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By M. B. Standing, R. I. Parsons, E. N. Lindblad

The recovery of the heavier components from a gas cap or retrograde pool is shown to be the greatest when the sand is cycled with a dry gas at a low pressure. This conclusion is in direct opposition to the belief that the most efficient production program is pressure maintenance and cycling at or near the dew point. The results are calculated from: (I) constant volume, variable composition pressure-volume-temperature tests on a mixture of trap gas and liquid from a producing well; (2) published equilibrium constant data and the measured composition of the dew-point material; and (3) the fact that in a sand section of homogeneous permeability, injected gas displaces reservoir gas nearly, quantitatively. The results are based on the simplifying assumption that variable permeability systems may be defined by the ratio of two statistical parameters, and that gas injected into an actual sand will behave as though the sand were composed of many layers, each of constant permeability. Introduction Pressure decline in gas-condensate type reservoirs is accompanied by the formation of a liquid phase throughout the reservoir. Over the past ten years the processing of the material from these types of reservoirs for the heavier hydrocarbon components and the return of the light fractions to the reservoir ("cycling") has become increasingly popular. It has often been stated that the purpose of such a program is to prevent the loss of the retrograde liquid phase formed in the reservoir. The purpose of this paper is to present the results of laboratory tests and computations concerned with several possible methods of producing a gas cap or condensate type of reservoir. The results show that the recovery of heavier hydrocarbons for this type of reservoir is not a maximum under conditions of cycling at or near the dew-point pressure. Instead, variations in permeability and the ability of the dry injected gas to revaporize condensate, point to cycling at a considerably reduced pressure as the optimum production-method. In addition the paper suggests a way of evaluating sands for their permeability variation. The calculations presented in the following sections of the paper are in terms of the production of the butanes and heavier fraction from the gas cap of a field which had an original pressure of approximately 3000 psi. Specifically, the calculations show: 1. To what extent the condensate formed in the reservoir after pressure decline can be recovered by the cycling of a dry absorber-plant gas through the sands. 2. Whether there would be greater recovery of hydrocarbons if cycling were instigated at the original reservoir pressure.

Jan 1, 1948

Development: Iron Ore In Peru Utah Construction Co., of San Francisco and a Peruvian Government corporation have signed an agreement for development of a large iron orebody in Peru. Most tests show 60 pct iron or better. Most of the ore is magnetite. Although ore will be shipped mainly to Eastern U. S. blast furnaces, shipments to the West Coast may develop as the orebody opens up. The construction firm indicated three American steel companies have shown interest in the project. The orebody is located 300 miles south of Lima and about 15 miles from the coast at the same longitude as New York City. Allen D. Christensen, executive vice-president of Utah Construction noted that the distance is shorter between Peru and the East Coast. The ore deposit measures about four to five miles in one direction and 10 miles in the other. As many as 15 outcroppings within these limits have been reported. Several of the outcroppings are thousands of feet long by several hundred feet wide, Christensen said. Shipments between 100,000 and 200,000 tons of ore per month are projected by the company. Cost of opening the mine to production may go over $5 million, Christensen said. It would include building of docks for ocean going vessels, housing, and heavy duty mining and processing equipment. The contract with the Peruvian government gives Utah Construction six to eight months for additional tests and a 20 year concession for mining the orebody. Peru will collect royalties on all ore. The company will also supply about 300,000 tons per year for an electric furnace to be installed by the Peruvian Government at Chimbote. No steel is produced in Peru now. Utah Construction formed the Argonaut Mining Co. last year, and was shipping iron ore from British Columbia to Japan at a rate of more than 50,000 tons a month, before winter weather decreased operations.

