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By A. U. Seybolt

The solubility limit of oxygen in columbium has been determined in the range between 775' and 1100°C by means of lattice parameter measurements and microscopic examination. The solubility is a function of temperature and varies, in the range given above, from 0.25 to 1.0 pct O, respectively. BECAUSE of the marked deleterious effect of oxygen upon the mechanical properties of some of the transition metals, it is desirable to know something about the solubility of oxygen in these metals. The brittleness caused by oxygen in solution is particularly marked in the case of the group VA elements, vanadium, columbium, and tantalum. The solubility of oxygen in vanadium has already been reported in an earlier paper,' and Wasilewski2 has given a value (0.9 wt pct) for the solid solubility of oxygen in tantalum at 1050°C. Brauer3 in 1941 investigated the Cb-0 system up to Cb2O5, but made no real effort to investigate the extent of oxygen solubility in the metal. He made the observation, however, that this solubility must be less than 4.76 atom pct (0.86 wt pct) oxygen. This estimate was made from X-ray diffraction results on the alloys CbO, CbO, and CbO; all alloys consisted of the terminal (Cb) solid solution plus CbO, but the last alloy containing 4.76 atom pct 0 showed only three very weak CbO lines. It is surprising that Brauer, by examining only three alloys, arrived at an estimate of the solubility which agrees very well with the results to be reported herein. Experimental Procedure A columbium strip obtained from Fansteel Metallurgical Products was cut into strips, 0.020x1/2x2 in. Two holes, about 3/16 in. in diameter, were made near the ends of the strips in order to hold them against a flat steel block for mounting in a General Electric X-ray spectrometer for lattice parameter measurements. The same holes were used to hang the specimens inside a fused silica vacuum furnace tube which was part of a Sieverts' gas absorption apparatus. The apparatus and method of adding oxygen gas has been previously described.1 According to the supplier, the columbium obtained had the analysis given in Table I. After degreasing the samples, approximately 0.001 in. was etched from each side of the samples in order to remove possible surface impurities from the last rolling operation. For this purpose the following cold acid pickle was found satisfactory: 8 parts HNO3, 2 parts H2O2 and 1 part HF. Various Cb-O compositions were obtained up to 0.75 wt pct O by the gas absorption and diffusion technique. After the sample had absorbed all the oxygen gas added at 1000°C, an additional 24 hr was allowed for homogenization. This treatment appeared to be adequate, as shown by the linearity of the lattice parameter-composition plot. More concentrated alloys were prepared by arc melting mixtures of Cb and Cb2O5 since it was very time-consuming to make Cb-0 alloys in the neighborhood of 1 pct O, or over, by the diffusion method. When the flat strip specimens were used, they were ready for the X-ray spectrometer after cooling from the Sieverts' apparatus. The cooling rate obtained by merely allowing the hot fused silica furnace tube to radiate to the atmosphere (when the furnace was lowered) was sufficiently fast to keep the dissolved oxygen in solution. Arc-melted alloys were reduced to —200 mesh powder in a diamond mortar, wrapped in tantalum foil, sealed off in evacuated fused silica tubes, and then heat treated as indicated in Table 11. The fused silica tubes were quickly immersed in cold water without breaking the tubes after the heat treatments. The tantalum foil prevented reaction between the fused silica and the sample; there was no reaction between the powdered samples and the foil at 1000°C, but some trouble was experienced at 1100°C. At this temperature level a reaction between the sample and the foil was sometimes observed, which resulted in erroneous parameter values. Experimental Results Hardness Tests: Since most of the X-ray samples were in the form of flat strip, it was convenient to obtain Vickers hardness numbers as a function of oxygen content. Compared to the V-O case,' oxygen hardens columbium much more slowly, presumably because of the larger octahedral volume in colum-bium (about 12.0 compared to 9.3Å3 in vanadium), hence, requiring less lattice strain for solution. The plot of VHN vs wt pct O is shown in Fig. 1.

Jan 1, 1955

By L. W. Bahney

FREQUENTLY in using a thermo-electric pyrometer for measuring the temperature of a furnace, a hole is drilled at the back or side of the furnace, through which is introduced the tube containing the thermo-couple. At times the couple is left almost where it drops, for the reason that it soon becomes too hot to be handled easily, and the space at the back or side of the furnace may be so small and uncomfortably hot that an easy and accurate adjustment is nearly impossible. In order to overcome this clumsy and unscientific method of using the thermo-electric pyrometer, I designed an adjustable stand, to hold the clay or quartz tube unclosing the platinum and plati-num-rhodium leads that constitute the couple of the Le Chatelier thermo-electric pyrometer. This stand also allows an easy and rapid adjustment of position to varying heights and angles, as may be desired for special reading. This stand is illustrated in Fig. 1. The couple in the tube might be of better service if the tube were held a little higher above the charge in a roasting-dish, changing the height and angle if desired. The stand, made of 1.5-in, water-pipe and mounted on casters, is heavy enough so it cannot be tipped over easily. It is adjusted to any position, and has a universal clamp which holds the clay or quartz protecting-tube. To avoid disturbing the wires of the couple at the cold junction each time the tube is moved, the cooling-bottle sets in a wire basket so placed that it moves forward or back with the couple. To overcome the necessity of leveling and adjusting a galvanometer at each furnace, a switch-board is used to connect

Jan 1, 1910

By AIME

WELL known as an outstanding practical metallurgist, the Chairman of the Institute of Metals Division also possesses a rare combination of research and administrative abilities. Louis W. Kempf was born in Muskegon, Mich., on March 22, 1898. Following his graduation from high school, he obtained considerable experience in the automobile industry while employed by Continental Motors, the Studebaker Corp., and Dodge Brothers. He enlisted in the U. S. Army Signal Corps in 1917, and served overseas with an aviation unit. In 1919, Mr. Kempf entered the University of Michigan and earned both B.S. and M.S. degrees. While there he was elected to Tau Beta Pi, Phi Lambda Upsilon, Alpha Chi Sigma, and Gamma Alpha. In 1924, the Aluminum Co. of America secured his services as a research metallurgist. With a steady job he married Elizabeth Skelley in Cleveland in 1926. They have one son now seventeen. After six years Mr. Kempf was made manager of the Cleveland research division of the Aluminum Research Laboratories which position he held until last year. In 1945 he was promoted to assistant director of the Laboratories. He will direct research involving process metallurgy in Cleveland and New Kensington.

