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By C. B. Daellenbach, T. D. Tiemann

The prevention of quartz flotation by chelation of activating ions with the tetrasodium salt of EDTA in oleic acid flotation was investigated using a small vacuum flotation cell. It was found that flotation of quartz could be entirely suppressed in the presence of activating ions during complete flotation of hematite. It was further shown that the concentration of activating ions liberated from Wisconsin Gogebic taconite is sufficient to float quartz in an oleic acid system. Large tonnages of low grade siliceous iron ores occur on the iron ranges of the Lake Superior district. Although the lower grade nonmagnetic types are currently not of economic importance, they constitute a large future potential source of iron and steel, and hence have been the subject for extensive research on their beneficiation. TACONITES Of particular interest to the Dept. of Minerals and Metals Engineering at the University of Wisconsin have been the low grade nonmagnetic taconites of the Wisconsin Gogebic Range. These occur as five members of the iron formation and have been described in detail elsewhere.' Essentially they consist of an intimate mixture of hematite, goethite and quartz, with minor amounts of siderite, magnetite, iron containing silicates, and manganese minerals. A typical mean analysis based on the Bureau of Mines analyses' is: SiO2-52.50%, Fe2O3-43.40%, (Fe-30.38%), A12O3-1.15%, P2O5-0.07%, Mn2O3-0.29%, CaO-0.07%, (S-0.03%), Loss on ignition-2.00%. The quartz in these ores is of a microcrystalline variety,2 and so intimately associated with the iron oxide minerals that extremely fine grinding, in the order of minus 325 mesh, is required for liberation. During grinding and subsequent flotation, the concentration of quartz activating ions in the pulp becomes sufficiently high to activate quartz which floats along with the iron minerals in the presence of oleic acid. cook3 and co-workers concluded that oxidized iron ores released appreciable quantities of quartz-activating ions in water pulps. This is shown to be true in the present investigation. As a matter of fact, application of this phenomenon, as well as the intentional addition of activating calcium ions, is made use of in the an ionic flotation of silica from the iron oxide minerals.4,5 In view of the above, it becomes almost impossible to effect a sharp separation of quartz in the oleic acid flotation of the iron oxide minerals from these taconites, even with satisfactory liberation. This fact led to the current investigation to find a means of linking the activating ions with a chelating agent. The aim was to establish basic data for the quartz-water-oleic acid system which might not only be applicable to iron ores, but also to the flotation of other siliceous ores as well. EXPERIMENTAL METHODS Vacuum Flotation Cell: The vacuum flotation used in this investigation is similar to that used by previous investigators.6,7,8 The cell consisted of a 100 ml graduated cylinder with the lip removed. Vacuum from a water aspirator was applied to the cell through a trap; suitable tubing, and a rubber stopper inserted in the top of the cell. Constant absolute pressure was maintained by means of a manometer connected to the trap with a tee. Flotation: The required amount of activating ion solution was pipetted into a beaker. This was then diluted to 99.0 ml with water having a pH below that desired for the test, or so adjusted with HC1. After addition of 1.0 ml of oleic acid solution (2.0 mg oleic acid per ml), the pH was readjusted to the desired value with NaOH, and the entire solution transferred to the cell containing 1.5 gm of quartz. After vigorously agitating the cell and its contents for 2 min, the vacuum was applied to the cell and the estimated degree of flotation observed for a 3-min period. Activating ions studied included Ca++, Mg++, Al+++, and Fe+ + + added as chloride solutions. In addition,