Jan 1, 1952

By Mark J. Klein

The creep of 043 was studied over the temperature range 1650" to 3200°F and over the stress range 3000 to 44,000 psi. The steady-state creep rate over this range of stress and temperature can be expressed by the equation where A is a constant, is the stress, and is -0.8 x 103 psi-'. Over a narrow range of stress variations c0 a and for this proportionality n varies from 3 to 30 in accordance with the relation n = aB. Above about 2400° F, H, the apparent activation energy for creep, is 110,000 cal per mole, a value about equal to that estimated for self-diffusion in this alloy. Below 2400°F, H increases with decreasing temperature reaching a value of -125,000 cal per mole at 1700° F. In this temperature region, H appears to be a function of the interstitial concentration of the alloy. MOST of the detailed creep studies of dispersion strengthened metals have been concerned with metals having fcc structures. However, there are a number of important refractory alloys with bcc structures that derive part of their high temperature strength from an interstitial phase and whose creep behavior has not been well defined. This paper describes the creep behavior of the bcc alloy, D43, over the temperature range 1650" to 3200°F (0.4 to 0.7 Thm) and over the stress range 3000 to 44,000 psi. In addition to colum-bium, this alloy contains 10 pct W. 1 pct Zr, and sufficient carbon (-0.1 pct) to form a carbide dispersion throughout the matrix of the alloy. The effects of variations in temperature and stress on the steady-state creep rate of this alloy are presented in this paper. EXPERIMENTAL PROCEDURES Creep tests were made in a vacuum of 106 torr under constant tensile stress conditions using a Full-man-type lever arm.' Creep specimens were machined from 0.020-in. D43 sheet (grain size -5 x l0-4 in.) processed in a duplex condition (solution annealed -2900°F, 40 pct reduction in area, aged 2600°F). The specimens were tested in this condition without further heat treatment. Specimen extensions over 1-in. gage lengths were continuously recorded using a high temperature strain gage extensometer. Differential temperature and stress measurements were used to determine temperature and stress dependencies of the creep rate. Activation energies were calculated from the changes in strain rate induced by abrupt shifts in the temperature during constant stress creep tests. The 100°F temperature shifts used in most of the activation energy determinations required 15 to 90 sec depending upon the temperature at which the shift was made. The dependence of strain rate on stress was determined by measuring the change in strain rate for incremental stress reductions during constant temperature tests. It has been shown that columbium-base alloys such as D43 are susceptible to contamination by gaseous interstitial elements during vacuum heat treatments.' In this regard, it is unlikely that these alloys can be heat treated without some loss or gain of interstitial elements despite the precautions taken to control the heat treating environment. However, several factors suggest that changes in interstitial concentrations of the specimens during testing did not affect the results presented in this paper. First, the dependence of the creep rate on the stress or temperature determined during the course of a single creep test showed no variations with the duration of the test. A variation would be expected if a loss or gain in interstitial concentration during the course of the test affected results. In addition, precautions taken during this investigation to minimize interstitial contamination by wrapping the gage lengths of the specimens with various foils2 (Mo, Ta, W) did not produce a detectable change in the stress and temperature dependencies relative to the unwrapped specimens. The averages of duplicate analyses for carbon and oxygen in several specimens determined before and after creep testing are listed in Table I. The combined nitrogen and hydrogen concentrations which were ordinarily less than 50 ppm did not change in a detectable way with creep testing. The analyses show that only minor changes in carbon concentration occurred during creep testing except for specimen 4. This specimen which was tested at 3100°F lost a significant amount of its carbon concentration to the vacuum environment. Specimen 1 gained 100 ppm of O, while specimens 2, 3, and 4, which were tested at progressively higher temperatures, lost increasing portions of their initial oxygen concentrations during testing. RESULTS AND DISCUSSION The Temperature Dependence of the Creep Rate. The apparent activation energy for creep, H, was de-rived from creep curves similar to that shown in Fig. 1. Steady-state creep was rapidly attained at the beginning of the test and with each change in temperature. This behavior suggests that the alloy rapidly attains a stable structure with each shift in temperature or that the structure is constant throughout the test. Since the dispersion will tend to stabilize the structure, the latter is probably the case. The activation energy was found to be independent of the direction of the temperature shift and the magnitude of the shift (50" or 100°F). Although H was approximately independent of the strain, there was a tendency for it

Jan 1, 1970

By Louis A. Carapella, Ralph Hultgren

WHEN F. Heusler1 found in 1898 that certain alloys containing only copper, manganese, and tin were ferromagnetic, the discovery excited a great deal of interest and led to numerous investigations. It was early found that tin could be replaced by aluminum, arsenic, antimony, bismuth, or boron without destroying the ferromagnetic nature of the alloys.2 Copper may also be replaced by silver.3 All these alloys have come to be known as "Heusler alloys." The aluminum alloys apparently were the most magnetic and have been most extensively investigated. However, no agreement has yet been reached as to the source of the ferromagnetism arising from these nonferromagnetic elements. Absence of reliable quantitative data makes speculation hazardous. The value of much of the earlier work was vitiated by lack of necessary precautions against contamination, and by lack of close control of heat-treatment. It was only recently established that in aluminum Heusler alloys" the ferromagnetism arose from a single phase, an ordered body-centered-cubic structure. With modern methods of preparation, heat-treatment, and X-ray examination, it is possible to prepare these alloys without contamination, to heat-treat them intelligently, and to determine what phase or phases are present in the finished sample. In the present investigation, a series of pure alloys in the comparatively neglected copper-manganese-tin system have been prepared, which consist of a single, body-centered-cubic structure (the beta phase) and whose compositions vary within wide limits. The magnetic saturation values of these single-phase alloys have been quantitatively determined, so that considerable data on the effect of composition on the ferromagnetism have been made available. In the course of the investigation some information on the extent of the stability of the beta phase and the nature of phases in adjacent regions of the ternary diagram has been accumulated. Anomalies in earlier data have been explained, and alloys have been prepared that are much more strongly magnetic than any previous Heusler alloys. PREVIOUS WORK In the original work of F. Heusler1 and coworkers,2 a maximum magnetic saturation value of I = 107 was found at the composition Cu6Mn3Sn, while a value for Cu2MnA1 of I = 443 was early measured. Ross and Grays found a second maximum at the composition Cu2MnSn, which was much more magnetic than Heusler's original alloy. F. Heusler6 then reinvestigated the system, confirmed their results,

Jan 1, 1941

By Charles L. Harness

STRONTIUM is an essential constituent of celestite (strontium sulphate), of the rarer strontianite (strontium carbonate), and of a few very rare minerals. Celestite is the chief ore but strontianite is more valued except for making the purest strontium salts, because of its ease of processing. The public knows strontium mainly as the source of the red flame in fireworks but it has many other uses. PROPERTIES The celestite of commerce is a massive mineral of varying texture: coarsely crystalline, fibrous, bladed, very fine grained or earthy. The color varies greatly with the nature of the impurities but the purer specimens are light blue (Latin, caelum, sky) or white. The strontianite of commerce is a massive mineral, more or less coarsely crystalline. The color varies with the impurities. Distinctive characteristics are effervescence with acids, density (3.68 to 3.71), and crimson strontium flame. A typical British celestite before World War II analyzed: SrSO4, 96.55 pct; SrCO3, 0.17; BaSO4, 0.25; CaSO4, 0.54; MgCO3, 0.15; R20,, 0.90; Si02, 1.38.10 A German strontianite analyzed: SrCO3, 90.9 pct; CaCO3, 7.5; BaCO3, 0.1; Fe2O3, 0.05; A1203, 0.1; SiO2, 0.04; S, 0.1; P, 0.005.10 ORIGIN AND MODE OF OCCURRENCE According to Clarke,9 strontia forms about 0.02 pct of the crust of the earth and is present in most igneous rocks, but in smaller quantities than barium. Under certain conditions, large masses of celestite are deposited from sea water with anhydrite. The presence of large amounts of celestite in some saline deposits and its absence in others suggests that the deposition of celestite depends on whether certain as yet undetermined concentrations of sulphate and chloride ions are reached in the brines. The most extensive of these sedimentary deposits are those of the Keuper (Triassic) in England, of the Zechstein (Permian) in Germany, and of various Cretaceous formations in Texas, Arkansas, and Utah. Of the deposits of southeastern California and western Arizona,

