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By Masatsugu Taniguchi

Onoda Cement Co., Tsukumi is one of the largest limestone producer in Japan. From mines called Suisho and Ganji, it supplies limestone for cement plant, lime manufacture, iron and steel industries and for many purposes. The Suisho mine is highly productive, though it's operations are governed by the utmost regard for its impact on the surrounding environment. However, it became difficult to meet additional expanding demand and to assure continuity of high rate production. Present production rate 1s 6 million tons per year. The Ganji mine, some 2 km south west of the Suisho mine, began first-stage development In mid- 1973 and in january I976 started production. The capacity of major facilities is 9 million tons per year. Full production is predicted in 1979. Mining and milling methods of these mines under strict environmental considerations are discussed.

Jan 1, 1976

By Oscar A. Glaeser

The purpose of this paper is to present specific applications of the fundamental principles of mine ventilation and the means that are at our disposal to accomplish the task of maintaining a healthful atmosphere in small mines and prospect openings. Need for Ventilation The range between the maximum oxygen content of normal air and the minimum safe content is extremely narrow, approximately 5 per cent. Furthermore, normal air must not be contaminated with irrespirable gases beyond definite limits, and mineral dusts are equally dangerous, although health impairment is slower. Tables 1 and 2 present the more common respiratory hazards encountered in mines. Adequate ventilation is the most effective means available to reduce or eliminate these hazards. Mechanical ventilation has reached varying stages of perfection in coal mines and in many large metal mines. The small mines and prospects rarely have a definite plan of ventilation. As a consequence underground workers are frequently exposed to health and accident hazards. The annual reports of fatalities in mines in the Western States record yearly many deaths due to asphyxiation and deaths caused by men falling down shafts and raises after being overcome by gas. At times mining operations are slowed up because there is no means of driving out the gas after blasting. For that reason only one shift is worked, or men wait from one to several hours for the "smoke" to clear out. Methane gas in varying quantities is widely distributed throughout California. It has been encountered in explosive concentrations in the coast range. It has been found on the Mother Lode and in quicksilver mines near the coast. Methane explosions have not been uncommon in underground operations and in tunneling jobs. These conditions and records indicate that there is room for improvement in mine-air conditions.

Jan 1, 1937

By Walter Crafts

ALTHOUGH many elements reduce the tendency to porosity in steel castings, manganese, silicon, aluminum, calcium, titanium and zirconium appear to be most generally suitable for the purpose. The manganese and silicon contents are usually maintained in a fairly constant range. Sili-con-killed castings often are made to be sound with little or no addition of the stronger degasifiers. In many cases, however, it is more practical to utilize the stronger degasifying elements, aluminum, calcium, titanium and zirconium. Since they greatly modify the composition, shape, and distribution of the nonmetallic inclusions, and thereby the ductility, the strong deoxidizers must be used in such a way as to form the least harmful types of inclusions. As the reasons for failure always to obtain good results have not been obvious, an effort has been made to determine the mechanism of solidification of steels deoxidized to produce certain types of inclusions. Diagrams representing the mechanism of their formation have been constructed from the appearance of the nonmetallic con-stituents and have not only illustrated the limiting features of specific deoxidizing treatments with respect to inclusion formation and ductility, but have also indicated a relation between inclusions and resistance to hot tearing. Three different types of deoxidation treatment have been used for obtaining sound castings with relatively high ductility. The first method is to make and cast the steel under such conditions that deoxidation with silicon and a small addition of a strong deoxidizer assures soundness. The effective addition that will promote soundness without causing the formation of intergranular inclusions varies with the furnace practice and composition, but may be limited to about 0.025 per cent Al, Zr or Ti. Up to 0.10 per cent Ca and 0.15 per cent V are also used for this purpose. The inclusions in these steels are characteristically glassy silicates and round or irregular sulphides. As pointed out by Sims and Lillieqvist,1

