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By A. B. Cox, L. W. Wark

An attempt has been made to compare the influences of the two most widely used depressants—alkalis and sodium cyanide—and the most widely used activator—copper sulfate—on the air-mineral contact induced by five sulfur-bearing compounds: (1) sodium di-ethyl dithio-phosphate (sodium Aerofloat); (2) potassium ethyl xanthate; (3) sodium di-ethyl dithiocarbamate; (4) potassium iso-amyl xanthate; (5) potassium di-n-amyl dithiocarbamate. Three different organic types are included in lhis group and for two of these types a higher and a lower homologue have been tested. The study of potassium ethyl xanthate, the preliminary results of which have been described,' was continued until there had been obtained a comprehensive account of the influence of variations in pH value and in the concentrations of xanthate, sodium cyanide and copper sulfate on the adsorption of this xanthate by galena, sphalerite, pyrite and chalcopyrite. With concentrations of copper sulfate and collector that the work with ethyl xanthate indicated would give the most illuminating. results, the other four collectors were tested, in a less exhaustive way. The same general principles determine the influence of alkalis, cyanide and copper sulfate, no matter to which type the collector belongs, but there is a gradation in the quantitative measure of such influence. In the list above, the five collectors are cited in the order of their capacity to withstand the depressants, sodium Aerofloat being the least resistant, potassium di-n-amyl dithiocarbamate the most resistant. This order coincides substantially with that of the solubilities of the heavy metal salts formed by double decomposition with the collectors, those formed from sodium Aerofloat being most soluble. There is little difference between the third and fourth members of the series, and under certain conditions their positions are reversed. In general, then, of the three types of collectors investigated, the dithiophosphate type is most easily influenced by depressants, and the

Jan 1, 1935

Curlisle: We're sitting in Don McLaughlin's office overlooking Sun Francisco Bay, and he's going to be good enough to talk about early days in California, maybe about his college years in Berkeley, maybe about his first jobs in mining. Now, Don, would you be good enough to start it off by saying something about George Hearst. I know he died before you were born, but you know a lot about the family, and you no doubt know a lot about him. Certainly, nobody in those days matched his record in getting hold of good mines. McLaughlin: George Hearst died, actually, in the very year that I was born, but as I more or less grew up in the home of Mrs. Phoebe Hearst, who was his widow, I heard a great deal about the mines and the people that made the great fortune she inherited and used so wisely. But I don't think I really had an appreciation of George Hearst until 1 became active in the mining world and realized how many major mines he had picked in the early days and how much he had to do with their development into successful properties. He started in the California gold fields, but it was on the Comstock that he made his first big stake out of his substantial share in the Ophir mine. I believe at that time he was on his own. Then, later, he became associated with Ben Ali Haggin and Lloyd Tevis in San Francisco, and scoured the West for them. They made a little money in Eureka, Nevada, and other places, but the first important property that he obtained for them was the famous Ontario Mine in Park City, which became one of the great silver lead producers of the Continent. Then later he acquired the Homestake.

Jan 6, 1965

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

IT has often been reported that coatings may strengthen single crystals and polycrystalline specimens of coarse grain size. This note reports the effect of a surface layer of fine grains on the creep-rupture properties of coarse grained nickel 99.8 pct pure. Sheet specimens were machined from cold-rolled material, finished by surface grinding and annealed at 1230°C in vacuum for 4 hr. Half of them were re-ground on faces and sides and annealed at 925"C for 1 1/4 hr. The double grind-anneal treatment produced a structure consisting of a surface layer of fine grains of 0.02 mm diam on a coarse-grained substrate of grains of 0.40 mm diam. Comparison with specimens which received only the single grind showed that the second grind-anneal did not alter the structure of the substrate. Several modifications were made in specimen design to eliminate erratic rupture behavior outside of the gage length. In the final design the gage section, oriented parallel to the rolling direction, was 1.00 in. long, 0.4 in. wide, and 0.0625 in. thick. End tabs were pinned in place. Although other configurations (welded end tabs, transverse orientation, and wider gage section) showed similar effects of a layer of fine grains, because of the erratic rupture behavior, only the data from the final design are reported here. Creep tests were performed at 650°C in air and in a vacuum of 10~5 mm Hg. Creep rates were measured from the movements of the lever arm. Since the broken sheet specimens could not be fitted together, elongations at fracture measured by means of gage marks, do not include the necked portions adjacent to the fracture. Results of the creep tests with and without the fine grained surface are given in Table I. An explanation for the lower strength in air than in vacuum has been proposed previously in terms of the reduction of crack propagation energy by gas adsorption.l In both environments the fine-grained layer produced a small decrease in minimum creep rate and, except for the shortest test in air, a substantial increase in rupture life. The elongation values at rupture, as they are measured here, do not demonstrate an appreciable effect of the grain structure but do show much smaller ductilities in air than in vacuum. Greater elongations maybe associated with the finegrained layer, however, especially in vacuum, in creep curves such as those in Fig. 1. Duplicate tests were not run to determine the re-producibility of the data. It is felt, however, that, in view of the consistent behavior, the prolongation of rupture life may be attributed to the effect of the fine-grained surface. In the data not reported be-

