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By Mark Sheppard

DURING the winter of 1937, the writer visited a West Virginia stone quarry at which the overburden is stripped hydraulically. The quarry is in a bed of limestone, about 200 ft. thick, which outcrops on a hillside above a small river; the quarry face is 175 ft. high. The top of the stone is cut in all directions by erosion channels, which are filled with a tough, red clay. Some of the larger channels are 30 ft. deep and 8 ft. wide. The thickness of the clay overburden ranges from a few inches to 10 ft., the average being estimated as less than 3 feet. The topography of the district is rugged, and the hillside above the quarry face is not suited to the use of the usual mechanical methods of moving dirt. Until hydraulicking was started 10 years ago, the over- burden was dug by hand labor, dumped to the quarry floor and transported to the dump in quarry cars. Cleaning deep channels was a slow and expensive process. When hydraulicking was started, the top of the quarry face was over 200 ft. above the level of the river. The pipe line was carried in a semi- circle around the top of the quarry about 200 ft. from the face and about 50 ft. above it. As there is no adequate supply of water above the quarry, the water must be pumped from the river. As quarrying progressed the pipe line was moved until the discharge points are now over 300 ft. above the river. Water is pumped from the river by a four-stage centrifugal pump having a 5-in. intake and a 4-in. discharge. It is direct-connected to a 200-hp., 2300-volt, 1760-r.p.m. induction motor. At 1760 r.p.m. the rated capacity of the pump is 750 gal. per minute under a head of 600 ft. The pump is installed in a house of frame construction on the river bank, about 10 ft. above normal water level, which also houses the pump for the mill-water supply. Above the pumps are hoisting bays into which the motors are raised whenever the river reaches flood stage. An 8-in. suction line, equipped with a strainer and a foot valve, takes the water from a concrete sump at the edge of the river. The pipe line from the pump consists of 1750 ft. of 8-in. spiral steel flanged pipe and 800 ft. of 4-in. spiral steel flanged pipe. The connection from the pump

Jan 1, 1938

By M. H. Harris

A solution has been obtained to the problem of calculating flow into a cased and perforated well. Equations describing the idealized system were solved by numerical analysis techniques on a high-speed digital computer. Computer experimentation indicated that the results are within 3 per cent of the exact solution. Computed results are presented as an apparent skin effect, on a series of dimensionless working curves. Productivity ratios can be rapidly calculated from these data for the wide range of wellbore and reservoir properties actually encountered in field practice. Any reasonable vertical unisotropy ratio can be included in the computation. Productivities can be calculated for wells perforated in a regular pattern, a single horizontal plane or a vertical line on one side of the casing. Solutions for asymmetrical perforation patterns can he easily obtained from the working curves. Solutions for flow into sells completed with a horizontal notch are also provided. Results show that productivity can be increased by extending perforation penetration. This is especially true for shallow penetrations. The highest productivity is obtained when perforations are arranged in horizontal planes, as opposed to a vertical line on one side of the casing. Four or five perforations in one plane will approach the maximum productivity. The effect of perforation hole diameter is small, and is rioticeable only in shallow penetrations. INTRODUCTION The perforating method of well completion has been successfully and widely used in most producing areas. In the past, the desired perforation results were achieved by simply shooting numerous large holes in the casing. A perforating scheme for an area, or particular well, was established by evaluating two types of experimental data: the well flow index and the productivity ratio.' 3 The well flow index test is a means of determining the relative flow capacity of perforations in a linear system. This test also gives information on the perforation size, shape and hole damage which can be expected under well-bore conditions. However, relative flow data from this test cannot be accurately tarnsformed into the radial wellbore system. Thus, no true indication of the productive capacity of a perforated well can be obtained from the well flow index test. A well productivity ratio is derived from electrolytic models built to simulate perforated wells. Available productivity ratio data 2,3 are limited in that all important variables are not extensively evaluated. For example, data are limited to well radii of 3 and 6 in., and to maximum perforation penetration of 1 ft. Practically no information is available on the pattern of flow into a perforation. The effect of various perforation patterns on well productivity has not yet been determined and the effect of perforation diameter has not been thoroughly studied. Also, it will be shown that this type of electrolytic model data is probably in error by as much as 10 per cent or more. Modern completion techniques such as limited-entry perforating, single-plane fracturing, steam and hot air injection and chemical consolidation of incompetent formations all rely on injection and/or production from a limited type of completion. These completions may consist of several high-capacity perforations or a horizontal notch which is equivalent to an infinite number of perforations in one plane. Proper design of these new completion techniques requires, in part, accurate estimates of a well's productive capacity. Data on perforated and notched well productivity have been determined in this investigation. Results are presented as a function of the pertinent variables. Equations describing the idealized system were solved by numerical analysis techniques on a high-speed digital computer. DESCRIPTION OF PROBLEM PRACTICAL APPLICATION The computed results can be applied to wells which meet several general specifications. An external drainage radius of the well must be known or assumed, but the well need not be drilled on a regular pattern. The well must be cased and cemented through the entire producing interval. And, the casing must be perforated with one or more horizontal planes of perforations. The perforation pattern itself must conform to three geometrical requirements. 1. The perforations in a plane must divide the plane into equal angular segments (Fig. 1). Four perforations per plane would be 90" apart. 2. Perforations in a plane must be directly above or beneath perforations in adjacent planes. For two shots per plane, perforations would lie in the BB' plane (Fig. 1). 3. Horizontal planes must have equal vertical spacing and be separated from the top and bottom of the formation by one half the spacing interval. Single planes of perforations should be in the middle of the formation. This is shown in Fig. 2 where h is the formation thickness in a single plane conlpletion or the spacnig interval in a multiple plane completion. The spacing interval at the top and bottom of the formation may vary somewhat without causing an appreciable error in the productivity calculation if the formation is reasonably thick and there are many horizontal planes of perforations. A special provision has been made to calculate the productivity ratios of wells with uneven spacing intervals, or for the case where a single plane of perfora-