Jan 1, 1940

By M. E. de Morton

Recovery and early recrystallization of heavily deformed, 99.98 pct Cr was investigated by studying metallographic structure. X-ray line sharpening, electrical resistivity, plastic properties, internal friction, and shear modulus. Appreciable recovery of resistivity, internal friction, and shear modulus together with some hardening and relief of internal strains occurred before the visible growth of a textured substructure above 350°C (recrystallization in situ). The complex behavior of shear modulus, internal friction, and its strain amplitude dependence during annealing are discussed qualitatively in terms of the relative mobility of dislocations. BY plastically deforming fully recrystallized 99.98 pct Cr above the brittle to ductile transition temperature, at -350°C. as in wire drawing, chromium can be made very ductile at room temperature. However, this ductility is lost on annealing at high temperatures when recrystallization takes place.' The present investigation was made to determine the general pattern of the changes in a number of physical and mechanical properties during recovery and recrystallization of heavily deformed chromium as part of an effort to elucidate the reasons for lack of ductility in the fully recrystallized condition. PREPARATION OF MATERIAL Wire specimens 0.027 in. in diam were prepared from arc-melted, electrolytic chromium by extruding, hot swaging and finally wire drawing at 300" to 350°C, i.e. above the brittle-to-ductile transition temperature. The total reduction in area of the wire was 98 pct and the last 3 pct of reduction was made at 100" to 150°C before cooling to room temperature. The impurity content of the material is shown in Table I. Internal friction and modulus measurements were made on a single specimen after annealing in situ at successively higher temperatures. For all other measurements, a fresh specimen was used for each temperature and annealing of these specimens was done in evacuated (0.001 mm Hg) and sealed silica tubes for 1 hr at the various temperatures up to 700°C. EXPERIMENTAL METHODS AND RESULTS The occurrence of a. transition in some physical properties of chromium at - 40°C2 imposed limitations on the temperature region where some of the measurements could be made. The reason for this transition in chromium is at present unknown but is probably associated with an antiferromagnetic state observed below - 40°C.* Heavy deformation produces an anomalous decrease in resistivity when measured at temperatures below -40°C4 though a normal increase is observed above this temperature. On the other hand internal friction in heavily deformed chromium5 over the temperature range 40" to 50°C is invariant with temperature. Above and below this range internal friction is strongly temperature dependent, increasing with increasing temperature. A temperature in this range was therefore convenient for both resistivity and internal friction measurements and for consistency the measurements of the mechanical properties were also made at about this temperature. No structural change has, however, been observed in careful X-ray measurements6 between -195" and 50°C, i.e. departure from cubic symmetry was not greater than 3:10,000; X-ray line sharpening measurements were therefore more conveniently made at room temperature.

