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By W. A. Turcotte, A. D. Paananen

Introduction The large reserve of fine grained oxidized iron-formation at the Tilden mine has been the object of research and development efforts to concentrate the iron oxides as far back as 1949. Due to the nonmagnetic nature of the ore and the fine grinding required to liberate the iron oxide minerals, this crude ore was not amenable to concentration by conventional methods. The iron oxides of the Tilden, ore body have a grain size of less than 25 microns and recovery of the finer, well-liberated iron oxides is essential. Conventional methods of desliming employing cyclones or thickeners were not feasible because of the excessive loss of iron oxides in the finer fractions. Development of selective flocculation-desliming was a key to commercialization of the process. Operations started in late 1974 with Algoma Steel Corp. Ltd., J & L Steel Corp., The Steel Company of Canada Ltd., Wheeling-Pittsburgh Steel Corp., Sharon Steel Corp., and The Cleveland-Cliffs Iron Co. as participants. Cleveland-Cliffs operates and manages the operation. Development of the Tilden Flowsheet The geology and ore reserves of the Tilden mine have been detailed in a paper by Villar and Dawe (1975). A joint program was undertaken in 1961 with the US Bureau of Mines in Minneapolis using the flowsheet developed by the Bureau employing the selective flocculation-desliming and calcium activated anionic silica flotation method (Frommer, et al, 1966; Frommer, 1964; Frommer, Wasson, and Veith, 1973). During this time, parallel testing at Cleveland-Cliffs Research Laboratory and Pilot Plant centered on the same type of desliming but was followed by the cationic flotation of silica with amine collectors (Columbo and Jacobs. 1976). The cationic silica flotation system was eventually chosen for its overall efficiency and simplicity. Regardless of the flotation method chosen, the technique of selective flocculation-desliming prior to flotation is the key to the success of the process. The flowsheet is described in detail by Villar and Dawe (1975). [Figure 1] shows a simplified one-line flowsheet of the Tilden concentrator. A total tailings thickener has been added to the original flowsheet and was placed in operation in 1978. The total-tailings thickener overflow reports to the reuse water pond and the underflow is pumped approximately 8 km (5 miles) to a storage basin. A flowsheet of the reuse water system is shown in [Fig. 2]. Selective Flocculation-Desliming Data have been published on the mechanisms and factors affecting selective flocculation in iron oxide-silica systems. The intent of this paper is not to discuss the theoretical aspects of selective flocculation, but rather to present experience gained from the commercial Tilden operation and from bench and pilot plant testing of fine-grained oxidized iron ores. From the bench and pilot plant testing prior to plant startup, certain reagent combinations and rates for the commercial Tilden plant were established. In the experience gained from three years of plant operation at Tilden, some of these reagent dosage rates have required significant adjustments due to changes in reuse water quality and to meet the requirements of varying ore types. Reuse Water The process water quality is a major concern at the Tilden mine and is constantly being monitored for selected chemical and physical characteristics. This monitoring has continued on a regular basis in order to gain a more thorough understanding of the interactions taking place in a dynamic water system and particularly as water quality is influenced by seasonal variations. Control of the reuse water chemistry is essential to the Tilden process both in the selective flocculation-desliming and flotation stages of concentration. With roughly 75% of the reuse water used in grinding-desliming operations, it is readily apparent that the biggest "reagent" in the selective flocculation-desliming process is water. Not enough can be said about the close control that must be exercised on the overall reuse water system. Control of the chemical treatment of the feed to the total tailings thickener is of utmost importance in order to produce a reuse water for the concentrator that is compatible with all stages of the concentrating process. There are many analyses made which aid in judging the quality of the water. Some of these are shown in [Table 1]. Five are particularly important and are monitored daily so that reagent adjustments can be made as required: suspended solids, calcium hardness, pH, dissolved silica concentration and temperature.

