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By Irving Fatt, Robert J. S. Brown

INTRODUCTION The wettability of reservoir rocks is recognized as one of the major factors that determines their multiphase flow properties. Multiphase flow properties in turn govern reservoir performance. For this reason, the reservoir engineer is vitally interested in the wettability of reservoir rock. The production research scientist is interested in wettability because the solution of the problem of improving waterflood recovery by use of surface-active additives may hinge on a detailed understanding of the wettability of reservoir rock. Early workers believed that all reservoir rocks were preferentially water wet. Continued study soon uncovered certain rocks which had flow properties that indicated that they were preferentially oil wet. Recent studies show that there is a spectrum of wettability. Some reservoir rocks have multiphase flow properties which indicate that they have an intermediate wettability. The differences in recovery observed among different reservoirs may, in part be the result of small differences in wettability. Differences in wettability amcng reservoir rocks may be the result of differences in the fraction of the total surface area that is preferentially oil wet and preferentially water wet. Nuclear magnetic relaxation measurements may provide a method for determining the fraction of preferentially oil wet and preferentially water wet area in porous media. Measurements to be reported here were made on water-saturated unconsolidated sand packs which were mixtures of preferentially oil wet and preferentially water wet sands. The resulting data show definitely that the fraction of each wettability in these sand packs can be determined by this nondestructive method of measurement. THEORY OF NUCLEAR MAGNETIC RELAXATION The details of the theory of nuclear magnetic relaxation have been presented previously1. In this paper, only a very brief review of the theory will be given to show its application to the measurement of fractional wettability. Nuclear magnetic relaxation is a process of adjustment undergone by certain atomic nuclei when their magnetic environment is changed. They adjust, or relax, to be in equilibrium with a new magnetic field. The reason that some atomic nuclei are affected by a magnetic field is that they themselves behave in some respects like tiny magnets. In particular the proton, the nucleus of the hydrogen atom, behaves as a magnet. The proton spins, somewhat as the earth spins on its axis. The spinning charge produces a magnetic field just as current traveling in a loop of wire produces a magnetic field. No net charge is required, however; for instance, the neutron has spin and magnetic moment. When the spinning proton is subjected to an externally applied magnetic field, its axis tends to line up with the magnetic field, somewhat as a compass needle tends to line up, but the spinning proton cannot do this as easily as the needle can. The proton also has mass, and its spinning mass makes the proton behave somewhat like a gyroscope. As is well known, a force which tends to change the axial direction of a gyroscope merely causes the gyroscope to precess: lhat is, the axis begins to trace out a conical surface. The gyroscope cannot actually assume the position suggested

Jan 1, 1957

By W. K. Hardy, H. H. Stadelmaier, L. J. Huetter

The ternary system Co-Sn-C was studied in the cobalt-rich region. The liquidus projection ulas established and two fonr -phase reactions were found. An isothermal section at 950°C was worked out. In the region studied the following phases were observed: cobalt-rich solid solution, graphite, binary compound y -cobalt-tin, and a ternary compound. As a result of the limited solubility of carbon in liquid cobalt-tin alloys, the investigation was limited to the cobalt-rich region. Tin contents up to 32 at. pct were studied. Cobalt of 99.99 pct purity, tin of 99.97 pct purity and synthetic graphite of 99.93 pct minimum purity prepare the alloys. Carbon determinations of all alloys were obtained by gas volumetric analysis. Samples were investigated microscopically and by X-ray diffraction using CoK, and FeK, radiation. Cooling curves were obtained with a number of alloys to determine the temperature of the four-phase reactions. The thermocouple was calibrated with the melting points of high-purity silver and copper. In the region studied the following phases were observed: Cobalt-rich solid solution (face-centered cubic) Graphite. Binary compound y (solidifies congruently at composition Cop~n)'. Ternary compound k which is face-centered cubic with superlattice and nonferromagnetic.' In Fig. 1 the fields representing the projections of the liquidus surfaces were determined by microscopic investigation and are labled by their primary phase. In the field labled C graphite is the primary phase. During solidification in this field much of the primary graphite was expelled through the surface of the melt. It could not always be established microscopically whether the remaining graphite was primary or purely eutectic. Therefore it was not possible to determine accurately the boundary curve which drops from the binary eutectic el at 1309 "~~ to the point of the four-phase reaction at F. The ter-nary carbide is the primary phase in the field labled k. To the right of this field the primary graphite is consistently nodular whereas flake graphite is observed at tin contents somewhat below F. The ternary carbide does not appear to solidify congruently. The graphite is attacked in a peritectic reaction along the boundary between k and C. Thus no graphite is observed in alloys in the k field. In alloys right of the boundary between k and C the graphite nodules are located in the center of the k crystallites, further documenting the peritectic nature of the reaction with the graphite. A four-phase reaction was found at F and 1120 &3"C. The most likely reaction is L+ CY-Co + C — k. Below the temperature of the binary eutectic ez at 1112" a second four-phase reaction was observed at E and 1100 lt3"C. It is the ternary eutectic L — CY-Co + k + y. Figs. 2(a ) to (e) show microstructures of the ternary alloys in the as-cast condition. Fig. 2(a) shows the eutectic a-Co + C (with some primary graphite) with the carbide k in the grain boundaries. Fig. 2(b) shows primary cobalt (dark areas) and the eutectic a-Co + k which is formed along F-E.