Jan 1, 1962

By M. Nicholas, D. M. Poole

The diameters of sessile drops have been found to increase linearly with time in five reacting binary metal systems. The spreading rates of the drops are markedly dependent on temperature and on prior alloying of the solid with the lower melting point metal, hut are independent of the drop volume, wetting atruosphere , solid-surface roughness, and prior alloying of the drop with the substrate metal. A mechanism has been suggested that relates the linear-spreading rate to lateral diffusion of the liquid-metal atoms into the solid at the drop edge. An Arrhenius- type equation has been derived that describes the temperature dependence 0) the spreading rate, and although the agreement between the actual and the predicted pre-exponen-tial terms is poor that between the activation energies is excellent and the variation in the spreading rate of copper on Ni-Cu alloys produced by different extents of alloying can be predicted with considerable accuracy. CHEMICAL interactions frequently change the wetting behavior of solid-liquid systems causing, for example, "secondary spreading1 of sessile drops beyond the size defined by the surface and interfacial tensions of the unreacted components. The kinetics of the contact-angle decreases associated with this spreading are similar for many systems, but few studies have been made with the objective of determining whether the similarities are a reflection of a common mechanism. Some workers2,3 have assumed the secondary spreading is controlled by changes in the liquid surface and liquid-solid interfacial tensions and hence by the composition of the liquid, and contact-angle changes measured by the vertical-plate technique have been used to follow the course of liquid-solid chemical reactions.4 Other processes that have been invoked to explain these time-dependent changes in specific systems include the removal of adsorbed gas from the liquid-solid interface.5 penetration of containment layers on the solid Surface,6 interdiffusion,1,7 reori-entation of the solid surface into a wettable configuration: vapor-phase transport of the liquid onto the solid in advance of the drop,9 and, from vertical-plate studies. capillary flow between oxide layers and the solid surface.10 One of the reasons for the profuseness of these suggestions may be the complexity of the contact-angle change kinetics. However, in an analysis of secondary spreading gold and copper on UC,11 it was found that the diameter of the contact area between the sessile drop and the solid surface showed a simple linear increase with time although contact-angle changes were more complex. To check whether the linearity was merely fortuitous! additional exploratory work was conducted with four reacting metal-metal systems: Au on Ni. Cu on Ni, Cu on Fe, and Ag on Au. Linear spreading was observed in every case even though the kinetics of the contact-angle changes were complex. A further detailed study of the kinetics of linear spreading of five reacting metal-metal systems has been made with the object of determining the mechanism involved. The influence of variables such as temperature, drop volume. and the initial composition of the drop on the linear-spreading rate has been measured and compared with those predicted by a number of possible mechanisms. The systems employed in this study (Cu and Au on Ni and Pt, and Ag on Au) were selected because of the availability of potentially relevant chemical and physical property data. the simplicity of their phase diagrams at the wetting temperatures, and the ease of experimentation. EXPERIMENTAL TECHNIQUES The purities of the metals used in the study were: copper, 99.9 pct; gold. 99.96 pct; nickel, 99.2 pct; platinum 99.99 pct; and silver, 99.999 pct. The wetting tests were performed in a split tantalum tube vacuum resistance furnace of a conventional design. The furnace element was held vertically and was 1 $ in. in diam and 6 in, long. Viewing ports were provided in the water-cooled chamber to enable the specimens to be observed in both the horizontal and vertical planes. The temperature in the hot zone of the furnace could be held at 1500" i 5°C for an indefinite time. The surfaces of the solid-plaque metals were ground flat on Microcut paper and both the sessile drop and substrate metals were ultrasonically cleaned in methyl alcohol prior to their insertion in the furnace. After loading, the furnace was pumped down to a pressure of 2 x 10-5 mm of mercury and degassed for 30 min at 900° to 950°C. The temperature was then increased at more than 100°C per min to that used in the wetting test. The vacuum at the wetting temperature was better than 5 x 10-5 mm of mercury. Dewetting and retraction of the drop on cooling did not occur and the contact-area diameters, therefore, were measured after solidification with a vernier traveling microscope. The diameters quoted later are arithmetic means of ten measurements. The standard error of the mean never exceeded 3 pct and was often less than 1 pct.

