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By T. D. McKinley

Theory, operational characteristics, and indicated precision and accuracy of analytical methods based on vacuum extraction, equilibrium pressure, and combustion approaches are reviewed. At the present time vacuum extraction at 1400°C and the equilibrium pressure method are recommended for determination of hydrogen in titanium and titanium-rich alloys. UNTIL a few years ago the role of hydrogen in titanium was an unknown factor with regard to its effect on the physical and mechanical properties of the metal. However, following the work of Jaffee and othersa-" it is now generally acknowledged that hydrogen has a degrading effect on titanium and its alloys. The chief manifestations are a decrease in impact strength in -systems and delayed cracking in a-ß systems. Since hydrogen does have a de- grading effect on titanium it is essential to control it within tolerable limits. It then follows that procedures for quantitative estimation of hydrogen are a primary requirement for the industry. For greatest benefit these methods should be simple, rapid, and precise. In addition to having these virtues, methods must be easy to duplicate in both equipment and technique to gain widespread use. After inherent accuracy has been established, the, required precision to make a method acceptable is dependent largely on the nature of the work at hand. Ability to obtain a representative sample has a pro-

Jan 1, 1959

By Strathmore R. B. Cooke, Iwao Iwasaki, C. S. Chang

The effects of aeration on an aqueous suspension of pyrrhotite were studied and their results correlated with flotation tests using xanthates as collectors. The effects of copper activation and of pH variation were determined and possible mechanisms postulated. PYRRHOTITE has long been considered a gangue mineral to be eliminated as tailing in the treatment of various sulphide ores. However, in recent years the world-wide lack of sulphur resources has called attention to this mineral as a potential source of both sulphur and iron. Its importance as an economic mineral, however, has not been particularly emphasized. For this reason very little is known about its response to flotation, except that it can be depressed easily in alkaline circuit, by long aeration,1,2 addition of oxidizing agents,3 or by starch.' The object of this work was to study the floatabil-ity of pyrrhotite. This includes the effect of oxidation by aeration, of copper activation, and of change in pH. Preparation of the Pyrrhotite Sample: It was desirable that the highest grade of pyrrhotite obtainable be used for this experiment, since the presence of other minerals could affect the surface properties.5 However, no pyrrhotite was available as crystals, and massive deposits of hydrothermal origin commonly contain considerable amounts of chalcopyrite. Pyrrhotite concentrate was, therefore, prepared from a sulphide deposit occurring near Aitkin, Minn. The deposit is of pyrometamorphic nature consistirlg mainly of pyrrhotite and pyrite with graphite, silicates, and carbonates as gangue. The ore, already crushed through 3 mesh when received, was screened at 65 mesh and the undersize discarded. The oversize was crushed through rolls, and then stage-ground dry in an Abbe porcelain mill, the —65 mesh portion being screened out after every 15 min of grinding until all the material passed through this size. The ground product was then concentrated with a drum-type dry magnetic separator. The rougher concentrate was cleaned twice and then demagnetized. The final product was split in a Jones splitter and stored in air-tight bottles. Microscopic examination of the concentrate showed that it was relatively clean and free of pyrite, locked particles, and gangue. By means of the krypton gas adsorption method," the specific surface was determined to be 3000 cm2 per g. The chemical and screen analyses of the final concentrate are given in Tables I and II respectively. It is a well-recognized fact that the oxidation of some sulphide ores during stockpiling, grinding, and conditioning affects their flotation behavior. The problem of oxidation may become serious in the case of pyrrhotite, since this is known to be more easily oxidized than many other sulphides. To ascertain the extent of oxidation, an experiment was carried out by aerating an aqueous suspension of pyrrhotite with air, oxygen, and nitrogen as follows. A 300-g sample of pyrrhotite in 2700 ml of water was agitated and simultaneously aerated in a Fager-gren-type laboratory flotation machine. A Precision wet test meter was connected to the air inlet valve, the flow rate of the gas being kept constant at 0.3 cu ft per min throughout the experiment. Samples of approximately 30 ml each were taken from the cell at 0, 4, 10, 20, 35, 60, and 90 min. After the pH was taken, each sample was filtered and the filtrate was analyzed for total iron and sulphur. The iron was determined colorimetrically by the thioglycolate method using a green filter.' The filtrate was oxidized with bromine to convert all of the soluble sulphur compounds into sulphate and this was determined with a Parr turbidimeter." When aeration tests were made in alkaline circuit, calcium hydroxide or sodium hydroxide was added at regular intervals to maintain a constant pH. A similar procedure was followed in an experiment to determine the abstraction of copper. ion by pyrrhotite. In this case various quantities of cupric chloride were added. The filtrate from each sample taken was analyzed for copper, total iron, and sulphur. The carbamate method with a green filter was used for the copper analysis,' since this method could tolerate a considerable amount of iron in the solution. A pneumatic cell, made from a 350-ml fritted glass Buechner funnel, was used for this experiment. The detail of the assemblage has been described elsewhere." In the present work a stainless steel baffle was inserted in the cell. This baffle overcame the tendency for the coarse pyrrhotite particles to be swirled around the wall of the cell and thus fail to collect in the froth. A 50-g sample of pyrrhotite was added to the cell which contained 260 ml of water. When pretreat-ment of the sample was desired, reagents, such as activator and pH regulator, were then added and the pulp was conditioned for a specified conditioning time. Prior to the addition of the collector approximately 15 ml of the solution were removed for pH measurement and for iron and sulphur analyses. Copper when used as activator was also determined. Collector and frother were then added and the pulp was conditioned for an additional 2 min. Air was admitted to the cell and the froth removed. The separation required from 4 to 6 min, depending on the characteristics of the froth. The float and non-float products were filtered, dried, weighed, and assayed for iron.

