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By W. V. Green

Creep of tantalum was measured at temperatures from 0.6 to 0.89 of the absolute melting temperature. The creep curves include first, second, and third stages. Steady-state creep rate depends on the fourth power of stress. The activation energy for creep throughout this temperature range is approximately 114 kcal per mole, measured by the aT technique. Subgrain formation occurs as a result of creep strain, and pile-up dislocation arrays are observed in etch-pit patterns. BECAUSE of its high melting point-which is exceeded only by those of rhenium and tungsten—and its high room-temperature ductility compared to most of the other high-melting-point metals, tantalum will undoubtedly be utilized in an increasing number of high-temperature applications. Alloying studies directed toward increased high-temperature strength must use data on tantalum itself as a base line in order to evaluate the effectiveness of the alloying additions. However, to date, no systematic study of creep of tantalum at temperatures above one-half of its melting point has been reported in the literature. Conway, Salyards, McCullough, and Flagella1 have measured linear creep rate of tantalum sheet as a function of stress, but at only one temperature, 2600°C. This paper describes a relatively thorough study of the high-temperature creep of tantalum. METHOD Material Tested. The commercially supplied, l/2-innch-diameter tantalum rod used for this work was electron-beam-melted, cold-forged, rolled, swaged, cleaned chemically, and vacuum-annealed for 1 hr at 1000°C, all by its manufacturer. The vendor's analysis included 60 to 170 ppm C, 3.4 to 4.2 ppm H, 60 to 80 ppm 0, 15 ppm N, and a hardness ranging from 66 to 81 Bhn and averaging 76 Bhn. Creep eimens Used. Two creep-tested specimens are shown in Fig. 1. The 1/4 in.-diameter gage section was 3/4 to 1 in. long, and terminated either at shoulders 5 mils high or at 20-mil-diameter tantalum wires spot-welded to the circumference of the gage section. Both kinds of shoulders served equally well as fiducial marks for optical strain measurements. The spot welding did not alter the creep behavior in any detectable way; the 5-mil- high sharp shoulders did not result in any detectable localized effect on the strain. Before testing, each tensile bar was first mechanically polished -id then electrochemically polished according to the method referred to by Forgeng2 as the "Thompson Ramo Woolridge" method, which was suitable for tantalum after small adjustments of technique were made. Two tensile bars tested at low stresses had 1/8-in.-diameter gage sections and utilized only the weight of the bottom grip for the applied load. Although these diameters were smaller than were desired for other reasons, applied loads were known with high precision in the tests in which they were used. Testing Procedure. Two different constant-load creep-testing machines were employed, one of which has been described by Smith, Olson, and Brown.3 In both, the tensile bar is held vertically on the axis of a cylindrical tungsten tube or screen heater by threaded tungsten grips. The tensile bars and associated grips are heated by radiation from the incandescent heaters, which are heated by their own electrical resistance. Both testing machines use pins to hold the bottom grips in place. The load is applied to a tensile bar through hanging weights, a constant force-multiplication lever, a pull rod sealed to the chamber lid, and a top grip threaded to the pull rod at one end and to the tensile bar at the other. In one machine, the vacuum seal is a bellows with a low spring constant; in the other, the seal involves a rotating "0 ring". With the latter, rotation is converted to translation with a crank shaft, so that elongation of the tensile bar is accommodated with no change of tensile load. The incandescent tensile bar is viewed by an external optical system through slots in the radiation shields and heater, and an enlarged image is projected on a ground-glass screen. Gage-length measurements are made on this image with cathetometers on traveling microscopes. With regard to creep-test results, the two machines were identical. Thorium oxide coatings were applied to the threaded ends of the tensile bars, to prevent diffusion welding of the tensile bars to the grips during testing. Specimen temperatures were measured with an L. & N. optical pyrometer which had been calibrated against a standard carbon arc, and were corrected fir window absorption by calculation from the measured spectral transmittance of the quartz observation windows. Longitudinal temperature gradients in the tensile-bar gage length and temperature drifts during testing were detectable but small, and were estimated to be 10°C or less. Accuracy of temperature measurement was confirmed by comparing the temperature measured on the surface of a special

