Search Documents

By Theo B. Comstock

In the summer of 1877, the writer led a party of four young men from Cleveland, Ohio, by way of the Great Lakes, to Prince Arthur's Landing (now Port Arthur), at the northwest corner of Lake Superior, thence, via the Dawson route and side journeys, as far as Cross Lake. It was the original intention to pass down the Pigeon river to its mouth, but the loss of one member of the party for six days in the forest, added to other obstacles, made it necessary to turn back. A well-filled note-book, together with illustrative collections, were sunk beyond recovery at the head of the Maligne rapids by the breaking of a tow-line, and two of our number (including myself) narrowly escaped drowning. I had, probably, obtained information of considerable economic value, but the necessity of travelling nearly 125 miles for provisions (excepting a meagre supply kindly furnished us by a Canadian government gang whom we fortunately met), rendered further note-taking impossible. Until now, such results of this expedition as could be recorded . from memory have gone unpublished, because of my inability to make them serve any useful purpose. The trip of the Institute to Vermilion Lake, only a few miles south and east of our turning point, gives some little excuse for presenting the following lines at this time. The ridge back of Port Arthur, Ontario, which follows approximately the course of the Lake Superior shore line, brings up the slates and accompanying strata through which the silver and gold veins of that region have penetrated. The interior district, hack from the lake, may be briefly described as a glaciated area, having its general drainage less modified by erosion than by the original structure. This statement, however, must be somewhat qualified with reference to minor details, which all bear the unmistakable impress of the ice-flow and its recession. In many respects there is much in this tract to remind one of the Sault Ste. Marie topography, excepting that the granitic character of the rocks is here largely replaced by fissile strata. The Kaministiquia river cuts through several of the parallel folds,

Jan 1, 1888

By W. G. Pfann

THE problem of forming points on wires that were from 0.002 in. to 0.010 in. in diam arose in the recent appearance of silicon and germanium point contact rectifiers as elements in microwave radar.1 In these devices a pointed tungsten wire makes a delicate contact with the surface of a semiconductor. Because the quality of such rectifiers is largely determined by the nature of this contact, considerable attention has been given to the formation of the metal point. Reproducibility of contour and freedom from burrs and even microscopic irregularities are considered essential. The operations involved must be simple and rapid enough for mass production. Previously tungsten wires had been provided with conical points by a grinding method which involved rotating a wire about its axis and causing it to bear at an oblique angle against a spinning abrasive disc. This was later complemented with an electrolytic polishing treatment which removed irregularities from the ground point and also rounded it off at the tip-a desirable feature. Finally, these operations were supplanted by the electrolytic pointing method described here. MECHANISM OF POINT FORMATION The wires to be pointed are partially immersed- in an electrolyte in a .vertical position whereupon they are provided with smooth rounded points entirely by electrochemical action. The process is independent of the depths to which the wires penetrate the electrolyte because the points are formed at the surface level. It may be used to point a single wire or many of them simultaneously and is applicable to wires of different diameters within a limited range. Solution of the immersed portion of a tungsten wire is accomplished by making it the positive electrode in an electrolytic cell, as shown in Fig I. While the wire is maintained at constant voltage the current through the cell falls continuously, principally because of the decrease in wetted area which results from solution of the tungsten. This increase in resistance occurs in a reproducible manner and is used as a control in the process. As the immersed portion of the wire dissolves, it remains cylindrical in shape except for the short section which is wetted by the meniscus. Here the rate of solution is lower and decreases as the top of the meniscus is approached. The result is the formation of a tapered section inside the meniscus. As solution continues, the cylindrical section either dissolves entirely or drops off just before complete solution, leaving only the taper which is now sharply pointed. Further action causes this point to become rounded and then quite blunt, until finally the end of the wire is almost plane. Fig 2 shows the stages in this development. Contour PF is most representative of those used in point contact rectifiers. Thus a variety of point

Jan 1, 1947

By John Griffen, David H. Davis

Much of the ground to be covered by this paper was ably covered by a paper presented by Messrs. Morrow and Jordan1 before a joint meeting of the Iron and Steel Section of the Engineers Society of West-ern Pennsylvania and the A.I.M.E. Pitts-burgh Section at Pittsburgh in the spring of 1940. As that paper was not published, the present authors have availed them-selves of Mr. Morrow's kind permission to use information given therein. Similar figures for the latest years available have been added to many statistics originally presented. It is unfortunate that Mr. Jordan's death removes his stimulating guidance and help, which the authors would have welcomed and have found invaluable in the past. One interested in the Pittsburgh seam should not fail to read the exhaustive and authoritative paper by Eavenson2 presented in 1938. As Allegheny, Fayette, Greene, Washington, and Westmoreland Counties contain practically all the reserves and furnish nearly all of the production from the Pittsburgh seam in Pennsylvania at the present time, this area only is intended when reference is made to the Pittsburgh seam in Pennsylvania. On much of the seam in Greene and Washington Counties, which contain a large proportion of the total reserves, insufficient data are available to determine the detailed characteristics of the seam with any degree of finality. It is hoped that the data presented here will fairly well indicate the probable characteristics. Economic Importance of the Pittsburgh Seam The Pittsburgh seam in Pennsylvania is of primary importance as a coal resource, not only because of its substantial reserves but because it contributes such a large proportion of the coal used in the country and an even larger proportion of that used in the manufacture of coke. Mr. Ashley3 placed the estimated recoverable reserves (1935) of the Pittsburgh coal bed in Pennsylvania at 7,500,000,000 tons.* Although a considerable portion of this tonnage is not now suitable for coking coal, because of its high sulphur content, undoubtedly the supply of coking coal will last for many years and that not suitable for coking will furnish industry with an ample supply of energy. In attempting to assess the contribution of the Pittsburgh seam to total coal production and to that of coal used in making coke, one finds that the statistics published annually by the U. S. Bureau of Mines, Minerals Yearbook, do not give tonnages classified as to seams but only as to districts or states and counties. However, it happens that, at present and during much of the