Jan 1, 1981

By Foster Fraas

Most commercial electrostatic separators utilize the electrical property of conductivity, but although based on the same principles, they are constructed in a variety of forms, a common one being the simple roll type. Some information obtained during an investigation of that type of separator, and which indirectly is applicable to other types, is presented here. In Fig. I material discharged from hopper 6 is fed onto grounded rotating roll 2. Electrode 3 is at a high electrical potential with respect to roll 2, and any conductive particle in contact with roll 2 therefore acquires an electrical charge of such polarity that, when present in the electrical field, the force on it is in the direction of electrode 3. A detailed description of the charging by conductance as utilized in electrostatic separators may be found in a previous publication.' As a result of this force, the path of the projected particle is changed in increasing amounts in the direction toward region C as the magnitude of the charge is increased. With the dividing edge 4 the projected particles may be divided into two fractions —those in region C designated as "deflected" or"deflectant"and those in region B designated as "residue." When material is passed over the roll only once, a complete separation is seldom obtained, therefore most commercial separators contain several roll-separator units in series, and some practical machines use as many as I2. In this paper a "pass" means the passage of material over a single-roll unit. The procedure is to repass either residue B with a low potential on electrode 3 or deflectant C with a high potential on 3. Most electrostatic separations follow a flowsheet of roughing and cleaning either the concentrate or the tailing, or both. In a specific instance, a dry, heated mixture of wet cleaned chromite and garnet from an

Jan 1, 1943

By Foster Fraas

Most commercial electrostatic separators utilize the electrical property of conductivity, but although based on the same principles, they are constructed in a variety of forms, a common one being the simple roll type. Some information obtained during an investigation of that type of separator, and which indirectly is applicable to other types, is presented here. In Fig. I material discharged from hopper 6 is fed onto grounded rotating roll 2. Electrode 3 is at a high electrical potential with respect to roll 2, and any conductive particle in contact with roll 2 therefore acquires an electrical charge of such polarity that, when present in the electrical field, the force on it is in the direction of electrode 3. A detailed description of the charging by conductance as utilized in electrostatic separators may be found in a previous publication.' As a result of this force, the path of the projected particle is changed in increasing amounts in the direction toward region C as the magnitude of the charge is increased. With the dividing edge 4 the projected particles may be divided into two fractions —those in region C designated as "deflected" or"deflectant"and those in region B designated as "residue." When material is passed over the roll only once, a complete separation is seldom obtained, therefore most commercial separators contain several roll-separator units in series, and some practical machines use as many as I2. In this paper a "pass" means the passage of material over a single-roll unit. The procedure is to repass either residue B with a low potential on electrode 3 or deflectant C with a high potential on 3. Most electrostatic separations follow a flowsheet of roughing and cleaning either the concentrate or the tailing, or both. In a specific instance, a dry, heated mixture of wet cleaned chromite and garnet from an

Jan 1, 1943

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Jan 1, 1938

By R. Maddin, N. Ujiiye

ALTHOUGH the cold-rolled texture for body-centered-cubic metals and alloys is well known (see, e.g., Barrett'), the pole figure representing the texture may be interpreted in two ways. It may be regarded as consisting of several ideal preferred orientations with an associated spread (a view which is shared among several investigators2), or it may be regarded as consisting of two sets of continuous preferred orientation also with an associated spread."." Recently, Chen and Maddin7 noted a stable (001) [loo] end orientation for molybdenum single crystals rolled at low rates of reduction provided the initial rolling. orientation" was close to the cube ori-