Jan 1, 1962

By W. H. Fulweiler

The writer would define the term "Use Classification" as a discussion of the qualities that coal should possess to fulfill the requirements of the industry or process in which it is to be used. The general problem of the gas industry is to transform the maximum amount of the thermal energy in coal into a gas of specified quality. The qualifications that a coal should possess to be useful in the gas industry are complicated by probably a greater number of factors than in most industries. The most important of these is the delivered price of the coal. While the- general problem of the industry is as given above, yet the actual problem is the production of gas of a specified quality at the minimum cost. The relative cost of coal and the selling prices for the residuals which are influenced to a large extent by geographical locations are of determining importance as effecting the cost of the gas. It is unfortunate that we cannot disassociate cost figures from a discussion of the desirable characteristics and this results frequently in the use of coal in one location that will be looked upon as quite impossible in another location more favorably situated. Without going into any discussion of the freight rate problem we might merely point out that in general the freight on the coal is equal to or greater than the mine price. It must be evident, therefore, that price must always be considered in any discussion of the effect of the characteristics of a given coal. Two Classes of PRocesses In discussing the characteristics of coals for use in the industry, we must divide the processes in use into two classes: (1) where the coal is destructively distilled at high temperatures resulting in the formation of coke in the liberation of gas and by-products, and (2) where the coal is consumed by combustion in air or steam with a production of gas and by-products leaving only clinker as a residue. The Germans differentiate these two types of processes in their words"' entgasung'" and'" vergasung."' In the distillation processes, we have the effect of the coal on the yield of gas and its quality; the quantity and quality of coke; and the

Jan 1, 1930

By D. B. Kibler

THE Florida hard-rock field extends from Suwanee and Columbia Counties in northwest Florida to south of Croom, Florida, in Hernando County. This area is approximately 100 miles long and varies from 2 to 30 miles in width. Florida hard-rock phosphate was discovered at Hale Springs, about one mile northwest of the town of Dunnellon, Marion County, in the year 1888, by Albertus Voight, who lived within a few hundred yards of the spring. Soon after this discovery there was a great influx of land speculators and wildcat operators into the vicinity of Dunnellon. A few years later phosphate was found in Alachua, Levy, Citrus and Hernando Counties, and a great number of small crude plants were built from Newberry, Alachua County, all the way to Croom, Hernando County. Phosphate was found in many places as "outcrops." Looking for outcrops was the first method used by the early prospectors in searching for deposits. Several years passed before any systematic method of prospecting was used. EARLY MINING The early method of mining hard-rock phosphate was with picks and shovels, wheelbarrows, mules and wagons. The pick-and-shovel method was used altogether until about 1900, when some of the larger operators began to use railroad-type steam shovels of from ½ to 1-yd. capacity. Picks and shovels, with negro labor loading the phosphate ore (called "matrix") into wooden side-dump skip-cars, was continued until about 1907. From the discovery of hard-rock phosphate until approximately 1905, overburden was removed with mules and scrapers. At some places, the overburden was loaded into side-dump skip-cars by negro laborers and the cars were then pulled up an incline with a steam hoisting engine. The maximum depth of overburden that could be economically removed by hand labor, mules and scrapers was approximately 15 feet. About 1905 one of the companies erected a producer-gas powerhouse near Dunnellon and generated its own electricity and about the same time the larger companies began using hydraulic methods for the removal of overburden. From the year 1888 through the year 1939, approximately 75 companies were operating at one time or another in the hard-rock territory, on approximately 500 locations. The hard-rock deposits are more irregular and have higher mining costs than the pebble-rock deposits, therefore they have not been competitive in the domestic market, but because of the higher grade of the hard rock it is in demand for the export trade. Discovery of phosphate outside of the United States has made it increasingly difficult in recent years for the hard-rock companies to survive, so today only three companies are operating. These

Jan 1, 1941

By D. B Kibler

The Florida hard-rock field extends from Suwanee and Columbia Counties in northwest Florida to south of Croom, Florida, in Hernando County. This area is approximately 100 miles long and varies from 2 to 30 miles in width. Florida hard-rock phosphate was discovered at Hale Springs, about one mile northwest of the town of Dunnellon, Marion County, in the year 1888, by Alber-tus Voight, who lived within a few hundred yards of the spring. Soon after this discovery there was a great influx of land speculators and wildcat operators into the vicinity of Dunnellon. A few years later phosphate was found in Alachua, Levy, Citrus and Hernando Counties, and a great number of small crude plants were built from Newberry, Alachua County, all the way to Croom, Hernando County. Phosphate was found in many places as "outcrops." Looking for outcrops was the first method used by the early prospectors in searching for deposits. Several years passed before any systematic method of prospecting was used. Early Mining The early method of mining hard-rock phosphate was with picks and shovels, wheelbarrows, mules and wagons. The pick-and-shovel method was used altogether until about 1900, when some of the larger operators began to use railroad-type steam shovels of from ½ to I-yd. capacity Picks and shovels, with negro labor loading the phosphate ore (called "matrix") into wooden side-dump skip-cars, was continued until about 1907. From the discovery of hard-rock phosphate until approximately 1905, overburden was removed with mules and scrapers. At some places, the overburden was loaded into side-dump skip-cars by negro laborers and the cars were then pulled up an incline with a steam hoisting engine. The maximum depth of overburden that could be economically removed by hand labor, mules and scrapers was approximately 15 feet. About 1905 one of the companies erected a producer-gas power- I house near Dunnellon and generated its own electricity and about the same time the larger companies began using hydraulic methods for the removal of overburden. From the year 1888 through the year 1939 approximately 75 companies were operating at one time or another in the hard-rock territory, on approximately 500 locations. The hard-rock deposits are more irregular and have higher mining costs than the pebble-rock deposits, therefore 1 they have not been competitive in the domestic market, but because of the higher grade of the hard rock it is in demand for I the export trade. Discovery of phosphate outside of the United States has made it increasingly difficult in recent years for the hard-rock companies to survive, so today i only three companies are operating. These