Jan 1, 1955

By G. R. Gohn, S. M. Arnold

The results of stress-corrosion tests upon several non-ferrous sheet metals are presented in this paper. The metals include tough pitch copper, five binary brasses, two leaded brasses, one copper-silicon alloy, two tin bronzes, and two nickel-silver alloys. The tests indicate that for most of these sheet metals, externally applied bending stresses below the yield point (0.01 per cent offset) do not result in stress-corrosion cracking as determined by the A.S.T.M. Tentative Method of Mercurous Nitrate Test for Copper and Copper Alloys (B 154-41T).~ Only in the cases of low brass, high brass and medium leaded brass, all cold-worked 4 B & S numbers hard, was any corrosion cracking observed below the yield strength, and in all cases such failures occurred at stresses above the proportional limit for these materials. However, when some of the same materials which showed no evidence of stress-corrosion cracking at stresses below the yield strength, are stressed beyond the yield point, stress- corrosion cracking is quite apt to occur. Since experience has shown that some of these materials, particularly the brasses, are susceptible to stress-corrosion cracking under service conditions, these tests would indicate that, besides externally applied stress and corrosion, plastic deformation in addition to that resulting from the original cold working of the material is also required to produce conditions conducive to stress- corrosion cracking.

Jan 1, 1945

By E. W. Parker

THE anthracite region, from which there is produced annually about 80,000,000 tons, or approximately 15 per cent. of the total coal supply of the United States, has a combined area of a little less than 500 sq. mi. The total area occupied by the bituminous fields (including the sub-bituminous and lignite fields) is in the neighborhood of 400,000 sq. mi., so that 15 per cent. of the total output comes from this small area of only a little more than 0.1 per cent. of the coal-producing territory. of the United States. The productive anthracite area is divided into a series of basins or troughs, roughly parallel, extending. in a northeast-southwest direction through the. Counties

Jan 1, 1921

By S. Arthur Krom

(New York Meeting, February, 1912.) THE James diagonal-plane slimer is specially adapted to handle the finest slimes, but it will also handle sands as coarse as 40-mesh. The saving efficiency of this machine is due to the original construction of the deck, and to the rapid reciprocating movement imparted to it by the head-motion. The deck consists of a plurality of connected planes, having a certain fixed ratio of inclination one to another. These planes intersect each other diagonally to the stroke-line of the table and are arranged so as to give the pulp on the table a double treatment. This double concentration performed by the diagonal-plane deck produces cleaner concentrates and tailings than those obtained by the operation of two separate machines. The action of the diagonal planes settles, combines, and holds all the concentrates in one compact mass, sharply defined from the gangue, and easily cut away without loss. Many slime-concentrating machines distribute the feed-pulp for a distance of 4 or 5 ft. only, and upon a very limited settling-surface. This results in a thick, heavy deposit, from which it is impossible to stratify the values and wash, away the gangue, the resulting products being dirty concentrates, and tailings carrying high values. The diagonal-plane slimer distributes the feed-pulp for a distance of 10 ft., and upon a settling-surface having an area of 40 sq. ft.; in other words, it spreads the pulp thinly on the table, which allows the metallic values to settle through the gangue quickly, forming a bottom stratum from which the thinly-distributed overlying stratum. of gangue is easily brushed away by the feed-water without disturbing the underlying concentrates. Referring to Fig. 1, plane A is the main settling-section, of the table. The feed pulp flows gently down this plane and is