Jan 1, 1967

By E. Miller, J. M. Eldridge, K. L. Komarek

Aclivilies of magnesium in liquid Alg-Si alloys have been delermined between 5 and 60 at. pcl Si, close to the melling point of Mg2Si, by an improved isopieslic melhod. Silicon specinrens, held in alumina crucibles and graplrile conlainevs of special design, were healed in a letrlpevalure gvadient and equilibrated with mag-nesilcrrl rapor in a closed lilanium system. The ther-madynamic Junctions were calculated and compared with the thermodyuamic properties of the other three mg- Gvoup IVB systems. Lattice paramelers of three Mg2X compounds were measured. The bonding in the Mg2X compounds is largely covalent with small and uarying amounts of metallic and ionic conlvibutions. The Mg-Si phase diagram1 has one congruent melting compound, Mg2Si, of essentially stoichiometric composition, two eutectics, and very limited terminal solid solubilities. Little information is available on the thermodynamic properties of this system. The free energy of formation of Mg2Si has been determined by the Knudsen cell technique2 in the range 572" to 680oC, by the transportation method3 between 858" and 950oC, and by the electromotive-force method4 in the range 400o to 600°C. Kubaschewski and villa5 and caulfield6 have measured the heat of formation of Mg2Si. An electromotive-force study of magnesium-rich liquid alloys was recently published by Sryvalin el al.7 The present investigation was undertaken to complete a general survey of the thermodynamic properties of the homologous series of Mg-Group IVB systems, i.e., Mg-Pb,a9,Mg-Sn,10,11 mg-Ge,12and Mg-Si. An isopiestic technique, previously developed for similar measurements on liquid Mg-sn11 and Mg-Ge alloys,12 was modified for the Mg-Si system. Specimens of the nonvolatile component, silicon, were contained in dense alumina crucibles placed inside covered graphite crucibles which were heated in a temperature gradient in an evacuated and sealed titanium reaction tube and equilibrated with magnesium vapor of known vapor pressure. The alumina crucibles prevented contact between the highly corrosive liquid Mg-Si alloys and graphite. The graphite cruci- bles effectively preserved the high-temperature equilibrium composition of the liquid alloys containing highly volatile magnesium on termination of the experiments during the quench to room temperature. EXPERIMENTAL PROCEDURE Silicon of semiconductor-grade purity (E. I. du Pont de Nemours and Co., Brevard, N.C.) and 99.99+ pct Mg (Dominion Magnesium Ltd., Toronto, Canada) were used. Graphite crucibles with press-fitted lids were machined from high-density (1.92 g per cu cm) rods (Basic Carbon Corp., Sanborn, N.Y.) which had a maximum ash content of less than 0.04 pct. The alumina crucibles had a purity of 99.7+ pct (Triangle RR grade, Morganite, Inc., Long Island City, N.Y.). In preliminary runs the liquid alloys were contained in graphite crucibles following the exact procedure developed for the Mg-Ge system.'2 These runs failed due to appreciable reaction between the molten Mg-Si alloys and graphite, and the results have been discarded. The procedure was then modified and the Mg-Si alloys were subsequently held in alumina crucibles. For most of the runs alumina crucibles of known weight and approximately 6.3 mm ID, 12.5 mm height, 1.0 mm wall thickness were loaded with weighed amounts of silicon and encapsuled in tightly covered weighed graphite crucibles 5/16 in. ID, 2 in. helght, 3/32 in. wall thickness). The graphite crucibles were machined from rods which were 85 pct of the theoretical density. These crucibles were therefore sufficiently porous so as to permit magnesium vapor to effuse through the silicon under the experimental conditions of approximately 970O to 1220°C and 1 day equilibration time. However, negligible magnesium was lost from the crucible during the quench due to the slow effusion rate through the pores of the graphite. The inner alumina crucible prevented the liquid alloys from contacting the graphite, and the very tightly fitting graphite crucible lids served to retain any magnesium vaporizing from the alloys inside the crucibles during the quenching step.12 The loaded silicon-alumina-graphite cells were positioned, one above another, on a 16-in.-long titanium thermocouple well and tied securely to the titanium tube with thin molybdenum wires held in grooves around the circumference of the graphite crucibles. A thin (0.005-in.) molybdenum strip prevented contact between the graphite crucibles and the titanium. This assembly was lowered into a titanium reaction tube (la in. ID, 16 in. long, $ in. wall thickness) closed on one end which contained a 11/2-in.-long cylinder of magnesium at the bottom. The inner titanium thermocouple well was positioned eccentrically in the large tube because of the eccentric mounting of the cells on the well. Appropriate modifications of the titanium cap"'12 were made to join the inner and outer titanium

