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By C. W. Volek, G. Mandl

Steam-injection tests in the field have shoum that heat transport into the oil/water region, ahead of the steam zone, may have a significant effect on the production process. Earlier theoretical work on reservoir heating by hot-fluid injection can be used to describe the growth of the steam zone, but only if heat transport from steam zone into oil/water region is neglected. It therefore became necessary to re-examine and extend the earlier theory. It was found that this theory ceases to be consistent with the physical model of the process at a certain critical time, tc, which depends on reservoir thickness, temperature, and quality of the steam. The critical time marks an important change in the heat flow across the condensation frovt: the heat flow, which is purely conductive during 0 < t < tc&apos; becomes predominantly convective at t = tc. Accordingly, at t = tc, the equation which governs expansion of the steam zone changes. On the basis of the new equation, an approximate description for the steam-zone growth during t > tc is developed by making use of upper and lower bounds for the exact solution of the problem. The boundary conditions for heat and mass flow inside the oil/water region are established, and a simple method of detennining the saturation at the downstream side of the condensation front is presented. Experimental results show that the theory gives an accurate description of steam-zone expansion before the critical time. At times near critical time, and also after critical time, experimental data show theoretical steam-zone volumes to be high. Even so, the accuracy of the calculated steam-zone volumes is sufficient for practical purposes. THEORY OF STEAM-ZONE GROWTH INTRODUCTION The engineering evaluation of steam-drive processes is based mainly on a mathematical description of reservoir heating by hot fluid injection presented several years ago by Marx and Langenheim.l This theory can be used to determine the growth of the steam zone,2 provided the flow of heat from the steam zone into the liquid zone ahead of the condensation front (Fig. 1) is neglected. Since we must expect, however, that heat transport into and inside the liquid region (the region between condensation front and production wells) will affect both the water/oil flow and the growth of the steam zone, it is necessary to re-examine and to generalize the Marx and Langenheim theory as applied to steam drive, which will hereafter be termed the "old" theory. Observations made in several field tests emphasize the need to study the heat flow across the condensation front (CF). On several occasions it was discovered that heat was transported in the liquid zone far ahead of the advancing CF, resulting in an early breakthrough of warm water. This seems to occur most often when high injection pressures are applied, when "wet" kONINKLIJKE/SHELL EXPLORATIE EN PRODUKTIE LABORATORIUM RIJSWIJK, THE NETHERLANDS SHELL DEVELOPMENT CO. HOUSTON, TEX.

Jan 1, 1970

By R. J. Colony

MINING geology does not lend itself - very readily to a review embracing "improvements in methods," as perhaps do shop practices or laboratory procedures. The "methods" used in mining geology are simply the application of geology to mining; winning the ore, the handling of material, mechanical appliances, all belong strictly to mining proper, and have no place in a review of geology as applied to mining. A comprehensive review would necessarily cover a .very broad field, which could be subdivided into many -parts. Only a few of these can be discussed here. .Those that have been suggested to the chairman indude :

Jan 1, 1930

By F. G. Miller, T. D. Mueller, L. B. Davidson

A mathematical model of reservoir behavior during one cycle of the intermittent steam injection process is presented in this paper. A cycle of the process is considered to be composed of three stages: injection, condensation and production. The model concentrates on behavior during the production stage. The influence of several parameters on production improvement is described, using the results obtained with a numerical equivalent of the model. Reservoir system parameters considered are thickness, reservoir thermal conductivity, oil viscosity, solution gas-oil ratio and the change in oil effective permeability with temperature. Operating parameters investigated are heat injection rate, steam temperature and cumulative injection time. In the face of considerable uncertainty, the model appears to give a fair prediction of the behavior observed during an actual test. This makes the model a useful means of selecting projects. It is shown that the model may also be utilized to select an optimum set of operating conditions for a particular project. Results of this study show the extent to which production improvement depends on each of the parameters investigated and give an indication of the range of system conditions within which the process would be effective. INTRODUCTION In recent years the intermittent steam injection or steam soak process of oil recovery has become a popular method of improving recovery in reservoirs bearing high-viscosity hydrocarbons. Production improvement due to the process results from heating the reservoir near the wellbore. The process is applied on an individual well basis and is executed in a series of cycles, each consisting of three stages: injection, condensation (the soaking period) and production. During the injection stage, high-pressure steam is injected into the reservoir surrounding the well-bore. This study assumes that injection is carried out over the entire vertical section of the reservoir rock that can be exposed to fluid injection. The condition of steam entering the reservoir is considered to fall within the following limits: (1) steam pressures less than 1,000 psig, (2) steam temperatures between 300 and 700F and (3) steam quality less than 90 percent. The last restriction is due to equipment limitations. Normally, injection re maintained for less than 3 weeks. After termination of injection, the condensation stage begins. The well is shut in for several days, supposedly to make certain that the injected steam condenses. This condensation would insure the retention of injected heat. The production stage is initiated when the well is opened again. Reservoir response during this stage determines the effectiveness of the process (response is defined as the oil production rates, the water production rates and the wellbore temperatures observed during the entire production stage). The immediate response of the reservoir is sometimes quite good. Sets of case histories by Longl and by Owens and Suter2 give some typical figures for response. Duration of the production stage is equal to the time needed for the oil production rate to decline to some predetermined value. This usually requires 4 to 6 months. Termination of the production stage coincides with the start of the next cycle. The process is continued, cycle by cycle, until it becomes unprofitable to continue. One simple model2 and two more sophisticated models3,4 of the process have been presented. These are based on fundamentally different assumptions than those used in this investigation. Although the three models might be modified to fit the assumptions used in this study, it is felt that greater rigor would result by developing a

