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By M. I. Sherman, J. D. H. Strickland

USE of a hydrometallurgical approach to the oxidation of sulfide ores and extraction of metals therefrom may have advantages over the more common smelting techniques when a low grade deposit is difficult to concentrate or the subsequent separation of metals, coexisting in the ore, is laborious by any known smelting operation. For economic reasons, the most promising oxidants are either atmospheric oxygen or electric power. The use of oxygen, or air under pressure, has recently been revised. Pyrrhotite has been converted to iron oxide and elementary sulfur' and a variety of sulfides have been treated by Forward and co-workers.2-4 Generally sulfate is the end form of the sulfur but with galena in an acid medium, elementary sulfur can be formed." For economic reasons chlorine and ferric iron salts are about the only possible alternatives to the atmosphere as oxidizing agents for base metal sulfides. If aqueous solutions of chlorine or ferric iron are employed, the reduction products can be oxidized electrolytically in situ and used again, thus acting as catalysts for electric power as oxidant. The use of ferric salts for this purpose is established hydrometallurgical practicea but, although chlorine gas has been employed in the dry state at an elevated temperature, its use in aqueous solution at or near room temperature has not found favor. The reaction of chlorine water with the soluble sulfide ion has been studied by several workers,7-9 and both sulfate and elemental sulfur are found as end products, the latter being favored by the presence of a low concentration of oxidant relative to that of sulfide in solutions of about pH 9 to 10. Of direct bearing on the work in hand are an early American patent" and a recent Austrian patent." The former advocates stirring powdered ore with an aqueous solution of ferric chloride chlorine oxides and chlorine. In the latter it is claimed that both metal and sulfur can be obtained by electrolysis, in a diaphragm cell, of a metal ore slurry in brine. Details in these patents are scant and no data or explanation is given for the mechanism of the reaction which, in the Austrian work, is attributed to the (unlikely) action of nascent chlorine at the anode surface. No mention is made of possible differences in behaviour between various ores. Apparatus A complication encountered when working with chlorine water is that a serious loss of chlorine occurs by gas partitioning unless an enclosed system is used and any air space in the apparatus is kept very small and constant. Arrangements were made, therefore, to take out samples for analysis without letting air into the system to replace the liquid removed. For convenience in studying a heterogeneous reaction the apparatus was so designed that a reproducible controlled stirring rate could be maintained and the ratio of surface area of ore to volume of solution was approximately constant throughout any experiment. The apparatus used is shown in Fig. 1. The ground ore was placed in the horizontal cylindrical vessel, A, of about 1 liter capacity, heated by a constant temperature circulating bath pumping water through the concentric jacket, B. By adding chro-mate to this water, an ultraviolet radiation filter effectively surrounded the reaction vessel, greatly reducing any possible photochemical decomposition of chlorine solutions. Stirring was effected by glass paddles, C, attached by an axle to a magnet which was rotated by another powerful Alnico magnet, D, outside the glass end, this magnet being itself rotated by an electric motor electronically controlled to constant speed. Speed could be varied from about 150 to 900 rpm and was measured and held to within 1 pct of a given value. The end of the reaction vessel remote from the stirring magnet was closed by another one-ended glass cylinder, E, connected by thin polyethylene bellows, F, clamped by screw clamps and watertight rubber gaskets to the main vessel. Through E, a glass electrode and calomel electrode projected into the solution and a hypodermic syringe pierced a small bung and allowed acid or alkaline to be added to maintain a constant pH. By pushing the fully extended bellows until the two cylinders touched, from 50 to 100 ml of solution could be forced out through a sintered disk into the three-way tap system, G, either to waste (for flushing purposes) or up into a 10 ml burette where the solution could subsequently be measured out for analysis. The ore samples were introduced at H, the tube being stoppered by a thermometer of —1 to +52ºC range, graduated to 0.1°C intervals. To prevent ore from being ground in the end bearings of the stirrer these bearings were pro-