Jan 1, 1968

By E. A. von Hahn, T. R. lngraham

The rates of cementation of pd11 on electropolislzed copper cylinders were studied in aqueous perchloric acid solutions at pdII concentrations from 0.02 to 0.1 mM. The cylinders were rotated at various high speeds to reduce the diffusion layer to a minimum thickness. In 0.1 M HClO4 solutions, the cemented palladium is dense, adherent, and shiny. The rate data indicate that there are two stages in the deposition. In the initial stage, the rate of cementation is first order with respect to the pd11 concentration. The second stage is much slower. The first stage is consistent with rate control by the diffusion of pd11 ions to the copper surface, and/or chemical reaction at the surface, and the second stage is consistent with rate control by the diffusion of copper ions from the cop-per surface through the deposit of cemented palladium, out to the main body of solution. In 0.001 M HClO4 solution, only the first stage is evident and the rate is more rapid than at higher acidities. This rate enhancement is attributed to PdOH+ ions that predominate at low acidity and aye more reactive than unhydrolyzed pdII. The deposit is porous and loose. All of the cemented deposits are Pd-Cu alloys rather than pure palladium. Activation energies are 9.5 kcal per mole in 0.1 M HClO4 and 7.4 kcal per mole in 0.001 M HClO4. CEMENTATION or displacement reactions occur between aqueous solutions of metal salts and immersed metals according to the general equation: where M1 is electrochemically the more noble metal. Although these reactions find considerable application in metals recovery processes (e.g., the cementation of copper192 or gold3), in electrorefining processes (e.g., solution purification before electrolysis4,5), and in plating and metal finishing processes,6 few studies have been made of the kinetics of such reactions.7-9 The rates of cementation reactions will depend on one or more of the following factors: a) chemical reactions at the metal-solution interface; b) ionic transport to or away from the interface;'-' and c) the character and adherence of the cemented deposit on the substrate metal,6a,10 because the deposit will inhibit the rate of transport of dissolving ions (M2m+) into the solution. In this investigation, the kinetics of the early stages of cementation were studied to obtain an understanding of the reaction mechanism under conditions in which the deposit was sufficiently thin that its inhibiting effect could be disregarded. To achieve this, very dilute solutions in Mn+ were used. Cementation rates are often fast in the initial stages and transport-contr01led.9 To find conditions under which transport control would shift to chemical control, very high stirring velocities were used to minimize the diffusion-layer thickness. Of the many possible cementation reaction systems, the palladous perchlorate-copper system was chosen for this investigation because it was believed to involve simple ion-for-ion exchange. In addition, there are no interfering side reactions, such as the reduction of hydrogen ions, and anion effects are usually absent in perchlorate solutions. EXPERIMENTAL Materials. Reagent-grade chemicals and redistilled water were used in all experiments. Palladous perchlorate stock solutions (0.02 M) were prepared by dissolving 99.5 pct Pd sponge (Johnson Matthey and Mallory Ltd.) in concentrated nitric acid, adding concentrated perchloric acid, evaporating twice slowly (to prevent PdO precipitation) to a small volume, and diluting in a volumetric flask. To prevent gradual hydrolysis of PdII, the stock solutions were made 0.4 M in HC104. Tests for pdIV (Ref. 11) and C1- were negative. Copper strips were cut accurately from 0.025-in. electrolytic tough pitch sheet, Sample 1 (Mines Branch stock or Canadian Copper Refineries Ltd., Montreal), or from oxygen-free, high-conductivity sheet, Sample 2 (American Metal Climax O.F.H.C. brand, sold by Utility Brass and Copper Corp., Brooklyn). The strips were annealed for 1 hr at 335°C in a stream of purified nitrogen (Union Carbide, Linde Division) which had