By Charles T. Holland

IN connection with the problems of bumps in coal mines, much has been written concerning the manner in which roof action and methods of mining enter [ ] into the pressure effects observed but little has been written upon the relationship between the physical properties of coal and associated rocks and the cause of bumps. The question of the strength of bituminous coal, of its elasticity, and the energy it can absorb and store has been neglected to a considerable extent in connection with this problem. STRENGTH OF COAL It is generally agreed that one of the necessary conditions for bumps is a strong [ ] coal.1 Therefore, since the strength of coal is an important factor, a study of this property should be made. Several investigators have conducted laboratory experiments upon the strength of coal, using small cubical or rectangular test pieces. An attempt will not be made to go into all of these investigations, but they are briefly summarized in Table I. Experiments of the U. S. Bureau of Mines8 and of Lawall and Holland (pp. 27 and 34 of ref. 9), however, indicate that regardless of whether the coal is a soft and weak semibituminous (Pocahontas No. 3) or a hard and strong bituminous (Stockton) coal, the maximum ultimate unit stress developed in laboratory tests is higher in small cubes than in larger cubes of the same coal.

Jan 1, 1942

By S. G. Cupschalk, F. A. Dahlman, J. J. Wert

Studies have been undertaken to determine the indicidual effects of particle size, degree of long-range ovder, antiphase domain size, and root mean square stran on the microhardness and yield strength of ordered alloys. Dnta have been analyzed for Cu3Pt initzally ordered to a value of 0.82 and after deformations of 1 and 6 pct. It was observed that deformation fleatly reduced the degree of long-range order. Furtherrnore, wztkin this range of relatively small deforntntlons, the average particle size changed very little while the antiphase domain size was greatly reduced. Smultaneosly, the mcrohardness changed by a factor of two durzng the deforrtation process. PREVIOUS studies have reported some of the effects of cold work on the broadening of X-ray diffraction peaks. These investigations were performed on powder and wire samples representing both ordered and disordered states; i.e., the specimens were initially studied in a severly cold-worked condition. By comparing the difference in line shape between the annealed and cold-worked peaks, fundamental information was obtained concerning particle size, strain distribution in different crystallographic directions, degree of long-range order, and change in antiphase domain size. Considerable theoretical work has been done concerning the analysis of diffraction data obtained from cold-worked metals. Stokes&apos; expressed the change in diffraction profiles in terms of Fourier coefficients. Much of the work in this area has been summarized by warren2 in an extensive review article concerning the analysis of plastic deformation by X-ray diffraction. Cohen and Bever3 applied these techniques in studying the effects of cold work on alloy systems exhibiting long-range order. They utilized the Fourier coefficients of fundamental peaks in conjunction with those of the superlattice peaks to determine the change in antiphase domain size. Little work of this nature has been reported for ordered systems that have undergone small degrees of plastic deformation. The purpose of this investiga-tion was to determine the effects of small deformations in such a material with respect to particle size, strain distribution in various crystallographic directions, antiphase domain size, degree of long-range order, and hardness. EXPERIMENTAL PROCEDURE CusPt was used for the initial investigation since the order-disorder transformation takes place with- out a change in crystal structure. The transformation is readily detectable via X-ray diffraction techniques due to the large difference in the scattering factors of copper and platinum. Additionally, the alloy is relatively low melting (approximately 1300°C) and is easily deformable in both the ordered and disordered states. 1) Specimen Preparation and Cold Working. A 100-g, 12-in. diam., cylindrical specimen of Cu3Pt was prepared by melting and casting 99.99 pct pure Cu and Pt i.n vacuo. Prior to any mechanical working, the material was homogenized in a vacuum for 60 hr at 100O0C, and surface defects were removed by machining to a depth of approximately 116 of an in. The material was then cold-rolled, with an intermediate anneal, into a strip approximately 12 in. wide by 14 in. thick. Straightening and flattening removed another 0.025 in. from the thickness. After a recrystallization treatment at 750°C for 30 min, the specimen was slow-cooled from 55OoC, at the rate of 6°C per hr, down to 150°C to induce superlattice formation. This treatment yielded an ASTM grain size of 7 and a degree of long-range order equal to 0.83 0.06. After obtaining X-ray and Knoop hardness data, the sample was cold-rolled approximately 0.75 pct in one pass through a hand-operated jewelers&apos; mill. X-ray and hardness data were again obtained and the specimen was reduced an additional 5.41 pct in a single pass through the mill. 2) X-Ray Measurements. The specimen was examined in the ordered condition and after the two degrees of cold working previously mentioned using a General Electric XRD-5 unit equipped with a spectrometer and scintillation counter. Using Mo-Ka radiation with a zirconium filter, six orders of the 100 reflection were obtained. It was anticipated that point counting would be necessary for an accurate determination of the low-intensity peaks and tails: however, it was demonstrated that, by using a scanning speed of 0.2 deg per min and the appropriate time constant, the recorded data were sufficiently accurate. Thus, for ease of experimental procedure, all peaks were recorded on chart paper. Specimen position in the holder was considered to be insignificant after making a series of measurements of the same peak area in different positions with respect to the beam. Since peak overlapping did occur at high values of 20, it was necessary to separate the peaks graphically prior to analyzing the data in order to minimize this source of error. The peak tails were also carefully drawn to obtain the best possible data. Fourier coefficients of the line profiles were calculated on an IBM 7072 computer, and graphical meth-ods2j3 were employed in analyzing the results. For this type of calculation, in which the line profile is represented by intensities taken at set intervals, the intervals selected must be sufficiently small to give an accurate representation of the line profile. It was decided that for 20 = 0.02 deg the line profiles were