Jan 1, 1958

By J. L. Gillson

Historically, rock deposits and sand deposits of titanium minerals came into production about the same time, although there may be some argument as to what is meant by production. Beach deposits of heavy minerals in India (Figs. 1-4) and Brazil (Figs. 5) were worked for monazite about the turn of century, but as there was then no market for titanium minerals, these were thrown away. The rock rutile deposits at Roseland, Va., Fig. 6, were worked to supply rutile for titanium chemicals and for coloring ceramics long before there was a titanium pigment business. The pigment industry started about the middle twenties, both in Europe and the U. S., and almost simultaneously the rock deposits at Ponte Vedra Beach near Jacksonville, Fla., were worked for titanium content. Since those days, production from both types of deposits has continued to grow at a rapid rate; many deposits of both types have been found, and reserves have grown to very large figures. In total tonnage of reserves, there is no doubt that the rock deposits are far ahead of the sand deposits; nevertheless there is a very large tonnage of commercial sands available. It is the quality of titanium mineral in the sand and the relatively lower costs of operating sand deposits that have kept them abreast, at least in annual tonnage produced, with the rock deposits. The principal titanium mineral used is ilmenite, but as soon as that mineral began to be sought as a titanium ore, it was obvious that there are ilmenites and ilmenites. Textbook ilmenite should have the composition FeOTiO2 and should analyze 52.6 pct TiO2 and 36.8 pct iron as Fe. The Indian ilmenite, for almost a generation the standard ore for manufacturing pigment in the U. S., was found to analyze about 60 pct TiO, and only 24 pct. Fe, and most of the iron is in the ferric condition. The whole process of pigment manufacture in the U. S. was built up on the use of a raw material of that grade, and the American chemical engineers who operate the pigment plants shuddered at the thought of using a rock ilmenite with 45 pct or so of TiO, and nearly 40 pct Fe. Intensive search was made around the world to find other deposits of rich black sand, like the Indian beaches, but although a few were found, there was some objectionable feature about each. A deposit in Senegal, south of Dakar (Fig. 7), was worked for a while, but an organic coating on the grains made attack by acid difficult. Modern practice would have included a scrubbing operation, in a caustic soda bath, to eliminate the organic coating. Brazilian deposits were numerous, but individually small, and shipping from them difficult. Deposits on the east coast of Ceylon had many attractive features, but the ilmenite analyzed only 54 pct TiO2 and could have been used only with a penalty. Sand deposits with 2 pct ilmenite, like those now worked in Florida, would not have been considered commercial ore, even if they had been known at that time. Most rock ilmenites are associated or mixed with hematite or magnetite, which accounts for the lower titanium and higher iron values than in the sand ilmenites. The Norwegians, English, and Germans, with cheap Norwegian rock ore at hand, learned to install in their pigment plants adequate capacity on the black side, as it is calltd, and counterbalanced the extra cost of plant, and larger amount of acid used, by the lower cost of ore. When World War II arrived, two of the largest pigment manufacturers in the U. S. had to learn how to use the Adirondack ilmenite, but one of them very gladly went back to sand ores when the Florida deposits came into large-scale production after the war. The other continues to use Adirondack ilmenite and finds it commercially attractive to do so. Rutile is not a raw material for titanium pigment manufacture by the sulfate process, since it is insoluble in sulfuric acid. In addition to its small consumption in chemicals and ceramics it began to be used in quantity in welding rod coatings. With the outbreak of World War 11, and the tremendous need for welding rods in shipbuilding and other structural steel construction, rutile suddenly became in heavy demand. The sand deposits on the eastern shore of Australia (Fig. 8A) which had been worked in a small way since 1934 were brought into production, and some stream placers in Brazil were worked and rutile concentrates shipped to American

Jan 1, 1960

By H. Y. Jennings

An extensive field and laboratory experimental program was carried out to compare the waterflood behavior of carefully preserved soft and unconsolidated cores with measurements on the same cores after extraction. Results obtained from using idealized consolidated and unconsolidated porous media in which wettability could be carefully controlled were contrasted with the preserved core data. The controlled tests on idealized porous media investigated the effect of wettability, flood rate, core length, core permeability and consolidation on the displacement of high viscosity oils. It was concluded from these studies that waterfloods are more favorable when carried out with crude oil in preserved soft and unconsolidated cores than with the same cores after they have been extracted and re-saturated. Waterfloods are usually more favorable when carried out with crude oil in extracted .soft and unconsolidated cores than with refined oil of the .same viscosity in the same cores. The less favorable behavior of extracted soft and unconsolidated cores compared to preserved cores is due to alteration of the core by extraction. Preserved cores saturated with native water and oil should be used for laboratory displacement experiments because they more accurately reflect true reservoir behavior INTRODUCTION The demand for low gravity crude oil created by refinery modernization has focused attention on increasing the production of this viscous crude oil. Billions of barrels are in place in fields that are depleted, or nearly depleted, by primary production mechanisms. Since low gravity reservoirs are relatively recent, geologically, the solid matrix material is usually soft and unconsolidated sand. Such formations are also characterized by a high clay content. Evaluation of sophisticated oil recovery processes with the associated high capital investments has increased the demand for special core analysis tests on material from these soft and unconsolidated sand reservoirs. Data in this paper have resulted from an extensive field and laboratory experimental program. The initial objective vras to provide soft and unconsolidated sand cores for laboratory measurements with as little alteration as possible from their reservoir condition. A secondary objective was to compare the waterflood behavior of these carefully preserved cores with measurements on the same cores after they had been extracted and resaturated. When the comparison showed markedly different behavior the final objective was to attempt to explain the difference by making measurements on idealized porous media free of clay in which initial wettability could be carefully controlled. EXPERIMENTS MATERIALS Core Material The preserved cores used in this study were obtained with as little alteration as possible from their reservoir conditions. Special techniques were developed to satisfy this objective. The cores were cut with native crude whenever the crude had the necessary properties to satisfy the minimum drilling fluid requirements. A pure hydrocarbon chromatographic tracer was added to the crude to provide a simple, safe and inexpensive method to distinguish between oil filtrate and formation oil. Details of the tracer technique used in this study and the procedures used to handle and process the soft, unconsolidated cores have been published.' The core samples were then preserved and packaged at the well site with a dip-applied strippable plastic, or by using a rubber sleeve from a rubber-sleeve core barrel. The final step was to insure that the carefully taken and preserved samples were not altered by processing in the laboratory. Some soft and poorly consolidated sands were carefully shaped in the lab and encased in a protective mounting without disturbing their three-dimensional integrity. Many samples were so poorly consolidated that they literally flowed from the package when the seal was broken. A technique was developed to obtain cylindrical plugs from these samples by using liquid nitrogen as the drilling fluid in a conventional core-drill, drill-press assembly. The idealized porous media consisted of sintered rods of Alundum RA 139, outcrop sandstone identified as Al-hambra sandstone and packs of No. 130 Nevada sand. This sand is 95 per cent 140-200 mesh. (Physical properties of these porous media with those representative of preserved cores are in Table 1.) The natural cores and most of the idealized porous media were 1 1/2-in. in diameter and 3-in. long. The samples used to study the effect of core length were 1 1/2-in. in diameter and 12-in. long. Liquids Water and oil produced from the formations being studied were protected from the atmosphere and collected in carefully cleaned glass or plastic-lined containers. The production was free of chemical additives such as emulsion breakers and corrosion inhibitors. The crude oil was