Jan 1, 1944

By David H. Davis, John Griffen

Much of the ground to be covered by this paper was ably covered by a paper presented by Messrs. Morrow and Jordan1 before a joint meeting of the Iron and Steel Section of the Engineers Society of West-ern Pennsylvania and the A.I.M.E. Pitts-burgh Section at Pittsburgh in the spring of 1940. As that paper was not published, the present authors have availed them-selves of Mr. Morrow's kind permission to use information given therein. Similar figures for the latest years available have been added to many statistics originally presented. It is unfortunate that Mr. Jordan's death removes his stimulating guidance and help, which the authors would have welcomed and have found invaluable in the past. One interested in the Pittsburgh seam should not fail to read the exhaustive and authoritative paper by Eavenson2 presented in 1938. As Allegheny, Fayette, Greene, Washington, and Westmoreland Counties contain practically all the reserves and furnish nearly all of the production from the Pittsburgh seam in Pennsylvania at the present time, this area only is intended when reference is made to the Pittsburgh seam in Pennsylvania. On much of the seam in Greene and Washington Counties, which contain a large proportion of the total reserves, insufficient data are available to determine the detailed characteristics of the seam with any degree of finality. It is hoped that the data presented here will fairly well indicate the probable characteristics. Economic Importance of the Pittsburgh Seam The Pittsburgh seam in Pennsylvania is of primary importance as a coal resource, not only because of its substantial reserves but because it contributes such a large proportion of the coal used in the country and an even larger proportion of that used in the manufacture of coke. Mr. Ashley3 placed the estimated recoverable reserves (1935) of the Pittsburgh coal bed in Pennsylvania at 7,500,000,000 tons.* Although a considerable portion of this tonnage is not now suitable for coking coal, because of its high sulphur content, undoubtedly the supply of coking coal will last for many years and that not suitable for coking will furnish industry with an ample supply of energy. In attempting to assess the contribution of the Pittsburgh seam to total coal production and to that of coal used in making coke, one finds that the statistics published annually by the U. S. Bureau of Mines, Minerals Yearbook, do not give tonnages classified as to seams but only as to districts or states and counties. However, it happens that, at present and during much of the

Jan 1, 1944

By F. N. Rhines

STUDIES upon the sintering of metal powders, in the solid state, have led to the proposal that the surface energy of the powder particles provides the driving force that causes points of contact between pairs of particles to grow into broad welds which isolate the residual vacant space into pores that tend to spheroidize and gradually to diminish in total volume.' Investigators differ with regard to the mechanism of the movement of the metal, under the influence of surface energy, to accomplish these changes. One school asserts that there is a mass movement of the metal, referred to as a "viscous flow," while the other school prefers to view the movement as a self diffusion process, wherein individual atoms are, transferred without disturbance of the basic pattern of the crystal lattice. Extensive experimental studies upon the sintering of copper, conducted recently by A. J. Shaler,2 have been in- terpreted by their author as support for the viscous flow mechanism of transport, the theory of which was developed originally by J. Frenkel.3 Duplicating a portion of this work with minor changes, G. C. Kuczynski4 is led to the alternate view, namely, that the initial stages of sintering, at least, proceed as a self-diffusion process. Both of these investigations were designed to deal with an isolated unit of sintering, i.e., with the shrinkage of a single pore, or with the growth of a single point weld. It remains to ascertain the behavior of a typical metal powder compact composed of a large number of particles of varying size and sintering to a body with a multiplicity of pores. The observation of density changes alone during sintering is not sufficient in such a case; it is essential to know how the internal geometry of the compact changes. This has been the object of the present investigation, the results of which are used to support the self-diffusion mechanism of sintering. The present studies consist in the measurement of the number of pores as a function of size and time at temperature during the sintering of a copper compact made from a commercial copper powder lightly pressed and sintered in several different atmospheres. A brief survey was made also of the change in shape of the pores, under the influence of the same variables. All of this was done by direct observation with the microscope. Densities were measured on the same sample. It is found that, while the compact is exhibiting an overall shrink-