Jan 1, 1964

By A. W. Schlechten, R. F. Doelling

Parkes' process crusts were vacuum distilled using a shortened Pidgeon retort. Zinc was effectively removed below 800°C and recovered as a zinc sheet easily stripped from the furnace liner. Lead dasdistillationazinc required about 950°C and the resulting lead condensate tillationtended to stick to the thin metal liner. Final purity of residue is limited only by nonvolatile metals such as copper. THE successful commercial application of vacuum distillation for the removal of zinc from lead, as described by W. T. Isbell,' raises the question of whether or not a similar method can be used for other metal separations. Preliminary laboratory experiments on the vacuum distillation of Parkes' crusts by one of the authors' gave such encouraging results that it was decided to make a series of tests with large scale equipment to determine the results that might be expected in plant operation. The pilot-plant test results are reported in this paper. The great advantages of vacuum dezincing are its simplicity, the relatively low temperature of operation, and the fact that the zinc is recovered in the metallic state ready for use again in the desilveriza-tion of lead bullion. These same advantages and others would be realized from the vacuum distillation of the zinc-lead-silver crusts made in the Parkes' process. Zinc readily will distill over at temperatures of 800" to 900 °C as contrasted with the 1200°C or more used in the Faber du Faur furnace. Furthermore, the recovery of zinc as metal is practically perfect since there is no loss by oxidation or fuming. If the vacuum distillation is continued and hastened by raising the temperature to around 1000°C, the lead will distill over at an appreciable rate and deposit in a warmer zone of the condenser. This lead will contain a small amount of silver, but it can be returned to the desilverizing kettles and there is not the chance of loss that there is in disposing of the rich litharge from cupelling. The lower temperatures required will mean a saving of fuel and less wear on the equipment. One further point is that the vacuum distillation could be run on a small scale practically continuously, so as to avoid the accumulation of large amounts of silver-rich material and the need of assembling a large crew for special cupellation runs. It should be pointed out here that the final purity of the silver residue will depend on the copper or iron content of the crusts, as these and other metals with low vapor pressure will not be eliminated. The idea of treating the silver-zinc-lead crusts from the desilverization of lead bullion by vacuum distillation is not a new one, but such experiments have not been reported, as far as can be determined. In 1912, T. Turner presented a paper3 before the Institute of Metals on the vacuum distillation of brass, and a member of the audience suggested that he try his method on Parkes' crusts. In 1935, W. J. Kroll, noted for his discovery of debismuthiz-ing lead by calcium additions, published a paper' on vacuum distillation of metals and pointed out possible applications in the lead industry. Principles of Separation The successful separation of two or more metals by distillation depends upon an appreciable difference in the effective vapor pressures of the metals in the alloy to be treated. The vapor pressures of the common metals have been determined with considerable accuracy; for example, at 800°C the vapor pressures of the individual metals which are of particular interest in this paper are about .as follows: Zn, 241 mm; Pb, 0.0553 mm; and Ag, 0.0000276 mm. Unfortunately,, data are not available on the activities of the components in the ternary system Zn-Pb-Ag, but it can be estimated that on the basis of the vapor pressures of the individual metals a good separation can be made by distillation. The preliminary laboratory tests previously mentioned' supported this assumption. The pilot-plant size vacuum distilling furnace is shown in Fig. 1. It consisted of an abbreviated Pidgeon retort, 5 ft long with an ID of 8 in., heated by six silicon carbide elements placed symmetrically

Jan 1, 1952

In the January Bulletin a list was published of Societies' publications, magazines, etc., which were duplicates and were discarded at the time of-the consolidation of the libraries of the three Founder Societies. A second list published herewith includes text books which are duplicates and which will be disposed of about April 1, 1916, by the Board of Directors of the Institute through the, Library Committee.. If, meanwhile, members desire to secure some of these books, they are asked to communicate at once with the Secretary as. this is an unusual opportunity to secure books at an extremely low price. Airy, George Biddell.-Magnetism, London, 1870, Bd. Alberti, Friedrich von.-Halurgische geologic. Erster Band. Zweiter Band. Stuttgart, 1852, Bd. American Iron and Steel Association.-Ann. Rep. of the Sec'y. Statistics of American and, Foreign Iron Trades, 1877. Phila., 1877, Bd. Same, for year 1878. Phila., 1879, Bd. American. Telephone and Telegraph Co.-Ann. Rep. of Directors to Stockholders, 1911. N. Y., 1912, paper. Armagnat, H.-Induction Coils. Trans. by Otis Allen Kenyon, N. Y., 1908, Bd. Armstrong Cork Co. Insulation Dept. Nonpareil Corkboard Insulation. Pittsburgh, 1909, Bd. Associazione fra gli Industriali Metallurgici Italian.-The Metallurgic industry of Italy. Description of some of the principal works. Milan, 1911, Bd.

Jan 2, 1916

By Chas. Y. Clayton, Francis B. Foley, W. E. Remmers

DuRing the summer of 1919, the late Dr. Henry M. Howe, then Chairman of the Division of Engineering of the National Research Council, organized a committee to obtain a better insight into the behavior of carbon steels under the influence of various treatments by a proper control of the time and temperature factors. During part of 1919 and 1920, work in connection with this investigation was carried on at Dr. Howe's laboratory at Bedford Hills, N. Y. During 1921 there was an enforced hiatus in the work, occasioned by the illness which resulted in Dr. Howe's death in 1922. At that time one of the present authors compiled the results of the work which had been done and this was published in 1923.' Following the publication of this work, it seemed desirable to carry on in the same manner an investigation of steel of C 0.75 per cent., which steel had not been as fully treated as had the other steels of C 0.34 and 0.52 per cent., used in the published work. Furthermore, certain unusual results have been obtained in the treatment of C 0.52 per cent. steel by quenching and drawing, and repetition of this part of the work seemed advisable. This has been done during the past year at the School of Mines and Metallurgy of the University of Missouri at Rolla, Mo., by a cooperative undertaking of the School and the Bureau of Mines, working in conjunction with the Committee on Heat Treatment of Carbon Steels of the National Research Council. The present paper is a report of the results obtained in this work.