Jan 1, 1967

By P. D. White, J. T. Moss, J. S. McNiel

Results of experimental work on the in situ combustion process were first published in this country in 1953' when Kuhn and Koch described results of a three-well test in Jefferson County, Okla. Shortly there-after Grant and Szasz2 described field studies in Nowata County, Okla., in which several modifications of the basic combustion process were investigated by injection of various oxidizing gas mixtures other than air. In the past five years speculation concerning this method of oil recovery has continued, with a number of interesting papers on various aspects of in situ combustion appearing in the literature3,4,5,6,7. However, only one of these' provided actual engineering information on pattern-type field experiments. The primary objectives of the Oklahoma three-well test were to check operation of specially designed electrical ignition equipment and evaluate problems associated with initiation of combustion in a natural oil sand reservoir. Immediately following successful completion of this test in the Pontotoc sand, plans were activated for a second field experiment to be conducted in the same sand a short distance away. The objective of this second field test1 as to establish a relationship between field observations and information derived from laboratory experimentation and computations. Secondary objectives of the test were to develop operating tech- niques and define operating problems, and to obtain information that would assist in the economic and engineering appraisals of the process. Careful planning was required since this test was designed with the hope of providing basic information on the characteristics and operation of a combustion drive. It was necessary to include test facilities which would not only permit precise control and measurement of the process variables but would also provide sufficient flexibility of control to insure that variables in the combustion process could be studied during the course of the test under a wide range of conditions. In order to accomplish these objectives elaborate instrumentation and several control wells were included in the design of the test installation. This type installation was felt to be well suited for an experimental study, but was in no respect intended as a counterpart of a commercial-scale operation. PRELIMINARY LABORATORY WORK An important objective of the field experiment, as stated previously, has been to obtain reliable data on operating variables which might be compared with similar data obtained in laboratory combustion tests. The value of successful correlations between quantities that can be measured in the laboratory and those obtained in a full-scale commercial venture has been well established for other industrial processes. The difficulty of following a process underground should make such correlations even more essential here. Also. approaching the field test phase of development of in situ combustion, it was considered desirable to precede design of test equipment with laboratory combustion studies under a variety of conditions to establish likely ranges of variables. These included temperature, air injection rate, frontal advance rate and produced gas composition.

By G. S. Scott, G. W. Jones

ECONOMIC waste caused by mine fires may become considerable,15 especially if a fire is allowed to spread or temporarily to get beyond control. It is important, therefore, to act promptly whenever a fire is suspected and to make every action count. To contribute toward its extinction effectively it is necessary to know at the earliest possible moment, and continuously thereafter, what is happening at the seat of the fire, which may be in a remote or inaccessible area, and also to recognize what may be expected as a result of any proposed combative measure. In combatting a fire the mining engineer and the chemist should cooperate, first deciding upon the course of action to be taken and then drawing upon the mining engineer's intimate knowledge of the physical structure of the fire area, the cost and time required to carry out proposed operations, and the probable efficiency with which these operations could be performed, and upon the chemist's knowledge for the results to be expected therefrom. After the initial steps to be taken have been decided, it devolves upon the mining engineer to see that they are carried out and upon the chemist to evaluate the results and to keep the mining engineer continuously informed in regard to a variety of matters-such as the composition and toxic or asphyxiating properties of the atmosphere in which the men may be working, whether the fire is increasing or decreasing in intensity and its probable temperature, the quantity of air leakage and the explosion hazards of the fire area. The purpose of this paper is to discuss what the chemist can and cannot contribute as a member of the fire-fighting personnel. The technical literature contains several hundred papers relating directly and indirectly to mine fires, and this fact alone is testimony to the complex nature of the phenomena involved in the birth, life, and final demise of a fire. A fire may be stopped (I) by preventing oxygen from reaching the coal or (2) by removing the conditions necessary for the rapid reaction of coal with oxygen; i.e., decreasing the temperature. All methods of prevention or control. necessarily must be based upon one or the other, or both, of these two principles. . The chemistry of a fire may be understood readily if the low-temperature oxidation of coal is considered as a starting point; then oxidation at higher temperatures (or combustion) ; and with these, the composition of the solid and gaseous products resulting from the oxidation or from the effects of the heat liberated. This discussion refers particularly to Pennsylvania anthracite, although much of the material applies equally well to coals of lower rank. OXIDATION OF COAL Oxidation of coal fundamentally is confined to the surface; that is, the rate at which oxygen penetrates into the interior of a solid block of coal is so slow that it may be ignored.6,16 Oxidation starts when a fresh surface is exposed, and the rate is

Jan 1, 1942

By Raymond C. Boettner

The present work had for its purpose: 1) the identification of crack nucleation sites in AISI 4340, quenched to martensite and tempered over a range of 'temperatures; and 2) the comparison of fatigue processes in AISI 4340 with processes observed previously in pure metals From constant def1ection-bending fatigue tests, martensite boundaries were identified as the favored crack nucleation sites in quenched and tempered AISI 4340. It, also, was concluded that the fatigue processes operating- in this lous-alloy steel were similar to Processes observed in pure tnetals. ALTHOUGH much engineering data has been accumulated on the fatigue properties of quenched and tempered martensitic steels,' fatigue as a process is not as well understood in martensite as it is in pure metals.' Important features of the fatigue process, such as the identity of the nucleation sites, have not been determined in the commercially important high-strength low-alloy structural steels. The present work had for its purpose: 1) the identification of crack nucleation sites in a low-alloy steel, i.e., AISI 4340, which had been quenched to martensite and tempered over a range of temperatures; and 2) the comparison of fatigue processes in the AISI 4340 with processes observed previously in pure metals. This comparison of the fatigue processes in the different tempers was restricted to the high-strain low-cycle part of the S-N curve. Under these test conditions, previous work on a number of metals has shown that a large number of cracks are nucleated in less than 30 pct of the fatigue life.3 Furthermore, crack nucleation sites are not restricted to inclusions but are also associated with intrinsic structural characteristics of the metal. MATERIAL A 20-lb ingot of vacuum-melted AISI 4340 (for composition see Table I) was hot-rolled to 1-in.-diam rod and then cold-rolled to a 1-in.-wide strip, 0.08 in. thick. Fatigue specimens, see insert of Fig. 1, were machined from the strip with the long dimension parallel to the rolling direction. m this orientation, the stringers of 1 to 2 p inclusions present in the sheet lay parallel to the stress axis in the specimens. The specimens were austenitited at 2050°F in order to obtain a large prior austenite grain size, i.e., 2 mm, which facilitated the subsequent identification of the prior austenite boundaries. A helium atmosphere was used to minimize decarburization. After austenitiza-tion at 2050°F, the specimens were transferred to a 1450°F furnace so that specimen distortion was held to a minimum in the subsequent oil quench. Previous work4 indicated that refrigeration in liquid nitrogen prior to tempering reduced the percentage of retained austenite in the quenched specimens to less than 5 pct. Tempering was carried out in air over the temperature interval of 200°to 800°F to produce a range of mechanical properties, Table I. The preparation of the fatigue specimen was completed by grinding about 0.005 in. from each surface and electropolishing in a chrome trioxide-acetic acid solution for 30 min. Examination of etched cross sections of specimens prepared in this fashion showed the foregoing specimen preparation to be adequate for the removal of the decarburized layer present after the heat treatment. Transmission electron microscopy showed that the as-quenched microstructure of this alloy consisted of a mixture of martensite plates containing either a high density of dislocations or microtwins. Previous work5'6 indicated that in the course of oil quenching autotem-pering resulted in the formation of E carbide on the martensite and microtwin boundaries. Tempering for 2 hr at temperatures up to about 400°F resulted in further precipitation of the E carbide. Finally, at about 400°F, cementite began to replace the E carbide on the martensite and microtwin boundaries in addition to forming a Widmanstatten structure within the plate matrix. EXPERIMENTAL S-N curves were obtained using electropolished specimens cycled at 1800 cpm as cantilever beams in fully reversed bending at selected constant deflections. The deflections were translated into surface strains by means of a calibration curve obtained through the use of strain gages. An argon atmosphere was used to minimize environmental effects. To investigate the development of fatigue slip bands, the specimens of the different tempers were unidirec-tionally bent to a surface strain of 0.005 to 0.007, photographed to record the location and appearance of slip bands so introduced, and then cycled to failure