Jan 1, 1942

By D. B. Kibler

The Florida hard-rock field extends from Suwanee and Columbia Counties in northwest Florida to south of Croom, Florida, in Hernando County. This area is approximately 100 miles long and varies from 2 to 30 miles in width. Florida hard-rock phosphate was discovered at Hale Springs, about one mile northwest of the town of Dunnellon, Marion County, in the year 1888, by Alber-tus Voight, who lived within a few hundred yards of the spring. Soon after this discovery there was a great influx of land speculators and wildcat operators into the vicinity of Dunnellon. A few years later phosphate was found in Alachua, Levy, Citrus and Hernando Counties, and a great number of small crude plants were built from Newberry, Alachua County, all the way to Croom, Hernando County. Phosphate was found in many places as "outcrops." Looking for outcrops was the first method used by the early prospectors in searching for deposits. Several years passed before any systematic method of prospecting was used. Early Mining The early method of mining hard-rock phosphate was with picks and shovels, wheelbarrows, mules and wagons. The pick-and-shovel method was used altogether until about 1900, when some of the larger operators began to use railroad-type steam shovels of from ½ to I-yd. capacity Picks and shovels, with negro labor loading the phosphate ore (called "matrix") into wooden side-dump skip-cars, was continued until about 1907. From the discovery of hard-rock phosphate until approximately 1905, overburden was removed with mules and scrapers. At some places, the overburden was loaded into side-dump skip-cars by negro laborers and the cars were then pulled up an incline with a steam hoisting engine. The maximum depth of overburden that could be economically removed by hand labor, mules and scrapers was approximately 15 feet. About 1905 one of the companies erected a producer-gas power- I house near Dunnellon and generated its own electricity and about the same time the larger companies began using hydraulic methods for the removal of overburden. From the year 1888 through the year 1939 approximately 75 companies were operating at one time or another in the hard-rock territory, on approximately 500 locations. The hard-rock deposits are more irregular and have higher mining costs than the pebble-rock deposits, therefore 1 they have not been competitive in the domestic market, but because of the higher grade of the hard rock it is in demand for I the export trade. Discovery of phosphate outside of the United States has made it increasingly difficult in recent years for the hard-rock companies to survive, so today i only three companies are operating. These

Jan 1, 1942

By J. E. Lawver

On the basis of both laboratory and pilot-scale tests, a newly developed high-tension electrostatic process is technically and economically feasible for the production of iron ore superconcentrates containing 0.02 to 0.20% silica at iron recoveries of 85 to 90%. The process can be used to recover both a superconcentrate and a pellet-grade concentrate, from a feed containing middlings, and the system is not unduly upset from changes in feed structure and composition. The adverse affect of excess quantities of material finer than 30 microns, i.e., above 10% in quantity can be avoided by a desliming step. Finally, because of the cost of drying, the best feed for the process appears to be dry-ground ores as well as spiral, flotation, or magnetic concentrates.

Jan 1, 1970

By Don K. Smith

The Reclamation Program for the Northern Zone of the Indus Plains in West Pakistan involves the construction of 30,000 irrigation wells to serve 20 million acres with an annual pumpage of nearly 40 million acre-ft. Detailed hydrologic studies indicated that mild steel would be satisfactory for casing; however, within two years after construction, about 10% of the wells began to fail due to encrustation and corrosion of the casing. A search to find a noncor-rosive substitute for the steel casing disclosed that only fiberglass-reinforced plastic pipe satisfied all requirements. The results of initial use of fiberglass have been highly satisfactory and have resulted in a lower over-all well cost. Advances in technology pomise further reduction in prices and improvement in performance. The northern zone of the Indus Basin comprises a vast area of essentially level land in West Pakistan which is irrigated by means of a complex system of canals that distribute more water to more land than any other irrigation system in the world. In spite of the development of this extensive irrigation system, production of food and fiber has not met the requirements of the country. The major reasons that crop production has not reached anticipated levels are the lack of adequate irrigation supplies and effective subsurface drainage. As a result, yields per acre are among the lowest in the world for areas where irrigation is practiced, and many thousands of acres of valuable crop land have been removed from production or seriously affected by salinity and waterlogging. To rectify the problems of irrigation supply and drainage the Government of Pakistan has undertaken a program of Salinity Control and Reclamation which is being administered by the Water and Power Development Authority. The Authority retained Tipton and Kalmbach, Inc., of Denver, Colo., as engineers for the program in the northern zone of the Indus Basin. This program consists of the construction of about 30,000 irrigation wells to provide drainage for waterlogged lands and full irrigation supplies, including leaching requirements, for all cultivated lands. The program will ultimately ensure the productivity of 20 million acres and involve an annual pumpage from groundwater storage of nearly 40 million acre-ft of