Jan 1, 1926

By George B. Langford

ON THE QUESTION of postwar controls there are today three schools of though ; some advocate state control of everything the socialists ; second are those who advocate the removal of all governmental control over industry - the freedom of enterprise ideal ; and third are those who advocate a middle course - sufficient control to stabilize economic and industrial life, and to prevent violent fluctuations such as we saw in the interwar years. I advocate this third course. I firmly believe un free enterprise, but not in freedom of enterprise, or laissez faire, and there is a great and significant difference between these two.

Jan 1, 1944

By George W. Doffing

Numerous contradictory statements have been made in the past regarding the importance of the seasonal influence of demand for motor fuel on prices of oil securities. It has often been said that the time to buy oil securities is in the spring, or just prior to the heavy consuming season for gasoline. The fallacy of this argument is brought out in the following paragraphs. Seasonality of Oil-security Prices The indexes used in this paper as indicators of prices of oil securities and general industrials are those compiled by Standard Statistics Co. The oil producing and refining stock index includes 14 representative petroleum companies, while the all-industrials index is made up of 347 issues. All figures are stated as relatives, with 1926 = 100. The primary basis of the index, and one that gives a good weighting of the relative importance of the company within the industry, is the total market value of the stock issue outstanding; i.e., the market price times the number of shares outstanding. Adjustments are made for the addition or elimination of issues from the group index, for stock dividends, split-ups, stock rights, et cetera. At the present time the oil producing and refining index includes the following companies: Atlantic Refining Co., Consolidated Oil Corporation, Continental Oil Co., Gulf Oil Corporation, Humble Oil & Refining Co., Ohio Oil Co., Royal Dutch Co., Shell Union Oil Corporation, Socony-Vacuum Oil Co., Standard Oil Company of California, Standard Oil Co. (Indiana), Standard Oil Co. (New Jersey), Texas Corporation, Union Oil Company of California. In calculating the seasonal for oil-security prices several periods have been selected as indicat,ive of major changes in the industry, as follows: 1. 1918 through 1936. This gives an over-all picture of the industry during the motor-vehicle, motor-fuel era. 2. 1927 through 1936. This period includes the control stages, both voluntary and coercive. 3. 1927 to September, 1933. This is the pre-code period of control.

Jan 1, 1937

By Don C. Blackmar

The production of non-ferrous secondary metals has become a large and important industry in the United States, and deals with practically cvery type of manufacturing concern. Its business is unique in that it generally buys frorn its customers as well as sells to them, whether they are individuals, cities, corporations, or the United States government. Its operations are of vital importance to the success and prosperity of nlany of the nation's most important manufacturers; yet there are few industries about which less is generally known by those outside it, whether concerning the rliagnitude of its operations or the details of its actual technique. The industry itself is to blame for this meager publicity, because its technical men have made few attempts to openly exchange ideas, in spite of the excellent examples set by the iron and steel or the copper and brass industries. Whether this is due to the ancient shroud of secrecy generally supposed to cover smelting operations, or because its technical men actually felt that the industry was too puny to be interesting, is hard to say. This paper will consider its subject in a general way, attenlpting to show something of the size and importance of the industry, as well as its fitness to do its work well. Attention will be called to the sound economic reasons for the handling of non-ferrous wastes by specialists, and to the often unseen losses of metals and labor which occur when manufacturc~rs rcclairn thrir own metallic wastes. Magnitude of the Modern Industry No particular thought is given to the kitchen accident whereby a ruined saucepan is sorrowfully tossed into the ash can, yet it is a fairly safe guess that within a month this saucepan, together with hundreds of its follows, will again be in service, perhaps in an autonlobile crankcase, or in an electric vacuum sweeper. It is by this conversion of the useless into the useful, whether from home or large manufacturer, that the secondary tonnage is built up.

DAVE BARTLEY and Edwin F. Gray, miners, late of Shasta County, California, young, healthy, and "dead broke," arrived at Ely, Nevada, one evening in the summer of 1900. Before rustling jobs and going to work, they decided to look around the camp, and in pursuance of this plan they visited a number of claims owned by D. C. McDonald, Justice of the Peace and pioneer of the district. Among the claims he showed them were the Ruth (named after his daughter) and the Kearsarge. Both were regarded as possible gold or silver properties. For no very definite reason the two miners changed their plan and took a lease and option to buy the two claims for $3500. After the transaction was closed and the partners were alone, Gray asked Bartley what he thought of the ground. "If she's good for anything, it's copper" was the reply; and, so far as the records disclose, that was the first time that anyone ever thought of Ely or the Robinson mining district, as it was called, as a possible copper area. There were some slight surface indications of copper, but it is probable that the fact that Bartley had just come from a copper district had something to do with his predilection for a metal that was much despised around Ely. In any event, his hunch was good, and he spoke with the wisdom of an oracle. For thirty years prospectors had sought gold and silver around the camp. Several stamp mills and cyanide plants had been put up and a hundred shafts had been sunk, but fate had been indifferent in its rewards to the optimistic owners. Copper ore would have to be hauled by wagon, 150 miles down Steptoe Valley to the Southern Pacific Railroad, and there was scant hope of finding ore that would bear this cost. W. B. Graham, who ran the general store in Ely, grubstaked Bartley and Gray, furnishing them with food and mining