Jan 1, 1968

By K. D. Jacob

IN the decreasing order of the tonnages involved, the uses of phosphates can be grouped conveniently into three general classes, namely, fertilizer; chemicals for military, industrial, and technical purposes; and mineral feed for livestock. The quantity of phosphate used as fertilizer, principally in the form of superphosphate, has always exceeded by far that used for all other purposes, though in recent years a marked increase has occurred in its consumption for the other two general classes of uses. Prior to the present century large quantities of superphosphate, as well as a considerable portion of the production of phosphorus chemicals, score made from bone materials which were plentiful and cheap in some areas and which could be more easily processed than phosphate rock for the manufacture of chemicals. Today, however phosphate rock has almost completely displaced bone as a raw material for the manufacture of chemically processed phosphates in nearly all countries of the world.

Jan 1, 1944

By Henry Faul

Measurement of radioactivity of rocks and ores has developed into a complete method of geophysical exploration. The problem falls into three natural categories: (1) surface radiation measurement in the field and underground; (2) radioactivity logging of drillholes; and (3) laboratory analysis of samples. Portable counters are used in the field for tracing radioactive formations and for quanti tative estimates of radioactive content of surface rock. Wartime advances in battery design make it possible to construct small precision counters that can be carried easily. Even the smallest conventional diamond drillholes can be logged, and actual content of the radioactive element can be measured. The exact grade of very thin active layers or veins can be estimated only approximately. Samples may be analyzed for their alpha, beta or gamma activity, and beta assaying is the best suited to rapid routine operation. Simple calibration with standard samples is sufficient for rough work, but a density correction is necessary when greater precision is required. Samples with high emanating power should be fixed and stored for three weeks to reestablish the radium-radon equilibrium prior to precision assaying. Carno-tite can be fixed by sintering or molding with plastics. Among the important new developments, a low-voltage Geiger tube has been 'designed recently, and crystal scintillation counters hold great promise for high-efficiency gamma-ray measurement. Introduction During the last few years we have witnessed an unprecedented rise in the demand for radioactive minerals, coming as a direct consequence of the discovery of nuclear fission and subsequent developments, the full impact of which is by no means in sight even now. It remains certain, however, that radioactive minerals, and especially those which can be used as ores of uranium and thorium, will continue to be of great interest not only to the prospector and mine operator but also to the various inspection parties envisioned by most of the schemes advanced for the control of nuclear energy on a world-wide basis. It is clear, therefore, that the measurement of radioactivity in rocks in the field as well as in samples in the laboratory has become a method of geophysical exploration of some importance. If we consider the recent technological advances in the general fields of nuclear physics and electronics it seems proper to review the present status of the methods and procedures of radiological exploration. General Considerations Equilibrium If we take a fixed amount of uranium that has just been purified, some of it will immediately start decaying into its first daughter element which in turn decays into its own daughter and so on down the line until the last daughter is reached—a stable isotope of lead. The rate at which a radioactive element decays is frequently expressed as the half-life, which is the length of time required for the decay of half the atoms in a given amount. The half-life is inversely proportional to the decay constanl X which is defined as the number of atoms which decay in one unit of time divided by

Jan 1, 1949

By Henry Faul

Measurement of radioactivity of rocks and ores has developed into a complete method of geophysical exploration. The problem falls into three natural categories: (1) surface radiation measurement in the field and underground; (2) radioactivity logging of drillholes; and (3) laboratory analysis of samples. Portable counters are used in the field for tracing radioactive formations and for quanti tative estimates of radioactive content of surface rock. Wartime advances in battery design make it possible to construct small precision counters that can be carried easily. Even the smallest conventional diamond drillholes can be logged, and actual content of the radioactive element can be measured. The exact grade of very thin active layers or veins can be estimated only approximately. Samples may be analyzed for their alpha, beta or gamma activity, and beta assaying is the best suited to rapid routine operation. Simple calibration with standard samples is sufficient for rough work, but a density correction is necessary when greater precision is required. Samples with high emanating power should be fixed and stored for three weeks to reestablish the radium-radon equilibrium prior to precision assaying. Carno-tite can be fixed by sintering or molding with plastics. Among the important new developments, a low-voltage Geiger tube has been 'designed recently, and crystal scintillation counters hold great promise for high-efficiency gamma-ray measurement. Introduction During the last few years we have witnessed an unprecedented rise in the demand for radioactive minerals, coming as a direct consequence of the discovery of nuclear fission and subsequent developments, the full impact of which is by no means in sight even now. It remains certain, however, that radioactive minerals, and especially those which can be used as ores of uranium and thorium, will continue to be of great interest not only to the prospector and mine operator but also to the various inspection parties envisioned by most of the schemes advanced for the control of nuclear energy on a world-wide basis. It is clear, therefore, that the measurement of radioactivity in rocks in the field as well as in samples in the laboratory has become a method of geophysical exploration of some importance. If we consider the recent technological advances in the general fields of nuclear physics and electronics it seems proper to review the present status of the methods and procedures of radiological exploration. General Considerations Equilibrium If we take a fixed amount of uranium that has just been purified, some of it will immediately start decaying into its first daughter element which in turn decays into its own daughter and so on down the line until the last daughter is reached—a stable isotope of lead. The rate at which a radioactive element decays is frequently expressed as the half-life, which is the length of time required for the decay of half the atoms in a given amount. The half-life is inversely proportional to the decay constanl X which is defined as the number of atoms which decay in one unit of time divided by

Jan 1, 1949

By E. G. Bailey

The bituminous coal industry faces a real problem, if it desires to retain the position in the power-generation field to which it is economi-cally entitled. More power is probably produced today for electrical energy, for steam-driven and steam-heating industries and processes, for transportation by rail, water, highway and air, collectively, than ever before, and yet the total bituminous coal production has decreased about 38 per cent, from 575,000,000 tons in 1926 to 357,500,000 tons in 1934. It is not the intention of the writer to recommend coal as a fuel for automobiles and airplanes, but rather to point to these forms of transpor-tation as being responsible in a very measurable degree for reducing the coal consumed by railroads. Petroleum products may still further reduce consumption of locomotive fuel through the extension of the use of Diesel-driven trains. Oil-burning steam-driven locomotives are replacing coal in some places, where railroads operating high-speed pas-senger trains are willing, temporarily at least, to pay a premium for the fuel, that is low in ash and produces less smoke and practically no cinders. In the navy and ocean-going passenger ships, oil is so firmly estab-lished, and has such definite advantages over coal as formerly fired, in steaming radius, in ease of bunkering, cleanliness, and reduction in firing labor, that very outstanding developments in the handling and burning of coal will be required in order to replace oil. For freighters on the Great Lakes, coal is the logical fuel, but there is great and immediate need of radical improvements in its use, else that market also may be lessened. It is not within the scope of this paper to discuss in detail bitumi-nous coal for either locomotive or marine use, but, rather, generation of power in stationary plants, consisting of electrical generating stations and that very large group of miscellaneous industrial plants, such as paper, rubber, textile, steel and other industries that use electrical, mechanical, and steam power, derived from either hydro or some form of fuel.