Jan 1, 1957

By G. R. Purdy, J. A. Malcolm

The isothermal dendritic precipitation of y in p CuZnSn is compared with the isothermal formation of Widmanstatten a plates in p CuZn. Although both precipitates are evidently bounded by semicoherent interfaces, the dendritic shape of y evolves through smooth "sinuoidal" shape perturbations, while a-p interfaces tend to be strictly planar, or rnicroscopically faceted. An estimate of the average inter-facial free energy of cube-oriented y in p through the Mullins-Sekerka analysis indicates that it is low (of the order of 50 ergs per sq cm). Interface mication is apparently controlled by volunle dij'usion, and the observed anisotropy in growth probably results from anisotropy of inter facial free energy. Studies of the grain boundary precipitation of y in p indicate that the precipitate can grow in both $ grains, but becomes unstable with respect to the grain with which it shares a mobile semicoherent interface. Facets observed at the tips of Kurdjumov-Sacks-oriented Wid-manstatten a plates correspond to variants of an irrational hahit, near (231)0. Comparison with Hu and Smith's determination of relative interfacial free energies of a-(3 boundaries suggests that this system possesses an extremely deep o cup, which results in an ej'ective low-o zone. The possible effects of such a cup on the stability of a-p interfaces are discussed, a needles, grown during rapid continuous cooling, possess microscopically smooth interfaces, and are characterized by a high degree of' damage in the region of the boundaries. These boundaries, induced to move on tempering at 200"C, become faceted as equilibrium is approached, which seems to indicate that boundary structure and mobility in this system are dependent on the local degvee of departure from equilibrium MULLINS and sekerkal have elucidated the phase boundary stabilizing effect of surface tension. a factor not taken into account in previous treatments of morphological development. Their analysis applies to the isothermal growth of a pure spherical precipitate (planar in the limit of infinite radius) in a slightly supersaturated solution, under conditions of inter-facial local equilibrium and isotropy of interfacial free energy. More recently, several other factors which might tend to stabilize planar interfaces have received attention. These are: i) interface diffusion;4"8 and ii) slow interfacial reaction. cahn7 included a slight anisotropy in interfacial free energy, and showed that it has no stabilizing effect, but forces shape perturbations to reflect the anisotropy. shewmon4 noted that dendritic morphologies are rarely observed in solid-solid systems, and, in particular, postulated that slow interfacial reaction occurs at all boundaries between proeutectoid ferrite and austenite, except those which propagate parallel to {11 l)y planes (for Kurdjumov-Sachs [K-S] related phases). Previously, Aaronson~ had proposed interfacial reaction at the broad faces of Widmanstatten plates, and expected that the lateral motion of high-mobility incoherent ledge edges would produce planar precipitates bounded by law-mobility semi-coherent interfaces. The problem of interfacial reaction during the dif-fusional formation of precipitates has often been ignored, although it is apparent that a small component of chemical reaction must exist at any moving interface." Further, all solutions of the diffusion equations for boundary conditions corresponding to isothermal growth predict infinite growth rate at time zero, so that elements of interfacial reaction would be most easily detected at early times. However, reported deviations from diffusion control are comparatively rare," and the local-equilibrium diffusion-control model appears adequate for the description of many isothermal growth systems.'2"9 Cahn14 has treated the problem of migration of an interface which is able to reach positional energy minima, and concluded that such an interface, if subjected to a high local ther-modynamic "driving force", may migrate normal to itself without the benefit of ledges. As local equi-

Jan 1, 1968

By John W. Tieman

Research on processes to remove sulfur oxides from flue gas has been in progress for many years. Pioneers in this field were the British who, in the early 1930's, installed a full-scale flue gas scrubbing unit on a 120 MW boiler using alkaline water from a Thames estuary plus chalk. Since that time, various methods have been studied by many investigators. Federal laws covering air pollution started with the 1955 Air Pollution Control Act. With the advent of the Air Quality Act of 1967, and subsequent publishing of criteria and available technology for control of sulfur oxides in January 1969, the clamor for information on commercially available control techniques to remove sulfur from fossil fuels has rapidly increased.

Jan 8, 1972

By C. H. Li, R. J. Stokes, T. L. Johnston

A portion of the Ni3Cr-Ni3Al phase dzagram has been investigated, including the precipitation of 1 (Ni3Al) as well as the existence of ordered Y (Ni matrix), Extensive metallographic studies by electron microscopy have been carried out and X-ray diffraction diagrams have been taken at both elevated and ambient temperatures, No long-range ordering of the phase was found above 893°C (1639°F) in the compositional range investigated. The high rate of formation of the ordered ?1 phase upon quenching has been confirmed, a phenomenon which up to the present Lime has retarded the understanding of this phase diagram, Specimens with controlled amounts of ?1 exhibited up to a six-fold improvement in yield and creep strength compared with single-phase Ni-Cv-A1 alloys. MOST of the important high nickel heat-resistant alloys are related to the nickel-chromium-aluminum system. One of the important functions of the aluminum, often accompanied by titanium, is to produce a precipitate of the very fine ?1 phase (Ni3A1, X) where X may be Ti, Cr, or other elements. A number of investigators1-" have demonstrate the presence of y' in these alloys but most of their materials contained large amounts of other elements resulting in appreciable amounts of con- fusing phases such as carbides. Further clouding of the precise role of y' has been the suspected existence of an ordering reaction in the y matrix itself, ro-3,12-17 It appeared from these investigations that aluminum in Ni-Cr alloys would raise the ordering temperature of the matrix from 540°C at NisCr to 1300°C at Ni,Al. In support of this possibility, the matrix phase in the parallel Ni-Fe-A1 system is ordered to very high temperatures.1 OBJECTIVES OF THIS RESEARCH From this survey of the literature it appeared desirable to conduct an investigation of the simple Ni-Cr-A1 system using the alloys of the highest available purity to avoid the complication of foreign phases and thereby isolate the structures in the Ni-Cr-A1 system. Procedures were developed to study ? - ?o and ? - ?1 equilibria. Preliminary mechanical tests at elevated temperatures were also conducted.

