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THE 125th meeting of the Institute was held in New York, Feb. 20-23, 1922, inclusive, and was the most successful annual meeting of the Institute ever held; there was a larger registration, there were more sessions of importance, and a greater number of sessions, than in any previous year. The total registration was 1331, comprising 351 New York members, 393 visiting members and 587 guests. At the annual business meeting of the Institute, held on Tuesday, Feb. 21, with President Ludlow presiding, there was a much larger attendance than usual. The report of the tellers was read and the following officers were declared elected: Arthur S. Dwight, Director and President-District 0 J. V. W. Reynders, Director and Vice-president-District 0 A. R. Ledoux, Director and Vice-president-District 0 Charles F. Rand. Director-District 0 George D. Barron, Director-District 0 William H. Bassett, Director-District 1 Thomas B. Stearns, Director-District 8 William Kelly, Director-District 5

Jan 3, 1922

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

By Cyril Wells, Paul E. Busby, Donald P. Hart

EARLY workers in the field have established that the diffusion of nitrogen follows normal diffusion laws. Concentration-penetration data from layer analyses of reasonably pure iron specimens nitrided in an atmosphere of CO-NH, are given in the literature,' and were utilized to calculate diffusion constants for nitrogen. The diffusion of nitrogen in y-iron may be represented approximately by the equation D - 1.07x10-' e-:".'m'"'r The diflusion coefficients, D, given by this relation represent mean values, since carburization occurred simultaneously with nitriding. The rate of diffusion in a-iron has been determined from calculations based on data obtained by measuring the internal friction of samples at each of several frequencies and temperatures.' The expression for the diffusion of nitrogen in a-iron derived from these experiments is D= 1.4x10-1 e-it tudent Increasing carbon content decreases the diffusion of nitrogen in a-iron.3 Oxygen, either dissolved or combined, has been shown' to exert a marked influence on the diffusion of nitrogen from a nitriding atmosphere. D values increase rapidly with increasing amount of dissolved oxide in the metal, but diffusion is completely inhibited if preliminary oxidation has produced the slightest trace of iron oxide on the surface. Diffusion coefficients have also been calculated from permeability and solubility data,' but these values are of questionable accuracy since the boundary conditions assumed may not actually exist. Experimental Method The method selected for determining the diffusion coefficient of nitrogen in a-iron in the present investigation was the so-called fractional saturation method. This method consists of heating the specimen in an atmosphere of H2-NH8 mixtures of known composition for a predetermined time. Following this treatment, the specimen is analyzed for nitrogen; and the diffusion coefficient is calculated from a known relationship of the fractional saturation, time of diffusion, and dimensions of the specimen. This relation is based on a solution of Fick's second law and assumes that the surface of the specimen immediately reaches a given concentration which remains constant during the diffusion anneal. Tabular solutions are available4-5 and provide the relationship between fractional saturation and the quantity \/Dt /a, where D is the diffusion coefficient in cm2 per sec, t is the time of the diffusion anneal in seconds, and a, in the present experiments, is the half-thickness of the slab specimen in cm. The method is adequately discussed elsewhere.9-10 Material The material for this study consisted of 3/32 in. thick (0.24 cm) carbonyl iron plate. The major impurities in this iron are oxygen and carbon, which are readily removed by long time high temperature treatment in an atmosphere of purified hydrogen. In order to reduce the diffusion anneal time for saturation runs, some of this material was rolled to a thickness of 0.015 in. (0.038 cm) prior to the hydrogen treatment. Hydrogen treatments were carried out in a hydrogen-purified Armco iron tube heated in a global