Jan 1, 1951

By Enid C. Plante

This paper deals with the flotation of the mineral fluorite (calcium fluoride) and of two associated gangue minerals, calcite and quartz. The aim of the investigation was to produce "acid-grade" fluorite, which must contain less than one per cent of silica. Several reagents are used successfully in practice for floating fluorite from its ores. Oleic acid is the most widely used collector, usually at temperatures above 60°C, with sodium silicate as a dispersant for quartz and quebracho or tannin to depress calcite. Sulphides (e.g., galena) are often removed first by xanthate flotation. Many investigators23 report results in which more than 80 pct of the fluorite is recovered in a concentrate assaying 96 pct or more of fluorite and less than I pct of silica. This investigation was undertaken with the intention of floating the gangue, which is the minor constituent of the ore, from the fluorite. Hence emphasis was first placed on the cationic compounds that float quartz. No satisfactory separations were obtained in this way, and other reagents were investigated to discover whether these were more effective than oleic acid in floating fluorite from quartz in the usual way. The first part of the paper describes experiments with several long-chain collectors available commercially. Most of this work has been by captive-bubble and cylinder flotation tests, with some batch tests in a flotation machine. The second part describes the use of sodium cetyl sulphate as a collector for fluorite and includes laboratory tests and extension of the work to batch tests in the flotation machine. A method for determining the adsorption of sodium cetyl sulphate on fluorite has been developed and is described. Theory of Collection by Paraffin-chain Salts It may be assumed that these compounds are adsorbed at the mineral surface in one or more of three ways outlined by Kolthoff:12 1. Exchange adsorption between lattice ions in the mineral surface and collector ions in solution. Closely related is adsorption by the collecting mechanism postulated by Taggart,17 in which there is metathesis between the collector and the mineral cation or anion. 2. Exchange .adsorption between adsorbed gegen ions (p. 67, ref. 19) and collector ions in solution. 3. Adsorption of nonelectrolytes (polar-nonpolar) without displacement of adsorbed ions. With cationic collectors, inorganic cations in the solution (e.g., hydrogen ion) compete with the collector ions and therefore act as depressants, while inorganic anions have the same effect with anionic collectors. From this follows the general conclusion that ions of the same charge as

Jan 1, 1949

By Myron A. Pugacz, Frank S. McKenna, Clarence E. Jackson

The notched-bar impact test has proved worth while in certain applications as a test for control of the quality or the heat-treatment of steel. In view of the serious thought that even so simple a test as the tensile test has evoked during the past years, it is not surprising that the notched-bar impact test should have inspired much experimental work. The correlation of the great number of data has not been successful, although steady progress has been made toward a better understanding of this test. Progress has been made, especially, in the isolation of the effects of the many variables that control the results. The stress system imposed on a specimen with a notch is so complicated and unpredictable that no simple evaluation of the test has been possible. Because of this uncertainty, many engineers hesitate to use the notched-bar impact test, and this attitude may well continue until a better understanding of the effects of the variables in the test are available. Without doubt, any additional data that may be presented should be accompanied by as complete a description of the - details of test as possible, so that it may be added to the general fund of information that is to serve as the basis for the theory of the notched-bar impact test. The many factors that may control the test results have been pointed out repeatedly. The importance of the effect of the type and dimensions of the specimen has been recognized. Most of the work reported by American investigators has been limited to small-size (Charpy) specimens tested as a simple beam; two types of notches (Fig. I) have been commonly used. Considerable data have also been presented by many investigators using a small specimen tested as a cantilever beam; this commonly being called the Izod test. Here, however, a shear component of stress makes the stress system even more complex than that present in the simple beam type of test, hence a critical analysis is difficult. Much work has also been reported by investigators using the tension type of specimen. A second variable that must be controlled is the testing temperature. An indication that the tests were performed at room temperature is not sufficient, since in many steels a variation of a few degrees in the actual testing temperature may be sufficient to give an entirely different range of results. Other factors, such as the composition and condition of the material being tested and the speed of test, should also be considered. Many investigators have contributed data and theoretical discussions on the problems encountered in notched-bar test-