Jun 1, 1912

By R. L. Curfman

From January 1, 1965 through July 5, 1970, the very difficult potash ore body of Texasgulf Inc. near Moab, Utah was mined by conventional methods. The mine was gassy, the temperature was high and structural conditions precluded a satisfactory or economical extraction ratio due to the undulating configuration of the ore horizon. In 1966, 67, and 68, alternative mining methods were considered, among which was solution mining of the ore body. Cost studies indicated that the use of crystallizers to evaporate the large amounts of water attendant to solution mining offered no chance of economic success. In 1969 additional testwork and cost studies were carried out utilizing solar evaporation. These studies showed economic potential and justified additional investigation. As a result of these studies, Texasgulf now gathers potash solids from these solar evaporation ponds, (Fig. l), after pumping them from the underground mine as brine. The investigations were concentrated in four basic areas : (1) area evaporation rates and crystal growth habits; (2) underground solution tests including heat transfer rates; (3) accelerated evaporation tests to provide material for metallurgical testing, and (4) tests of evaporation pond lining materials and application techniques, along with area surveys to ascertain if sufficient earth was available in the near vicinity to con-

Jan 1, 1974

By Walter W. Bradley

Mining by hydraulic process of the important gold-bearing gravels of the Sacramento Valley in the basins of the Yuba, Bear and American rivers began in 1853, and continued at an ever-increasing rate for 30 years. In its most active days it reached an annual production of $15,000,000, and averaged $10,000,000 per year over the 30 years. During that period no provisions were made to prevent the debris from being discharged into the water courses, and ultimately large quantities of silt, sand and gravel were washed down to the lower valleys; filling channels, causing overflow of agricultural lands and difficulty in maintaining navigable depths in the Sacramento River. Agitation and suits filed because of these damages finally resulted in the injunction decision of Judge L. B. Sawyer,' in the U.S. Circuit Court, Jan. 23, 1884, which closed down practically all hydraulic mining operations not having means to restrain their debris. In 1893 (approved March 1, 1893), Congress passed the act introduced by Representative Anthony Caminetti, of California, creating the California Debris Commission, composed of three officers assigned from the Engineer Corps of the U.S. Army, and since that time it has been legal and possible within the drainage systems of Sacramento and San Joaquin rivers to conduct hydraulic mining of gold-bearing gravels behind dams built under this commission's permit and supervision. In the watersheds of the Trinity and Klamath rivers, which flow directly to the Pacific Ocean and do not affect navigation or agriculture, operating permits from the California Debris Commission are not required. There is a measure of restriction there, however, through what is known as the Trinity and Klamath River Fish and Game District. Chap. 215, Stat. 1931, in order to secure relatively clear water for the fishing season, provides that between July 15 and October 15 each year there must not be discharged into these rivers debris that will cause a turbidity greater than a content of 50 parts per million in the

Jan 1, 1937

By B. Russell, J. R. Tuffley

The stability regions of the normal sulfate and the various basic sulfates of lead in 02-SO2 and PhS-SO2 gas atmospheres were calculated from available thermodynamic data over the temperature range 600o to 1200oC. Roasting experiments were carried out on samples of synthetic lead sulfide at various temperatures and for various roasting times. Compounds in the oxidized surface layers were identified by X-my techniques. The order in which the various reactions occurred was determined by considering the experimental results in conjunction with the thermodynamic calculations. The results of these investigations were applied to the sintering of lead sulfide concentrates, and the extent to which each of the various reactions occurred in a sinter bed was determined. PRODUCTS which may be formed during the roasting of PbS are PbS04, PbSO4. PbO, PbSO4 . 2PbO, PbSO4 . 4PbO, PbO, and Pb.1, 2 The formation of some sulfates has been studied by a number of investigators3-' whose experiments have mostly been confined to the temperature range between 500" and 850°C. Culver, Gray, and spooner3 were able to isolate the reactions which formed PbSO4 and PbSO4. PbO by carefully controlling the compositions of the roasting gases. The kinetics of these reactions were studied within the temperature range 673" to 807°C. Gardner4 and Merrick5 also studied the kinetics of oxidation of PbS. Gardner disregarded the existence of basic sulfates and, as a result, misinterpreted some of his experimental data. Merrick recognized that most of the products of oxidation were mixtures of basic sulfates, but was unable to identify the individual components. Hoschek6 oxidized PbS in air at temperatures up to 800°C. The products were analyzed after roasting had proceeded for some minutes, but no attempt was made to follow the reactions in the initial stages. Consequently, no roasting mechanism was derived. He also showed that PbSO4 and PbSO4 - 4PbO decomposed slowly in air at temperatures in the region of 800°C. The stability regions of sulfates in the temperature range 500" to 850°C have been only partially determined, while practically no information is available for higher temperatures. In the lead sintering process, PbS concentrates are roasted at temperatures within the range 1000o to 1200°C. In order to investigate sulfate formation, it is necessary to determine the effects of temperature and gas composition upon the various oxidation reactions and upon the regions of stability of the various lead sulfates. Kellogg and Basu2 introduced an equilibrium diagram similar to those in Figs. 1 to 3 which provides a convenient medium for represent-