Jan 1, 1970

By D. B. Kibler

Pill Florida hard-rock field extends from Suwanee and Columbia Counties in northwest Florida to south of Croom, Florida, in Hernando County this area is approximately 100 miles long and varies from 2 to 30 miles 1n width Florida hard-rock phosphate was discovered at Hale Springs, about one mile northwest of the town of Dunnellon Marion County, in the year 1888, by Albertus Voight who lived within a few hundred yards of the spring Soon after this discovery there was a great influx of land speculators and wildcat operators into the vicinity of Dunnellon A few years later phosphate was found in Alachua, Levy, Citrus and Hernando Counties, and a great number of small crude plants were built from Newberry, Alachua County, all the way to Croom, Hernando County Phosphate was found in many places as "outcrops " Looking for outcrops was the first method used by the early prospectors in searching for deposits Several years passed before any systematic method of prospecting was used EARLY MINING The early method of mining hard-rock phosphate was with picks and shovels, wheelbarrows, mules and wagons The pick-and-shovel method was used altogether until about 1900, when some of the larger operators began to use railroad-type steam shovels of from 1/2 to 1-yd capacity Picks and shovels, with negro labor loading the phosphate ore (called "matrix") into wooden side-dump skip-cars, was continued until about 1907 From the discovery of hard-rock phosphate until approximately 1905, overburden was removed with mules and scrapers At some places, the overburden was loaded into side-du nip skip-cars by negro laborers and the cars were then pulled up an incline with a steam hoisting engine The maximum depth of overburden that could be economically removed by hand labor mules and scrapers was approximately 15 feet About 1905 one of the companies erected a producer-gas powerhouse near Dunnellon and generated its own electricity and about the same time the larger companies began using hydraulic methods for the removal of overburden From the year 1888 through the year 1939, approximately 75 companies were operating at one time or another in the hard-rock territory, on approximately 500 locations The hard-rock deposits are more irregular and have higher mining costs than the pebble-rock deposits, therefore they have not been competitive in the domestic market, but because of the higher grade of the hard rock it is in demand for the export trade Discovery of phosphate outside of the United States has made it increasingly difficult in recent years for the hard-rock companies to survive, so today only three companies are operating These

Jan 1, 1941

In accordance with the usual custom, manuscripts to be presented at the next meeting of the Institute must be in the hands of the, Secretary before July 1, 1917. Manuscripts to be properly distributed in advance of the meeting must be in the hands of the Secretary before June 1, 1917. At the last meeting of the Institute 45 papers were presented, and 42 of them were actively discussed. This experience makes us believe that advance distribution is the best possible means of getting a good discussion of papers and of securing for them the interest of the members of the profession. It will be impossible, however, to give the papers proper distribution if they bare not received before June 1, 1917.

Jan 4, 1917

By A. Rosen, P. Wynblatt, J. E. Dorn

The temperature, strain rate, and structure dependence of the flow stress in a poly crystalline Fe-2 pct Mn alloy was investigated between 77" and 370°K. It was possible to identify the low-temperature data from 77° to 160°K with Dorn and Rajnak's theory of the Peierls mechanism of plastic deformation. Above 160°K one or more thermally activated mechanisms must he operative; however, these were not identified in this investigation. The mechanistic basis for the rapid decrease in the flow stress of bcc metals with an increase in temperature over the low-temperature range is yet being debated. Various dislocation mechanisms have been suggested in the past but the agreement between the various proposed theories and the experimental results have not been definitive. In the present paper, the authors will demonstrate that the plastic behavior of polycrystalline iron containing 2 wt pct Mn plus interstitials agrees excellently with predictions based on the Peierls mechanism from 77" to 160°K whereas from 160" to about 370°K other as yet unidentified thermally activated mechanisms take over. Undoubtedly, the overlap of these mechanisms with the Peierls mechanism contributed to the difficulties of rationalizing the low-temperature behavior of iron and its alloys. I) EXPERIMENTAL TECHNIQUES AND RESULTS Although extensive data are now available on the effect of temperature and strain rate on the flow stress of various bcc metals and alloys, it was, nevertheless, deemed necessary for the objectives of the present study to obtain highly accurate data of the type most pertinent for checking the theories on a series of well-documented work-hardened states. Iron containing 2 wt pct Mn was used in this investigation in order to obtain a lower ductile to brittle transition temperature than that for iron.' The additional elements present were 0.004 pct C, 0.05 pct 0, 0.004 pct S, 0.003 pct P, 0.006 pct N, and 0.001 pct Si. The as-received 3/8 by 3/4 in. bars were cold-rolled to 0.100-in. thickness, recrystallized under argon for 30 min at 1073"~, further cold-rolled to 0.063-in. thickness, and finally recrystallized under argon for 30 min at 1000°K. This treatment gave a stable reproducible equiaxed grain structure having an average grain diameter of about 90 p. Prior to the final recrystallization treatment, the sheet was machined into tensile specimens 1/4 in. wide having a 1.625-in.-long gage section. All specimens were tested in controlled-temperature baths on an Instron Testing Machine. For convenience in the theoretical analyses the data will be given in terms of the shear stress for flow, 7, the shear strain rate, f, and the shear strain, y. A series of three standard strain-hardened states were obtained by prestraining specimens at 300°K and at a shear strain rate of 7.68 x lo-' per sec to three stress levels of 6.89 X l08, 10.3 X lo8, and 14.5 x 10' dynes per sq cm, respectively. Immediately following this prestrain the temperature bath was changed and each specimen was pulled in tension at either f = 7.68 X lo-' or f = 3.06 X 10"3 per sec. In terms of the accuracy that was achieved, the values obtained did not deviate more than *0.1 X 10' dynes per sq cm and * 1°K from the reported values of stress and temperature and not more than *5 pct in the reported values of the strain rate. The tensile stresses were converted to shear stresses using a factor of 1/2. The shear stress for the initiation of flow at the test temperature was determined by taking a y = 6.16 x 10'3 offset. from the modulus line at which point good accuracy could be achieved in determining y and the associated flow stress 7, with only a negligible increase in the pre-

Jan 1, 1965

By Ta M. Li

Expanded mine-mill capacity and greater operating flexibility are part of the dramatic changes taking place in the Tennessee mining operations of Asarco, Inc. Climaxed by the recent start-up of the $6.3 million Young mill in September 1975, Asarco has pushed Tennessee back into number one position as the leading zinc mining state. Furthermore, start-up of the Young mill is expected to insure a much-needed and continuing domestic zinc supply, at a time when US mines can only supply one-half of 1975 domestic consumption.