Jan 1, 1967

By W. E. Bonini, E. A. Hickok

IN the course of an investigation directed toward expanding ground-water facilities in Essex and Morris counties, New Jersey, the Board of Water Commissioners of the city of East Orange authorized a seismic-refraction survey' for the purpose of de-lineating bedrock topography below unconsolidated overburden. Results of the survey were highly satisfactory and led to the preparation of a comparatively detailed bedrock contour map. Knowledge of the bedrock depth and configuration was an important aid in selection of sites for test drilling. The portion of the East Orange Water Reserve under consideration is in the flood plain of the Pas-saic River about 10 miles west of Newark, N. J. The flood plain is about 175 ft above mean sea level and is bordered by low hills rising to elevations of approximately 250 ft. The bedrock underlying the Water Reserve consists of sandstone and shale of the Triassic Brunswick formation and is covered everywhere by deposits of unconsolidated glacial outwash sand and gravel, lacustrine clay, and recent river silt as much as 150 ft thick. Yield of wells in the sandstone and shale averages 100 to 200 gpm. Since production wells constructed in the sand and gravel aquifer in the buried river valley shown on the contour map (Fig. 1) yield 300 to 1400 gpm, it was proposed to locate additional production wells in this buried valley, where the yields per well would be maximum. In 1939 and 1946 the East Orange Water Dept. had electrical-resistivity surveys made to determine depths to bedrock. From the resistivity data the exploration company prepared a bedrock contour map. A well field expansion program begun in 1955 utilized this information to locate sites for test wells along a predicted northward extension of the buried valley in which existing production wells are located. After several test wells (wells 201-205) had been drilled, it became apparent that the resistivity information was unreliable." For example, test well 201 recorded bedrock at a depth of 72 ft, whereas the resistivity depth determination was 130 ft. As a consequence, the test drilling program was temporarily suspended and a seismic survey was under- taken to determine the topography and extent of the buried valley known from well records to underlie the existing well field. In the first phase of this study, several seismic shot point locations were placed at sites where well logs had been obtained previously. This procedure is necessary in a new area to determine whether the seismic method is applicable and what degree of accuracy is to be expected. At the East Orange Water Reserve, depths obtained from the shot points near test wells 202, 203, and 204 were within 8 to 11 pct of the depths logged (Table I). With this assurance that accurate results could be obtained, additional seismic spreads were located on the Water Reserve. Using a portable refraction seismograph, in the fall of 1955 a crew of four men shot a total of 29 reversed seismic spreads in a period equivalent to six field days. Charges as heavy as 3 1b of 40 pct dynamite were necessary at a few places to overcome ground vibrations caused by traffic on nearby highways. At most other sites, a 1-1b charge was sufficient. Travel-time plots were made for all spreads, and depths and true velocities were calculated according to formulas for multiple sloping layers by Ewing, Woollard, and Vine.' The plot of spread 7 (Fig. 2) is typical of the short spreads in which bedrock was shallow—about 50 ft in this case. Where there were not enough arrivals through the bedrock to define the high velocity bedrock line, the spreads were lengthened. This was done by placing shots on line several hundred feet away from each end of the line of geophones. It was then possible to construct complete reverse plots for both short and extended shot points (see spread 27, Fig. 3). Four individual depths were calculated from each extended spread. Three and in some cases four seismic layers were observed. The surficial layer had a velocity range of 900 to 1200 fps, the lowest velocity recorded. This seismic layer is above the water table and is interpreted as recent river silt. The bedrock had the highest velocities, which ranged from 10,600 to 16,400 fps. Intermediate velocities ranged from 4500 to 6800 fps. In every case the intermediate layer was within