Jan 1, 1961

ASIDE from the John Fritz Medal, in which the Institute participates through its representation on the John Fritz Medal Board, the Institute itself has five major awards to make annually for excellence in technical papers, as follows: The Robert W. Hunt Medal and Prize, The J. E: Johnson, Jr. Award, The Lewisohn Platinum Prize to senior members, and the James Douglas Medal. ROBERT W. HUNT MEDAL AND PRIZE The partners of Robert W. Hunt established a fund which was presented to the Institute at a fitting ceremony on May 27, 1920, to' establish an annual medal and a sum of money to be awarded under the following rules: 1. The award shall consist of two prizes; first of a gold medal, second of a sum of money; a certificate to accompany each prize. The money prize shall not be awarded to a member over 40 years of age, but under unusual circumstances, both prizes may be allotted to one person provided that he is not over 40 years of age. In general it will be understood that the Committee shall award the money prize to the younger men, rather than the medal. 2. The awards shall be made not oftener than once a year to that person or persons contributing to the Institute the best original paper or papers on iron and steel. The scope of the term" iron and steel" shall be determined by the sub-committee considering the awards. In general, papers dealing with the practical side of the subject have preference over those dealing with the theoretical side in recognition. of the fact that Captain Hunt's main contributions to the industry have been in the improvement of production and quality of material. 3. A sub-committee of three to five, including the Chairman of the Iron and Steel Committee, shall be appointed by the Iron and Steel Committee annually to adjudge the award subject to approval. 4. The awarding committee shall submit its report to the Iron and Steel Committee at its October Meeting, and the award be certified to the Secretary of the Institute in time to permit the presentation to be made at the Annual Meeting of the Institute. 5. The recipient of the award shall be ,designated "The Hunt Medallist." This prize is administered by the Iron and Steel Committee. J. E. JOHNSON, JR. AWARD This award is made from the income of a fund of $3000 donated by Mrs. Margaret Hilles Johnson in memory of her husband, J. E. Johnson, Jr., who was a prominent engineer, author of two valuable volumes on iron blast-furnace construction and practise, vice-chairman of the Institute's Iron and Steel Committee, and a frequent contributor of papers to the Institute's Transactions. This prize is administered by the Iron and Steel Committee. The intent of the donor is to encourage young men in creative work in branches of the metallurgy or manufacture of pig iron with which the professional activities of Mr. Johnson were chiefly concerned. The control of the fund and distribution of the awards having been vested in the Board of Directors of the Institute, this Board has made 'the following regulations concerning it:

Jan 1, 1925

By Howard I. Epstein, John R. Buzek

Thickeners are simply large tanks, usually circular in shape, which are designed to allow settling of solids and to operate with continuous overflow of clear water and underflow of thick pulp. The dimensions of the thickener are usually such that dewatering of very fine pulps may be accomplished while still overflowing clear water. Some thickeners such as the Center, Hardinge and Hydrotator types combine thickening with filtering2 while others such as the Dorr type are pure thickeners. l .2 , 3 A schematic diagram of the traction type Dorr thickener is shown in [Fig 1]. This type is appropriate for tanks over 15 m (50 ft) in diameter. This tank employs a rotating raking mechanism which moves the settled material toward the central discharge. For this and other thickeners, it is common to have a shallow conical tank bottom in order to conform to the geometry of the raking mechanism, and it is often desirable to elevate the tank for ease of access to the product. When the tank does not rest on the ground, the forces resisted by the cone are large, and thick plates must be employed. The fabrication of these tanks requires temporary supports in order to erect the cone. A flat-bottomed tank could also be used because the settled material would soon form a hardened conical surface. However, because of the presence of large bending forces, even larger plate thicknesses are required than for the conical bottom. Significant cost savings often can be realized by the use of a scalloped-bottomed tank such as the one partially shown in [Fig. 2]. The particular scalloped bottom discussed in this paper employs radial beams forming the outline of the cone-shaped bottom. These beams are supported directly by columns. Cone segments are hung between adjacent beams. The exact geometry of these segments depends upon the cone angle and radius, the number of radial beams, and their inclination. The geometry is chosen to satisfy certain clearance restraints and to utilize the material as efficiently as possible. The resulting thickness of these segments is significantly less than that of the equivalent plate for the tank with a conical bottom. This result, along with the simpler fabrication procedures required, accounts for the cost savings associated with this design. The raking mechanism employed may be the same as for the conventional conical bottom since the settled material soon forms a conical surface. Determination of the internal force mechanism for the scalloped bottom leads to designs that utilized material efficiently and thus maximize the cost savings. The complicated geometry of these bottoms along with the difficulty in analyzing the structure are factors which may have limited the use of scalloped-bottomed tanks to date. When such tanks have been built, the uncertainties associated with the internal forces have led to designs that are somewhat inefficient. In this paper, equations relating the geometric parameters are presented along with simplified closed-form solutions for the internal forces in the cone segments, from which the loads applied to the beams and the loads carried to the cylindrical tank shell can be deduced. An example is presented to show the magnitude of the savings which may be realized with this configuration.

Jan 1, 1979

By S. K. Sarkar, B. Dr. Singh

INTRODUCTION India like USA has traditionally relied on bord and pillars as dominant underground method. Coal has generally been mined at shallow depth from relatively thick and horizontally bedded coal seams. These' factors contributed towards large scale adoption of bard and pillar. After nationalisation of coal industry in two stages in 1971 and 1973, large scale mechanisation and modernisation programmes were undertaken. Longwall mining was identified as one of the major that area for increasing underground coal production. The idea to introduce longwall mining was mooted to increase productivity and to promote conservation and safety. The nationalised coal industry has already worked about twenty longwall faces with different types of support. The tempo of introducing longwall is catching up and a number of longwall programmes with, Self advancing supports of different types and Capacity are in active stage of implementation. The country has not yet started producing mechanised Supports and therefore supports and machineries are being imported from U.K. and other countries of the continent. The of the major problem faced in the longwall projects is to choose suitable type and capacity of supports. The suppliers and manufacturers of these supports are not competent enough to choose and offer the right type and capacity of supports as their knowledge and information about Indian strata conditions are extremely limited. The Central Wining Research Station (Q.!RS), has undertaken a research programme for evaluating the rock mechanical conditions obtaining in the proposed longwall locales and has worked out a method for selection of proper type and capacity of supports on the basis of projected strata behaviour at the proposed locale. STRATA CCNTROL FAILURES Indian coal industry had made some attempts to introduce longwall caving in the early fifties after a working group set up by the Government of India had recommended its adoption to increase productivity and to modernise mines. Approximately 20 longwall faces were tried in the major Indian coalfields of Jharia, Ranigunj and Karanpurr between 1951 and 1968. The supports used consisted of 20T hydraulic props or 35140~ friction props. A number of these faces had suffered total strata control failures and a large number of support elements were lost. The Central Mining Research Station initiated a research programme to analyse these failures in the general background of behaviour of Indian coal measure strata at longwall faces. All the available data regarding the cases of failures were collected and physico-mechanical properties of overlying roof rocks were determined in the laboratory. Simultaneously, observations were continued to establish the behviour pattern of Indian coal measure strata at longwall faces. These studies were helpful in analysing the occurrences of collapse. BEHAVIOUR OF INDIAN COAL MEASURE STRATA The coal measure strata encountered in the principal Indian coalfields of Jharia, Ranigunj and Karanpura are in general strong in nature however, the immediate roof (mostly up to 1.5 to 2 m) in most of the cases is weak and false bedded shale. MI idea about the strength properties of immediate and overlying roofs may be obtained from the following table.