Jan 1, 1933

By Don C. Blackmar

THE production of non-ferrous secondary metals has become a large and important industry in the United States, and deals with practically every type of manufacturing concern. Its business is unique in that it generally buys from its customers as well as sells to them, whether they are individuals, cities, corporations, or the United States government. Its operations are of vital importance to the success and prosperity of many of the nation's most important manufacturers; yet there are few industries about which less is generally known by those outside it, whether concerning the magnitude of its operations or the details of its actual technique. The industry itself is to blame for this meager publicity, because its technical men have made few attempts to openly exchange ideas, in spite of the excellent examples set by the iron and steel or the copper and brass industries. Whether this is due to the ancient shroud of secrecy generally supposed to cover smelting operations, or because its technical men actually felt that the industry was too puny to be interesting, is hard to say. This paper will consider its subject in a general way, attempting to show something of the size and importance of the industry, as well as its fitness to do its work well. Attention will be called to the sound economic reasons for the handling of non-ferrous wastes by specialists, and to the often unseen losses of metals and labor which occur when manufacturers reclaim their own metallic wastes. MAGNITUDE OF THE MODERN INDUSTRY No particular thought is given to the kitchen accident whereby a ruined saucepan is sorrowfully tossed into the ash can, yet it is a fairly safe guess that within a month this saucepan, together with hundreds of its fellows, will again be in service, perhaps in an automobile crankcase, or in an electric vacuum sweeper. It is by this conversion of the useless into the useful, whether from home or large manufacturer, that the secondary tonnage is built up.

Jan 1, 1928

By Ernest Gayford

When the United States Government started buying gold at varying prices per ounce, set by the President and the Treasury Department, the gold miner found himself facing new conditions, as gold became a commodity with a fluctuating market price. While it was self-evident that the miner was to receive more for his gold than the old established price of $20.67 per ounce, there was an element of uncertainty, which made it difficult, and perhaps dangerous, to decide to invest his time and money to produce gold, especially if the profit would represent only the difference between $20.67 an ounce and the new price as set from day to day by the Government. When, however, on Jan. 30, 1934, the United States went off the gold standard, the price of newly mined gold being rather definitely set at $35 per ounce, with some assurance that the price would be maintained at or near this figure for a long time to come, the gold miner was justified in revaluing his property on the basis of the new price, and the prospector was offered inducement to spend his time and energies hunting for new mines, or going back to old locations previously abandoned as of doubtful value. It is interesting to see what this new price means to the producer of newly mined gold, and how much of the increase is passed on to the producer. It will be found that, as with the base metals, the nearer he can get to producing a finished product himself the greater his reward will be; the net returns for bullion being necessarily higher than for the same amount of gold shipped in concentrates to the smelter. Bullion can be shipped to the United States mints or Government assay offices under the following terms and conditions. An affidavit must accompany the shipment, stating, among other things: 1. The source of the gold; whether ore, tailings or placer. 2. The tons of ore, tailings or cubic yards of gravel from which the shipment was recovered.

Jan 1, 1935

By Frederick Görannsen

McDuffie county, once a part of Columbia county, lies in the eastern part of central Georgia, about 20 miles west of the Savannah river, and bounded on the northtwest by Little river. Wrightsboro, now almost forgotten, was one of the principal towns of Georgia before the Revolutionary war, and much of the land hereafter described as belonging to one of the principal gold-bearing sections of the South had been taken up by the early agricultural settlers, and was already under cultivation. Indeed, some of the present mining companies can trace their chain of title back to the original grant of King George III., made in 1771. The first discovery of gold in Georgia, however, was not made until 1823, when two English miners, who had emigrated to this country and were traveling as peddlers through this section, discovered quartz, rich in gold, on what is now known as " the 40-acre lot," and owned by the Columbia Mining Go. These men had no money to buy the lands, and not being able to stake off a claim and begin work, as is the custom in other places, they were forced to seek the aid of the native farmers. In this we are told that they were for a long time unsuccessful; the farmers and land-owners not knowing or caring anything about gold mining. In 1826, Jeremiah Griffin, a wealthy farmer, became interested with them, and they did some prospecting and located several rich veins. Mr. Griffin soon became enthusiastic, and bought about three thousand acres of supposed gold-lands, lying along Little river.. This purchase was unfortunate for the mining industry, as it effectually shut out all other prospectors, and confined entirely to Mr. Griffin and his associates the mining development of the whole region. As a consequence, the ground was never covered, arid there are virgin lands in this section now, which offer to the prospector as