Jan 1, 1967

By Robert Baschwitz, John Chipman

The distribution of silicon between liquid silver and Fe-Si-C alloys has been studied at 1420oand 1530°C. The data are consistent with earlier studies. New data of Hager on the liquidus lines of the system Ag-Si and the distribution data are used to obtain the activity coefficient of silicon in both liquid phases. Data on the heat of mixing in iron permit accurate extension to 1600°C. Equilibrium data involving SiO2 and silicon in liquid iron together with revised data on the free energy of SiO2 are used to fix the activity of silicon in the infinitely dilute solution. The binary system exhibits strong negative deviation from ideality. At infinite dilution ? Si at 1600" is 1.25 x 10&apos;3, and at concentrations up to NSi = 0.4 the slope d InySi/dNSi has a constant value of r; = 13. It is found that logysi in the ternary solutzon is approximately but not exactly the same function of Nsi + NC as of NSi in the binary. The results are consistent with currently available data on the free energy of Sic and its solubility in molten iron. LIQUID solutions of the system Fe-Si-C have acquired considerable importance as the laboratory prototypes of blast furnace hot metal. Equilibrium studies involving such solutions and slags approximating those of the blast furnace have yielded useful information concerning the thermodynamic properties of blast furnace slags. In studies of this kind great importance attaches to a knowledge of the thermodynamic activity of silicon in the solution as a function of temperature and composition. An attempt was made by Chipman, Fulton, Gokcen, and askey&apos; to evaluate all of the pertinent data on this system and to deduce the desired relation between activity, composition, and temperature. These authors published data on the solubility of graphite and Sic in molten Fe-C-Si solutions and on the distribution of silicon between liquid iron and liquid silver. They showed further how the activity of silicon in very dilute solutions in liquid iron could be calculated from equilibrium data involving the molten alloy and solid SiO,. These calculations rested on the published thermodynamic properties of SiO, in- cluding its heat of formation which at that time was recorded as -209.8 kcal. This value has been under suspicion for some time and has recently been replaced by the concordant results from two independent laboratories2,3 which place the heat of formation of a-quartz at -217.6 kcal. This revision necessitates a re-evaluation not only of the activity of SiO2 in slag but also of silicon in molten iron. It is the purpose of this paper, therefore, to recalculate the activity of silicon, and in furtherance of this objective to present new data on its distribution between liquid Fe-Si-C alloys and liquid silver. HEAT OF SOLUTION OF SILICON IN IRON In order to determine the effect of temperature upon the activity coefficient it is necessary to know the heat of solution of silicon in iron as a function of composition. This is found in the data of Korber and Oelsen4 shown in Fig. 1. The curve corresponds to the following equation, which is of a form suggested by Wagner:5 Here AH is the heat absorbed in kilocalories in forming one gram atom of molten alloy from its molten elements and the N&apos;s are atom fractions. The relative partial molal enthalpies of the components, each referred to its pureliquid state and defined as zFe = aFe - PFe and zsi = HSi — -psi, are shown graphically. At low concentrations zSi = -28.5 kcal, in agreement with Kijrber and Oelsen&apos;s computation. This is in good agreement with the value of -29.3 kcal obtained by Chipman and Grant6 using an entirely different method. ACTIVITY AT INFINITE DILUTION From the known free energy of SiO, it is possible to obtain the activity of silicon in dilute solution in liquid iron from equilibrium studies. The heat of formation of a-quartz is —217.6 kcal and the heat capacity and entropy data are given by Kelley and ~ing.&apos; The free energy of formation of ß-cristo-balite at temperatures above the melting point of silicon is expressed by the following equation: Si(Z) + O2(g) = SiO2 (crist); AF" =-226,500 + 47.50T [I] The value of the deoxidation product for silicon [%Si] x [%O]2 at 1600°C according to Gokcen and chipmans is 2.8 x 10"5, in agreement with results of Hilty and Crafts.9 More recent works of Matoba,