Jan 1, 1944

By Frank S. McKenna, Myron A. Pugacz, Clarence E. Jackson

The notched-bar impact test has proved worth while in certain applications as a test for control of the quality or the heat-treatment of steel. In view of the serious thought that even so simple a test as the tensile test has evoked during the past years, it is not surprising that the notched-bar impact test should have inspired much experimental work. The correlation of the great number of data has not been successful, although steady progress has been made toward a better understanding of this test. Progress has been made, especially, in the isolation of the effects of the many variables that control the results. The stress system imposed on a specimen with a notch is so complicated and unpredictable that no simple evaluation of the test has been possible. Because of this uncertainty, many engineers hesitate to use the notched-bar impact test, and this attitude may well continue until a better understanding of the effects of the variables in the test are available. Without doubt, any additional data that may be presented should be accompanied by as complete a description of the - details of test as possible, so that it may be added to the general fund of information that is to serve as the basis for the theory of the notched-bar impact test. The many factors that may control the test results have been pointed out repeatedly. The importance of the effect of the type and dimensions of the specimen has been recognized. Most of the work reported by American investigators has been limited to small-size (Charpy) specimens tested as a simple beam; two types of notches (Fig. I) have been commonly used. Considerable data have also been presented by many investigators using a small specimen tested as a cantilever beam; this commonly being called the Izod test. Here, however, a shear component of stress makes the stress system even more complex than that present in the simple beam type of test, hence a critical analysis is difficult. Much work has also been reported by investigators using the tension type of specimen. A second variable that must be controlled is the testing temperature. An indication that the tests were performed at room temperature is not sufficient, since in many steels a variation of a few degrees in the actual testing temperature may be sufficient to give an entirely different range of results. Other factors, such as the composition and condition of the material being tested and the speed of test, should also be considered. Many investigators have contributed data and theoretical discussions on the problems encountered in notched-bar test-

Jan 1, 1944

By W. R. Opie

The object of this paper is to show the manner in which typical electrodeposits of hexagonal-close-packed metals—zinc, titanium, and zirconium—tend to form. The conditions of electrodeposi-tion markedly affect the nature of the deposits in regard to crystal size, orientation, and appearance. No attempt is made to correlate cell conditions with deposit quality but, rather, characteristic types of deposits were selected and a study made to show the relationship between outward appearance and crystal structure. The zinc deposits were made in aqueous electrolytes and the titanium and zirconium deposited from fused salt baths. ZINC deposits studied were made in the American Smelting and Refining Co.'s Central Research Laboratories. They were representative of bright, shiny, smooth deposits, which can be obtained by using proper current densities and electrolyte addition agents, and of deposits which are dull and tend to be nodular. Four deposits were selected which ranged from smooth and bright to very nodular and dull, and their classifications are shown in Table I. These were examined microscopically and were found to differ quite markedly in outward surface structure and in microstructure. The outward surface variation is illustrated in Figs. 1 to 4. At X50 the texture could be seen to progress from granular to platelike to smooth. The microstructures of the deposits' cross sections from starting sheet to outer surface are shown in Figs. 5 through 8. The dull nodular deposits (sample Nos. 1 and 2) show some tendency for acicular growth. The platelike sample (No. 3) shows tendency for columnar growth development and the smooth deposit (No. 4) has a well developed columnar structure. Back-reflection X-ray patterns of the deposit surfaces revealed some interesting information. The crystal orientation was random in all deposits except the smooth deposit. Fig. 9 is a typical back-reflection pattern of a nodular deposit. All planes are reflecting in the proper relative intensity. The pattern of the smooth deposit is shown in Fig. 10. The only planes which reflect are the (10.4). This series of planes is in the right position, with the FeKa radiation used, to satisfy the Bragg equation if the basal planes {00.1) are at right angles to the X-ray beam. The results were interpreted to mean that in the bright smooth deposit preferred orientation has occurred with the basal hexagonal planes oriented in the plane of the sheet but with all other planes randomly oriented around the c-axis.

Jan 1, 1957

By A. L. Johnson, S. C. Lyons

A FEW years ago a leading American builder of centrifuges said, "No one uses a centrifuge if the job can be done any other way." This statement was essentially true at that time, not because the basic functional and economic principles involved did not frequently favor centrifugal methods, but rather because so many of the highly specialized features of the mechanical and functional peculiarities of continuous centrifuges had not been fully developed. The idea of using centrifuges in mineral dressing is definitely not new. There are literally hundreds of patents on centrifugal machines and processes for the mining industry. Many of them cover principles that are basic to the functioning of most centrifuges in operation today. In spite of this, until 1935, there were practically no successful applications of continuous centrifuges in the United States in the mineral industry, nor for that matter were there more than a mere handful of such machines in operation in North America in any industry. This was true despite the obvious desirability of machines that could furnish the advantages of high centrifugal settling forces in a continuous operation. The reasons for this are simple, even if not obvious: I. Finely divided solids, when thrown out of fluid suspension under high centrifugal forces, frequently exhibit physical properties (particularly rheological or flow properties) that are markedly different from those they possess when settled out by gravity alone, and machines that are not designed in careful detail to cope with these peculiarities seldom function satisfactorily. 2. Most continuous centrifuges embody a solids-conveying element in the form of a very special screw conveyor. The rotation of this member under conditions of operation calls for drive designs that were not satisfactorily provided until the introduction of the Bird gear unit about 1934. These matters will be touched on later. Continuous centrifuges are now operating successfully in the mineral industry. Some units have singly handled more than 500,000 tons of solids during the past ten years. Generally their operation has been characterized by large unit capacities, complete elimination of labor, minimum supervision, moderate maintenance and power costs. TYPICAL CENTRIFUGE APPLICATIONS Most materials classified by centrifuges are of subsieve particle size. Practically speaking, this means finer than l00-mesh. A unit of measure other than screens is needed in order to consider these products properly. Such a unit is the micron, which is equal to one one-millionth of a meter; roughly 1/25,000 of an inch. The opening in a standard 200-mesh screen is about 75 microns while a 325-mesh opening is roughly 43 microns.

