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By R. G. Jones, W. L. Kinney, R. E. Schilson, R. S. Wilson, G. A. Clark, H. Suralo

This paper discusses the results of the Fry conventional or cocurrent in situ combustion test, which was conduct-ed in a 3.3-acre inverted five-spot. The depth of the formation was between 880 and 936 ft; the oil had a specific gravity of 28.6° APl and a viscosity of about 40 cp at the reservoir temperature of 65°F. Preceding the combustion test, air injection tests were conducted which, in conjunction with geological studies, were used to evaluate the characteristics of the reservoir. Combustion was initiated on Oct. 13, 1961, with ignition being accomplished by a 40 kw electrical heater. The test phase of the project ended on Oct. 1, 1963. During the test, the average air injection rate was 1,520.-000 scf/D. Throughout the test, production of all fluids— gas, oil, and water—was monitored. Cumulative oil production credited to the project was 100,586 bbl. The cumulative air-oil ratio was 11,500 scf/bbl oil, and the oxygen uti1ization efficiency was 87 per cent. INTRODUCTION The Marathon Oil Co. conducted a successful in situ combustion test, beginning Aug. 22, 1961, at the Fry unit, Crawford County, 111. The purpose of the project was to test the feasibility of cocurrent in situ combustion as a means of oil recovery in the Fry type reservoir. Interest in in situ combulstion as an oil recovery tool has been stimulated mostly by the existence of large reserves of heavy viscous crudes with low expected recovery, usually less than 10 per cent. These are the so-called unrecoverable reserves, and most combustion tests to date have been conducted in this type of reservoir.1-4 In contrast, the Fry combustion test was conducted in a reservoir with a relatively high gravity oil having a relatively low viscosity. This paper discusses the performance of the test. The geology of the reservoir and the field operations are discussed in separate papers.5 TEST SITE The Fry combustion test was carried out in a 3.3-acre inverted five-spot portion of a lenticular body of Robinson sandstone. Net sand was 50 ft thick, porosity averaged 19.7 per cent, oil saturation was 68 per cent of pore volume, and water saturation was 20 per cent of pore volume. The oil in place was estimated at 1,040 bbl/acre-foot, or 171,600 bbl within the 3.3-acre pattern. The water in place was 326 bbl/acre-foot, or 53,800 bbl. The oil has a specific gravity of 28.7° API and a viscosity of 40 cp at the reservoir temperature of 65°F. AIR INJECTION PERFORMANCE Air injection took place in two phases, the phases separated by ignition of the reservoir. In the pre-ignition phase, air injection tests were conducted in the summers of 1960 and 1961. These indicated that the Fry reservoir was confined, and a high return rate of injected air could be expected. This proved to be an outstanding characteristic of the project, as cumulative gas production was 95.3 per cent of the air injected. The difference between the cumulative air injected and the total gas produced can be largely accounted for by the quantity of air stored in the reservoir. An estimated 16 X 10 cf of air remained in the burned-out portion of the reservoir and an indeterminate amount of gas was stored in the unburned but pressurized reservoir. Hence, a complete material balance of gases would account for nearly 100 per cent of the air injected. At times during the test, the daily gas production rate was 98 per cent of the daily air injection rate. Fig. 1 presents the air injection history of the Fry com-

Jan 1, 1966

By W. A. Ver Wiebe

It is becoming increasingly apparent that the State of Kansas contains one of the largest reserve areas for oil exploration in the United States. During the year 1936 no less than 54 new oil pools were discovered by drilling. In addition, seven gas pools were found, which may develop into oil pools when deeper horizons are tested. Several old pools increased their reserves when production was found in lower strata. The data presented in Table 2 indicate that nearly 2000 wells were drilled in the state during 1936. Of these more than 1214 found commercial quantities of oil and at least 61 found marketable quantities of gas. The data are conservative because complete results on drilling are not available for the eastern part of the state. Ellis, Rice and Russell Counties share honors with a total of 10 new pools in each. Barton County is prominent with six pools; while those counties claiming fewer new pools are Clark, Ellsworth, Harvey, McPherson, Ness, Pawnee, Rooks, Stafford and Trego. Important additions to our gas reserves were found in Finney and Haskell Counties, which are north of the extensive Hugoton gas area and may some day be part of it. At the close of the year there were 17,317 wells in the state rating as producers. By far the larger share (14,000) were classed as strippers and allowed to flow 100 per cent of their potential capacity, thus accounting for 33,500 bbl. a day. The remaining wells, capable of producing from 15 up to over 6000 bbl. per day, were limited in output according to these amounts. The largest wells having a potential of from 3000 to 7000 were allowed to flow from 2 to 3½ per cent of their official potential capacity. The percentage rises until wells of 15 to 20-bbl. capacity have a rating of slightly over 83. On the basis of these calculations the total potential capacity of all wells was 1,667,814 bbl., and the daily amount allowed was 175,851. Nine of the pools most recently opened were still unable to market their oil and were classified as "shut-in" pools. Total production for the state for 1936 was somewhat over 58 million barrels. Striking Geological Data Some interesting geological data were uncovered by deep drilling during the year. The most remarkable bit of information is the discovery

Jan 1, 1937

By M. J. Greaves, Alan English

Pelletizing on a commercial scale is only 10 years old; yet in this period more than 150 million tons of pellets have been produced. Instrumentation and controls have played an important part in the development of an entirely new industry in almost unprecedented time. Initially, most control circuits used in the pelletizing industry were manually operated, since the confidence factor in instruments and controls was quite low at that time. This changed considerably in recent years and improvements in the use of instruments and controls have probably developed more rapidly in pelletizing than in any other metallurgical process. Now, within a decade of the start of commercial operations, the use of manually operated controls has changed and consideration is being given to the utilization of computers for data logging and control purposes.