Jan 1, 1946

By G. Thomas, O. Johari

MEIERAN and Richman' have proposed a method for the determination of electron-diffraction patterns from twinned bcc crystals. It is the purpose of this note to present a general method capable of predicting the positions of all reflections from both matrix and twin regions for all possible orientations of cubic crystals. The method has been verified for twinning in explosively deformed copper, and is found to be a very useful tool when used in conjunction with stereographic projection, and dark-field electron microscopy. Let an isometric crystal be twinned in any (hkl) plane. The twinning can be considered either as a reflection in the twin plane or as a 180-deg rotation about the twin axis. In reciprocal space, the 180-deg rotation about the twin axis would place a given point p, q, Y to a new position P, Q,R, such that both will be equally inclined to the twin axis. This is represented in Fig. 1. If the coordinates of three such pairs of points are determined, the matrix of the transformation can be obtained.' It is also seen that such pairs would satisfy another condition, i.e., the vector [p,q,r] plus the vector [P,Q,R] will yield a multiple of hkl, i.e., the indices of the twin plane, because in isometric systems the axis [hkl] is perpendicular to the plane (hkl). This can be simplified by taking the points along the three axes. If a point h2 + k2 + 12, 0, 0 is taken along the x axis, it is seen that its new indices should be so as to yield a sum 2h2, 2hk, 2hl,i.e., 2h(h,k,1). (Also the points h2 - k2 - 12, 2hk, 2h1, and h2 + k2 + 12, 0, 0 are equidistant from the origin and both points make equal angles with the twin axis, i.e., cos-' h/dh2 + k2 + l2.) Similar operations for the points yield respectively, after the 180-deg rotation about the twin axis. Following the method due to Buerger,' the matrix of the transformation is obtained as follows: Using this matrix the indices of any other point in reciprocal space can be determined. This matrix is much simplified for (111) twinning commonly encountered in fcc metals, since are each equal to —1; hence

Jan 1, 1964

By William D. Klopp, Joseph R. Stephens

A substantial reduction in the 300°F ductile-to-brittle transition temperature for unalloyed chromium was achieved in alloys from systems which resemble the Cr-Re system. These alloy systems include Cr-Ru, Cr-Co, and Cr-Fe. Transition temperatures ranged from -300° F for Cr-35 at. pct Re to -75°F for 0-50 at. pct Fe. The ductile alloys have high grain gvowth rates at elevated temperatures. Also, Cr-24 at. pct Ru exhibited enhanced tensile ductility at elevated temperatures, characteristic of superplas-ticity. It is concluded that phase relations play an importarlt role in the rhenium ductilizing effect. The ductile alloys have compositions near the solubility limit in systems with a high terminal solubility and which contain an intermediate o phase. The importance of enhanced high-temperature ductility to the rhenium ductilizing effect is not well understood although both may have common basic features. CHROMIUM alloys are currently being investigated for advanced air-breathing engine applications, primarily as turbine buckets and/or stator vanes. The inherent advantages of chromium as a high-temperature structural material are well-known1 and include its high melting point relative to superalloys, moderately high modulus of elasticity, low density, good thermal shock resistance, and superior oxidation resistance as compared to the other refractory metals. Additionally, it is capable of being strengthened by conventional alloying techniques. The major disadvantage of chromium is its poor ductility at ambient temperatures, a problem which it shares with the other two Group VI-A metals, molybdenum and tungsten. For chromium, the problem is further amplified by its susceptibility to nitrogen em-brittlement during high-temperature air exposure. In cases of severe nitrogen embrittlement, the ductile-to-brittle transition temperature might exceed the steady-state operating temperature of the component. The low ductility of chromium would make stator vanes and turbine buckets prone to foreign object damage. The present work was directed towards improvement of the ductility of chromium through alloying, with the anticipation that any improvements so obtained might be additive to strengthening improvements achieved through different types of alloying. The alloying additions for ductility were selected on the basis of the similarity of their phase relations with chromium to that of Cr-Re. The reduction in the ductile-to-brittle transition temperatures of the Group VI-A metals as a result of alloying with 25 to 35 pct Re is well established.a4 the temperature range -300" to 750° F. This phenomenon is commonly referred to as the &apos;<rhenium ductilizing effect"; this term is also used to describe systems in which the ductilizing element is not rhenium. Other alloy systems which have recently been shown to exhibit the rhenium ductilizing effect include Cr-Co and c-Ru.= In order to explore the generality of this effect, alloys were selected from systems having phase relations similar to that of Cr-Re, primarily a high solubility in chromium and an intermediate o phase. The following compositions were prepared: Cr-35 and -40Re; Cr-10, -15, -18, -21, -24, and -27 pct Ru; Cr-25 and -30 pct Co; Cr-30, -40, and -50 pct Fe; Cr-45, -55, and -65 pct Mn. Seven other systems were also studied which partially resemble Cr-Re. These systems have extensive chromium solid solutions or a complex intermediate phase, not necessarily o. The compositions evaluated include the following: Cr-20 pct Ti; Cr-15, -30, and -45 pct V; Cr-2.5 pct Cb; Cr-2.5 pct Ta; Cr-20 pct Ni; Cr-6, -9, -12, and -15 pct 0s; Cr-10 pct Ir. The compositions of alloys in these systems were chosen near the solubility limit for the chromium-base solid solutions, since in the Group VI-A Re systems, the saturated alloys are the most ductile. These alloys were evaluated on the basis of hardness, fabricability, and ductile-to-brittle transition temperatures. In addition to the studies of alloying effects on ductility, an exploratory investigation was conducted on mechanical properties at high temperatures in Cr-Ru alloys EXPERIMENTAL PROCEDURE High-purity chromium prepared by the iodide deposition process was employed for all studies. An analysis of this chromium is given in Table I. Alloying elements were obtained in the following forms: Commercially pure powder — iridium, osmium, rhenium, and ruthenium. Arc-melted ingot — titanium and vanadium. Electrolytic flake — iron, manganese, and nickel. Sheet rolled from electron-bearn-melted ingot — columbium and tantalum. Electron-beam-melted ingot — cobalt. Sheet rolled from arc-melted ingot — rhenium. All alloys were initially consolidated by triple arc melting into 60-g button ingots on a water-cooled hearth using a nonconsumable tungsten electrode. The melting atmosphere was Ti-gettered Ar at a pressure of 20 torr. The ingots were drop cast into rectangular slabs and fabricated by heating at 1470" to 2800° F in argon followed by rolling in air. Bend specimens measuring 0.3 by 0.9 in. were cut from the 0.035-in. sheet parallel to the rolling direction. The specimens were annealed for 1 hr in argon, furnace cooled or water quenched, and electropolished prior to testing. Three-point loading bend tests were conducted at a crosshead speed of l-in. per min over