Jan 1, 1947

By R. J. Wasilewski

The resistivity of single crystal and of polycrystalline metal has been determined between 77° and 1500°K. At comparable purity, the resistivity of the poly crystalline metal differs from that calculated from the axial resistivity values. The observed anisotropy is briefly discussed. A zone refined titanium rod was obtained from F. J. Darnell.1 The hardness of this material varied between 52 and 64 Bhn, indicative of its high purity. Single-crystal specimens were cut out from a few large grains, elongated predominantly along <1120>. Resistance measurements were taken with specimens immersed in liquid nitrogen, solid CO,, and acetone, and at ice point, and then recorded continuously between room temperature and 1200" to 1250°C, throughout at least one full heating and cooling cycle at a rate of l° to 3°C per min. Four probe measurements were taken using spot-welded Pt wire 0.003 in. in diam as potential terminals, and the electromotive force drop was determined poten-tiometrically. A standard resistance, in series with the specimen, served to determine the dc current (generally about 80 ma) in the circuit. In order to eliminate spurious thermal electromotive forces, the circuit polarity was automatically reversed at 5-min intervals, and the mean of the two adjacent readings taken as the true electromotive force value. The discrepancy between the readings at reversed polarities was generally of the order of a few µ v, as all the spot-welded joints were contained within a volume of some 5 mm cube. The relative resistance (R T/R 273o) variation with temperature is tabulated below, and shown in Fig. 1, as measured during the first heating run. The discontinuous drop in resistance, corresponding to the a — ß transformation, started for both initial orientations at 1170°K; i.e., some 15°K above the accepted value of 882°C (1155°K). Judging by the temperature ranse of transformation—some 30°K for the single crystal and 20°K for the polycrystal-line specimen—this difference is believed caused by the solution of the oxygen present initially on the surface of the specimens. The general trend of the resistance vs temperature shown in Fi,;. 1 is in qualitative agreement with that previously reported for polycrystalline titanium metal. 2,3 Significant anisotropy is, however, indicated by the crossing over of the curves for <1120> and <0001> orientations at 273°, 650°, and 1000°K. This difference is most startlingly shown in Fig. 2, where instantaneous temperature coefficients (l/R273 x dR /dT) are plotted for both the first heat-

Jan 1, 1962

By N. A. Stockett

Southeast Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. Tons World production................. 2,000,000 United States Production .........- 460,000 Southeast Missouri production..... 142,000 The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country&apos;s production. The largest previous year&apos;s in in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averaging over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. I, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,980,000 short tons of pig lead. • About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of st. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in st.Francois county, Prospecting In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jack-hamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling—100-ft. centers of holes, and sometimes less—is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more. To date, geophysical and other methods of prospecting, apart from diamond and Mining Practices of the St. Joseph Lead Company in Southeast Missouri

Jan 1, 1943

By N. A. Stockett

Southeast Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. Tons World production................. 2,000,000 United States Production .........- 460,000 Southeast Missouri production..... 142,000 The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country&apos;s production. The largest previous year&apos;s in in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averaging over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. I, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,980,000 short tons of pig lead. • About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of st. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in st.Francois county, Prospecting In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jack-hamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling—100-ft. centers of holes, and sometimes less—is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more. To date, geophysical and other methods of prospecting, apart from diamond and Mining Practices of the St. Joseph Lead Company in Southeast Missouri

Jan 1, 1943

By H. W. Russell, Paul D. MILLER

IT is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranular corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels have been ably discussed by Bain and co-workers1-3 and by other investigators.4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a. mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measurements, measurement of the degree of cracking produced on bending over a mandrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A-10 11 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. EXPERIMENTAL METHOD A small area of the steel under test is subjected to an anodic treatment in a cell that can be clamped onto a sample or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8-in. diameter. The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