Jan 1, 1964

By Eugene R. Rice

(Canal Zone Meeting, November, 1910.) THERE are many methods for determining the meridian, but all of those in common use involve at least two separate observations, one for latitude and one for azimuth. Such observations made upon a south star at any hour are open to the objection of possible inaccuracy due to ignorance of the absolute refraction, and also to slow change in the altitude of the star when near the meridian. The method of observing a circumpolar star at elongation, besides requiring a separate observation for latitude, is open to the serious objection that clouds may obscure the star at the critical moment. Moreover, a tedious wait for the star to come to elongation is sometimes necessary. Many of us can recall long, cold, weary vigils, waiting for Polaris to reach elongation. For observing a circumpolar star at any hour, not only the latitude, but also the true time, must be known. This it is practically impossible to obtain, except in regions reached by the telegraph, and usually then one has to know the longitude also, in order to reduce "standard time" to "local time." The results obtained by this method, when the star is at culmination, are not very good, unless the true local time is absolutely known. The methods of obtaining the meridian from the sun, by means of a solar attachment, or by direct observation, while good, are not absolute, by reason of refraction, change in declination of the sun, and small change in vertical angle, when the sun is near the meridian. For these two methods, latitude, time, and approximate longitude have to be known. In the method here described, only one observation is needed, and from it azimuth, latitude, and sidereal time are computed. In other words, one can observe a circumpolar star-Polaris

Nov 1, 1910

By C. Scala, M. Gondouin

Published laboratory data have established that very significant streaming potentials can exist across mud cakes subjected to pressure differentials such as exist between a mud column and formation fluids. Since shale is similar in kind and in properties to a well-formed mud cake, it appeared possible that streaming potentials might also arise across shales. A practical consequence would be that the streaming potential contribution to the SP would be smaller than might otherwise be assumed since the SP is measured with respect to the "shale bare line". The resultant contribution would be the difference between the streaming potential across the shale and that across the mud cake. In order to investigate this possibility, a laboratory apparatus was devised for measuring streaming potentials under pressure conditions normally encountered in wells. Reported data on streaming potentids across mud cakes were verified. More important, appreciable streaming potentials were found across shale samples. As in the case of mud cakes, the shale potentials varied with the concentration and nature of the impregnating electrolyte. Dependence on pressure was In a different rela-tion than that for mud cakes, possibly because of the lower compressibility of shales. The differences in streaming potentials between the shales md mud cakes were generally small, although they might vary considerably in practice depending on the relative electro-kinetic properties of the particular shale-mud cuke combination. A "poorly eflective" shale with a "very eflec-tive mud cake" would produce the largest negative addition to the electrochemical component of the SP. Results of field experiments with pressurized wells were considered in the light of the laboratory results. INTRODUCTION Field experiments wherein the pressure of the mud column in a borehole was varied have often indicated the presence of a streaming potential, but its magnitude was not easily predictable and its sign sometimes changed from one formation to another in the same well.' In the interpretation of SP logs from standard surveys, nevertheless, the correct value of R,, is very frequently obtained, within the limits of field accuracy, using only the simple electrochemical expression of the SP provided that proper corrections are made for bed thickness, ion activity, etc.' Accordingly, it was apparent that the streaming potential component of the SP in a borehole was considerably more complex than commonly assumed and clarification was indeed necessary The close similarity in nature and constitution of a shale to a well-compacted mud cake suggested that a streaming potential might also exist across shales as pointed out by M. P. Tixier in 1953 and as recently emphasized by Wyllie." e practical consequence would be that the streaming potential across the mud cake would be canceled, at least in part, on electrical logs since the SP is recorded with respect to the shale potential as a base line. This appeared to be a plausible explanation for many of the effects observed but no supporting data were available. In 1955 preliminary experiments at low pressures were conducted in our laboratories which supported the hypothesis of the shale streaming potential and formed the basis for later studies at borehole pressures.* EARLY LOW PRESSURE EXPERIMENTS The early experiments were conducted primarily to determine the possibility of a streaming potential across shales. The shale used was a compact type designated as No. 7 from Reagan County, Tex. (Permian). Cut samples were saturated for over one month in .2 to 2.0-N NaCl solutions. In order to eliminate all electrode polarization effects, a dynamic method was used. A transient pressure of about 1 atm was applied across