Jan 1, 1969

By Wolfgang O. Gluschke

INTRODUCTION Virtually all countries have general legislation covering most aspects of mining and mineral processing, including investment and tax laws, safety and health regulation, and specific rules applying to exploration reporting procedures. Yet most developing countries negotiate individual agreements with foreign investors for major mineral projects, in particular when all or part of the expected output is exported. Such agreements are known under several different names, as for example concession agreement; technical assistance agreement or service contract; management agreement; production sharing contract; joint venture; or contract of work. The objectives and conditions governing such contracts are as diverse as these titles are. While a mining project is only one among a large mumber of similar undertakings in industrial countries, in most developing countries such projects usually have a dominating position within the country&apos;s economy. The general legislation is often inadequate and insufficiently detailed to cover all aspects of large projects with extensive foreign inputs and international markets. Therefore, the need for specific arrangements. Specific arrangements may also become necessary due to the complexity of markets for mineral products, the large number of participants - equity partners, suppliers, financial institutions, buyers, etc. - or economic and political conditions in the host country and fiscal regulations in the home country of the investors. Most agreements are concluded between governments, or government agencies, in developing countries and private industry headquartered in developed market economies - Canada and the United States of America in North America, Western European countries, Japan, South Africa and Australia - or, in some instances, with state-owned firms in these countries. There are fewer agreements between developing countries and the centrally planned economy countries - Eastern Europe and the USSR - which cannot be considered here because of absence of adequate information. Agreements can be concluded at any of the different stages from exploration through closing of a mine. While most contracts are negotiated at the time when a potentially viable ore body has been delineated and investigated sufficiently to anticipate a realistic time for commencement of production, other agreements start with "grass-roots" exploration, during operation of a mine, smelter or refinery or, exceptionally, after a temporary shutdown. While several major provisions are included in all types of agreements, others are covered in much more detail (or not at all) in some contracts reflecting the specific work programme of each project. While it is realized that subdivision and classification of complex contractual relations is necessarily arbitrary to a certain extent, such grouping is useful in practical terms, especially for the non-specialist. The following discussion, therefore, will start with a description of the major forms of contractual relation - concession, investment contract, joint venture, management agreement, service and production sharing contracts. Major issues covered in all, or almost all, agreements will then be dealt with. These include stages of development, corporate structure and control, fiscal arrangements, infrastructure development and environmental law, and dispute settlement and renegotiation. FORMS OF CONTRACT RELATIONS There has been marked change in the type of agreement entered into during the 1960s (and before) and the early 1970s and the period thereafter. While straight "concessions" - granting of exclusive rights to foreign investors over a certain deposit or areas with little restriction or well-defined obligations - were the rule during the first half of this century, more complex agreements have evolved since. Some of these cover every conceivable aspect, foreseen or only possible, and define rights and obligations of all partners to the last detail. Over the years, agreements have without doubt become more beneficial for the developing host countries, in part as a result of well-publicized nationalizations, as for example in Chile, and in part due to changed attitudes in all countries

Jan 1, 1985

By Clarence Hicks

THE labor policy, of the Standard Oil Co. (New Jersey) is founded. first of all on paying at least the prevailing scale of wages in the community; on, the eight-hour day, with time and one-half for overtime; one day&apos;s rest in seven; sanitary and up-to-date working conditions; just treatment assured each employee; payment of accident benefits beyond the amount prescribed by the State compensation law; health supervision by a competent medical staff; payment of sickness benefits after one year&apos;s service; cooperation with employee in promoting thrift and better social and housing conditions; and assurance for a generous annuity at the age of 65, guaranteed for life after 20 years of service. Most of these features have been a part of the company&apos;s policy for many years, but it is only during the past two years that the cooperation of employees in determining these matters has been definitely assured through industrial representation. Industrial representation, in the Standard Oil Co., is a principle rather than a procedure. It is built upon the belief that personal association of those interested in any problem leads to a mutual understanding and a fair decision as to what is right. Fully believing in this, principle, representatives of employees and representatives of management evolved a simple plan, the basis of which is that it gives every individual employee representation at joint conferences on problems and fundamental principles affecting all those interested in the industry. It is based on cooperation, not antagonism; its operation makes perfectly clear both to management and to employees that their interests are identical, that mutual understanding and cooperation insure progress and success for all. Furthermore, experience has definitely shown that representatives of the employees are not only alert for the employees&apos; interests but are as keen as the representatives of the management in determining and insisting upon fairness to the employer.

