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By C. C. Harris Discussion by B. K. Loveday

B. K. Loveday (National Institute for Metallurgy, Johannesburg, Republic of South Africa) - The paper and subsequent technical note' describing a method of determining the parameters of the three-parameter size-distribution equation developed in the paper were read with much interest. This equation was also used at National Institute for Metallurgy (NIM) to describe size distributions in grinding tests, because it was necessary to have a single equation to describe the size distribution at any time during a test. A graphical method also was used to determine the three parameters, and the use of this method as an alternative to Professor Harris's latest method is discussed here. The three-parameter model can be expressed as follows: Eq. 1 can be rearranged and transformed to Yield a linear reiationship between Y and X (transformed) log

Jan 1, 1970

Established as a Society February 26, 1957 OFFICERS AND COMMITTEES Wayne E Glenn, President Earl M Kipp, President-elect John S Bell, Past President R A Morse, Vice-President W D Owsley, Vice-President Everett G Trostel, Treasurer Joe B Alford, Executive Secretary 6300 North Central Expressway Dallas 6, Texas

Jan 1, 1960

By D. F. Malott

The Michigan Dept. of State Highways makes extensive use of geophysics for subsurface surveying which would be applicable for uses in other fields. Examples of resistivity surveys are given which include a proposed large-volume excavation with suggestions for land use after excavation, subsurface evaluation for engineering design, and a subsurface survey for land appraisal. An example of a combined refraction seismic and resistivity survey is shown where the resistivity is used for outlining the unconsolidated soils, while the seismic method is used to outline bedrock and to evaluate it for rippability. A refraction seismic survey at the bottom of bridge caissons for evaluation of bedrock uniformity and a rehtive aid in assessing rock strength is reported. These past several years have been a period of unprecendented construction and commercial expansion. Vast private manufacturing complexes and government road, power, and office projects are being built or are in planning stages. Nearly everywhere, municipalities are expanding outward and upward. Many towns are developing into cities and many cities are displaying new skylines, and the building boom shows little sign of slowing down.

Jan 1, 1970

By K. E. Merklin, F. D. DeVaney

Students of the modern blast furnace seem unanimously agreed that they are observing a major revolution in practice. Rather than changing construction and operation of the furnaces, most of the great advances now under way deal with the raw materials feed. Prepared burdens have gained increasing significance during recent years. Sizing, concentration, and agglomeration have all become bywords to greater production and reduced operating costs. The remarkable results with test furnaces in which self-fluxing sinter makes up part or all of the ore charge foretell even greater improvements. Other investigators have reported many of these advances, and it is enough to predict here that more and more operators will turn to the use of self-fluxing sinter. This change in the operator's requirements comes at a time when one major section of the iron ore regions, the Mesabi, is finding it difficult to maintain, let alone improve, the tonnage and grade of its shipping product. To meet the new demands with respect to quality and structure, the iron ore producers of this area turned first to screening, crushing, and concentrating intermediate ores. More recently, declining higher-grade reserves have led to multimillion-dollar investments in plants to treat the low-grade magnetic taconites.1,2 To yield a suitable concentrate, the Minnesota magnetic taconites must be ground to about 80 pct through 325 mesh, too fine to be charged directly to the blast furnace or to make acceptable feed to the sinter strand. The pelletizing process was developed to meet the structure requirements laid down by the blast furnace operators. Taconite producers are succeeding in their efforts just when the attention of the blast furnace man is being drawn to the great advantages of self-fluxing sinter.3 The taconite operators are ready with an alternative. Why not produce sclf-flus ing pellets? At the Hibbing laboratory of Pickands Mather & Co., where much of the early work was done that led to Erie Mining's 7.5-million ton taconite plant at Hoyt Lakes, Minn., preliminary investigations have been made. Present Taconite Operations: Details of this work will be clarified by a brief review of agglomeration practice in commercial taconite plants. After the taconite has been ground to about 80 pct through 325 mesh to liberate the magnetite grains, the ore is concentrated on magnetic separators, thickened, and filtered to about 10 pct moisture. This structure and moisture fit in closely with the conditions required to produce good balls. It has been found with taconite concentrates that at least 60 pct of the feed to the balling drum must be —325 mesh to obtain good ball compaction within reasonable time. The filter cake moisture usually permits a slight water addition at the balling drum, and further balling control is obtained by adding about 12 Ib of bentonite and 1 1/2 lb of soda ash per dry short ton of concentrate. These additives, and occasionally small quantities of fine coal, are thoroughly mixed with the filter cake ahead of balling. The swelling property of bentonite improves the green and dry strength of the balls so they can be handled without breakage until they are fired. Soda ash is added for pH control to insure maximum performance of the bentonite, and coal is added for more heat in the firing process when required. The balls, normally 3/8 to l-in. diam, are brought to a temperature of 2350" to 2500°F in the indurating furnace. Heat for this process comes from three sources: 1) fuel burned in the combustion chamber, 2) oxidation of the magnetite concentrates to hematite, and 3) coal added to the balls. Pellet strength is developed by grain growth and bridging and, if enough slag-forming constituents are present, by slag bonding. Conversion to hematite is usually close to 100 pct in the fired pellets. Batch Test Procedures: Initial studies of self-fluxing pellets were made by producing balls on a batch basis under carefully controlled laboratory conditions. The l-in. balls, uniform in size, were fired in an oxidizing atmosphere in a standard laboratory muffle furnace. The firing procedure consisted of

