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By Strathmore R. B. Cooke, Thomas E. Bam

The paper discusses the mineralogy, structure, and strength of magnetite pellets fired in air and in a neutral atmosphere at various temperatures. The information obtained from this investigation is used to explain the origin of the structures occurring in pellets produced by pilot-plant operation. MUCH experimental work has been performed on i-VL the mechanism of agglomeration and pelletiz-ing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiold and Ilmonil much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the micro-structures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.' Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl metha-crylate monomer." The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45"C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.' Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of, these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wiistite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1953

By Strathmore R. B. Cooke, Thomas E. Bam

The paper discusses the mineralogy, structure, and strength of magnetite pellets fired in air and in a neutral atmosphere at various temperatures. The information obtained from this investigation is used to explain the origin of the structures occurring in pellets produced by pilot-plant operation. MUCH experimental work has been performed on i-VL the mechanism of agglomeration and pelletiz-ing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiold and Ilmonil much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the micro-structures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.' Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl metha-crylate monomer." The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45"C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.' Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of, these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wiistite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1953

By P. CHARTERIS A.

THE following scanty notes on the Roumanian oil-region may serve as an introduction to more detailed future study and description. The Roumauian oil-belt, follows the outer edge of the sweep of the Carpathian Mountains, and may, in a broad sense, be regarded as a prolongation of the Galician belt. It is distributed over a tract of country from 300 to 400 miles in length, with a width of from 15 to 20 miles, and is believed to cover an area of at least 20,000 hectares (59,420 acres). The Government claims that 16,000 to 17,000 hectares of its land is petroliferous. The primary deposits of petroleum are considered to be in the Padeogene (Oligocene) and the Neogene (the salines of the Miocene) formations. Most of the other repositories, especially those of Muntenie, are only secondary, the petroleum there having been introduced by the orogeneric movements which raised the Carpathian Mountains. The oil-field has been divided by the Roumanian survey into two regions, the Flysch and the Sub-Carpathian, as is shown in the accompanying sketch-map, Fig. 1.(p. 518). So far as is yet, known, practically all the seepages and .productive pits and wells are situated oil anticlinals. Those which outcrop in the Flysch region. (called Paleogene anticlinals), as indicated in the sketch-map, Fig. 1, are : Solontz, Middle Oligocene; Moineshti, Moineshti and Tagu-Ocna-beds of the Eocene.

Jul 1, 1906

By A. R. Troiano, E. A. Steigerwald, F. W. Schaller

The initiation of localized cracking in hydrogenated high strength steel was dependent on the developmeni of a critical hydrogen conceniration and relatively insensitive to the magnitude of the applied stress. The stress was believed to influence the deluyed failure process by providing the means for grouping the hydrogen. On the basis of an assumed distribution law the observed changes in the lower critical stress as a function of notch acuity, yield strength, and temperature were predictable over a significant range of these variables. THE phenomenological characteristics of delayed failure in high-strength steel have been comprehensively investigated and the behavior has been attributed to the strong embrittling action of hydrogen.1-3 Delayed failure or, as it is also termed, static fatigue, is the most sensitive means of detecting hydrogen embrittlement since it allows the maximum time for hydrogen diffusion during a test.3 The nature of delayed failure cail be aptly described by four parameters which are schematically depicted in Fig. 1. The upper critical stress corresponds to the rupture stress in a conventional notch tensile test. The lower critical stress or static fatigue limit is the stress below which no delayed failure will occur. The incubation period is the time required for the formation of the first crack and the fourth parameter is the failure time. An increase in hydrogen content, notch acuity, or strength level of the material increases the susceptibility for delayed failure by decreasing the lower critical stress, the incubation period, and the time to failure.lY3 A decrease in test temperature prolongs the incubation period in accordance with the lower diffusion rate of hydrogen, and also de-