By W. C. Clarke

An empirical study of the nature of the embrittle-ment which occurs in martensitic and semiaustenitic precipitation hardening stainless steels upon exposure at temperatures of from about 550" to 875°F has been undertaken. This work was aimed at determining cazusation and means of controlling this phenomenon. A commercial copper bearing precipitation hardening alloy was used as a basic material for study. The effect of heat treatment variables was studied as was the effect of variations in analysis. It is concluded from the evidence that martensitic and semiaustenitic precipitation hardening stainless steels are subject to 885°F ernbrittlement similar to that observed in the straight chromium stainless steels. A characteristic of precipitation hardening stainless steels which has limited their use in certain applications is that they embrittle when held at temperatures in the range of from about 550" to 900°F. This is true to a more or less degree in all currently available alloys, either the basically martensitic type or the semiaustenitic type. The rate of embrittlement varies markedly with exposure temperature, being low at 550" to 600°F and in-creasing as the temperature increases. In spite of this embrittlement, these alloys with their unique combination of high mechanical strength, reasonable toughness, and good corrosion resistance are used in many hundreds of applications. Nevertheless, there are potential applications where the embrittle-ment described is a limiting factor. The purpose of this investigation was to study the embrittlement of these alloys and to find a way to control or eliminate it. GUIDELINES USED IN PRESENT WORK The work reported in this paper is based on a study of 17-4 PH*, a very widely used alloy. It has been used *Trademark of Armco Steel Corp., licensor. in pressurized water and boiling water atomic reactors operating at about 550°F for a number of years. As the life of such equipment is extended or operating temperatures are raised, the possibility of embrit-tlement becomes of increasing concern to materials engineers. Much investigation work was done with respect to the use of 17-4 PH at 550°F. K. C. Antony&apos; states "Such estimation" (of an activation energy for the diffusion of chromium in iron) "would indicate W. C. CLARKE, Jr. is Senior Research Engineer, Advanced Materials Division, Armco Steel Corp., Baltimore. Md. This manuscript is based on a talk presented at the symposium on New Developments in Stainless Steel, sponsored by the IMD Corrosion Resistant Metals Committee, Detroit, Mich., October 14-15, 1968. significant secondary aging is improbable at temperatures less than 700°F within normal component service life". This statement is modified however by the recognition of the accelerating tendencies of applied stress and internal stress as well as the possible effect of irradiation. In this investigation of 17-4 PH, the H 1100 (1900°F-1 hr oil quench or air cool + 1100°F-4 hr-air cool) condition was used, partly because this condition is normally used in atomic reactors. As shown later, the precipitation hardening temperature has no real bearing on the rate of embrittlement. An exposure temperature of 800°F was selected since embrittlement at 800°F is rapid, permitting development of relative data in time periods of 400 to 500 hr. For those not familiar, a nominal present day analysis of 17-4 PH is: C Mn P S SiCrNiCuCbN 0.04 0.30 0.015 0.015 0.60 16.00 4.30 3.25 0.23 0.030 TYPICAL BEHAVIOR OF 17-4 PH Figs. 1 and 2 show the behavior of a commercial heat of 17-4 PH under the conditions defined. Characteristically, 800°F exposure causes a rapid drop in Charpy V-notch impact strength. Tensile and yield strengths gradually increase and a gradual loss of elongation and reduction of area occur, accompanied by an increase in hardness. Notched tensile strength increases to 125 hr exposure and then sharply decreases after exposure for 500 hr. The notched vs un-notched tensile ratio remains virtually constant to exposure for 125 hr (1.67 to 1.56) but drops to 1.15 after 500 hr. Tensile ductility is not alarmingly affected even after much longer exposure times than these. For example, samples aged at 1100°F for 1 hr exposed at 800°F for 4000 hr showed a drop in elonga-tion of from 13 to 11 pct and in reduction of area of from 58 to 37 pct. Notched impact is the property SmIgth KSI 3JJ[/__________^UTS-Nrteh 260 ;/- 240 —^ 200 UTS-Smooth________._, o ioo mo Sob" m Too Hours Exposure Fig. 1—Effect of exposure at 800°F for various times on notched tensile strength and smooth tensile and 0.2 pct yield strength of 17-4 PH in the H 1100 condition.