Jan 1, 1961

Born, March 28, 1853 Died July 23, 1916 On July 25, 1916, the Board of Directors adopted the following minute and directed that it be entered upon the records of the Board & published in the Bulletin of the Institute, and thereof be sent to the family of Mr. Kirchhoff: Charles Kirchhoff was one of the oldest, most widely known and most highly esteerned members of the American Institute of Mining Engineers. On his return in 1875 from a European course of study, to begin a highly successful professional career, he joined the Institute, then just commencing to acquire both national and international recognition. He became at once, and-for more than 40 years continued to be, its earnest , and active supporter, serving it as Manager, Councilor or Director for terms aggregating 9 years,-as Vice-President for 2 years, and twice as President for a year. During the critical period of the erection of the United Engineering Society's building, and the transfer of the Institute to permanent head-quarters therein, Mr. Kirchhoff was its efficient representative in the United Engineering Society, and on the Building Committee. In 1910, amid the congratulations of colleagues, employees, and innumerable friends, Mr. Kirchhoff retired from active business as Vice- President and General Manager of a great technical publishing company. Yet he sacrificed of his well-earned leisure yet one more year, to serve the Institute as President through 1911.

Jan 9, 1916

By F. L. Bosqui, A. D. Wilkinson

EVEN though the world has not been crying for more copper for the last three or four years there has been some important mill and smelter construction. Discovery and development of large new high-grade copper deposits in Africa has led to the construction of extensive reduction facilities there, prominent among which is the concentrator and smelter of the Rhokana Corporation at N'Kana. Northern Rhodesia. The 3000-ton concentrator adjoins the central shaft. A little over half a mile to the southeast, at an altitude of 40,010 ft., is the smelter, designed on the site by 1. H. Wynne. It is arranged primarily to treat N'Kana copper concentrates, but can also handle concentrates and direct-smelting ore from outside sources. Excavations were started late in 1930; concrete was first poured on Jan. 6. 1931; and the first blister cop¬per was cast on March 1.9, 1932, less than fifteen months later. During this period, which included several months of heavy tropical rains, some 10,000 cu. yd. of concrete was poured and 41000 tons of structural steel erected under the supervision of construction engineer, A. Ek, with a labor force of 60 to 30 Europeans and about 300 natives. The steelwork was fabricated by Head Wrightson & Co. in England, and the boiler plant equipment furnished and erected by the International Combustion Co. Ltd.