Jan 3, 1920

By Charles Willis

THE problem of the curtailment of forces in large numbers does not often come to employment departments and is, therefore, a problem that many departments are not prepared to handle intelligently. Those companies that are able to measure the individual efficiency of each man would probably lay off men according to their individual ability, irrespective of dependents, citizenship, or other considerations. During the war when labor was scarce, the business of the employment manager in industry was hiring men and carefully placing them where they were best fitted to work. The careful selection of employees had developed to a considerable extent before the war, and was becoming a recognized science. In the last few months, however, the cancellation of copper contracts, the accumulation of large stocks, the necessary curtailment of production because the copper could not be sold, and lack of any immediate prospects of the copper market opening, have led to a universal reduction of forces; and the problem that industry now confronts is that of discharging rather than employing. The problem has been aggravated by the cancelation of contracts in many war industries with the consequent turning loose of hundreds of thousands of men, a great amount of unemployment, and the return of the soldiers and sailors. The problem has now become one of reduction of working force with the least hardship and the least injustice, and yet caring for the returning soldiers, sailors, and marines who have been in the service of the government for nearly 2 years, and who have offered the supreme sacrifice. The Copper Queen Branch of the Phelps Dodge Corpn., operating at Bisbee, Ariz., found it necessary, along with all of the-other copper companies of the country, to reduce its force materially. In making this reduction it was, after due consideration, decided to classify employees with respect to dependents, length of service, and citizenship. The question of individual efficiency or workmanship was not considered. Copper

Jan 9, 1919

By Charles A. Chase

This paper, descriptive of a single mine, is presented in the belief that it may furnish useful suggestions to mine-managers encountering similar problems; and it includes the details which will enable them to estimate the value of the methods employed—especially where these depart from common practice. Tt should be added, however, that this mine is not typical of the San Juan district, but differs markedly from neighboring mines in physical conditions and metallurgical requirements. The Liberty Bell mine is situated in San Miguel county, Colo., on the west front of the San Juan mountains, 2 miles north of Telluride. The vein was discovered in 1876 by Wm. L. Cornett, who, with subsequeilt locators, took up claims along the apex. A few hundred feet of development-work was accomplished, and a few? tons of ore were smelted or milled; but profitable working proved impossible under existing

Jan 1, 1912

By E. A. Gulbransen, K. F. Andrew

The gas-metal reactions of zirconium are very interesting. The metal is extremely stable at room temperature to reactions with the several gases present in air and the metal will stay bright indefinitely. However, at temperatures of several hundred degrees higher the metal reacts readily with oxygen, nitrogen and hydrogen. This behavior, in addition to the fact that zirconium is one of the higher melting point metals which might have high temperature applications under the proper conditions, resulted in the work reported in this communication. There are several factors which indicate that zirconium might have good oxidation resistance at elevated temperatures. These are: (1) the high melting point of approximately 1860°C, (2) the high melting point of the oxide of approximately 2675°C, (3) the high degree of thermodynamic stability of the oxide to chemical reaction and the low decomposition pressure of the oxide and (4) the possible formation of a continuous oxide film since the volume ratio of oxide to metal is greater than unity. The unfavorable factors are: (1) the metal reacts to form nitrides, hydrides and carbides, (2) the oxide is soluble at elevated temperatures in the metal and (3) the oxide ZrO2 undergoes crystal structure transformations at high temperature. The oxidation resistance of this metal is not only a question of the rate of film formation but is complicated by the fact that the oxide and other reaction products dissolve in the metal which in turn will affect the physical and mechanical properties of the metal. The protection of the metal to nitride formation must be considered separately from the oxide problem. One unfavorable factor is that the volume ratio of the nitride to the metal is about unity. This indicates that a discontinuous film might be formed. This paper will present measurements on the rates of reaction of the metal with O2, H2 and N2 over a wide temperature and pressure range. The reaction in high vacuum and the stability of the several compounds formed will be presented. The results are correlated with fundamental rate theory and with the physical and chemical structure of the metal and film. Literature Although many papers have been published on the chemical reactions of zirconium with various gases, comparatively few are concerned with the protective nature of the metal and its reactions at normal pressures. The studies in the pressure range below 0.01 mm of Hg gas pressure are largely of interest in the nature of the adsorption of gases by hot filaments in high vacuum apparatus. The reactions of zirconium in this pressure range have been reviewed by Fast8 and by RaynOr.27 In spite of certain differences of opinion as to the maximum adsorption temperatures for various gases, the low pressure range is qualitatively understood. Some of these papers will be mentioned briefly here. 1. LOW PRESSURE Ehrke and Slack&apos; find that oxygen reacts above 885°C and hydrogen above 760°C. Nitrogen does not react up to a temperature of 1527°C. Fast9 on the other hand observes that oxygen is absorbed above 700°C and nitrogen at temperatures exceeding 1000°C. Hydrogen is absorbed from 300" to 400°C and liberated between 500" and 800°C. It is readsorbed at 862°C and released above 862°C. Hukagawa and Nambo22 find a rather complicated picture for the absorption of oxygen. A rapid initial absorption is found between 180" to 230°C. Further oxygen is not taken up until a temperature of 450°C is reached. The optimum temperature for complete absorption is 650" to 700°C. Nitrogen is found to be completely adsorbed at 600°C. However some of the gas is evolved at higher temperatures. Their data on the absorption of hydrogen indicate some of the gas is removed at 550°C. Guldner and Wooten17 in a study of the low pressure reactions of zirconium with various gases observed that the reaction with oxygen occurs at temperatures above 400°C and that the oxide is formed. The reactions with carbon monoxide and carbon dioxide occur rapidly at temperatures of about 800°C with the oxide and carbide being formed. Zirconium reacts at temperatures of 400°C slowly and at 800°C rapidly to form the nitride and with hydrogen and water at 300°C to form the hydride and a mixture of the oxide and hydride respectively. 2. NORMAL PRESSURE DeBoer and Fast3 in a study of the electrolysis of oxygen in zirconium find that the metal absorbs up to 40 at. pct of oxygen without forming a new phase. The solubility of nitrogen in the lattice has been studied by de Boer and Fast4 and Fast10 and is found to be considerable. At higher temperatures the oxide dissolves in the lattice at an appreciable rate according to Fast10 and the zirconium surface becomes active. De Boer and Fast4 and Hägg18 have studied the solubility of hydrogen and find that at room temperature the solubility corresponds to ZrH1.95 Desorption occurs on lowering the pressure. Hydrogen is stated to be more soluble in the ß-form and the