Jan 1, 1903

By D. H. Bacon

Nearly all men are too busy with their own affairs to keep informed of the progress in other lines. From time to time we read statistics showing the development in some industry that astonish us; but the feeling of surprise soon fades: to be followed by others that likewise pass away. A short resume of what has been done in one line may be of interest. Down to late in the fifties the ore-product of Lake Superior mas handled over a mule-tram-road to Marquette; now the Duluth, South Shore and Atlantic, the Chicago and Northwestern, the Wisconsin Central, the Duluth, Superior and Western, the Duluth, Mesabi and Northern, the Duluth and Iron Range and the Lake Superior and Ishpeming railroads serve the shippers. Down to nearly 1870 a 700-ton ship was an enormous craft, the loading of which required two days; the unloading being seldom accomplished in that time. In 1871 the largest ore-barge carried 1050 toils and made twelve trips per season. Now the cargoes reach 5000 tons, the loading requiring less than three hours, and the unloading ten hours. Now the mines cover more land than was familiar to even the " timber-cruiser " when the Jackson mine was opened. The annual shipments have grown from a few thousand to 10,000,000 tons, and the ability of the mines to produce is not taxed. Lake-freights are at one-eighth, and rail-freights at one-quarter, of early prices. The deeper waterways, commodious locks and large ships of to-day are in a greater measure due to the movement of ore than to any other cause. Great savings have been made in each detail of each department. The only item of cost that has not been lessened, I am glad to say, is the money paid to men. Wages, measured by what they will buy, are as high

Jan 1, 1898

By Charles E. Parsons

One of the greatest factors in our industrial development is cheap and convenient power. Long-distance electrical transmission has now reached such a stage that it is feasible, and practicable, to utilize the water-power of the country which was heretofore too remote for consideration. In all of the changes of energy from its various sources to its electrical applications, water-power stands pre-eminent in point of economy. Power-users the world over have endeavored to utilize this force in preference to any other, and until long-distance transmission was found practicable it seemed that every available water-power in this section of the country was doing its full share for the benefit of mankind. The success of each great industrial development has been clue in a greater part to some one man one who is just a step in advance of the rest in his particular field; one who is able to grasp a situation and foresee possibilities; and, above all, one who has that indomitable pluck and perseverance which sees in each obstacle one more step toward success. Such a mail is Eugene L. Ashley, for it was through his efforts that the development of the greatest power on the Hudson river was made possible. For several years prior to 1897 the various properties along the river between Glens Falls and Palmer Falls were in the hands of speculators. These men knew the value of waterrights, but they had not the ability to assemble the properties and finance such an undertaking. In 1897 Mr. Ashley began buying these water-rights, and, after two years of litigation, title mas secured to all of the properties along each side of the river, and the Hudson River Water-Power Company was organized to construct a dam and transmit power to the surrounding cities and villages. A contract was let for a dam

Jan 1, 1904

The resignation of Herbert Hoover, Director General of Relief in Europe, from his post as Chairman of the Board of Directors of the Food Administration Grain Corporation, in which capacity he had served for nearly two years; and the reorganization of the corporation under the name of the United States Grain Corporation, with Julius Barnes, United States Wheat Director, as its new head, took place at the annual meeting of the stockholders, held in New York, July 1. This action on the hart of Mr. Hoover is believed to be one of the first steps in his intended withdrawal from public service upon the conclusion of the war service of the various departments of the Food Administration, or as soon as they shall have been absorbed by other agencies. The Grain Corporation has been, for the past two years, a vast collection and distribution agency. Its function has been to assist in supplying to the Allies and the American Army and Navy large quantities of wheat, wheat flout, and other foods, with very little disturbance of American prices, and with such an even control of American distribution that reserves from one crop to another have been brought down to the lowest possible compass and without the dvelopment of actual scarcity anywhere in the United States. In the year just past, it carried on all the buying and the shipping for, the Belgian Relief Commission, until the commission retired on May 1 and the Belgian Government itself undertook its own overseas supplies. During the twenty-two months of its existence the corporation had disbursed $3,500,000,000 and collected an equal amount, selling for over-seas shipments commodities valued at $1,800,000,000, at an operating expense of about $3,250,000, or one-sixth of 1 per cent. During this time it has not lost a single dollar through fire loss.