Jan 1, 1970

By R. L. Bell, T. G. Langdon

A technique was developed- for determining the grain strain, and hence the grain boundary sliding contribution, occurring during the high- temperature creep of a magnesium alloy, from the distortion of a grid photographically printed on the specimen surface. The results were compared with those obtained from measurements of grain shape, both at the surface and interrwlly, and it was concluded that the grain shape technique may substantially underestimate the grain strain and overestimate the sliding contribution due to the tendency for migration to spheroidize the grains. ALTHOUGH a considerable volume of work has been published on the role of grain boundary sliding in high-temperature creep, many of the estimates of Egb (the contribution of grain boundary sliding to the total strain) have been in error due to the use of incorrect formulas or inadequate averaging procedures.&apos; One of the most easy and convenient measurements from which to compute Egb is that of v, the step normal to the surface where a grain boundary is incident. Unfortunately, this parameter is also the one associated with the treatest number of pitfalls. Values of v have been used to calculate Egb from the equation: egb =knrVr [1] where k is a geometrical averaging factor, n is the number of grains per unit length before deformation, v is the average value of v, and the subscript ,r denotes the procedure of averaging along a number of randomly directed lines. If the dependence of sliding on stress were assumed, it would be possible, in principle, to calculate k from the known distribution of angles between boundaries and the surface. This in itself is difficult because the distribution depends on the history of the surface,&apos; but the problem is even further complicated by the fact that v depends on other factors such as the unbalanced pressure from subsurface grains.3 However, the great simplicity of the measurement procedure for v makes it highly desirable that this problem of k determination should be overcome. In the present experiments, this was achieved by the use of an indirect empirical method in which the grain strain, eg, at the surface was determined by the use of a photographically printed grid. The assumption here is that the total strain, et, is simply the sum of that due to grain boundary sliding, egb, and that due to slip or other processes within the grains, eg. SO that: Et = Eg + Egb [2] Thus k is given by: In practice, it is customary to indicate the importance of sliding by expressing it as a percentage of the total creep strain; this quantity is termed y (= 100Egb/Et). The determination of Eg from a printed grid within the grains avoids the difficulties due to boundary migration which should be considered when the grain strain is calculated from measurements of the average grain shape before and after deformation. As first pointed out by Rachinger,4,5 however, this latter technique has the particular advantage that it can also be applied in the interior of a polycrystal. Recently, several workers have produced evidence on a variety of materials6-&apos;&apos; to support the observation, first made by Rachinger on aluminum,4,5 that 7 can be very high, 70 to 100 pct, in the interior, even when the surface value, determined from boundary offsets, is very much lower.10&apos;11 Although there have been criticisms both of the shortcomings of the grain shape technique&apos;&apos; and of the different procedures used to determine y at the surface,&apos; it seemed important to check whether measurements of sliding by grain shape gave values of y which were truly representative of the material. In the present experiments, grain shape measurements were therefore made both at the surface and in the interior for comparison with one another and with the independent measurements of grain strain using the surface grid technique. EXPERIMENTAL TECHNIQUES The material used in this investigation was Magnox AL80, a Mg-0.78 wt pct A1 alloy supplied by Magnesium Elektron Ltd., Manchester. Tensile specimens, about 7 cm in length, were prepared from a 1.27-cm-diam rod, with two parallel longitudinal flat faces each approximately 3 cm in length. The specimens were annealed for 2 hr in an oxygen-free capsule, at temperatures in the range 430° to 540°C, to give varying grain sizes, and, prior to testing, the grain size of each was carefully determined using the linear intercept method. This revealed that the grains were elongated -0.5 to 5 pct in the longitudinal direction. Testing was carried out in Dennison Model T47E machines under constant load at temperatures in the range 150" to 300°C. At temperatures of 200°C and below, tests were conducted in air with the polished flat faces coated with a thin film of silicone oil to prevent oxidation; at higher temperatures, an argon atmosphere was used. To determine v,, each test was interrupted at regular increments of strain and the specimen removed from the machine. At the lower strains, when v, was less than about 1 pm, measurements were taken on a Zeiss Linnik interference microscope;

Jan 1, 1969

By T. Federighi, S. Ceresara, C. Panseri

The results of an exploratory investigation by means of resistivity measurements at -195ºC, on the aging characteristics of a set of Al-Mg alloys with a maximum content of 7 pct Mg, are reported. Whereas for dilute alloys (Mg < 1.5 pct) only a decrease in resistivity is observed at about 100°C (due to the elimination of quenched-in vacancies), for more concentrated alloys such a decrease is preceded by an increase in resistivity in the range between -60ºand +40°C. Following some previous suggestions, this increase is considered as good evidence for clustering of solute atoms @reprecipi-tation process). From the analysis of the results it appears that, although the process is substantially similar to that observed in other Al-rich alloys, it is characterized by a strong interaction between vacancies and zones. THE process of formation of Guinier-Preston zones, i.e., preprecipitation,1&apos;2 which occurs during the aging at about room temperature in many supersaturated aluminum-rich alloys, has been extensively investigated in the past few years by several workers.2,3 owever, a very interesting question arises when the case of Al-Mg alloys is considered: although it is very easy to supersaturate Al-Mg alloys, just in the same way as for many other aluminum alloys showing preprecipitation, only very little experimental evidence was available until a short time ago in the literature supporting the existence of "natural" aging in supersaturated Al-Mg alloys (see, for example, Refs. 4 to 6). On the other hand, as is well known, the X-ray method is not useful in this case because the X-ray scattering factors of magnesium and aluminum atoms are about the same. Recently, however, Cordier and Detert7 have stressed that during the aging at about room temperature of a supersaturated Al-Mg 10 pct alloy it is possible to detect an increase in resistivity; since, as is well known, such an increase is observed also in most alloys showing preprecipitation, the above authors have interpreted their results as evidence for the formation of magnesium-rich clusters (or Guinier-Preston zones) during the aging. In the course of or ientative investigations on preprecipitation in several aluminum-rich alloys, we also could detect a similar phenomenon in more dilute Al-Mg alloys, see Instituto Sperimentale Metalli Leggeri, Annual Report, 1959, and also Ref. 8. Since the details of our observations, although of a preliminary nature, differ from those of Cordier and Detert and allow one to draw a more advanced picture of the preprecipitation process in Al-Mg alloys, we have thought it useful to report our results in this paper and to comment on them briefly.