Jan 1, 1950

By P. G. Nahin, A. Grenall, R. S. Crog, W. C. Merrill

A progress report of an experimental investigation into the role of clay in reservoir performance is presented. The Paper gives some of the reasons for considering clay as a significant component and outlines the objectives of a broad field of stud) which it is intended to pursue. Descriptions of the analytical methods used are given; these include X-ray diffraction. elec tron miscroscopy, thin section petrography, infrared spec-troscopy, and cation exchange analysis. A suite of the more important clay minerals has been assembled and characterized l~y these methods for use as standards in core analysis. From the data obtained it appears that although no one method of analysis is diagnostic for all of the clay minerals the infrared technique shows considerable promise in this direction. For the present, one or more supplementary methods should be used to confirm the clay mineral identifications. The methods of analysis are applied to field cores taken from repesentative and widely differing strata especially as regards their susceptibility to damage by fresh water. well.; completed in the stevens and Gatchell zones in San Joaquin valley are I,articularly clear-cut examples of this behavior with stevens zone wells being more adversely affected by fresh water. cores from these zones have been studied and are discussed. It appears that differences in this behavior can be ascribed to differences in the nature of the contained clays. The value of the infrarecl spectra of the clay fractions in establishing the identity of the predominant clay minerals is given particular emphasis. INTRODUCTION It is a challenge to the technical resources of the petroleum industry that when the economic limit of production is reached, from 40 to 70 per cent of the oil in California reservoirs remains unproduced even by use of the best presently known methods of recovery. The magnitude of this abandoned volume of oil can be appreciated when it is considered that to 1950 in excess of 8 billion bbll has been produced from California reservoirs with estimated economically recoverable reserves in known fields and pools totaling nearly 4 billion bbl.24 If for every barrel of oil produced there is at least another barrel still in place, it is evident that the revenue obtained from the recovery of only a .few per cent of this volume would repay the cost of the required research manyfold. From well completion experience. production behavior, and a growing body of laboratory data it now appears certain that the mineral composition of a producing stratum has an important bearing on the productivity and ultimate yield. In addition to the organic component and water, the cores con,ist of gravel, sand. silt, and clay" in diverse variety of (a, composition and (b) texture. It is the composite effect of these two factors which is probably responsible in large measure for the way in which the oil flows to the well. The role of the clay and fine-size accessory minerals is not clear but there is a growing opinion, based on their physical and chemical properties, that it is a significant one. of particular importance are the prime facts: 1. The silt and clay fractions of the reservoir matrix possess the highest surface area per gram, and 2. The silt and especially the clay fractions are the most chemically reactive of the inorganic constituents present. Only within the last few years has the knowledge of clay mineralogy and the techniques of identifying the clay minerals reached such a stage as to enable reliable inquiry into the composition of argillaceous sediments.2,8,10,11,12,16,26 It is the purpox of this and succeeding papers to add to the fund of information on the role which these materials play in the production of petroleum from California formations by correlating their presence and associated properties with observed reservoir behavior. In the present paper attention is directed to their possible influence on damage by fresh water. OBJECTIVES The attack on this problem divides naturally into two broad phases: 1. Determination of the nature of the clays and their relationships to the other mineral components, and 2. Determination of the physico-chemical relationships between the clays and the interstitial fluids. In the work described in this paper the emphasis has been on phase 1, which stems logically from the necessity of identifying and understanding the materials to be dealt with in Phase 2. Based on the authors&apos; present opinion that not all of the minerals which occur in oil-bearing formation are of equal importance in their effects on the flow and recovery of oil, it was decided to focus attention first upon the clay minerals content and then. later perhaps. work into the field of the normally larger size non-clay minerals and fractions. The