Jan 7, 1965

By N. Mao

This paper presents the results of a research effort to develop a technique for estimating in situ stresses by measuring stress-induced velocity anisotropy around a borehole. Relevant parameters required to make the estimate were identified and measured in the laboratory on a 35.6 cm (14.0 in) cube of Nugget sandstone with a 10.2 cm (4.0 in) diameter hole, under biaxial loading. Two pairs each of radially and tangentially polarized transducers were placed inside the hole with displacement directions either parallel or perpendicular to the principal stress directions. With this configuration, relative travel times were measured by both a pulsed phaselocked loop technique and a cross correlation of digitized waveforms. The biaxial velocity data were used to back-calculate the applied stress. The standard deviation of the differences between the calculated and applied stresses is 0.62 MPa (90 psi) for a stress level up to 8.63 MPa (1250 psi).

Jan 1, 1984

By HOMER L. WILLIAMS

WHILE some of the mining companies have been pumping a small amount of water for some time, it is only in recent years that large quantities of water have been encountered in the Tonopah district. The water appears to be in different zones or belts so that the draining of one property does not necessarily affect the one adjoining. Consequently, each company has its own pumping plant and its own conditions. The companies panes handling the largest amount of water are the Tonopah Extension Mining Co., Halifax Tonopah Mining Co., West Tonopah Consolidated Mining Co., and Great Western Consolidated Mining Co. The Halifax shaft is on the eastern end of the district and the other three properties on the western. The ore-bearing formation occurs at greater depth on -the eastern and western ends, hence the water problem in these properties.

Jan 1, 1921

By S. Shapiro, G. Krauss

The strutural and cr~stallo~aphic features of the plates of austenite produced by the martensite to aus-tenite or reverse martensitic tramformation have been determined in an Fe-33 wt pct Ni alloy. Micro-focus X-ray techniques and single-surface trace analysis 072 bulk samples yielded two distinct habit planes, (0.174, 0.309, 0.~35)~ and (0.375, 0.545, 0.749jM. The former plane uas the one predorninantly observed and its existence was verified by transn~ission electron microscopy. The orientation relation-ship between the reversed austenite and the parent martensite was approximately the same as the Nishiyamna and other relationships reported for the direct tramformation. Replica and thin-joil obser-vations show that both high densities of tangled dis-locations and occasional twins constitute the fine structure of the reversed austenite. Application of the phenomenological theory to a variant of the predominant habit plane defines an irrational plane and direction for the second shear in accordance with the comnplexity of the fine structure. The shear accompanying the reverse martensitic transformation is at least 0.51, the maximnum value of- the tangent oJ the tilt angle measured on surface replicas. A mechanism relating the fine transformation twins in martensite to the nucleation of reversed austenite of the predominant habit is proposed. The reversal of Fe-Ni martensite takes place both at the edges of martensite plates and in a piecewise fashion within them.' The shear-type nature of the reverse transformation is verified by the surface relief which accompanies both edge-type reversal2 and the fragmentation of plates of martensite' as a result of rapid heating above the A, (austenite start temperature). The orientation relationship between the edge-type reversal product and the parent martensite, as determined by transmission electron microscopy, is reported to be within 4 deg of either the Kurdyumov-Sachs or Nishiyama relationships,' but there is no work at present in the literature relating to the crystallography of the platelike reversed austenite. The fine structure of reversed austenite after heating to 50°C above the Af is reported4 to be composed primarily of tangled and jogged dislocations in concentrations up to 10" per sq cm. A replica investigation of partially reversed Fe-Ni martensites5 corroborates the increase in dislocation density following reversal and presents indications of other possible modes of fine structure. This paper reports on an investigation performed to examine in detail the morphology and crystallography of the plates of reversed austenite and the shear which accompanies their formation in a matrix of Fe-Ni martensite. EXPERIMENTAL PROCEDURE Discs of a high-purity Fe-32.9 wt pct Ni single crystal served as the starting material. The single crystal had been produced in the course of an earlier investigation6 and the carbon content was determined at the time to be 0.006 wt pct. The M,, and the A,, were respectively -120" and 300°C. Partial transformation to martensite was performed at -125°C and reversal of some of the martensite was accomplished by heating in the temperature range 340" to 355°C. Most samples were heated to the reversal temperature by immersion' in a salt bath for 2 min. For surface-relief studies some polished and etched Samples were heated in a tube furnace for ten min in a hydrogen atmosphere maintained over the samples throughout the heating and cooling cycles. Samples were prepared for metallographic examination by electropolishing and etching with an HC1-HNOs-H20 et~hant.~ On one of the surface-relief samples two sets of fiducial scratches were placed on the etched sample by drawing it over a slurry of 0.06 p alumina on a "microclothJ'. The orientations of individual plates of martensite were determined by X-ray analysis. A Rigaku-Denki microbeam X-ray generator in conjunction with a Micro-Laue camera with facility for precision location of the sample in front of the beam was employed for this purpose. The collimator size was 30 p and the specimen to film distance was 5 mm. The Laue photograms were enlarged to an equivalent 3-cm specimen to film distance for analysis. The orientation of each of the plates of martensite was compared to that of the parent austenite and the relationship be -tween the two phases was, in all cases, within a few degrees of those predicted for the direct transformation. The orientation relationship between one of the larger plates of reversed austenite and its parent martensite was determined in a similar manner. The habit plane of the islands of reversed austenite in the X-rayed plates of martensite was determined by a single-surface trace analysis. Each reversal island had with the parent phase one comparatively straight boundary which was presumed to represent the habit plane trace. The pole locus technique7 was applied to traces from six different plates of martensite to determine the indices of the habit plane. A 40-cm stereographic net was employed for this analysis The morphology and fine structure of the reversed austenite were studied by electron microscopy of pre-shadowed direct carbon replicas,5 and the macroscopic shear was evaluated by a two-stage replica technique similar to that employed in electron fractog-