Jan 1, 1965

By J. B. Cohen, S. L. Sass

The nucleation process for y', Ni3Ti, is shou'n to change from heterogeneous to uniform as the undercooling within the phase boundary increases. As unifornz nucleation beconres copious, (100) alignment is observed in the early stages of aging; howecer. whether or not the alignment is due to spinodal decomposition could not be determined. The presence oi a large-scale reversible segregation of titanium and not the intermediate precipitate y' may be the cause of the initial strengthening in this alloy system and the discrete regions detected magnetically by Ben-Israel and Fine. Evidence is presented for the role of dislocations in the formation at long aging tines oJ the equilibrium precipitate . ThE nickel-rich portion of the Ni-Ti phase diagram consists of a terminal fcc solid solution of titanium in nickel called y.' For temperatures below 1290°C if the solubility limit is exceeded and the temperature is high enough, the excess titanium will combine with nickel to form q, Ni3Ti, a four-layer hcp ordered structure with stacking sequence ABAC."~ Since a change in structure is involved, formation of q is slow and a metastable precipitate referred to as y' forms. This metastable precipitate is an ordered cubic phase in the unconstrained state having a structure similar to Cu3Au (LIZ) with the composition Ni,Ti."'5 From X-ray studies,8, 7 the following sequence is indicated for the precipitation reaction at low temperatures: 1) The appearance of satellites around low-index diffraction spots and splitting of high-index spots, indicating the formation of a slightly tetragonal phase in an imperfectly periodic arrangement. The tetragonal phase is y' or the depleted matrix, depending on the volume fractions of matrix and precipitate (and hence, the alloy composition); tetragonality apparently arises from coherency strains. 2) The appearance of diffraction spots from the equilibrium second phase, q. Ben-Israel and Fine'" used magnetic methods to measure the changes in matrix composition during aging, and to estimate the precipitate composition in a Ni-10.1 at. pct Ti alloy. They observed that the alloy, solution-treated at 1270°C and quenched, contained heterogeneities with discrete compositions which gradually vanished upon aging. It was suggested that y' may initially form as a defect structure with several possible compositions deficient in titanium as compared to Ni3Ti; the composition Ni3Ti develops with prolonged aging. The initial composition was Ni6Ti which would require a very large deviation in stoichiometry for y'. It was noted that at 700°C the precipitation reaction was 80 pct complete after 2 hr and that the volume fraction of second phase was 0.2 after 1 hr. Mihalisin and Decker' suggested that the equilibrium precipitate, besides being nucleated at grain boundaries, could also form at stacking faults. ~errick" examined the formation of in Ni-Cr-Ti, and suggested that a collapsed vacancy cluster within y' acted as a nucleus for intragranular q at high temperatures, 820" and 900°C. After long aging times at lower temperatures, 650" and 750°C, diffraction patterns taken from regions containing ribbons of stacking faults showed spots associated with q. Aging greatly enhances the mechanical properties of these alloys, even at high temperatures, and the metastable precipitate y' is thought to be responsible.' At 600°C the hardness of a Ni-10.1 at. pct Ti alloy increases rapidly during the first 20 hr of aging and continues to increase slowly thereafter.'" At 700°C the hardness reaches a maximum at 1 to 2 hr and then decreases.l1 In this paper the kinetics of formation of y' and the mechanism of transformation to in a Ni-Ti alloy are described. Evidence is presented that suggests that large-scale regions of titanium segregation are present initially and these may have an important influence on the initial strengthening of the alloy: these regions may be the heterogeneities detected by Ben-Israel and Fine. I) EXPERIMENTAL TECHNIQUES The Ni-10.3 at. pct Ti-0.6 at. pct A1 alloy was prepared by vacuum melting. Its chemical analysis is given in Table I. A 0.007-in.-thick strip was sandwiched between foils of the alloy and placed in an open Vycor tube with titanium chips (to get oxygen) and solution-treated for ; hr at 1150°C in a Globar Furnace under a flowing argon atmosphere. Following a quench into an ice-brine mixture at -5" to -2"C, a sample to be aged at temperatures up to and including 700°C was sealed in an evacuated Vycor capsule before being put into a fused salt bath. Aging above 700°C was carried out on bare samples in a salt bath. When removed from this bath and quenched into an ice-water mixture, the sample was normally coated with a thin layer of oxide easily removed with emery