Jan 1, 1967

By James H. Courtright, Kenyon Richard

TOQUEPALA is a porphyry copper deposit in which mineralization is localized by a large breccia pipe formed in close genetic relation to intrusive rocks. The deposit is in southern Peru, 55 airline miles north of the small city of Tacna and the same distance inland from the port of 110. Quellaveco and Cuajone, geologically similar deposits, lie 12 and 19 miles north of Toquepala. Chuquicamata is 400 miles to the south. The deposit is high on the southwestern slope about 20 miles from the crest of the Cordillera Occidental of the Andes Chain. It lies in a mountainous desert where the steep southwesterly slope of the Andes is dissected by a succession of rapidly downcutting, deep canyons. Local topography is moderately rugged with a dendritic drainage pattern and an elevation of 8000 to 14,000 ft. Volcanic peaks along the crest of the Cordillera rise over 19,000 ft. Local precipitation, including a little snow, amounts to about 10 in. during January and February, but general runoff in the region is slight. Throughout southern Peru the springs and streams are widely separated. Crude canals irrigate small farms on terraced slopes along the streams and provide sparse subsistence to the semi-nomadic inhabitants. During the past decade, engineering and geological explorations of the region, as well as the mineral deposits themselves, have required construction of a network of several hundred miles of roads. Before this, roads extended only a few miles inland. Many areas still can be reached only by trail. Toquepala was briefly described in 19th century geographical literature as a copper deposit, and it received desultory attention from Chilean prospectors early in the present century. It was first recognized as a mineralized zone of possible real importance by geologist O.C. Schmedeman during an exploration trip for Cerro de Paso Copper Corp. in 1937. The discovery was late as compared to earlier recognition of Chuquicamata, Potrerillos, and Braden of Chile and Cerro Verde of southern Peru. This was due partly to the region's difficult accessibility but principally to the obscure character of the outcrop evidence of copper. From 1938 until 1942 Cerro de Pasco Copper Corp. partially explored the deposit by adits and diamond drillholes. This campaign was supplied by a 60-mule pack train continuously shuttling over a 30-mile trail. Northern Peru Mining & Smelting Co., a wholly owned subsidiary of American Smelting & Refining Co., undertook regional engineering stud- ies in 1945 and drill exploration in 1949. According to published data1 the deposit contains 400 million tons of open pit ore averaging a little over 1 pct Cu. It is currently undergoing large-scale development by Southern Peru Copper Corp., which is owned by American Smelting & Refining, Phelps Dodge, Cerro de Pasco, and Newmont Mining. Summary of Geology: The deposit is situated in a terrane composed of Mesozoic(?) and Tertiary volcanic rocks intruded by dioritic apophyses of the Andean Batholith. These formations are exposed in a northwesterly trending belt about 15 miles wide. Along the northeast they are unconformably overlain by Plio-Pleistocene pyroclastic rocks, which occupy much of the crest of the Andes, and along the southwest they are covered by the Moquegua formation of Pliocene(?) age. The mineralized area, oblong in shape and about 2 miles long, has been a locus of intense igneous activity. Several small intrusive bodies having irregular forms occur within and adjacent to a centrally located, large breccia pipe. The mushroom-shaped orebody consists of a flat-lying enriched zone of predominant chalcocite with a stem-like extension of hypogene chalcopyrite ore in depth within and around the pipe. This breccia pipe is relatively large and has been formed by repeated episodes of brecciation. Small satellitic pipes occur at random within a 2-mile radius of this central pipe. These too were individual sourceways of mineralization, although not always of ore grade. Within and around the zone of breccia pipes and mineralization there are a few faults and veins, but these are discontinuous random structures of minor significance. There are no regional or local systems of faults or other planar structures recognized which could account either for the mechanical development of the breccia pipes or for their localization as a group or as individuals. Hydrothermal alteration is pervasive in the zone of mineralization. Clay minerals appear to be abundant in places, but their percentages are undetermined. Quartz and sericite are the principal alteration products, and in many instances original rock textures are obliterated. The principal sulfides, hypogene pyrite and chalcopyrite and supergene chalcocite, occur mainly as vug fillings in the breccia and as small discrete grains scattered through all the altered rocks. Sulfide veinlets are relatively scarce. Sulfides are more abundant and alteration is more intense in certain rock units, such as the diorite and most of the breccias. Although the Toquepala mineral deposit is similar in most respects to the porphyry copper deposits of southwestern U. S., it most closely resembles the Braden deposit of Chile, as described by Lindgren