Jan 1, 1968

By Franklyn W. Oatman

In order that the conditions which obtain in an oil well may be readily understood, a brief description of a typical California well and a number of the phenomena accompanying same will be given. That the necessity for the exclusion of water be realized, the effects of water intrusion, a description of methods of prevention, .and a discussion of causes of failure will be presented, followed by a summary and recommendations. Fig. 1 shows a section of a typical well which illustrates the relation of oil sands to overlying strata. It indicates a deep water sand separated from the oil sand by shale, and the proper place for the final shutting off of water. In this well a comparatively thick stratum of compact shale protected the oil from overlying water so that the operation of landing the water string was a simple matter. In some wells the protecting stratum may be only from 3 to 5 ft. thick and very careful operation is necessary in order to land the water string of casing properly and not puncture through to the oil sand. The cases just cited are common, but occasionally, after excluding overlying water, productive oil sands are drilled through in the expectation of finding more productive underlying sand, and a water-bearing stratum is tapped. In this case the problem is the reverse of the normal; water must be prevented from ascending rather than descending. A discussion of well-drilling methods is not within the scope of this paper, except such operations as pertain to shutting off of water. A brief outline of the several conditions which may accompany drilling follows. Some or all may be present in any particular case. The direct relation of these to prevention of intrusion will be discussed in detail further on. In drilling, the hole becomes more or less irregular in shape, and rough, and as the casing follows the bit into the well it does not fit snugly against the walls. As a result, water may descend between the casing and walls of the well. If a circulation pump is not used during drilling, the hole is simply punched through and the pulverized material removed from the well by means of a bailer. If circulation is maintained there is a continual flow of water down inside the casing and up around the outside between the pipe and the walls of hole. This keeps an open space around the pipe.

Jan 1, 1915

By Michael Hoch, Seong Kwan Rhee

The ternary system Zr-Cr-0 was investigated at 1200°, 1500°, and 1700°C. The isotherms at these temperatures were determined by metallographic and X-ray diffraction analysis of carefully selected alloys. AS a part of a series of investigations1-4 of the ternary and quaternary phase diagrams on refractory metals and their compounds, the ternary system Zr-Cr-O was investigated at 1200°, 1500°, and 1'700°C. The binary diagrams Zr-Cr, Zr-O, and Cr-0 as reported by Hansen5 and Levin et a1.' and the existence of a ternary coompound ZrsCrsO (q-carbide structure a. = 11.96A) provided a good base for this investigation of the Zr-Cr-O phase diagram. MATERIALS The materials used and their suppliers were: Zirconium powder, 99.4 pct pure, Charles Hardy, New York; Zirconium dioxide, Fairmount Chemical Co., Newark, N.J.; Chromium powder, 99.85 pct pure, Fairmount Chemical Co., Newark, N.J.; Chromium sesquioxide, 99.86 pct pure, J. T. Baker Chemical Co., Pillipsburg, N.J. Though the materials used were not "hyperpure", the impurities present do not affect the results (lattice parameters, phase boundaries) within the experimental accuracy. EQUIPMENT AND PROCEDURE The detailed procedures and equipment used for this investigation were similar to those described elsewherel' "ith the exception that in this study an induction-heated argon-atmosphere furnace was used. The latter furnace was used to prevent the vaporization of chromium metal in samples in the higher temperature range (above 1200°C). The tungsten crucible was induct ion-heated in a vertical quartz tube filled with argon gas. The quartz tube was 1-1/2 in. in diameter and 10 in. long; it was connected at the top and bottom to water-cooled copper plates. The argon gas of a purity 99.995 pct was further purified by being passed through zirconium metal chips which were maintained at 800°C in a silica tube 1 in. in diameter and 30 in. in length. The furnace was flushed with argon gas for an hour before starting heating; during heating, a slight (3 cm oil) overpressure of argon was maintained in the system. Power was supplied by a 20-kw Ther-Monic Induction Generator. The samples rested on a tungsten-wire basket; the wire basket was connected to a tungsten wire which passed through the tungsten crucible lid, and entered the system on top through a Wilson-type seal. By pulling on the wire, the sample was removed from the crucible and dropped to the water-cooled copper base of the furnace. Because of the presence of argon gas, the cooling of the sample was even more rapid than in the vacuum furnace.' EXPERIMENTAL RESULTS AND DISCUSSION 1) Isothermal Section at 1200°C. The compositions investigated have been numbered within the phase diagram, Fig. 1, and all the pertinent information about the samples can be found in Table I. This table lists the composition of the samples, the phases present in the room-temperature diffraction patterns, the phases detectable in the microstruc-ture, and calculated lattice parameters of the a-zirconium phase. The shapes of the various phase