By Stephen Krickovic

AS it is commonly understood in the bituminous coal mining industry, pillaring means removal, as completely as is practical, of all pillars formed in the development of headings and rooms on first mining. The degree to which this can be accomplished, termed percent of recovery, is of course dependent generally upon the physical conditions of the bottom and the overburden, the system of min-

Jan 1, 1956

By E. L. Tucker

IN THE metallurgy of precious metals, it has been standard practice for years to use cyanogen compounds, so it was but natural that early investigators in the field of flotation should consider these compounds as possible flotation reagents. In Australian Patent 9508, of 1913, alkali cyanides were described as suitable reagents for the separation of heavy sulfide minerals, the reagents being employed either in an alka-line or neutral circuit. In U. S. Patent 1236501, of 1917, to John M. Tibbet, the use of cyanide in conjunction with soda ash or lime is described. One of the claims of this patent reads, "An improvement in the cyanide process for the treatment of ores comprising, mixing the ore with cyanide solution and oil and alkali: emulsifying the oil in the presence of the ore, the alkali and the cyanide solution, floating a portion of the values in the pulp by producing gas bubbles in the mixture-and removing the values floated." More recently, Sheridan and Griswold, in U. S. Patents 1421585 and 1427235, describe a somewhat similar process and have, successfully introduced it in. the mill of the Timber Butte Milling Co. U. S. Patent 1429544, of 1922, to Stevens, describes the use of double cyanides of copper, zinc, and lead. The success of cyanide as a reagent in the differential flotation of lead and zinc sulfides in highly complex ores is proof that these patents have a solid foundation.. Although the technique of their application to particular ores has been worked out in many cases, no one, so far as is known, has attempted to describe the nature of the action of the cyanide or to determine the ideal conditions for its, application. It was the purpose of the present investigation to gather information on these points. Naturally this would have been an exceedingly ambitious.

Jan 8, 1925

By Edward D. Thimons, Richard J. Kline

Converting the energy of falling water into useful work is a well developed engineering concept. Much of the electric power consumed in the United States is generated in this manner. It is easy to conceive that the water which flows down long vertical pipelines into deep nines could be utilized in a similar manner by allowing it to operate a turbine at the bottom of the pipelines. The mines in the United States are continually descending to greater depths in search of mineable deposits. Large quantities of water are carried down long vertical pipelines in order to be used for dust suppression, motor cooling, and refrigeration. Pumping the used water back to the surface is also required. The electrical costs associated with mining are also constantly escalating due to both increased demand and rising kilowatt hour costs. To help deal with this problem, the United States Bureau of Mines (USBM) has awarded a contract to Foster-Miller, Inc. of Waltham, MA, to investigate, evaluate, and demonstrate commercially available means of energy recovery for the deep mining industry. In other words, it demonstrates an efficient system for converting the energy of water flowing down vertical pipelines into useful mechanical or electrical energy.

Jan 1, 1982

By Robert A. Cook

In the increasing struggle to cheapen the cost of our iron and steel products a great deal of attention lias been given to economies in the manufacture of coke; and while but little lias been accomplished in this direction in the United States, the narrow margin between cost and market-price, which has obtained here for the past few years of continuing manufactur ing depression, has brought the coke-maker face to face with the problem, how to save, and benefit by it, the hitherto waste products of distillation. I These may be summed up under three heads, generally rank ing, in value, in the following order: 1. Ammonia salts.. 2. Oil- or tar-products. 3. Gas. There are cases in which the last may assume the position of greatest importance. The greatest obstacle encountered by the American coke maker, on investigating the subject, has been the apparent necessity of discarding his existing plant of bee-hive ovens, and erecting an entirely new and very expensive system of retort ovens, against the product of which Be has probably been prejudiced from his earliest knowledge of the subject. The object of this paper is to bring prominently before our coke-experts a brief history of the development at Sheffield, England, of a most successful system of the utilization of by products in connection with all already existing plant of bee hive ovens. This system has now been in satisfactory operation for about five years, and is applied to a series of blocks of ovens, comprising-about 140- in all At this plant, belonging to the well-known firm of Newton,

