Search Documents

By Paul Beck

WHILE the recrystallization properties of most of the practically important metals are known in considerable detail, those of lead are still relatively little known in spite of some valuable contributions in recent years. This condition probably is due to the difficulties involved in applying the usual methods of investigation. The microscopic method of discriminating between the elongated deformed grains of the familiar lenticular shape and the equiaxed recrys-tallized grains is not successful with fully refined lead: lenticular grains cannot be seen under the microscope with any amount of deformation whatever. The probable cause of this phenomenon was recognized long ago. With large deformation the time of recrystallization at room tem-perature is shorter than the period of preparation of the specimen for microscopic examination; with small deformation the deformed grains are not noticeably elongated in the first place. However, with small deformation the migration of the grain boundaries can be observed. The only systematic investigations yet published on the recrystallization of lead, those by R. S. Russell,1-3 make use of the conditions just described. Russell considered recrystallization completed when no further migration of boundaries could be observed. A serious objection to this method arises from the fact that there is no evidence to support the view that grain-boundary migration results only from recrystallization. If such migration does result from other sources after recrystallization is com-pleted-after the deformed grains have been replaced by new unde-formed grains-the "time of recrystallization" as determined by Russell may be too long. Furthermore, the method is subject to the above-mentioned limitation because of the unavoidable period of preparation of the sample. According to Russell, even with the fastest technique 5 min. elapsed before the deformed samples were ready for examination, and consequently no recrystallization time shorter than 5 min. could be measured.

Jan 1, 1939

By L. O. Howard

The practice of using acid-lined converters at the plant of the Old Dominion, Copper Mining & Smelting Co. was discontinued early in January, 1913, and replaced by basic-lined converters. The new equipment consists of one electrically operated 12-ft. upright converter stand and two basic-lined shells for same. These shells are provided with twenty-four 1 1/4-in. tuyeres. The mouths are 5 ft. in diameter. Owing to the fact that there is no bedding system or other large storage capacity between the mine and the smelter, the furnaces must handle as fast as produced ore and concentrates, which may vary considerably from day to day, both in tonnage and copper content. Consequently the converter is often crowded to its utmost capacity by the frequent fluctuations in the daily matte supply. From the foregoing, it will be seen that in no way can the 'converter be favored by running light charges or by transferring to it from other stands in operation. Neither can it regularly be allowed to cool between blows, and only occasionally can it be run at as low a temperature as might be wished. No copper precipitate or other foreign material high in copper is available to help out the tonnage. Repairs and alterations or the removal of defective tuyeres must wait until such time as a slight falling off in.the matte supply allows the converting operations to ease up. These variable conditions all combine to interfere with the systematic operating of the converter. The first 12-ft. shell was blown in on Jan. 6, 1913, and ran until June 27, 1913, when it was removed to patch the brick. A record of operations covering this period follows: Shell No. 1. First Campaign, Jan. 6,to June 27, 1913 Commenced blowing............................Jan. 6, 1913. Taken off stand for patching.....................June 27, 1913. Total blowing time..........................2,689 hr. 40 min. Total number of, blows made.............................. 664 Average time of blow............................ 4 hr. 3 min. Tons matte charged.................................. 18,157 Average copper content of matte................ 43.9 per cent. Average time blowing one ton. copper................ 22.5 min. Total copper made............................... 7,250 tons

Jan 1, 1915

Jan 1, 1924

Under the joint auspices of the Illuminating Engineering Society and the University of Pennsylvania there will be given about 20 lectures covering the general principles of illumination and the aspects of lighting practice. They will be held at the University of Pennsylvania in Philadelphia, from Sept. 21 to 28, 1916, inclusive. The subject of illumination of mines will be included in this series, which will be delivered by men selected on account of their qualifications to deal authoritatively with the several phases of the subject. In connection with the lectures there will be an exhibition of the latest developments in illuminating appliances, including lamps, accessories, photometers, together with novel applications of light. There will also be an inspection tour which will include visits to manufacturing establishments, laboratories, lighting companies and notable lighting installations. For further particulars apply to the Illuminating Engineering Society, 29 West 39th Street, New York City.

Jan 6, 1916

By NORMA D. MACFADDEN

WHILE the library work of the Woman's Auxiliary to the A. I. M. E. was founded three years after the formation of the Auxiliary, its present policy of establishing permanent libraries in mining camps throughout the United States dates only from 1924. Since then sixteen libraries have been established and thousands of books have found their way to homes of far-away miners, bringing pleasure and knowledge to a multitude of Americans and future citizens. Library work was initiated under the presidency of Mrs. H. W. Hardinge in 1922 and firmly established with her aid as one of the main activities of the Auxiliary. The first chairman served but a short time and Mrs. A. O. Ihlseng then took over the work of chairman of the Library Committee. To place the surplus books of Auxiliary members and their friends in use in mining camps was the immediate work of the committee. This was accomplished by placing a traveling library in the Bureau of Mines' cars and also by sending books for distribution to section chair- men in our larger mining camps.