Jan 1, 1949

Discussion of the paper of THEODORE P. HOLT, presented at the Salt Lake meeting August, 1914, and printed in Bulletin No. 91, July, 1914, pp. 1699 to 1708. F. S. SCHMIDT, Salt Lake City, Utah.-Any furnace that can make a chloridizing roast to yield an extraction of 92 to 93 per cent. and do this at a cost of less than 24c. per ton in a 10-ton unit opens great possibilities for the treatment of certain classes of ores. This cost does not include the salt and will be reduced to about 16 1/2c. per ton in the 35-ton furnace which are now being designed. On a trial run the roaster treated 9.6 ton: of Ontario stope fillings crushed to pass a ¼ -in. opening. The ore is well adapted to chlorination with the exception of insufficient sulphur and occasional days of high lime, but is not adapted to any other process The following is an analysis of the crude ore: Ag, 9.52; Au, 0.029 oz. Pb, 0.71; Cu, 0.11; SiO, 79.4; Zn, 0.57; S, 1.00; Fe, 7.9; Mn, 0.89 CaO, 1.20 per cent. The composition of the mix was: Per Cent. Dry crude ore : 83.4 Moisture 4.4 Salt 8.3 Coal dust 2.3 Pyrite, 70 per cent. pure 1.6

Jan 11, 1914

By A. M. Skov, L. F. Elkins

First response to large-scale water flooding in the fractured very low permeability Spraberry sand has led to a new unique cyclic operation. Capacity water injection is used to restore reservoir pressure. This is followed by marly months production without water irzjection and the cycle repeated. Expansion of the oil, rock and water during pressure decline expels part of the fluids but capillary forces hold much of the injected water in the rock. At least with reservoir pressure restored and with partial water flood development, field performance has proved this cyclic operation is capable of producing oil from the nzatrix rock at least 50 per cent faster and with lower water percentage than is imbibition of water at stable reservoir pressure. INTRODUCTION The Spraberry Field of West Texas presents unusual problems for both primary production and water flooding. Extensive interconnected vertical fractures in the fractional-md sandstone permitted recovery of oil on 160-acre well spacing, but they made capillary end effects dominant. Primary recovery by solution gas drive is less than 10 per cent of oil in place. The concept of displacement of oil from the sand matrix by capillary irnbibition of water has led to field techniques which promise greatly increased oil recovery. Free exchange of laboratory research, reservoir information and results of field pilot tests among the various companies has been very important in development of this technology. Five units covering a total of 170,000 acres have been formed for water flooding, and 10 other areas covering an additional 175,500 acres are in various stages of unitization. Part of the Driver Unit reaching fillup first has demonstrated very unusual waterflood behavior and indicated numerous operating problems that will develop within and among the various units. SPRABERRY ROCK AND PRIMARY PERFORMANCE The Spraberry, discovered in February, 1949, is a 1,000-ft section of sandstones, shales and limestones with two main oil productive members: a 10-15 ft sand near the top and a 10-15 ft sand near the base. In part of the field some thinner intermediate sands are oil productive, and others are water bearing. All sands have permeabilities of 1 md or less and porosities of 8-15 per cent. Ordinary core analysis and electric and radiation logs are ineffective in differentiating between oil productive and nonprcductive sands. Sands capable of containing producible oil are best identified by mercury injection capillary pressure measurement and, in some cases, by core water saturation. About 3,500 wells have been drilled in the 500,000-acre trend. Vertical fractures were observed in practically all Spraberry cores. Continuity and interconnection of fractures were confirmed by pressure interference among wells during early development.' Major fractures trend northeast-southwest as indicated by oriented cores and confirmed by five fluid injection tests, by analysis of the pressure transients observed during development,''' and by three interference tests in the Driver Unit Water Flood reported herein. Fracture spac- ing probably averages inches to a few feet. Spraberry wells typically produced 100-400 BOPD initially after hydrauLic fracture treatments. By 1962 oil production had declined to an average of 12 bbl/well/day, near the economic Limits of operation. Reservoir pressure had declined from 2,300 psi initially in the Upper Spraberry and 2,500 psi in the Lower Spraberry to 500-1,000 psi. Partial closing of the fractures with declining reservoir pressure is believed to be the cause of such low oil production rates at these relatively high reservoir pressures. Cumulative recovery of 208 million bbl of oil is 80 to 90 per cent of that recoverable by primary means. Performance of the entire reservoir is summarized in Fig. 1. IMBIBITION WATER FLOODING By 1952 reservoir performance indicated low primary recoveries. Most engineers, expecting serious channeling of injected fluids through the fractures, held little hope for secondary recovery. With its extensive background of research on the fundamentals of fluid flow within reservoir rocks, Atlantic's Research and Development Division on short notice in 1952 conceived that displacement of oil by capillary imbibition of water into the rock might significantly increase Spraberry recovery. Laboratory data reported by Brownscombe and Dyes scaled to probable reservoir conditions showed potential waterflood recovery equal to or greater than primary recovery with a 10-15 year flood life.= A pilot test using three 40-acre injection wells, one central producing well and 18 surrounding observation wells demonstrated technical feasibility of the process. Injection of 1.5 million bbl of water from November 1952 to August 1955 proved water entered the rock and displaced oil