Jan 1, 1897

By W. C. Hagel, J. H. Westbrook

Usittg a sectioning technique with Agl10 as the tracer, the diffusion of silver in silver-excess (45.8 at. pct Mg), near-stoichiometric (49.8 at. pct Mg), and magnesium-excess (52.0 at. pct Mg) cylinders of CsCl-type AgMg was determined from 500" to 700°C. Diffusion coefficients conform to the expression D = Do exp (-q/RT) where the respective Do values are 1.53, 0.280, and 0.134 sq cm sec-I and the Q values are 41.3, 40.6, and 38.0 kcal g-atom-'. Lnttice-parameter and density measurements were performed on a more numerous assortment and wider range of compositions. Substitutional defects were found on both sides of stoichiometry. Activation energies for other rate processes in these alloys show related trends with changing composition, although silver may not be the rate-detemining species. KNOWLEDGE of diffusion coefficients is necessary for a quantitative understanding of the many rate processes (e.g., grain growth, precipitation, sintering, oxidation, or mechanical deformation) occurring in solids. Although these data are available for most metals and common alloys, they are quite limited for intermetallic compounds—a group of materials whose unique physical and mechanical properties are presently attracting great interest. From a fundamental viewpoint, diffusion in intermetallic compounds also offers several engaging aspects owing to: their ordering, the possibility of introducing large, stable concentrations of lattice defects, and the variety of bonding types and crystal structures which can be found. In the case of CsC1-type compounds, some previous work has been directed at examining the role of vacancy defects by changing their concentration compositionally. The diffusion of Co60 was measured in 0 NiAl1- and in P COA., Except for the results of Smoluchowski and Burgess, isothermal diffusion coefficients were found to pass through a minimum at the stoichiometric composi- they decreased sharply on what was reported by Bradley and co-wrkers' to be the vacancy-rich (aluminum excess) side of stoichiometry. This investigation of the diffusion of Agl110 in AgMg was undertaken both as an adjunct to a concurrent study of its deformation behavior and for the purpose of obtaining information on the influence of lattice defects and temperature on diffusion in another CsC1-type intermetallic compound. Bcc AgMg remains ordered up to and melts congruently at 820°C. Solubility limits at 300°C are about 41 at. pct Mg and 53 at. pct Mg. It is one of the Hume-Rothery electron compounds with a 3/2 electron-atom ratio. Previous investigations of its properties include hardress,' tenile,'-' electrical reistivity, and thermodyna-mic1',14 studies. Indications of a high bonding strength may be found in the large heat of mixing1' and in the 6-pct vol contraction on compound formaticp, as calculated using atomic radii of l.40 and l.55a for Ag and Mg. EXPERIMENTAL PROCEDURE Alloys were prepared by the induction melting of selected fine silver (99.95) and low-iron magnesium (99.95) in magnesia crucibles under 1 atm of A. Supplied by the Handy and Harmon and Dow Chemical Cos., respectivelv. Melts were poured under argon into graphite molds providing 1 1/8-in.-diarn. by 4-in.-long ingots. These were homogenized in evacuated and argon-filled fused-silica capsules by heating for 16 hr at 750'. Three 1 in.-diam. by 3/4-in.-long cylinders were machined from the mid-portion of each ingot for diffusion measurements. Three alloys, analyzing 45.8, 49.8, and 52.0 at. pct Mg were taken as representing the extremes of interest, with 49.8 at. pct Mg being very close to the stoichiometric composition of 50.0 at. pct Mg.