Jan 1, 1934

By S. H. Ward

Since the advent of the first airborne electromagnetic system, it has been evident that such systems were inherently limited to shallow depths of exploration of the orderof 100 to 200 feet. Hence in 1948 the author and his associates commenced a study of the feasibility of applying natural audio frequency magnetic fields to investigation of the electrical properties of the subsurface in order to provide a system capable of overcoming this limitation. This research culminated, in the summer of 1958, in the development of a new airborne prospecting device — AFMAG. This device has detected surface massive sulphide bodies while flown at heights as great as 3000 feet. Hence, by inference, it is deduced that it could find similar sulphide bodies if they were buried 2500 feet below surface and the aircraft flown at 500 feet. Thus a considerable improvement over conventional airborne electro-magnetic systems is obtainable with AFMAG. Airborne exploration in mountainous terrain involving deep valley fill now becomes possible. Examples are presented of the results of actual airborne AFMAG test surveys over known deposits of massive sulphide mineralization. Interpretation of the data is discussed with particular reference to the knowledge of size, dip, depth, depth extent, and conductivity of causative bodies as deduced from the flight records. The possibility of mapping major geologic structures, for both mining and oil exploration purposes, is discussed with the aid of examples of airborne AFMAG data. INTRODUCTION Electrical prospecting with natural audio frequency electromagnetic waves as a source has, within the last three years, become a practical reality. Both airborne and ground survey instruments under the trademark "AFMAG" (for audio frequency magnetics) have been used successfully in the search for conductive mineral deposits. It is the object of this paper to discuss the principles of airborne AFMAG and to illustrate its application by means of examples obtained over known geological situations. WHY AFMAG? In view of the large number of good airborne electromagnetic systems available for purchase or contract surveying, one may well ask, "Why another new system?". Primarily the answer lies in the fact that AFMAG does not suffer from the very limited depth of exploration available with, and inherent in, any conventional airborne electromagnetic system. AFMAG is not conventional insofar as an artificial transmitter is not required. Only a receiving and detecting device is employed. The electromagnetic fields measured are those from millions of electrical discharges in the atmosphere (e.g;..- lightning strokes). Their random distribution in time and space make these fields difficult to employ and it is only with recent advances in the electronics of geophysical instrumentation that this has become possible. A second reason for AFMAG and one of its

Jan 1, 1961

By C. Feng, C. Elbaum

Knoop hardness measurements were carried out on large grains of iodide titanium containing different amounts of oxygen. For each oxygen content the hardness is recorded ainingas a function of the crystal orientation and of the angle 4 between the indenter diagonal and the projection of the C (hexad) axis in the surface. The results can be expressed by the following relation; hardness = n-k cos 2ø, where n and k are constants for a given oxygen content and crystal surface orientation. A NISOTROPY of hardness is a well-known phe-nomenon and has been reported for many metals.1-3 At the present time, however, such information is not available in the literature for titanium. Consequently, a systematic study of the simultaneous effects of oxygen content and crystallographic orientation on the hardness of titanium was undertaken in this laboratory. Evaluations of oxygen content in titanium are frequently carried out through hardness tests. Although such procedures may be justified in small grain specimens, the results of the present investigation indicate that the anisotropy of hardness should be taken into account in the case of coarsegrained specimens as well as in the case of pronounced preferred orientation. Materials and Experimental Procedures Iodide titanium, 99.99 pet pure and containing of the order of 0.002 wt pet O, was used throughout this investigation. The metal was arc melted in an argon atmosphere and cold rolled into strips 1/16 in. thick. These strips were subsequently recrystal-lized and strain annealed in vacuum (10" mm Hg or better) at 850°C in order to produce crystals varying in diameter from 10 to 25 mm. Oxygen was introduced into selected large crystals by heating at 700°C in an atmosphere of pure oxygen under an observed pressure of approximately 50 mm Hg. Each sample was subsequently annealed in vacuum at 850°C for 100 hr, in order to homogenize the oxygen content throughout the specimen. It was found that longer annealing was not necessary, for no change of surface hardness in a given direction was detected after prolonged annealing. The oxygen content was determined by the difference in weight of the specimens before and after the oxidation-annealing cycle. The accuracy of oxygen determination is within ±0.1 mg in samples weighing 0.5 to 1 g. A vacuum fusion analysis of oxygen was performed on several samples and gave results in good agreement with the ones obtained by the weight change. It should be emphasized that expected weight losses through evaporation of the metal in vacuum at 850°C' are many orders of magnitude lower than the precision of these measurements. Following the annealing treatment, both oxidized and unoxidized crystals were carefully polished. All detectable traces of surface cold working were removed by repeated polishing and etching. Laue back reflection X-ray patterns were taken for each crystal for the purpose of determining the orientation and ascertaining the absence of substructures detectable by this method. Hardness measurements, using a 1 kg load, were subsequently carried out on a Tukon hardness tester equipped with a Knoop indenter. The Knoop indenter was used throughout this work because indentations obtained by means of a Vickers indenter are considerably distorted due to the anisotropy of the elastic constants in titanium. Such distortions are much less pronounced in the case of Knoop indentations, although for some orientations a cer-

