositions shown in Table I were prepared by arc melting. High purity electron beam zone refined titanium (Materials Research Corporation Grade I—total impurity content =250 ppm) was used; the other source materials are given in the table. A commercial Ti-8 wt pct Mn alloy was used for studies of this system. After homogenization the materials were rolled or cut into strip approximately 1/4 in. by 2 in.; the strip was then heated at temperatures of 1200" to 1300°C for several hours by passage of a direct current through the strip in an ultra high vacuum system (<10-torr) and then quenched by admitting high purity helium and switching off the current. This treatment resulted in crystals up to 2 in. by 2 in. by A in., almost all of which had a [100] direction nearly perpendicular to the plane of the strip. The crystals were cut from the strip by spark machining and their composition checked by lattice parameter measurements supported by chemical analysis. 2) X-Ray Diffraction Methods. Lattice parameter measurements were made using a modification of the single crystal spectrometer described by ond. In this technique the crystal angles for reflection on either side of a highly collimated primary beam are measured. Generally the 400 CuK, or the 400 CuKp reflections of the bcc lattice were used. In the as-quenched crystals a precision of 1 in 105 was obtained, but due to line broadening the parameters in aged materials could only be measured to 1 in lo4. This accuracy was, however, quite adequate for the purposes of these experiments and enabled the composition of the p phase to be obtained to 10.1 pct in all systems except Ti-Nb where the lattice parameter change with composition is very small. The precipitation and growth of the w phase was examined using a single crystal goniometer attached to a Phillips diffractometer. The relative intensities and line shapes of b-phase and w-phase reflections

Jan 1, 1970

By H. S. Bell

It seems unnecessary to dwell upon the advantages of the modern pipe still as compared with the older type of distillation equipment used by oil refiners. The relatively low installation cost, coupled with remark-able operating efficiencies of pipe stills, precludes the consideration of other types except in rare instances where some peculiarity of product or plant may have an influence. The question of the actual heat required to distil petroleum is quite involved. We have extensive data on the latent heats of the various hydrocarbons under different conditions of pressure. We also have information regarding the specific heats of various oils and the effect of temperature thereon. Because of the complexity of petroleum and of each fraction, it seems impossible to analyze theoretically the partisl-pressure effect of the great number of hydrocarbons upon one another during distillation. If a distillation curve and percentage analysis of any crude or product are available, it is possible to construct a curve with ordinates representing per cent. distilled and B. t. u. per pound or per gallon, or other desired unit. To do so the crude is split into fractions, of 5 or 10 per cent. The boiling point and gravity of each fraction being determined, it is possible to evaluate the heat required. As each fraction is removed, the residue must be raised to a higher temperature and latent heat supplied for the successive fraction. As the calculations progress, the latent heats decrease while the specific heats increase. Such a curve is illustrated by Fig. 1 for a typical 39.9° Be. North Texas crude. The chart is illustrative of batch distillation. Theoretically, if the oil were heated by a single flash in a pipe still, the partial-pressure effect of the light products would result in the removal of the same amount of vapors at a lower temperature. Practically, we find that because of the necessarily extensive fractionating equipment required when separating many products all in vapor phase, the oil has to enter the separator at temperatures corresponding to or even above those required in the batch still. Furthermore, in single-flash distillation the vapors evolved in the heater must be superheated to the outlet temperature. Very little is