Jan 1, 1963

By C. F. Gates, H. J. Ramey

Recent literature shows that pronounced increases in oil recovery can result from the use of miscible systems in recovery operations. This literature also points out certain problems associated with maintaining miscibility, e.g., compositional changes resulting from alterations in pressure and temperature or from zone dilution. The purpose of the work described in this paper was to study miscible zones for possible use in waterflooding operations and examine the manner in which these zones break down. The fluid system selected for study was oil—terNary-butyl alcohol—water, which, because of its narrow range of miscibility, is ideally suited for investigation in short, linear systems. The laboratory-observed effects on oil recovery and zone stability of a number of variables are reported. Among the variables investigated were miscible zone size, viscosity ratio, length of travel, and interstitial water saturation. Results obtained with this system show that interstitial water adversely affects recoveries because of premature phase break. Salinity of the water further aggravates Ais situation. This effect, although pronounced for this system, would probably occur in any fluid system containing an alcohol. As expected, viscosity ratio has a decided influence on recovery efficiency and zone stability. The results also show that use of a suficieno zone size, even though the system has poor phase characteristics, yields higher oil recoveries than are obtained from straight water floods. Length-of-travel studies showed a square root relationship between zone growth and path length for favorable viscosity ratios. No such clear-cut dependence was observed under unfavorable viscosity conditions. INTRODUCTION As new oil reserves have become increasingly more difficult and expensive to find and develop, the oil industry has devoted more and more time and money to finding more efficient methods for exploiting known reserves. The increasing number of water floods is one manifestation of this attempt to improve oil recoveries from existing fields. Since considerable quantities of oil are by-passed by the waterflood process, it is only a partial answer to the problem. The search continues. Of late, several proposed processes have received the critical attention of investigators. Among them are gas drives, in situ thermal reactions and miscible displacements. The present paper is concerned with miscible displacements in conjunction with water floods. Recent literature1- reports that, under proper conditions, oil recoveries from LPG floods, propane sweeps, condensing gas drives, etc., approach 100 per cent of the oil in place in the region contacted by the flood. This literature also points out some of the problems associated with these processes, one of the main ones being the maintaining of miscibility. Compositional changes resulting from pressure and temperature variations or from zone dilution give rise to phase breaks and loss of miscibility, the conclusion being that, after loss of miscibility, much of the beneficial influence of the zone is lost.&apos; The results of the subject work show that, if sufficient zone material exists ahead of a phase interface, considerable improvement in oil recovery can be obtained. In order to increase our understanding of the behavior of miscible systems as they degenerate into immiscible processes, a laboratory system having rapid deterioration characteristics was needed. The fluid system oil—ter tiary-butyl alcohol (TBA)—water possesses these properties and was the system investigated. Although these fluids are different from those generally employed in miscible studies, an understanding of their behavior can be applied to other miscible slug processes. However, under conditions where mass transfer maintains a miscible system through multiple contacts, e.g., enriched gas drive or high pressure gas drive, the observed behavior of alcohol zones would not be applicable. The variables of interest were zone size, viscosity ratio, length of travel, initial water saturation, rate and core characteristics. Of these, only the effects of the following on zone breakdown and oil recovery are reported in detail: (1) zone size, (2) path length, and (3) initial water saturation. The effects of viscosity ratio and core characteristics are discussed in conjunction with other variables. Although initial water saturation is not envisioned as important to the phase behavior of hydrocarbon systems, e.g., LPG, it is important in alcohol systems. The properties of the fluids and cores used are given in Table 1. As previously stated, this fluid system was selected because of the limited range of miscibility

By Smith, George Otis

THE matter that I have on my mind this evening is engineering&apos;s need of an open forum. Our fathers of three centuries ago were pro-testanta for freedom of speech and thought in matters religious; later, our fathers were revolutionists for freedom of speech in matters political; until today freedom of speech has become so universal throughout the land that even in the sanctuary of our homes, at times, we have to turn off the loud-speaker. Talk is not always a condition of progress, but light is everywhere necessary to growth, whether the growing thing is a blade of grass, a baby chick, or a young idea, and we must regret anything that tends to shut out the light from the operations of business and industry. Of course, I realize there is little that is novel in what I am saying. Indeed, I have found that Dr. James Douglas-a name we love to honor in our Institute-as long ago as 1907, gave an address at the Toronto meeting that any of us would be proud to be author of twenty-one years after. Dr. Douglas at that time spoke on secrecy in the arts and the text then taken by this leader in metallurgical technique and in the constructive management of big business was "the dangerous temptation to adopt secretive methods by very large corporations." In both thought and language Dr. Douglas was direct and vigorous and he needs no internreter. He advocated the wide open door for ideas on two counts: advancement of technical knowledge and education of public opinion. A few sentences will serve not only to prove the vision of James Douglas, but also, I hope, tempt you to hunt up his address in the Institute&apos;s TRANSACTIONS, and thus get his whole thought first hand.