Jan 1, 1970

By K. A. Jackson, J. D. Hunt

A new classification of eutectics is proposed, based on tlze entvopies of wzelting of the tuio eutectic phases. The clnssification was used to predict suitable tvansparent analogs of the metallic systems. Experimental confir?nation loas obtained for the theovetical shape of the lamellar solid-liquid interface, fov the fault mechanisms of lanzellar spacing changes, and for the development of low-energy solid-solid boundaries between the lamellae. An explanation is presented to account jov the irvegular and coinplex regular structures zrhich are found in some eritectic systems. FrOM experimental observations, single-phase materials can be divided into two groups according to their solidification characteristics, those that grow as faceted crystals and those that do not. acksonl' showed from thermodynamic reasoning that the type of growth depended on a factor a which was almost thg entropy of melting. Most nonmetals have high entropies of melting (a greater than 2) and grow with crystalline facets. Most metals have low entropies of melting (CY less than 2) and grow almost isotropically with no facets. The authors propose that eutectics may be classified in a similar manner. There are three groups of eutectics, those in which both phases have low entropies of melting, those in which one phase has a high and the other phase has a low entropy of melting, and those in which both phases have high entropies of melting. Lamellar or rodlike structures are formed in systems in which both phases have low entropies of melting. In these alloys dendrites of either phase may be formed, when the alloy is rich in the relevant component. Examples are Pb-Sn, Sn-Cd, Pb-Cd, Sn-Zn, Al-Zn. Irregular, Fig. 14((), or complex regular, Fig. 14(b), structures are formed in alloys in which one phase has a high entropy of melting and the other has a low entropy of melting. Examples are A1-Si, Zn-MgzZnll, Pb-Bi, Sn-Bi. When the alloys are rich in the low entropy of melting phase, dendrites are formed; when the alloys are rich in the high entropy of melting phase, faceted primary crystals are produced. These crystals are sometimes called hoppers or pseudodendrites. In this work the term dendrite will only be used to describe nonfaceted primary crystals. Dendrites are not formed during solidification in high entropy of melting single-phase materials. The third group of eutectics includes alloys in which both phases have high entropies of melting. Each phase grows with a faceted solid-liquid interface. Since most metals do not have high entropies of melting, metallic examples in this eutectic group are rare. However they may occur between some intermetallics and semiconductors or semimetals such as silicon, germanium, and bismuth. Attempts have been made to study eutectic solidification visually by watching the growth process.374 Since metals are not transparent, the observations had to be made on external surfaces. This difficulty can be overcome by using transparent analogs of the metallic systems. As was mentioned earlier, most single-phase compounds have entropies of melting greater than 2 and so grow as faceted crystals. Recently organic materials with entropies of melting less than 2 were investigated.' These materials grow in exactly the same way as the low entropy of melting metals. When the materials are pure, they grow with a solid-liquid interface parallel to an isotherm; when they are impure, cells or dendrites are formed. Since these materials are transparent, have low melting points, and even have cubic structures, they should be ideal for making up transparent analogs of the metallic eutectics. The purpose of the present work was to investigate these organic eutectics and to see whether this quite different series of eutectics could be classified in the same way as the metallic systems. The observations made on the organic alloys are also discussed with reference to the current theories of lamellar growth. Explanations are proposed to account for the structures formed in the other eutectic groups. EXPERIMENTAL Thin cells containing the organic alloys were uni-direction ally solidified on a specially constructed microscope stage.' Uniform growth rates were obtained by moving the cells, with a motor drive, through a fixed temperature gradient, so that the solid-liquid interface remained stationary with respect to the microscope objective lens. The cells were made by fusing two microscope cover slides 7/8 by 7/8 by 1/100 in. together on three sides, leaving a gap of 1 to 3 mils between the slides, and these were filled by surface tension. A preliminary investigation of the phase diagram between two components could be made very rapidly. One side of the cell was filled with component A and the other side with component B. Since only a small amount of mixing could occur every composition from pure A to pure B was present in the cell. When the cell was placed in the temperature gradient a pictorial representation of the phase diagram was obtained. Eutectics, peritectics, "interorganics", and solid -solid transformations could be readily detected. Fig. 1 shows part of a eutectic phase diagram. The Sample was first grown slowly then stopped. The two

Jan 1, 1967

By AIME AIME

WITH the recent increase in the price of gold, its economic recovery at depths formerly considered impractical has become a present possibility. Two important difficulties must be met: pressure bursts of the rock, and the reduced efficiency of human labor subjected to the higher temperatures and the increased humidity at the greater depths. In the following abstract of a paper by J. H. Dobson, presented before the South African Institution of Engineers on

Jan 1, 1935

By G. K. Zaharlev

With a productive output growing at an annual rate of 8%, the Soviet mining industry should emerge as the world's leader in total mineral output during the 1980's. (The Soviet Union's share in the world's total mineral output in 1973 was estimated at 22 to 23%.) According to estimates by Soviet mining experts, the mineral potential of the Soviet Union will sustain the current 8% annual growth rate in the future.

Jan 12, 1974

By W. R. Hibbard

Evidence is presented which confirms previous findings that models of solution strengthening depending solely on lattice parameter changes are incomplete. Direct evidence for the Suzuki interaction of chemical effects was obtained from alloys with constant lattice parameter, for which solution strengthening was nearly independent of temperature from 300° to 20°K. SOLUTION hardening principles have been reviewed recently by Parker and Hazlett.' In addition, the interactions of dislocations and solute atoms were reviewed by Cottrell.' It is not proposed to review this information again here, but to refer only to those details which are pertinent to the developments which have occurred since these papers were published. Literature Survey To set the stage, it has been known for some time that solid solutions are stronger than the pure parent metals, and that the strength increases with increasing amounts of alloying element. One of the most extensive earlier investigations was that of Lacy and Gensamer,3 who reported that the solid solution strengthening of iron is a power function of the composition, that the relative strengthening is a function of the solubility limit, and that the rate of strain hardening is a function of the amount of solution hardening. Thus, the slope of the plastic portion of the stress-strain curve increases with increasing yield strength. An approach to the development of principles resulted from work by Gulyeav,4 who reported that the strengthening effect of solid solution alloys is periodic in character when plotted as a function of the atomic number of the solute. A more quantitative approach was to relate the amount of solution hardening to the lattice parameter of a solid solution. This was done quite early by Norbury,5 and later by Brick, Martin, and Angier,6 Frye and Hume-Rothery,7 and French and Hibbard. This relationship is only approximate in character. The next development was to relate the amount of solution hardening to lattice stress, as proposed by Frye and co-workers.9 They calculated what they called ionic overlap from the lattice parameter changes represented as a change in volume, using Bridgman's hydrostatic compression equation. The resulting correlation was somewhat improved as compared to the simple correlation with lattice parameter. The next step was carried out by Dorn, Pietrow-sky, and Tietz,10 who suggested an effect of valence differences in addition to the effect of lattice parameter. Their proposed parameter shows flow stress as a single valued function of the concentration and a relationship involving these two atomic variables. In addition, they contributed new data on the temperature dependence of solution hardening which indicated that it was a strong function of temperature for aluminum alloys. Allen, Schofield, and Tate11 carried the valency effect even further by reporting data indicating that with a given solvent element the stress-strain curve is a function of electron density, entirely neglecting the size factor, which varied by a factor of two. This evidence led to a quantum mechanical calculation by Cottrell, Hunter, and Nabarro,12 based on the formation of a dipole around an edge disloca-