Jan 1, 1929

By ROBERT. RICHARDS

I. INTRODUCTION The object of this paper is to enlarge the field of settling velocities treated by me in my former papers, Close Sizing Before Jigging, and Sorting Before Sizing.' There seemed need of work both on coarser and on finer sizes. Messrs. A. Sidney Warren and M. L. Nagel undertook the investigation for the coarser sizes, from 12.85 mm. down to 2.05 mm. diameter. Their work, because of the closer spacing and because of the increased number of observations and consequent stronger averages, called for a revision of the former work. Messrs. G., A. Barnaby and Ralph Hayden undertook this part of the work, from 2.49 mm. down to 0.28 mm., which is near the limit of sifting. Their work covers the ground much more minutely and comprehensively than the former papers. There remained to be covered the portion of the field too fine for investigation with the sieves. This part, covering the range of grains from 0.48 to 0.03 mm., was undertaken by Mr. E. S. Bardwell. For it he used the elutriation method. II. THE FIRST, OR COARSEST, SECTION OF THE FIELD. The first desideratum in this investigation was a series of sieves for sizing the sands preparatory to making the tests. It became necessary, therefore, to decide on a sieve-scale for this purpose. A sieve-scale is a series of sieves in which the dimensions of the holes of the successive members form a series increasing by a. definite ratio. There are three natural sieve-scales : 1, progressing by doubling the width of the hole for each suc-

May 1, 1907

By H. H. Podgurski, J. C. M. Li, Y. T. Chou, F. N. Davis, R. A. Oriani

When an Fe-2 pct A1 alloy is nitrogemted at 500ºC with a gus tnixture (NH3-H2) in which the nitrogen activity has been kept Lou] enough to avoid the formation of iron nitride, a two-phase alloy is generuled which consists of AlN particles and a ferrite phase cotaining a heavy network of dislocations. The amount of nitrogen contained in such an alloy, when equilibrated with the nitrogenating atmosphere, far exceeds both that needed to satisfy the normal solution requirements of a Fe and that needed to convert all of the aluninuwi to AlN. This excess nitrogen is accounted for as being trapped on dislocations, adsorbed at the ferrite -AlN interface, and as an en-Iuznced lattice solubility in strained ferrite. This excessive uptake of nitrogen had previously been attribuled by other investigators to the formation of a nonstoichiornetric aluminum nitride. Isotope exchange experiments revealed various amomts of exchargeable N14 present in the originally nitrided samples that could not be removed by reduction with HS at 500ºC. This exchangeable nitrogen has been identified us that bound to the AlN -ferrite interface. Estimates of inter facial areas in alloys containing -3 pct by weight of A1N are as high as 10 sq m per g of alloy. ThE first1 of this series of papers described the experiments forming the basis for the elucidation of the mechanism of the formation of aluminum nitride particles within an Fe-A1 alloy. It was found that not only are dislocations necessary for the nucleation of the AlN particles but also the nitriding reaction in turn produces a dense network of dislocations in the ferrite matrix. It was also observed that nitrogen in excess of that needed for the formation of stoichiometric AIN is taken up by the alloy without the formation of an iron nitride. The present paper is an analysis of the excess nitrogen sorbed by the nitrided Fe-A1 alloy which considers the structure generated by the formation of the aluminum nitride particles. Because of the high density of dislocations, this system has proved to be quite useful in studying nitrogen-dislocation interactions. Wriedt and Darken2 have already reported such studies in a cold-worked ferritic steel. EXPERIMENTAL Nitrogen Sorption. The specimens of this alloy were cold worked (50 pct reduction) to 0.011 in. thickness and chemically cleaned in a 2:1 concentrated phosphoric acid-50 pct hydrogen peroxide solution before nitrogenation. The flowing nitrogenating atmosphere (11 pct NH3-89 pct H2) was established before the ni- trogenating temperature was reached. The same gravimetric and gas-flow equipment described in an earlier paper1 was also used in this investigation. Changes in nitrogen concentration were followed gravimetrically when establishing the isotherms. In the isotope exchange experiments, concentration changes were followed volumetrically. In some instances chemical analyses (Kjeldahl method) were used to check for material balances in both the gravimetric and volumetric procedures. Our objective was to obtain reversible nitrogen sorption isotherms for alloys equilibrated with NH3-H2 gas mixtures over a large range of nitrogen activity* and temperature. The *Defined as equal to PN H /P3/2 ,where P corresponds to partial pressure in atmospheres. Actually the nitrogen activity, aN, in the alloy equals K PNH3 /p3/2H2, where K is the equilibrium constant for the reaction NH3 = N + 3/2H2. upper limit for nitrogen activity was below that which would produce iron nitride; for reasons which will become apparent later, most of the sorption studies were made in the temperature range between 400" and 500'C. The alloy sample studied most extensively in this investigation was given a series of successive reductions (100 pct H2) and nitrogenating treatments at 500°C to attain a stabilized structure. Presumably some dislocations were lost during these treatments. Throughout most of the sorption studies, temperature was held at ± 1°C and the gas-phase composition was held to k0.2 pet NH3. Based upon the results of numerous diffusion experiments with this alloy* the 'Results to be published in a third paper of this series. times chosen for equilibration were considered more than adequate, Nitrogen Isotope Exchange. The first exchange experiments were carried out by circulating a measured quantity of H2 and NH3* (with a predetermined isotopic *The NH3 was synthesized over a synthetic ammonia iron catalyst using H2, and N2, enriched with N15. AS the NH3 was formed it was removed continuously from the gas phase by circulating the mixture through a refrigerated (78ºK) trap. When most of the nitrogen had been converted to NH3, it was distilled from the trap into a glass storage vessel. composition, N15/N14) over a nitrided specimen at 450°C in a closed glass system. Attempts to reach the exchange limit isothermally, i.e., an isotopic ratio (N15/N14) in the gas phase identical with the extractable nitrogen in the nitrided alloy, were futile. The exchange rate between the gas phase and the alloy was too slow, involving many days. To circumvent the slow exchange with the gas phase, measured amounts of N15 and N14 were introduced into the alloy by nitrogenating with an NH3-H2, mixture at 500°C containing an N15/N14 ratio of 7.76; the charged specimens were then sealed by allowing an oxide film to form over them in air, and in this final condition the specimens were subjected to 500°C in vacuum for various times during which isotope exchange was allowed to proceed within the specimen. It was estab-