Jan 1, 1959

By Arnulf Muan, Egil Aukrust

Activities of COO in the three solid solution series COO-MgO, COO-MnO, and COO-"FeO" have been determined at 1200°C by equilibrating oxide samples with a metal phase (cobalt or a Co-Fe alloy) in atmospheres of known oxygen activities. The systems COO-MgO and COO-MnO are ideal, within limits of experimental error, whereas the system COO-"FeO" shows a slight positive deviation from ideality at the temperature of this investigation. KNOWLEDGE of activities of oxide components in solid solutions is necessary for the calculation of the cation distribution among coexisting oxide phases in many important metallurgical, ceramic, and geochemical systems. Very few activity-composition curves are available for such systems at the present time. A start on the prodigious job of obtaining such data has been made by studies of solid solutions with simple sodium chloride type structure containing NiO or "FeO" as a component.1-3 The present paper describes similar studies for solid solutions with sodium chloride type structure containing COO as a component. For the systems COO-MgO and COO-MnO, the activity solid solution is determined by the equation Here po and are the oxygen activities of the gas phase in equilibrium with the phase assemblages metallic cobalt plus oxide solid solution, and metallic cobalt plus pure COO, respectively. In the system CoO-"Fe07', the metal phase is a Co-Fe alloy rather than pure cobalt. In this case the activity of COO in the oxide solid solution is calculated from the equation where a& is the activity of cobalt in the metal phase. Because the system Co-Fe is close to ideal4 and the metal phase appearing in the present work contains less iron than cobalt even at the lowest COO concentrations of the oxide phases used may be set equal to N . Hence, Eq. [2] becomes The value of Nc, can be estimated from the relative stabilities of the oxides COO (see below) and I) EXPERIMENTAL METHOD Two different but closely related procedures were used in the present investigation to determine the activity-composition curves. In one method, the oxide solid solutions were equilibrated against

Jan 1, 1963

By F. W. Bowdish

A theoretical and experimental laboratory study has shown that the rate of breaking of oversized particles in a ball mill is proportional to 1) the concentration of such particles, and 2) the area of the balls, provided that the balls are larger than a certain size relative to the particles. If all undersized material were removed as formed, the rate of breaking would be almost independent of the quantity in the mill. Rate equations are given which are similar to those for zero, first, and second order reactions. Deviations of small balls from the equation for a second order phenomena are quantified by a factor called "nipping efficiency." Some data are correlated by a dimension-less equation, which is used to estimate nipping efficiencies from data not in the correlation. The investigation described here was undertaken after a literature survey revealed that little was known concerning the mechanism of breaking of particles within a ball mill and the effect of this mechanism upon grinding rates. One paper, by Roberts1 , offered a theory concerning the mechanism of breaking, and a rate equation for the breaking of particles larger than some size to particles smaller than that size. That paper provided the starting point for a theoretical and experimental investigation of grinding under carefully controlled conditions. THEORETICAL CONSIDERATIONS In his paper on the probability theory of ball mill grinding, Roberts theorized that "... a given expenditure of power leads either to a certain number of point to point blows per bp-hr or to a certain distance of line contact per hp-hr ..." He assumed that the balls touch each other during each blow or during moving contact. Then he said that a volume of pulp, dependent upon the size being considered, would be covered per minute within which all oversized particles would be crushed to particles smaller than that size. Naturally, the higher the concentration of oversized particles in the pulp, the higher the rate of which they would be broken. From this reasoning Roberts obtained the differential equation -dC/dt = k hp/ton C (1) where k is a constant for any size of particle, density of particle, and moisture content of pulp. C is the percentage of oversize in the material to be ground, t is the time, and hp/ton is the power input per ton of material in the mill. He then integrated the equation to log Co/Ct = k/2.3 hp/ton t , where Co and Ct are the percentage of oversize at time zero and t respectively. By always using the same quantity of material in a mill and assuming that it required constant power to run the mill, he was able to combine the horsepower per ton factor with the other constants to give an equation for a first order rate.