Jan 1, 1928

By Laurance S. Reid, Joe A. Porter

Gas dehydration plays an important part in the production of natural gas. Effective dehydration prevents formation of gas hydrates and the accumulation of water in transmission Systems,2,6,7 insuring uninterrupted gas deliveries at maximum efficiency under the most adverse weather conditions. At the present time, most gas companies require a maximum water vapor content of seven lb per million standard cu ft of gas. so that virtually all gas tendered for sale must he dehydrated to meet this specification. For a number of years it has been common practice to produce gas and gather it at a common point for dehydration prior to discharge into the transmission system.1,3,11,16,17 However, higher transmission line pressures, long gathering lines and relatively low ground temperatures have made it necessary to dehydrate gas at. or near. individual. wells in order to gather gas from a number of newly developed fields without unusual difficulty. Where gas has been dehydrated at pressures ranging from 300 to 800 psi in the past. future trends indicate that these processes may be operated at pressures as high as 2,000 psi. Economics of gas dehydration are of great importance, partitularly where facilities must he provided to process relatively small quantities of gas, such as the production from an individual well. Although the adsorption of water vapor from gas on a granular sorbent material such as activated bauxite, activated alumina, or one of the alumina-silica gels is highly effective and produces virtually "bone dry" gas, the cost of a small unit of this type is substantially greater than that of an absorption process which, through proper selection of the absorbing liquid, will dehydrate the gas sufficiently to meet pipe line specifications. For this reason, a great deal of emphacis has been placed on the development of small, inexpensive dehydration units8,24 and the search for more effective absorb. ent liquids has been intensified. A wide variety of methods for dehydrating gas are known&apos; and many of these have been used in industry. Earlier applications of the absorption process employed concentrated solutions of calcium and lithium chlorides as the absorbent. The severe corrosion problems inherent in handling these solutions and the relatively small dew point depressions obtained caused early abandonment in favor of, or conversion to. diethylene glycol when it was found that aqueous solutions of this organic liquid were more hygroscopic than the brines and were non-corrosive. Processes employing diethylene glycol-water solutions are widely used for gas dehydration at pressures ranging as high as 1,200 psi.13,14,15 At nominal pressures a dew point depression of 45° to 50°F may be be and the data of Russell et al." indicate that a minimum dew point is obtained from the effluent gas at a pressure of approximately 1,200 psi when the gas is in equilibrium contact with a 95 per cent by weight diethylene glycol solution. In a number of instances the dew point depression obtained with diethylene glycol-water solutions is not sufficient to produce a specification product without cooling the inlet gas. In a recent search for a better absorhent, triethylene glycol was used in a small commercial dehydration unit and subjected to rather exhaustive field tests.&apos; The data obtained were encouraging and indicated that, at pressures ranging from 300 to 500 psi, triethylene glycol porduced a substantially greater dew point depression than diethylene glycol. These results led to an investigation of the system natural gas-water-triethylene glycol in an effort to obtain vapor-liquid equilibrium data, to determine pressure limitations, and to develop other data pertinent to the design of gas dehydration processes. A review of the literature has failed to reveal any data which permit reasonably accurate calculation of the vapor-liquid equilibrium conditions for a solution of water and triethylene glycol in contact with natural gas at high pressure. Since these constituents form a non-ideal system, the Poynting equation18,21 or the usual combination of Raoult&apos;s and Dalton&apos;s laws19,20,22 would not be valid. Correction of Raoult&apos;s and Dalton&apos;s laws by the use of activity coefficients2&apos; is not feasible for available data are insufficient for the prediction of the actual increase in the ratio of the activity of one component in the vapor phase to its activity in the liquid. Therefore. experi-

Jan 1, 1950

By R. N. Orava, L. A. Rice

One of the difficulties encountered in the preparation of titanium specimens for transmission electron microscopy is the formation of a surface hydride phase during the thinning operation at ambient temperatures. This necessarily destroys contrast, obscures features of interest, and often leads to misleading results. By cooling the polishing solution to temperatures below 0°C this problem has been overcome in the past.&apos; However, since the cooling procedure is somewhat inconvenient, a technique was developed at this laboratory for thinning titanium at room temperature. The material examined was A-70 grade commercial-purity titanium purchased from the Crucible Steel Co. of America. The mechanical and thermal treatments, described elsewhere,* yielded a recrystallized grain size of 4 to 5 p. A slice, 0.5 mm thick and 1.5 mm wide, was cut from a bulk specimen2 using a diamond cut-off wheel. The sample was then coated with paraffin wax. Two concentric holes, about 0.03 in. in diam, one at each broad face, were scribed through the wax to the surface of the metal. Subsequent polishing for several minutes resulted in a preferentially thinned or "dimpled" region. Thereafter, the wax was removed and the entire specimen polished to the point of breakthrough at the base of the dimple. Polishing was effected chemically in a solution comprised of 30 pct HF and 70 pct HN03 by volume, kept at room temperature (20" to 25OC). The specimens were mounted in a stereo holder and examined at 100 kv in a Philips l00 B Electron Microscope. A micrograph from a foil prepared in this way is shown in Fig. 1. Several points are noteworthy. This electron micrograph shows neither evidence for the formation of a hydride phase due to specimen preparation nor, moreover, any obvious surface contamination in electron-transparent areas of a freshly prepared foil. Localized variations in foil thickness observed in some specimens seem to be a characteristic of this chemical polish but do not seriously detract from foil quality. With care, the lifetime of a good specimen exceeded 2 hr in the beam. On the other hand, the exposure of a sample to air at atmospheric pressure, when still warm from the beam, clearly resulted in the deterioration of a formerly clean area just previously in the field of view. An example in Fig. 2 of a contaminated region reveals features, and "spots", not unlike those observed in much purer material by Yamane and Ueda. Consequently, one can conclude that: 1) titanium can be thinned satisfactorily in a solution at room temperature for transmission electron microscopy; 2) large-scale precipitates, >50A in diam, are absent in commercial-purity, recrystallized, furnace-cooled, A-70 titanium containing about 3800 wt ppm interstitials and the same amount of iron; 3) care must be taken not to attribute surface contaminants to precipitates. The authors are grateful to the Franklin Institute for financial support and permission to publish.