Jan 1, 1970

By B. L. Averbach

Recovery and primary recrystalliza-tion in cold worked metals are usually considered as two competing processes. Some of the effects which usually accompany recovery are: alleviation of stress corrosion tendencies, changes in thermal emf,1 damping capacity,2 electrical resistivity,2 and magnetic properties,3 and only minor changes in hardness or the related strength properties. During primary recrystalliza-tion new unstrained grains are formed at the expense of the strained matrix. These new grains eventually become visible metallographically, and nucle-ation and growth kinetics have been indicated for this process.4,5 Frequent attempts have been made to study the cold-working phenomenon by observations on the line broadening by X ray diffraction patterns. Relatively few measurements of line intensities have been made, although Brind-ley and his collaborators, 6,7,8 by means of film techniques, compared the intensities of cold worked Cu, Ni, and Rh patterns with those from chemically precipitated powders. These precipitated powders were presumed to be strain free, and it was found that the intensities for the cold-worked materials progressively decreased as the Bragg angle increased except for the first line, where there was an increase due to reduction in extinction. This was interpreted as a randomness in atomic position induced by cold work. Such randomness is similar to that caused by thermal agitation and has been described as "frozen heat" displacement of 0.08-0.10 A from the mean atomic position. In a recent study9 on the effect of cold work in metals on their powder pattern intensities, the changes in integrated intensity for heavily cold worked alpha brass were observed as a function of the annealing temperature. These measurements were made with a manually operated Geiger-counter spectrometer using CuKa radiation monochromated with a rock salt crystal. Intensity measurements were made with a scaling meter over small intervals of angle, and the equipment was so arranged that the diffracted and incident beams made equal angles with the specimen. Intensities could be compared directly by simply interchanging specimens, and comparisons from day to day were made with a standard whose line intensities did not change on aging. It was shown that a cold worked alpha brass standard was stable for at least a year. Table 1 indicates the results of the integrated intensity measurements on a 70 Cu-30 Zn brass. In the sample preparation, a brass plate was first cold rolled 50 pct and then filed, screened to —325 mesh, compacted into briquettes at a pressure of 60,000 psi and finally annealed for one hour at various temperatures up to 400°C. The briquetting pressure did not seem to influence the integrated intensities, and most of the cold work was introduced by the filing. Although this method of cold work is not quantitative, it was used to obtain random orientation (and thus uniform diffraction lines) in order to make accurate measurements of integrated intensity. Back reflection patterns were taken in each case to check the uniformity of the lines, and from the observed line broadening it was apparent that this type of plastic deformation was quite severe. Care was taken to traverse the entire background of the pattern and to assign to each peak the total intensity above this background. The bases of the diffraction lines were quite broad and spread out over several degrees, even for the narrow peaks. The theoretical intensities were calculated to include a temperature correction, a dispersion correction, and a Lorenz- polarization factor corrected for the crystal monochromated beam. In Table 1 it was necessary to match the calculated and observed values at only one point, and the rest of the experimental values were converted directly to this arbitrary scale. The integrated intensities in Table 1 are listed in arbitrary units, and the accuracy was sufficient to reproduce any of the measured line intensities to within + 1.5 units. It is evident that the percentage error on the strongest line (111) was quite low. The calculated values and the observed intensities for the cold worked material matched reasonably well. As the annealing temperature was raised, however, the intensity of the strongest reflections, particularly the (lll), decreased measurably. Since the background intensities of all of these patterns were identical, such behavior could be interpreted as a primary