Jan 1, 1961

By A. W. McReynolds

One characteristic of plastic deformation which distinguishes it from elastic strain is the essential inhomo-geneity of plastic strains. Elastic strain varies continuously through a material, and average relative displacements of initially adjacent atoms are only small fractions of their initial spacing, (strains of the order of 0.01 or less). On the other hand, plastic flow corresponds to the appearance of discontinuities in strain of the lattice, such as dislocations or slip bands, where local strain, on an atomic scale, is several orders of magnitude higher. These discontinuities are visible on a microscopic scale as the familiar slip lines (Fig 1). In spite of this obvious microscopic inhomogeneity, however, macroscopic measurements almost invariably show a smooth curve of stress vs. strain (Fig 2b) even if measurements of linear strains be made to an accuracy of one part in 107. This macroscopic homogeneity of strain indicates that the discontinuities in strain on slip planes occur in increments too small or too slow to be recorded individually, and further that they occur sufficiently independent of one another so that the small increments add at random to a smooth stress-strain curve. The present paper describes observations of plastic strain in aluminum of commercial purity and in high purity Al-Cu alloys, where there exists a strong coupling between slip in various regions of the specimen such that once initiated it spreads rapidly through a large volume. The total effect is that of relatively large, rapid, and regularly spaced steps of strain followed by periods of only elastic strain. Fig 2a illustrates the type of "stair-step" stress-strain curve which results. The properties of this cooperative slip phenomenon will be described further in the section on results: in par- ticular it will be shown that each step corresponds to the propagation of a wave of plastic deformation through the specimen. Some interpretations of the mechanism by which it occurs will be made in the following section. Although the type of plastic wave phenomena to be described has not previously been reported, there are numerous cases of related effects in the plastic yielding of metals: YIELD POINT PHENOMENA The most familiar of such effects is the "yield point" observed in low carbon steels, brass, duralurninum, and the like. It consists in the sudden termination of the elastic portion of the stress-strain curve by a large plastic strain. Since the usual tensile machine is such that yielding of the specimen relieves the load, the resulting curve is as shown in Fig 3. As the strain continues, deformation occurs at a lower stress for some time, then follows a rising curve, but with no further sudden yielding. This effect has been observed in brass by Sachs and Shojil and later by many others. Edwards, Phillips and Jones2 made extensive studies of the effect in steel, and of the role of various alloying elements. Although there seems to be fairly clear evidence that the yield point is caused by a hardening of the material by precipitation of impurities, no satisfactory explanation for the sudden yielding has been given. Winlock and Leiter3 have shown that the strain. level of the upper yield point depends strongly on the rate of loading, the yield point increasing by almost a fac- tor of two as the strain rate goes from 0.002 in. per in. per min. to 4.4 in. per in. per min. This effect would seem to imply an incubation period before yielding is initiated at a certain stress. On the other hand, by going to very slow loading rates, Edwards, Phillips and Jones2 showed that the yield point does not become lower and eventually disappear as might be expected, but, on the contrary, begins to rise at loading rates below about 25 Ib per in. per min. becoming much higher than at rapid loading rates. STRAIN AGING If, instead of continuing straining of a specimen after occurrence of a yield point, the load is removed and the specimen aged, resumption of the test results in occurrence of another yield point as shown by the dotted curve of Fig 3. The new yield stress is generally higher than the previous maximum applied stress. This hardening of the material by straining and subsequent aging is undoubtedly related to quench age-hardening resulting from the aging of a specimen quenched from high temperature. Since neither effect is observed in pure metals, it is generally accepted that quench-aging in all cases is the result of hardening by precipitation of a supersaturated alloying element, and that strain-aging is probably a similar precipitation, accelerated by disruptions of the lattice by previous strain. Pfeil4 has shown that strain-aging does not occur in iron from which all of the carbon has been removed, but that only a very small carbon content, around 0.003 pct, is necessary to cause strain-aging. In accord with this observation is recent work by Dijkstra5 in this laboratory showing that the solubility limit of carbon in iron is extremely low, less than 0.001 pct at 400°C. Edwards, Phillips and Jones2 have shown that the strain-aging effect is also removed by the addition of small quantities of elements such as Mo, Mn, Ti, and the like, which readily form carbides. Their results demonstrate the

Jan 1, 1950

By P. R. Bradley

NO thought had been given to deep level mining at the Alaska Juneau mine prior to 1930, but in that year a prospect winze was started and continued for 1000 ft. vertically below the main haulage or adit level. The point at which this winze was started was selected entirely by the prevailing physical conditions, such as proximity to established workings, convenience, and the presence overhead of a substantial pillar of dimensions sufficient to lo¬cate the sheave wheel and loading pocket. It was, therefore, with some surprise that the unusually high-grade ore found just below the collar of the winze persisted, with certain vari¬ations, to a full depth of 1000 ft. vertically. Likewise this unusually high-grade ore was found to persist on the various crosscuts driven on levels at 200-ft. vertical intervals. To be brief, this deep level work found richer ore than any yet found in the mine over like areas, and inasmuch as the area was sufficient to plan for extensive deep level mining, plans for such work were given extended consideration.