Jan 8, 1919

By Wolfgang Pitsch

INVESTIGATIONS on the above topic have recently been published by Shapiro and Kraussl and Jana and wayman in this journal and by Kessler and Pitsch.- Parts of the results in these papers are in good agreement with each other but there are also some results which are substantially different. The main points of these differences shall be briefly discussed in this communication. Shapiro and Krauss' measured single-surface traces of the habit planes of reversed austenite plates formed within the martensite crystals and deduced from these measurements two distinct habit planes A = (0.174; 0.309; 0.935) and B = (0.375; 0.545; 0.749) within 3 deg. Kessler and pitsch4 found instead by two-surface analysis7 one habit plane n = {0.23; 0.62: 0.75) with a real scatter of 6 deg. The latter observation of a single habit plane apart from a certain scatter is in agreement with most of the investigations of martensite transformations. The differences between these two results are so great that they cannot be explained by experimental error. The purpose of this communication is to show that the A- and B-poles of Shapiro and Krauss are due to an erroneous interpretation of a single-surface trace analysis. The difficulties in the interpretation of such single-surface trace analyses are due to the high symmetry of cubic lattices, from which it follows that there are in general twenty-four equivalent possibilities of plotting a single-surface trace in a pole figure. All these possibilities must be taken into account, when putting different traces from different plates together in order to construct the habit plane. Alternatively the poles of all the traces may be plotted in a unit triangle. This is done in Fig. 1 with twenty-nine traces of different reversed austenite plates, all of this were measured by Shapiro and Krauss in the same plane of a single martensite ther traces taken from Fig. 13 in the Shapiro and Krauss paper' which were determined by electron diffraction. The traces in Figs. 1 and 2 have to be compared with the habits A, B, and n which are under discussion. Therefore the great circles of the poles A, B, and n are plotted in Figs. 3, 4, and 5 together with a 3-deg scatter region for poles A, B and a 6-deg scatter region for pole n. Comparing Figs. 1 and 2 with Figs. 3, 4, and 5 one finds the statements which

Jan 1, 1969

By R. J. Sherman, M. R. Achter

Creep rates have been measured for nickel at 1200°F in air and in vacuum, and related to the depth of surface cracks in the specimens tested in the two environments. The surface cracks were observed to grow faster in air than in vacuum in both short-time and long-time tests. Crack depths, however, could be correlated with creep rates only in the short-time tests. Although no cracks were observed in a relatively brittle Ni-Cr-A1 alloy creep tested at 1300°F, the appearance of alloy specimens fractured after interruption in creep indicated that there was a decrease of intergranular cohesion resulting from the diffusion of atmospheric gases into grain boundaries. PREVIOUS investigations1-3 have demonstrated that the effect of atmosphere on the high-temperature strength of nickel and nickel-base alloys may be reversed by changes in the stress or temperature of the test. At high stress and low temperature the creep-rupture life is longer in vacuum than in air, while at high temperature and low stress the relative strengths are reversed. A mechanism to explain this behavior was proposed based on two competing processes. Oxidation hardens and strengthens a metal, but adsorption of gas, by lowering surface energy, reduces the work required to propagate an intergranular crack. The controlling process is determined by temperature and stress. Basic to this mechanism is the concept that environment determines the ease of propagation of intergranular cracks and thus affects creep rate and rupture life. To explore the mechanism in greater detail, this investigation was undertaken to determine the effect of atmosphere on crack initiation and propagation rates in nickel1 and a relatively brittle Ni-Cr-A1 alloy.3 EXPERIMENTAL PROCEDURE The materials were the same as used previously. Nickel of 99.8 pct purity had the following impurity content: 0.02 pct Co, 0.03 pct Fe, 0.02 pct Mg, 0.03 pct Si, and 0.008 pct C. Rods were cold swaged from 1/2 in. to 3/8 in. in diam and machined into speci- mens with gage sections 1/4 in. in diam by 1-1/4 in. long. They were annealed in vacuum at 1600" F for 1 hr to achieve a grain size of 0.07 mm. The alloy was composed of 19.1 pct Cr, 3.6 pct Al, 1.7 pct Si, 0.57 pct Fe, 0.10 pct Mg, 0.027 pct C, 0.004 pct S, and the balance Ni. Sheet specimens of 0.500-in. width and 1.25-in. gage length were machined from 0.033-in.-thick strip and annealed in vacuum at 2000° F for 2 hr, resulting in a grain size of 0.036 mm. Large amounts of an intergranular phase were introduced as a result of the anneal. Creep tests on both materials, using equipment previously described by Shahinian; were conducted in air and in a vacuum of 1 x 10-5 mm Hg. They were continued to rupture and interrupted at various stages of the test. Although extensions were measured from dial gage readings of movement of the lever arm, it is considered that valid comparisons of creep rate may be made in this manner.l Two parameters were measured metallograph-ically* on longitudinal sections of nickel specimens interrupted during creep—the mean depth of surface cracks 2, and the density n as the number of cracks per unit length of surface. They were combined into one parameter by the relation p = n-d [1] As used here, p is equal to the total of crack depths per unit length of surface. RESULTS Nickel. It is well known that the incidence of intergranular cracking is increased with increasing rupture life. Indeed, it is evident in Tables I and I1