Jan 1, 1950

By Ralph Hultgren, Prodyot Roy

Manganese vapor pressures from 1250° to 1500°K were measured by conventional Knudsen and torsion-effusion methods in twelve Fe-Mn alloys with compositions from 9 to 80 at. pct Mn. The Knudsen re-sults agveed approximately with previous measurements found in the literature which indicated the solutions were nearly ideal. However, except for the higher manganese compositions, the initial torsion readings indicated much (up to 50 pct) higher vapor presszcres than the Knudsen method. These high readings decreased steadily with time. The results are interpreted as due to depletion of surface concentration of manganese during evaporation. Thus the initial torsion readings are the most nearly correct and Knudsen methods on alloys are to be regarded with suspicion unless it can be demonstrated that diffusion rates are rapid enough to replenish surface concentrations depleted by evaporation. For the lowest manganese contents and highest temperatures, depletion causes initial torsion readings to be too low. FEW thermodynamic data are available for alloys of the high-melting transition metals due primarily to experimental difficulties at the high temperatures involved. Measurement of vapor pressure is one of the most promising techniques to be applied to this problem. From the vapor pressure of a component of an alloy phase, its activity or its partial molar Gibbs energy can be directly calculated. From measurements over a sufficient range of temperatures and compositions the partial and integral Gibbs energies, enthalpies, and entropies may be determined through Gibbs-Duhem integration. For solid phases of variable composition, which commonly are found in alloys, measured vapor pressures are low because of depletion of the surface concentration of the more volatile component as it is selectively vaporized. Diffusion from the interior tends to restore the depleted concentration. The seriousness of the effect depends on the relative rates of diffusion and vaporization. Although depletion has been recognized as a factor,' direct measurements of its rate are lacking and quantitative estimates of its effect on measurements are uncertain. In the present work the vapor pressures above a series of Fe-Mn alloys have been measured by the torsion-effusion method. This method permits a measurement of the vapor pressure of manganese as soon as the sample comes to temperature and continuously throughout the run. The rate of decline of the apparent vapor pressure measures the rate of depletion and the torsion reading at zero time should be correct. At high manganese concentrations (70 and 80 at. pct Mn), the torsion reading remained nearly constant; surface depletion was negligible. There was a slow drop in measured pressure due to bulk loss of manganese from the sample. However, for lower manganese contents, especially at high temperatures, the depletion effect was considerable and the apparent vapor pressure decreased steadily with time. For these alloys the Knudsen method should give pressures which are too low. The measurement of pressure in the Knudsen method cannot be made until enough manganese has been vaporized to be weighable. The Knudsen result is therefore an integrated average between the initial and final vapor pressures. To verify this, conventional Knudsen measurements were also made with results in approximate agreement with previously published Knudsen measurements for these alloys. As expected, for the lower manganese contents the initial torsion readings of pressure were as much as 50 pct higher than the Knudsen. THE APPARATUS The apparatus, shown in Fig. 1, is capable of operating to temperatures up to 2000°K. A vacuum of 5 x 10"6 mm Hg can be maintained. Temperatures were measured to +3° by a W-Re thermocouple placed in the dummy cell, N. The torsion cell consisted of two alumina crucibles with holes in their covers. They were placed in the molybdenum holder shown suspended from the torsion wire. Rectangular torsion wires (1 by 4 mm) were found to have superior sensitivity and less residual distortion than circular (2-mm-diameter) wires. The precision of angular measurement was found to be *0.025 deg; the variation is no doubt due to temperature fluctuation and vibration. For the Knudsen experiments the alumina cell was set on the support, N. SAMPLE PREPARATION 800-g samples were prepared by melting together electrolytic iron and electrolytic manganese and pouring the melt into a water-cooled copper mold. Melting and pouring were done under a helium at-

Jan 1, 1965

By ALBERT C. RUBEL

RECENT developments in the use of the core barrel in rotary drilling have led to its wide application in all types of development. Its use is essential to the wild-catter and a valuable guide and check even in the most closely developed areas. A perfect core would be an unbroken sample of formation whose length is equal to the amount of hole made by the core barrel, whose diameter is great enough to show the lithologic character, texture and attitude of the material encountered, whose formation is so unaltered in character and so free of contamination from outside sources that it represents a true and complete sample of the formation penetrated. From such a core it would be possible to determine the lithologic character and economic importance of the formation, whether it is oil bearing or barren, the nature and attitude of the sands and shale bodies, valuable fossil evidence and other points which would assist in the correlation or in the selection of suitable points for water shut off or production.

Jan 1, 1924

By William H. Spice

Exploratory drilling in South Central Texas for the year 1944 showed a marked increase over that of 1943 and resulted in a similar increase in new fields discovered. In this area, which comprises the 30 counties included in district No. I, Oil and Gas Division, Railroad Commission of Texas,? 61 exploratory wells were drilled during 1944 as compared with 29 exploratory wells drilled during 1943, or an increase of over 100 per cent. Three new oil fields, two new gas fields and one gas-distillate field were discovered during the year, as compared with one new oil field and one new gas field discovered during 1943. These new fields were the result of exploratory drilling throughout the district along the Wilcox trend and the deeper Edwards lime trend, which was started during the previous year. The Wilcox trend yielded the new Loma iilta-Wilcox oil field and the San Caja gas-* tlistillate field, both in McMullen County. The Charlotte field, in Atascosa County, was discovered along the deeper Edwards lime trend. These three discoveries were of considerable importance and subsequent development should indicate the desirability of continued exploration along these trends. The other three discoveries, United oil field in Guadalupe County, Pederson gas field in Milam County and Van Cleve gas field in Zavalla County, were of minor importance. Charlotte Field, Atascosa County, was discovered by the Humble Oil and Refining Company's No. 3 Pruitt, completcd on Aug. 9, 1944, flowing 176 bbl. per day, 3/16-in. choke, 710 lb. tubing, 475 lb. casing pressures, 37.7º A.P.I. gravity, from the top of the Edwards lime from 6917 to 6923 ft. Two oil wells were completed during the year in this field. This discovery is 14 miles southwest of the same company's Imogene field, also producing from the Edwards lime but with considerable difference in reservoir characteristics. The discovery of this field is the result of surface geology and subsequent seismograph survey of the area. Loma Alta-Wilcox Field, McMullen County, was discovered by the Atlantic Refining Company's No. I Atkinson, completed on June I, 1944, flowing 102 bbl. per day, 9/64-in. choke, 1900 lb. tubing pressure, 37º A.P.I. gravity, from Wilcox sand from 6866 to 6869 ft. after being drilled to a total depth of 7185 ft. This discovery is the result of subsurface geology and an extensive seismograph survey of the entire area. Sun Caja Field, McMullen County, was discovered by Edwin M. Jones No. 2-C Ezzell, completed on June 2, 1944 as a dual completion in the Wilcox sands, flowing 1,740,000 cu. ft. gas with 53 bbl. distillate, 1/4-in. choke, 2035 lb. tubing pressure, 53.2º A.P.I. gravity, from sand 6416 to 6453 ft. and flowing 2,000,000 cu. ft. of gas with 127 bbl. distillate, 1/4-in. choke, 2500 lb. tubing pressure, 50º A.P.I. gravity, from sand 6889 to 6916 ft., after being drilled to a total depth of 7264 ft. Three gas-distillate wells were completed during