By W. S. Sanner

Experiments were conducted to determine the quantity and purity of ultraclean anthracite that could be prepared in the laboratory, using conventional separating techniques. A low, a medium, and a high-volatile anthracite were studied. Specific gravity separation followed by grinding, screening, and refloating at lighter specific gravities yielded small quantities of material purified to 1.0% ash, as follows: from low-volatile anthracite, 0.7%; from medium-volatile coal, 1.0%; and from high-volatile coal, 2.3%. The reduction in ash had no appreciable effect on the volatile matter or sulfur content of the coal. The limited quantities of material containing 1.0% or less ash obtainable indicate that if ultraclean coal is desired, a practical approach should include the processing units as an integral part of a convc.ntiona1 dense-media washing plant. Anthracite preparation practices during much of the industry's history were geared to maximum recovery of the larger sizes, pea through egg, which were used in hand-fired, domestic furnaces. Those sizes were cleaned to meet trade requirements, and the smaller sizes were usually higher in ash content. The impression, thus, was that ash content of anthracite always increased as the sizes got smaller. It was presumed that it was impossible to wash the finer sizes to extremely low ash contents. Following World War 11, the classical domestic market began to decline and the finer sizes assumed an increasingly large share of the market. For example, in 1949l 61% of the production was still pea and larger. Fig. l2 shows that -by 1955 these sizes accounted for only 50%, and in 1965, they were only 39% of the total anthracite produced. With the reduction in the market, increased quality was demanded, especially in export markets, and an increasing number of dense-media magnetite washers were installed in new and existing cleaning plants. In 1965, the coarse coal prepared at 59 breakers in the anthracite fields was sampled by the U.S. Bureau of Mines (USBM); approximately 50% of these plants were equipped with dense-media magnetite washers.3 Since 1950, more attention has been focused on the use of finer sizes for numerous industrial uses, including iron-ore sintering, pelletizing, foundry coke-making, cement manufacture, production of calcium carbide, and of carbon electrodes, etc. Most industrial uses require relatively clean anthracite, such as 10 to 11% ash for sintering and foundry coke, 7% for aluminum melting-pot cathode carbon, and 5% for carbide production. Hence, cleaning methods have been improved to the extent that dense-media washers, hydraulic cyclones, and flotation cells have been introduced as fine-coal-cleaning devices. It is now possible to wash the buckwheat, rice, and barley sizes (9116 X 3132-in.) to ash contents as low as 8 to 10% in dense-media devices, but washing the -3132-in. sizes to those limits presents more difficult problems, due mainly to the fineness of the material. This USBM investigation was conducted to determine the amount and purity of ultraclean anthracite that could be prepared in the laboratory, using conventional separating techniques. The goal was to reduce the ash content to a level acceptable for industrial carbon uses, including electrode manufacture, which generally requires an ash content of 1% or less. While low-ash content is of primary importance in selecting industrial carbons, the amounts of other constituents are also important, including iron, silicon, titanium, nickel, vanadium, and sulfur. They were not considered in this work, since their occurrence in deashed anthracite has been studied elsewhere.4 The results of the present investigation were used to design a flowsheet, suggesting a method for producing ultraclean anthracite as part of conventional preparation practice, using dense-media vessels, crushers, pulverizers,

Jan 1, 1970

By Martin Weinstein

A technique is described for preparing finegrained lead telluride by ultrasonic agitation of a solidifying melt. Material prepared by this technique is dense and chemically homogeneous. N-type PbTe, containing 0.03 mole pct PbIz, has been made and its thermoelecCric Properties have been measured as a function of temperature. For comparison, the properties of similarly doped PbTe made by cold pressing and sintering, and by extrusion, have also been measured. The ultrasonically prepared material compares favorably with the others in its thermoelectric-efficiency factor. Comparison of compressive-flow curves for the three kinds of PbTe show that the ulhasonically prepared material has much superior ductility. The cleavage strength of the ultrasonic material is related to the grain size, D, by the Petch relation:Extrapolation to infinite grain diameter yields a fracture strength of 5000 psi for single-crystal PbTe. WHEN metals and semiconductors solidify in a mold they normally assume one of three cast structures illustrated in Fig. 1.' Solidification in a casting starts at the mold walls where a large number of fine crystals of random orientation can be nucleated to form the chill zone. Because of the anisot-ropy of the growth rate, those crystals whose direction of maximum linear growth is parallel to that of the heat flow grow faster and crowd out the crystals of less favorable orientation. A second zone, having a preferred orientation, called the columnar zone, thus forms adjacent to the chill zone. The speed of growth of the columnar grains will depend, in the case of limited undercooling of the melt, on the rate at which heat can be abstracted. The columnar zone can extend to the center of the casting, Fig. l(a), but it is frequently followed, in solid-solution alloys, by another zone of equiaxed randomly oriented grains in the central portion of the casting, Fig. l(b). The equiaxed structure in Fig. l(c) represents the completely grain-refined case where the equiaxed grain size is small. The third type of structure is the most desirable because it imparts a somewhat higher strength for all except high-temperature applications, it reduces segregation of the doping constituent, and it reduces the possibility of hot tearing (the separation of grains due to the melting of a low-melting point constituent in the grain boundaries). In order to obtain fine-grained castings, the nu-cleation frequency must be increased and grain growth must be restricted. Various techniques have been employed for obtaining this end, namely: rapid cooling, vibration, and inoculation of the melt. The success of these techniques depends upon the characteristics of the metal species and on factors controlled by heat transfer through the crucible walls. Recent studies2" have shown that the application of ultrasonic energy to the solidifying ingot is an extremely powerful tool in the improvement of the crystalline structure of metallic castings. Both the mechanical properties and homogeneity of the ingots are improved. Ultrasonic oscillations may affect the crystallization process by 1) permitting subcritical nuclei to agglomerate and thus form nuclei of sufficient size to cause crystallization, 2) changing the state of surface adsorption of various catalysts found in the liquid melt, 3) breaking pieces of solid from the solidified surface near the supercooled region thereby increasing the number of possible nuclei, 4) causing temperature fluctuations to occur in certain parts of the melt thereby increasing the supercooling at specific points in the liquid, and 5) decreasing the critical nucleus size by increasing the pressure at specific points in the melt.' Various investigators have concluded that the effectiveness of the ultrasonic oscillations results from cavitation which disrupts the growing solid-liquid interface The present paper describes the application of ultrasonic oscillations to the crystallization of the semiconductor N-type PbTe. The purpose of this study is to prepare crystalline