Jan 1, 1936

By Albert Brokaw

THE so-called ?paraffin dirt" of the Gulf Coast oil fields has been con¬sidered an indication of the possible presence of oil and gas, and not a few wells have been brought in solely on the basis of such evidence. In a sense, it may be empirically justified as evidence of the presence of oil or gas, though it cannot be said to be infallible. If the writer is correctly informed, its association with oil and gas was pointed out by Lee Hager some years ago, and while it is commonly mentioned by geologists and operators in conversation, no discussion seems to have found its way into print. The present interpretation is based on laboratory study rather than on field investigation, and is put forth with the hope of stimulating discussion which shall lead to more complete understanding. The term "paraffin dirt" has been applied to soils with a peculiar texture, which has been described' as "curdy" or "rubbery." When moist, the material breaks much after the fashion of "green" cheese. It is rubbery under compression, but does not resemble rubber in tenacity or cohesion. When dry, the material ranges from hard clods to a horny mass of high tensile strength. The shrinkage in drying is very great, especially in the hornlike matter. The moist material ranges in color from dark brown in the specimens rich in organic matter to grayish in specimens containing more inorganic matter. All of the specimens studied were readily attacked by molds, which in some cases grew in great profusion on the samples. Samples exhibited a rather characteristic "swampy" or "mucky" odor when wet, and a characteristic odor of humic soils when moist.

Jan 4, 1918

By Lee Morris, Charles E. Lawall

This paper represents the results of a study to determine the source, mode of occurrence and conditions influencing the flow and liberation of large volumes of inflammable gas in the Pocahontas No. 4 coal bed in southern West Virginia. A study of this kind is of interest in connection with mine ventilation, because in the removal of gases from coal mines it is very important to know the origin, the occurrence and laws of gas flow. The study was started in April, 1931, and the data and observations were obtained throughout a period of 15 months of field work. Geology The country where this study was made is mountainous and rugged; great cliffs, precipitous slopes and deep narrow gorges are found throughout the area. The outcropping rocks consist of stratified layers of sandstone, shale, limestone and deposits of coal of Carboniferous age. The Pottsville series of the Pennsylvanian, lying at the base of this period, cover the greater portion of the area. A stratigraphic section of the Pocahontas group of the Pottsville series is shown in Fig. 3. The older rocks outcrop in the extreme southeastern part of the area, but are under drainage in the central and northern parts due to the gradual northwest dip of the strata. The structure has a general northeast-southwest trend (Fig. 1). North of Dry Fork anticline the strata have been only slightly disturbed by movements of the earth's crust; it is now a long monocline. Southeast1 of Dry Fork anticline the strata are warped into great arches and deep troughs and are broken by overthrust faults. All of this folding is probably the result of the intense folding associated with the formation of the Appalachian Mountains. Pocahontas No. 4 Coal Bed The Pocahontas No. 4 bed, lying approximately 550 ft. above the base of the Pottsville series, is one of the thickest and most gassy coal beds in

Jan 1, 1934

New Products Equipment

Jan 6, 1953

By F. L. Clerc

THE lead and zinc region of SW. Missouri is interesting, not only by reason of the value of its output, which ranges in the neighborhood of ten million dollars a year, but even more because of the facilities which it offers for the study of certain forms of ore-deposits, of which the loci and genesis are somewhat obscure. Although the mineral species found in the region are few and of common occurrence, crystallization has taken place on a generous scale, and unusual forms abound in many combinations, presenting examples of pseudomorphism, paragenesis, metasomatic replacement and the action of mineral-depositing and mineral-dissolving waters. For the mineralogist, lithologist, and specialist in certain lines of metamorphism, it has peculiar attractions, while the systematic geologist will perhaps find its chief claim to attention in the simplified problem it presents, in the study of ore-deposits. In addition to the phenomena above enumerated, it presents instances of well-developed comb-structure in the ores, fissures and faults, and slickensides-features usually associated with extensive movements in the earth's crust, and believed by some authorities to prove the deep-seated origin of the ores. In connection with these occurrences, the absence of all igneous rocks from this region is noteworthy and significant. For that reason, the simplified case presented by the Joplin region, from which these rocks have been eliminated as a factor, is specially valuable. Having had unusual opportunities to watch the development of this district, I have been deeply interested in the bearing of the revelations of the Joplin mines upon questions of universal importance to the science of ore-deposits ; and it was to my great regret that the project of a meeting of the American Institute of Mining Engineers at Joplin, proposed in 1892, was