Jan 1, 1957

By M. Felsenthal

Engineers are frequently faced with the problem of having to predict oil recovery from a solution gas drive reservoir in the early life of a field. This is often the time when actual laboratory or field-derived gas-oil permeability (kg/k0) data are not yet available. Although excellent collections of k0/k0 data for various types of rocks may be found in the literature,1,2,3 a need exists for a more detailed correlation of k0/k0 data with core properties such as porosity, permeability, clay content or pore-size distribution. It is the purpose of this article to present this type of correlation for sandstone material. The correlation is based on laboratory tests performed on over 300 core samples from 19 reservoirs in the United States and Canada. EXPERIMENTAL Cores were analyzed by routine procedures, using samples of conventional size (7/8-in. diameter, 7/8-in long) cut parallel to the bedding planes. Air permeability was measured at 1.67 atm mean pressure in a Hassler-type apparatus. Porosity was determined with the aid of a Ruska bulk volume meter and a Boyle's Law rock volume meter, An evaporation method' was used to evaluate irreducible water saturations. Core samples were saturated with 25,000 ppm NaCl brine. The brine was reduced to the irreducible saturation, and the remainder of the pore space was filled with kerosene. This was followed by multiphase flow tests using the so-called "dispersed feed" technique.5 n this technique, gas and oil (kerosene and kerosene-saturated air) were dispersed with the aid of a porous Alun-durn feed head, the face of which contained a waffle-shaped system of Lucite-lined grooves. Oil entered the back side of the feed head and emerged at the raised areas of the front face. Gas was introduced directly into the system of grooves at the front face. The gas-oil mixture then entered the test core which was kept in capillary contact with the feed head. Permeabilities were determined from rate and pressure measurements and saturations from weights. All determinations were performed at equilibrium or steady-state conditions. Pore-size distributions were determined on selected samples by a mercury injection technique.6 GENERAL CORRELATIVE TRENDS When examining data from a given reservoir, it was noted that k0/k0 vs saturation curves became generally less steep as specific air permeability increased, a development that has a favorable effect on oil displacement efficiency by solution gas drive. This trend has also been reported by others in the literature.' An effect of porosity on k0/k0 data was also noted. This effect was not generally discernible in a study of relative permeability data for a given reservoir but became apparent when data for sandstone reservoirs of similar lithology but differing average porosity were compared. For instance, in a comparison of argillaceous and/or calcareous sandstones from 11 reservoirs ranging in average porosities from 14 to 28 per cent, a definite trend was noted, indicating that for a given permeability k0/k0 curves became less favorable (i.e., steeper) as porosity increased. A similar trend was observed for a group of comparatively clean sandstones from five reservoirs ranging in average porosities from 15 to 21 per cent. For a given permeability and porosity, comparatively clean sandstones gave more favorable k0/k0 curves than argillaceous and/or calcareous sandstone or chert reservoirs. The laboratory studies also showed that least favorable k0/k0 curves were exhibited by shaly sandstone, conglomerate, and sandstone containing carbon inclusions. Table 1 lists the various source reservoirs classified by lithology types. To facilitate a correlation of k0/k0 data with core characteristcis, it was found expedient to work with

By Thomas C. Wilder

Jan 1, 1965

By A. Raja, C. C. Harris

Apparatus for maintaining constant — but adjustable — pulp level and rate of froth removal are described. The results of preliminary experiments into the effect of scraping speed on the rate of solid and liquid recovery with a semi-batch system are presented. Glass spheres restricted to a narrow size range is the solid under investigation. Graphical methods for estimating the mass of recoverable material and the zero error are given. The semi-batch procedure1 is extensively used in laboratory flotation testing, though the method is subject to variability of moderate severity. Raffinot2 concluded from a statistical study of the difference between replicate tests, that the ptincipal source of errot was the test itself and not sampling or chemical analysis. These differences can be ascribed principally to changes in pulp volume and reagent concentration, and uncontrolled rate and depth of scraping. Semi-batch testing has been criticized1 on these grounds as a means of investigating flotation kinetics. This paper discusses and describes modifications to laboratory flotation equipment which reduce the number of manual operations and lead to improved control. Kinetic studies were the primary reason for developing the apparatus described. It should, however be a useful aid in normal flotation testing. Some preliminary results of experiments are presented.

Jan 1, 1967

By R. J. Wensley

THE use of small substations for the supplying of 275-volt energy to the locomotive and cutting machines in coal mines is a well-established practice. A few years ago, when labor costs were lower, these substations were located as near to the load as possible, and an operator was provided for each station. This practice has now become so expensive that substations are being located with reference to other mining machinery, such as hoists or pumps, so that one operator can look after both. Some-times the substation is operated by one whose duties make him traverse quite a large area. In such cases the interruption of alternating-current supply may produce a long interruption in the direct current, as the station cannot resume service until this man reaches it. Such interruptions interfere seriously with production and may easily counterbalance the supposed saving gained by such operating methods. The grouping of substations for convenience in operating may also result in excessive copper loss and consequently poor trolley voltage, with its attendant evils of low locomotive speeds and increased locomotive motor maintenance. The speed of the coal-cutting machines will also be reduced. By relieving the substation of its, burden of the operating labor cost, the most economical location, from an electrical standpoint, may be chosen. The matter of machine insurance should also be considered. If an attendant is caring for several kinds of equipment, he cannot watch the machine continually for signs of trouble; therefore, continued overload, phase failure, low alternating-current voltage, bearing trouble, etc. may result. Some partly automatic equipments have been installed; these have protection against low voltage, reverse current, and bearing trouble and are provided with automatic reclosing circuit breakers. This is a step in the right direction but it does not go far enough to give first-class machine insurance.