Jan 1, 1961

By T. K. Perkins, L. R. Kern, R. E. Wyant

Many factors influence the results of hydraulic fracturing to stimulate well productivity. Most of these factors have been studied and their effects discussed in the literature. However, the movement of sand through the crack during fracturing has received little consideration. Exactly where the sand goes in the fracture, how it gets there, and how this might influence results have not been studied, judging from published reports. To get an answer to some of these questions we have studied sand movement through a simulated crack segment in the laboratory. Although the work is preliminary, we have answered some questions about sand movement in a semiquantitative sense. We are reporting our results at this time in the hope of stimulating interest and further study in this important aspect of fracturing. LABORATORY EXPERIMENTS Fig. 1 is a schematic diagram of equipment used in this study. A segment of a vertical crack 0.25-in. wide was formed between two Plexiglas plates, and movement of sand in fluid through the crack was observed under various conditions. Sand and fluid were injected into the crack at constant rates. The top and bottom of the crack were closed so that the fluid flowed horizontally. Because of gravity most of the sand settled to the bottom before moving very far through the crack. If the fluid velocity exceeded a certain critical value, then all the sand injected was washed on through the crack even though it had settled to the bottom. When the fluid velocity was less than this value when sand injection was started, most of the sand which settled in the crack remained in place until enough of the area open to fluid flow was blocked by the settled sand to increase the fluid velocity to the critical value.. At this point all injected sand moved on through the crack even though it settled to the lower portion of the moving fluid section. All sand previously settled remained in place. When fluid velocity was increased at this paint by increasing fluid injection rate (without also increasing sand injection rate), some of the previously settled sand was washed out until enough area was open to flow that the velocity dropped to the critical value. Conversely, when the fluid velocity was decreased by decreasing the fluid injection rate (without changing the rate of sand injection), additional sand would settle until the critical velocity was again attained. In short, the critical velocity is an equilibrium value which the system will automatically seek, if possible. The equilibrium (or critical) velocity was measured under several conditions. The results of these measurements are shown in Pig. 2 where the equilibrium velocity is shown as a function of the amount of sand injected per minute. The points falling in the shaded band shown in Fig. 2 were obtained with water. The higher viscosities were obtained by adding CMC (carboxymethylcellu-lose). Data indicate that the equilibrium velocity is not very sensitive to sand size or transport fluid viscosity, or to sand injection rate (except at very low rates). Points connected by the solid CUrve in Fig. 2 were obtained with water and 20- to 40-mesh steel shot. The equilibrium velocity is apparently fairly sensitive to difference in density between particle and fluid. Only one run was made with a gelled fluid and that was gelled water at zero sand injection rate as shown in Fig. 2. (Measurements of equilibrium velocity at zero sand injection rate were made by filling the crack

By J. F. Havard

The enterprises based upon the industrial minerals are diversified in geologic habit, mining systems, processing techniques and marketing methods. Nevertheless, in 1972 these enterprises faced many of the same frustrations and hopes and knotty problems and crucial decisions. Volume and profits were generally improved but were uneven in extent and effect. The U.S. cement industry, for example, was unable to meet demand in major markets. It was constricted by a frozen low-level price structure, faced expensive pollution control measures and watched heavy imports penetrating its markets from several European nations, Mexico and Canada.

Jan 1, 1973

By R. F. Rolsten

VAN Arkel 1 prepared ductile tantalum by the thermal decompoiition of tantalum pentachloride on a resistively heated wire (2000° C) in an evacuated bulb maintained at 100°C. Burgers and Basart2'3 observed the formation of a mixture of tantalum carbide and free metal when a carbon deposition base was used. campbel14 suggested the thermal decomposition of the iodide if a lower decomposition tem- perature was desired. To date, the details for preparing high-purity iodide tantalum have not been disclosed. EXPERIMENTAL The tantalum to be purified was symmetrically placed around the clear quartz deposition surface centrally located within a 64 mm cylindrical Vycor bulb. The deposition vessel usually employed5 was modified6 by incorporating a reentrant fin,mer in place of the customary metal filament in the head