Jan 1, 1964

By D. T. Peters

To better understand the Co-Mo interaction in maraging steels, the precipitate reversion behavior of two alloys closely related to the 18 Ni-250 grade has been studied. The reversion experiment is carried out by aging at a low temperature, T1 (preaging temperature), for some period of time and then aging at a higher temperature, T2, called the reversion tetnperature. Aging and reversion tmzperatures used were in the range 679 to 1050°F. Reversion is marked by an increase in resistivity and a decrease in hardness. It teas found that some reversion took place at all cornbinations of T1 and T2 but that pronounced rei3ersion resulfed for an Fe-18 pct Ni-5 pct Mo-8 pcl Co alloy exposed to preagz'ng' temperatures at or below 850°F. A similar alloy not containing cobalt exhibited no such discontinuity in reversion behazior with TI. The results are interpreted in terms of two types of molybdenum-rich precipitates, one nucleated at dislocations and the other in the matrix. The increased supersaturation resulting from the presence oj- cobalt evidently provides sufficient energy to nucleate the matrix phase. Anotnalies in the temperature dependence of the resistivity decrease and peak hurdness in the Fe-18 pct Ni-5 pct Mo-8 pct Co alloy as a junction of aging temperature noted in an earlier study are explained on this basis. SEVERAL investigatorsl-9 have studied the details of the precipitation-hardening reaction of the maraging steels. The great majority of conclusions have been drawn from transmission electron microscopy. Although much has been learned by this method, alternate techniques which will give information earlier in the aging process are needed for a more complete understanding of the series of precipitation steps probably involved in the aging reaction. Peters and cupp'' have recently shown, by measurements of the kinetics of precipitation, that an 18 pct Ni-Co-Mo maraging steel shows a distinct change in precipitation behavior at aging temperatures below 850°F. The results were interpreted in terms of the existence of two types of precipitates at low aging temperatures. Only one precipitate type is present at higher aging temperatures. The low-temperature precipitate was found to be a particularly effective strengthener. No evidence for the additional low-temperature precipitate was found in the 18 pct Ni-5 pct Mo ternary alloy. The object of this investigation was to study further the characteristics of the two types of precipitates and the interaction between cobalt and molybdenum characterizing this system. Some preliminary experiments indicated a difference in reversion behavior in specimens aged above and below 850°F. This suggested that knowledge of the reversion behavior might shed some light on these two questions. Hardy and Heal11 have defined reversion as the loss of hardness, electrical conductivity, or other properties caused by heating for a very short time at temperatures above the aging temperature. The precipitate reversion referred to in this paper is entirely distinct from "austenite reversion" often referred to in maraging steel literature. This latter phenomenon could more accurately be called the diffusion-controlled formation of austenite. Much has been written about reversion in several of the aluminum-base binary and ternary alloys.'2-16 Two explanations for reversion have been advanced. Based on the classical nucleation theory of Volmer-Weber-Becker-Doring,17 Konobeevski18 suggested that reversion was due to the size of the precipitate particles

Jan 1, 1968

By L. F. Engle, M. A. Hewedi

SUMMARY Initial interest in using solutions of ammonium salts to leach native copper was documented in notes from an AIME meeting in 1871; By 1916-1917, application of the NH3-CO2-H2O system to recover nonferrous metals attained commercial significance, when it was used as a process for copper recovery by Kennecott Copper Corporation and Calumet & Hecla Mining Company. The Caron work in the early 1920s, Freeport Sulphur Company’s achievements leaching Cuban laterites during World War II, out- standing accomplishments in both eastern and western Canada, recovery of manganese related to the work of Dean -- all serve as landmarks as this One Century Review surveys a base for future technology. Current emphasis on compatibility of metals-producing systems with the need to meet environmental protection criteria provides special encouragement to researchers and engineers to find accept- able ways of recovering metals. The ever-present demand of management to design, build and operate facilities on a profitable basis provides additional impetus to apply information from the technical literature to that need. Examination of the general approach to this paper will reveal much that is firm and positive with respect to empirical results -- extractions, recoveries, amenability to familiar proven equipment and materials of construction common to the industry. Although there are many references, there are gaps in the basic scientific data that if filled could lead to even more usefulness; the paper attempts to indicate where further information is needed.