Mar 1, 1907

By R. K. Buhr, H. Thresh, M. Bergeron, F. Weinberg

The microsegregation of nickel and chromium in directionally solidified AISI 4340 steel castings has been measured using electron probe microanalysis. Minimum concentrations were observed to occur at the center of the dendrite stalks, as reported previously. However, the position of the maximum concentrations could not be determined from the dendrite configuration. An etching technique has been developed which shows the position of maximum concentration. Measurements were made of the distribution of nickel and chromium in the dendritic structure. The ratio of maximum to minimum concentration was determined as a function of primary dendrite arm spacing for both as-cast and partially homogenized materials. The results are compared with observations reported in the literatuve. A S part of an investigation of solute segregation in directionally solidified AISI 4340 steel casting, electron probe microanalysis was used to measure the distribution of nickel and chromium in the dendritically segregated material. This complemented the observations on the segregation of radioactive phosphorus obtained by autoradiographic techniques in the same castings.' Kattamis and I?lemings2 have reported similar measurements, using electron probe microanalysis, on dendritically segregated AISI 4340 steels. They found minimum solute concentrations occurred at the center of dendrites, maximum concentrations occurred in the center of interdendritic regions, for symmetrically oriented dendrites, and a regular variation of concentration within dendrite arms. The ratio of maximum to minimum concentration was found to be essentially independent of position in the castings, except near the chill surface where it was somewhat higher. Assuming complete diffusion in the liquid and no diffusion in the solid during freezing, they considered that isoconcentration curves in the steel were homothetic. As a result, isoconcentration curves of the various elements, contour surfaces of dendrites produced by isothermal-transformation studies, and the contour of the solid-liquid interface would all be similar, and could be superimposed by a uniform expansion or contraction of the contours. Preliminary results of the present investigation suggested that isoconcentration curves were not homothetic. It was also evident that points of maximum concentration could not be predicted from the dendrite configuration. Since the ratio of maximum to minimum concentration appeared to be an important parameter in defining the overall segregation in a casting, other techniques for determining the point of maximum concentration were investigated. In addition the overall solute distribution associated with the dendritic structure was examined for both nickel and chromium, and the consistency of the distribution for neighboring dendrites was determined. METHOD Fifty-pound heats of AISI 4340 steel were cast in a manner similar to that used by Flemings et al3 with a water-cooled copper base plate and exothermic sides and top. The nominal composition of the material was C, 0.41 pct; Mn, 0.66; Si, 0.35; S, 0.012; P, 0.010; Ni, 1.88; Cr, 0.95; Mo, 0.28. The steel solidified directionally from the chill surface, with a dendritic structure which increased in dendrite arm spacing with increased distance from the chill. Results of the general investigation of the cast structure and segregation of radioactive phosphorus in these castings have been reported elsewhere.' For the present measurements, sections were cut from the casting at several distances from the chill surface. The sections were subsequently heat-treated, mounted, and then polished on a plane perpendicular to the general freezing direction of the casting. Electron probe microanalysis was carried out with the JEOL-JXA3 microprobe using a voltage of 25 kev and beam current of 0.15 µa. The take-off angle is 22 deg. Quartz crystals were used in the spectrometers and measurements made for Ka radiation from both nickel and chromium simultaneously. A thin layer of carbon was deposited on all specimen surfaces prior to examination in the microprobe. Early measurements were made on polished surfaces, with indentation marks produced by a hardness tester to indicate the area of interest. It was found desirable to use etched surfaces, as opposed to polished surfaces, to reduce sample preparation time and more readily relate the microprobe scan to the structure. To determine if this could be done, without introducing significant errors, a series of measurements were made on polished and etched surfaces of the same specimen. Both polished and etched surfaces produced similar results within normal scatter as shown in the observations. Subsequent measurements were then made on etched surfaces. Measurements with the microprobe analyzer were made by point counting, for periods of 100 sec, at 10-µ intervals. Ten-second counts were made on pure nickel and chromium standards, incorporated in the specimen mount before and after each set of measurements. The results were adjusted for background, then corrected for dead time using the expression:

Jan 1, 1969

By W. L. Prehn, Adele Chambers, R. L. Slobod

The centrifuge has been found to be an extremely useful tool for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. The use of the centrifuge for determining the properties of small core plugs has been discussed in the literature,',' but practically no experimental evidence has been presented justifying the use of this method in preference to other methods (mainly disc method) now in use. Data have been accumulated and are now presented demonstrating the advantages of the centrifugal method, some of which are: (1) rapid establishment of equilibrium, (2) excellent precision yielding very reproducible results, (3) availability of high pressure differences between phases, (4) simple operational procedure, and (5) ability to establish connate water, residual oil, or to obtain complete capillary pressure curve in one day or less. A commercially available centrifuge capable of speeds up to 3,800 rpm, and a high speed attachment providing a maximum rate of rotation of 18,000 rpm were used in this work in conjunction with core holding tubes designed specifically for this application. In view of the outstanding advantages associated with the use of the centrifuge the conclusion has been drawn that this method should be used in place of the more tedious, slower, and less reliable disc method for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. INTRODUCTION The need for accurate values of connate water, residual oil, and capillary pressure curves in reservoir engineering has been recognized for many years, and the extent of the effort devoted toward solving these problems is reflected in the large number of papers3-" which have appeared in the literature during the past decade. Most of the methods discussed in the recent literature employ a porous disc as a semi-permeable membrane to separate two immiscible phases and make pos-ible the application of an explicit difference in pressure between two phases in the core. Thus, in the determination of the capillary pressure curve the wetting phase (water) is displaced by the non-wetting phase (air or oil). Several investigators1,2 have used centrifugal forces to develop pressure differences between phases. As a result of the first work' in this field the conclusion was reached that "the more rapid centrifugal method for measuring irreducible saturation may have equal value, (compared to use of discs) but more work is required to establish this point." This work was followed in 1945 by a more detailed study2 in which the concepts of this experimental work were more clearly enunciated. A method for calculating saturation for any given speed of rotation based on the observed volume of water displaced was developed and a wider application of the method was suggested. The absence of any subsequent pertinent literature on this subject is interpreted as indicating that no additional work has been completed to substantiate or deny the earlier claims and suggestions of promise contained in the original papers on this subject. One purpose of this report is to provide evidence designed to establish the practical value of centrifugal methods in determining core properties such as connate water and capillary pressure curves. It is also our purpose to suggest a broadening of the scope of this tool to include determinations of residual oil by gas or water drives. THEORY AND PRACTICE IN USE OF CENTRIFUGE Hassler and Brunner2 have clearly presented the basic concepts involved in the use of the centrifuge by relating the performance of a small core in a field of high acceleration to the

Jan 1, 1951

By R. L. Slobod, W. L. Prehn, Adele Chambers

The centrifuge has been found to be an extremely useful tool for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. The use of the centrifuge for determining the properties of small core plugs has been discussed in the literature,',' but practically no experimental evidence has been presented justifying the use of this method in preference to other methods (mainly disc method) now in use. Data have been accumulated and are now presented demonstrating the advantages of the centrifugal method, some of which are: (1) rapid establishment of equilibrium, (2) excellent precision yielding very reproducible results, (3) availability of high pressure differences between phases, (4) simple operational procedure, and (5) ability to establish connate water, residual oil, or to obtain complete capillary pressure curve in one day or less. A commercially available centrifuge capable of speeds up to 3,800 rpm, and a high speed attachment providing a maximum rate of rotation of 18,000 rpm were used in this work in conjunction with core holding tubes designed specifically for this application. In view of the outstanding advantages associated with the use of the centrifuge the conclusion has been drawn that this method should be used in place of the more tedious, slower, and less reliable disc method for determining capillary pressure curves and for establishing connate water and residual oil in small core plugs. INTRODUCTION The need for accurate values of connate water, residual oil, and capillary pressure curves in reservoir engineering has been recognized for many years, and the extent of the effort devoted toward solving these problems is reflected in the large number of papers3-" which have appeared in the literature during the past decade. Most of the methods discussed in the recent literature employ a porous disc as a semi-permeable membrane to separate two immiscible phases and make pos-ible the application of an explicit difference in pressure between two phases in the core. Thus, in the determination of the capillary pressure curve the wetting phase (water) is displaced by the non-wetting phase (air or oil). Several investigators1,2 have used centrifugal forces to develop pressure differences between phases. As a result of the first work' in this field the conclusion was reached that "the more rapid centrifugal method for measuring irreducible saturation may have equal value, (compared to use of discs) but more work is required to establish this point." This work was followed in 1945 by a more detailed study2 in which the concepts of this experimental work were more clearly enunciated. A method for calculating saturation for any given speed of rotation based on the observed volume of water displaced was developed and a wider application of the method was suggested. The absence of any subsequent pertinent literature on this subject is interpreted as indicating that no additional work has been completed to substantiate or deny the earlier claims and suggestions of promise contained in the original papers on this subject. One purpose of this report is to provide evidence designed to establish the practical value of centrifugal methods in determining core properties such as connate water and capillary pressure curves. It is also our purpose to suggest a broadening of the scope of this tool to include determinations of residual oil by gas or water drives. THEORY AND PRACTICE IN USE OF CENTRIFUGE Hassler and Brunner2 have clearly presented the basic concepts involved in the use of the centrifuge by relating the performance of a small core in a field of high acceleration to the