Jan 1, 1967

By K. V. Hoover, D. M. Lapham

In Pennsylvania, 310 sampled sites of clay and shale have been studied with regard to potential use, lithology, physical properties, fired properties, major-element chemical analyses, and quantitative five-component X-ray mineralogy. Approximately 80% of the samples are of some potential use. Binary correlations of test data vs. potential use indicate that certain empirically determined parameters may be critical. These are: lithology, particularly for medium to superduty refractories and lightweight aggregate; kaolinite content for refractories vs. low-temperature fired product sources; quartz analyses with an apparent necessary minimum quantity for brick; quartz content, which is low in high grades of lightweight aggregate; mica content, which is low for refractories and possibly high for lightweight aggregate; total iron, which is low for refractories and shows a 4.0% minimum for lightweight aggregate; carbon dioxide, which is low for refractories, beneficial in lightweight aggregate, and probably restrictive for some tiles; chlorite-vermicalite, which is low for refractories and possibly beneficial in lightweight aggregate. In Pennsylvania, clay and shale materials constitute one of the state&apos;s major economic mineral resources. To date, the testing program indicates considerable development potential in brick, tile, and lightweight aggregate industries and perhaps a future potential for aluminum from shales that exceed 20% AID..

Jan 1, 1972

By A. W. Schlechten, R. P. Abendroth

Jan 1, 1960

By Alfred H. Hesse, Edwin T. Myskowski

The development by the U. S. Bureau of Mines of a process for purifying manganese by electrolysis has stimulated interest in manganese alloys. While recent publications have shown some alloys of manganese and copper to possess rather unusual properties, none have included information on tensile properties, which have an important bearing on the usefulness of the alloys. Manganese-copper alloys can be heat-treated, since the single phases that exist at high temperatures may be retained by quenching. According to Persson,1 when quenched alloys containing from about 30 to nearly IOO per cent manganese are reheated, alpha manganese is precipitated (Fig. I). Calculations based on Persson&apos;s X-ray data indicate that this decomposi-tion is accompanied by a change in volume of as much as ; per cent. The reason that this large volume change has not been noted probably is the slow rate at which equilibrium is reached by these alloys. In an investigation on hardening by cold-work and heat-treatment, Dean and Anderson3 found that quenched alloys increase in hardness with manganese content and that high-manganese alloys harden very slowly with cold-work, while high-copper alloys harden much more rapidly. Heat-treatment has little effect on manganese-copper alloys containing less than 40 per cent Mn, and affects those alloys containing more than 40 per cent in accordance with their manganese content and heat-treating temperature. Dean and Anderson4 also found that cold-work increased electrical resistance of alloys containing from 50 to 80 per cent Mn, and that heat-treatment of alloys containing from 40 to 96 per cent Mn altered the electrical resistance considerably. Dean, Anderson and Potter6 have shown that the high vibration damping capacity that characterizes manganese-copper alloys containing 40 to go per cent Mn is affected by cold-work and heat-treatments. Highest vibration damping capacity at low stresses was obtained by heating for 2 hr. at 450°C. (842°F.) after quenching from solution temperatures. Preparalion of Alloys.—The alloys for these tests were melted in a 17-lb. basic-lined high-frequency induction furnace using electrolytic manganese, grade A ingot copper and a 70-30 CU-Mn master alloy (69.80 per cent Cu, 0.12 Fe, 0.04 Si, 0.006 S, 0.07 C, balance Mn). The manganese was heated slowly to expel excess dissolved gases and melted before the addition of copper. No fluxes or covers were used. The melts were cast in tapered iron molds and the ingots were reduced go per cent when forged to 1/2-in. rounds. These rods were given 2-hr. solution treatments at temperatures that depended upon the composition (Table I). Tensile Tests.—The tensile specimens, 0.313-in. diameter (1.25-in. gauge length),

Jan 1, 1942

By Edwin T. Myskowski, Alfred H. Hesse

The development by the U. S. Bureau of Mines of a process for purifying manganese by electrolysis has stimulated interest in manganese alloys. While recent publications have shown some alloys of manganese and copper to possess rather unusual properties, none have included information on tensile properties, which have an important bearing on the usefulness of the alloys. Manganese-copper alloys can be heat-treated, since the single phases that exist at high temperatures may be retained by quenching. According to Persson,1 when quenched alloys containing from about 30 to nearly IOO per cent manganese are reheated, alpha manganese is precipitated (Fig. I). Calculations based on Persson&apos;s X-ray data indicate that this decomposi-tion is accompanied by a change in volume of as much as ; per cent. The reason that this large volume change has not been noted probably is the slow rate at which equilibrium is reached by these alloys. In an investigation on hardening by cold-work and heat-treatment, Dean and Anderson3 found that quenched alloys increase in hardness with manganese content and that high-manganese alloys harden very slowly with cold-work, while high-copper alloys harden much more rapidly. Heat-treatment has little effect on manganese-copper alloys containing less than 40 per cent Mn, and affects those alloys containing more than 40 per cent in accordance with their manganese content and heat-treating temperature. Dean and Anderson4 also found that cold-work increased electrical resistance of alloys containing from 50 to 80 per cent Mn, and that heat-treatment of alloys containing from 40 to 96 per cent Mn altered the electrical resistance considerably. Dean, Anderson and Potter6 have shown that the high vibration damping capacity that characterizes manganese-copper alloys containing 40 to go per cent Mn is affected by cold-work and heat-treatments. Highest vibration damping capacity at low stresses was obtained by heating for 2 hr. at 450°C. (842°F.) after quenching from solution temperatures. Preparalion of Alloys.—The alloys for these tests were melted in a 17-lb. basic-lined high-frequency induction furnace using electrolytic manganese, grade A ingot copper and a 70-30 CU-Mn master alloy (69.80 per cent Cu, 0.12 Fe, 0.04 Si, 0.006 S, 0.07 C, balance Mn). The manganese was heated slowly to expel excess dissolved gases and melted before the addition of copper. No fluxes or covers were used. The melts were cast in tapered iron molds and the ingots were reduced go per cent when forged to 1/2-in. rounds. These rods were given 2-hr. solution treatments at temperatures that depended upon the composition (Table I). Tensile Tests.—The tensile specimens, 0.313-in. diameter (1.25-in. gauge length),