Jan 1, 1973

By H. A. Wentworth

THE Huff electrostatic plant of the United States Smelting Company operated in conjunction with its wet concentrator at Midvale, Utah, was the second plant of substantial size installed using the Huff process, and the first plant to be put in operation on the so-called Western complex ores. In spite of the machinery being of early design and consequently embracing many of the mechanical weaknesses incident to a pioneer plant the mill has operated steadily and uniformly since the summer of 1909, about five years now, without any material change other than some re-arrangement of the machinery for better handling of the sizes. The ore, at present coming almost entirely. from the company's mines in Bingham, is of practically the same composition as that upon which the plant was first put in operation. The crude ore, consisting of the sulphides of copper, lead, zinc, and iron, and containing small amounts of gold and silver, is brought by train and delivered to the hoppers of the wet concentrator, where by jig and table treatment, there are produced a shipping lead concentrate, a tailing and a middling product, the latter being conveyed in push cars to the adjoining electrostatic mill. The crude ore delivered to the wet concentrator contains from 6 to 9.5 per cent. zinc. At times the plant is used also for the treatment of custom ores from the Bingham district and elsewhere, and at such times the results of the plant vary according to the material in use, but as by far the larger portion of the product is that from the company's own mines, the results given below are fairly indicative of the general work obtained. The accompanying diagram illustrates graphically the flow of the ore through the electrostatic mill. The middling coming from the wet mill containing from 15 to 18 per cent. moisture is hoisted while on the cars by an elevator, and delivered from the top of the elevator to a hopper over the drier. The drier first installed was of too low capacity to take care of the moisture present in the tonnage to which the mill was later

Jan 8, 1914

By H. F. Yancey

THE jig may be termed the standard coal-washing machine. Although exact figures on the relative tonnages of coal treated by the various coal-cleaning processes are not available, it is known that a large part of all the coal given special cleaning treatment is handled by jigs. This wide use of the jig warrants a special study of its performance. In this paper are presented the results of an analysis of work done by a three-compartment jig in treating bituminous coal from the Thick Freeport bed in Allegheny County, Pa. Certain systems of washing coal require sizing before washing, while others treat unsized coal. The prevailing practice, however, for the preparation of coking coal from the more easily washed coal is to treat an unsized or natural feed at about -1 in. size and smaller. Under such conditions, the minimum size of particle that is beneficiated has long been and is still a matter of discussion and conjecture. In a careful laboratory investigation Jüngst1 concluded that the practical limit of settling of fine coal is reached at from 0.02 to 0.008 in. On the other hand, Hancock2 has found that single-compartment jigs, used in preparing coal for the domestic market, usually allow most of the heavy (refuse) particles smaller than 1/4 in. to go into the washed coal. He also states that it is impossible with the ordinary coal jig to make any noticeable improvement in the quality of the coal finer than 20 mesh (about 1/30 in.). Because of its importance in coal cleaning, the work described in this paper was undertaken for the purpose of obtaining information on this subject, as a part of the general coal beneficiation program being carried out by the Bureau of Mines.

Jan 4, 1925

By Charles H. White

+1HARVARD UNIVERSITY, CAMBRIDGE, MASS. The equipment of a laboratory in which students are to be trained for practical work in metallurgical chemistry presents many difficulties not encountered in the fitting up of a commercial or works laboratory. At an industrial plant the chemical work required usually demands the frequent repetition of a comparatively limited number of methods. In a steel-works laboratory, for instance, by far the larger part of the work consists in making determinations of the usual impurities found in iron and steel; at a smelter the great bulk of the work is confined to the analysis of ores, slags, mattes, and fuels, which involve the frequent application of perhaps not more than a dozen different methods. In a laboratory of this character, therefore, those operations most frequently applied may each have a certain section set apart and fitted permanently with such apparatus as best facilitates the carrying out of this one operation. The work of a commercial or custom laboratory is perhaps more varied than that of a works laboratory, but the couditions are similar in these respects, that there is usually no great need for economy of space, and that a few skilled workmen are employed to carry the determinations through from beginning to end without interruption. On the other hand, the laboratory of a technical school should be planned on such a scale that a comparatively large number of students may work at the same time, and each desk should be equipped for general metallurgical analysis. In most institutions for technical education the student's program is so arranged that his day is divided among several subjects in the course of study; only a few consecutive hours being devoted to one subject, or spent in one laboratory. Therefore, those appliances should be provided that render possible the safe continuation of such processes as

Jan 1, 1905

By Richard A. Conkling

D. W. OHERN, Oklahoma, Okla. (communication to the Secretary*). -The author states: "A shale layer buried beneath 2,000 or 3,000 ft. of strata, in some instances, will upon folding become thicker in the synclines and thinner on top of the anticlines." In any series of folded strata there is a level of no strain. Provided the strata do not slip on each other, there would be above this level a thickening of strata in the synclines and a thinning on the anticlines, as the author states, while the converse would obtain below this level. In order that the author's