Jan 1, 1962

By H. H. Klepfer, K. J. Gill, P. Chiotti

SOME observations relative to the U-Zn system have been made by other investigators. Chipman1 and Carter2 have reported the preparation of several U-Zn alloys and point out that these alloys are generally difficult to prepare. Chipman1 reported evidence for a high melting compound at about 90 atomic pct Zn and the possible existence of a eutec-tic between the compound and uranium. Raynor," in a theoretical discussion of the alloying properties of uranium, included zinc among the elements predicted to have little or no solubility in a, p, or y uranium. In the present investigation, thermal analyses, X-ray, metallographic, and vapor-pressure data were obtained to determine the phase boundaries. The relatively high zinc pressure over most of the alloys at temperatures of 900 °C and above proved troublesome and special techniques had to be employed in preparing suitable alloys. Materials and Preparation of Alloys The metals employed in this investigation were Ames Laboratory biscuit uranium containing less than 500 ppm total impurities and Bunker Hill slab zinc or Baker Analyzed reagent granulated zinc, both with a purity of 99.99+ pct. Due to the high vapor pressure of zinc and the high reactivity of both uranium and zinc with oxygen at only moderately high temperatures, alloys were prepared in closed containers which had either been evacuated or evacuated and filled with helium. High purity magnesia, magnesia containing 10 pct calcium fluoride, and tantalum proved to be suitable crucible materials. Tw-o different procedures, described below, were used to prepare alloys, the latter being the most satisfactory. The metals, uranium turnings and granulated zinc, were cleaned with dilute nitric acid, rinsed, dried, and placed immediately in a helium-fill'ed dry box. The two metals were placed' in a 10 mil Ta crucible. The charge was enclosed in the tantalum crucible by welding on a preformed tantalum cap. This assembly was enclosed inside a stainless steel (AISI 309) bomb. The bomb was made by welding a piece of stainless steel plate on each end of a stainless steel pipe. All these operations were carried out in a helium atmosphere. These assemblies were heated in a muffle furnace at temperatures between 1100" and 1200°C for 10 to 15 min or held as long as 15 to 20 hr in the 950" to 1000°C temperature range before quenching. Spectrographic and chemical analyses showed no tantalum pickup by the alloys, indicating no reaction between the alloys and the crucibles. However, some of these crucibles failed, probably due to imperfections in the welds of the stainless steel or tantalum crucibles. The second and most satisfactory method was to prepare the alloys by powder metallurgy techniques. The procedure was to press degreased and acid-etched uranium turnings with granulated zinc into 20 g compacts under 20,000-psi pressure. The compacts were placed in MgO crucibles, and sealed in evacuated Vycor or fused silica tubes. The alloys were then heated as long as two weeks at about 550°C in a muffle furnace. The pressed compacts were observed to expand by several volume percent during heating and it was necessary to make allowances for this expansion in order to avoid breaking the crucible and Vycor tube. This method was found very satisfactory for preparing alloys which were suitable for thermal analysis or vapor pressure studies. Experimental Methods and Results The phase diagram for the U-Zn system at 1 atrn pressure, shown in Fig. 1, is based primarily on vapor pressure measurements and on thermal analysis taken at temperatures below 950°C. Fig. 2 shows the U-Zn diagram at 5 atrn pressure, constructed on the basis of thermal analysis of alloys in sealed containers up to 1150°C and on the basis of metallographic, X-ray, and analytical data. The alloys sealed under vacuum were actually under their own vapor pressure and those sealed in an atmosphere of helium were under an additional pressure due to the helium. At temperatures up to 1100°C the zinc pressure is 5 atrn or less for these alloys; consequently the maximum pressure over the alloys sealed under a helium atmosphere was 10 atrn or less at temperatures up to 1100°C. Changes in pressure of this order of magnitude do not appreciably alter the position of most solid-solid or liquid-solid phase boundaries. In constructing the phase diagram for a pressure of 5 atm, the effect of pressure on all phase boundaries except those for liquid-vapor or solid-vapor regions was considered negligible.

Jan 1, 1958

By J. D. Forrester, Erich Sarapuu, T. C. Cheasley

RANKING high in the nation's wealth of natural resources, readily available liquid and gaseous hydrocarbons are nevertheless falling steadily in supply, while industrial requirements for hydro- carbon compounds are greater today than during the peak period of World War II. Theoretically, several processes will increase the future supply of liquid and gaseous fuels, but the practical application of these methods depends on two controlling factors: 1-that enough carbon- bearing material be available to warrant industrial exploitation, and 2-that the given process be physically, chemically, and economically applicable. With regard to the first factor, the Western Hemisphere is fortunately well supplied, see Table I.

Jan 9, 1954

By T. E. Davidson, C. G. Homan

This report deals with a study of the effects of extreme hydrostatic pressure on a polycrystalline material which exhibits a high degree of elastic anisotropy. Metallographically prepared polycrystalline bismuth samples were subjected to pressure levels up to 20,000 atm in a piston type gas-liquid system. The observed structural changes consisted of deformation localized along the grain boundaries, which appears to be a boundary migration phenomena, and widespread slip and cross slip. Subsequent deformation is progressive with increased pressure, and is substantially different in type from the deformation characteristic of uniaxial compression. A large amount of interest has been shown in recent years in the effects of extreme pressure on metals. In this connection, many investigations into the effects of pressure on physical and mechanical properties and reactions have been undertaken. Due primarily to the experimental difficulties involved, there has not been a great deal of study of the structural changes resulting from exposure of metals to extreme pressure. It has been difficult, for instance, to produce a true hydrostatic stress state in many of the extreme pressure devices used, and also to directly examine specimens metallographically before and after pressurization. The results of a preliminary investigation into one of the effects of extreme pressure, and its associated true hydrostatic stress state, on the structure of metals are discussed herein. Metals exhibit varied degrees of anisotropy in their physical and mechanical properties. Significant among the anisotropic properties is the modulus of elasticity, which varies by a factor of as much as three in some of the fcc metals, and by much larger factors in some of the less symmetrical elements. As a result of the variation of the modulus of elasticity with crystallographic direction, shear stresses will be induced in polycrystalline samples under true hydrostatic compression. Depending on several factors, these shear stresses could become of suffi- cient magnitude to cause localized plastic deformation. Presented herein are some of the structural changes observed in polycrystalline bismuth as a result of exposure to hydrostatic pressures of up to 20,000 atm. Although several other materials in both bicrystal and polycrystalline form are also currently under investigation, bismuth was chosen initially, due to its low symmetry and moderately high degree of anisotropy in the elastic properties. The fact that extreme hydrostatic pressure can induce structural changes in some elements in the polycrystalline state is of importance in itself. However, it may also be a factor in many of the other extreme pressure effects. For instance, this localized plastic deformation could substantially lower the recrystallization temperature, thus altering the effects of extreme pressure on this phenomenon. Also, as commented on by ridgman,' the hysteresis in the polymorphic transition of polycrystalline bismuth under extreme pressures could possibly be attributed to structural changes brought about by unequal compressibility. Therefore, to accurately determine the true effects of extreme pressure on metallic substances, one first must determine if any structural changes due to hydrostatic compression are also simultaneously occurring. The purpose of this work has been to determine whether the shear stresses induced by hydrostatic pressure in an anisotropic polycrystalline material, such as bismuth, could reach a magnitude great enough to cause plastic deformation and to study the resultant structural changes and effects. THEORY In a metallic crystal, the elastic properties are dependent upon the crystallographic direction and plane. Depending upon the degree of anisotropy of the elastic properties and other factors, internal shear stresses of sufficient magnitude to cause localized plastic deformation may be induced in polycrystalline material by true hydrostatic compression. The following highly simplified two-dimensional model of two adjacent grains in a polycrystalline aggregate under hydrostatic pressure serves to schematically demonstrate how these shear stresses arise in an anisotropic material.