Jan 1, 1935

By G. C. Trevorrow

STRIP mining during 1943 increased considerably with further extension of mechanical loading in mines already partly mechanized; with the considerable introduction of mechanical loading into hand-loading mines; and with improvements in the use of loading equipment. Extension of the use of machinery both in strip mining and underground is due to reduction in labor supply and increased cost of labor, together with the increased demand for coal during the period of labor shortage.

Jan 1, 1944

By K. A. Natarajan, I. Iwasaki

Platinum electrodes are not inert as often thought to be. The reactivity of platinum electrodes can explain their erratic behavior in many electrochemical measurements of metallurgical interest, e.g, in flotation systems, streaming potential measurements, contact-angle measurements, and in leaching systems. The anomalous behavior of platinum electrodes in redox potential measurements in aqueous systems was studied through Eh and pH measure ments in water-oxygen, iron-water-oxygen, and manganese-water-oxygen systems. Stability relations between Fe++ and Fe (OH), and between Fe (OH), and Fe (OH), were studied to judge the correspondence between experimental and theoretical equilibrium lines. The practicality of redox potential measurements in estimating ferric-ferrous ratios in aqueous systems was investigated along with their suitability as indicators in leaching operations, e.g., the removal of iron by aeration from manganese leach solutions. Platinum electrodes have often been used in the measurement of dissolved oxygen concentrations and of redox potentials (Eh) in a variety of fields, e.g., analytical chemistry,' corrosion," geology and mineralogy,,'' biology,"' sewage treatment,' * hydrometallurgy,"I" and flotation."la The effectiveness of Eh-pH diagrams, first reported by Pourbaix' in 1949, has contributed much towards the theoretical understanding of numerous problems encountered in the metallurgical industry. Not many references are available in the literature, however, wherein attempts have been made to confirm Eh-pH diagrams from experimental measurements. One reason might be that, in spite of the apparent simplicity of the electrochemical technique, the direct measurement of Eh involves complex practical problems.' Factors such as the purity of the solution, the type of electrodes used, the history of the indicator electrode, and the type of atmosphere (namely, oxidizing, reducing, or inert) do have effects on the measured Eh values. The influence of mixed potentials cannot be underestimated. The poisoning of platinum electrodes by organic and inorganic impurities present in the solution may lead to erratic results. Platinum, commonly thought to be an inert electrode material, is not really so, as attested by a number of previous investigators who advised caution concerning the anomalous behavior of platinum electrodes in various electrochemical measurements.'" In the present article, a few pertinent experiments related to Eh-pH measurements in systems of interest in the metallurgical and water pollution fields are described in an attempt to correlate such information with what is already known, especially in the electrochemical literature. Iron-water and manganese-water systems were selected with a view of studying the correspondence between experimentally observed and theoretically established equilibrium lines. The work included an investigation of the behavior of platinum electrodes with respect to pretreatment and adsorption characteristics, the measurement of dissolved oxygen concentrations and their relation to Eh, the determination of the electrode potential of the ferric-ferrous couple at different pH, and the measurement of oxidation potentials in iron-manganese leaching systems. Experimental Procedure A rotating platinum electrode was used in many of the measurements to study the effect of rotation on measured Eh values. The electrode made by the Pine Instrument Co. consisted of a stainless steel rod with a platinum disk soldered to the end. It was covered with a Teflon insulation along the sides, so that only the circular tip of the electrode was exposed to the solution. Prior to its use, the platinum surface was brightened on a metallurgical polishing wheel with alumina as an abrasive, unless specified otherwise. The electrode was rotated with a Sargent cone-drive motor at 350 rpm. The contact of the electrode with the external circuit was made by filling a notch at the top of the stainless steel shaft with mercury and by dipping a copper wire into the mercury pool. The performance of the rotating platinum electrode was compared with the performances of a Beckman platinum button electrode and a platinum wire electrode. All the potentials were measured with respect to a saturated calomel electrode. A saturated KC1-agar bridge was used to minimize the liquid junction potential. A Beckman Zeromatic pH meter together with a Beck-man electrode switch was used to measure both the Eh and pH. A double-walled, all-Pyrex jar with a capacity of about 1 liter and themostated by circulating water of constant temperature was used for a reaction cell. Four equally spaced ports in the cover provided access for a glass electrode, a salt bridge connecting the saturated calomel electrode, a dispersion tube for bubbling gases into the cell solution, inlet and outlet tubes for passing the desired gases over the solution, and a graduated burette for introducing reagents from outside. The rotating platinum electrode was inserted through an opening in the top-center of the cover, and a positive gas pressure was maintained inside the cell to prevent air from entering into the cell compartment. A magnetic stirrer was used to mix the solution inside. For the determination of dissolved oxygen in the test solutions, the polarographic techniquex was used.

Jan 1, 1971

By N. W. Perry

Some months ago a gentleman gave me a handful of minerals which he had collected in an arroyo, or dry stream-bed, that ran through the town of Ramos, State of San Luis Potosi, Mexico, as a sample of the class of ore that might be expected in the mines of that section. I was, however, familiar with those mines and their ores, and cast the pebbles aside as of no interest. I afterwards returned to Mexico and took charge of two groups of mines, one in the State of Zacatecas, and the other in the town of Ramos, State of San Luis Potosi. While I was thus engaged, it was a very frequent occurrence for parties to bring me specimens of rock, ores, etc., for my opinion on them; and one day a man brought me a half-dozen or more small pieces of a very black shiny mineral, desiring to know what it was. I did not recognize it, and desired him to give me the specimens for analysis, which he promised to do in a day or two. He never did give them to me, for he lost them ; but he said there were plenty more where these came from—at Ramos—and he could get them at any time for me. I thought no more of the matter until after my return to this country, when, one day, in looking over some of my old " trash," I came across the specimens at first referred to as having been cast aside so carelessly. I noticed two distinct minerals among the pebbles : one being erubescite or tetrahedrite, the predominating mineral of the mines of Ramos, and the other a hard black shining mineral, the same that I had wished to analyze in Mexico. On testing for hardness I was surprised that it scratched topaz with some degree of ease, thus placing it above 8 in the scale of hardness. Trying it with a corundum, I sometimes succeeded in scratching it, but at other times it would scratch the corundum, and at still other times neither would produce the slightest effect on the other. Crystallized topaz would be ground to a powder in attempting to scratch the black mineral, without abrading it in the slightest. It must, therefore, be placed at 9 in the scale of hardness. It is of the deepest opaque black, not unlike pitch-blende in ap-