Jan 1, 1959

By R. F. Hehemann, Darrell W. Smith

The kinetics of alloying- in W-5 rot pct Re powder compacts were investigated at temperature about the upper limit for the formation of the x phase, such that a single intermediate phase was involved in the process. The rates and directions of motion of the a-o and o-b interface were assessed as functions of tinze at the sintering teri7peraticve by quantitative izetallog-ralhic techtziques. The iiotion 01 these interjuces could be specified approxitnate1.y by u Parabolic )-ate law and deviations from this ,rate law were attribuled to a complex interaction between surface dif'fusion and volume diffusion during the initial stages of sintering. WHEN binary or more complex alloys are produced by sintering compacted blends of elemental powders, a complication is encountered which does not arise in the sintering of pure metals. In addition to concern for grain size and densification, the rate of inter diffusion of the component elements must be considered. The general problem of alloying during sintering has been treated by numerous investigators.'-7 These investigations have been concerned only with systems that form continuous series of solid solutions and a concentric-sphere diffusion model4 provides a useful description of homogenization in these stems.' Some controversy remains, however, over the contribution of surface and grain boundary diffusion to the homogenization process. Heckel% ePorts that homogenization can be described by volume diffusion at all temperatures, whereas other invetiators'' recognize the importance of surface and grain boundary diffusion, particularly at lower temperatures. Analysis of the homogenization process in partially miscible systems is complicated by the motion of the interfaces separating the individual phases. A simple analytical solution does not exist for such finite systems with spherical symmetry. It was the purpose of this work to examine the kinetics of the formation and dissolution of an intermediate phase in a binary system through an assessment of the motion of the interfaces separating this phase from the terminal solid solutions. PROCEDURE The W-Re system is an example of a partially miscible binary system and was selected for study because of its current importance in refractory-metal technology. The equilibrium phase diagram, Fig. 1, shows that the o phase will be formed by interdiffu-sion between tungsten and rhenium. At temperatures between approximately 2125" and 282O°C, the o phase will appear as the only intermediate phase in the diffusion system. In this work, a mixture of elemental powders containing 5 pct Re was employed. In such a mixture, the rhenium particles will be distributed randomly in a tungsten matrix. During sintering, a o-phase layer will form at the W-Re interface. The development and subsequent disappearance of the o phase are controlled by the relative rates and directions of motion of the 0-0 and a-p interfaces. The motion of these interfaces can be inferred from quantitative metallographic measurements of the average radii of the o shells surrounding rhenium particles. Elemental tungsten and rhenium powders of commercial purity were employed in these investigations. The rhenium powder was spheroidized from +200 mesh agglomerates by plasma-arc spraying and was then classified to yield a powder composed of essentially