Jan 1, 1962

By F. A. Forward, J. Halpern

A new process for extracting uranium from ores with carbonate solutions is described. Leaching is carried out under oxygen pressure to ensure that all the uranium is converted to the soluble hexavalent state. By this method), alkaline leaching can be used successfully to treat a greater variety of ores, including pitchblende ores, than has been possible in the past. The advantages of carbonate leaching over conventional acid leaching processes are enhanced further by a new method which has been developed for recovering uranium from basic leach solutions. This is achieved by reducing the uranium to the tetravalent state with hydrogen in the presence of a suitable catalyst. A high grade uranium oxide product is precipitated directly from the leach solutions. Vanadium oxide also can be precipitated by this method. The chemistry of the leaching and precipitation reactions are discussed, and laboratory results are presented which illustrate the applicability of the process and describe the variables affecting leaching and precipitation rates, recoveries, and reagent consumption. THE extractive metallurgy of uranium is influenced by a number of special considerations which generally do not arise in connection with the treatment of the more common base metal ores. Perhaps foremost among these is the very low uranium content of most of the ores which are encountered today, usually only a few tenths of one percent. A further difficulty is presented by the fact that the uranium often occurs in such a form that it cannot be concentrated efficiently by gravity or flotation methods. In these and other important respects, there is evident some degree of parallelism between the extractive metallurgy of uranium and that of gold and, as in the latter case, it has generally been found that uranium ores can best be treated directly by selective leaching methods. It is readily evident that this parallel does not extend to the chemical properties of the two metals. Unlike gold, which is easily reduced to metallic form, uranium is highly reactive. It tends to occur as oxides, silicates, or salts. Two ores are of predominant importance as commercial sources of this metal: pitchblende which contains uranium as the oxide, U3O51 and carnotite in which the uranium is present as a complex salt with vanadium, K2O-2UCV3V2O5-3H2O. These ores may vary widely in respect to the nature of their gangue constituents. Some are largely siliceous in composition, while others consist mainly of calcite. Sometimes substantial amounts of pyrite or of organic materials are present and these may lead to specific problems in treating the ore. Further complications may be introduced by the presence of other metal values such as gold, copper, cobalt, or vanadium whose re- covery has to be considered along with that of the uranium, or whose separation from uranium presents particular difficulty. In general, there are two main processes for recovering uranium in common use today.'.2 One of these employs an acid solution such as dilute sulphuric acid to extract the uranium from the ore. A suitable oxidizing agent such as MnO, or NaNO, is sometimes added if the uranium in the ore is in a partially reduced state. The uranium dissolves as a uranyl sulphate salt and can be precipitated subsequently by neutralization or other suitable treatment of the solution. The second process employs an alkaline leaching solution, usually containing sodium carbonate. The uranium, which must be in the hexavalent state, is dissolved as a complex uranyl tricarbonate salt, and then is precipitated either by neutralizing the solution with acid or by adding an excess of sodium hydroxide. The latter method has the advantage of permitting the solutions to be recycled, since the carbonate is not destroyed. This is essential if the process is to be economical, particularly with low grade ores. With each of these processes, there are associated a number of advantages and disadvantages and the choice between using acid or carbonate leaching is generally determined by the nature of the ore to be treated. In the past, more ores appear to have been amenable to acid leaching than to carbonate leaching and the former process correspondingly has found wider application. With most ores, acid leaching has been found to operate fairly efficiently and to yield high recoveries. One of the main disadvantages has been that large amounts of impurities, such as iron and aluminum, sometimes are taken into solution along with the uranium. This may give rise to a high reagent consumption and to difficulties in separating a pure uranium product. Excessive reagent consumption in the acid leach process also may result