Jan 1, 1959

By Ralph Arnold

Since 1915, when Elk Basin field was brought in, eight oil fields have been developed in Montana and the production has arisen from 50,000 bbl. in 1916 to 8,000,000 bbl. in 1926. The production for 1927 was 5,121,600 bbl. and the total up to the end of 1927 was 27,138,239 barrels. The eight fields, with their year of discovery are: Elk Basin, Carbon County (1915); Devil's Basin, Petroleum County (1919); Cat Creek, Petroleum County (1920); Soap Creek, Big Horn County (1921); Kevin-Sunburst, Toole County (1922); Lake Basin, Stillwater County (1924); Pondera, Pondera and Teton counties (1927); and Bannatyne, Pondera and Teton counties (1927). About 170 wildcat wells have been drilled in the state of which 8 were successful and 162 gas wells or dry. Hence, only one out of 21, or 5 per cent. of the wildcats have been successful. The average depth of the wells has been 1600 ft. and the average cost $32,000 apiece. • Up to Jan. 1, 1927, a total of 1376 wells have been drilled in the producing oil and gas fields of the state, of which 904, or 66 per cent., were successful oil wells; 82, or 6 per cent. were gas; and 390, or 28 per cent, were dry. The percentage of dry wells is excessive as compared to the wells in other states, due to the uncertainties of limestone reservoir rocks. The total production of oil to Jan. 1, 1927, has been 22,016,639 bbl. and of gas 7,265,330,000 cu. ft. The average price at the well for the oil has been $1.47 per bbl. and for gas about 4 c. per 1000 cu. ft. The value at the point of consumption has been about 23 c. per 1000 cu. ft. The total revenue derived from crude oil has been $32,277,119, and from gas 8350,613, or a total income to the producer of $32,727,832. Each well drilled in the state has already (to Jan. 1, 1927) averaged a return of over $21,000. The total number of domestic (Montana) oil and gas companies organized, since the first in 1885, has been 844, of which 702 are still alive and 142 dead. Oil and gas companies registered for operation within the state to Jan. 1, 1927, but with outside charters, are 143, of which 66 are alive and 77 are dead. Outside the few distributing companies, which are included in these figures, the grand total of 997 companies which have

Jan 1, 1928

By D. H. Newland

New York has a small but not insignificant place in the oil and natural gas industries of the United States. It has had a continuous record as an oil producer since 1872, with an aggregate yield of about 104,000,000 bbl. The reported output for 1935 was 4,237,000 bbl., a gain of more than 10 per cent for the year and a total that has been exceeded only in the early period of flush production half a century ago. The industry has been steadily building up since 1920 with the successful practice of the water drive, which has given a new lease of life to pools that had been practically drained of oil recoverable by pumping. An additional output of 2000 bbl. or more per acre is being procured by this method. Altogether the fields in New York State cover about 55,000 acres. Their limits are well defined and it is unlikely that they will be extended in the future, although there is some prospect of finding additional supplies by deeper drilling. The oil from New York is all classed as Pennsylvania grade, for which the recent price has been about $2.50 a barrel. It is refined at Olean, Wellsville and Bolivar, in the oil district, and partly in Pennsylvania refineries. Exploration for natural gas, outside of the established districts, was considerable during the year. Altogether 59 wells were drilled, distributed over 13 counties, of which 33 were listed as producers and 26 were dry. At the close of the year, 13 wells were in process of drilling. The 33 producing wells had a combined estimated flow of 278 million cubic feet per day. The best results were obtained from exploration in Allegany County, where out of eight wells drilled to the Oriskany sandstone five were successful and showed a combined open-flow capacity of 107 million cubic feet. The Oriskany sandstone was encountered at a depth of 4500 to 4900 ft. In Steuben County, next east of Allegany County, two out of seven wells to the Oriskany proved productive, and one of these, in the town of Greenwood, on the Watkins structure, was probably the largest that has so far been opened in the state, with a reported yield of 35 million a day. In the central part of New York interest was awakened by the activity shown in exploring for gas in the Trenton limestone, in Camden, Florence and Rome townships, Oneida