Jan 5, 1976

By Ursula E. Wolff

The precipitation of carbides from an alloy containing 33 pct Ni, 21 pct Cr, balance iron, was investigated electron microscopically by means of extraction replicas and thinned metal foils. Annealing temperatures ranged from 565°to 870°C and up to several thousand hours. M23C6 precipitated in pain boundaries, incoherent and coherent twin boundaries in that sequence. The orientation relationship between carbides and austenite matrix was determined and correlated with the morphology of the carbides and with the type of boundary in which precipitation occurred. In large-angle grain boundaries, as well as in coherent twin boundaries, the carbides had the same orientation as one of the adjacent pains. These carbides formed sheets of individual flakes with shapes related to the orientation of the boundary. In incoherent twin boundaries carbides precipitated in ribbons composed of pavallel rods. An unidentified subcarbide was found to precede precipitation of M23C6 in these boundaries. The M 23 C6 rods had a kind of fiber texture with (110) parallel to the long dimension of the rods and ribbon, and with orientations of both of the adjacent twin-related austenite crystals Predominant in the texture of the carbide. A hard sphere crystal model has been used to discuss orientation and morphology of the carbides in terms of free volume and vacancies available in the boundaries. A number of papers have dealt with the morphology of chromium carbide (M23 C6) precipitated in austenitic stainless steels.1"7 In all these investigations, the carbides were examined in the electron microscope by means of extraction replicas. With this technique, the carbides retain the spatial distribution they had in the bulk sample. However, since the matrix is dissolved in the process, the particles can turn in an unpredictable way; and the orientation relationship between matrix and carbides cannot be established. In this paper the results of studies on extraction replicas and on thinned metal foils are reported. These studies were undertaken to determine the matrix-to-car bide orientation relationship, and to correlate the orientation of the carbides with their morphology. PROCEDURE The material used was an austenitic alloy with 33 pct Ni, 21 pct Cr, balance iron, containing approximately 0.05 pct C. Coupons of 1.25-mm sheet were first solution-annealed at 1050°C for 15 min and air-cooled. Then, to precipitate the carbides, samples were isothermally annealed in the range from 565" to 870°C for times up to several thousand hours. All further specimen-preparation procedures were carried out after the final anneal. Carbon extraction replicas from polished and etched surfaces were made with 10 pct bromine in methyl alcohol.' Thin foils were prepared from punched-out 3-mm-diam disksg which fit into the electron-microscope holder. The disks were prethinned by grinding to approximately 0.5 mm thickness, and then electro-polished in a polytetrafluoroethylene holder1' with a solution containing 5 pct perchloric acid in acetic acid to which 10 g per 1 Cro3 and 5 g per 1 nickel chloride were added (etchant modified from that of Briers et al."). This solution dissolves neither the carbides nor the austenite around the carbides preferentially. By using extraction replicas, electron micrographs and selected-area electron-diffraction patterns were taken from the same carbide arrays. By using thin foils, electron micrographs were made from a grain boundary area containing carbides. Electron-diffraction patterns were then taken from the same area and from each of the adjacent grains separately. In this manner, the orientation of each grain could be determined without interference by the carbide pattern. A peculiarity of extraction replicas should be pointed out. After the matrix is etched away, the carbide arrays float freely in the etching and washing solutions, and are held in place only at the anchoring points in the carbon replica. When the replica is picked up with a screen the carbide arrays tend to flip to one side. Thus, while the surface features are preserved, the original arrangement of the carbides may severely and unpredictably be disturbed whenever the specimen contains large amounts of interconnected carbides. Nevertheless, it is possible to correlate the different morphologies of the carbides with the type of boundary in which they have precipitated. RESULTS 1) Extraction Replicas. Fig. 1 shows that the grain boundaries usually are curved, multicornered surfaces of random orientation. The coherent twin boundaries (which are (111) planes) cut a grain into parallel slices. Incoherent twin boundaries occur at the ends and on the steps of twins and are often narrow, parallel-sided strips which are much longer than they are wide. Different morphologies can clearly be distinguished for the M23Ce carbides precipitated in each of these types of boundaries, and agree well with those observed by kinzel.2 The kinetics of this precipitation has been investigated." The first carbides precipitate in junctions of three grain boundaries and fan out from there into the adjoining boundary surfaces, Fig. 2(a). These carbides are oriented randomly, Fig. 2(b), and become coarser and thicker as annealing time increases. The large-angle grain boundaries are next to fill