Jan 1, 1928

By Frank C. Kelton

It is perhaps not widely realized that extraction and saturation processes carried out on oil well core samples alter the properties of these samples to varying degrees. On the other hand it is felt by some that quick-freezing of core samples increases their permeability and porosity significantly. Accordingly, laboratory tests were carried out on 49 pairs of horizontally adjacent samples in order to differentiate between the effect of quick-freezing per se on permeability and porosity of the samples, as distinguished from the effect of the identical saturation treatment on permeability and porosity of the companion samples. Also, additional field data were obtained on comparison of frozen vs unfrozen companion samples. LABORATORY INVESTIGATION OF FREEZING us SATURATION EFFECTS Procedure The samples used in these tests were two-cm cubes cut in horizontally adjacent pairs from cores from eight Gulf Coast and Mid-Continent wells, which cores had not previously been frozen. These samples were extracted with carbon tetrachloride, dried, and air permeabilities run in the conventional manner. They were then evacuated and saturated with brine of 25,000 ppm sodium chloride content, and porosities determined by gain in weight. The samples were partially desaturated by evaporation down to an average brine saturation of 68 per cent. One sample from each pair was quick-frozen by covering with dry ice after wrapping in a single layer of paper, and allowed to remain frozen for about two hours; the companion sample from each pair was not frozen. After thawing the frozen sample, all samples were immersed in tap water overnight in order to leach out most of the brine. Air permeabilities were re-run, and the samples were again saturated with brine to determine a second porosity value. For purposes of averaging of data, the samples were grouped according to four permeability ranges, from 0 to 10, 10 to 100, 100 to 1,000, and 1,000 to 3,840 md. Average permeability and porosity changes for the frozen vs the unfrozen adjacent samples are shown in Table 1. Discussion As may be seen from Table 1, the averages of the per cent permeability increases for the quick-frozen samples ranged from 3.8 to 12.9 per cent among the four permeability groups. The average changes among the four groups of unfrozen companion samples ranged from a decrease of 0.2 per cent to an increase of 9.3 per cent. There was no particular correlation of these changes with magnitude of permeability; however, the increase for each group of frozen samples paralleled the increase for the corresponding unfrozen samples. The differences between the two sets of values are believed to be a valid indication of the effect of the quick-freezing in itself, since the treatment of the two samples in each pair was identical except for freezing. The permeability changes which are strictly the result of the quick-freezing are shown in the sixth column of Table 1. These range from a decrease of 0.9 per cent to an increase of 4.0 per cent; the overall weighted average is 1.2 per cent, as compared to an average increase of 6.8 per cent caused by the saturation treatment of the samples not frozen. The average porosity changes are in general smaller than the changes in permeability, and range from a decrease of 2.3 per cent to an increase of 3.3 per cent. The overall weighted average change ascribed to the quick-freezing is 1.0 per cent of porosity. Many factors can contribute to the changes in permeability and porosity observed when subjecting cores to the simple processes used in these tests. Such are: hydration and swelling of clay, adsorption of ions, changes in surface structure and wettability, expansion and compression effects due to ice formation, shrinking and cracking, leaching of salts and colloids, displacement of particles resulting in either blocking or enlarging of pore openings. Whatever particular mechanisms are involved. however, it is apparent not only from this study but also from other investigations in the literature&apos; not directly concerned with quick-freezing, that the effects produced by commonly used extraction, saturation and drying techniques may be of considerable magnitude The results of this study indicate that for the particular samples and techniques used, such effects are of the order of five to six times the effect of quick-freezing. insofar as changes in permeability are concerned. It may be argued that these samples might not include extremely shaly material where the effect of freezing upon permeability may be much greater. However, had such material been available for these tests, it would undoubtedly have been very susceptible also to alteration by the extraction and saturation treatment used. To investigate this point further, the individual sample data were re-grouped according to the magnitude of the average per cent permeability increases for the pairs of samples, irrespective of permeability. The results

Jan 1, 1953

By D. Turnbull, R. E. Cech

FISHER, Hollomon, and Turnbull have developed a theory for the nucleation of martensite. They first tested the theory on Fe-C alloys and low alloy steels. The major factor influencing nucleation of martensite was considered to be statistical composition fluctuations occurring in small regions at high temperature and frozen-in on quenching. These local regions of varying size and composition serve as nucleation centers. They become supercritical, one by one, as temperature is progressively lowered, resulting in temperature-dependent or athermal transformation. Fisher next applied nucleation theory to substi-tutional solid solution alloys. Detailed predictions were made for Fe-Ni alloys because of the availability of free energy data on this system. It was shown that composition fluctuations that were significant energy-wise did not occur, and nucleation frequencies could be calculated from average properties of the system. Nucleation was predicted to occur as time-dependent and having the functional relationship to give a C curve of nucleation frequency vs temperature. The analysis further predicted that the nucleation frequency was extremely sensitive to composition. Experimentally, it would be found that the transformation in some compositions is so slow that measurable amounts will not form in a reasonable length of time. With other compositions, only slightly different, the nucleation frequency becomes so great that the material becomes transformed while still distant in temperature from the maximum nucleation frequency. On quenching an alloy of such composition, the observed transformation kinetics would be similar to those found in Fe-C alloys. Cech and Hollomon repeated experiments of Kurdjumov n which the kinetics of transformation were similar to those predicted by Fisher for Fe-Ni alloys. The alloy studied in this investigation contained 73.3 pct Fe, 23.0 pct Ni, and 3.7 pct Mn. Fisher,&apos; using an idealized model for the extent of transformation as a function of the number of martensite crystals per grain of parent phase, derived nucleation frequencies from the transformation curves of Cech and Hollomon. Complicating influences such as coupling effects between grains in the polycrystalline specimens were neglected. Nevertheless, excellent agreement was found between the theoretically and experimentally derived nucleation frequencies. These experiments, however, could not provide a critical test of the theory. Experimental nucleation frequencies could vary widely from those calculated, depending upon the extent of deviation from ideal partitioning and the extent of coupling effects. Further, since the compositions of material theoretically analyzed and experimentally determined were different, the free energy changes involved in the experimental work could only be estimated. Also, the effect of heterogeneities on the transformation kinetics was not considered. For these reasons, it was decided that experiments designed to test the validity of the Fisher analysis must be conducted on binary Fe-Ni alloys, which were the ones considered theoretically by Fisher. The martensite transformation in Fe-Ni alloys has been the subject of considerable study. Machlin and Cohen have shown that transformation proceeds in a manner quite unlike that in any other ferrous alloy system. They found that single crystals would transform to a large extent in a single burst. In large grain polycrystalline specimens, frequently more than one grain and sometimes the whole specimen would transform at the same instant in this manner. Results on filings indicated that different particles would undergo the burst transformation at widely different temperatures. These results support the conclusion that the transformation behavior could not be described by a single nucleation frequency as would be the case if the nucleation were homogeneous. It appeared that further work was necessary to define the factors responsible for burst-type transformation, so that the conditions could be altered to favor homogeneous nucleation of martensite if such could be accomplished. This report summarizes the results of some experiments conducted with powdered Fe-Ni alloys for this purpose and the re-