Jan 1, 1942

By Edwin T. Myskowski, Alfred H. Hesse

THE development by the U. S. Bureau of Mines of a process for purifying manganese by electrolysis has stimulated interest in manganese alloys. While recent publications have shown some alloys of manganese and copper to possess rather unusual properties, none have included information on tensile properties, which have an important bearing on the usefulness of the alloys. Manganese-copper alloys can be heat-treated, since the single phases that exist at high temperatures may be retained by quenching. According to Persson,1 when quenched alloys containing from about 30 to nearly 100 per cent manganese are reheated, alpha manganese is precipitated (Fig. I). Calculations based on Persson&apos;s X-ray data indicate that this decomposition is accompanied by a change in volume of as much as 5 per cent. The reason that this large volume change has not been noted probably is the slow rate at which equilibrium is reached by these alloys. In an investigation on hardening by cold-work and heat-treatment, Dean and Anderson&apos; found that quenched alloys increase in hardness with manganese content and that high-manganese alloys harden very slowly with cold-work, while high-copper alloys harden much more rapidly. Heat-treatment has little effect on manganese-copper alloys containing less than 40 per cent Mn, and affects those alloys containing more than 40 per cent in accordance with their manganese content and heat-treating temperature. Dean and Anderson4 also found that cold-work increased electrical resistance of alloys containing from 50 to 80 per cent Mn, and that heat-treatment of alloys containing from 40 to 96 per cent Mn altered the electrical resistance considerably. Dean, Anderson and Potter5 have shown that the high vibration damping capacity that characterizes manganese-copper alloys containing 40 to 90 per cent Mn is affected by cold-work and heat-treatments. Highest vibration damping capacity at low stresses was obtained by heating for 2 hr. at 450°C. (842°F.) after quenching from solution temperatures. Preparation of Alloys.-The alloys for these tests were melted in a 17-lb. basic-lined high-frequency induction furnace using electrolytic manganese, grade A ingot copper and a 70-30 Cu-Mn master alloy (69.80 per cent Cu, 0.12 Fe, 0.04 Si, 0.006 S, 0.07 C, balance Mn). The manganese was heated slowly to expel excess dissolved gases and melted before the addition of copper. No fluxes or covers were used. The melts were cast in tapered iron molds and the ingots were reduced 90 per cent when forged to ½ -in. rounds. These rods were given 2-hr. solution treatments at temperatures that depended upon the composition (Table I). Tensile Tests.-The tensile specimens, 0.313-in. diameter (1.25-in. gauge length), which were enclosed in evacuated Pyrex

Jan 1, 1942

By Edwin T. Myskowski, Alfred H. Hesse

THE development by the U. S. Bureau of Mines of a process for purifying manganese by electrolysis has stimulated interest in manganese alloys. While recent publications have shown some alloys of manganese and copper to possess rather unusual properties, none have included information on tensile properties, which have an important bearing on the usefulness of the alloys. Manganese-copper alloys can be heat-treated, since the single phases that exist at high temperatures may be retained by quenching. According to Persson,1 when quenched alloys containing from about 30 to nearly i00 per cent manganese are reheated, alpha manganese is precipitated (Fig. I). Calculations based on Persson&apos;s X-ray data indicate that this decomposi¬tion is accompanied by a change in volume of as much as S per cent. The reason that this large volume change has not been noted probably is the slow rate at which equilibrium is reached by these alloys. In an investigation on hardening by cold-work and heat-treatment, Dean and Anderson3 found that quenched alloys increase in hardness with manganese content and that high-manganese alloys harden very slowly with cold-work, while high-copper alloys harden much more rapidly. Heat-treatment has little effect on manganese-copper alloys containing less than 40 per cent Mn, and affects those alloys containing more than 40 per cent in accordance with their manganese content and heat-treating temperature. Dean and Anderson4 also found that cold-work increased electrical resistance of alloys containing from 50 to 80 per cent Mn, and that heat-treatment of alloys containing from 40 to 96 per cent Mn altered the electrical resistance considerably. Dean, Anderson and Potters have shown that the high vibration damping capacity that characterizes manganese-copper alloys containing 40 to g0 per cent Mn. is affected by cold-work and heat-treatments. Highest vibration damping capacity at low stresses was obtained by heating for 2 hr. at 450°C. (842°F.) after quenching from solution temperatures. Preparation of Alloys.-The alloys for these tests were melted in a 17-lb. basic-lined high-frequency induction furnace using electrolytic manganese, grade A ingot copper and a 70-30 Cu-Mn master alloy (69.80 per cent Cu, 0.12 Fe, 0.04 Si, 0.006 S, 0.07 C, balance Mn). The manganese was heated slowly to expel excess dissolved gases and melted before the addition of copper. No fluxes or covers were used. The melts were cast in tapered iron molds and the ingots were reduced go per cent when forged to ½ in. rounds. These rods were given 2-hr. solution treatments at temperatures that depended upon the composition (Table I). Tensile Tests.-The tensile specimens, 0.313-in. diameter (1.25-in. gauge length), which were enclosed in evacuated Pyrex