Jan 1, 1884

TWENTY-FOUR of the 28 local sections and the two divisions of the Institute were represented at the meeting. Three sections failed to appoint delegates and two of those appointed failed to attend the delegates' meeting proper. Four sessions were held, two on Monday and two shorter adjourned ses-sions on Tuesday and Wednesday. Even at the end many things remained to be said and, in view of the amount of time the delegates lost from technical ses-sions the feeling was general that next year it would be advisable to hold their meeting the day before or day after the general meeting. Every part of the country was represented from Boston to Los Angeles and Seattle to Washington. All phases of Institute work and policy were taken up in the most informal way and the delegates will carry back to the sections, as they brought to headquarters, many ideas that will prove useful and stimulating. The time was divided between reports by the delegates on section activities and reports by officers of the In-stitute and of the various joint activities on the work at headquarters : A. D. Flinn told of the work of Engi-neering Foundation; W. V. Brown discussed the Em-ployment Service; J. A. Sohon explained what the Library is doing; T. T. Read told how the sections could help MINING AND METALLURGY ; H. Foster Bain discussed Institute affairs in general and asked and answered questions. An interesting new feature of the meeting was the appearance by request of Directors Turner and Smith of the U. S. Bureau of Mines and U. S. Geological Survey to answer inquiries as to the needs and work of their Bureaus. So much attention had been paid this year by the western sections to the diminished funds made available at Washington for research on mining problems that many questions came up. The accom-panying figures epitomize the answers.

Jan 3, 1928

By M. S. Rashid, C. J. Altstetter

Allotropic transformations in cerium have been studied by dilatometric, resistometric, X-ray diffraction, and metallographic techniques. The dilatometric study indicated that, on cooling below O°C, the high-temperature fcc phase, y, transforms partly to the hexagonal phase, ß, and, on further cooling, to the collapsed fcc phase, a. The amount of $ phase present at room temperature is increased by repeated cycling through the a-y transformation. It has been shown metallograPhically that the y-ß transformation has many characteristics of a martensitic transformation. In contrast to the y-ß transformation the ?-a transformation does not give the manifestation of a shear transformation. Small cellular ? domains of random shape and size collapse to a in a short time with no apparent coordination with neighboring domains. The considerable confusion in the literature over the existence of more than one high-temperature fcc phase is discussed. Two such phases have been reported in the literature and an attempt is made in this study to clarify the situation. Twelve fcc and two hcp structures have been shown to be easily reproduced or eliminated. It is proposed that the two "additional" allotropes reported in the literature and fourteen of the phases detected here are not allotropes of cerium but are due to contamination. CERIUM exists in several allotropic forms, but there is some disagreement over what the forms are. Furthermore, the conditions favoring the presence of a particular allotrope and the nature of the transformations from one form to another are uncertain. The objectives of this research were 1) to ascertain the allotropic forms of cerium, 2) to establish the conditions under which the allotropes exist, 3) to study the effects of annealing and thermal cycling on the allotropic transformations, and 4) to study the transformation mechanisms. Dilatometric, resistometric, metallographic, and X-ray diffraction techniques were employed. The form of cerium commonly found at room temperature is fcc and is designated ?. A complex hexagonal phase, 8, forms when y is cooled to slightly below room temperature. At still lower temperatures the y fcc structure transforms to an fcc form with a much smaller lattice parameter, termed a cerium. A bcc form, 6, which exists just below the melting point (800°C), will not be considered further in this work. There is a substantial body of experimental evidence (reviewed by Gschneidnerl) which favors the acceptance of these four allotropes, though some investigators have tried unsuccessfully to observe the ß hexagonal form.'-' There is disagreement, however, over the phase-transformation temperatures, due, in part, to broad hysteresis and overlapping of the transformations between the a, ß, and ? forms. The transformations are also sensitive to prior thermal and mechanical treatment. The differing purity of cerium used by different investigators is undoubtedly a factor. Cerium is difficult to separate from other elements and is quite reactive, igniting spontaneously when it is filed in air. The highest purity of cerium to date is reported to contain several hundred parts per million by weight of impurities, and early investigations were carried out on cerium containing several percent of impurities. There have been reports of more than one fcc allotrope at room temperature. Gschneidner, Elliott, and McDonald5 obtained diffraction patterns of an fcc phase with a lattice parameter about 1 pct less than that of the ? phase, instead of the y phase, on slowly cooling cerium filings from 23° to -198°C and warming them back to room temperature. However, when the sample was heated to 447°C and cooled to room temperature it consisted of only the ? phase. They have designated this new fcc phase "a-? intermediate", and say it is quite sensitive to impurities. After prolonged high-temperature treatment of a powder specimen, Weiner and Raynor2 obtained a diffraction pattern of an fcc phase of lattice parameter about 1 pct less than the ? phase. This they called the y' phase. It could not be reconverted to the y phase and is claimed to be different from the a-? intermediate phase.5,6 Dialer and Rothe3 reported two fcc phases* after cycling their powder specimens between room temperature and -192°C. Gschneidner, Elliott, and McDonald5 suggested that one of the fcc structures obtained by Dialer and Rothe was equivalent to their "a-? intermediate" phase. Table I presents some pertinent data on the proposed allotropes. For the ?(fcc)-ß(hexagonal) transformation