Jan 1, 1982

By T. D. Tiemann

The caustic extraction of silica from Wisconsin and Minnesota taconite was investigated by bomb digestion over the temperature range from 312 to 40S°F at caustic concentrations from 25 to 500 gpl. Residual concentrates containing as much as 65 pct iron were obtained. The high rate of silica extraction is related to a microcrystalline variety of quartz, since it is shown that the rate of extraction of silica from quartz is directly proportional to its surface area. Increasing dependence on foreign ore reserves makes the need for developing the technology necessary for treatment of our low grade ores even greater than it was at the time of World War 11, when much research was conducted on the extraction of alumina from clays. Representative of these were the studies carried on at the University of Illinois.' More recently, the U. S. Bureau of Mines investigated the production of alumina from anorthosite, and currently the aluminum industry is showing renewed research interest in this field. The studies reported here are part of a continuing research program based on the above concepts and aimed at the eventual development of processes for the treatment of low grade ores, particularly those of iron. The fact that large reserves 3 of low grade nonmagnetic taconite are contained in the iron formation of the Wisconsin Gogebic range have made this ore an important and attractive target for investigation. The idea of removing silica by caustic extraction is not new.495 The digestion in caustic solution of ground flint, diatomite, and other forms of chalcedonic silica is the basis for the production of soluble sodium silicates by the wet-process. Upgrading bauxites by the caustic extraction of silica has been investigated6 and is the subject of a German patent.7 Although mention is made by Roe' of the caustic extraction of silica from low grade Michigan and Wisconsin iron ores, and he lists a number of patents and references on the subject, recent work in the field does not appear to be extensive. As far as the author knows, there has been no work in this field on these particular ores. It is hoped that this paper will stimulate further investigation which will eventually lead to an econclmic means of processing these large low grade reserbes. TACONITES The taconites investigated in this study were from Minnesota and Wisconsin. That from Minnesota, a semi-taconite, Nas obtained from the Oliver Iron Mining Division, U. S. Steel Corporation, and represents a sample of an oxidized iron formation from their King Mine on the Mesabi range. The Wisconsin taconite came originally from the trench sampling of the U. S. Bureau of Mines, and represents a composite of the Norrie, Pabst, Yale, Plymouth, and Pence members of the Gogebic iron formation. Assays on these samples are given in Table I. A typical calcu1atr:d average analysis of the Wisconsin taconite is given in Table 11. Chemically, the Minnesota semi-taconite sample contains about 39 pct iron and 39 pct silica, while the Wisconsin taconite contains 30 pct iron and 53 pct silica, both on the dry basis.

Jan 1, 1962

By R. L. Manegold

IN RECENT years there has been a decided trend toward bringing ores and coal out of open-pit and underground mines by long, sloping single-stage belt conveyors. Because the high investment cost of haulage conveyors dictates maximum speed and full loading for economy, conveyor belts are running faster than ever before, with a greater burden on the belts. In addition, larger blocks of ore are being mined and conveyed. Rougher use of large mining equipment generates more tramp iron; mechanical loading rejects nothing. Therefore the extraction of tramp iron and other deleterious materials for the protection of haulage conveyors at transfer points, chutes, and idlers is becoming an increasingly difficult job. In our experience, the best method of protecting long haulage conveyor belts is to extract the tramp iron, at least the large tramp iron, ahead of the main haulage conveyor or series of conveyors. It is most practical to collect the tramp iron at the earliest source -possible, usually directly after the primary car unloading dump or after the primary crushers, which are ordinarily not affected by tramp iron, see Fig. 1. The coal or ore from its primary source is fed by chutes or feeders onto a buffer or shock belt conveyor, a short, ruggedly built conveyor system that can be considered somewhat expendable. Its primary function is to bring the ore up to speed for transmission to the haulage conveyor. There is no assured method of protecting this conveyor from tramp iron damage at its feed end. Likewise, there is a possibility, although remote if the magnet applied to this belt is installed correctly, that the tramp iron extraction process will damage the shock belt, which is, however, short and comparatively inexpensive. Magnetic head pulleys with their maximum effective range of about 8 or 10. in. cannot be considered for large installations, even though they are desirable because of the continuous and, automatic tramp, iron removal feature. Further, the most dangerous form of tramp iron with respect to potential damage to a haulage conveyor is the long rod, roof bolt, or rail segment, which is not extracted satisfactorily because of the limited tangential contact of such an iron shape with the magnet. Magnetic head pulleys are also undesirable because the dribble or fines from the head pulley discharge at the same point as the tramp iron. Screens must be used to separate the fines from the magnetics, resulting in additional expense and loss of head room. Magnetic detectors have been used with success, but they only indicate the, presence of iron, and the conveyor belt must be stopped for its manual removal. The, stoppage of any conveyor means that all preceding equipment must be stopped or a cascade of material on the idle conveyor will result. Occasionally combinations of detectors and magnetic, head pulleys are used. The detector precedes the magnetic head pulley and detects only large pieces of tramp iron, while the magnetic pulley subsequently takes out the smaller ferrous metals. Suspended magnets overcome the disadvantages of magnetic head pulleys, detectors or a combination of both. There are several magnetic extraction problems involved in applying a suspended magnet at this