Jan 1, 1951

By Irving Fatt, R. M. Weinbrandt

Efforts have been made for many years to observe pore structure of sedimentary rocks on a microscopic scale. A better description of the pore structure in reservoir rock would aid in the development of relations between flow through tube network models and flow in consolidated reservoir rock. The unique qualities of the scanning electron miscroscope (SEM) make it the ideal tool to use in a study of pore structure. Previous methods of studying pore structure included plastic casts of pore space and optical microscopy.l-7 There is now available a new method to observe three-dimensional flow channels in reservoir rock: a scanning electron microscope having variable magnification from X20 to X20,000 and approximately 1000 times the depth of focus of the conventional light microscopes. This microscope also can obtain stereoscopic images and can measure and diagram flow channels so that it is possible to construct a network of tubes that will model consolidated reservoir rock. THEORY OF THE SCANNING ELECTRON MICROSCOPE The scanning electron microscope (SEM) functions by projecting a beam of electrons through magnetic focusing lenses at a specimen and recording secondary electrons excited by the primary beam. The amount of secondary electron emission portrays the topography of the specimen because more secondary electrons are emitted from high points than from low points. A schematic of the SEM is shown in Fig. 1. The property of the SEM that is of most importance in this study is its great depth of focus. The depth of focus results from using electrons

Jan 1, 1970

By S. Harries Daddow

IN order to get an idea as to the strength of steel rails, it will be well to review the tests to which iron rails have been subjected. In England, Mr. Ashcroft found that the best 80 pound rails broke under a 300 pound weight, falling 15 feet. In Germany the Society of Railway tyfanage1-s determined 011 and have long applied a test of 1000 pounds falling 101/2 feet, as the standard which all first-class iron rails must reach. In this country no inspection nor test is applied, but tests made show that iron rails fro; our most reliable makers, break under a G foot fall of a 1500 pound drop as an extreme test, most of those tested breaking under a far less test; some breaking with less than a 3 foot fall of the same weight. Everywhere where steel has been used, engineers have come to the conclusion that some test is required to show the regularity and strength of the product. As compared with iron, the tests which steel will stand are wonderful. After numerous experiments partially based on the experience of the rail-mill at Graz, belonging to the Southern Railway of Austria, the Society of German Railway Managers fixed upon a test of 2000 pounds falling 138 feet. They found that this test represented the steel which suited their necessities, and also found that with steel of otherwise average purity, this test represented about one-half per cent. of carbon, and made it a rule to take no steel containing under three-tenths of a per cent. of carbon, because it was too soft. They expressed a hope that a harder steel could soon be made tough enough to stand the same test. I n England, a test was adopted of 2240 pounds, falling 15 to 17 feet on the rail on heavy bearings. This test has been found satisfactory under heavy traffic on average road-beds, and has been invariablyPILLAR of coal, which are designed and left in our mines as the means of supporting the overlying strata of our coal-beds, and securing protection to the miner, are not only insufficient for these purposes, but the most objectionable means of providing the desired security to life and property. Though such pillars are left at a great sacrifice to the owners of collieries and mineral lands, loss to the resources of the commonwealth, and ultimate privation to the public, they defeat the very ends for which they are designed, and not only do not secure life and property, but are as fatal to the one as ruinous to the other. Propositions.-It is eminently desirable that the resources of the Common wealth-particularly our mineral wealth in anthracite coal, which is limited-should be carefully utilized and made available, not only to ourselves but our posterity. Yet, speaking as an anthracite miner, we are wasting our resources of coal with a recklessness which will bring ruin in the end, unless checked, not only to the iron manufacturing interests of the East, whose chief protection, in competition with the iron-masters of the interior, lies in a cheap and abundant supply of anthracite furnace fuel, but to the best interests of the State. It is, consequently, not only desirable, but necessary, that we should realize every ton of coal from each colliery, and every acre of coal area, in order that our resources may not be wasted at present, to breed want in the future, and to realize the greatest present benefit to the mine, the miner, and the public. It is not possible, however, to secure these ends, if we continue to leave, as we do at present, from one-third to one-half our resources in anthracite as pillars in our mines. But our sad bills of mortality, our abandoned collieries, and our yawning mountain-sides, present ample evidence that even this enormous waste of coal, though left for the purpose of protecting life and property, is as totally inade-