Jan 1, 1967

By F. E. Jaumot, R. L. Smith

Self-diffusion in zinc at temperatures below 200°C has been studied using both single crystal and polycrystal samples. Anomalous results were obtained for single crystal samples, the data indicating that in some cases grain boundary diffusion predominated. These anomalous results are presumed to be due to low angle lineage boundaries in the single crystals. When volume diffusion occurred in either single or polycrystal samples, the values for the diffusion coefficient were as much as several orders of magnitude larger than would be expected from high temperature data. ONSIDERABLE work has been done on self-^-*diffusion at temperatures in the neighborhood of two thirds of the melting temperature (in OK) and higher, but very little has been done at lower temperatures. This is particularly true of self-diffusion in single crystals. This paper reports work on self-diffusion in zinc at temperatures below 200 °C where both polycrystalline and single crystal samples have been used. The measurements were made using both the sectioning and absorption techniques. The experiments on diffusion at low temperatures were initiated primarily for three reasons: to obtain data from single crystal diffusion covering a wide range of temperatures, to obtain values of the activation energy for grain boundary diffusion, and to obtain, if possible, a lower limit to the temperatures at which the absorption technique may be used. It is possible to determine whether volume or grain boundary diffusion predominates at low temperatures by analyzing the manner in which the concentration of the diffusing atoms varies with the depth of penetration. The analysis is possible only for the sectioning technique. For volume diffusion and for the boundary conditions of the present experiment, the curve of the logarithm of the concentration, C, vs the square of the penetration depth, x, is a straight line with the slope proportional to — 1/D. If grain boundary diffusion predominates, Fisher' has shown that a curve of In C vs the first power of the penetration depth should be a straight line. This linear dependence of concentration on depth has been observed experimentally by several investigators. (See, for example, refs. 3 and 4.) Following Fisher's analysis, the grain boundary diffusion coefficient can be written as where 8 is the grain boundary width, D, is the volume diffusion coefficient at the temperature involved, t is the time of diffusion, C is the concentration of diffusing material, and x is the depth of penetration. A more general analysis employing the same model as Fisher's but with fewer assumptions has been given by Whipple.' In contrast to Fisher's analysis the more general analysis of Whipple does not always yield a straight line relation between In C and x. Recently Turnbull and Hoffman have discussed both analyses and have applied the Fisher-Whipple model to a more refined dislocation model of the grain boundary. They have also discussed the possibility of a large effect of grain boundary direction on diffusion. In the case of the absorption technique, for which results are also given, one simply gets a value for the diffusion coefficient with no indication of the predominating mechanism. Experimental Techniques Single crystals of 99.99+ pct Zn were grown using a modified Bridgman method. Polycrystal samples were prepared in three grain sizes (small, about 4 mm2; medium, about 9 mm'; and large, about 25 mmz) by quenching, air cooling, and furnace cooling. The grains of the polycrystalline samples tended to be columnar, with some preferred texture such that the c-axis was inclined at about 20" to 25" from the normal to the diffusion face, particularly in the medium and large grain size samples. The samples were cut from the rod, polished, and heavily etched, and faces cut accurately parallel using a jeweler's lathe. They were again etched to remove the lathe smear and annealed for 3 hr at 250" to 300°C. After annealing, they were etched, examined, and the orientation determined by Laue back reflection photographs. They were then electroplated with Zn. The plated surfaces were examined for uniformity; nonuniform coatings were removed by etching and the samples replated without additional preparation. For the diffusion anneals, the samples were placed in pairs, with active faces together, in evacuated Pyrex tubes. Constant temperature baths were used, and the variation in temperature did not exceed ±l°C, Diffusion runs were made at l00°,

Jan 1, 1957

By C. F. Cornell, R. C. Emmett, D. A. Dahlstrom

FOR many years the disk-type and cloth-covered drum filters have found widest application in liquid-solids separation, which uses continuous filters. The disk type is less expensive, occupies less floor space per square foot of filtration area, and requires negligible down time for filter media changing. However, because filter cloth is billowed out by the blowback in the cake discharge, it is very short-lived if the scraper blades are set too close. Consequently cake weight is very important in assisting cake discharge, which normally necessitates a minimum cake thickness of 3/8 to ½ in. Also, the vertical position of the disks eliminates the possibility of efficient cake washing for removal of soluble values. The disk-type filter is generally limited, therefore, to applications that require no cake washing and form relatively thick cakes within the normal range of filter cycle times. The conventional cloth-covered drum filter is a more flexible unit, permitting wider variation in the percentage of cycle time devoted to cake formation, dewatering, or washing, as required by the application. Thinner filter cakes can be discharged because a horizontal line across the filter medium at the location of the scraper blade is equidistant from the edge of the blade at all points. The scraper blade therefore may be set a short distance from the filter medium or, where wire winding is not used, a floating scraper can be utilized so that the contour of the cloth can be followed. The drum filter is generally employed when there are difficult filtering slurries with resultant thin cakes or when cake washing to recover soluble values must be practiced. Difficulties sometimes encountered in continuous filter operation can be summarized in the following four categories: 1) Low filtration and/or washing rates due to blinding of the filter medium. 2) Poor cake discharge resulting from sticky cakes, filter medium blinding, or too thin a cake for the particular type of filter. 3) High filter media costs caused by short life and frequent down times for cloth changing. This results from blinding or from abrasion by the scraper blade when cakes are thin. 4) Blowback of filtrate at cake discharge because not enough air passes through the cake to purge the drainage area and filtrate lines during dewatering. To reduce or eliminate blinding tendencies several modifications have been tried, for example, cover-cleaning showers, blowback under the feed slurry, and snap-blow cake discharge. In many cases, however, this simply retards the rate of blinding, since the filter medium is kept clean at its outer surface only by these methods. As blinding usually occurs within or on the back of the medium, the operator is finally forced either to remove the cloth and scrub the medium intensively with a cleaning solution or acid-rinse it on the filter—all resulting in down time, short cloth life, and additional costs.