Jan 1, 1936

The ability of activated charcoal or carbon to adsorb complex metal ions has been recognized for many years, but it wasn't until the late 1940s and early 1950s that attempts were made to employ carbon-In-Pulp or C. I. P. processing to the recovery of gold. Early plants using the process were those at the Golden Cycle in Cripple Creek, Colorado, the Getchell Mine near Golconda, Nevada, and at the Idria Mine in Honduras. Recovery of the carbon from the pulp was done by screening or flotation, and recovery of gold from the carbon was done by burning the carbon (a very difficult task) or by sending it to a smelter. Unfortunately at the time, the price of gold was still fixed at $3-5 per ounce and labor costs were rising to the point where these mines were no longer able to operate. Consequently, C. I. P. treatment was temporarily forgotten. In the early 1970s, however, Homestake Mining Company at Lead, South Dakota, were being forced by environmental regulations to discontinue the use of mercury for amalgamation in their 7,500 ton per day plant, and at the same time were encountering high labor costs in the slime circuit of the plant, where over 2,000 tons of slimes were filtered each day in Merrill plate and frame filter presses. Shortly before that, researchers of the United States Bureau of Mines had developed the caustic -cyanide method of stripping gold from activated carbon and an electrolytic cell (now known as the Zadra cell) to recover gold from the carbon strip liquor. Homestake and the United States Bureau of Mines then jointly operated a C. I. P. pilot plant at Lead. Results were immediately favorable and a 2,400 ton per day C. I. P. plant was then built to treat the slime fraction of the Homestake ore. (See Au and Ag Cyanidation Plant Practice, Volume I, SME of AIME, 1975. Later, Homestake built a second plant at Creede, Colorado, to treat the slime fraction of the tailings from a silver-lead flotation plant. Next was Duval Corporation's 3,000 ton per day C. I. P. plant at Battle Mountain, Nevada. Both of these latter plants are described in this volume. C. I. P. operations under construction at the time of this writing are as follows: Pinson Mining Co. , Nevada Gold Freeport Gold Company, Nevada Gold Compania Minera El Indio, Chile. Silver and Gold

Jan 1, 1981

By D. H. Newland

New York has a small but not insignificant place in the oil and natural gas industries of the United States. It has had a continuous record as an oil producer since 1872, with an aggregate yield of about 104,000,000 bbl. The reported output for 1935 was 4,237,000 bbl., a gain of more than 10 per cent for the year and a total that has been exceeded only in the early period of flush production half a century ago. The industry has been steadily building up since 1920 with the successful practice of the water drive, which has given a new lease of life to pools that had been practically drained of oil recoverable by pumping. An additional output of 2000 bbl. or more per acre is being procured by this method. Altogether the fields in New York State cover about 55,000 acres. Their limits are well defined and it is unlikely that they will be extended in the future, although there is some prospect of finding additional supplies by deeper drilling. The oil from New York is all classed as Pennsylvania grade, for which the recent price has been about $2.50 a barrel. It is refined at Olean, Wellsville and Bolivar, in the oil district, and partly in Pennsylvania refineries. Exploration for natural gas, outside of the established districts, was considerable during the year. Altogether 59 wells were drilled, distributed over 13 counties, of which 33 were listed as producers and 26 were dry. At the close of the year, 13 wells were in process of drilling. The 33 producing wells had a combined estimated flow of 278 million cubic feet per day. The best results were obtained from exploration in Allegany County, where out of eight wells drilled to the Oriskany sandstone five were successful and showed a combined open-flow capacity of 107 million cubic feet. The Oriskany sandstone was encountered at a depth of 4500 to 4900 ft. In Steuben County, next east of Allegany County, two out of seven wells to the Oriskany proved productive, and one of these, in the town of Greenwood, on the Watkins structure, was probably the largest that has so far been opened in the state, with a reported yield of 35 million a day. In the central part of New York interest was awakened by the activity shown in exploring for gas in the Trenton limestone, in Camden, Florence and Rome townships, Oneida

Jan 1, 1936

AVERY great profit is derived from removing the gilding and retrieving gold, without destroying the works of silver or other metal. If this method did not exist, the greater part of the gold that is put on certain works would be lost. Even though you might think to scrape it off patiently with a sharp scraper, if it had been drawn with draw-plates, or if it were at the bottom of objects where the scraper could not enter easily, it would be utterly in vain. Therefore, I find that to do this it is necessary to use one of three methods. The first is when it is found on a thin object. Take a large crucible, fill it with mercury, and heat it on a little furnace. When you see that it begins to boil and simmer, put your work in it and stir it around, shaking and rubbing it well in this, and finally rub it with a scratching tool until you see that the mercury has drunk up and absorbed all the gold. Then, having done this, take the said mercury and pass it through an untanned leather purse, and in the bottom of this you will find all the gold like sand. Put this in the bottom of a crucible or in something else over a charcoal fire and evaporate it. If the objects are of a thicker form the gilding is removed from them in another way, by covering them with powdered sulphur and lighting a fire on them. When you see them burning well with the fire all around, beat them in a clean bowl of wood or something else and collect everything that separates with the sulphur from the work; this will be gold in the form of a leaf wherever it has been touched by the fire. The gold is then extracted from this burned sulphur by purifying it in a cupeling hearth with lead. The third method is to touch the gold that you wish to take off the works with an aqua fortis made from saltpeter, rock alum, vitriol, sal ammoniac, and some verdigris.* This acid dissolves and eats the gold by virtue of its corrosive power. Having thus touched the gold with this acid and having saturated the latter with a quantity of gold, put it in a cucurbit and evaporate it over a little furnace as is done with silver, collecting the acid and the spirits if you wish.