By C. K. McArthur

THE subject of classification is so broad that this discussion is confined to what the author believes is of prime importance in connection with proper grinding and classification. The years passed have witnessed many noteworthy changes in fine grinding and classification, which have been accompanied by a readjustment of ore-dressing flowsheets for the preparation of better ground and/or sized products at an expenditure of less power, steel and maintenance than formerly. Nowhere in the industry is more being done in the way of experimental work to lower costs than in grinding circuits, because, at best, grinding costs are high. Recent years have indicated that, on the average, finer grinding has a real application. Without careful preparation of the process feed, no operation can be highly efficient or successful. In an earlier paper, the findings of an extensive survey at representative concentrators were presented1. Also, in the year of 1935, a technical discussion was given by Dr. J. V. N. Dorr (Some Notes on Classification Trends in America) before the Chemical, Metallurgical and Mining Society of South Africa In both papers mentioned, much has been said regarding flowsheets, grinding and classification. The author is very familiar with these papers, having had considerable to do with the actual operation of the flowsheets, as well as large mills and classifiers in the work described. Some data from the second paper have been included in the following discussion. Circulating Load In this particular paper it seems advisable to deal with the classification phases of the work that to a major extent govern the success of any closed-circuit grinding unit. The question has often been asked in connection with a closed circuit: "What circulating-load ratio should be carried?" This is really an

Jan 1, 1937

By A. A. Burr, D. G. Ebeling

The effects of casting texture, grain orientation and grain size upon the performance of Alnico permanent magnets is described. Single-crystal specimens were produced by special sintering and grain coarsening techniques to study the effect of crystal orientation. In addition to texture and orientation effects, an analysis of the results indicates that the permanent magnet performance is impaired by a refinement of the grain size. AN excellent historical review of the development of Alnico permanent magnets has been prepared by Bozorth.1 The desirable permanent magnet characteristics of Fe-Ni-A1 alloys were discovered in 1932 by Mishima.2,3 The work of Ruder' showed that the alloys were age-hardenable, and Betteridge5 defined the best composition and heat treatment for the magnetically isotropic alloy known as "Alnico 3." Horsburgh and Tetley0 increased the energy product by the addition of cobalt and copper, "Alnico 2," and Oliver and Sheddon7 demonstrated that cooling in a magnetic field improved the residual induction of this alloy. Jonas8,9 then disclosed the great practical benefits of heat treating an alloy of higher cobalt content in a magnetic field and the resulting alloy, "Alnico 5," has become the standard of the industry. This paper describes the fundamental aspects of a procedure which can be used to further improve the properties of these anisotropic permanent magnet alloys. A study of the casting techniques used in the production of anisotropic Alnico permanent magnets indicated that the magnetic quality was affected by the as-cast macrostructure. Improved performance was observed in magnets containing a high percentage of columnar grains whose long axes were parallel to the magnetic axis of the casting. McCaig10 studied the effect of such columnar grain structures upon the magnetostriction characteristics of similar alloys, however no data was presented showing the effects on other magnetic properties. The following paragraphs describe two experiments which were conducted to determine the effect of various grain orientations upon the energy product. Special composite molds were prepared of highly conductive and highly refractive components to remove the heat of solidification from the casting in a controlled manner. Representative macrostructures produced by these techniques are shown in Fig. 1, along with the relative volumes of favorably oriented columnar grains. The alloy, Alnico 5, has the highest permanent magnet performance of any commercial magnet material. It has the nominal weight composition of 8 pct Al, 14 pct Ni, 24 pct Co, 3 pct Cu, and 51 pct Fe. A heat of this material was cast into molds producing the type A and B grain structures shown in Fig. 1 and pairs of the resulting magnets were placed in heat-treating boats so as to eliminate any biasing effects of boat position. After a standard heat treatment the type A magnets, with 16 pct of the volume composed of favorably aligned grains, had a maximum energy value of 3,940,000 gauss-oersteds, while the type B magnets with 73 pct aligned grains averaged 5,090,000. This large im-

Jan 1, 1954

By Francois Clerf

IRON ORE fields are situated in both the East and West of France (see maps). The eastern deposit is by far the most important from a tonnage point of view, not only in France, but in all Europe. The ores of this region are known as minette, and are situated in the Lorraine ore fields and the Briey plateau. The iron ores of the West are those of Normandy, Anjou and Brittany. Before the war, a large number of important German companies had acquired considerable interests in these western fields and a heavy trade with Westphalia had begun. Recently, however, conditions have changed and some of the mines of Brittany and Anjou are now idle. From a geological point of view, in Anjou and Brittany, a series of synclines extends from the northwest to the southeast, containing a number of seams of varying thickness and generally intercalated in Silurian and sometimes in Devonian formations. The ore is generally a hematite or a magnetite. The composition varies from 48 to 52 per cent of iron and from 8 to 12 per cent of silica. Con¬servative estimates indicate a con¬siderable tonnage of workable ores (150,000,000 metric tons).