Jan 9, 1921

By E. H. Boswell, E. M. Cushing

The Mississippi embayment east of the Mississippi River is part of a vast geologic and hydrologic province. The abundance of water available is largely responsible for the agricultural history of the area and is perhaps the key factor in the rapidly accelerating trend toward industrialization. The multiple artesian aquifer systems that underlie the region and the alluvial aquifer along the Mississippi River are virtually undeveloped sources of fresh water in that they are yielding only a fraction of the water available. The potential yield of the 12 aquifer systems is estimated to be about 25,000 mgd (million gpd) of which only about 600 mgd is presently being withdrawn. The amount of water in storage in these systems is about 1600 trillion gal. Ground water having a dissolved-solids content of less than 500 ppm is generally available at depths of less than 1000 ft, and water having a dissolved-solids content of less than 1000 ppm is available in some places to depths of more than 3000 ft. Iron is the most common troublesome chemical constituent in the ground water. Water in varying amounts is also available from streams within the region. The amount of water which originates within the region and which leaves it as streamflow during a year averages about 50 million acre-ft (about 45,000 mgd). An additional 375 million acre-ft (about 340,000 mgd), which originated outside the region, leaves the region as streamflow during an average year. Some streams have considerable flow during periods of no precipitation and the water during these periods generally has a low dissolved-solids content. Large quantities of water from streams and waterbearing sands (aquifers) are available in the Mississippi embayment east of the Mississippi River. Most of the region is underlain by aquifer systems that will yield large quantities of water to wells, making ground water the most readily available source of fresh water. About 90% of the water used in the region is obtained from wells. Streams have been used primarily to dispose of, and dilute, wastes that have been dumped into them. The Mississippi, Ohio and Tennessee rivers, and the lower parts of the Tombigee and Yazoo rivers also serve as a means of transportation. This nominally water-rich region receives from 48 to 56 in. of precipitation in average years and is crossed by several large rivers. The largest, the Mississippi River, is the western boundary of the region discussed in this paper. The economy of the region is basically agricultural, but industry has become increasingly important since World War 11. The diversification and mechanization of agriculture have resulted in a surplus of manpower, most of which is being absorbed by the expansion of industry. Further industrial expansion probably will occur because of the available manpower, natural resources and economical transportation. Increasing demands on available water supplies will be made and the future economic growth of the region will be largely dependent upon wise utilization and management of the water resources.

Jan 1, 1969

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 D. A. Elgillani, M. C. Fuerstenau, J. D. Miller

Adsorption of lead and ferric iron on quartz and alumina is presented as a function of pH. Only the hydrolyzed species of these metal ions, FeOH++ and PbOH+, adsorb significantly on each of these minerals. Zeta potentials of quartz were measured as a function of pH in the presence of various additions of aluminum, lead, and magnesium salts. Sign reversal occurs at the pH values where significant concentrations of hydroxy complexes are formed. Models of adsorption are presented in the absence and presence of collector. The mechanism of adsorption of metal and collector species in the activation of nonmetallic minerals is still the center of considerable discussion in spite of the extensive study given this system. Until recently, the view was widely held that hydrated metal ions were responsible for this phenomenon. This fact is surprising, since it had been shown that the pH range in which flotation is effected corresponds to that in which metal ion hydrolysis occurs.' Additional support of this concept was pro vided by the work of Wolstenholme and Schulman in another system.' Later work has shown that hydroxy complexes of metal ions are the active species. These studies have also indicated that basic aqueous complexes of metal-collector may be necessary for flotation.3-7 Depending on the molecular weight of the collector, formation of these complexes may occur before or after precipitation of the metal-collector salt has occurred. Ion pair formation can occur when low molecular weight collectors are involved because relatively high concentrations of metal hydroxy complex and collector can be present in solution before precipitation occurs. This is not the case when high molecular weight collectors are used. A model of aqueous complex adsorption has been presented6,7 in which it has been assumed that adsorption occurs by the formation of water from adsorbed hydroxyl and hydrogen of the hydroxyl contained in the complex. Other authors8 have suggested that hy-droxy complexes are involved in these systems but that collector adsorption occurs by replacement of the hydroxyl of the adsorbed metal hydroxy complex with a fatty acid anion. All of these investigations have involved mineral surfaces that were negatively charged so that it is not possible to state with certainty whether hydrated metal ions or hydroxy complexes are the active species in this system. Use of a positively charged mineral should be helpful, however, since the hydrated metal ion will be repelled from this surface. On the other hand, if the hydroxy complex adsorbs by splitting out water, surface charge should have no effect because of the free energy decrease that the system will experience when water is formed. In this regard, sapphire is well-suited for study, since its surface is positively charged until approximately pH 9. Electrokinetic studies of quartz in the presence of various metal ions should also be useful in establishing the mechanisms of adsorption in these systems. That is, if the hydroxy complexes adsorb by water formation, drastic changes in the zeta potential should occur in the pH range in which hydrolysis occurs. In this view, adsorption of ions of widely different hydrolysis characteristics on both sapphire and quartz was measured. In addition, zeta potentials of quartz were measured as a function of pH in the presence of various metal ions and compared with flotation responses obtained under similar conditions. Experimental Materials and Techniques Reagent-grade aluminum, ferric and magnesium chlorides, and lead nitrate were used in this investigation. Adjustments in pH were made with reagent-grade HCl or KOH. Conductivity water, made by passing distilled water through an ion exchange column, was used in all of the experiments.