Jan 1, 1955

Jan 1, 1920

By David J. Mack

The structures and properties of the copper-aluminum alloys have been the subject of much study since the classic investigation of Carpenter and Edwards1 focused attention on. the engineering utility of these alloys. It was recognized at an early date that the metallographic structures developed in the aluminum bronzes were similar to those developed in steels, both in the annealed and the rapidly cooled state. Most investigators have been concerned with the acicular, martensitic-like structure formed from the 0 solid solution upon rapid quenching; the transformation of the ß under equilibrium cooling to a lamellar eutectoid having been relatively neglected. With the introduction in 1930 by Davenport and Bain2 of the isothermal transformation technique for studying eutectoidal decompositions, a new field was opened. Although an enormous amount of work has since been done on the isothermal transformation of steel, study of structurally analogous systems has been almost totally overlooked. The outstanding exception was the prize-winning paper† of Smith and Lind1ief³ ho investigated the decomposition of the 0 phase in copper-aluminum alloys by isothermal methods. This was followed in 1934 by Wasserman's review' of available information on analogous transformations in eutectoid alloys. Since that time no comprehensive study of isothermally transformed eutectoids analogous to steel has appeared, although many valuable contributions have been made to an understanding of the structures developed in such systems. Important papers have been published by Kurdjumow, Gridnew and co-workers, Obinata,18.'9 Greninger,20.21 and Others. The work to be described in this paper was an outgrowth of preliminary studies on the isothermal transformation of a entectoid aluminum bronze, after it became apparent that the alloy under study was reacting somewhat differently than the similar alloy used by Smith and Lindlief. Preliminary Experiments The material used in this study was a high purity aluminum bronze especially prepared by Ampco Metal, Inc. It analyzed: Copper—88.07 pet, Aluminum—11.89 pct, Iron-—0.02 pet, Manganese—-.OI pct, Others—Balance. Although some disagreement exists on the exact composition of the eutectoid, this alloy was believed to be of essentially eutectoid composition even though some pro-eutectoid* delta particles existed in the microstructure of furnace cooled specimens. Specimens transformed isothermally at temperatures slightly below the eutectoid showed relatively large amounts of pre-eutectoid delta, but as will be shown later, this results

Jan 1, 1949

Alfred Stansfield, Montreal, Canada:—In Professor Howe's paper on the position of Ae3, he shows its industrial importance in determining the temperature to which steel should be heated for " grain refining." Several years ago I carried out a research on the " burning " of steel and found that while hypo-eutectoid steel should be heated to Ae3, hyper-eutectoid steel that has been very much overheated must be reheated to the curve Sa on the carbon-iron diagram, in order to redissolve the pro-eutectoid cementite and thus to obtain recrystallization and grain-refining. This treatment was necessarily only partly successful, and I should like to ask whether the conditions of heat treatment for refining overheated high-carbon steels have been ascertained. Speaking of the &'Persistence of Solidificational Segregation " Professor Howe quotes an experiment made by Mr. Stead in which a bar of 1.2 per cent. carbon steel was immersed in a large mass of molten blast-furnace slag and allowed to cool with it. The steel was heated ; above the solidus (curve An on the carbon-iron diagram), but below the liquidus (curve AB). A drop of eutectic carbon-iron alloy, rich in carbon, had liquated out and hung below the bar. This agrees exactly with my own observations on the burning of steel, but my interpretation differs somewhat from that of Professor Howe. Professor Howe considers that the fusion of a part of the metal (rich in carbon) shows that the solidificational irregularities of composition had persisted through the rolling and heat treatment of the steel, as otherwise no part of the steel would have been sufficiently fusible to melt. It does not appear to me that such an explanation is necessary. A piece of steel represented in temperature and composition by any point within the area ABa will ultimately resolve itself into a solid phase and a liquid phase in equilibrium with each other. It may appear that if the steel were absolutely uniform no fusion could take place, but, the smallest nucleus of high-carbon, fusible alloy would ultimately bring about this separation into liquid and solid phases, by diffusion of the carbon from the solid to the liquid areas. A nucleus sufficient for the purpose might be provided by an area of pro-eutectoid cementite which had not become diffused during the