Jan 1, 1962

By William C. Aitkenhead, John A. Jaekel

Uranium deposits in the Spokane Indian Reservation, as well as those around Mt. Spokane, are essentially low grade, much of the ore containing less than 0.2 pct U808. The Mining Experiment Station of the Division of Industrial Research, State College of Washington, has been engaged in intensive research on the amenability of these low grade ores to froth flotation. The results: successful flotation of autinite, chief mineral constituent. At the outset of this work the goal was a concentrate of 1 pct U308 with a 90 pct recovery from ores containing less than 0.2 pct U3O8. Most of the work has been done on argillite ore from the Midnight mine on the Spokane Indian Reservation. The goal has not been attained using this ore, but samples of the granite ore from Mt. Spokane yielded successful results. For example, a concentrate containing 11.2 pct U308 was produced from a Mt. Spokane high grade ore containing 1.27 pct U3O8 with a recovery of 97.8 pct. Another Mt. Spokane ore yielded a concentrate of 5.0 pct U3O8 from an ore containing 0.13 pct U3O8, with a recovery of 85 pct. This same ore gave a recovery of 93.5 pct when the grade of concentrate was reduced to 2.0 pct.

Jan 1, 1959

By E. J. Eisenach, Edward Matsen

AT the present time the Climax Molybdenum Co. is the largest molybdenum producer in the world and the operator of the largest underground mine in North America. It has grown steadily and rapidly since its beginning in 1917. Only 250,000 lb of MoS2 were produced during the first year from 1917 to 1918 when the company was formed. Operations were suspended shortly thereafter because of the lack of a market and knowledge of the uses of molybdenum. During World War I it was used as a substitute for some rare metals and for minor chemical purposes. After 5 years of intensive research and sales promotion, Climax metallurgists succeeded in finding proper applications for the newly discovered metal and the mine was reopened in 1924. Demand for molybdenum increased gradually and in 1930, 3.5 million lb of MoS2 were produced. In the meantime, research work for additional uses of molybdenum continued until it had established itself as one of the most important alloying elements in producing high quality steels. After the start of World War 11, from January 1942 to October 1953, 43 million tons of molybdenum ore were mined and 484 million lb of MoS2 were produced. Climax mine is located in Colorado, 100 miles southwest of Denver and 12 miles northeast of Leadville on the Continental Divide of the Rocky Mountains. The principal mine workings range from 11,170 to 12,000 ft in elevation. Topographically, it lies in the base of a large cirque that is surrounded by Mt. Bartlett to the north, Clinton Peak and McNamee Peak to the east and Ceresco Ridge to the south. This cirque opens to the west and to the Ten Mile Valley.