Jan 1, 1951

By W. C. Merrill, P. G. Nahin, A. Grenall, R. S. Crog

A progress report of an experimental investigation into the role of clay in reservoir performance is presented. The Paper gives some of the reasons for considering clay as a significant component and outlines the objectives of a broad field of stud) which it is intended to pursue. Descriptions of the analytical methods used are given; these include X-ray diffraction. elec tron miscroscopy, thin section petrography, infrared spec-troscopy, and cation exchange analysis. A suite of the more important clay minerals has been assembled and characterized l~y these methods for use as standards in core analysis. From the data obtained it appears that although no one method of analysis is diagnostic for all of the clay minerals the infrared technique shows considerable promise in this direction. For the present, one or more supplementary methods should be used to confirm the clay mineral identifications. The methods of analysis are applied to field cores taken from repesentative and widely differing strata especially as regards their susceptibility to damage by fresh water. well.; completed in the stevens and Gatchell zones in San Joaquin valley are I,articularly clear-cut examples of this behavior with stevens zone wells being more adversely affected by fresh water. cores from these zones have been studied and are discussed. It appears that differences in this behavior can be ascribed to differences in the nature of the contained clays. The value of the infrarecl spectra of the clay fractions in establishing the identity of the predominant clay minerals is given particular emphasis. INTRODUCTION It is a challenge to the technical resources of the petroleum industry that when the economic limit of production is reached, from 40 to 70 per cent of the oil in California reservoirs remains unproduced even by use of the best presently known methods of recovery. The magnitude of this abandoned volume of oil can be appreciated when it is considered that to 1950 in excess of 8 billion bbll has been produced from California reservoirs with estimated economically recoverable reserves in known fields and pools totaling nearly 4 billion bbl.24 If for every barrel of oil produced there is at least another barrel still in place, it is evident that the revenue obtained from the recovery of only a .few per cent of this volume would repay the cost of the required research manyfold. From well completion experience. production behavior, and a growing body of laboratory data it now appears certain that the mineral composition of a producing stratum has an important bearing on the productivity and ultimate yield. In addition to the organic component and water, the cores con,ist of gravel, sand. silt, and clay" in diverse variety of (a, composition and (b) texture. It is the composite effect of these two factors which is probably responsible in large measure for the way in which the oil flows to the well. The role of the clay and fine-size accessory minerals is not clear but there is a growing opinion, based on their physical and chemical properties, that it is a significant one. of particular importance are the prime facts: 1. The silt and clay fractions of the reservoir matrix possess the highest surface area per gram, and 2. The silt and especially the clay fractions are the most chemically reactive of the inorganic constituents present. Only within the last few years has the knowledge of clay mineralogy and the techniques of identifying the clay minerals reached such a stage as to enable reliable inquiry into the composition of argillaceous sediments.2,8,10,11,12,16,26 It is the purpox of this and succeeding papers to add to the fund of information on the role which these materials play in the production of petroleum from California formations by correlating their presence and associated properties with observed reservoir behavior. In the present paper attention is directed to their possible influence on damage by fresh water. OBJECTIVES The attack on this problem divides naturally into two broad phases: 1. Determination of the nature of the clays and their relationships to the other mineral components, and 2. Determination of the physico-chemical relationships between the clays and the interstitial fluids. In the work described in this paper the emphasis has been on phase 1, which stems logically from the necessity of identifying and understanding the materials to be dealt with in Phase 2. Based on the authors&apos; present opinion that not all of the minerals which occur in oil-bearing formation are of equal importance in their effects on the flow and recovery of oil, it was decided to focus attention first upon the clay minerals content and then. later perhaps. work into the field of the normally larger size non-clay minerals and fractions. The

Jan 1, 1951

PUBLIC hearings began before the Committee for Reciprocity Information on May 24, 1950, for the purpose of unearthing data and opinion that will be helpful in the forthcoming reciprocal tariff and other trade-barrier negotiations at Torquay, England, on September 28th of this year. The conference this fall will constitute the "third round" of tariff negotiations under the General Agreement on Tariffs and Trade concluded at Geneva in 1947. The United States plans to negotiate with 17 other countries on possible tariff modifications on various articles all the way from baby carriages and bottle caps to lead and zinc-bearing ores. On May 31, June 1 and June 2, spokesmen appeared before the Committee for Reciprocity Information on behalf of the domestic lead and zinc mining industries. Producers of these metals protested the inclusion of paragraphs 391 (lead-bearing ores, dust and mattes), 392 (lead bullion, lead in pigs and bars, and scrap lead), 393 (zinc-bearing ores of all kinds), and 394 (zinc in blocks, pigs or slabs, and zinc dust) of the Tariff Act of 1930, as amended in the list of articles to be considered for possible tariff concessions at Torquay. It was pointed out that although operating costs have more than doubled since 1939 tariffs on these metals were actually higher in that year than at present. This, coupled with the detrimental effects of the recent series of devaluations, has sounded the death knell for a substantial number of domestic lead and zinc mines-a most undesirable development in the face of the ominous international situation, according to these spokesmen. It was urged that higher rather than lower tariff rates are needed on these metals. The opinion was expressed that it was inconsistent to foster a high living standard in our western areas and then, once it is attained, to undermine that condition by minimizing the protection that was partly responsible for it. The main theme of some arguments implied that although every effort should be made to close the "dollar gap" abroad, serious consideration must be given the methods employed lest our national security position be jeopardized in the process. The House Committee on Foreign Affairs completed hearings on H. J. Res. 236, to provide for United States membership and participation in the International Trade Organization. Hearings began on April 19th and ran for over five weeks. Many witnesses from industry and government presented voluminous testimony, which will not be available for public distribution for several weeks. However, it is no secret that the most controversial provisions of the Draft Charter of the ITO are: (1) Article 17 (Chapter IV on Commercial Policy) which would obligate members to negotiate for the reduction of tariffs and the elimination of trade preferences; (2) Article 20 which would prohibit the use of quantitative restrictions for protective purposes; (3) Article 16 which promulgates rules to implement the principle of non-discrimination in international trade; and (4) provisions permitting the use of protective measures for promoting economic development, particularly in backward areas, even though such provisions are inconsistent with those of the three articles cited above. United States membership in the International Trade Organization is essential to the successful operation of that body in view of this country&apos;s position as the economic giant in the present international trade pattern. Many countries are reluctant to take any action toward the ratification of the charter until it is known what course America will pursue. However desirable or undesirable the ideal of free multilateral trade may be it is unlikely that this Government&apos;s participation in the ITO will materialize soon. Advices in Washington indicate that H. J. Res. 236 will not be enacted during the present session of Congress. The legislative pattern designed to secure Congressional approval of the ITO is similar to that of the St. Lawrence Seaway project. The Seaway project was pending in treaty form for several years before the Foreign Relations Committee of the Senate and when the Administration decided to incorporate this project into bill form it was found that, while it passed the House promptly, the Senate decided to pigeonhole it because of the obvious intent to circumvent the constitutional prerogative of the Senate to advise and consent to the ratification of treaties. The ITO bill may be slated for a similar fate. It is deemed essential by western Senators and Congressmen that the present session of Congress enact some form of mining legislation before its adjournment, now set for July 31st. These legislators from prominent ore-producing states do not desire to return to their home areas in the fall emptyhanded. Aside from that, it is entirely superfluous to reiterate the necessity for maintaining a healthy domestic mining industry as a bulwark against a sharp rise in the temperature of the "cold war". Now that S. 2105 has failed a new bill is taking shape in the Senate Interior and Insular Affairs Committee. It is similar in language to H. R. 8221 (to encourage the conservation and development of the mineral resources of the United States) reported by the House Public Lands Committee on May 3, 1950, but so far has failed to receive approval of the House Committee on Rules. There are some qualified observers in high circles in Washington as well as in the mining industry who favor a tax incentive program to stimulate investment in mining enterprises, as opposed to a conservation and exploration program. The Bureau of Mines and the Treasury Department have undertaken a joint study to determine the need for modification of the tax laws as they apply to mining. The study is scheduled for completion before the end of the year, and appears to be supplementary to the investigation initiated by the National Minerals Advisory Council which culminated in the submittal of recommendations to the Secretary of the Interior in December 1949. The "cold war" is largely responsible for the increased demand for metals. Stock-pile purchases and heavy industrial demand due to military needs distort markets and disrupt normal price trends. Such activity has an unhealthy influence on metal production, luring some producers into a state of dependency on the continuation of this condition. When stock-pile objectives are met sometime in the future purchases must then come to a halt unless international "fireworks" are touched off. It can only be hoped that technological improvements and further mechanization of mines coupled with the stimulus of a rising population will offset the anticipated drop in industrial demand and cessation of stockpile purchases when the international crisis abates.