Jan 1, 1914

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Jan 1, 1938

By G. M. Ritcey

Continuous contacting equipment for solvent extraction can be divided into two major areas, according to whether their mode of operation is stagewise or differential (Figure 1). Mixer settlers and the recent Kenics and Sulzer mixers typify the stagewise contactors. In these counter- current contactors, the aqueous and the organic phase are mixed and then separated in a large settling area before the next stage of mixing. Countercurrent differential contact- ors, such as centrifuges and various types of columns, are more compact in that they require less ground area than mixer settlers. [ ] Contactors, in addition to being either stagewise or differential, can be further subdivided into non-agitated and agitated depending on the method used for mixing the phases and producing the countercurrent flow. The simplest contactors such as spray, packed, or perforated plate columns achieve both the mixing and countercurrent flow by means of the gravity difference between the two phases. In agitated contactors such as the Scheibel, Reciprocating Plate, and Sieve-Plate Pulse, mechanical agitation is introduced but gravity differences still produce countercurrent flow. To conserve plant space, and for large throughput with short contact time, centrifugal contactors are used where possible. The reader can refer to reviews on the subject (1-11).

Jan 1, 1978

By J. A. Knox, R. M. Lasater, J. M. Tinsley

Chemical squeeze treatments have been used to provide temporary relief from certain production problems. The chemical fracture-squeeze technique, combining the effects of a fracturing treatment and a squeeze operation, has been more successful than conventional squeeze operations. Knowledge derived from well stimulation and reservoir engineering research provides a means for predicting the theoretical effective life of such a treatment. Analysis of theoretical equations and concepts developed allows selection of improved treatment techniques based on specific formation conditioins. Theory used in this analysis was developed as an extension of previous electrical model studies made to establish the expected flow and pressure profiles adjacent to a fracture system. The chemical fracture squeeze technique can be utilized in the economic application of corrosion inhibitors, emulsion breakers and paraffin and scale inhibitors. Application of this technique is shown to be effective. The slow return rate of injected chemicals, controlled by the resultant flow profiles and treatment variables, permits extended periods of chemical effectiveness. Results of field treatments are given, showing that the concepts outlined above for chemical fracture-squeeze treatments are valid and that applying this technique can help alleviate many current production problems. INTRODUCTION Much progress has been made in the last 10 to 15 years in developing chemicals for use in stimulating wells, maintaining production and protecting well equipment from damage due to corrosion. Not too many years ago, some wells seemed to dry up or wear out. In many cases the wells were produced as long as possible without any attempt at maintaining productivity. Even with the advent of new and better stimulation techniques, a rapid decline in production was observed. Methods of removing and, in some instances, preventing damage have been developed. Among thosc factors responsible for uneconomical production are scale, paraffin, corrosion, bacteria, water blocks and emulsions. Soluble scale-prevention chemicals have been developed1,2 that can be placed in a formation along with frac- turing sand. As the water produces back across this bed, the solid material dissolves slowly and can provide long-term protection from scale. However, bottom-hole temperature and salinity of produced water vary widely and both these factors influence the rate of solubility. Scale inhibitor composition is also a controlling factor. Some of the solid material may be crushed, increasing the surface area exposed to water and increasing the rate at which it dissolves. Some of the material may never be contacted by water and can be lost. However, this type of treatment has been very successful in many instances and has helped maintain economical production for extended periods of time. Liquid scale inhibitors, which are more widely applicable and more stable, have been developed in recent years; however, because they are liquids, their use has been restricted to treatment down the annulus, using metering pumps to provide proper concentrations in the produced fluid. This has prevented use in wells containing packers, in dually completed wells and in gas-lift and flowing wells. Wells that operate with an open annulus may also experience severe corrosion problems due to introduction of oxygen. Paraffin inhibitors3 have been developed that can be fractured into a well as particulate solids to be slowly dissolved in the produced fluid. These materials are not usually effective in wells with a bottom-hole temperature in excess of 120F since solubility rate may be too fast if that temperature is exceeded or if aromatic content of the oils is unusually high. Corrosion inhibitors have been developed that can be fractured' into a well for long-term feedback, but development of a material with proper solubility or feed rate has been difficult. Corrosion inhibitors are available in many different forms. Liquids have been lubricated down the annulus or sticks or pellets dropped down tubing. Inhibitor squeeze treatments5 devcloped a few years ago led to development of inhibitors with particularly strong film-forming properties.6,7 This technique basically involves displacing a highly concentrated solution of the inhibitor into the formation through the tubing. Kerver and Hanson8 studied the adsorption properties of inhibitors on various types of formations. They showed that, even though the inhibitor was displaced radially into the true permeability, it could be produced back for a long period of time because of slow desorption from the rock. Methods developed for monitoring the return of these inhibitors generally have established 1 to 6 months as the effective limit before retreatment is necessary.9 Inhibitors displaced into the interstices of the formation sometimes cause emulsions that either hamper production or cause treating problems on the surface.