Jan 1, 1959

By V. B. Kurfman

The temperature, strain rate, and orientation deDendence of defbrnzation of single-crystal MgAg has been examined. The crystals exhibit a tendency to single glide and little or no hardening at 25°C for many orientations. A much higher hardening rate is observed when multiple glide occurs, such as can be initiated by surface defects. The tendency for easy glide becomes less dependent on surface preparation and orientation as T — 100°C and bars so tested often fail after one-dimensional necking-. At T > 200°C (transition temperature for single-crystal notch sensitivity and poly crystalline ductility) single glide diminishes and two-dirnensionul necking begins. The crystals do not strictly obey a critical resolved shear stress law, but show the influence of {loo) cracks in determining the slip mode. The results are correlated with the difficulty of sciperdzslocation intersection and semibrittle behavior of this compound in single-crystal and poly crystalline form. Comparisons are made with the slip selection mode observed in tungsten, with the reported observations of easy glide in bee metals. and with the mechanical behavior of poly crystalline MgAg. PREVIOUS work on tensile deformation of polycrys-talline MgAgl and bending deformation of single-crystal MgAg2 has shown that the compound is semi-brittle (i.e., notch and grain boundary brittle). If this semibrittleness is supposed to result from the difficulty of multiple glide (associated with the problems of superdislocation intersection) one might expect single crystals deformed in tension to show pronounced single glide and strong orientation dependence of hardening rate. These experiments were done to examine this supposition and to study the tensile deformation of a highly ordered system which may be considered bcc if the difference between the two kinds of atoms is ignored (actual structure: CsC1). EXPERIMENTAL Single-crystal ingots were grown by directional freezing as previously described.' These ingots were sliced into a by a by 2 in, rectangular bars by electric discharge machining, then round tensile bars were conventionally machined to 1/8-in.-diam by 1-in.-long reduced section. The bars were typically tested without an anneal because of the problem of magnesium vapor loss and they were typically tested as mechanically polished. The analyses are within the same limits as those reported earlier; i.e., the average composition for each specimen is within 0.5 at. pct of stoichiometry, while the total range from end to end in a given specimen varies from 0.7 to 1.4 at, pct. There has been no indication in the results of any variation in slip or fracture mode attributable to the composition fluctuations. The slip systems were determined by two-surface analysis of the bars after testing to failure at room temperature. Single glide was so dominant that there was little difficulty in identification of the dominant slip system even though the tensile elongation to failure often approached 7 to 8 pct in room-tempera- ture tests. Elevated-temperature testing was done in a silicone oil bath and low-temperature testing was done in liquid Np or a dry-ice bath. All stress measurements are reported as engineering stress unless otherwise specified, and crosshead travel is used as the strain measurement. RESULTS The tendency toward single glide is best seen in the pictures, Figs. 1, 2, and 3, which depict deformation at fracture as a function of test temperature. While it is possible to find regions of secondary slip by careful microscopy, such regions are very small. The development of a ribbon-shaped configuration from an initially round section bar pulled at 100°C is typical, occurred by single glide, and illustrates the degree to which such glide continues. At temperatures =100°C the bars typically show elongation of 20 to 50 pct by predominently single glide. Despite the large elongation, fracture even at 150°C occurs in a brittle mode, Fig. 2, in the sense that it is an abrupt failure which shows no discernible necking in the second dimension of the bar's cross section (i.e., there is no appreciable action of any slip modes which would decrease the broad dimension of the cross section). Near 200°C the fracture mode changes slightly. Although most of the sample extension is by single glide, after the bar develops the characteristic ribbon shape it begins to neck in the second (i.e., broad) cross-sectional dimension. The bar becomes very thin in the "necked down" region, Fig. 3, and the reduction in area approaches 100 pct. Often there oc-

Jan 1, 1967

By J. Philibert, A. G. Guy

Diffusion in the presence of deformation was studied by the method of vacuum dezincification of copper-rich and silver-rich solid solutions containing 7 to 30 pct Zn. The specimens were designed to permit the study of diffusion in separate portions of a given specimen characterized by strain rates ranging from essentially zero to approximately 10 sec-. No effect of deformation on diffusion was observed. BEGINNING with the work of Buffington and Cohen: interest in the question of the effect of stress or strain on diffusion has largely been concentrated on the enhancement of diffusion in specimens subjected to Continuous plastic deformation. The present research is a contribution to this limited area. However, as a preliminary to focusing attention on this special topic, it will be desirable to make a broad survey of the larger question, especially since there has been considerable foreign work in areas outside those of current interest in the United States. Since most of the topics referred to in the following section are both complex and imperfectly understood at present, it has been expedient in most instances to offer only a guide to the general nature of the work rather than a critical evaluation. PREVIOUS WORK The effect of elastic stress on diffusion has received considerable attention, especially with regard to the thermodynamic driving force for diffusion. The thermodynamic treatments have been based on the work of Gibb, Voigt, Planck, and Leontovich.' Konobeevskii and Selisski6 made a first attempt at treating the problem in 1933, and Gorskii7 a few years later gave a solution applicable to single crystals as well as to polycrystalline specimens. In 1943 Konobeevski8 published treatments that have been the basis of much Russian work up to the present. For example, Aleksandrov and Lyubov used his work in explaining the velocity of lateral growth of pearlite. Early work in the United States was that of Mooradian and Norton, which showed that lattice distortion tends to be relieved before it can significantly affect the diffusion process. Druyvesteyn and Berghoutl1 observed a slight effect of elastic strain on self-diffusion in copper, while de Kazinczy12 found that both elastic and plastic deformation increased the rate of diffusion of hydrogen in steel. On the other hand, Grimes58 observed no effect of either elastic or plastic straining on the diffusion of hydrogen in nickel. High-frequency alternating stresses have been reported by various investigator s13-l5 to increase the rate of diffusion. A special form of elastic stressing is the imposition of hydrostatic pressure, a condition that is amenable to Conventional thermodvnamic analysis. Most of the experimental results in this area are consistent in showing a slight decrease in diffusion rates at high pressures.16-l8 Although Geguzinl reported a pronounced effect of relatively small pressures, Barnes and Mazey20 failed to Corroborate this finding, while Guy and Spinelli21 advanced an explanation of the phenomenon observed by Geguzin. It has been recognized that the thermodynamic treatment of diffusion phenomena in an arbitrarily stressed body is complicated by the fact that the desired state of quasi-equilibrium of the shear stresses cannot be maintained during a general diffusion process. However, attempts have been made by Meix-ner22-24 and Fasto to treat certain restricted cases, such as relaxation. FastovZ7 has also incorporated the general stress tensor into the thermodynamics of irreversible processes. The lattice strain that accompanies the formation of a solid solution has been the subject of much study,28-s0 and indirectly it has entered into many recent theories of diffusion. However, some Russian investigators31'32 have taken other views of this matter and have predicted large effects on diffusion rates because of concentration stresses.o In completing this brief resume of previous work involving elastic strains and before proceeding to a consideration of the effect of continuous plastic deformation, it should be pointed out that deformation of various additional types may also influence diffusion. The effect of cold-working on subsequent diffusion has been studied directly by AndreevaS and by Schumann and Erdmann-Jesnitzer, while indirect evidence has been obtained by Miller and Guarnieri and by Vitman.38 Thermal stresses may also influence diffusion, contributions to this subject having been made by Fastovs7 and by Aleksandrov and Lyubv. The work of Johnson and Martin,o Dienes and Damask,3Band DamaskS considered the question of radiation-enhanced diffusion. In considering previous work on the subject of plastic deformation and diffusion, attention will be directed to those studies concerned primarily with diffusion rather than with its relation to Creep, e.g., the work of Dorn, or to the acceleration of diffusion -controlled reactions. Observations of the effect of