Jan 1, 1964

By L. J. Dijkstra, R. J. Sladek

IN earlier work the effect of manganese on the general behavior of nitrogen in iron was the subject of a careful examination by Fast.' Part of the investigation was made, in collaboration with one of the present authors (L.J.D.), by using the internal friction method. This technique, which has been described elsewhere,' showed some significant changes in the properties of Fe-N alloys by the addition of a small amount of manganese namely: 1—Under standard conditions the maximum of the nitrogen peak in pure iron appears around 20 °C and the half width is about 27 °C. By addition of 0.5 atomic pct Mn a general broadening of the internal friction peak occurs. The half width is increased by about 9°C. Moreover, a shift of the maximum of about 5°C toward a higher temperature takes place, Fig. 2. 2—The precipitation of nitrogen from the supersaturated solution, measured, e.g., at 200 °C, was inhibited by the addition of the amount of manganese given in effect 1. The broadening of the nitrogen peak was confirmed in more recent work3 on samples which were prepared from Westinghouse Puron iron. The effect of manganese on the rate of precipitation, however, was much less striking than in the earlier work' based on Philips high purity iron. Theory To explain the first change in properties just referred to, effect 1, the following two assumptions were made:' First, every manganese atom in sub-stitutional solid solution creates around it six interstices located between an iron and a manganese atom, as is evident from Fig. 1. These interstices, conveniently called Fe-Mn interstices, have for nitrogen a free energy level which is AG* lower than the normal Fe-Fe interstices between two iron atoms. For such low concentrations of manganese as 0.5 atomic pct, the possibility that two manganese atoms will be nearest neighbors can be disregarded. Second, it is assumed that in addition to the normal relaxation time TFe at least one new relaxation time, Mn, Fe, enters in the phenomena which is associated with the elementary diffusion jumps between a Fe-Mn interstice and an adjacent Fe-Fe interstice. Fig. 1 gives schematically the free energy for a nitrogen atom as a function of its position along the line ABC. A tentative analysis of the nitrogen peak in a 0.5 pct Fe-Mn alloy based on these assumptions has been made in Fig. 2. The dotted curve with a maximum at 22°C is caused by jumps between Fe-Fe interstices, the dotted curve with maximum at 32°C by jumps between an Fe-Mn and an Fe-Fe interstice. The two effects added together give the dash-dot internal friction curve for the alloy. In the following these two components will be referred to as the normal peak at 22°C and the abnormal one. (The small secondary peak at

Jan 1, 1954

By N. Mungan

Laboratory water floods were performed in oil-wet and waterwet alundum and Torpedo cores, displacing a refined oil with n-hexylamine or Triton X-100 solution. Also, some floods were performed in which a sucrose solution was displaced with n-butyl alcohol. The Purpose ot the tests was to see if the oil recotlery could be increased and to examine what role the inter-facial tension reduction and wettability change play in the recovery mechanism. it was found that the chromatographic transport of amine was influenced by core wettability. In oil-wet cores, the rate of advance of the amine band could be predicted from equilibrium chromato-graphy, while in water-wet cores the amine band moved faster than predicted, indicating a non-equilibrium process. By reducing the interfacial tension to 1.1 dyne/ cm, oil recovery was increased. More oil was recovered from Dri-filmed cores than from water-wet cores. Reversing the wettability of the porous media from oil-wet condition also resulted in some additional oil recovery. Neutral wettability floods did not increase oil recovery. INTRODUCTION Interfacial forces in petroleum reservoirs are responsible for retention of large quantities of residual oil. Increasing exploration costs have created an incentive to attempt recovery of this residual oil by new and novel processes. One novel process involves changing the interfacial forces by introducing a chemical into the reservoir during water flooding. Recently, several investigators have carried out laboratory displacement tests using amines. lt3.4 The amines adsorbed onto initially water-wet core surfaces, changing them to oil wet. Additional oil was recovered when the cores were flooded in a manner reversing the. wettability from oil-wet conditions. In all these studies, the wettability reversal was considered responsible for increased oil recoveries although it was noted that amines also reduced oil-water interfacial tension. In the present study, displacement experiments were performed in water-wet and Dri-filmed cores. The purpose was to separate the effects of lowering the interfacial tension from changing the wettability. LABORATORY STUDY All experimental data given in this paper have been obtained at a temperature of 70F + 1 and prevailing atmospheric pressure. FLUIDS AND MATERIALS The oil used in these experiments* was washed with H2S04 and passed through two 100-200 mesh silica-gel beds to remove unsaturates and surface active impurities. Normal hexylamine** of practical purity was used, and the alundum cores*** were composed of nearly pure A1203. Fused quartz (SiOi) and Lucalox (A12 )t plates were used in the contact angle measurements. DISPLACEMENT TESTS Displacement tests were performed in alundum and Torpedo cores. Before displacement runs, cores were acidized with 0.1 normal HCI, flushed with distilled water and fired at 1,200F to make them water wet. This procedure also reduced water sensitivity of the Torpedo cores. Oil-wet cores were prepared from water-wet cores by flowing several pore volumes of 1 per cent by weight Dri-film SC-87 solution in heptane through the cores, flushing the cores with nitrogen, evacuating, and finally heating the cores at 300F for 4 or 5 hours. Between floods, cores were cleaned by conventional procedures and treated again as above.