Jan 1, 1945

By AIME AIME

I am happy to welcome you to the twenty-third conference of the National Open-Hearth Committee, and our joint conference with the Blast Furnace Committee, of the American Institute of Mining and Metallurgical Engineers. It is appropriate that, for our fifteenth year anniversary, we should meet in the hotel and the city where this Open-Hearth Committee was inaugurated in 1925. At that first meeting, only a handful of men from a number of steel companies met to discuss ways and means to start a movement to improve the practical and metallurgical technique of open-hearth operations among independent manufacturers, as the United States Steel Corporation had carried on for many years.

Jan 1, 1940

By Attilio Ligasacchi

The production of magnetite in copper smelting has been the subject of wide investigation in the past.1-9 It is accepted that most of the magnetite is produced in the converters and returned to the re-verberatory furnace with the converter slag. Part of this magnetite is circulated back to the converters in the matte. As a result, if proper fluxing practice is not followed, and temperatures in the converting process are not strictly controlled, an undesirable circulating load of magnetite may occur. This might ultimately lead to saturation in the reverberatory bath with consequent settling of the magnetite at the furnace bottom. This paper contains the cumulative results of a series of investigations on the formation and control of magnetite presently being conducted by the metallurgical department of the Chino Mines Division of Kennecott Copper Corp. THE METHOD USED FOR THE DETERMINATION OF MAGNETITE AND OTHER MAGNETIC MATERIALS Conventional wet chemical magnetite analyses are neither reproducible nor theoretically sound. These analyses are sensitive to time, temperature, and heating rate-all factors which tend to decrease their accuracy and reproducibility. To overcome the unreliability of the above method, H. W. Mossman1 developed an inductance bridge magnetite "meter" which completely replaces the wet chemical analysis with the advantage of quicker and reproducible results. Fig. 1 is a schematic diagram of the meter in use in the Chino metallurgical laboratory. When a pulverized specimen with magnetic properties is placed in coil A of the inductance bridge circuit, the permeability of the core is increased, causing a voltage drop across the coil. The unbalance is amplified to operate the balancing motor which adjusts the movable iron core in coils C and D to bring the bridge back to balance. An indicator arm connected to the movable iron core indicates directly the percent, or weight, of the magnetic material in the specimen. Coil B acts as a reference coil and a zero adjustment. The meter is standardized with a set of various amounts of -100 mesh pure magnetite crystals (99.8 pet Fe3O4) thoroughly mixed in a test tube with -100 mesh quartz sand. These mixtures are combined with inert transoptic powder and heated to 140° to 160°C (melting point of the powder) and subsequently cooled to room temperature, solidifying the whole mixture, in this manner eliminating any possible preferential orientation of the magnetite grains. In order to determine the effect of the particle size" of the magnetite and other magnetic materials on the meter determinations, five size fractions were obtained by wet screening of the 99.8 pet pure magnetite and several reverberatory matte and slag samples. The following size fractions were investigated: -80 + 100; -100 + 150; -150 + 180; -200 + 250; -250 + 300 and -100 mesh. The deviation of the meter readings for the various sizes of each sample never exceeded ±0.3 pet. This deviation is considered well within the accuracy needed for common smelter operation procedures. Further investigation proved also that grinding slag and matte samples in our laboratory disc grinder normally produced a powder constituted of 95 pet -200 + 300 mesh. For practical purposes a - 100 mesh size was used as standard for our studies. It was also found that for rapid determinations tamping of the sample in the test tube was sufficient and gave comparable results with those samples solidified with transoptic powder. For the purpose of this study we define the magnetite content in copper smelter slags and matte as the equilibrium amount of crystalline Fe3O4 existent in the specimen at a given reference temperature, excluding any secondary magnetite precipitated in the specimen during nonequilibrium conditions. MAGNETITE DETERMINATION IN SLAGS Since it is impossible to ascertain the status of equilibrium of a conventional slag sample, due to