Jan 1, 1962

By W. M. Wojcik, R. F. Kowal

Oxygen and sulfur distributions in commercial, 5-ton ingots of killed, medium carbon steel are described. Oxygen distribution is found to vary with deoxidation practice. Irregular distribution of oxygen within ingots makes necessary special precautions in sampling of rolled products for analysis of oxygen. Oxygen distribution is discussed in terms of recently published solidification concepts which had been successfully applied to simpler cases of segregation. These concepts have been found inadequate to explain observed oxygen distributions. Convective movements of the liquid metal, as determined by tracer elements, are shown to be capable of accounting for the observed distributions of oxygen. IN an effort to explore the origin of surface and subsurface imperfections in pierced steel products, a study of oxygen and sulfur segregation was made on ingots cast in open-top and hot-top molds. The results of our previous investigations1"3 have indicated the importance of the location and amount of oxide inclusions in an ingot. Inclusions close to the surface of the ingot have been found to contribute greatly to the formation of imperfections in the surface of finished products. This study of the effects of deoxidation and casting practice on segregation and the resulting oxygen distribution in ingots was initiated to determine the parameters controlling the location of inclusions in an ingot. Segregation of solute elements during solidification of low-melting binary alloys has been studied in the past.1, 5 Formation and growth of inclusions in iron melts have been studied under specific conditions."- In spite of these and other recent studies,10-12 segregation during solidification of commercial, killed steel ingots is not well understood. Consideration of solidification rates, of segregation during solidification of the chill, dendritic, and central zones, and of material balances for the segregated elements has indicated that a simplified theoretical solidification model is not adequate. However, the observed high oxygen contents in localized volumes of the dendritic zone can be rationalized if additional effects of convection currents in the ingots, precipitation, and rapid growth of new phases are considered. EXPERIMENTAL PROCEDURE Steelmaking and Processing. A group of nine killed. medium carbon steel heats having compositions listed in Table I have been studied. The deoxidation and mold practices used were varied to give a wide range of steel oxygen contents. The amounts of aluminum added to the ladle and the ingot casting practices (hot top and open top) were the main variables. The steel was made by a duplex practice in 160-ton tilting basic open-hearth furnaces. All nine heats were top-cast into 24 by 24 in. big end down, fluted molds, to a height between 60 and 76 in., using both open tops and exothermic hot tops. The deoxidation practice and the tapping and teeming details for each heat and ingot studied are given in Tables II and III, respectively. Hot-top practice is indicated by the letter H following the heat designation. Furnace and ladle temperatures were measured by standard disposable-tip, Pt/10 pet PtRh thermocouples. Teeming-stream temperatures were obtained as described by Samways et al.,13 by immersing a Pt/10 pet PtRh thermocouple, covered by a silica sheath, into the teeming stream under the nozzle. The output of this thermocouple was recorded with Leeds & Northrup Speedomax potentiometer. Calibration of the latter thermocouples was based on the freezing point of a pure iron/oxygen alloy (2795°F). The accumulated errors of measurements were within ±10°F. The thermocouple measurements were supplemented in this investigation by continuous recording of a ratioing, two-color pyrometer (Shawmeter), protected from smoke by a blast of clean air within the sighting tube, and calibrated to read with better than ±10°F accuracy. Following teeming of three heats, P, R, and T, tracer elements were added to the steel in the molds to obtain a record of the progress of solidification. As soon as the teeming stream was shut off, a 0.010-in.-thick steel can containing a mixture of crushed standard ferro-titanium and ferro-vanadium (0.05 pet of each alloy element) was plunged into the middle of the steel pool to a depth of 6 in. In about 30 sec no indication of the can or its contents remained. The surface of the open-top ingots solidified in 20 to 30 sec. A study of liquid metal movement and the precipitation of oxides was facilitated materially by use of the tracer technique as titanium has a low distribution coefficient between solid and liquid steel while vanadium has a high distribution coefficient.