Jan 1, 1959

By R. P. Smith, L. S. Darken

FOR a high-purity iron-carbon alloy, the phases existing at equilibrium at temperatures slightly above the temperature of the metastable eutectoid are austenite and cementite (hyper-eutectoid) or austenite and ferrite (hypo-eutectoid) and those below the eutectoid temperature (carbdn content > 0.02 pct) are ferrite and cementite. Such an alloy, held in a carefully controlled and measured temperature gradient (about 1 cm per deg) which includes the eutectoid temperature, then quenched and examined metallographicall.y, provides a precise measure of the eutectoid temperature. The samples were hollow cylinders approximately 1.3 cm OD, 0.63 cm ID, and 2.5 cm long, which had been carburized to the desired carbon content at 1000°C with an appropriate hydrogen-methane mixture. In order to cool the samples to room temperature with a minimum change of carbon content and absence of cracks they were quenched in a Cerro Bend bath at 480°C, followed by a water quench to room temperature. Three cylinders were suspended in the furnace1 in a purified helium atmosphere, by a closed end, thin wall, silica tube which also served as a thermocouple well. The top and bottom cylinders served only as a means of making the temperature gradient along the center cylinder more uniform. The temperature was determined with a platinum-platinrhodium thermel calibrated by comparison with a thermel certified (* 0.5OC) by the National Bureau of Standards. After holding in the temperature gradient for 24 to 72 hr the samples were quenched in Cerro Bend at 480°C, followed by

Jan 1, 1960

By O. D. Gaither

This paper is an analytical study of the flow of fluids through small vertical conduits. Small conduits are defined as 11/4-in. nominal diameter tubing size and smaller, and approximately twice this area for annular conduits (i.e., 1- X 21/2-in. annulus and smaller). Experimental data are presented for the 1-X2-in. and 11/4- X 2%-in. annuli, and the I-in. and 11/4-in. tubing, since these represent the small conduit sizes and configurations generally encountered in oilfield applications. Data have been gathered for these conduits for single-phase water, single-phase gas and two-phase water-gas mixtures, with particular emphasis on high gas-liquid ratios. Water rates in excess of 2,000 BID and gas rates in excess of 2.5 MMcf/D, and two-phase flow ratios in between these two, represent the scope of the data gathered. Existing equations have been applied to predict flowing pressures and compared with experimental data. New correlations have been developed. INTRODUCTION The increased economic pressure on the domestic oil industry in the United States has constantly required the use of new techniques and equipment designed to reduce the cost of finding and producing oil and gas. Since tangible items are most readily apparent in economic analysis, the advent of lower-cost well completions was inevitable. One of the methods used to reduce costs which has received widespread attention is the slim-hole completion technique where tubing is used as the well casing and in which small conduits are used for tubing if necessary. Small conduits, defined by Kirkpatrick1 as "11/4-in. diameter nominal tubing and smaller for tubing flow and less than twice the 11/4-in. diameter nominal tubing internal flow area for annulus flow", have also found widespread usage as siphon strings for de-watering gas wells and as "kill" strings in deep high-pressure oil and gas wells. The growing use of small-diameter tubing has resulted in an increased need for development of improved methods to measure or predict flowing bottom-hole pressures since the physical dimensions generally preclude the use of subsurface-recording pressure gauges. Even in the cases where small bombs are available, the relatively high velocities encountered at nominal flow rates make it necessary to use excessive weight bars or special hold-down devices. Attempts to use recognized correlations to accurately predict flowing or gas-lift performance in wells equipped with small conduits have been generally unsuccessful. Insufficient field data were available to allow the development of a correlation on this basis, and an experimental approach was applied in an attempt to obtain a workable relation. The experimental approach used to obtain the data presented in this paper was actually a compromise between a field installation and a laboratory study. A test well 1,000 ft in length was used to obtain flow data on single-phase liquid, single-phase gas and two-phase water-gas flowing mixtures. Liquid rates up to 2,200 B/D and gas rates up to 3 MMcf/D were used in the single-phase flow studies. Two-phase flow rates from 100 to 600 B/D with gas-liquid ratios from 500 to 8,000 cu ft/bbl were recorded. Experimental data were obtained for single- and two-phase flow through 1-in and 11/4-in. nominal tubing, and through the annuli between 1- and 2-in. and 11/4- and 2%-in. nominal tubing strings. Experimental results for the two-phase flow are compared to the Poettmann-Carpenter correlation2 which is widely used as a comparative standard for development of multiphase flow predictions in flowing and gas-lift wells. Correlations developed by Tek,3 Baxendell and Thomas" were also investigated. The experimental data recorded herein fell in between the two flow regimes as defined by Ros," and this correlation also failed to yield satisfactory results. The fact that existing correlations failed to confirm the experimental data led to the need for development of a new correlation. Although a two-phase flow study was the primary objective of this investigation, data were also recorded for single-phase flow of water and gas, and constants were developed relating to pipe roughness and equivalent diameters for annular flow. These single-phase studies assisted materially in the development of certain of the two-phase flow results. Considerable previous work has been published which presented relationship of surface measurements to bottom-hole condition. The works of Buthod and Whiteley,6 Jones,' Poettmannb and the Texas Railroad Commission" are classic examples of the successful use of mathematical relationships which allow acceptable predictions of subsurface pressures, when gas is the flowing fluid. Darcy and others have derived relationships which may be used with minor modifications to predict subsurface flowing conditions in injection and water-supply wells. As previously stated, the application of the single-phase flow relationships