Jan 1, 1960

By G. F. Butterworth

The metallographic structures most frequently encountered in rifle barrels, and which are illustrated by the accompanying photomicrographs, fall naturally into two groups, distinguished by the method used to, produce in the stock a physical condition having the requisite properties. The fist group consists of "rolled" barrels; that is, barrels subjected to hot working by rolling in or near the critical range. In the second group, the stock, which is smaller in diameter than the first, is upset to form the butt end and is then heat treated by giving it a quench and a draw. These barrels will be referred to as " heat-treated " barrels. The structure of the rolled barrels resembles closely that of the same steel after annealing. There is the same network of excess ferrite outlining the grain boundaries, but the grains themselves are composed of sorbite rather than pearlite. The grain size is closely related to the rolling temperature. The critical-point curves of this grade of steel, which is approximately 0.50 to 0.60 per cent. of carbon and 1.00 to 1.30 per cent, of manganese, show a single very pronounced point between 1300" and 1350" F. (704" and 732" C.). Barrels rolled within this temperature range give an exceedingly fine grain, shown in Fig. 1. In fact, the grains may be so fine that, at a low magnification, they may be confused with the heat-treated structure shown in Fig. 6. A magnification of 500 diameters, however, will always resolve a rolled barrel into the characteristic structure shown in Fig. 2. As the temperature is increased, the grains are found to be larger. If, on the other hand, the rolling temperature is below the critical range, the structure previous to rolling will not be obliterated, the only effect of rolling being to elongate the coarse sorbite grains in the direction of rolling, Fig. 3. This distortion is greatest at the muzzle. Heat-treated barrels are quenched in oil from above the critical range, which should give a martensitic structure, Fig. 4, but the presence of some troostite in the martensite is frequently noted when the quench has not been sufficiently drastic, Fig. 5. The structure brought about by the subsequent draw is not so striking, though quite as typical. It is sorbitic or sorbito-pearlitic, and under a low magnification appears almost homogeneous, as in the case of fine grains of pepper and salt well mixed together, Fig. 6. This structure is substantially the same for all

Jan 1, 1920

By J. Geertsma, F. de Klerk

During the hydraulic fracturing treatment of an oil or gas well the liquid pressure in the borehole is increased until tensile stress in the surrounding rock exceeds tensile strength. Once a tensile fracture is initiated, it is penetrated by liquid from the borehole and fracture propagation under continuous hydraulic action takes place. The fracturing liquid carries a propping agent to ensure a highly permeable flow channel after pressure release. Field results range from failure to obtain increased production to outstanding success. In all cases, however, it unfortunately remains uncertain whether the values chosen for the operational parameters, such as injection rate, pumping time and fluid viscosity, were in fact the ideal ones. Though experience provides a lead, a more satisfactory way to predict results would seem to be to subject the fracture propagation process to a theoretical analysis that (1) makes the maximum use of the relevant physical information and (2) so simplifies the resulting calculations that the field engineer gets practical data that he can handle comfortably. We are attempting here to do this in connection with the prediction of fracture width and areal extent before pressure release. What remains of the fracture afterwards depends on the distribution of the propping agent between the fracture walls, and that is a separate story. Idealization of the Problem To keep the problem tractable, a number of simplify- ing assumptions have had to be made: 1. The formation is homogeneous and isotropic as regards those of its properties that influence the fracture-propagation process. 2. The deformations of the formation during fracture propagation can be derived from linear elastic stress-strain relations. 3. The fracturing fluid behaves like a purely viscous liquid; i.e., any peculiar flow behavior due to the addition of gelling agents or other additives is neglected. Moreover, the effect of the propping agent distribution on the distribution of fluid viscosity in the fracture is not taken into account. 4. Fluid flow in the fracture is everywhere laminar. 5. Simple geometric fracture-extension patterns are assumed — either radially symmetrical propagation from a point source (Fig. 1A) or rectilinear propagation originating from a line source (Fig. 1B). In the first case the periphery of the fracture is circular, in the second case it is rectangular. 6. A rectilinear propagation mode can be accomplished only by injection over a large perforated interval, thus forming a line source. Such a rectilinear fracture must therefore be located in the vertical plane. A circular propagation mode might be expected from injection through a narrow band of perforations. This forms a point source. Because gravity effects are excluded from our considerations, the fracture propagation plane may in this case assume any angle with respect to the wellbore as far as the

Jan 1, 1970

By J. F. Breedis

The stabilization of austenite in Fe-Ni alloys against martensitic transformation after reversion has been attributed' to the lattice imperfections remaining from previous transformation. More recently, however, such stabilization has been associatedzy3 with compositional changes which occur in martensite during slow heating. Dislocation arrangements in deformed austenitic stainless steels strongly influence transformation to martensite on quenching.4 Therefore, it is of interest to observe the transformation behavior of stainless steel after reversion, especially since previous studies have been confined to Fe-Ni alloys. The transformation-product morphology also differs in the two iron-alloy systems;6 plate martensite forms in the latter while stainless steel transforms to lath-type martensite. Samples of Fe-16 wt pct Cr-12 wt pct Ni (maximum C + N = 0.005 wt pct, 0 = 0.02 wt pct), prepared by vacuum melting and casting from high-purity components, were annealed at 900°C for 24 hr, after cold rolling to produce a 40-p grain diameter. The M, temperature of this alloy is -80°C and samples are fully austenitic after annealing. The amount of martensite present after quenching, annealing, and requenching was determined magnetically, to within 0.01 wt pct, using a vibrating specimen magnetometer. Nearly 14 pct of martensite forms during the initial quench in 1 min at -196°C. Two-min and 2-hr anneals were done in air and in evacuated quartz capsules, respectively. All specimens were electro-polished before making the magnetic measurements.