Jan 1, 1965

By C. Chu

A theoretical investigation has been made of the forward combustion process using a one-dimensional linear mathematical model, taking into consideration the effect of the vaporization-condensation which occurs on the leading edge of the heat wave. This work involves the solution of five coupled partial differential equations. Besides the vaporization-condensation phenomenon, these equations account for conduction, convection, combustion, heat loss, diffusion and bulk fluid flow. For the one-dimensional linear model studied, the vaporization-condensation phenomenon does not induce appreciable change in the temperature at the combustion front; and its primary effect is to create a steam plateau and to increase the length of the heated zone ahead of the combustion front. This effect becomes more pronounced at lower pressures, higher porosities or reduced gas saturations. The peak temperature and the temperature profile on the leading edge of the heat wave stabilize after a certain period. The length of the steam bank remains practically constant, although the length of the water bank increases as the heat wave advances. INTRODUCTION The existence of the vaporization-condensation phenomenon in the heat-wave process and the important role played by the phenomenon have been recognized by several investigators. Kuhn and Kochl stated that steam plateaus were frequently observed on the temperature records of their experiments. The steam plateaus were attributed primarily to the vaporization and subsequent condensation of the interstitial water existing in the oil sand. Szasz2 suggested that both lighter hydrocarbons and water are vaporized on the leading edge of the heat wave, carried forward in the gas stream, and then condensed to create banks of oil and water. Martin et al suggested that the vaporization-condensation phenomenon is one of the main mechanisms of the heat-wave process, along with thermal expansion and viscosity reduction. Wilson et al. reported the existence of a steam plateau several inches in length in their small-scale tube-run experiments. However, this important phenomenon has never been taken into consideration in the numerous theoretical analyses by various authors. 5 The purpose of this work was to study the thermal aspects of a linear heat wave, taking into consideration the vaporization-condensation on the leading edge of the wave, to determine the effect of this phenomenon on the temperature profile of the reservoir, and to investigate how this effect varies when other process variables are changed. THEORY We consider a reservoir of porous medium of cross-sectional area A, extending from x = 0 to x = L. This reservoir contains, aside from the solid matrix itself, a gas phase and a "combined liquid phase" which is a combination of two immiscible liquid phases — namely, an oil phase and a water phase. The oil present in the reservoir is assumed to consist of three fractions, a noncondensable gas, a nondistillable residuum, and a vaporizable oil fraction which may be present in both the gas phase and liquid phase. Before the heat-wave process begins, preheating has taken place and has imparted an initial temperature distribution T,(x) to the reservoir. At the start of the process, a stream of oxygen-bearing gas is introduced through the face at x = 0. This gas supports the combustion of the residual fuel and supplies the heat throughout the process. In order to develop a tractable system of equations, the model properties are postulated as follows: (1) the system is isotropic and homogeneous; (2) there is a uniform fuel content throughout the reservoir; (3) combustion takes place in a moving vertical planar region of infinitesimal thickness; (4) the temperatures of the fluids and the solid matrix are identical; (5) radiation is negligible; (6) the gas and liquid saturations are uniform throughout the reservoir and remain unchanged