By M. E. Wadsworth, W. H. Dresher, W. M. Fassell

HIGH temperature-high pressure techniques have long been used to great advantage in the organic chemical industry, the petroleum industry, and the paper industry. Only recently, however, have these methods been used to extract metals from their ores on a commercial scale. The Chemical Construction Corp., together with interested producers of nickel and cobalt, has done much to develop methods of producing nickel and cobalt powders by the use of high temperature-high pressure techniques.' The Howe Sound Co. is currently operating a plant near Salt Lake City in which the new Chemical Construction Corp. technique is applied to cobalt-arsenic sulfide concentrates. In this method the concentrates are leached in a dilute solution of sulfuric acid under air pressure at a high temperature. Near Edmonton, in Alberta, Canada, the Sherritt Gordon Co. is also using the new method in conjunction with its ammoniacal leach process.' National Lead Co., at Fredricktown, Mo., is operating a process similar to that of Howe Sound. In spite of the rapid growth of high temperature-high pressure hydrometallurgical processes, there has been very little work done on fundamental principles involved in this type of process. Conse- quently the literature lacks any significant data in this field. Oxidation of pyrite,3 sphalerite,4 galena," and recently molybdenite" in alkaline solutions has been reported to some extent. This investigation was initiated, therefore, to broaden the application of high temperature-high pressure hydrometallurgy and also to contribute some insight into the basic mechanisms of oxidation in an aqueous medium under these conditions. In addition to the immediate consequences of these processes much valuable information remains to be learned about fundamental reactions when they are carried out at temperatures and pressures slightly higher than those normally encountered. Leaching of molybdenite by alkaline solutions under oxygen pressure has recently been reported in the Russian literature by E. S. Usataya,6 ho found that leaching rate increased with an increase in the pH of the solution—the strongest effects being observed at a pH of 10—and also with an increase in temperature. Usataya also has reported the formation of a protective film on the surface of the molybdenite when the leaching solution was weakly alkaline, neutral, or acidic. He believes that this oxidation process explains the migration of Mo++ in the oxidation zones of molybdenite ore deposits and the subsequent impoverishment of the ores. Equipment: The high temperature-high pressure reaction unit used in this work was especially designed for kinetic studies of this nature, emphasis being placed on accuracy of measurement and precision of control. As details of the unit's construction and operation have been discussed elsewhere,' only basic features and principles of operation will be discussed at this point.

Jan 1, 1957

By D. J. DeLazaro, W. Rostoker, R. E. Riley, M. Hansen

KNOWLEDGE of the isothermal transformation behavior and the TTT chart method of graphically summarizing such information has been of invaluable aid to the ferrous metallurgist in understanding and developing heat treatments intended to provide specific mechanical properties. It is to be expected that similar lines of study directed to titanium-base alloys will be as profitable. This paper summarizes, on conventional TTT charts, the isothermal transformation products and pertinent reaction rate data for binary alloys of titanium containing 1, 3, 5, 7, 9, and 11 pct Mo, respectively. The results so presented were derived from metal-lographic examination. Some X-ray diffraction work was done to clarify certain points of question. Ti-Mo System To the authors' k.nowledge, TTT charts have only been used to describe the reaction rates of eutectoidal decompositions. It would seem that the kinetics of decomposition of any unstable solid solution might be conveniently described in this manner. The equilibrium diagram of the Ti-Mo system' is shown in Fig. 1. The similarity with the Fe-Ni system will be recognized. Additions of molybdenum serve to stabilize the /3 phase to increasingly lower temperatures. The solubility of molybdenum in the a phase is restricted to less than 1 pct at 600°C. Under normal conditions. a homogeneous ,8 structure quenched to a, temperature in the a f & field will reject a of invariant composition. The rate at which this occurs depends on the degree of undercooling and the degree of supersaturation of /3. The structural character of the rejected phase may also be expected to be related to the undercooling. Materials and Experimental Methods A sponge titanium was used which has a nominal impurity content as reported in Table I. The nominal composition of the molybdenum used is also included. The alloys were prepared in 150 g melts by arc melting in an evacuated water-cooled copper crucible of the type reported in an earlier paper.' The pancake-type ingots were forged to 1/4x1/4 in. bars and homogenized for 24 hr at 1000°C in evacuated Vycor bulbs. Specimens Vi in. thick were cut from these bars for heat treatment. The heat treatment cycles followed an invariant procedure. The specimens were soaked at 1000°C for 20 min under a helium protective atmosphere prior to quenching into a lead bath held at a temperature corresponding to a chosen degree of undercooling. After a prescribed period of time at this temperature, the specimen was removed and water quenched. A series of specimens so treated for progressively longer periods served to establish the times for initiation and completion of the decomposition of the /3 phase at a particular temperature. Although heat treatment of unprotected specimens in a lead bath does permit surface contamination by lead diffusion, this method is necessary to insure sufficiently rapid quenching rates. As long as the bath treatments were of less than 1 hr duration. the contaminated surface was not unduly deep and could be removed without excessive grinding. Metal-lographically, the contaminated zone could be readily distinguished from the pure binary alloy. Transformation Characteristics of Ti-Mo Alloys Metallographic examination showed that a supersaturated p phase may decompose by one of two processes. Alloys containing 1 to 9 pct Mo, when quenched in water from the homogeneous /3 field,

Jan 1, 1953