Jan 3, 1917

By F. E. Bash

A GREAT many industrial operations require the application of heat to carry on or complete processes, in which cases the temperatures must often be controlled within very narrow limits. For the lower temperatures, this control is not, as a rule, difficult as a number of types of reliable pyrometers are available for the work; for example, the mercury and resistance thermometers and the thermocouple. For temperatures above a red heat, thermocouples, platinum resistance thermometers, and total radiation and optical pyrometers may be used, depending on conditions. It is often undesirable, and sometimes impossible, to take temperatures of material by immersing the pyrometer in it or by placing the temperature-measuring device in a position in which it will attain the temperature of the material. The pyrometer may contaminate the product; the temperature may be so high that the pyrometer will not hold its calibration, clue to ineffectual protection and consequent contamination; the object may be inaccessible, as a lamp filament, etc. In such cases, a total radiation or optical pyrometer must be used. The disappearing-filament, or Morse, type of optical pyrometer works on the following principle: An objective lens, Fig. 1, focuses the image of the object whose temperature is desired in the plane of the lamp filament at F, which is at the principal focus of the ocular lens shown in the eye-piece. By this arrangement the eye will not have to accommodate itself first to the lamp filament and then to the object at a distance, and the lamp filament will appear superposed on the object. To balance the instrument, the current is adjusted by means of a rheostat until the tip of the lamp filament just disappears against the object as a background. Figs. 2, 3, and 4 show the appearance of the filament when too cold, too bright, and just balanced.

Jan 8, 1919

By J. T. Norton, N. J. Grant, A. M. Gervais

An investigation of the creep deformation of coarse grained specimens of high purity aluminum in the temperature range 800' to 1150°F, permitted the formulation of a theory explaining the formation of kink bands. The X-ray Laue back-reflection technique was used in conjunction with metallographic studies to determine the crystallographic elements involved in kinking and to measure the rotations of the bands. THAT metals deform by the formation of kink bands was first shown by Orowan1 in 1942. He manually compressed cadmium single-crystal wires, the basal planes of which were parallel to the wire axis and to the direction of compression. He found that kink bands formed quite suddenly. Similar experiments were performed by Hess and Barrett2 on zinc with a hydraulic testing machine to permit slower more careful compression. They observed that kink bands formed progressively with increasing compression. Recently Washburn and Parker3 observed the formation of kink bands in zinc single-crystal specimens during tension creep experiments. Each of these authors observed the formation of kink bands but did not make a complete analyses of the crystallographic relationships. In addition to these studies on hexagonal metals, extensive investigations of kink bands formed during deformation of aluminum in tension at room temperature have been reported. Two types of deformation bands have been observed during the deformation of aluminum at room temperature. These are: 1—kink bands: these exhibit a sharp curvature of the lattice along certain surfaces, and 2—bands formed by secondary slip along certain regions. As has already been shown by Honeycombe,4 it is important to point out the difference characterizing the two types of deformation bands. In the first case. for moderate deformation, only one system of slip planes normally is active; in the second case, however, two slip systems are active in the deformation bands. The latter have a rumpled surface because of the action of the two slip systems. In the present work only the first type of band was studied and to avoid any confusion the term kink band will be used exclusively in the discussion which follows. Honeycombe' observed that very narrow kink bands (width, 0.01 mm) formed along the (110) planes during the deformation of high purity aluminum at room temperature. He observed narrower ones in commercially pure aluminum and found also that their width decreased with decreasing temperatures. Chen and Mathewson5 reported the formation of kink bands during tensile testing of single crystals of high purity aluminum at room temperature and pointed out that some rotation occurred about a [211] direction. The influence of the bending moment on the formation of kink bands was illustrated by the experiments of Rohm and Kochendorferl0 who used a Polanyi apparatus to obtain pure shear during tensile testing of high purity aluminum single crystals. Under such conditions only one slip system was active and no kink bands were observed; consequently, no noticeable asterism was detected after deformation. The influence of the bending moment will be discussed later. Calnan8 gave a detailed account of the work performed on kink bands obtained during deformation of aluminum at room temperature. Because no explanation of the process of kink band formation in creep was given in the previous investigations and because some of the above observations are vital to the following discussion the brief review of the literature has been given. It is proposed in the present work to provide an explanation of kink band formation during creep deformation at elevated temperatures. Results and Discussion Kink bands were observed to form during tensile creep testing of high purity (99.995 pct) aluminum specimens, having a very large grain size, in the temperature range 800" to 1150°F. These observations were made in grains which occupied the whole cross section of the specimen. The specimens were originally round (diameter, 0.187 in.; gage length, 1 in.) and had parallel flats milled to permit easier metallographic and X-ray observations. The final

Jan 1, 1954

By A. J. Shaler, J. Prieto Isaza, J. Wulff

Tantalum metal has a number of unique properties which give it widespread application in modern technology and in research. In electronic apparatus involwing high temperatures in vacuo some of the refractory metals 6ecome brittle. Tantalum retains its ductility at elevated temperatures, and this property, together with its low vapor pressure and its ability to absorb gases, make it important in this field. Its chemical inertness in the presence of acids, halogens, and other corrosive media, makes it useful in chemical apparatus and in neuro and orthopedic surgical applications. As an addition to tungsten carbide in steel-cutting grades of cemented-carbide tools, the carbides of tantalum and of its sister element colum-bium have found considerable use. The present-day method1 of manufacturing tantalum is to sinter a powder compact of the metal in vacuo. Because tantalum-columbium alloys are difficult to work and since tantalum ores almost always contain columbium, the two metals must be separated chemically, the products of the separation being generally in the form of potassium tantalum fluoride and potassium columbium oxyfluoride. These salts are used in fused-salt electrolytic baths from which coarse metallic powder is deposited as a sponge at the cathode. Finer powder can be made from the coarse product or from tantalum scrap by first submitting it to an embrittling heat treatment in hydrogen and then crushing it. The fine hydrogen-containing powder may subsequently be degassed in vacuo at a high temperature. Prompted by the success of others2,3 in the magnesium reduction of titanium and zirconium halides; one of the authors undertook4 an investigation of the thermochemistry of the reaction between solid magnesium and gaseous tantalum penta-chloride, a subject which had not previously been studied. He found that the heat of formation of tantalum pentachloride is approximately 364,250 cal per mol at temperatures lower than the melting point of magnesium. A value of 83 units was found for the standard entropy at these temperatures. With these values, it was shown that magnesium and tantalum pentachloride are capable of reacting exo-thermically at temperatures less than the melting point of magnesium, and that no great violence is to be expected when these substances are heated together. The exothermic nature of the reaction indicated that the Drocess should be efficient and should not require much externally applied energy. Tantalum pentachloride is not commonly made commercially, and any process using it therefore involves the subsidiary problem of producing and handling this substance. A series of experiments was carried out in which dried chlorine saturated with carbon tetrachloride was passed over heated tanta-