Jan 1, 1967

By R. H. Winn

A method for the selection of the most suitable corrosion inhibitor for a particular system is given. The method involves the evaluation of surface passivity by means of copper ion displacement after the metal surface has been subjected to the corrosive atmosphere. The application of the method to the selection of suitable inhibitors for use in producing wells is described. Correlation with recognized laboratory tests has beet1 found to be good within the limitations of the test. The use of the test to evaluate inhibitor persistencc is described. INTRODUCTION Corrosion as it is associated with the industry shows wide variations in its qualitative as well as its quantitative aspects. This complicates the work of the corrosion engineer. In the past few years the efforts of the corrosion engineer have been further taxed by the large numbers of products being marketed as corrosion inhibitors by various manufacturers. These products are submitted to him together with a limited amount of data to support their use as inhibitors. The data are usually authentic and reliable yet all too often when these products are applied to an actual corrosive system the results are disappointing due to the ineffectiveness of the inhibitor and the corrosive system. The corrosion engineer must select a comparatively limited number of inhibitors for field trial from the large number available. The selection is usually made on the basis of a standardized laboratory test such as that adopted by the National Association of Corrosion Engineers or by field experience in an area; however, testing of this type is discouraging on large numbers of compounds, particularly in view of the specificity of environment. It has been an object of this work to devise a method which will allow the corrosion engineer to select the best inhibitor for a specific environment under field conditions. The test would of necessity be rapid and inexpensive. It would preferably eliminate the need for expensive and delicate instruments. STATEMENT OF THEORY The test as developed makes use of the fact that metal ions will be displaced from solution by metals having a more positive electrode potential. Thus, if an active iron surface is exposed to a solution of a copper salt, free copper will plate spontaneously on the iron surface as it is displaced from the salt solution by iron ions. If the iron surface is passified, as by coating with an insulating-type organic corrosion inhibitor, it is no longer capable of displacing the copper ions due to its own limited ionization. The result will be a change in the amount of copper plated upon exposure to a neutral copper salt solution. In practice it has been found possible to measure the magnitude of the alteration of the cell potential by determining the copper deposited on a standard iron surface under controlled conditions. This means that, as the film builds up, the resulting shift in the electrode potential tends to cause the iron surface to act more like a noble metal, resulting in a reduction in the cell potential to a point that copper will no longer plate spontaneously. Obviously, the salts of other metals such as silver, gold or platinum might be used for this operation; however, copper was selected because of the color difference of the plate, the comparatively low cost of copper salts and the ease of evaluation of the plated copper. Furthermore, its high cell potential provides a substantial driving energy. The determination of the copper is readily done colorimetrically by dissolving it in 5 per cent ammonium hydroxide solution containing 2 per cent potassium per-sulfate. The blue color of the copper ammonic complex ion so developed may be compared with standards prepared by dissolving known quantities of copper powder in the same reagent. In routine screening it is seldom desirable to determine the amount of copper plated. It is usually more important to determine the concentration of inhibitor required to prevent the plating of copper.