Jan 1, 1952

By D. B. Jugle, J. B. Darby

The equilibrium solubility limits of the transition elements Ti, V, Cr, Fe, and Co in liquid tin were determined in the temperature range from 827" to 1211°K. Since the equilibrium concentration of Ti, V, or Cr in liquid tin is moderately dilute in the temperature range investigated, the solubility data were employed to estimate the partial molar enthalpy and the partial molar excess entropy of solution for the three solutes in liquid tin. The reference state s for titanium or vanadium were selected relative to the solute in an intermetallic compound. The thermodynamic quantities for chromium were calculated relative to pure chromium. RECENT experiments1 have shown that the rate of solution of several transition elements in liquid aluminum can be qualitatively predicted from a knowledge of the temperature dependence of the solvent-rich liquidus. In order to extend the analysis to binary tin systems,' it was necessary to know the equilibrium solubility of several of the first-long-period transition elements in liquid tin. Since solubility data for the tin-rich portion of binary systems are meager, the present investigation was undertaken to determine the equilibrium solubility limit of Ti, V, Cr, Fe, and Co in liquid tin in the temperature range from 850" to 1200°K. EXPERIMENTAL PROCEDURE A useful technique3 to determine the equilibrium solubility of a solute in a liquid-metal solvent consists essentially of placing a pure solute in contact with a pure solvent and allowing sufficient time for equilibrium to be attained at the temperature of interest. Subsequently, the solvent is removed and the equilibrium solute concentration in the solvent is determined by an appropriate analytical procedure. The technique can be applied very successfully to relatively simple systems such as the copper-germanium system.3 However, in many binary systems of transition elements with tin, several intermediate phases are known to exist and precipitation of the phases from solution, in solubility experiments, can lead to an erroneously large solubility. The difficulty was avoided in the present work by equilibration of the most solvent-rich intermediate phase with the pure solvent over a range of temperatures. The compounds employed in this investigation, and the temperature range over which each compound is in equilibrium with liquid tin are listed in Table I. No stable intermediate phases are reported in the chromium-tin system4 and, therefore, pure chromium was utilized as the solute. The stoichiometric compounds were prepared by arc-melting on a water-cooled copper hearth in a helium-argon atmosphere. The elemental tin employed in.this investigation was 99.998 pct pure, and typical lot analyses of the transition elements were reported elsewhere.' A sample of an appropriate solute, in the form of a button and in sufficient quantity to exceed the equilibrium solubility, and the pure tin solvent were placed in a high-purity recrystallized-alumina crucible. The crucible and contents were placed in a horizontal furnace under a high vacuum (10-6 torr) and held at temperature for periods varying between 24 and 72 hr. A water-cooled quench tank, partially filled with diffusion-pump oil, was attached close to one end of the

Jan 1, 1970

By N. E. Grosvenor

Several methods have been proposed for determining the tensile strength of rock. These have been tried out over the past several years, but the results have been erratic and of doubtful value. The tensile strength of rock is its weakest property, and this property apparently enters into all failure phenomena, whether underground or on the slope of an open pit. Therefore, it is essential that detailed quantitative information is known about the tensile strength of rock if the design engineer is going to select the proper pit slope, pit orientation, or orientation of underground workings so as to give the most economical and safest mining condition. This quantitative information may be used to orient the pit in such a manner as to allow steep slopes along two sides. This information possibly may be used to orient the direction of either underground workings or open pits so as to decrease powder consumption and to increase blasting efficiency. Hence it is of prime importance that a method of determining accurately the tensile strength of rocks be developed. The U. S. Bureau of Mines states' that no standard methods have been proposed by the ASTM for testing the tensile strength of rock. The method described in the Bureau publication is said by them to be unsatisfactory. A similar test that has been used in our laboratory in place of the USBM test is shown in Figs. 1 and 2. h this test the core is placed in a set of grips that has been designed for one particular size core. The grips are designed to distribute the stress around the core if they are tightened correctly. A universal joint or a flexible cable may be used in conjunction with the apparatus to prevent bending or twisting of the specimen. The main difficulty encountered with the system shown is the failure of the specimen within the grips. The possible cause of the failure within the grips may be due to a stress concentration set up by the uneven tightening of the grips. This method can be used only for tests on cores, and even then has been found to be totally unsatisfactory because of the failure within the grips. The U. S. Bureau of Reclamation has been using a test similar to the sketch shown in Fig. 3. Sulfur is cast around each end of the specimen to form a bearing surface and then a ring grip is used to apply a tensile stress. The grips are in contact with the sulfur cast and do not touch the specimen. This method is unsatisfactory, apparently because a large number of the specimens appear to break within the sulfur cast. Professor Wuerker of the University of Illinois uses the test shown in Fig. 4.' Professor Wuerker states2 that this method has given definite and reproducible results with the weakest as well as with the strongest rocks. The test is a supplement in all cases where cores cannot be obtained. The principle and equipment are the same as for the test for tensile strength of hydraulic-cement mortar. Soft

Jan 1, 1961

By H. L. Gilbert, H. A. Johansen, R. G. Nelson

High purity electrolytic chromium plate has been hydrogen-reduced and arc-melted under inert atmosphere to give sound ingots. These ingots may be hot forged to break the as-cast structure and then worked at 500°C to finished form. An intermediate and final high temperature anneal gives best ductility and grain refinement. HE increasing interest in refractory metals for I use in high temperature gas turbines, jets, and rockets has led to great efforts in exploiting the fifth and sixth groups of transition elements. Much of the interest has centered upon production of metals that can be worked and fabricated by normal means to produce various engine parts or components having the high temperature characteristics of oxidation resistance and high creep strength required for such uses. If these pure elements do not exhibit all of the desired characteristics, it may be possible to obtain a high purity alloy that will. Since, in all cases, development of these transition elements has depended to a large extent upon removal of oxygen and nitrogen as a means for producing ductile metal, the hypothesis has been accepted that oxygen is the normal embrittling material in a high grade electrolytic chromium metal. Various methods have been employed in an effort to remove this oxygen by direct or indirect attack.' Many workers have endeavored to produce pure chromium through reduction of the oxide by carbon or active metals, while others have recommended fusion electrolysis of chromium salts or reduction of these salts by active metals, such as sodium or calcium. Hydrogen reduction of the oxide or chloride and thermal dissociation of the iodide have been reported to give high purity metal. Experimental Work The U. S. Bureau of Mines, Northwest Electro-development Laboratory, has systematically re-examined the more promising methods and developed two which produce metal having ductility at temperatures lower than heretofore described. It has been found' that oxide-free chromium chlorides in a NaCl-KCl carrier salt may be mag- nesium-reduced and the byproduct salts distilled off in vacuo to give a high purity chromium sponge. Fusion analysis conducted under the supervision of W. W. Horton of Knolls Atomic Power Laboratory showed the oxygen and nitrogen both to be below 10 parts per million on a selected sample. A small amount of carbon is carried over in the final metal from the chlorination and reduction steps which are carried out in graphite crucibles. This trace of carbon is not detrimental to hot ductility. A more practical method for producing ductile metal is through hydrogen reduction of high purity electrolytic chromium. Normal electrolytic chromium will, if "developed" for a few minutes at 1100°C in high vacuum, be found by the method of Adcock:; to contain about 1 pct chromium sesquioxide (Cr2O3). This small amount of oxygen may be effectively reduced by hydrogen.2, 4 The method employed was to crush electrolytic chromium plate in a gyratory crusher to pass 60-mesh; finer crushing appears to offer no advantage. A nitric acid leach removed the iron picked up during crushing. The leached powder was rinsed until neutral with distilled water and vacuum-dried.