Jan 1, 1965

By R. E. Zimmerman

ALTHOUGH flotation of coal is considered relatively new in the United States by coal-preparation engineers, actually it has been practiced to some extent for the past 30 years, It is practiced much more widely in Europe than in the United States. Commercial plants are operating in nearly all major coal-producing countries of the world. A froth flotation plant has been operating since 1930 at the Champion No, 1 preparation plant of the Pittsburgh Coal Co. Unfortunately the term flotation is widely used in the United States by coal-preparation engineers to designate dense medium processes of coal cleaning. As used here, flotation means those processes for cleaning fine sizes of coal in which the coal is collected in a froth or matte at or near the surface of a pulp. The refuse particles remain in the pulp. Two distinct types of flotation are practiced: froth flotation and agglomeration. FORMS OF FLOTATION The theory of the principles of flotation and of the physicochemical foundations surrounding this process has become a complex and scientific field and coal-preparation engineers contemplating use of flotation processes would do well to study the works of Gaudin, 2, 5 Taggart, 3 Zimmerman, 4 Wark, 6 Ralston, 7 Petersen. 8 Bulk Oil Flotation.-In this process the separation of mineral from gangue is accomplished by virtue of the fact that minerals of metallic lustre, as sulphides, or hydrocarbons, as coal and graphite, are wetted preferentially by oil in the presence of water and consequently pass into the interface between oil and water; while gangue or rock is wetted by water and remains in the medium. Beginning in 1860 with Haynes and later between 1897 and 1907, at least 25 patents were granted for bulk oil flotation. Large quantities of oil are required, generally 3 to 25 per cent by weight of feed, and recovery of such oil is a major problem. The Elmore process 3 (1901 and 1902) is an example of a bulk oil process, The Trent process (1902-25) has been used for the cleaning of coal on a commercial scale, According to E. W, Davidson 9 there were five such plants operating in the United States by 1925. They have since been abandoned.

Jan 1, 1950

By M. J. Pool, R. K. Saxer, J. R. Myers, D. S. Dickson

ThE equilibrium phase diagram of the Mo-Cr system, described by anssen,' indicates that chromium and molybdenum form a continuous series of solid solutions above 1673K. The liquidus and solidus have been reported to have a minimum at about 12 at. pct Mo and 2133°K by Bloom and Grant2 and by Putnam, Potter, and Grant.3 X-ray studies by Trzebiatowski and ploszek4 and Baen and Duwez' revealed no indication of solid solution decomposition after long anneals at 1473", 1273", 923", and 873°K. However, Bloom and rant' by means of cooling and heating curve analysis of alloys containing up to 45 at. pct Mo found thermal effects at temperatures approximately 100" * 30°K below the liquidus. The only previous thermodynamic study of the Cr-Mo alloy system was made by Laffitte and Kuba-schewski6 who used the Knudsen effusion method at 1471°K. These investigators reported the possibility of a miscibility gap because they observed positive deviations from ideality in their chemical activity

Jan 1, 1970

By P. A. Tucker, C. R. Hudgens, D. E. Etter, D. L. Roesch, D. B. Martin

The equilibrium phase diagram of the Pu-Cd system is presented based on data obtained by differential thermal analysis, metallography, and electron-microprobe X-ray analysis. Liquidus temperatures range from 320° to 934°C. The system contains one congruently melting compound, PuCd, (945°C), and three incongruently melting compounds, PuCd, (800°C), PuCd, (730°C), and PuCd11 (410°C). A liquid-miscibility gap extends from 2 to 60 at. pet Cd with the monotectic reaction isotherm at 910°C. INTEREST in the potential use of plutonium alloys as reactor-fuel materials has prompted investigation of the phase equilibria in plutonium binary systems. A cursory investigation of the phase equilibria in the Pu-Cd binary system was conducted by differential thermal analysis (DTA), metallography, and electron-microprobe X-ray analysis (EMX). Extensive solid solubility of cadmium in both e and 6 plutonium was predicted1 based on atomic radii and electronegativities. Liquid immiscibility between these two elements was also predicted based on Mott's extension of Hildebrand's method. In the only previous investigation of the Pu-Cd system,2 two intermetallic compounds, PuCd11 (incon-gruent melting point 406°C) and PuCd8, were identified. EXPERIMENTAL The plutonium metal used in this work had a total impurity content of 500 ppm; the major impurities were: carbon (215 pprn), silicon (75 ppm), iron (60 ppm), nickel (40 ppm), and aluminum (25 ppm). The cadmium was reagent grade with a purity of 99.99 pet. The DTA technique for the study of plutonium alloys was previously described in detail.3 The alloys to be studied were prepared in tantalum DTA specimen capsules which were sealed by inert-gas welding. The alloys were homogenized in the liquid state in these sealed capsules which prevented the loss of cadmium by vaporization. Only the thermal arrests in the DTA heating curves were used to define the transformation temperatures of the system since supercooling affected many of the results during cooling. After the alloys were analyzed by DTA, the same alloys were used for the metallographic studies. Metallographic examinations were conducted in the manner described for plutonium alloys., No reaction was detected between the alloys and the tantalum capsules. Alloys for EMX analysis were placed in metallographic mounts together with specimens of unalloyed plutonium and cadmium which served as standards. The samples were highly polished but unetched. No protective coatings were applied to the surfaces of these radioactive specimens. Such coatings are detrimental to the excitation conditions and have been found to be unnecessary for the control of radioactive contamination. RESULTS The results of the DTA studies are presented in Table I. The phase diagram, constructed from these data plus the metallographic and EMX results, is presented in Fig. 1. The congruently melting compound, PuCd2, was identified by the occurrence of a maximum melting point (945°C) at 33.3 at. pet Pu-66.7 at. pet Cd and by the presence of a single phase in this composition.