Jan 1, 1967

By R. J. Stoehr, F. Howell

Since the ore mined in the Grants-Ambrosia Lake uranium area is taken from a water-saturated sandstone formation, part of the milling operation includes a drying process. The authors discuss the merits and disadvantages of two methods: natural drying and mechanical gas-fired drying; operating and cost data are included. In the Grants-Ambrosia Lake uranium area, approximately 7000 tons of ore are mined each day from a water-saturated sandstone formation. This ore is sampled and treated at four separate milling operations. Prior to the design and initial construction of the milling facilities, very little was known as to the physical properties of the ore which would be handled in the sampling and crushing facilities at the mills. All four mills initially were constructed without ore-drying facilities. As mining proceeded, it was determined that, even after drying the ore in place by use of drainage development underground, the moisture content of the ore as hoisted averaged approximately 18 pct. Actually, some of the mines produced ores which resembled cream-of-wheat in character and had a moisture content in excess of 24 pct. Each of the four mills had a differently designed sampling and crushing plant; therefore, the moisture content of the ores had varying adverse effects upon the operation of the plants. It was determined after some experience that most of the sampling and crushing facilities could not economically handle ore if the moisture content was greater than 10 pct—one operator considers 12 pct moisture as a maximum. In all of the plants, moisture content over 8 pct increases costs to some extent. In addition to the added sampling and crushing costs, some of the mills were located 15 to 20 miles from the mines and the high moisture content of the ores increased the haulage costs from the mine to the mill. It was generally conceded that it was necessary to employ some method to reduce the moisture content of the ore prior to sampling. Several methods were considered: 1) natural drying at the mine site, 2) mechanical gas-fired drying at the mill site, 3) mechanical gas-fired drying at the mine site, 4) radiant heating on concrete clabs, and 5) infrared shed drying. After preliminary investigation all possibilities but natural drying and mechanical gas-fired drying at the mill site were eliminated. NATURAL DRYING A cooperative feasibility study was conducted on the natural drying method. This study indicated the following: 1) During summer months May through September, ore piled 4-ft deep would dry from +20 to +10 pct HzO in 30 days with no mechanical turning. 2) In the first four days after piling a reduction of 5 to 7 pct total moisture content was accomplished by drainage and absorption of the water into the underlying ground on which the ore was piled, providing the ground surface absorption rates approached 10 gal per sq ft per day. After the first four days the decrease of moisture caused by drainage was practically nonexistent. 3) In the summer months drying by evaporation amounted to approximately 0.1 pct decrease in total moisture per day and mechanical turning of the ore could increase this as much as three times. 4) Climatic conditions of the area indicated that: a) Air temperatures averaged 64' May, June, July, August, September; 41" October, November, December, March, April; 31" January, February. b) Average rain fall was 10 in. with 40 pct of this occurring during July and August. c) Only on very rare occasions were there over five consecutive days with below freezing temperatures. d) The annual evaporation rate was approximately 75 in. On the basis of this study, two of the mill operations decided to attempt to meet the moisture specifications by natural drying supplemented by mechanical turning. The other two operations decided upon rotary gas-fired drying at the mill site. The natural drying method has been quite successful in practice. The ore running approximately 18 pct moisture is trucked from the head frame and piled in rows about 6 ft wide, 3 1/2 ft deep, 5 feet apart during the months of May through September. In approximately 30 days this ore will

Jan 1, 1961

By H. L. Riley, B. W. Gandrud

AS far as the present writers know, this system of flotation has not been used elsewhere in this country, but in the last couple of years it has been introduced, with minor variations, at one plant in England and one in Wales.' The system has been described and discussed in a number of publications.2-5 The following is quoted from an abstract of the latest of these,5 a paper presented at an International Conference on Industrial Combustion in 1952. On the basis of experience to date with the commercial plants, it is believed that the kerosene-flotation process incorporates all the necessary elements to make it greatly superior to anything else now available for treating of fines in wet processes of coal preparation. Additional study and investigation are still needed, however, to determine if certain phases of the process can be improved to such an extent as to make it generally satisfactory and acceptable to the industry. Further improvements will be needed with respect to the capacities of the flotation cells and the reagent consumption. The situation referred to above explains why an investigation is being made of the possibilities of achieving better cell capacities. Results obtained from this investigation, which is still in progress, are believed significant with regard to both cell capacity in general and the relation of cell design to cell capacity in particular. Commercial equipment now being used in a laboratory-type investigation should have performance characteristics similar to those of the larger machines. Equipment and Procedures: All flotation tests have been made in a standard Denver sub-A 24x24-in. unit cell of 12-cu ft volume. Cell modifications to make it more suitable for the tests were an adjustable front-wall section for varying cell depth and a perforated scraper-drag assembly for removal of the float product. There is also an apron dry-coal feeder, a gravity-feed water supply, reagent feeders, and a centrifugal pump that feeds the mixture of coal, water, and reagents into the flotation cell. A wattmeter connected into the drive-motor circuit records the power requirements of the impeller throughout each run. Dry coal, water, and reagents are all fed through a pan-type intake to the feed pump. A Sturtevant blower was set up to furnish air for supercharging. A centrifugal pump with a garbage-can intake provides for disposal of refuse flow to an outside settling tank. Figs. 1 and 2 show the flotation cell; Fig. 2 also illustrates the blower for supercharging. For purposes of this investigation, the percentage by weight of the feed coal recovered in the float product under a standard set of conditions has been considered as the criterion of cell capacity. The authors realize that such a criterion may be somewhat unorthodox, as the term cell capacity is usually understood to refer to feed input and ordinarily takes into account the ash analyses of the float product and refuse. However, the word capacity is flexible enough so that Webster gives one definition as maximum output, a definition which seems to justify, at least partly, acceptance of the above criterion. It has been the authors' experience in the Birmingham district that the ash-reduction efficiency of the coal-flotation process is generally satisfactory and that the only real problem is to increase the rate of float recovery so that the feed rate to any given bank of cells can be increased without undue loss of coal in the refuse. Originally it was planned to operate the flotation cell to simulate continuous operation during sampling periods. It was assumed that operating for reasonable time with feed coal, water, and reagents turned on would stabilize conditions so that the weight of float coal discharged during a fixed time interval would be an accurate measure of the rate at which the coal was being floated. It developed, however, that this supposition was erroneous. The float coal, caught for fixed time intervals and weighed, gave widely varying results in duplicate runs. Efforts to correct this trouble failed, and it was decided to try to operate on a batch-test basis, whereby all the float coal produced during a run on a known weight of feed coal would be caught in tubs, dewatered, and weighed. This method gives consistent and reproducible results, with total float product weight rarely varying by more than 3 or 4 pct on duplicate runs. The standard test procedure is as follows: A 132-lb sample of dry feed coal is weighed and placed in the feed hopper. The feeder is adjusted for a rate of 800 lb per hr. Feed water and reagents are turned on, and the feed and refuse pumps are started. One minute later the impeller is started. Six minutes are allowed for the cell to fill up with the water-reagent mixture. The feed of dry coal is started at the end of this 6-min period. One minute later the float-coal removal drag is started. The float coal is caught in one tub for the first 6 min after the flow of feed coal starts. Tubs are then changed, and the float coal is caught in a second tub until the feed coal runs out, when the tubs are again interchanged to catch the float coal for the remainder of the run in the first tub. The cell is kept running for 3 min with the water and reagents on after the feed stops to allow residual float coal to be removed. At the end of a test the wet float coal in both tubs is weighed and the total weight recorded. The product in the second tub is used for moisture determination and screen-size analyses. When the