Jan 1, 1954

By A. A. Burr, D. Caplan

IN carrying out experiments in metal-gas systems, it is often difficult to estimate how long a reaction period must be allowed for equilibration. This is especially true in systems for which the diffusion coefficient is not known. In an investigation of the Cr-O system, the necessary information was obtained in the way described subsequently. Two pieces of chromium sheet of different thicknesses were packed in mixed powders of chromium and Cr2O3 and sealed into an evacuated metal capsule by welding. Austenitic stainless steel proved suitable as a capsule material up to 1350°C and molybdenum at higher temperatures. The capsule then was heated at a specific temperature for a time sufficient to saturate with oxygen the thinner but not the thicker specimen. The time is readily estimated from a preliminary experiment if a sufficient thickness differential is chosen. Under these experimental conditions, the metal sheet is exposed to a partial pressure of oxygen equal to that of the dissociation pressure of the oxide and hence can become saturated with oxygen without developing any second phase. After cooling, both samples were analyzed for oxygen by the vacuum fusion technique. Assuming that the surface of the specimens is kept saturated with oxygen throughout the experiment, the diffusivity can be calculated by application of the appropriate solution to Fick's second law. This is most conveniently accomplished by use of a plot of mean fractional saturation (Cm-Co) / (Cs-Co) vs (Dt) ½/L as given by Darken,' where t is time, L the half-thickness of the sheet, and D the diffusion coefficient. Cm, the mean concentration at time t, is given by the oxygen percentage in the thicker specimen; Cs, the constant surface concentration, is the oxygen percentage in the thinner specimen; Co is the oxygen content of the original chromium sheet. (Cm-Co) / (Cs-Co) is calculated and the corresponding (Dt) ½/L is read from the graph and D thereby calculated. By performing the experiment at two temperatures and plotting log D vs 1/T, the D for any temperature is established. (The activation energy for diffusion may be obtained from the slope of the line.) Once D is known as a function of temperature, it is a simple matter to estimate the correct reaction time for experiments with single specimens at other temperatures by equating (Dt) ½/L to its value for effective saturation. Darken' points out that this is approximately unity. The solubility of oxygen in chromium, as determined from the thin samples at each temperature, proved to be approximately 0.03 pct at 1350°C and less at lower temperatures. Due to low solubility and to the known difficulties of the vacuum fusion method in this low range, the values obtained for D (5x10-0 sq cm per sec at 1350°C) are estimated to be correct only within an order of magnitude. Nevertheless, the method has proved useful in estimating reaction times. Its usefulness will be greater in metal-gas systems where the solubility is appreciable. A second function of the method is to permit the determination of diffusion coefficients in systems for which the conventional techniques are experimentally difficult or impossible.

Jan 1, 1956

By W. M. Fox, D. P. Detwiler

IN the course of research on semiconducting inter-metallic compounds, it became necessary to obtain gallium metal of greater purity that that available commercially. Several methods were considered for further purification, including acid leaching,' fractional crystallization,' and zone-refining.3-5 The method of fractional crystallization was discarded as being equivalent to zone-refining in purification but inefficient in material and time. Both acid leaching and zone-refining were tried, and the method finally adopted is a combination of the two. The acid leaching technique has been reported' to produce gallium in which no impurities are detectable spectroscopically. Although this method is very effective in removing oxides and surface contaminants, semiconducting material made of gallium subjected only to leaching indicated little reduction in the concentration of metallic impurities. Zone-refining, however, appears very effective in removing trace metallic impurities, but comparatively ineffective in removing the surface oxide film. Consequently, the method evolved consists of acid leaching to thoroughly clean the surface, followed by zone-refining to remove metallic impurities. The low melting point and relatively high thermal conductivity of gallium introduce some difficulty in maintaining frozen and molten zones in zone-refining. To accomplish this, it is found necessary to reduce the effective ambient temperature by circulating ice water in coils about the regions that are to be kept frozen, while heat is supplied to the molten regions by resistance coils. The power supplied to the heating coils is regulated by a constant-voltage transformer and a variable autotransformer. Both heating and cooling coils are mounted on a transite base. The gallium ingot is held in a closed pyrex tube sliding inside the heating and cooling coils, the reciprocating method of Tanenbaum et al. being employed to move the molten zones through the ingot at a rate of 2 in. per hr. This apparatus is shown in Fig. 1. The results of a spectroscopic analysis f a zone-refined ingot, as well as of the material as-received and after acid leaching, are shown in Table I. The ingot was 32 cm in length, and received 37 molten-zone passes, the molten zone being about 4 cm long. The only impurity found was lead, the following elements being reported also as checked but not found in the pure material: Al, Sb, As, Ba, Be, Bi, B, Cd, Ca, Cr, Co, Cb, Cu, Ge, Au, Fe, Mg, Mn, Mo, Ni, Pt, Si, Ag, Na, Sr, Sn, Te, Ti, W, V, Zn, and Zr. There thus appears no indication of pickup of Al, Mg, or Si from the pyrex boat as reported by Zimmerman' in his fractional crystallization. Thus it appears that definite removal of lead from gallium occurs during the zone-refining process. It also may be concluded that a more sensitive analytical procedure than spectroscopy is required to evaluate quantitatively the purity of zone-refined metals. One such procedure which is proposed for use in the near future is the measurement of very low temperature resistivity. Although this will not identify the impurities present, it offers a very sensitive check of total impurity. Acknowledgment This work was supported by the Air Research and Development Command, United States Air Force.