Jan 1, 1965

By V. B. Kurfman

Grain refinement of Mg-Al melts by carbonaceous additions has been attributed to nucleation by aluminum carbide. The effects of process and alloy variables are interpreted and predicted in terms of the dispersion and chemistry of this phase. The grain coarsening action of Be, Zr, Ti, R.E., chlorination, temperature extremes, and prolonged holding times is described. Measures necessary to insure an adequate dispersion of the catalyst are discussed. CARBON inoculation treatments have become fairly well known and used for grain refinement of magnesium alloys containing Al. Although there is general agreement that a nucleation process occurs, the process is not understood and the inoculants are used in a rather empirical fashion. The treatment is applied to the class of alloys containing 3 to 10 pct Al, i.e., AZ31A to AM100A. Typical methods involve melting, alloying, and adjusting the temperature to 1400° to 1450°F. Then 0.01 to 0.5 pct C as CaC2, C6C16, or lampblack is added by any convenient means, and the melt poured within 10 to 30 min. Investigators generally have been impressed by an assumed similarity of this refinement process to superheat grain refinement, which depends on heating approximately the same alloys to a temperature in the range of 1550" to 1650°F, then pouring promptly after the melt is cooled to the pouring temperature. Various predictions have been made that carbon refinement would replace superheating in commercial practice due to reduced process costs, but this replacement has not fully taken place because of production difficulties and conflicting observations. Davis, Eastwood, and DeHaven1 agree with Nelson2 and wood3 in suggesting that an excess of inoculant may be harmful. Wood however says that overtreat-ment is not a problem in production use of hexa-chlorobenzene inoculation, and Hultgren and Mitchell4 claim no evidence of harm from excess additions. Various grain coarsening reactions are known to occur, including the possibility of overtreatment mentioned above. Trace amounts of Be,2 Zr, and Ti may prevent refinement by either a carbon treatment or a superheat. Occasionally treatment with cl25 may cause coarsening, although the Battelle refinement process' uses a CC14-C12 blend. Grain coarsening also tends to occur on holding at temperatures below 1350°to 1400°F, especially after a superheat treatment, and for this reason Nelson2 stresses the desirability of a refinement method useful at lower temperatures for open pot melting practice. Since a carbon treatment can be made to work at temperatures below 1400°F, it seems desirable to investigate the mechanism of the refinement and the mechanisms of the coarsening reactions in order to establish control conditions for use in commercial production. The identity of the nucleating phase must first be established and then the factors affecting its chemistry and physical dispersion must be determined. THE IDENTITY OF THE NUCLEATING PHASE Davis, Eastwood, and DeHaven suggested that the nucleating phase in this system is Al4c3,1 but Mahoney, Tarr, and LeGrand8 disagree, largely because they found no evidence of the compound in alloys after carbon treatment and because there is no indication that aluminum carbide should be unstable over the temperature range used in the superheat treatment. This latter objection is based on the assumption that both the carbon treatment and the superheat treatment introduce the same nuclei. Electron diffraction studies have been made to identify the nucleating phase. Samples of grain refined A292 have been selectively etched SO that clean surfaces are obtained and so that secondary phases are in relief. Electron diffraction patterns from these surfaces have established that the carbon treatment of A292 introduces into the metal a large number of small, plate-like particles with a structure very similar to Al4C3. In most cases, the plate-like nature of the particles prevented positive identification but in the cases where the identification could be made the particles proved to be AIN A14C3. However, enough variation in lattice constants was observed so that all compositions from pure A14C3 to the 50:50 solid solution A1N.Al4C3 were probably present.14 In A14C3 and especially AlN.Al4C3 the A1 atoms occur in layers within which they have the same hexagonal symmetry and spacing as the Mg atoms in a single basal plane of a magnesium crystal. The solid solution spacing lies between the 3.16 of AIN and the 3.3? for Al4C3, in satisfactory agree-

Jan 1, 1962

By Ted H. Eyde

Both private industry and the Interior Department have become alarmed about the enormous amount of Federal land that has been withdrawn from appropriation either under the Mineral Leasing Laws or the Mining Law of 1872. According to a recent article by Gary Benethum and L. Courtland Lee, governmental actions have withdrawn nearly 400 million acres from the operation of the Mining Law of 1872 and over 500 million acres from the Leasing Laws. An addition al 100 million acres for the Mining Law of 1872 and 70 million acres for the Leasing Laws are either encumbered or being managed in such a way as to constitute a defacto withdrawal from mineral development. This means simply that mineral exploration end development under the Mining Law of 1872 is either prevented or discouraged in an area the size of the states of California, Arizona, Washington, Oregon, Nevada, Utah, Idaho, and one half of Colorado combined. Under the Mineral Leasing Laws, exploration and development is either prevented or discouraged in an area equal in size to all the states east the Mississippi River, except Maine.

Jan 1, 1976

1.Assessment of methane content in coal. Given a naturally low methane content in 11 Coal Seam and the fact that the areas of the 11 Seam adjacent to the tunnelway were degassing for a very, very long time due to previous development and mining, it is conservatively estimated that the remaining in -situ methane is less than 0.5m3/tonne. 2. Continuous miner cutting rate based on the past practice. The best loading rate recorded at the past operations of Smoky River Coal was 45 seconds for a 8 tonnes shuttle car. Using these records, the maximum peak loading rate potential at the face is calculated at 0.178 tonnes per one second or 10.67 tonnes per one minute. 3. Methane release at the face. ?The actual face methane liberation, conservatively assumed at 40% of the total in situ content: 0.20 m3/tonne ?The peak cutting rate: 0.178 t/sec ?The maximum (peak) face methane release: 0.20*0.178 = 0.036 m3/sec