Jan 1, 1942

By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,' and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80' to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

By Walter Lang

The year 1931 has shown a marked change over 1930 in New Mexico, with respect to the volume of activities attendant upon the petroleum industry. Although the total production of oil and gas this year exceeds that of preceding years, the results have been attained from established units operating under restriction, but capable of supplying far more than the economic conditions justify. The presidential order of March 12, 1929, that "there will be complete conservation of Government oil in this administration," has merely anticipated a normal consequence of overdevelopment. As a result of the combined economic and legal restrictions imposed, very little new drilling has occurred during the year. Even in proven areas the drilling of offsets has been curtailed to the absolute limit of requirements. Scouting and sample-cutting, which in 1930 were still in a state of feverish activity, are at low ebb, and lease buying has reached a condition of stagnation. A number of the major oil companies have either materially reduced their field and office forces or completely eliminated local office representation. Two tests of particular interest, because correlation shows them to be structurally high although they failed to produce, are the National Securities well drilled six miles west of the town of Hobbs, on sec. 33, T.18 S., R.37 E., Lea County, to a total depth of 4272 ft., which developed a flow of 4,000,000 cu. ft. of gas at 3860 ft., and a show of oil; and the Western Drilling Co. No. 1 State, sec. 16, T.20S., R.32 E., Lea County. The latter test found dead oil at 2575 to 2580 ft., and sulfur water at 2745 ft., increasing to 2780 ft., representing the zone from which production was generally expected. The well was drilled to 4013 feet. The discovery of sulfur at about 950 ft. in the deepening of an old water well (Pearson, NE. 1/4 sec. 8, T.16 S., R.25 E.) drilled in the Little Cottonwood area northwest of Artesia led the Union Sulphur Co. to drill three prospect tests on a block of acreage in the vicinity during the summer and fall. The results of the investigation have not been disclosed. The Kummbaca Oil and Gas Co. drilled the T. J. Kerline No. 1, in sec. 34, T.21 N., R.30 E., Harding County, gaging 3,654,000 cu. ft. of 98 per cent CO² at 940 ft. The Barton structure, 20 miles east of Albu-

Jan 1, 1932

By E. J. Rapperport, J. P. Pemsler

We have made calculations to evaluate the sensitivity of atomic absorption as a technique to measure vapor pressure changes with temperature. Our conclusion, supported by the experimental findings presented in this work, is that the ultimate sensitivity of the technique is well below lo-' Torr. This magnitude of vapor pressure sensitivity makes the method extremely attractive for thermodynamic studies. Atomic absorption techniques have been used previously in this connection by Scatchard and Boyd' and by vidale2 with a much lower sensitivity reported. Scatchard and Boyd's work measured cadmium pressure over Ag-Cd alloys in the range 0.02 to 0.3 Torr, and Vidale estimated that sensitivities of only 10"5 to 10"6 Torr are to be expected. Atomic absorption appears to be particularly well-suited to thermodynamic studies for several reasons: A) It is extremely sensitive; our experiments indicate an ability to measure vapor pressure changes of 10"9 Torr. B) It is highly selective; there is seldom interference among the resonant wavelengths of the various species. C) It may be performed in an absorption cell under static conditions. This alleviates such problems as surface impoverishment of alloys, attainment of equilibrium, and temperature measurement and control. D) Simultaneous, or near-simultaneous, vapor pressure measurements may be made for several elements in a given system. Experimental. The physical basis of the technique is the highly selective absorption of particular wavelengths by specific atomic species. In most atomic absorption work the element of interest is incorporated into a hollow cathode lamp to provide a characteristic spectral source of high intensity. The spectra lines characteristic of the element in the cathode are attenuated by atoms of that element in the radiation path. Radiation from silver or cadmium hollow cathode lamps was directed along a path containing a 10-cm evacuated silica cell. The cell was positioned within a silica windowed furnace and contained silver, cadmium, or an Ag-Cd alloy. As the furnace temperature was elevated, the number of atoms of the absorbing element in the vapor phase within the cell rose, and the resonant radiation was increasingly absorbed. Intensities were measured by passing the radiation through a Techtron Model AA-4 one-half meter grating atomic absorption spectrometer equipped with a photo-multiplier detector. In order to minimize instabilities in the source, the hollow cathodes were allowed to warm up for several hours and were run at only 2 5 to 30 pct of their maximum rated amperage. In addition the attenuated beam was monitored before and after each reading. The attenuation of resonant wavelengths may be related to vapor pressure by the following relationships.