Jan 1, 1949

By H. T. Clark, S. Feigenbaum

THE importance of measuring the temperature of molten steel in the open-hearth furnace has been recognized for many years. Poor temperature control may be costly to steelmaking operations and lead to a lowered quality of the steel. Low or excessive temperatures may shorten the life of the furnace, ladles and molds. Rates of reactions in the furnace and efficiencies of deoxidizers are known to change materially with a change in the temperature of the metal and slag. Ladle skulls and mold and stool stickers cause steel to be scrapped instead of being converted into useful products. Finally, the structure, segregation and surface condition of ingots are affected by the teeming temperature. Mill investigations of the effect of bath temperature upon steelmaking operations have been largely qualitative in character, based upon observations by practical melting men. The physical chemist has used the empirical information available and has reached reasonable and useful conclusions with respect to the various melting processes. The introduction of a reliable direct- reading pyrometer will permit accurate quantitative evaluation of the effects of temperature and should furnish a more rational basis for study of the thermo- chemistry of steelmaking. The problem is not merely one of making a small number of temperature measurements in the open-hearth furnace. This has been done by several methods to a degree of precision that was apparently satisfactory. Considerable effort by a number of investigators has been directed rather to the development of an open- hearth bath pyrometer that would be both accurate and practical for routine measurements. To be practical, the pyrometer should be inexpensive to operate; that is, the installation, operating and maintenance costs should be exceeded by the tangible benefits to the open-hearth operator. Temperatures from 2800° to 3100°F. are encountered in the open-hearth furnace. The surface of the molten metal is covered by several inches of slag, which prevents direct observation of the metal surface for optical or radiation measurements. Both slag and metal are highly reactive at these temperatures and will attack to a greater or lesser extent any material immersed in them. Adequate protection of thermocouples, which of necessity must be brought to the temperature of the bath, has generally resulted in a large, heavy assembly made up of .brittle materials, unsuited for handling on the open-hearth floor. The lie of the equipment was short and maintenance was an important consideration. EARLIER WORK Any one of a number of physical proper- ties of liquid steel could conceivably be used as a basis for temperature measurement. Efforts to the present time, however, have been confined largely to measuring either the thermal electromotive force generated between two dissimilar materials immersed in the steel or the intensity of radiation from the surface of the steel. These

Jan 1, 1946

By Enid C. Plante, K. L. Sutherland

PRACTICAL metallurgists are unanimous in stating that oxidation of mined sulphide ore adversely affects separation of the constituent minerals under standard conditions in a mill. Frequently, the need for different operating conditions in different plants is attributed either to the extent of oxidation of the mineral surfaces or to soluble oxidation products. The investigations reported in this paper study the effect of oxidation on the primary condition necessary for flotation, namely that of adhesion of an air bubble to the mineral. OXIDATION PRODUCTS FROM SULPHIDE MINERALS Weinig and Carpenter1 state that the relative rates of oxidation of some sulphides are: FeAsS > FeS2 > CuFeS2 > ZnS >PbS > Cu2S tetrahedrite. They also show that oxidation is rapid at first, that sulphides of older geological formations are more stable than those of recent date and that mixtures oxidize more rapidly than any one mineral alone. The more rapid oxidation of mixtures is borne out by results of Gottschalk and Buehler2 who found that PbS, ZnS and CuS oxidized 8 to 20 times faster when pyrite was present. Only the end products of oxidation, sulphate and the metal ion, were identified in these tests. Gaudin3 states that pyrite is difficult to oxidize in the laboratory. Winchell,4 using pyrite containing 99.98 pct FeS2, allowed water to percolate through a bed of this ground material. At the end of three months only a trace of Fe +++and S04- were found. Even after 10 months the quantity of Fe+++ was only 7.8 mg and S04- 25.5 mg per liter of percolating solution. Carmichael5 confirmed Winchell's results on the slow oxidation of pyrite. Usually the oxidation of sulphide surfaces has been conducted in neutral or acid solutions, the acidity being caused by the oxidation products. Eliseev and Nagirnyak6 found that treatment of pure pyrite with lime gave only thiosulphate, but considered it possible that thiosulphate was obtained not by oxidation of the pyrite itself, but by oxidation of calcium disulphide. Mitrofanov7 suggested that thiosulphate was formed by the following process: oxidation of sulphide to give free sulphur (this frequently happens with marcasite), followed by oxidation of the sulphur to sulphur dioxide and reaction of the sulphur dioxide with sulphur to give thiosulphate. Ferric and ferrous hydroxides, or similar compounds, were shown to be present. The Research Staff of the United Verde Copper Co.8 treated ore from the United Verde mine with lime. Thiosulphate, sulphide and polysulphides were stated to be

Jan 1, 1947