Jan 1, 1965

By Forrest F. Craig

Both early and more recent1 laboratory measurements of gas-oil relative permeabilities were made by subjecting oil-saturated cores to external gas drives. In these runs it was generally assumed that the flowing gas/oil ratio was constant at every point throughout the core. Using this assumption, the resulting equation for the gas-oil relative permeability ratio becomes A where Q is the flow rate at the producing end of the system. This relative permeability was then specified for the average saturation of the core. The assumption and resulting equation fail to recognize that in an external drive, the oil flow rate varies from zero at the injection end to a maximum at the producing end. The assumption also fails to consider the existence of a saturation gradient during an external drive. This saturation gradient is due solely to non-steady-state flow. Some authors2,3,4 have used this erroneous method of calculating relative permeability ratios from external drives. Other authors5,6,7 have used relative permeability ratios in calculating expected field performance by external drive, using Equation (1) and making the incorrect assumption that the saturation is uniform within the driven portion of the reservoir. To find the correct relation between the relative permeability. ratio at the average saturation and the produced gas/oil ratio, the insertion in Equation (1) of a factor, F, to adjust it for oil velocity gradient has been considered. The equation then takes the form Assuming that the oil velocity is directly proportional to the distance from the injection point leads to the conclusion that, for a linear system, the average oil velocity is one-half that at the producing end. Thus, the average gas/oil ratio is twice the produced gas/oil ratio, and Equation (2) is transformed into However, here again the existence of a saturation gradient is not recognized. The produced gas/oil ratio is related to the relative permeability ratio at the saturation of the outlet end of the system. It can be shown quite readily that, if the true log k,/k, saturation relationship is linear over small ranges of saturation, then d log kjko Where aaxv and u2 are the average and outlet saturations, respectively. Examination of Equation (3) shows that the factor F cannot have a single value over the whole saturation range. Another method of dealing with external drives is that of Buckley and Leverett.' Their method, which assumes no gas expansion and outlet end effects, considers fully the saturation gradient present due solely to the displacement mechanism during an external drive, and applies Equation (1) to each point along this gradient. The calculation of production history using relative permeability ratio is straightforward. However, the calculation of relative permeability ratios from production history by this method is impractical. In a recent paper, Welge,1 using an approach similar to that of Buckley and Leverett, presents a simplified method for determining the saturation at the producing end of the system. At thi; saturation, the relative permeability ratio calculated by Equation (1) applies exactly, after breakthrough of the stabilizej front. By this method, relative permeability ratios or production history may be calculated with equal ease. Use of this method as a laboratory tool in determination of relative permeability ratios by external drive requires the knowledge of the total injected fluid volume; in addition to the average saturation and producing ratio. As a preliminary test of this method of calculation, laborntory external gas drives were run on a 3% in. diameter, 11 in. long sample of Nellie Bly consolidated sandstone. This core sample had a permeability of 824 md and a porosity of 28.1 per cent. The driving fluid was air. Three different oils were used, having viscosities of 1.4, 9.8, and 125 cp, respectively. The runs were made under identical pressure differentials,

Jan 1, 1952

By G. K. Burgess

(New York Meeting, October, 1913.) 1. COOLING AND HEATING CURVES BY G. V. BURGESS AND J. J. CROWE. § 22. THE results published in Professor Howe's paper 10 of our determinations on the Ac3 and Ar3 points for a series of commercial carbon steels 11 containing manganese in varying proportion, represent the average temperatures found by taking several (4 or 5) heating and cooling curves. The accompanying curves, Figs. 6 and 7, are, for each steel, the first heating and cooling curves as obtained by' the inverse-rate method of Osmond, using a cylindrical chronograph sensitive to -0.1 sec. for recording .time. Simultaneous observations were also taken by the differential method with a platinum neutral and plotted by Rosenhain's derived differential method and gave substantially the same results, the curves having sensibly the same contours in both cases.12. The observations were taken in vacuo on cylinders 5/8 by 1 in. in length bored to center with a 1/8-in. hole to receive porcelain insulated thereto-couple, and inclosed in an out- and in-glazed Berlin porcelain tube heated electrically by, platinum foil wound on the tube. The vacuum was usually better than 0.1 mm. The heating and cooling of the furnace was automatically controlled by a salt-water rheostat with shaped electrodes, giving a uniform rate of heating and cooling.

Jan 6, 1913

[†AARONSON, ALFRED E., Vice-Pres., Mid-Co. Petroleum Co., Mid-Co. Bldg., Tulsa Okla. '18 ABADIE, EMILE R., Min. Engr Box 927, Porterville, Cal. '76 ¦ABADILLA, QUIRICO A. Student, Colorado School Of Mines, Golden, Colo. '20 ABBOTT, CLARENCE E., Gen'l Supt. Iron Mines Div., Tenn. Coal, Iron & R. I. Co., 1405 Minnesota Ave., Bessemer, Ala. '04] [ ]