Jan 1, 1956

By E. H. Crabtree, Neil S. Parker

The custom milling plant of the Eagle-Picher Mining and Smelting Co. is at Sahuarita, Arizona, approximately 20 miles south of Tucson. It is connected by a 2-mile railroad spur to the main line of the Southern Pacific Railroad between Tucson and Nogales. The capacity of the plant is 500 tons per day. The mill is conventional except perhaps in the rather wide variety of ores treated. These vary from straight copper ores, from which only one concentrate is produced, and lead-zinc or copper-zinc ores from which two concentrates are produced, to complex gold-silver-copper-lead-zinc ores, which require the simultaneous production of three or lour concentrates. Custom ores are received in lots varying in size from a few truckloads to several carloads. Similar ores, after crushing and sampling, may be commingled, or individual lots may be milled individually. The ores are first dumped either into one of two 200-ton railroad bins, or into one of the two 75-ton truck bins. From these bins the lot of ore is individually crushed in a 24 by 16-in. jaw crusher to 3-in. size, and then to ½-in. size in a 3-ft Symons shorthead crusher. After crushing to ½-in., the ore is conveyed to the automatic sampling plant. This consists of three Vezin samplers in series, each successively cutting out 10 pct, 10 pct and 5 pct of its feed. After No. I sampler, the material passes through a mixing barrel and is then crushed to -in. in a set of rolls before passing to No. 2 sampler. Between No. 2 and No. 3 samplers, the ore is again mixed in a mixing barrel. The final sample, consisting of one pound per ton of ore, is taken to the laboratory, where it is further crushed to 1/8-in. in a coffeemill, and then riffled down to the size required for grinding in a pulverizer. The capacity of the crushing and sampling plant is up to 100 tons per hour, depending upon the character of the ore. After sampling, the ore is stored in five ore-storage bins, consisting of four 200-ton bins and one 175-ton bin. Each of these bins is discharged by means of belt feeders and conveyor to the ball mills, so that ores may be composited for milling in any required ratio, or milled separately by themselves. Fine grinding is done in one 6 by 4-ft Allis-Chalmers ball mill and one 8-ft by 36-in. Hardinge mill. These two mills both discharge to one 54-in. Akins Simplex High weir classifier. The classifier sands can be returned to either or both mills, so that flexibility in grinding for different ores is easily obtained. Flotation equipment consists of four 66-in. Fagergren machines for copper-lead roughing and six similar machines for zinc roughing. Lead-copper bulk concentrate is cleaned and recleaned in eight No. 18-S Denver machines, and zinc concentrate is cleaned in three 66-in. Fager-grens. Copper-lead differential separation

Jan 1, 1949

By B. Otto Pixler

Mud-analysis logging provides identification of the fluid content of formations drilled by the rotary method and permits the accurate correlation of oil and gas shows with the depth. Mud-analysis logging eliminates much coring and has an especially important application in drilling programs when coring is particularly hazardous or the electric log is difficult to interpret correctly. An appreciation of the factors that influence the results of the mud analysis, such as rate of penetration, mud properties, coring, and characteristics of reservoir rock as related to the "flushing effect," permits a better understanding of the mud-analysis log. Recent studies of the relationship of the two gas readings obtained by the gas-detector instrument have proved significant. The difference between the total combustible gas reading and the higher molecular weight gas reading indicates the presence of methane. With few exceptions, zones not showing an increase of methane probably can be condemned. Mud-analysis logging furnishes valuable information, which generally cannot be obtained by other methods. Introduction Logging by mud analysis of wells drilled with rotary tools is a direct method of locating oil-and-gas-bearing formations. The use of this method of logging has increased each year until now more than 20 field units are being used in 13 oil-producing states and in some foreign countries. Several papers1-9 have been published in the petroleum trade journals describing in detail the equipment and the application of mud-analysis logging. This paper will discuss briefly the method and review its application and some of the late developments. Method As the drilling of a well progresses, the drilling bit dislodges and disintegrates a cylindrical section of the formation. If oil or gas is contained in the pore spaces of the cylinder, some of the contents of these porous spaces will be entrained in the drilling fluid. In wall logging by mud analysis, the mud is continuously examined for oil and gas on its return to the surface, and the results are correlated back to the actual depth of the hole at the time the mud was clearing the eyes of the bit. The test for gas is made by diverting a portion of the circulating mud from the flow line to a separator or gas trap, where the mud is thoroughly mixed with air and a portion of the gas entrained in the mud is removed. A stream of air is drawn coun-tercurrent to the flow of mud in the gas trap, thus materially assisting the separation of the gas from the mud. The air-gas mixture is then drawn into a "hot-wire" gas-detector instrument where the percentage of the combustible gas is determined. The presence of oil in the formation drilled is detected by a physical examination of the drilling mud under ultraviolet light. A sample of the mud is treated to reduce the surface tension and gel strength, after which it is placed in a viewing box. This box is so constructed that all external light is excluded and so that the sample may be subjected selectively to either ultra-

Jan 1, 1946

By Charles C. Rodd

PRIOR to 1938, proration procedure in Kansas required the physical testing of wells in order to set up a basis for allocating production. Subsequently the use of liquid-level data and bottom-hole pressure data was authorized on certain types of wells as a basis for calculating well capacities, thereby permitting wells to be tested at low rates and with small volumes of production. This paper gives some attention to the equipment used for obtaining liquid-level data but in general it is devoted to the theoretical and physical factors involved in well testing by drawdown methods. These tests are divided into two classifications: (1) liquid-level data used directly to calculate capacities, and (2) liquid-level data and liquid-level measuring equipment used in connection with other data to determine bottom-hole pressure. Equations and calculations for both types of tests are shown. Well capacities calculated from fill-up data have not been used generally but offer a simple means of testing some wells. Theoretical factors and calculations for such tests are shown. IN the state of Kansas, proration laws required that the "ability of a well to produce" be given consideration in state allocation orders and for many years this was the only factor used in prorating the allowed oil. The "ability of a well to produce" was the quantity of oil that could be obtained from a well in a prescribed period, usually 24 hr. Early in the history of State-regulated proration, Kansas operators realized that, unless some restriction were placed upon equipment, the competition between producers to obtain large well "potentials" might result in a race to install the largest pumping equipment. Consequently, restrictions were placed upon the size of tubing and length of pump stroke that could be used in pumping wells during potential tests. Later, restrictions were placed also upon the size of tubing and chokes that could be used in flowing walls. Despite the restriction set-up, better pumping equipment was designed and installed, pumps were improved, and various devices were invoked to obtain high rates of production for short periods of time. By 1937 pumping cycles of forty to forty-five 54-in. strokes per minute were not uncommon, and numerous wells had produced at the rate of 3500 bbl. per day for short periods. Such production was far beyond any rate that could be long sustained. Equipment necessary to take "potentials" was several times larger than that needed for normal producing purposes, and repairs and replacements required by the high pumping speeds were excessive. Also, many operators were beginning to suspect that the high rates of production maintained during "potential" tests were conducive to early water encroachment. By 1938 large-scale physical testing of wells in Kansas ended, the use of the bottom-hole pressure gauge had become common, engineers and operators were becoming familiar with the term "productivity index," and bottom-hole pressure was being used as a factor in allocation in many areas. There were many drawbacks, however, to large-scale use of