Jan 1, 1956

By D. C. Seidel, E. F. Fitzhugh

The Colorado School of Mines Research Foundation has developed a hydrometallurgical process for recovering nickel from oxidized ores, including both the iron-rich laterites and magnesium-rich, soft silicates. Known as the HSO-HTCP (Hydrothermal Sulfidization Oxidation-High Temperature Cementation in Pulp) Process, the system consists of feed preparation, sulfidization, oxidation, precipitation (cementation), and calcination and melting. This paper deals primarily with the sulfidization and oxidation phases of the process. Nickel sulfide ores lend themselves readily to concentration before smelting or pressure leaching, but neither of the major oxidized ore types — the iron-rich laterites and magnesium-rich, soft silicates-has been directly concentrated. Upgrading of crude ore in current practice is limited to cobbing lumps of the harder, lower grade rock (protore) from the softer, enriched silicate ore, because only a small percentage of the nickel in these ores occurs in discrete, contrasting mineral particles. There is no apparent mineralogical contrast in the superficial, iron-rich lateritic ores and, in fact, there is no firm assurance that the nickel atoms are within the lattices of the limonite minerals, or else irregularly adsorbed on the limonite. Within underlying, "rotten rock" silicates, occasional veinlets of gamierite and related nickeliferous silicates are found.' The gamierite veinlets, however, are only incidental, and the majority of the nickel atoms occur as erratic replacements of magnesium atoms in the micaceous chlorites of the ore mass. Pyrometallurgical processes account for nearly all the nickel currently being recovered from oxidized ores. Plants in New Caledonia, Oregon, Japan, Brazil and Greece smelt the ores to make ferronickels or a sulfide matte,2 and the ammoniacal leaching3 at Nicaro, Cuba, is preceded by a reducing roasL4 The only fully hydrometallurgical installation has been the politically ill-fated Freeport Nickel Co. enterprise, and this process was limited to lateritic ores.5p6 A hydrometallurgical technique which might handle both laterite and the typically richer silicate ores has been an enticing goal. The technique described here was developed at the Colorado School of Mines Research Foundation, Inc. on behalf of the Republic Steel Corp. It uses sulfur, heat, air and metallic iron to recover nickel from these ores. Inasmuch as the ores are treated as aqueous slurries, the cost of drying a plant feed that normally carried 30% or more moisture is eliminated, and there are no dust problems. Patent applications have been filed by Republic Steel Corp. on the procedures used for getting the metal into solution and on the subsequent recovery without liquids-so l ids separation of the slurry. It is referred to as the HSO-HTCP Process (Hydrothermal Sulfidization Oxidation — High Temperature Cementation in Pulp). THE PROCESS FLOWSHEET The results of various experimental studies have been combined to form the continuous flowsheet illustrated in Fig. 1. This flowsheet serves as a general pattern showing the sequence of the operations which include: (1) feed preparation; (2) sulfidization; (3) oxidation; (4) precipitation (cementation); and (5) calcination and melting. This paper deals primarily with the sulfidization and oxidation phases of the process. Feed preparation: In general, the silicate ores can be considered as earthy rather than hard, and preparation might be carried out before the addition of water in a trommel, or with water in a scrubber or log washer. This breaks up the earthy particles, allowing the hard lumps to be separated by screening. The oversize material from most ores is relatively barren and may be discarded. If there is occasion to control the iron-magnesium ratio in the plant feed, laterite, which normally breaks up readily into fine sized particles, and silicates are mixed in suitable proportions. The fine product slurry from the initial steps is mixed with elemental sulfur and fed to a conventional ball mill, although the amount of actual grinding that takes place is relatively small. The object of milling is to complete the disintegration to natural particle size and to produce an intimate mixture of the ore and elemental sulfur. This pulp, which is almost entirely -200 mesh, has a pH of about 7.0 and normally can

Jan 1, 1969

By M. D. Banus, M. B. Bever, A. K. Jena

The heals of formation at 78", 195, and 273°K of the ternary compound h3SbTe2 based on the elements and based on the binary compounds In Sb and [inTe have been measured. The heats of formation at these temperatlcres of the binary compounds In Sb and In Te based on the elements have also been determined. Heal contents and free energies of the three compounds have been calculated from 0° lo 80I)°K. The free energies of joyrrzalion, heats of formations, and entropies of formation at 298°K have also been calculated. The results shown that the tertnary compound is metastable with vespecl to InSh and ln Te below 696 °K. bul is slable above that temperature. The weaker bonding of results in a positice entropy of formation which with incrensirzg temperature makes increasing negative conlvihtclions to the free energy and above 696°K renders the compound slable. THE ternary compound In3SbTez occurring in the quasi-binary system In Sb- In Te' forms on cooling at 829°K by a peritectic reaction.' Observations at 673" and 573 K have shown that this ternary compound decomposes slowly into the binary compounds InSb and1n~e.l'' It has not been possible to analyze the metastable behavior of the ternary compound because up to the present time data on its thermodynamic properties have been lacking. Some information on the binary compounds, however, is available. The heat of formation of InTe at 273°K and its free energy at 673°K are kn~wn.~'~ The heats of formation of InSb at 78", 273', 298", and 723°K have been measured5-' and its heat capacity between approximately 12" and 300"Kg9l0 is also known. In the investigation reported here the heats of formation at 78% 195% and 273°K of the ternary compound In3SbTez have been measured. The heats of formation of the binary compounds InSb and InTe at these temperatures have been obtained by combining new calorimetric results with previously published data. The heat contents and free energies of the three compounds at various temperatures from 0" to 800°K have been calculated. Against the background of this information, the metastability of the ternary compound will be discussed. 1) EXPERIMENTAL 1.l) Preparation of Specimens. The materials used consisted of the elements indium, antimony, and tellurium, the binary compounds InSb and InTe, and the ternary compound In3SbTez. The elements, obtained from American Smelting and Refining Co., had a nominal purity of 99.999+ pct. The compound InSb was Cominco semiconductor grade; the compound InTe was prepared from the elements by melting under a vacuum of 10-h m Hg followed by slow cooling. Three batches of specimens of the compound In3SbTez were used. One batch was prepared by melting appropriate amounts of the elements in an evacuated and sealed Vycor tube. The melt was held at approximately 100°K above the liquidus for about 8 hr, shaken repeatedly, and quenched into a mixture of ice and water. The specimen was annealed in vacuum at 760°K for 4 weeks. In preparing a second batch, a mixture of the component elements was melted and quenched in water. The resulting ingot was powdered. The powder was pressed into pellets, which were annealed in vacuum at 748" to 773°K for 4 weeks. A third batch was prepared in the same manner as the second, except that the starting materials were InSb and InTe rather than the elements. Metallographic examination of samples of the three batches and X-ray diffraction examination of a sample of the second batch did not reveal evidence of microsegregation or a second phase. The results obtained with the three batches showed no systematic differences. 1.2) Calorimetry. The calorimetric method has been described in detail." Samples of the compound In3SbTez, mechanical mixtures of InSb and InTe in the proportion of 1:2, and mechanical mixtures of indium, antimony, and tellurium in the proportion of 3:1:2 were added to a bismuth-rich bath at 623°K in a metal-solution calorimeter. These additions were made from 78°K (liquid nitrogen), 195°K (dry ice and acetone), and 273°K (ice and water). The heat effects of the additions were measured. The difference in the heat effects of the additions of a compound and the additions of the mixtures of its constituents, adjusted for differences in the concentration of the bath, is the heat of formation of the compound. In the concentration range not exceeding 1.5 at. pct solute, the heat effect of the additions was a linear function of concentration. The heat of formation refers to the temperature from which the additions were made, namely, 78", 195", or 273°K. Several calibrating additions were made in each calorimetric run. The calculated heat capacity of the calorimeter and hence the calculated heat effects of the additions of samples depend upon the values adopted for the heat contents of the calibrating substance. In this investigation bismuth at 273°K was used and a value of 4.96 kcal per g-atom was taken for (HGZ3"k . 2) RESULTS AND DISCUSSION 2.l) Heats of Formation. The heats of formation of the ternary compound In~SbTez from the component elements indium, antimony, and tellurium and from