Jan 3, 1954

By P. R. Sahm, T. V. Pruss

Mixtures of fine GaSb and Gds as well as preal-loyed GaSbl,As, powders were hot-pressed at 690°C and 25,000 psi. Dense alloys with compositional gradients of less than 5 pct were obtained from mixtures containing about 20 mol pct GaAs. For x < 0.2, there were increasing compositional gradients, and for x > 0.2 a GaAs-rich second phase appeared in the microstructure. Densification as well as alloying wlechanisms were enhanced by dissociation and, possibly, oxidation reactions of the powders. Densification of coarse prealloyed material, however, primarily depended on plastic flow phenomena and required temperatures just below solidus and pressures of 50,000 psi Thermal and electrical properties were measured. Although in no case was the figure of merit of melt growth materials approached closer than to within 25 pct, the better overall thermoelectric properties were found in coarse-grained, prealloyed materzals which had been compacted to near theoretical density and where grain regrowth had been induced. Similar results are believed to hold in other binary 111-V compound systems if processed under similar conditions. The densification of unalloyed GaSb powders during pressure sintering (= hot pressing) was shown to depend strongly on powder particle size.&apos; Fine powders displayed a "liquid skin effect" that enhanced compaction through the presence of liquid gallium, whereas coarse powders compacted predominantly by plastic flow. The liquid skin effect, in particular, appeared attractive for alloying GaSb with other, higher-melting, III-V compounds, and to densify these in a one-step operation. This is of special interest in the case of III-V compound alloys as the conventional techniques of melt growth or long-time annealing of powders2 is very time-consuming, especially in cases where a large separation of liquidus and solidus can be expected, such as in GaSbl alloys.2 It was felt that experimentation with this system, a particularly unfavorable example, would allow us to extrapolate to several other, more favorable, cases. Uses of Ill-V alloys are most evident in thermoelectric energy conversion devices.&apos; For this reason certain thermal and electrical properties were measured and compared to those of melt-grown material and to hot-pressed prealloyed powders. EXPERIMENTAL PROCEDURE The pressure-sintering apparatus has been previously described.&apos; Using this equipment, both powder mixtures of GaSb with GaAs and prealloyed GaSbl-,As, powders were hot-pressed. The mixtures were pre- pared from cast GaSb and melt-grown GaAs. The prealloyed material was obtained from stoichiometric melts, initially heated to 1200°C in an evacuated quartz ampoule, and then annealed in the solidus-liquidus interval. A typical annealing cycle consisted of a heating to 850°C (1 hr), extended successive annealing at 750°C (65 hr), and slow stepwise cooling (25 hr) to below solidus. The GaSb, GaAs, and GaSbl-,As, materials were ground in a vibrational mill to particle sizes below 500 . A jet mill reduced these further where necessary. Fine powders were analyzed by Coulter counting for their size distribution. Average sizes by volume were calculated from the data. Mixing of the powders, where necessary, was carried out through rapid vibrational motion. The hot-pressing operation consisted of a degassing period of 15 hr, in most cases at 690°C, followed by several hours of compression, normally 25,000 psi at 690°C for powder mixtures and 50,000 psi at 710°C for prealloyed powders. The chemical compositions were confirmed by X-ray fluorescence analysis. To estimate the degree of solid solution achieved, lattice parameters were determined and interpreted according to Vegard&apos;s rule. In addition, optical microscopy helped to correlate the relative amounts of the phases present as well as the degree of porosity to the measured density. To reveal grain boundaries, polished surfaces were etched4 with H 2 O:H 2 O:HCl = 2:l:l. In several cases microscopic concentration gradients were monitored by electron-probe analysis-. RESULTS AND DISCUSSION Alloying and Densification of GaSn-GaAs Powder Mixtures. After preliminary experiments showed that no appreciable alloying took place in mixtures of coarse GaSb (22.5 p) and fine GaAs (2.5 p) powders, hot pressing of mixtures was confined to fine powders only (3.1 and 2.4 p, respectively). Alloying and densification apparently occurred simultaneously with a grain regrowth mechanism which depended on the presence of a liquid phase.&apos; The liquid phase was provided by the dissociation of GasbS particles into liquid gallium and antimony above 555°C. This not only enhanced grain regrowth and densification, as in unalloyed GaSb,&apos; but took on additional importance here for the alloying process. Alloying was speeded up by the resulting liquid-solid interaction as compared to the very slow solid-state diffusion process normally expected at these temperatures.&apos; The results obtained with a series of powder mixtures have been compiled in Table I. It is seen that for mixtures with less than 20 mol pct GaAs, x < 0.2, the compositional ranges increased and for x > 0.2 a GaAs-rich phase and free antimony appeared in the microstructure in sizable amounts.

Jan 1, 1968

By E. W. Murbach

The oxidation of uranium carbide by oxygen at various pressures, and by air, has been investigated at temperatures up to 600°C. Arc-melted and cast uranium carbide displays oxidation behavior that appears to be dependent on its treatment after melting. ccReactive" uranium carbide, which results from exposure of freshly melted material to laboratory air, ignites in oxygen at about 275° to 350°C depending on pressure, and in air at about 350°C. The product of the initial oxidation appears to be UO2+.. Continued heating produces U30,. The initial oxidation rate is poportional, roughly, to the square root of the oxygen pressure. The activation energy determined for the initial oxidation reaction is 7.1 kcal, from 400° to 600°C in 10 mm of oxygen. AN investigation of low-decontamination methods for reprocessing uranium carbide reactor fuels is being carried out at Atomics International. One of the reprocessing cycles includes oxidation of the fuel at relatively low temperature (300° to 500°C) and reaction of the product oxide with carbon at elevated temperatures (above 1500°C) to produce uranium carbide. A number of small-scale experiments have been carried out in which uranium carbide was oxidized in air and oxygen at various pressures to measure reaction rates and to obtain other information concerning the oxidation process. In initial experiments with arc-melted UC, ignition was observed at about 275°C in oxygen or 350°C in air. However, similar experiments by Neymark&apos; at 426°C in air showed no ignition. It was soon determined that the difference in oxidation behavior was due to the treatment of the UC following arc-melting. Neymark&apos;s experiments were carried out with freshly melted UC while those reported in the

Jan 1, 1963