Jan 1, 1942

By E. A. Gulbransen, J. W. Hickman

Recent work by the authors1 on the oxide films formed on alloys of titanium and zirconium with nickel and copper indicated that an investigation of the oxides which form on alloys of copper and nickel might permit the relative rates of formation and diffusion of the ions of these metals to be determined. This binary system is of further interest since the alloys which form are of the solid solution type over the entire range. In addition nickel is much more oxidation resistant than copper. A comparison of the free energies of formation of the simple oxides which may occur on these alloys indicates that nickel oxide should be observed over the entire time and temperature ranges of oxidation for all alloy compositions~i In order for nickel oxide to predominate on the surface, it is necessary that nickel ions form and diffuse to the surface. Two factors which may influence the formation of nickel oxide may be the ionic sizes, where cu+ is o.,,6-,4 and ~i++ is o.,oh;, and the charges on the ions. On the basis of size, Ni++ should diffuse more readily than Cu+ while on the basis of charge, Cu+ should form more readily than Ni++. According to Uhlig2 passivity to corrosion in an alloy appears at a critical composition which for copper-nickel alloys is related to the tendency of the d band of electronic energy states to fill with elec-trans. This in in the copper- nickel alloys corresponds to 40 at. pct nickel at which composition Uhlig2 (quoting La Que's data) states that the alloy system becomes passive. Magnetic and specific heat data indicate that the d band of copper-nickel alloys is flied at 60 at. Pet Or or 4O at. pct nickel. Matt and Jones3 have shown that if, on alloying nickel with copper, one considers a copper atom to be identical with a nickel atom except for an extra electron (nickel has the configuration: 3ds 4s2 and copper: 3 dl0 4s) then at 60 at. pct copper or 40 at. pct nickel enough electrons are contributed by copper to fill the d band of the alloy. At this composition the magnetic susceptibility approximates zero according to Grew.4 Although the electron diffraction data will not determine the rates of the several reactions which may occur during oxidation, yet a determination of the structures of the surface oxides may yield information concerning the relationships, if any, which may exist between the oxide structures which form and that composition where the magnetic susceptibility approximates zero. It is quite possible, of course, that the mechanisms of the oxidation and corrosion reactions may be so widely different that no correlations between them may be possible. Survey OF Literature The metals, copper and nickel, which are face-centered cubic, form solid solution alloys which are face-centered cubic with no superstructure for all compositions. Three oxides of nickel have been investigated structurally by X ray diffraction. Of

Jan 1, 1949

By A. Lee Barrett

MINE power systems are quite different in many respects from those usually found in industrial plants. Wide areas are served, usually by a circuit which is connected continuously throughout the mine. In some mines one circuit may run for several miles. There are usually a small number of branch circuits involved considering the areas covered. In all mines circuits are sectionalized at approximately 2500 ft by means of switches. All, or at least most branch circuits, are sectionalized by manual switches. In some mines automatic sectionalizing gear is used to give automatic overload protection at various strategic points in the system. However at the present time this practice is by no means general. Circuit hazards in mine electric systems are much greater than those encountered in industrial installation. Falls of roof or coal form a prominent hazard which may break the wire and may cause ground faults or partial ground faults. Ordinarily electric cables in mines cannot be insulated, there- fore n fall can easily cause a short circuit. The humidity in most mines is greater than 95 pct and at many points the floor is wet and water may be dripping from the roof over insulators, increasing the difficulties at that point. All electrical circuits must be contained in the mine entries and space must also be provided for moving equipment and men. Consequently, because of the proximity of the power circuit to the locomotives and other moving equipment a considerable hazard is introduced. Mine haulage track is not always good so that wrecks are not unusual. A wreck frequently does consider- able damage to the power circuit. A ground fault frequently results in heavy arcing which may be sustained. If the damage to the circuit is mechanical it may mean that a trip of coal has wrecked and a great deal of coal dust could be thrown into the air as a result of the wreck. The arc resulting from the ground fault could ignite the coal dust and a mine explosion would result. A continued ground fault, even if high in resistance, also may ignite the coal which may be on the bottom of the entry and a mine fire may result. The fire hazard is one of the most serious hazards in any coal mine. Since the mine circuit is completely interconnected, any power interruption resulting from a fault seriously affects the whole operation. Unless the mine is completely sectionalized the whole mine will be shut down until the fault is located and the proper switches are opened to isolate the fault; even then large areas may still be without power if they are supplied by a single power circuit which may be opened in isolating the fault. Further, mine power is usually supplied from a relatively small number of substations and the fault may be on a stub feed circuit, in which case power cannot be restored until the fault has been cleared. Practice varies widely with respect to placement of substations. Usually they will be spaced from I to 2 miles in 500V operations, and at 1 mile intervals or less, in 250 V operation. Actual mining operations govern substation placements and no general rules can be followed.