Jan 1, 1963

By H. S. Kalish, F. J. Dunkerley

INTRODUCTION AND PREVIOUS WORK THE determination of the low temperature tensile properties of tin and tin-lead alloys was initiated as part of an extensive research program on the phasial equilibria of tin binary systems below 13.2°C and the property changes associated therewith. A survey of the literature revealed that, although some room temperature tensile data were available for tin and a few tin-lead alloys, there existed no survey report of the low temperature tensile properties of these alloys. Accordingly, the tensile data for tin and a series of pure tin alloys containing from 0.01 to 50 pct lead were measured at eleven temperatures from -196 to +20°C and are presented here in survey form. In addition to the importance of these tensile data as a preliminary to certain fundamental research, this information promises also to be of commercial importance because of the 'extensive use now being made of tin-lead solders in refrigeration and gas liquefaction equipment. Occasional failures of the solders in low temperature service have been attributed by some metallurgists to low temperature mbrittlement, while others hold that failure results from the transformation of the tin-rich phase of the solder from the solid white (beta) to the powdered gray (alpha) form. From the data previously available in the literature, neither of these explanations can be completely corroborated. Cohen and van Lieshout1 have established the beta to alpha tin transformation at 13.2°C and have shown that strain accelerates the transformation. Further, they showed that although I pct lead retarded the transformation, it was not eliminated. It will be pertinent, then, to note whether the beta to alpha transformation of the tin-rich phase will occur in a short-time tensile test. Polanyi and Schmid2 studied the tensile . properties of tin single crystals at -185°C and report that tin is brittle at-this temperature. In 1946, Kostenets3 reported that pure tin was brittle at -196 and -253°C, while lead remained ductile at both these temperatures. He also studied the tensile properties of tin-lead alloys containing from 10 to 75 pct lead at -253, -196 and +17°C. The ultimate tensile strength increased more than two times in going from room temperature to -196°C and about three times that value on further cooling to -253°C. All the alloys were brittle at -6°C except those containing more than 75 pct lead. Even at -253°C, the 75 pct lead alloy retained 36 pct elonga¬tion in a 30 mm-ga. length. Creep is also an important phenomenon

Jan 1, 1948

By Henry Lloyd Smyth, J. Ralph Finlay

The most important area of the so-called Keewatin rocks of northern Minnesota is that which runs westerly from Lake Saganaga, near the national boundary, and finally disappears beneath the drift (or has not been farther traced), in the neighborhood of Vermilion Lake. With this belt we have a general acquaintance, extending back some four years. During the past year we have had the opportunity of studying in considerable detail a small part of it, embracing an area of about 12 square miles on the south and east shores of Vermilion Lake. In this paper we desire to record our observations and conclusions, which seem to us important. II.—Literature. Outside the Minnesota Geological Survey, the list of the investigators who have studied the geology of the Vermilion Lake area is not long. Whittlesey, in 1876,* mentioned the occurrence, in the area about Vermilion Lake, of rocks resembling the Canadian Laurentian. Chester,? in 1884, described the iron-ore at Vermilion Lake as occurring in connection with jasper and quartzite, intimately bedded with the country-rock, chiefly sericite schist, and standing in a nearly vertical attitude. The Vermilion iron-bearing rocks, and those of the Mesabi range, he says, are of the same age.

Jan 1, 1896