Jan 7, 1950

By AIME

One of the operations of the J. L. Shiely Co. is quarrying in a hard granite gneiss with intrusions of gabbro or trap. During the winter of 1948-1949 the quarry ramp was lowered about 30 ft and during the 1949 season practically all drilling was done from the quarry floor, developing a face from 72 to 83 ft for the entire quarry area. The performance and cost table shows our record for 1948 and 1949.

Jan 1, 1950

By Bernt Ellingsaeter, Terkel Rosenqvist

IN the silicothermic reduction of magnesia, burned dolomite is treated with high grade ferrosilicon in an evacuated steel retort at temperatures between 1150° and 1200°C. The following reaction is assumed to occur MgO + CaO + 1/2 Si (Fe) - Mg(g) +- & Ca,SiO, + Fe with the equilibrium constant on the basis of thermodynamic data for the substances involved and assuming unit activity for all solid constituents, Kubaschewski and Evans&apos; calculated the magnesium pressure as a function of temperature logp,, (mmHg) = 15.06-1.61 T- log T- 13,16O/T. Pidgeon and King," who measured the magnesium pressure by means of a flow method, found values about three times the calculated ones. This may be caused by uncertainties in the thermodynamic data, but may also be caused by the formation of other reaction products, such as Ca,SiO,, which is known to be the stable silicate in equilibrium with lime. Whatever the exact reaction may be, it is evident that as long as all other factors are maintained constant the magnesium pressure will vary with the silicon activity, viz: p,, = &,. (p,,) ", where (p,,)" is the magnesium pressure by the reduction with silicon of unit activity. In the present investigation, p,,, was therefore measured for various grades of ferrosilicon and their silicon activities were calculated. The experimental method was similar to that used by Pidgeon and King. Briquettes of burned dolomite and Fe-Si alloys were placed in a 1 in. heat resistant steel tube and were heated to 1200°C. By means of a flow of purified hydrogen, the magnesium vapor was swept into a condenser filled with steel wool. From the amounts of hydrogen used and magnesium condensed the magnesium partial pressure was calculated. First a tube of 28 pct Cr steel, and later a tube of Kanthal D (a ferrous alloy with 22.6 pct Cr, 2 pct Co, and 4.5 pct Al), was used as a heat resistant tube. The latter tube showed the best heat resistance. The dolomite used had the following composition: 43.6 pct MgO, 55.5 pct CaO, 0.2 pct K,O + NalO, 0.2 pct Fe,O,, and 0.3 pct insoluble. The ferrosilicons were prepared from 98 pct Si of technical grade (0.7 pct Al, 0.3 pct Ca, and 1 pct Fe) by melting with various amounts of electrolytic iron of high purity. The alloys thus obtained were analyzed on their iron and silicon contents, which added up to between 99 and 100 pct. The amounts of reactants were chosen so that there would always be an excess of the oxides, and the average decrease in silicon content during the experiments would be about 1 pct. Most of the reaction occurred in the part of the reaction mixture facing the gas flow. The change in the silicon concentration in the part facing the condenser was, therefore, negligible. To facilitate the reaction, about 1 pct fluorspar was added to the briquette mixture. Fluorspar does not enter the reaction, but is known to act as a