Jan 1, 1969

By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,' and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80' to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

By S. Suphi Yavasca, A. M. Gaudin

THIS paper is intended as a contribution to our knowledge of the mechanism of comminution and of the work of crushing. In a previous paper' it was shown that with quartz comminution proceeds as follows I. The size distribution of broken fragments made by a single fracture is such that the new surface on each grade is the same. 2. Multiple fracturing results in a size distribution such that in the fine sizes the surface per grade is the same in every grade; in coarse sizes the surface per grade decreases gradually with increasing size. In that paper it was mentioned that determinations on minerals other than quartz were in course of completion in order to establish the generality of these observations. In this paper, condensed data2 are presented for galena, pyrite and glass. Galena and pyrite are crystalline material and glass is noncrystalline. Galena has excellent cubic cleavage. Pyrite, although cubical, does not have marked cleavage. Quartz, on which the original determinations were made, does not cleave and although crystalline (hexagonal) breaks conchoidally. Glass breaks much like quartz. It is apparent, therefore, that the minerals selected represent some range in character of the solid without covering all possible types. GLASS Fifteen glass marbles were crushed individually in the pendulum crusher described in the preceding paper,1 then subjected to careful screening for 30 min. Six sized fractions were selected and cleaned in a hot 0.12 N solution of hydrochloric acid, washed with distilled water and dried on a hot plate. This was followed by an examination with a binocular microscope, to remove foreign matters not eliminated in cleaning as well as to eliminate "compacts" of fine particles. These compacts are groups of fine iragments that seem to be mechanically stuck together as a result of localized compacting during the comminution operation. The presence and the abundance of these compacts may be related to the amount and direction of the forces applied in different crushing devices. Since, properly, such compacts should be entirely eliminated in the sizing analyses, it is necessary to remove them to the last before making surface determinations on sized fractions. For example, with a - 28 + 35-mesh glass the surface areas of two samples, one cleaned with acid and under the binocular, the other only washed, were 102 and 172 sq. cm. per gram, respectively. Examination of the samples under an Ultropak microscope showed that washing alone failed to remove the compacts and also that it fails to remove certain fine dusts attached to the particles. Cleaning with acid loosens the fine dusts and

Jan 1, 1945

F. G. CLAPP, New York, N. Y. (written discussion *).-Whatever processes of appraisal have been found most correct and feasible in one field or group of fields will generally prove most adaptable in others. So far as the California fields are concerned, Mr. Requa's paper appears to outline the most up-to-date processes of appraisal. It remains, then, to discuss and adapt these and to make such revisions in methods and processes of calculation as will give us results elsewhere. The trouble about most attempts to place a value on oil lands, whether in this country or elsewhere, has been that many of the so-called "experts" called upon to express an opinion either have not possessed the requisite engineering and geological knowledge to make an accurate appraisal of the lands, or that they were not furnished with sufficient information for the purpose in hand. The Independent. 011. Producers' Agency of California, for whom Mr. Requa's original report was prepared, had many advantages in this respect not generally available to engineers making reports, as all existing information seems to have been at the experts' disposal within the limits of a large number of properties, practically commensurate with the extent of the fields in question. Hence the report could be and was more accurate than any similar report for a single company is likely to be in other fields. Very few companies are so exempt from competition that all the data on neighboring leases of other companies will be freely turned over to them. In many companies, certain available data are concealed from the engineer who makes the reports, particularly if the properties are supposed to be worth less than their apparent value. In the case of other companies, having the best of intentions, the data are insufficient to help the engineer greatly in his appraisal, simply because the oil business has been so, unsystematic in most fields that only the largest and wisest companies have kept accurate figures regarding runs and gravity of oil from individual wells and from different depths. In many wells, which ran wild for clays or weeks in the older fields, there was a waste which is not recordable with exactness. These and many other difficulties confront even the most experienced expert in actual practice outside of the California fields. We may justly say, therefore, that an engineer in other fields of the United States and in the European, South American and Asiatic fields, must not only begin where the Independent Oil Producers' Agency

Jan 4, 1918

By S. Suphi Yavasca, A. M. Gaudin

This paper is intended as a contribution to our knowledge of the mechanism of comminution and of the work of crushing. In a previous paper1 it was shown that with quartz comminution proceeds as follows: 1. The size distribution of broken fragments made by a single fracture is such that the new surface on each grade is the same. 2. Multiple fracturing results in a size distribution such that in the he sizes the surface per grade is the same in every grade; in coarse sizes the surface per grade decreases gradually with increasing size. In that paper it was mentioned that determinations on minerals other than quartz were in course of completion in order to establish the generality of these observations. In this paper, condensed data1 are presented for galena, pyrite and glass. Galena and pyrite are crystalline materials and glass is noncrystalline. Galena has excellent cubic cleavage. Pyrite, although cubical, does not have marked cleavage. Quartz, on which the original determinations were made, does not cleave and although crystalline (hexagonal) breaks conchoidally. Glass breaks much like quartz. It is apparent, therefore, that the minerals selected represent some range in character of the solid without covering all possible types. Glass Fifteen glass marbles were crushed individually in the pendulum crusher described in the preceding paper,' then subjected to careful screening for 30 min. Six sized fractions were selected and cleaned in a hot 0.12 N solution of hydrochloric acid, washed with distilled water and dried on a hot plate. This was followed by an examination with a binocular microscope, to remove foreign matters not eliminated in cleaning as well as to eliminate "compacts" of fine particles. These compacts are groups of he irag-ments that seem to be mechanically stuck together as a result of localized compacting during the comminution operation. The presence and the abundance of these compacts may be related to the amount and direction of the forces applied in different crushing devices. Since, properly, such compacts should be entirely eliminated in the sizing analyses, it is necessary to remove them to the last before making surface determinations on sized fractions. For example, with a — 28 + 35-mesh glass the surface areas of two samples, one cleaned with acid and under the binocular, the other only washed, were 102 and 172. cm' per gram, respectively. Examination of the samples under an Ultropak microscope showed that washing alone failed to remove the compacts and also that it fails to remove certain fine dusts attached to the particles. Cleaning with acid loosens the fine dusts and