Jan 1, 1968

This paper "On Coal" was published in three issues of The Western Gleaner in 1814. Name of author is not given. This magazine was started by Cramer, Spear & Eichbaum, in Pittsburgh, Pa., in December 1813, and ran for about two years. Copies are very rare, and this one is made from an original in the Darlington Library, University of Pittsburgh. This is almost certainly the first general article on coal published west of the Allegheny Mountains, and one of the earliest in this country. ON COAL Its Natural History-Mining of Coal-Phenomena occasioned by Fire-damp-Method of Coking-Distillation of Tar from Pit-coal-Gas-light-Coal, a Manure I. NATURAL HISTORY OF COAL There are few productions of nature which present to the philosopher a wider field of investigation than pit-coal. A substance highly inflammable is found in the deep recesses of the earth, sometimes loaded with numerous superincumbent strata of hard rock, and extending frequently along with these strata through a vast expanse of territory. Though metals may be said to be inflammable substances, as they combine more or less rapidly with oxygen when placed under particular circumstances, yet the character of rapid combustion with disengagement of light and heat, seems to belong. principally to such substances as are derived either from the animal or vegetable kingdom. That this is probably the case with regard to coal we are further induced to believe, by the remarkable circumstance, that the chemical analysis of this natural production yields especially, though in various proportions, those materials which constitute essentially the vegetable. And if any thing was wanting to confirm, us in that opinion we might trace in a number of fossile substances the gradual transition of the vegetable into the state of mineral coal. This fact is so intimately connected with the natural history of coal, that we cannot think it superfluous to give it some farther development. Among the great number of principles which the chemist is capable of tracing in the vegetable kingdom, the presence of extract, resin and fibre seem to form the characteristical marks of plants.-If vegetable matter be boiled in water, and the water, after having been strained and filtered, be exposed for some time to the open air, a flocculent precipitate takes `place from every part of the liquor; which soon subsides to the bottom of the vessel containing it. This is the extract; altered, indeed, by exposure, and now no longer soluble in water, a change which is supposed to depend on the absorption of oxygen; and if, by any means the proportion of oxygen be increased, the extract gradually becomes of a darker color, blackens, and approaches to the state of charred wood.

Jan 1, 1942

By R. W. Hertzberg, F. D. Lemkey, J. A. Ford

The technique of unidirectional solidification has been applied to the A1-AI3Ni and A1-CuAl2 ezltectic alloy systems; the controlled microstructure of A1-A3Ni consists of parallel A13Ni whiskers emhedded in an aluminum matrix while the Al-CuAl2, system solidifies as parallel alternate lamellae of aluminm and CuAl2. Mechanical tests (tension and flexure) have shown that the particle-matrix interface bond formed during unidirectional solidification allowes for efficient load transfer from the matrix to the reinforcing phase. Strength and fracture characterstics of the alloys were studied as a function of phase orientation; the tensile strength of controlled Al-Al3Ni samples was 43,000 psi (three times greater than that of as-cast specime~s). The strength of the Al-CIA2, cutectic was studied as a function of lamellae-flexure stress-axis orientation using a microbend apparatus. A twofold increase in outer fiber stress was observed as the lamellae were rotated from a position of no reinforcing (perpendicular to the stress axis) to one of maximum reinforcing (parallel to the stress axis), The brittle reinforcing constituent in each alloy (A13Ni and CuAl2) was observed to he the nucleating phase for fracture. It is to be concluded from this investigation that unidirectionally solidified eutectic alloys have a potential use as reinforcing coniposite) materials. In a recent review article, Chadwick1 has described the work of many investigators in the area of controlled solidification of binary eutectic alloys. Thus far, more than twenty eutectic alloys have been unidirectionally solidified to produce structures consisting of two phases in the form of alternating lamellae or as whiskers embedded within a continuous matrix; in either case, the phases are aligned parallel to the growth direction. In particular, Kraft and Albright2 have shown that the Al-CuA1, eutectic alloy exhibits a lamellar microstruc- ture as a result of unidirectional solidification while Lemkey, Hertzberg, and Ford3 have studied the A13Ni whisker-aluminum matrix morphology in the A1-A13Ni system. Whether these alloys could exhibit reinforcing behavior would have to depend upon the strength and volume fraction of the reinforcing phase (AI3Ni and CuA12) and the nature of the bond between the reinforcing phase and the matrix. Hertzberg and Kraft4 have shown that the interface bond between chromium whiskers and a copper matrix in unidirectionally solidified Cu-Cr is particularly good while Lemkey and Kraft5 have reported chromium-whisker tensile strengths in excess of 1,000,000 psi. However, with the chromium volume fraction being less than 2 pct, no reinforcing behavior was displayed by the Cu-Cr alloy.6 In view of the encouraging results concerning the good interfacial bond and high strength of the reinforcing phase in the Cu-Cr system and preliminary mechanical test data reported by Lemkey et al.3 for the A1-A13Ni system, the A1-CuA1, and A1-A13Ni eutectic alloys containing 50 and 10 vol pct, respectively, of the reinforcing phase give promise of possessing mechanical reinforcing behavior. Based on this premise, the objective of the investigation was to study the strength and fracture behavior exhibited by these anisotropic microstructures. EXPERIMENTAL PROCEDURE Controlled Solidification Procedure. An extensive description of the technique of unidirectional solidification has been presented elsewhere.' However, the pertinent details for each eutectic system studied are discussed below. Al-A13Ni System. Several master heats of this alloy were prepared by vacuum-induction melting in an A12O3crucible and casting in SiO2 mold or by induction melting in alumina crucibles under argon. The initial heats were prepared from 99.99 pct A1 and 99.99+ pct Ni, while later heats used 99.999+ pct A1 and 99.99+ pct Ni. Specimens of these master heats were unidirectionally solidified using induction and resistance heating sources and argon atmospheres at growth rates from 1.1 to 28.7 cm per hr. The thermal gradients in the liquid were controlled in the range of 26" to 36°C per cm for these runs. Al-CuA12 System. The master heat and controlled

Jan 1, 1965