By Eugene S. Perry

The oil and gas industries in Montana continued through the year of 1937 with but little change. No new fields were discovered, and production of old fields did not vary greatly. No outstanding wildcat wells were drilled. Perhaps most notable were extensions in the western part of the Kevin-Sunburst field. Acid treatment of wells in the Kevin and Pondera fields continued with gratifying results.

Jan 1, 1938

By J. W. Rutter, K. T. Aust

In previous studies of grain boundary migration in zone-refined lead, the authors used bicrystal specimens consisting of a striated crystal which was grown from the melt, and an adjacent striation-free crystal, introduced by artificial nucleation and growth.1 While this method permits the study of the motion of individual grain boundaries, it does not provide control of the relative orientations of the grains. The present note will describe a technique for controlling the orientations of the two crystals in this type of specimen. The technique consists essentially of placing a striated crystal and a striation-free crystal of controlled orientations end-to-end in a graphite trough, then melting a short zone at the junction of the two crystals and allowing it to freeze to form the desired grain boundary. The apparatus used to carry out this process is illustrated in Fig. 1. It consists of a trough milled from high-purity graphite,with grooves in the underside for the placement of thermocouples. The graphite piece fans out on one end at the level of the bottom of the trough; the sides of the trough are completed in this region by the attachment of a mating plate with a slot cut at any desired angle to permit reorientation of the crystal placed at this end of the assembly. The joint between the crystals is made at or near the point where the slotted plate joins the rest of the trough. The thermocouple slots are deepened in this region so that the thermocouples are separated from the melt by only 1/32 in. of graphite. An induction heater, with suitable temperature control, is used to obtain the molten zone. The two single crystals used are first chemically polished in a solution consisting of eight parts glacial acetic acid and two parts 30 pct hydrogen peroxide. They are then placed in the trough with the ends to be joined at the position of the thermocouples. Next, cooling is applied to the two crystals by means of air

Jan 1, 1962

Jan 1, 1918

By Gerhard Derge

METALLURGISTS have used borax as a fluxing agent traditionally, but until recently elemental boron has played an insignificant role as an alloying element. Neither the metal nor its compounds have been regarded as important metallurgical materials and there is a surprising lack of knowledge concerning their metallurgical behavior. The new applications to steelmaking of both boron and borates, which arose in part from wartime incentives and restrictions, have been seriously handicapped by this lack of data. For example, rasorite, a naturally occurring sodium borate, has been shown to be an effective substitute for aluminum as a ladle deoxidizer in rimming steels.1 Likewise, the effectiveness of boron as an alloying agent has been demonstrated, 2,3 giving deep hardening when used in restricted amounts. The exploitation of both of these uses has been retarded by the difficulty of attaining suitable metallurgical control. Recognizing that the most important information required was a knowledge of the equilibrium between boron and oxygen dissolved in liquid iron, Gurry4 calculated this relation from the best thermal data available. However, estimates of the entropy of melting of boron, the activity coefficient of boron in liquid iron and the activity coefficient of B203 in slag were involved, and experimental work on this problem was obviously desirable. The experiments to be described were planned to establish the boron-oxygen relations in liquid iron and to demonstrate at the same time the ferroborate slag compositions in equilibrium with various amounts of oxygen in liquid iron. Accordingly, slags containing varying proportions of iron and boron oxides were held in contact with molten iron, and samples of both slag and metal were analyzed. The limitations upon the accuracy of the data will be considered, but in a practical sense the oxygen levels that can be attained in iron by iron borate slags, and the amounts of boron in iron at these oxygen levels were established. EXPERIMENTAL PROCEDURE No entirely suitable refractory was found for the mixtures of iron oxide and boron oxide used as slags. Crucibles of silica, magnesia, Ramix, beryllia, and zirconia were all tried unsuccessfully. The most satisfactory method discovered for handling them was the rotating-crucible technique, which creates a parabolic crucible of liquid iron 5,6 Even this was not entirely successful, for at steelmaking temperatures (1600°C.) the slags had such a low surface tension that they crept up to the refractory and slowly dissolved it. These difficulties made it impossible to maintain a constant slag composition for an unlimited period of time. However, by using the rotating

Jan 1, 1946