Jan 1, 1971

By AIME AIME

The Washoe plant, 1 in Anaconcla. Mont., together with the local street-railroad, ranches a. foundry and machine-shop a brick-plant and the Montana hotel, form a property under one management; to which should be added the mines in Butte owned by the company, from which part of the ore-supply of the plant comes. The Anaconda Copper Mining Co., controlled by the Amalgamated Copper Co., was reorganized under the laws of Montana in 1893. A map of the plant, showing the numerous departments and illustrating the details of tracks, pipe-lines, and charging-stations for compressed-air locomotives, is given in Fig. 1.

Jul 1, 1906

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 E. C. Stephens

The eastern Washington— Idaho clay region stretches along the northeast margin of the Columbia basin for 150 mil es. The three better known and developed clay areas are Clayton, Wash., (2 miles north of Spokane); Mica, Wash., (10 miles southeast of Spokane); and Moscow-Deary-Bovill, Latah County, Idaho (about 80 to 90 miles southeast of Spokane) see Fig. 1. Clays from the eastern Washington— Idaho clay area have been mined for more than 50 years. At present Mica, Washington deposits are used by the Gladding—McBean & Co. to make a variety of bricks and ceramic products and Latah County, Idaho clays are used by the A. P. Green Fire Brick Co. to make refractories. The Anaconda Co. made an intensive investigation of the clay deposits in the northeastern Washington-!daho area in 1919 to determine the existence of a supply of raw materials from which alumina could be made. The greater part of the work, which included systematic drilling and shaft sinking, was concentrated at Mica, Wash. This was part of a research project carrted on by the Anaconda Metallurgical Research Dept. under the direction of Frederick Laist and F. Frick and it was terminated in 4920. V. D. Perry, Vice President and Chief Geologist for The Anaconda Co., in 1952 assigned the writer to make a preliminary study of clay and other potential sources of alumina ore in the Pacific Northwest with particular emphasis on those deposits which might be of future importance to The Anaconda Co9s. then new aluminurri plant at Columbia Falls, Mont.

Jan 1, 1961

By J. D. Rice, S. C. Pitzer, C. E. Thomas

Interpretation of pressure build-up data obtained in the conventional manner has often been difficult because of the deviation from theoretical behavior. Major causes of this deviation have been attributed to damage and afterflow, and to fluid redistribution in the wellbore which, in extreme cases, can result in a pressure hump in the early portion of the build-up curve. Theoretical investigations show that bottom-hole pressure is definitely influenced by phase redistribution in the tubing column during surface shut-in tests, and that the magnitude of the effect is sensitive to the producing gas-oil ratio and stabilized rate of flow in the well. For field experiments a wire-line tubing packer, which can be run in the tubing against a stabilized flow rate, was developed for bottom-hole shut-in tests. By use of this bottom-hole .shut-in method, pressure humps previously observed in surface shut-in tests were completely eliminated and the effects of afterflow minimized. Analog and digital computer studies have been made to obtain theoretical curves for comparison with field curves, and remarkable agreement between the results of bottom-hole shut-in tests and theoretical curves has been obtained. INTRODUCTION Pressure build-up data from shut-in wells have been used by the petroleum industry to determine the permeability of the formation, to estimate wellbore damage, to evaluate the static reservoir pressure and to speculate reservoir volume. Calculation of these factors is based on methods of analysis developed for theoretical systems whose build-up curves have a charac- teristic shape when the wells are shut-in at the sand faCe.1,2,3,5,8,10 However, field curves obtained by conventional surface shut-in methods do not always exhibit this characteristic. Such factors as stratification, rock heterogeneities and irregular reservoir geometry can cause the character of a build-up curve to deviate from that predicted by theory for a simple system. In addition, all field build-up data are affected by the methods utilized in obtaining the measurements. Conventional surface shut-in techniques allow two effects to occur which contribute directly to the manner in which pressure builds up at the sand face. The first, afterflow, has been recognized for some time and methods are available for estimating the magnitude of its effect and for correcting its influence.' The second, phase segregation in the tubing column after shut-in, has been reported only recently and appears to exert a considerable influence on the character of field build-up curves.!' In extreme cases, phase segregation can produce "pressure humps" in the early portion of the build-up curve. Such curves have been considered anomalous and have defied analysis. It is the purpose of this paper to discuss the effect of phase segregation in the tubing string during build-up and to present a bottom-hole shut-in technique for obtaining field build-up data which minimizes the influence of afterflow and eliminates phase segregation effects. It will be shown that reliable reservoir information can be calculated from build-up measurements obtained using this method, even though conventional surface shut-in tests on the same wells yield anomalous data. DISCUSSION OF PHASE REDISTRIBUTION EFFECTS Some of the effects of phase redistribution on pressure build-up curves have been described previously by Matthews and Stegemeier" who have presented evidence that phase segregation is responsible for the pres-