May 1, 2003

By E. S. Peters, M. J. van Rensburg, M. Le Roux, Q. P. Campbell

"The demand for energy has continued to rise worldwide in line with population growth. The majority of South Africa’s electricity is supplied by coal-fired power stations. The amount of fine coal (-2 mm) generated at coal processing plants has increased, due mainly to mechanized mining methods. Fine coal retains more water, which lowers its heating value.Drying the coal is costly and it is difficult to achieve the required moisture content. Consequently, coal fines are often discarded. An estimated 8% of the total energy value of mined coal is lost1.Fluidized bed technology is often used to dry coal thermally, but this method is expensive and has an adverse environmental impact. The objective of this study was to investigate the removal of moisture from fine coal (<2 mm) in a fluidized bed operated with dry fluidizing air at moderate temperatures as the drying agent. The effects of different air temperatures and relative humidity levels were investigated in a controlled environment. The study further investigated the influence of coal particle size on moisture removal.The drying rate was found to increase with increasing temperature. The relative humidity of the drying air had a more pronounced effect on the drying rate, even at temperatures as low as 25°C.. It became more challenging to remove moisture as the particle size decreased. The gain in calorific value was greater than the energy required to dry the coal samples, showing that a fluidized bed using moderately warm dry air is an energy-efficient drying technology. The energy efficiency of the fluidized bed compared favourably with other thermal drying methods.Paper written on project work carried out in partial fulfilment of Degree in Chemical Engineering(NWU) - Pursuing Masters in Coal Beneficiation"

Jan 1, 2015

By T. Watanabe, S. Hayashi, M. Hayashi, K. Nagata, H. Fukuyama

Chemical states of fluorine in CaO-SiO2-CaF2glasses in a composition range of CaO/SiO2=0.5?1.3 and 5?25 mol%CaF2have been investigated by 19F solid-state NMR with and without MAS. The isotropic chemical shifts of the glasses are close to those of cuspidine crystal (59.4 and64.3 ppm with respect to C6F6) and CaF2crystal (58.6 ppm). The fluoride ions are coordinated with four or less than four calcium ions in this composition range. The chemical shifts move to the lower frequency with an increase in the CaF2content, whereas those are not affected by theCaO/SiO2ratio. The ionic distance between calcium and fluoride ions increases with an increase in the CaF2content. The chemical state of fluorine is not disturbed by the degree of polymerization of the silicate network. Comparing the MAS and static NMR spectra, the second moment attributed to 19F-19F dipole-dipole interaction has been estimated. The values of the glasses range over 3.1?7.3107Hz2andthose are larger than the calculated value of cuspidine crystal. This indicates that fluoride ions form Ca-F clusters in the glasses and that the size of clusters increases with increasing the CaF2content. Keywords: chemical state of fluoride ion, CaO-SiO2-CaF2glass, solid state 19F NMR spectroscopy

Jan 1, 2004

By Eric S. Weiss, Deno M. Pappas, Timothy M. Barton

During the past few years, the Pittsburgh Research Laboratory of the National Institute for Occupational Safety and Health (NIOSH) has been evaluating developments in sealant support systems from a ground control perspective. The proper selection and use of a sealant material can significantly enhance ground control which may result in a decrease in worker related injuries due to ground falls. The purpose of this paper is threefold: to briefly review the current state-of-the-art technology in shotcrete and membrane developments, to evaluate the preliminary findings of a long-term underground study of various types of sealant materials, and to examine installation practices that are critical for an effective sealant material. The underground study utilizes NIOSH’s Lake Lynn Laboratory Experimental Mine to evaluate the long-term performance of several types of shotcrete and membrane materials. Sealant performance to date have been evaluated on a regular basis over a two year period. Although the study is still ongoing, critical mining practices were identified that may seriously effect the bond of the sealant materials to the mine roof and rib; most notably, the importance of scaling and thorough cleaning of the rib prior to application. Also, results froman extensive series of Schmidt Hammer tests found that the shotcrete increased in strength by 70% during the humid summer months.

By R. Fernández, E. Marczak, A. Collins

Newmont roasting plant in Carlin, Nevada commenced operating in December 1994. Over the years, refractory ores and pyrite concentrates from different gold deposits constituted the feed to the facilities. Historical plant performance indicated that the roasting temperature was the main variable that affected the structural characteristics of the calcine which, in turn, affected the recovery of gold by cyanidation. Gold recovery as a function of roaster temperature was closely monitored since October 2000. Original design temperature was 550oC. Lower roaster temperatures of around 500oC resulted in gold recovery increase by more than 6 percent. This increase was directly related to an increase of the surface area of the calcine. The implementation of an “intelligent” process control system helped significantly in achieving steady low roasting temperatures thus achieving high gold recoveries between 92 and 93 percent. Under those conditions, several roasting campaigns with high-arsenic-containing ores were conducted, which resulted in a significant decrease of gold recovery. The reduced gold recovery was caused by the loss of surface area (e.g. porosity) of the calcine as the arsenic content of the roaster feed increased.

Jan 1, 2007

By D. E. Pollock, T. W. Beck, J. A. Organiscak

This work presents the findings from a number of NIOSH studies evaluating the impacts of emerging technologies that may reduce dust exposures for continuous mining and roof bolting personnel. These technologies include use of a wet head cutting drum on a continuous mining machine that places water sprays on the cutting drum instead of placing them on a manifold outby the drum. Evaluations at two separate operations showed that the use of the wet head sprays reduced dust levels at the miner operator in the return air, although these reductions were quite variable. NIOSH also assessed the effectiveness of a canopy air curtain for protecting roof bolting personnel. The data showed that dust levels were lower beneath the air curtain than outside the air curtain. This study also suggested several future modifications to the air curtain to in-crease its effectiveness. Finally, NIOSH evaluated mist drilling technology for its effectiveness in controlling respirable dust exposures of bolting personnel. A recent study showed that higher dust levels existed around a machine using the mist system compared to a machine using a conventional vacuum system for dust control. Unfortunately, the true impact of mist drilling was confounded by this machine operating downwind of the continuous miner for much of the study.