Jan 1, 1963

By J. C. Fisher, J. H. Hollomon, David Turnbull

Understanding of the diffusion problem has recently been furthered by the analysis of Birchenall and Meh1.l They pursued the problem of the variation of the diffusion coefficient with composition for non-ideal solid solutions. Their analysis follows the tradition of Wagner,l Jost, Dehlinger, and Darken & who assumed the net flux of diffusing material to be proportional to the gradient of a quantity related to free energy. The basic assumption in Birchenall and Mehl&apos;s formulation of the problem is that the net flux of diffusing material is proportional to a thermodynamic activity gradient. To estimate the applicability of the derived relations, they corrected the diffusion coefficients of carbon in austenite by utilizing Smith&apos;s6 activity data for carbon, and the diffusion coefficients for zinc in copper with activity data computed from the vapor pressure measurements of Har-greaves.&apos; The corrected coefficients for carbon were virtually independent of carbon concentration. For the diffusion of zinc in copper a moderate variation of diffusion coefficient with concentration remained after the correction. The problem of diffusion can be formulated in another way than that used by Birchenall and Mehl. The method is that of chemical rate theory and has been used by Eyring and his coworkers8,9 as well as by Eyring and Zwolinskilo in a discussion to Birchenall and Mehl&apos;s paper. As yet the method has not been applied to substitu-tional solid solutions. On the basis of their assumptions, Eyring and Zwolinski derived a relation between the diffusion coefficient and activity that is identical with that of Dehlinger and Darken but which does not correct for the variation of the diffusion coefficient with concentration as well as does the relation derived by Birchenall and Mehl. It was thought that the theory of diffusion would be more complete if the inconsistency between the two analyses could be rationalized and if diffusion in substitu-tional alloys were analyzed on the basis of the concepts of the chemical rate theory. Chemical Rate Theory According to the theory of absolute reaction ratess the reaction +..... +X, Eq I is viewed as taking place in two steps. First the reactants A1, A², . . . A; combine to form an activated complex M with which they are in equilibrium: A1 + A1+ . . . + A=M. Eq 2 Second the activated complex decomposes to give the products XI, XZ, . . . Xi: M?X, + X²+ . . . +Xi Eq g It has been showns that the number of activated complexes decomposing per unit volume per unit time is given by the expressiont kT -h CM † The transmission coefficient has been taken as unity.

Jan 1, 1949

By David Turnbull, J. H. Hollomon, J. C. Fisher

Understanding of the diffusion problem has recently been furthered by the analysis of Birchenall and Meh1.l They pursued the problem of the variation of the diffusion coefficient with composition for non-ideal solid solutions. Their analysis follows the tradition of Wagner,l Jost, Dehlinger, and Darken & who assumed the net flux of diffusing material to be proportional to the gradient of a quantity related to free energy. The basic assumption in Birchenall and Mehl&apos;s formulation of the problem is that the net flux of diffusing material is proportional to a thermodynamic activity gradient. To estimate the applicability of the derived relations, they corrected the diffusion coefficients of carbon in austenite by utilizing Smith&apos;s6 activity data for carbon, and the diffusion coefficients for zinc in copper with activity data computed from the vapor pressure measurements of Har-greaves.&apos; The corrected coefficients for carbon were virtually independent of carbon concentration. For the diffusion of zinc in copper a moderate variation of diffusion coefficient with concentration remained after the correction. The problem of diffusion can be formulated in another way than that used by Birchenall and Mehl. The method is that of chemical rate theory and has been used by Eyring and his coworkers8,9 as well as by Eyring and Zwolinskilo in a discussion to Birchenall and Mehl&apos;s paper. As yet the method has not been applied to substitu-tional solid solutions. On the basis of their assumptions, Eyring and Zwolinski derived a relation between the diffusion coefficient and activity that is identical with that of Dehlinger and Darken but which does not correct for the variation of the diffusion coefficient with concentration as well as does the relation derived by Birchenall and Mehl. It was thought that the theory of diffusion would be more complete if the inconsistency between the two analyses could be rationalized and if diffusion in substitu-tional alloys were analyzed on the basis of the concepts of the chemical rate theory. Chemical Rate Theory According to the theory of absolute reaction ratess the reaction +..... +X, Eq I is viewed as taking place in two steps. First the reactants A1, A², . . . A; combine to form an activated complex M with which they are in equilibrium: A1 + A1+ . . . + A=M. Eq 2 Second the activated complex decomposes to give the products XI, XZ, . . . Xi: M?X, + X²+ . . . +Xi Eq g It has been showns that the number of activated complexes decomposing per unit volume per unit time is given by the expressiont kT -h CM † The transmission coefficient has been taken as unity.

Jan 1, 1949

By H Pray, H. W. Russell, Paul D. MILLER

It is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranu-lar corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels has been ably discussed by Bain and co-workers1-3 and by other investigator4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measuremerits, measurement of the degree of cracking produced on bending over a malldrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A.-1011 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. Experimental Method A small area of the steel under test is subjected to an anodic treatment in a cell that can be &apos;lamped Onto a a Or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring Or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8- diameter&apos; The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941