Jan 1, 1925

By J. W. Spretnak, V. Kandarpa

Stress -induced ordering of carbon atoms is studied in a series of Fe-Mn-C alloys. A prominent peak is found in the vicinity of 280°C at frequencies of the order of 1.0 cps, with an associated activation energy of 37 kcal per mole. The height of the peak is linearly rekzted to the concentration of carbon in solution. The distortion of octahedral holes by manganese atoms appears to be predominant over carbon-carbon pair interactions. RELAXATION by stress-induced ordering of point defects is expected whenever the introduction of these point defects produces distortions which have a lower symmetry than that of the lattice. Under zero stress, the isolated point defects occupy the crystallographic-ally equivalent positions in the lattice, as these represent states of equal energy. However, if the defect sites are asymmetric, application of an uniaxial stress will split the energy states, and a redistribution of the defects among various states will take place. This is the case of the internal friction peak called the Snoek peak,1 resulting from isolated interstitials in bcc metals. The interstitial sites in this case have tetragonal symmetry. In the case of fcc and hcp lattices, such an effect is not expected from isolated point defects because of the symmetrical nature of the interstitial sites. However, internal friction peaks arising from interstitial diffusion have been reported both in hcp2,3 and fcc4-8 lattices. These peaks are often explained on the basis of stress-induced ordering of interstitial solutes, caused by the deviation of interstitial sites from their cubic symmetry through the presence of nearby defects. In the case of fcc lattices, evidence for interactions of both the substitutional-interstitial4,6,13 and interstitial-interstitial types5'798'14 have been presented by various investigators. The purpose of the present investigation was to study the internal friction peak attributed to the diffusion of interstitial carbon atoms in high purity austenitic manganese steels and to account for the peak in the light of the existing models. MATERIALS The Fe-Mn-C alloys used in the present investigation were made in two different ways, designated as Type I and Type 11. Type I alloys were made from high purity Fe-Mn alloys obtained in the form of 0.04- in.-diam wires from Materials Research Corporation, Orangeburg, N.Y. These alloys were carburized to different levels using gas mixtures of H2 and CH4 at 1000°C. Type I1 alloys were made in this laboratory starting with zone refined iron, spectrographically pure manganese, and spectrographically pure carbon. They were melted in an argon arc melting furnace and drawn into 0.04-in.-diam wires. All the wires were annealed at about 900°C for 3 hr prior to the internal friction experiments. After the measurements of internal friction, the phases in the samples were identified by X-ray diffraction and the carbon determined by the combustion method. EXPERIMENTAL PROCEDURE In the present work, a classical Ke-type pendulum was used. The details of the equipment were described previously by D. T. Peters.9 Dry helium at 40 torr was used in all the experiments. The internal friction, measured as the logarithmic decrement of the torsion amplitude of vibration was determined as a function of temperature, from ambient to about 500°C. The background internal friction was assumed to have the form of the exponential of the inverse temperature and was subtracted from the raw data. The height of the peak was measured at the position of the maximum in the plot of the internal friction versus temperature. The activation energies of the peaks were measured by the peak shift method. The internal friction values for an alloy were obtained as a function of temperature at different frequencies of vibration. The position of the peak changes with frequency, the higher the frequency the higher the peak temperature. The activation energy of the process associated with the peak is obtained using the formula

Jan 1, 1970

By L. C. Brown, A. J. Stewart

Phase transformations have been studied in Ag-Zn alloys quenched from the high-temperature bcc 0 phase and lying in the composition range 37.4 to 50.0 at. pct Zn. On quenching, the alloy with the lowest zinc content transformed to massive a (fcc); all other alloys formed the ordered (3' phase. On deformation, a martensitic reaction took place forming a close-packed structure. At Lou' zinc contents transformation to this structure was complete. However, above 43 at. pct Zn a p.rogressively increasing amount of ß' was retained following deformation. The close-packed structure was fcc at lower zinc contents (under 47 at. pct Zn) and either hcp or a mixture of fcc and hcp at high zinc concentrations. The structures produced by cold working were unstable and on aging transformed to the ß' phase or the complex hexagonal to phase. For low zinc contents (under 43 at. pct) the fcc st-ructure transformed directly to the equilibrium To phase. With higher zinc contents, some 13' was retained following defownation, and on aging the amount of this phase relative to the close-packed structure increased. On further aging both structures transformed cornpletely to PO. Metallographic examination indicated that the nature of the deformation product depended very markedly on the mode of deformation. Tensile deformation gave a microstructure characteristic of thermal martensite. KING and Massalski1 have shown that an alloy of Ag-50 at. pct Zn quenched from the high-temperature bcc ß phase undergoes a low-temperature ordering reaction forming ß' which can be retained to room temperature. On deformation an hcp phase is produced, although this is unstable and the structure reverts completely to ß' on aging. In the present paper, the work of King and Massalski is extended to cover a wide composition range in the p phase, observations being made of the structure of the quenched 13 and of the effects of deformation and aging. The relevant portion of the Ag-Zn phase diagram is shown in Fig. 1. King and Massalski have shown that close to stoichiometry the ß' phase is the equilibrium structure at low temperatures. The approximate composition range of this phase, taken from a recent paper by Pops and Massalski,3 is shown on the phase diagram. The locations of atom sites are very similar in the ß' and to structures, and the 4, structure can be derived from the 0' structure by a small movement of atoms mainly in the direction of the cube diagonal.4'5 However, the probability of filling any particular atom site by a silver or a zinc atom is markedly different in the two structures. The structure can be considered partly ordered but the arrangement of the ordered atoms is completely different from that in the p' structure and transformation from ß' to requires a large fraction of the atoms to change position. It has been shown that the ß' transformation is thermally activated involving normal nucleation and growth processes.5,8 Massalski and Barrett7 have shown that in the Cu-Zn binary the (3 phase can be retained in the ordered state to room temperature over a wide composition range. On deformation a new close-packed phase is produced, the structure varying from fcc to a mixture of fcc + hcp to hcp alone with increasing zinc concentration. It appears that an ordering reaction is necessary to retain the bcc phase to room temperature. In CU-Ga,8 the bcc phase cannot be retained to low temperatures as it transforms by a massive reaction above the ordering temperature of the ß phase. The structure of the massive phase is very similar to that in Cu-Zn, varying from fcc to fcc + hcp to hcp with increasing zinc concentration. Similar structures have also been observed in CU-A1,9 Ag-Cd,10,11 and Ag-Al.12 EXPERIMENTAL The alloys were prepared by melting fine silver (99.99 pct purity) and electrolytic zinc (99.999 pct