By C. S. Samis, D. P. Seraphim

In the presence of oxygen, galena is oxidized in an aqueous medium containing ammonium acetate in accordance with the following reaction: PbS + 1/2 0, + 2 NH~Ac -» PbAc, + So + 2 NH: + H2O. This reaction was studied in an autoclave under oxygen pressure by polarographic measurement of the concentration of lead ion in solution. Oxidation rate is parabolic. The reaction products are lead acetote and elemental sulfur, the latter forming a film on the galena crystal. Reaction kinetics appear to be determined by the diffusion of lead from the galena phase to the solution interface through the film of sulfur. RECENT applications of pressure leaching on a commercial scale have emphasized the metallurgical importance of the oxidation of sulfide minerals in aqueous media by oxygen under pressure. Research experience has shown that sulfates, thio-nates, and metal oxides are the products of humid oxidation of sulfide minerals in basic solutions. The metal oxides may be solubilized in the presence of a complexing ion.' Certain oxide minerals are also amenable to treatment by this type of oxidation.' Several kinetic studies have been made of reactions of this type. Stenhouse' found that pyrite (FeS?) oxidized in a sodium hydroxide solution to produce a soluble sulfate and an insoluble layer of iron oxide and that the kinetics of the reaction were controlled by oxygen diffusion through the oxide layer. Andersen' studied the oxidation of galena (PbS) in a sodium hydroxide solution under oxygen pressure. He found the lead and sulfur to be simultaneously oxidized to produce plum bite ions and sulfate ions, and that the reaction rate was proportional to the surface area of the galena. The kinetics appeared to be determined by the reaction of oxygen and water with the galena surface. In each of the above reactions the metal and sulfur components of the mineral were oxidized simultaneously and at equal rates. In the present study the alkaline medium has been replaced by an approximately neutral solution of ammonium acetate in which lead sulfate is soluble. Under the conditions no sulfate was produced and no sulfur could be detected in the solution. The metal component of the mineral was solubilized and the liberated sulfur remained as a film of elemental sulfur on the surface of the galena crystal. A kinetic study of this reaction was undertaken to establish the kinetic mechanism and to determine the rate controlling step. Specific reaction rates were determined by oxidizing crystals of galena of measured surface areas in an autoclave maintained at the desired temperature and oxygen pressure. The rate of reaction was followed by measuring the concentration of lead in the ammonium acetate solution with a cathode ray polarograph, employing stationary platinum electrodes incorporated in the autoclave. Experimental Materials and Equipment Crystals of galena obtained from Violamac Mines, Retallack, B. C., were selected for oxidation because

Jan 1, 1957

By W. C. Phalen

The production of salt in the United States divides itself at the outset into two distinct classes…

Jan 1, 1915

By J. H. Brophy, M. H. Kamdar, J. Wulff

A constitutional diagram for the Ta-W-Re alloy system is presented. Rhenium dissolves in the complete range of solid solutions between tungsten and tantalum up to 48 wt pct in tantalum 'to about 30 wt pct in tungsten. Intermediate x and u phases only are found. X-ray diffraction and fluorescence, metallography and melting-point measurements were employed. THE constitution diagram of ternary alloys of tungsten, tantalum, and rhenium for temperatures above 1000°C is reported in this paper. Alloys in this system rich in tantalum and tungsten are of interest for high-temperature applications, and those rich in rhenium for electronic applications. No ternary phase diagram appears to be available in the literature. The three-component binary diagrams have been previously established1-3 and the present ternary data are consistent with these. EXPERIMENTAL TECHNIQUES Commercially pure tantalum (99.7 pct), rhenium (99.99 pet), and tungsten (99.9 or 99.95 pct) powders were purchased from Fansteel Metallurgical Corp., Chase Brass and Copper Co., and Fansteel or Westinghouse Electric Corp., respectively. These powders were pressed without binder and arc-melted under helium. The preparatory and analytical techniques employed were identical to those used for the Ta-Re system investigation carried out in this laboratory.324 These included X-ray diffraction and metallographic phase identification, X-ray fluorescent and wet chemical analyses, solidus determinations and heat treatments in a resistance-heated tantalum-filament vacuum furnace. For microstructural examinations standard mechanical polishing techniques were used through diamond laps. Polished speciments of all compositions were etched by swabbing with 4 parts HI?, 4 parts HNO3, and 1 part H20. Since the microstruc-tures of alloys containing one or two phases closely resembled their counterparts in the respective binary systems, typical examples are omitted in this presentation. In all the alloys examined, it was possible to observe the number of phases present. Particularly when there were small amounts of one phase involved, it was possible to identify it only by a combined conclusion based on X-ray diffraction, position of an alloy in a composition series, and the phase rule. A total of 100 different alloy compositions was arc-melted and studied in the as-cast condition metallographically and by X-ray diffraction. Specimens of each of these compositions were heat-treated at 2680, 2530, and 2020°C for 1, 2, and 4 hr, respectively. Those which were treated at 2020 were given a preliminary homogenization treatment at 2500°C for 1 hr. Specimens of 25 alloys were heat-treated at 1200o C for 168 hr. Solidus temperature measurements were made by the detection of incipient melting in eighteen alloy compositions. The metallographic and X-ray diffraction results are summarized in Table I. Graphically, this information appears in the isothermal plots of Figs. 2 and 3. Within the accuracy of the experimental methods, two such plots are sufficient to locate these data, since the results for 1200°C were similar to 2020 and those at 2530 resembled 2680

Jan 1, 1962