Jan 1, 1957

By Hiram Brown

The problem of stress corrosion has been discussed a great deal recently, but many factors have as yet not been clarified. There are many interpretations of the definition of the word, different corrosive media are used, and numerous methods of stressing are utilized. Some quarters believe that the inherent strength of the material under test is the determining factor of its resistance to stress corrosion, while others think that the natural corrosion resistance of the material is the determining factor. This paper is intended merely to set forth the limited experience we have had and to discuss some of the other stress-corrosion tests which have been made with light alloys.

Jan 1, 1945

Jan 1, 1887

By D. W. Lillie

It has been demonstrated that considerable bend ductility exists in bulk specimens of polycrystalline high-purity silicon. The possibility of hot-forming at 1200°C is suggested. EXCELLENT corrosion resistance in many media and low cross section for absorption of thermal neutrons (0.13 barn) would make silicon of interest to nuclear engineers were it not for extreme brittle-ness and the difficulty of fabrication by any reasonable means. The use of silicon for structural purposes also has been considered in view of its light weight and oxidation resistance. Johnson and Han-sen&apos; have investigated the properties of silicon-base alloys and concluded that there was no way of making pure silicon or silicon-rich alloys ductile at room temperature. In view of reports of appreciable ductility in germanium single crystals above 550°C&apos;." and some plastic deformation in single-crystal silicon above 900oC,&apos; the present investigation was undertaken to define more precisely the limits of high-temperature ductility in pure silicon. After this investigation was begun torsion ductility in both germanium and silicon was reported by Greiner." Through the courtesy of F. H. Horn, a small bar of cast extra high-purity silicon was obtained and small bend specimens were made from it by careful machining and grinding. All of the reported tests results were obtained from samples from this bar (bar No. 1) and one other of similar source (bar No. 2). No complete analysis was obtained but, based on analysis of similar semi-conductor grade material, metallic impurities were under 0.01 pct total. Vacuum-fusion analysis for oxygen showed a value of 0.0018 2 0.0003 pct for the first bar tested and metallographic analysis showed no evidence of a second phase. Bend tests were carried out on an Instron tensile machine using a bend fixture with a 1 -in. span loaded at the center. Supporting and loading bars were 0.250 in. round and the load was applied by downward motion of the pulling crosshead of the machine. Specimen thickness and width were approximately 0.10 in. and % in. respectively. Loading rate was controlled by holding crosshead motion constant at 0.02 ipm. In some cases a smaller specimen was used on a 5/8-in. span with a 0.129-in.-diam loading bar. The entire bend fixture was surrounded by a hinged furnace and all heating was done in air atmosphere. Temperature measurement was made with thermocouples fastened directly to the bend fixture within less than 1 in. from the specimen. Autographic stress-strain curves were recorded during each test, and breaking load, total deflection, and plastic strain could be obtained from these curves. Stress was calculated from the beam formula S = 3PL/2bh2, where P is the load in pounds, L the span in inches, b the specimen width in inches, and h the specimen thickness in inches. This formula is strictly correct only in the elastic range but has been used to calculate a nominal stress for convenience in the plastic range. The stress given is the maximum stress in the specimen. Results The results of the complete series of tests are shown in Table I. The first group of tests (specimens Nos. 1-6) showed the beginning of plastic flow at a test temperature of 900°C, so two additional tests (Nos. 8 and 9) were made at 950°C on small-size specimens from bar No. 2. Specimen No. 8 was tested in the as-machined condition, and No. 9 was heat-treated in hydrogen at 1300°C for 2 hr, cooled to 1200°C and held 1 hr, cooled to 1000°C and held 1 hr, cooled to 900°C and held 1 hr, and finally cooled to a low temperature before removal from the hydrogen. It is apparent that the heat-treatment had a significant effect on yield strength and ductility. In addition, the magnitude of the yield point was conslderably reduced in the heat-treated specimen as is shown m Fig. 1 by tracings of the stress-strain curves. After obtaining a furnace capable of reaching higher temperatures specimens Nos. 10 to 13 were tested at 1100 and 1200°C. Strain rate was increased by up to a factor of 10 to see whether the ductility observed was excessively strain sensitive. Specimen NO. 10, strained at 0.02 ipm and 1100oC, was still bending at a deflection of 0.322 in. when the load rate was increased to 0.2 ipm, resulting in immediate

Jan 1, 1959