Jan 1, 1936

By F. R. Brotzen, L. D. Whitmire

Single crystals of high-purity molybdenum were de-formed at temperatures from 195°to 473°K, and the effect of deformation on the electrical resistivily was deler-mined. To separale the resislivity components of point and line defecls some cryslals were annealed at 473°K. The vale of resislivily increase wilh strain was nearly linear and was strongly dependent upon the deformation temperature. Point dejects are annealed out without any effect on the flow stress. At low temperatures the flow stress is a linear function of the square root of the resistivity increase attributable to dislocations. ELECTRICAL-resistivity measurements have been used successfully to gain information on structural changes in metallic materials. During plastic deformation the electrical resistivity rises because of electron scattering from newly created lattice defects. Such measurements lend themselves, therefore, to corroborating results from direct observation of lattice defects and, to a certain extent, to correlating defect densities and distribution with mechanical properties. Published information on research with single crystals of the bcc metals of Group VI, particularly molybdenum, is still limited. Yet, molybdenum single crystals of relatively high purity can be readily prepared by electron-beam-melting techniques. Furthermore, some valuable information on the defect structure of deformed crystals by direct observation is available. Lawley and Gaigher,1 for example, have examined dislocation configurations in deformed molybdenum crystals by means of transmission electron microscopy. Their results revealed that the dislocation density and distribution were strongly dependent upon the deformation temperature. These findings differed from those by Keh and weissmann,2 who found that the average dislocation density in polycrystalline iron deformed between 138° and 298°K depended only on the degree of strain and not on the deformation temperature. Martin3 and peiffer4 showed that point defects introduced in polycrystalline molybdenum by cold work can be eliminated by annealing at a relatively low tempera-ture. In view of their work it became apparent that resistivity measurements of suitably annealed crystals could disclose changes in their dislocation structure and contribute to the understanding of the work hardening of molybdenum crystals. EXPERIMENTAL PROCEDURE Crystals were grown by electron-beam zone melting5,6 of 0.062-in.-diam molybdenum rods (99.99 pct) supplied by General Electric Lamp and Wire Division, Dover, Ohio. The crystals, about 4 in. long, were prepared by using five zone-refining passes at a speed of about 6 mm per min in a vacuum of about 5 X l0-6 Torr. The resistivity ratio of the crystal, p(4.Z°K)/p(273°K), was generally near 10-3. These crystals were used as tensile specimens of uniform diameter in the "as-grown" condition. They were oriented for maximum shear on the (011)[111] slip system (Schmid factor >0.49). The specimens were held in spherically seated Templin-type grips so as to minimize bending. Samples were deformed on an Instron machine at a strain rate of about 5 X 10-5 sec-1 in an isopentane bath with dry ice at 195°K, in ice water at 273°K, and in a vegetable-oil thermostat at 373° and 473°K. The temperature in the latter was maintained constant within +2°K. Resistance measurements were carried out with a Kelvin double bridge. The resistance of the potential leads was kept low by using large-diameter wires outside the low-temperature bath. Many of the resistance data were checked by measurements made with an ac bridge. Current and potential leads were spot-welded to the specimens. The distance between the potential leads, about 3 in., was also considered to be the gage length for the strain measurements. Diameter and gage length of the samples were measured optically with an error of less than 2 pct. These measurements were used also to insure that the deformation had been uniform over the gage length of the specimen. Resistivity changes were then determined from the resistance measurements at 4.2°K assuming constancy of volume. In the course of a test, the crystal diameter, gage length, and resistance at 4.2°K were determined first in the initial state and subsequently for various amounts of elongation.

Jan 1, 1968

1910, hundreds of thousands of dollars of work and equipment in a 1500-foot shaft, crosscuts and pumping had found only copper-lean pyrite in two cross- cuts, and nothing in a third. Going aimlessly along the third crosscut one day, after looking at the barren face I happened to notice a dark spot in the white limestone, near the floor on one side. I picked, and found it was a little triangle of rich chalcopyrite. Next day I took Bill Gohring, then mine superintendent, in to see it. He said nothing else had succeeded so we might as well try that. The new drift broke into a full face of high grade copper ore in the first round, and continued in rich ore for 2200 feel broken only by a couple of short stretches of lean pyrite. The earlier crosscuts had happened to cut these lean areas. Q: Was there any single thing that called your attention to that little dark spot in the side of the Briggs crosscut, rather than to any other discolored spot? Joralemon: Nothing very definite. Maybe luck, maybe that indefinable subconscious thinking that

Jan 9, 1964