Jan 1, 1969

By J. M. Smith, G. P. Willhite, J. S. Dranoff

Heat transfer rates were measured in sandstones with flow of gases perpendicular to the direction of energy transfer. Effective thermal conductivities ker ranged from 0.7 to 1.7 Btu/(br)(ft)(°F). The contribution of the solid phase appeared to be the most important in these consolidated materials, although the thermal conductivity of the gas had some effect. The velocity of the gas through the pores of the sandstones had no influence upon ker up to values of 168 lb/(br) (sq ft) in agreement with data obtained for unconsolidated beds of glass beads. The present results indicated that gas mixing, and hence heat transfer by convection in the pores, is less for perpendicular transfer of energy than when fluid flow and energy transfer are in the same direction. HEAT TRANSFER PERPENDICULAR TO FLUID FLOW IN POROUS ROCKS Heat transfer in porous media with pore sizes in the micron range depends upon the fluid in the pores and the geometry of the solid phase. The best characterized system is a bed of solid spherical particles. Heat transfer in this system has been studied extensive1y (Ref. 8 summarizes the literature up to 1959) when the pores contain stagnant fluid. When the fluid is in motion the directions of flow and energy transfer have an effect on the heat transfer rates, as demonstrated by comparing the work of Willhite, et al l3 for perpendicular flow and that of Kunii and Smith9 for parallel flow of energy and fluid. For perpendicular flow, no increase in effective thermal conductivity ke was noted up to mass velocities G of 77 lb/(hr) (sq ft). In contrast, for parallel flow ke, increased with G in the same range of flow rates. These higher values of ke in the direction of flow also have been observed3,4,10 in beds of larger particles, 0.1- to 0.5-in. diameter. For beds of consolidated materials, such as porous rocks, data are not available for these compar- isons, although Adivarahan1 reported results for the parallel case. Hence the primary objective of this work was to measure ke values for perpendicular flow of fluid and energy in porous rocks. Of interest also was the variation in effective conductivity with fluid velocity. APPARATUS AND PROCEDURE In the experimental method, a constant heat flux was applied to the inner surface of an annular section of the porous rock. By cooling the outer wall, a temperature gradient through the annular sample was established and measured with thermocouples placed within the sample at various radial positions, and at three elevations (A,B.C). The location of the 2-in. O.D., 3.75-in. long sample in the apparatus is shown in Fig. 1. Fluid entered the bottom (1) of the 3-in. I.D. (approximate) steel shell, flowed upwards through the sample and out at the top (3). pressure taps (2,4) were used to check the permeability of the sample. The energy flowed radially from the centrally-located electric heater through the sample and was absorbed in the water-cooled jacket. The samples studied were naturally occurring sandstones from different locations with the properties given in Table 1. These materials are identical with those used by Adivarahan 1 for the parallel flow of energy and fluid. Prior to use they were refluxed with toluene to remove hydrocarbons and leached with distilled water to remove soluble salts. Each sample was visually examined and discarded if large nonhomogeneities, such as cracks or stone particles, were noted. Eight copper-constantan thermocouples were inserted in holes drilled radially into the sample with

By F. H. Gilpin

SINCE Noah pitched his ark within and without with pitch, the use of asphalt in human endeavor has been increasing-for Noah's pitch was asphalt. Asphalt is a bituminous material found in nature, either pure or admixed with smaller or greater quanti-ties of mineral and non-mineral materials, or obtained by the refining of crude asphaltic-base petroleum under proper methods of control. Native or "natural" asphalts are scattered through-out the world, though the commercial value of the various deposits varies greatly, depending upon both their accessibility and magnitude and the quality of the material found. It is an acknowledged fact that such asphalts have been produced through natural causes by practically the same application of tempera-ture and pressure as are used in the modern refining of crude asphaltic-base petroleum. The best known of all the native asphalt deposits are those of Trinidad Lake in the Island of Trinidad, British West Indies, and of Bermudez Lake in Vene-zuela. Asphalt from Trinidad Lake, after refining to remove organic and some inorganic diluents, contains approximately 35 per cent, of inorganic residue, and the asphalt thus produced must be fluxed with lighter asphaltic or semi-asphaltic base oil to make it com-mercially utilizable. The refined asphalt obtained from the Bermudez Lake deposit contains from 4 to 6 per cent. of inorganic material which cannot be removed. This asphalt, also, must be fluxed to produce com-mercial products. Small quantities of similar materials are available in other locations. The best pure native asphalt' is known as. gilsonite and is mined in com-mercial quantities in the State of Utah. In numerous places in the United States, particularly Oklahoma and Kentucky, there are deposits of sand¬stone and limestone impregnated with bitumen, which are known as rock asphalts. These rock asphalts may be used, particularly in the paving industry, either as found or by slight fluxing; from some deposits the asphalt is extracted and marketed commercially.

Jan 2, 1923