Jan 1, 1942

By H. T. Clark

Within the last twenty years at least three sets of lattice constants for the room temperature (alpha, hexagonal close packed) phase of titanium have been reported in the literature. These values, summarized in Table 1, differ one from another by amounts far greater than can be explained on the basis of inaccuracies in parameter measurements. This paper presents new values determined for high purity titanium. It also details the effect of two elements, oxygen and nitrogen, on these parameters and shows that two of the previously reported values are probably in error because of the presence of one or both of these elements in the material used for examination. Preparation of Samples The titanium+ used for this study was prepared by the thermal decomposition of titanium tetraiodide7 on a hot titanium filament. This titanium rod was prepared for X ray examination by melting about 10 g in purified argon in an electric arc furnace on a cold hearth. This cast button was cold rolled to 0.040 in. thick sheet, cleaned, annealed in vacuum at 1000°C and cold rolled to 0.020 in. thickness. About 0.003 in. of surface material was then removed by hand grinding on papers to remove any contamination caused by the rolls and the sample was bent to the radius of the focusing camera. The sample was then vacuum annealed at 600°C, a temperature just high enough to cause recrystallization, producing a fine grained structure. Such a structure is essential in sheet specimens prepared for focusing cameras in order to have a sufficient quantity of grains to develop continuous diffraction lines. The use of sheet specimens rather than powder samples appears to be essential for the X ray examination of titanium. This is because of titanium&apos;s exceptionally high gettering power and its rapid absorption of adsorbed gases, water -vapor, and the like at annealing temperatures. While the effect of this contamination may be neglected for sheet specimens, its effect on 200-300 mesh powder is appreciable. Titanium alloys of oxygen and nitrogen were prepared by a technique simi- lar to that described above except that the required amount of the highest purity titanium oxide or nitride available was added prior to melting in the arc furnace. These materials were added by placing them in holes drilled in the titanium. A small weight loss invariably occurs during the melting of these oxygen and nitrogen alloys. This is believed to be due entirely to the loss of some of the powdered compound in the blast of the electric arc, an assumption which is justified on the basis that there is no weight loss during the melting of titanium metal and that wet analyses for nitrogen on representative samples have checked with the calculated analyses when it was assumed that the entire loss during melting was due to the loss of titanium nitride powder. These alloy buttons were reduced to sheet in the same manner as used for the unalloyed titanium. Experimental Procedure A North American Phillips 12 cm diam symmetrical precision focusing vacuum camera and copper radiation

Jan 1, 1950

By T. C. King

AT the new Graham-Central Mill of Eagle-Picher, near Galena, Ill., material is simultaneously dewatered and introduced into the ball-mill scoop boxes by the use of variable-speed, 24-in. spiral classifiers. This arrangement has proved satisfactory in that the moisture content of the wet feed is reduced, thus allowing maintenance of density within the mills, and a constant feed at any desired rate to the mills is provided. In this mill the primary feed is wet crushed to minus ½ in. and preconcentrated by jigs to produce a bulk lead-zinc-iron concentrate and a waste tailing. The jig concentrate is then dewatered by a conventional dewatering classifier and stored in, bins ahead of the ball mills. Even though this material is well dewatered, the discharge at the bin bottom is sloppy because of the gradual drainage of the water from the surface of the particles. Conventional belt feeders with vertical cutoff gates are unsatisfactory because of the flushing characteristic of the wet sand.

Jan 1, 1950

By J. A. Berge, R. S. Mateer, R. G. Aspden

IN a study of the cold-rolling characteristics of iron-base alloys with 3 to 12 pct Al, the influence of aluminum content on the cold-rolling textures was evaluated. This work was undertaken to determine if binary iron-aluminum alloys possessed cold-rolling textures similar to other body-centered-cubic alloys and to contribute additional information on the effect of solute concentration on the cold- rolling textures. Gradual changes in cold-rolling textures with an increase in solute content have been observed in copper1 and in titanium.2 Iron-base alloys containing 3.0, &apos;6.0, and 12.0 pct aluminum were vacuum-induction-melted in a magnesia crucible and permanent-mold cast. The materials used were high-purity electrolytic iron and 99.99 pct grade aluminum. Each ingot was 1 in. square in cross section by 12 in. in height. The bottom half of each ingot was soaked for 1 hr at 1000°C and rolled at 1000°C to a thickness of 0.055 in. with the long axis of the ingot parallel to the rolling direction. The strip was reheated between passes to maintain a rolling temperature of 1000°C.

Jan 1, 1960

By Irwin H. Cornell

BRIEFLY stated, the history of the St. Joseph Lead Co. is the story of how a group of men, working for ten years as officers without salaries and stockholders without dividends, developed a small mine in Missouri into what became a large and prosperous corporation. Their courage and faith in the scattered surface deposits of lead coupled with the management&apos;s engineering vision and sound financial judgment should prove an inspiration to present-day mining operators and investors. In 1717, John Law&apos;s company, known as "The Company of the West," was formed in France and letters patent were granted, for a period of 25 years by Louis XV, for exploration in the Mississippi River Valley. One of the underlying purposes of the expedition, headed by Mr. Renault and Mr. La Motte, a French metallurgist, was development of the lead mines in the area now known as Southeast Missouri.

Jan 1, 1947