Jan 1, 1947

By M. J. Pool, P. J. Spencer, J. R. Guadagno

THE present work was carried out as part of a general program to study the magnitude and concentration dependence of exothermic heats of solution of various metals in liquid tin. Thermodynamic data for the Te-Sn system are very limited, particularly for dilute alloys. Indeed, apart from the prior heat of solution determinations of Pool,1 the only other published values are those of McAteer and seltz2 who carried out electromotive force measurements on solid alloys of compositions from 75 to 95 at. pct Te at temperatures between 543° and 668° K, of Colin and Dro-wart3 who made mass-spectrometric studies of the vapor in equilibrium with solid SnTe, and of Robinson and Bever4 who determined the heat of formation of SnTe by solution calorimetry. The present work thus provides further thermodynamic information for this system, specifically in a temperature range where the solubility of tellurium is very limited. The liquid metal solution calorimeter used in this investigation has been described previously.' No further discussion of its design or operation will therefore be given here. For each series of measurements a tin bath consisting of approximately 70 g of 99.99 pct pure Sn was carefully weighed out and inserted in the calorimeter which was maintained at the desired temperature to within ± 1/4°c. Tellurium, of 99.999 pct purity, was supplied by Atomergic Chemetals Co., a division of Gallard-Schlesinger Chemical Manufacturing Corp. Approximately 0.0006 to 0.001 g-atom specimens of tellurium were used for each experimental run and these were added to the calorimeter from a temperature of 273" K. Heat of solution values were calculated by analysis of a strip-chart recorder plot of the heat effect accompanying the solution of each sample in the tin bath. The heat capacity of the latter was determined at regular intervals during a series of tellurium drops by using pure tin or tungsten calibration samples, the heat contents of which were obtained from the standard compilation of Hultgren et al5 The composition of the bath was calculated after each drop from a knowledge of the weights of tin and tellurium added. Values of the heat of solution of tellurium at 725" and 775° K are listed in Table I together with the corresponding tellurium contents of the alloys. The data are also plotted as a function of tellurium concentration in Fig. 1, which includes the equivalent data obtained by pool' at 750° K. It can be seen that the heat of solution remains

Jan 1, 1969

By S. Suphi Yavasca, A. M. Gaudin

This paper is intended as a contribution to our knowledge of the mechanism of comminution and of the work of crushing. In a previous paper1 it was shown that with quartz comminution proceeds as follows: 1. The size distribution of broken fragments made by a single fracture is such that the new surface on each grade is the same. 2. Multiple fracturing results in a size distribution such that in the he sizes the surface per grade is the same in every grade; in coarse sizes the surface per grade decreases gradually with increasing size. In that paper it was mentioned that determinations on minerals other than quartz were in course of completion in order to establish the generality of these observations. In this paper, condensed data1 are presented for galena, pyrite and glass. Galena and pyrite are crystalline materials and glass is noncrystalline. Galena has excellent cubic cleavage. Pyrite, although cubical, does not have marked cleavage. Quartz, on which the original determinations were made, does not cleave and although crystalline (hexagonal) breaks conchoidally. Glass breaks much like quartz. It is apparent, therefore, that the minerals selected represent some range in character of the solid without covering all possible types. Glass Fifteen glass marbles were crushed individually in the pendulum crusher described in the preceding paper,' then subjected to careful screening for 30 min. Six sized fractions were selected and cleaned in a hot 0.12 N solution of hydrochloric acid, washed with distilled water and dried on a hot plate. This was followed by an examination with a binocular microscope, to remove foreign matters not eliminated in cleaning as well as to eliminate "compacts" of fine particles. These compacts are groups of he irag-ments that seem to be mechanically stuck together as a result of localized compacting during the comminution operation. The presence and the abundance of these compacts may be related to the amount and direction of the forces applied in different crushing devices. Since, properly, such compacts should be entirely eliminated in the sizing analyses, it is necessary to remove them to the last before making surface determinations on sized fractions. For example, with a — 28 + 35-mesh glass the surface areas of two samples, one cleaned with acid and under the binocular, the other only washed, were 102 and 172. cm' per gram, respectively. Examination of the samples under an Ultropak microscope showed that washing alone failed to remove the compacts and also that it fails to remove certain fine dusts attached to the particles. Cleaning with acid loosens the fine dusts and

Jan 1, 1947