Ground support audits are sometimes necessary in ageing underground mines. Usually, the purpose of such audits is to assess the state of the ground support in various parts of the mine, identify areas that require attention and establish rehabilitation requirements. In 2005, Brunswick Mine, located in Bathurst, New Brunswick, Canada, completed a comprehensive mine-wide ground support audit. The areas examined included excavations in several mining blocks, as well as ramps, shaft stations, garages, shops, etc., throughout the mine. A vast amount of data was collected over a period of two weeks by multiple auditing teams. The audit was followed by a data digitisation exercise, and the creation of a data management system to store audit results and keep track of subsequent rehabilitation activities as they occur. One aspect of the data management system was the incorporation of a function for reporting on ground rehabilitation progress, along with the capability of updating mine level plans for easy visual presentation of this progress. This article describes the approach implemented at the mine to carry-out the audit, as well as the database constructed to manage the results.

May 1, 2009

By Rufus Flinchum

Two of the most critical concerns a blaster faces today are airblast and flyrock. Airblast, sometimes called noise or overpressure, can cause damage to neighboring structures, especially windows. It also is the cause for many vibration complaints. The human sense of hearing is often more acute to identifying source than the sense of touch. When a blast occurs, the airblast is what identifies the event. The vibration that may be felt is then associated with the airblast. Vibrations of greater magnitude, such as passing trucks or construction work on the house, go unnoticed because their sounds are familiar or expected. Flyrock is the number one killer and cause of damage. Elasting laws provide limits for these two concerns. Failure to comply may result in fines, closing of the operation, and even prison. Airblast and flyrock originate from two distinct areas, the open face and the bench surface. Each of these areas is addressed in the detailed proven procedures that follow, and if used by the blaster in conjunction with his own blasting knowledge, a sound blasting plan can be developed to minimize the occurrence of airblast and flyrock.

Jan 1, 1992

By D. R. Hack, N. M. Sirakov, M. L. Feves, M. Iwanowski

This paper presents a new approach capable of volume calculation of 3D reconstructed geological objects. The method is based on a well-known concept that states the volume of an object can be computed as the limit of the sum of the area of infinite number of sections, which cut the 3Dobject. Since shortage of input data about the geological objects usually exists, Mathematical Morphology and polynomial interpolation are employed to generate a set of intermediate sections between the set of initial sections. A Mathematical Morphology tool is applied to compute the area of the two of sets initial and generated 2D sections. Regularities together with Delaunay Triangulation are employed to perform 3D reconstruction. A formula is developed on purpose of volume calculation of the reconstructed objects. A set of ten theoretical, electrical resistivity cross-sections were generated and used to perform an experiment to show the capability of our approach to estimate the volume of complex 3D geological object in case of sparse 2D sections. The volume determined using the morphological approach presented in this paper show good correlation with the volume of the original input object. Advantages and disadvantages of our volume calculation approach are discussed in the conclusion of this paper. Keywords: electrical resistivity, sparse 2D sections, geological objects, smooth 3D visualization and volume calculation.

Jan 1, 2003

It is a great honour to be privileged to address The Institute for a second time as President and I appreciate it more than I can say. Eight years ago in Hobart I tried to cover the development of the mineral industry in Tasmania. That was a general subject. Tonight I want to be more specific - I propose to talk to you about rutile.The choice of subject for a Presidential Address is never easy. One is addressing an informed audience and the best one can do is to try to crystallize a particular subject and to present it in a form that willbe of interest to those who listen.I looked carefully at the addresses given by our Presidents over the past seven or eight years. The titles are impressive, the content excellent, and the length, as published, much greater than I had hoped.It is therefore with some trepidation that I have chosen as a subject one only of the three crystal forms of titanium dioxide. This subject is not as limited as may at first appear.There are two aspects with which I can deal - the mineral itself, which has become familiar as the major product of the East Coast beach sand operations, and the lesser-known &quot;synthetic&quot; product, which is the major pigment in almost all the white paints in common use today, and in cosmetics and white-walled tyres and toothpaste, and even the better types of fine papers. The synthetic form of rutile is&apos; the &quot;whitest&quot;of white pigments.

Jan 1, 1966

THE machine from which the following results were obtained makes one of a row of seven at work in the Junction North, Concentration Mill at Broken Hill, New South Wales. It consists essentially of a belt for dressing purposes, which travels round two 12-in drums situated at either end of a wooden frame. This frame is supported on wooden legs, and the whole is affixed to two iron castings, one on either side of the frame. A to-and-fro motion is obtained from an eccentric shaft, which, together with the stationary end of the supporting legs, is carried by the iron castings. A belt drive to the forward drum provides a constant rate of travel to the dressing belt.The top half of the dressing belt is supported on 3-in rollers spaced about 12-in centres along the frame of the vanner. A fairly thick dressing belt is used, and no trouble whatever is experienced from the formation of gutters between the rollers.These belts are 28 ft 4 in long, 4 ft wide, 3-16 in thick, and are made of two-ply 32-oz duck, with a coating of rubber on either side. The surface available for dressing is about 10 ft 6 in x 3 ft 8 in- ie, about 38&apos;5 square feet. The machine is driven atthe rate of 245 i-in strokes per minute, while the dressing belt travels at 15 feet per minute...

Jan 1, 1909