Jan 1, 1965

By R. F. Mehl, M. Gensamer

Although a large number of X-ray photograms of cold-rolled steel have been published, two circumstances have led to the experimental work reported in this paper. The first is that no complete study, making use of the pole-figure method of Weverl, has been made of cold-rolled low-carbon steel. Wever has published pole figures of mild steel subjected to plane parallel deformation1, 2 and undoubtedly he has applied the method to cold-rolled mild steel, but the authors have not found these data published. Kurdjumow and Sachs3 have applied the method to the study of rolling and recrystallization textures in electrolytic iron; their results will be referred to later. The reason for this dearth of papers using the pole-figure method is obvious; a greater number of photograms and more analytical work (although this work is quite simple and straightforward) are required to construct a pole figure than most investigators have felt worth while, despite the fact that no other method of which the authors are aware will satisfactorily depict the orientations of the crystallites in a polycrystalline aggregate. The second circumstance that led to the work reported in this paper was the appearance of a paper by Wayne A. Sisson4 on the same subject. In his valuable study of the factors influencing the development of preferred orientations in cold-rolled mild steel, Sisson made one observation that required confirmation; that is, that at some stage of the rolling process the type of preferred orientation changed from the type that gives a photogram characterized as a "six-point" X-ray pattern to that known as a "four-point" pattern. A similar observation had been made by Tam-mann and Heinzel5, who studied the orientations developed in the rolling of steel by the specular reflection of light from the etched surface of rolled samples. These workers also found that the type of preferred orientation changed during the rolling process. The authors had some difficulty in seeing how this behavior could be consistent with modern views on the genesis of preferred orientations, particularly with those of Wever2

Jan 1, 1936

By R. F. Mehl, M. Gensamer

Although a large number of X-ray photograms of cold-rolled steel have been published, two circumstances have led to the experimental work reported in this paper. The first is that no complete study, making use of the pole-figure method of Weverl, has been made of cold-rolled low-carbon steel. Wever has published pole figures of mild steel subjected to plane parallel deformation1, 2 and undoubtedly he has applied the method to cold-rolled mild steel, but the authors have not found these data published. Kurdjumow and Sachs3 have applied the method to the study of rolling and recrystallization textures in electrolytic iron; their results will be referred to later. The reason for this dearth of papers using the pole-figure method is obvious; a greater number of photograms and more analytical work (although this work is quite simple and straightforward) are required to construct a pole figure than most investigators have felt worth while, despite the fact that no other method of which the authors are aware will satisfactorily depict the orientations of the crystallites in a polycrystalline aggregate. The second circumstance that led to the work reported in this paper was the appearance of a paper by Wayne A. Sisson4 on the same subject. In his valuable study of the factors influencing the development of preferred orientations in cold-rolled mild steel, Sisson made one observation that required confirmation; that is, that at some stage of the rolling process the type of preferred orientation changed from the type that gives a photogram characterized as a "six-point" X-ray pattern to that known as a "four-point" pattern. A similar observation had been made by Tam-mann and Heinzel5, who studied the orientations developed in the rolling of steel by the specular reflection of light from the etched surface of rolled samples. These workers also found that the type of preferred orientation changed during the rolling process. The authors had some difficulty in seeing how this behavior could be consistent with modern views on the genesis of preferred orientations, particularly with those of Wever2

Jan 1, 1936

ANY discussion of State-supported schools of mining and metallurgy needs to be prefaced by a definition, since the first school to offer a mining curriculum, the Pennsylvania. Polytechnic College, was established by a grant from the State. But, so far as can be determined, it received no further State support. It would be tiresome to go into precise details, and it will be enough to stipulate that by State schools are meant those which derive their main financial support from regular appropriations made by a State legislature. The University of Michigan was the first of these to. offer a mineral industry curriculum; its story, as well as those of Wisconsin and Illinois, has been related in the preceding chapter.* Arranging the others in chronological order involves making a decision as to what weight to attach to plans for giving instruction, as contrasted with its effective initiation. This may appropriately be illustrated by the history of mineral industry education in California. CALIFORNIA Among those who came to California in 1849 and the following years were many New Englanders who had a keen interest in education. Some of them, mostly Congregationalists and Presbyterians, sought to establish a school of higher education around San Francisco Bay and eventually succeeded in opening the "Scientific and Classical School at Contra Costa" in Oakland, at Broadway and 5th St., on June 90, 1853. This prospered so well that it was chartered by the State as the College of California" on April, 13, 1855. Developing so rapidly that its quarters became. cramped, in 1864 it not only bought a tract of

Jan 1, 1941

By A. G. McGregor

DURING the past 5 years, five new copper-smelting plants have been built and put into operation in the State of Arizona. The monthly copper output from these plants averages from 5,000,000 to 18,000,000 lb. Previously, there never was as much activity in copper-smelting plant construction in the same length of time in all the rest of the world. Naturally, in this amount of work, some new problems were met and new features in plant design and. equipment developed. Some of these features are described in this paper. CONCENTRATE HAULING, UNLOADING AND SAMPLING SYSTEM (a) Concentrate Car The International Smelting Co. has provided at its plant at Miami specially designed cars for hauling the concentrates from the mills of the Inspiration Copper Co. and the Miami Copper Co.. The car has a bottom that is readily made tight to hold flotation concentrates and is quickly and cheaply unloaded. Figs. 1, 2 and 3 show views and details of the car. The main feature of this car is the slot in the bottom throughout its length, which is closed by means of short planks that overlap like ship-lap as shown by Fig. 1. At one end of the car an iron gate operated by a screw and hand wheel is provided, which clamps or presses the planks together, making the bottom tight. A removable tapered plug rests vertically over this gate when the loading of the concentrates at the mill commences.