Jan 1, 1957

By C. N. Reid

Slip-line studies on deformed chromium single cvystals showed the usual bcc behavior. At room temperatuve, cross slip was prevalent—slip was not confined to a given plane, but the slip direction was (111). At -10O0K, slip occuvred on (110) planes, twins on(112) planes, and cleavage on (1001 planes. A single-crystal tensile specimen with an axis close to [011] showed a pronounced yield drop and high strain rate sensitivity which zclere used to derive relevant parame tevs in a dislocation dynamics treatment. Transmission electron microscope studies confirmed the existence of (110) slip planes and showed ecidence of loops punched out by precipitates and of grown-in dislocations promoting tangling. OF recent years experimental studies have been made of the deformation characteristics of single-crystal molybdenum and tungsten, but very little has been published on the behavior of single-crystal chromium. During a study of the mechanical properties of chromium, single-crystal studies were made which have already been partially described.&apos; However, additional information was generated which was not directly relevant to the main theme of Ref. 1, and, therefore, was not reported. In view of the need for complete documentation of deformation modes, the experimental observations made on the deformation of single-crystal chromium are summarized here, together with an electron-microscope study of the associated dislocation structures. It was found that, in terms of the deformation modes, chromium is a conventional bcc metal, showing a very pronounced yield-point phenomenon. Further, it was found that the flow strength of these crystals is very sensitive to the strain rate. Finally, the crystals were observed to contain many unidentified precipitates, which often were associated with prismatic dislocation loops. EXPERIMENTAL METHODS Single crystals were grown from rods of wrought chromium by the method of zone annealing. Rods of "1/4in.-diam were supported vertically in an argon atmosphere while an induction coil was moved up the rod at 1 in. per hr. The power was adjusted to just below that required for melting, and the process produced single crystals in about 30 pct of the rods used. The orientations of the crystals, in general, lay near [011] and are summarized in Fig. 1. Before this treatment, the wrought material contained 35 pprn C, 68 ppm O, and 12 ppm N.* An analyzed single crystal *Usual metallic impurities found in iodide chromium are: Al, 5 ppm; Ca, A ppm; Cu, 2 ppm; Fe, 75 ppm; Yg, 0.5 ppm; Yn, < 3 ppm; Mo, < 3 ppm; Ni, 4 ppm; Si, < 20 ppm; Ti, < 1 ppm; V, 4 ppm; Zr, < 3 ppm. contained 10 pprn C, 79 ppm O, and 50 pprn N. Tension and compression specimens were shaped from the crystals by mechanical grinding, followed by the electrolytic removal of about 0.010 in. from the surface in a perchloric/acetic acid bath. All specimens had a gage length of 0.75 in., and tension specimens had a diameter of 0.100 in., while that of the compression samples was 0.200 in. Mechanical tests were carried out at a rate of 1.3 pct per min, and temperatures below 0°C were attained by means of a nitrogen cryostat similar to that of Wessel.2 EXPERIMENTAL RESULTS Modes of Deformation. In addition to the tensile properties of these crystals, which are described in Ref. 1, deformation markings on the surface were studied. Crystals A and F, Fig. 1, were deformed in tension at 300°K to 10 and 16 pct strain, respectively. The surfaces contained visible slip lines, about 1 C( apart, composed of both straight and wavy segments. They did not define a single plane, and so determination of the slip plane was not possible. However, the slip direction was deduced by comparing the axial orientations of the crystals before and after deformation. Fig. 2 is representative, and shows that the axis ro-

Jan 1, 1968

IN THE early period of steelmaking, ingot structure and segregation presented no difficult problems. Crucible melting required very small ingots which, if properly deoxidized, gave little segregation, and a small inserted hot top prevented pipe. As larger ingots were poured [ ] from Bessemer and open-hearth furnaces, segregation, piping, and gas evolution became increasingly important. The first studies of solidification were made by Gathmann (l) and the Brearley&apos;s (2) who used stearine to show the effects of shrinkage and mold shape. Figure 78 shows a series of stearine ingots at various stages of solidification. These studies indicated that the liquid solidifies at a nearly uniform rate, starting at the walls and bottom of the mold and progressing inward, and demonstrated the formation of secondary pipe in big-end-down molds. Stearine illustrates the mechanics of solidification, and exaggerates pipe because of its great

Jan 1, 1944

IN the early period of steelmaking, ingot structure and segregation were of no practical importance. Crucible melting required very small ingots that gave little segregation, and a small inserted hot top prevented pipe. As larger ingots were poured from bessemer converters and open-hearth furnaces, segrega- [ ] tion, piping, and gas evolution became increasingly important. The techniques of making semikilled and rimmed ingots were developed with little knowledge of the actual mechanism of the process. The first studies of solidification were made by the Brearleys1 and Gathmann,2- who used stearine to show the effects of shrinkage and mold shape. Fig 11-1 is a picture of a series of stearine ingots at various stages of solidification. These studies showed that the liquid solidifies at a nearly uniform rate from the sides and bottom of the mold and demonstrated the formation of

Jan 1, 1964

By J. F. Wolff

J. G. WOLFF, Duluth, Minn. (communication to the Secretary*).-In raising the question (" Newly Discovered Fossil Remains in the Cretaceous Shale," p. 1784) as to the possibility of the so-called Cretaceous remnants found on top of Mesabi Range orebodies really being Jurassic, the writer was acting under a wrong impression. In speaking of the matter with different geologists of note who have visited Northern Minnesota during the past year, lie understood one of them to refer to Jurassic shales existing quite extensively in Northwestern Minnesota. This apparently was entirely a misunderstanding. In answer to an inquiry in regard to this matter, Prof. W. H. Twenhofel, paleontologist at the University of Wisconsin, said that the known Jurassic nearest to Northern Minnesota is in Western Dakota. From the reproductions of fossils shown on p. 1785, Prof. Twenhofel tentatively correlated them as "middle-upper Cretaceous."

Jan 2, 1917

By J. N. Roberts, K. V. Gow

In a recent review of the field of plastic deforrnation of metal single crystals, Maddin and chenl indicated the need for systematic investigations of the crystallography of the slip process with special attention to: a) The effect of the orientation of a crystal on the appearance of slip lines, b) The effect of high temperatures on the slip systems of aluminum, c) The effect of strain rate on the crystallography of slip. The present paper deals with the effect of temperature and strain rate on the mechanism of deformation of aluminum single crystals similarly oriented for single and duplex slip. The work of several investigators has shown that in aluminum at high temperatures other slip systems in addition to the predicted {I l l) <101> may operate. The most generally reported additional systems

Jan 1, 1959