By F. J. Chernosky

Most previous studies of coal flotation utilized chemically pure reagents. Since such reagents are not available in quantity, a study of various wmmercially available reagents as frothers was undertaken. Flotation procedures similar to those used in a large number of commercial coal flotation plants were employed. The reagents used were compared on yield-selectivity-wst basis. The selectivity was found to be relatively constant with yields above 70% but the reagent cost varied greatly. The types of reagents available were compared. In the past, a number of papers have been written on the use of various reagents as coal flotation frothers. For the most part, these have been an attempt to correlate the intrinsic chemical and physical proper- ties of the reagents or reagent groups to the floata-bility of various fine coals. Because of the type or nature of evaluations made, chemically pure reagents were normally used. Generally, these reagents are unavailable in commercial quantities. Therefore, the results obtained with these reagents were usually limited in usefulness to the plant operator or metallurgist. This paper presents the results of a study in which commercially available forms of various reagents were used as flotation frothers. Flotation procedures which would conform in general to those employed in a large number of commercial coal flotation plants were utilized. The objective of the test was to compare these reagents on yield-selectivity-cost basis, that is, 1) the yields obtained, 2) the ash levels obtained and 3) the reagent cost relating to these results. REAGENTS The reagents employed have been grouped into the following chemical classes: 1) aliphatic alcohols, 2) terpines, 3) glycols (synthetic water-soluble

Jan 1, 1963

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

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 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 John Nunes, Frank R. Larson

Temperature-dependent functions of various ten-sile flour stress and fracture parameters were investigated on iron and low composition alloys of Fe-C, Fe-Cr, Fe-Mn, and Fe-Ni. Data were obtained over a range of test temperatures from 200" to -196"C at an initial strain rate of 0.01 min". It was found that the strain-hardening exponent, n, for the Fe-Ni alloys increased significantly at very low testing temperatures with increased alloy addition. Also, the stress and strain at fracture followed a predictable transitional type of behavior. The flour stress-temperature dependence was evaluated employing the relation: M where it is shown that composition can strongly influence the constant M. An empirical formula describing this effect is as follows: M = MI (equivalent at. pct Ni)-'" Some preliminay, tests were run on several commercial steels to test the generality of this relationship. One of the phenomenological explanations of the ductile-to-brittle transition encountered in bcc metals is based upon the difference in the temperature dependence of the flow and fracture stresses.' It states simply that the fracture stress is relatively insensitive to temperature and that the yield or flow stress rises rapidly with decreasing temperature so that, when the flow stress reaches the fracture stress, brittle fracture occurs without appreciable plastic deformation. This behavior is illustrated schematically in Fig. 1 where the ductile-to-brittle transition is shown to occur at two possible temperatures. The lowest temperature, TB, represents essentially completely brittle behavior while the higher temperature, TN, represents "notch" brittle behavior. Support for this theory is obtained when it is observed that fcc metals, which do not commonly have a ductile-to-brittle transition, also do not commonly exhibit any strong temperature de- pendence of the yield stress. This relationship of yield or flow stress behavior with the ductile-to-brittle transition has been generally observed for most metals representative of these two crystallo-graphic structures. One exception to this generalization appears in the case of tantalum where no apparent ductile-to-brittle transition has been observed. However, this may simply be an indication that this type of behavior is not directly related to the flow stress and that some other mechanism such as twinning must also be operative. A comparison of the typical temperature dependence of the yield stress of some representative metals is shown in Fig. 2. In the study of the temperature dependence of the strength of metallic materials, considerable ef-

Jan 1, 1963