Jan 1, 1948

By B. Otto Pixler

Mud-analysis logging provides identification of the fluid content of formations drilled by the rotary method and permits the accurate correlation of oil and gas shows with the depth. Mud-analysis logging eliminates much coring and has an especially important application in drilling programs when coring is particularly hazardous or the electric log is difficult to interpret correctly. An appreciation of the factors that influence the results of the mud analysis, such as rate of penetration, mud properties, coring, and characteristics of reservoir rock as related to the "flushing effect," permits a better understanding of the mud-analysis log. Recent studies of the relationship of the two gas readings obtained by the gas-detector instrument have proved significant. The difference between the total combustible gas reading and the higher molecular weight gas reading indicates the presence of methane. With few exceptions, zones not showing an increase of methane probably can be condemned. Mud-analysis logging furnishes valuable information, which generally cannot be obtained by other methods. Introduction Logging by mud analysis of wells drilled with rotary tools is a direct method of locating oil-and-gas-bearing formations. The use of this method of logging has increased each year until now more than 20 field units are being used in 13 oil-producing states and in some foreign countries. Several papers1-9 have been published in the petroleum trade journals describing in detail the equipment and the application of mud-analysis logging. This paper will discuss briefly the method and review its application and some of the late developments. Method As the drilling of a well progresses, the drilling bit dislodges and disintegrates a cylindrical section of the formation. If oil or gas is contained in the pore spaces of the cylinder, some of the contents of these porous spaces will be entrained in the drilling fluid. In wall logging by mud analysis, the mud is continuously examined for oil and gas on its return to the surface, and the results are correlated back to the actual depth of the hole at the time the mud was clearing the eyes of the bit. The test for gas is made by diverting a portion of the circulating mud from the flow line to a separator or gas trap, where the mud is thoroughly mixed with air and a portion of the gas entrained in the mud is removed. A stream of air is drawn coun-tercurrent to the flow of mud in the gas trap, thus materially assisting the separation of the gas from the mud. The air-gas mixture is then drawn into a "hot-wire" gas-detector instrument where the percentage of the combustible gas is determined. The presence of oil in the formation drilled is detected by a physical examination of the drilling mud under ultraviolet light. A sample of the mud is treated to reduce the surface tension and gel strength, after which it is placed in a viewing box. This box is so constructed that all external light is excluded and so that the sample may be subjected selectively to either ultra-

Jan 1, 1946

By R. C. Rumble

To /neet the need for a subsurface flowmeter capable of measuring low rates of flow, a new type flowmeter has been built and tested in the field. This instrument is self-contairzed, can be run on a wire measuritzg line, and may be run through 2-in tubing. It consists of a rotameter flow-measuring assembly used in conjuncfion with a conventional subsurface instrument clock and chart. Integral with the tool is an inflatable packer which, by effecting a seal between casing and tool, diverts all fluid through the metering assembly. Packers of different size adapt the tool to different sizes of casing or liner. The flowmeter is capable of measuring rates of flow as low as 4 BID. The flowmeter has been run experimentally in seven wells. It has yielded satisfactory resrrlts in five of the wells, and in the other two it failed to operate because of loose sand in the hole. INTRODUCTION One of the oldest problems facing the producing branch of the petroleum industry is the location of depths of entry of fluid into a wellbore and the determination of the amount of fluid entering at each depth. This problem is often encountered in oil and gas wells completed in single producing horizons as well as in multiple pays; it is a common problem in oil wells which produce excessive volumes of gas. Several subsurface instruments designed to detect and meter flow in the producing interval of wells have been described in the literature.1,2,3,4 Most of these, however, were apparently intended for use in wells producing at relatively high rates of flow, and consequently lack sensitivity to low flow rates. Because of this and of other possible disadvantages inherent in these instruments, development of the subsurface flowmeter described in this report was undertaken. DESIGN OF FLOWME'I'ER Design Requirements In considering the requirements for a flowmeter that would not be subject to the limitations of devices existing at the time work was started, attention was first given to the size of the tool. Such an instrument should be of sufficiently small diameter that it could be lowered readily in 2-in tubing in a producing well. The flowmeter should contain a recording unit so that it might be run on a wire measuring line with conventional reeling equipment. It should not be too long to be accommodated by a portable lubricator of the type used for running conventional subsurface instruments. The metering mechanism of the flowmeter should not be affected appreciably by the viscosity or density of the flowing fluid. Such an instrument should record flow rates in the range from less than 10 B/D to over 100 B/D. To achieve this, a packer should he provided to divert through the instrument all fluid flow in the wellbore. This packer should be of such nature that in the event of excessive flow the fluid would bypass the instrument instead of forcing it up the wellhore. General Description A flowmeter incorporating most of the desired features outlined above was developed and built. The instrument is an elongated tubular device terminated on

Jan 1, 1956

By Franz Fohr

On July 27, 1919, there passed away a simple, unassuming gentle-man, who, throughout his life, allowed his intense modesty to keep him-self in the background and during his later years effaced himself so thoroughly that but few of his acquaintances knew aught of him. Yet he was one of our accomplished metallurgists, who did good work in the practice of his profession and lived an upright life. Now that he is no longer with us Franz Fohr cannot plead to be overlooked, and those who fondly remember him will be gratified by his receiving his due. Franz Fohr was born, Sept. 7, 1838, in Mannheim, Germany. Of his ancestry, education, and early career we know scarcely anything. We do not even know just when he came to America, or. what led him hither. The first record of his professional work in this country, found among his papers, shows that from July, 1870, to Jan. 1, 1872, he was superin-tendent of the Newark Smelting & Refining Works, then owned by Ed-ward Balbach & Son. At that time the Balbach works at Newark, established in 1850, and the Selby works at San Francisco, established about 1866, were the only important silver-lead refineries in the United States. Mr. Fohr may have been associated with the Balbachs for some time before he became superintendent of their plant or he may have come from Germany but a short time previously. At all events, it is certain that he was at that time an experienced and accomplished metallurgist. After leaving Newark and going to San Francisco, he soon formed a connection with Thomas H. Selby & Co. Early in 1874-this firm sent him to New York to procure information respecting the manufacture of white lead. His engagement in New York terminated on-Jan. 31, 1875. During 1875, Mr Fohr spent some time at Silver Islet and in the Lake Superior copper region, but of his work there no record remains. In the latter part of 1875, or early in 1876, he associated himself as metallur-gist with the Boston Silver Co., operating at Saint John's, Summit County, in which William L. Candler, of Boston, was the moving spirit. That company was developing its mine in 1875. At the end of that year it "had about 800 tons of ore on hand, about three-fourths of which is dress-ing ore, to be concentrated in its very systematic establishment and to be smelted into pig lead." Evidently Mr. Fohr was engaged for the latter purpose. Henry A. Vezin, erudite and painstaking, was the mechanical engineer for the company. In the fall of 1876, Anton Eilers took his family for the first time so far West as Denver and Mr. Fohr went with them. I do not think that Mr. Eilers had any connection with the Boston Silver Co., save possibly in a consulting capacity, but he visited Saint John's and the enduring friendship among Eilers, Fohr, and Vezin, which terminated only with their deaths, dated from that time.

Jan 12, 1919