Jan 8, 1916

By B. A. Joyce, R. W. Bicknell, R. J. Bennett, P. J. Etter

Epitaxial layers of silicon have been grown on single-crystal quartz and alumina by two types of chemical reaction the hydrogen reduction of trichlorosilane and b) the pyrolysis of silane. These reaction systems are described. The cqsfallography of the two systems, as determined by electron and X-ray diffraction, is discussed, and epitaxial mechanisms suggested. The electrical behavior is briefly considered, and the design and properties of field-evert devices fabricated in the epilaxial material are also discussed. RECENT work carried out in these laboratories" has shown that it is possible to obtain epitaxial deposits of silicon on single-crystal quartz and alumina. The purpose of this paper is to describe the method of preparation of these layers using both the hydrogen reduction of trichlorosilane and the pyroly-sis of silane, to compare the crystallographic behavior of films on the two substrates, and to present some initial results of the electrical behavior of silicon layers on alumina. The structural study has been carried out using electron and X-ray diffraction and electron microscopy. The electrical assessment has been made in terms of conductivity and mobility determinations by the van der pauw3 technique, and by measurements on metal-oxide-semiconductor assemblies. 1) FILM PREPARATION Both quartz and alumina substrates, approximately 1 sq cm in area and 0.4 mm thick. were prepared from slices cut parallel to within a few degrees of (11.0), (10.0), and (00.1), and polished mechanically down to about 0.3 p diamond grade. Chemical polishing of alumina slices, using phosphoric acid at elevated temperatures, has also been used; epitaxial silicon layers have been grown on these substrates, but the process is not entirely reliable, possibly because the large strain present in the Verneuil-grown alumina crystal affects the chemically prepared surface. The two reaction systems are fairly conventional and are described briefly below. a) Trichlorosilane-Hydrogen System. The apparatus is shown schematically in Fig. 1. The substrate was heated by induction, with a fused-quartz encapsulated graphite hemicylinder as susceptor. The procedure for carrying out a deposition was to heat the substrate to reaction temperature in a stream of

Jan 1, 1965

By Ursula E. Wolff

Il.lechanica1 twins have been observed in brigsten single crystals of a variety of axial orientations defornzed at room temperature in tension or bending. The twins formed near the final fracture and were up to 3 p thick. The twinning plane was always of the type (113). Twinning at room ternperature occurred only after considerable prior slip. Twins usually preceded fracture and nucleated cracks. The crack surfaces often alternated between a (001) plane and the twin interfaces. Secondary twins could also nucleate from cracks. In the absence of twinning tensile samples failed by shear; twinned samples failed by cleavage. On the assumption that observed sudden load drops in the stress-strain curves are associated with twinning, a critical resolved stress for twinning of 60, 000 to 65, 000 psi was calculated. MeCHANICAL twinning has been observed in iron and iron alloys at low temperature by a number of investigators.'-7 Similarly, for high-purity tungsten, twinning has been reported for deformation temperatures below 211°K.8-10 In W-Re and Mo-Re alloys, 20 pct Re was determined as the lower limit for twin formation at room temperature." Since the twins are generally very narrow, they are usually identified only by etching techniques. The expected (112) habit plane has always been confirmed by angular analysis of the surface traces. Recently, however, a complete identification by X-ray analysis has been performed on twins in a Mo-35 pct Re alloy.12 During an investigation of the deformation charac- teristics of tungsten single crystals, twins were revealed in tensile and bend samples deformed at room temperature. This paper deals with the conditions for such twinning and the relation of twinning to fracture. EXPERIMENTAL PROCEDURE Tungsten single crystals, 1/8 in. in diam, of a variety of axial orientations were grown from un-doped material by four-pass electron-beam zone melting. A representative analysis is given in the following table: From these crqstals, tensile samples with 1 in. gage lengths were made by surface grinding, leaving shoulders for gripping. The diameter after grinding was 0.082 in. The distorted surface layer was then removed by ele1:trolytic polishing which reduced the diameter of the gage length to 0.080 in. Tensile tests were carried out at room temperature in an Instron machine under two different sets of conditions: a) Rigid mounting; strain rate 0.02 in. per in. per min. b) Gimbal mounting; strain rate 0.002 in. per in. per min up to a total strain of approximately 0.2 pct, then 0.01 in. per in. per min to fracture. Stress axis and growth direction coincided in all samples and are subsequently called orientation.

Jan 1, 1962