Jan 1, 1967

By F. F. Craig

Many full-scale waterflooding operations are preceded by pilot floods, one purpose of which is to provide an estimate of recoverable oil. A laboratory model study was made to determine the influence of the producing wells' effective productivity on the oil recovery efficiency of single five-spot pilots, as well as single injection well pilot floods. The effective productivity is indicated by the value of Condition Ratio, defined as the actual well productivity to that of on undamaged and non-stimulated, normal-sized well in the same formation. The effects of initial gas satrcration and mubility ratio on recovery eficiency were also investigated in this model study. Model test results skowed that at favorable mobiliry ratios, a five-spot pilot flood can provide a direct quantitative estimate of the recoverable oil in the pilot area. If the pilot producer's Candition Ratio is 2.2 or more, upwards of 90 per cent of the recoverable oil in the pilot area is recovered from the inside producer, regqrdless of the mobility ratio or initial gas saturation. This Condition Ratio can be achieved with preyent fracturing techniques. Model studies also showed that over the range of imposed injection pressure differences and regional pressure gradients normally encountered in field operations, there was no effect on the recovery efficiency of a five-spot pilot waterflood. Model studies of single injection well pilot waterfloods showed that with no initial gas saturation, the total oil recovery at the offset producing wells can indicate the oil recovery possible by full-scale waterflooding. It is essential that the Condition Ratios of the offset wells be above 1.4. If an initial gas saturation exists prior to water injection, the recoverable oil cannot be directly evaluated by a single injection well pilot flood. However, the production per formance of such a flood can be used to provide information on volumetric sweep efficiency. INTRODUCTION Oil reservoirs are conlplex structures and cannot always be fully studied in the laboratory. Therefore, many operators consider it prudent to evaluate a waterflood prospect by means of a pilot flood. Pilot waterfloods generally involve one of two well arrangements: a single five-spot pilot waterflood, involving four injectors and an internal pilot producing well; and a single injection well pilot flood (sometimes called an inverted five-spot pilot) having one injector and four sur- rounding pilot producers. Some pilot floods are composed of multiple five-spot pilot patterns. To yield information applicable to field-wide performance, the pilot must be located in a representative portion of the reservoir. Pilot floods generally are conducted for one or more of the following reasons: (1) to determine whether water could be injected at desirably high rates, (2) to determine whether an oil bank or zone of increased oil saturation is formed by water injection, and (3) to estimate the oil recovery by waterflooding. Many of the early pilot water-floods were conducted for only the first two reasons. As soon as a buzz in oil production was obtained in the pilot, water injection was initiated throughout the entire lease or field. A number ot laboratory studies have been directed toward determining conditions under which a pilot flood could yield a quantitative estimate of the oil recovery possible by full-scale pattern flooding. One of the early studies of single five-spot pilot flooding' showed that well damage to the inside pilot producer could reduce the total amount of oil recovered. In a study of the single injection well pilot flood pattern,' the results indicated that if the model boundaries were no closer than a half-well spacing beyond the pilot pattern, the pilot performance in the laboratory is unaffected by these boundaries. In another study,? he effect of initial gas saturation and mobility ratio on the ratio of production to injection rate for various groupings of five-spot patterns was defined by mathematical and analog methods. In a study4 involving both potentiometric and flow model experiments at a mobiliry ratio of unity, four different pilot patterns were studied. These included a single five-spot, a single injection well pilot, a cluster of four single injection well pilots and six inverted five-spots. In this study the ratio of well diameter to the distance between injection and producing wells was held constant at 1:1000. The effect of the 7 ratio-—the ratio of the pressure drawdown at the producing wells to the pressure build-up at the injection wells on the pilot performance-was studied. The values of 7 ratio ranged from 0 to 0.34. Results showed that both the total oil recovery and the total fluid production from the pilot relative to the cumulative injection increased with increasing values of the 7 ratio. The effect of both the ratio of injection to producing rates and mobility ratio on the oil recovery performance of a liquid-saturated single five-spot pilot flood was studied in a series of flow model tests.5 Rate ratios ranged from one to four, and mobility rates ranged from 0.1 to 10. Resulls of these tests showed that at low rate ratios, the pilot producers may recover up to four times the recover-

Jan 1, 1966

By T. W. Guy

IN approaching the problems of sampling coal, a brief statement of certain facts that are more or less taken for granted may he helpful: 1. The coal-mine operator needs reliable data as to the physical and chemical characteristics of his coal in order to plan and control intelligently its mining, preparation, and marketing. The consumer needs such data in order to select the equipment and the coal best suited to meet his requirements, to check the quality of fuel delivered, and the efficiency of its use. Various government control agencies require such data as a basis for classifications and establishment of limits, for use in carrying out the requirements of federal, state or municipal laws. 2. All such data must be obtained by analyses, measurements, or tests made on samples, which are taken to represent the coal tested. It is now becoming generally recognized that, in accordance with statistical laws, test results from samples are not expected to represent the exact qualities of the lot or lots from which they are taken, except within statistical, or "expected" limits. Such limits are definitely specified by some present standards of the American Society for Testing Materials and the British Standards Institution. 3. Samples that give ash within satisfactory limits are usually assumed to be sufficiently accurate for other analyses, except under special conditions such as meeting close specifications for coals showing wide variability in sulphur, fusibility of ash, or other quality. 4: In. modern coal sampling the increment is recognized as the basis for taking samples. For a given accuracy the number and weight of increments specified are increased with: (a) the expected ash, and (b) the top size designation of the lot to be sampled. 5. It is extremely important that every sampler recognize that: the specified number and weight of increments are minimums, and that. the precautions to be used in order to take them properly are also minimums; that in the reduction of the gross sample the sizes specified for the coal after each stage of the crushing are maximum; that the quantities specified to be taken after each crushing stage are minimum; that any short cuts or failures to meet the requirements specified will reduce the statistical accuracy of the results, although it is possible that one or two checks on a few results may seem to show otherwise.

Jan 1, 1943

By C. S. Brooks

Several of the commonly used methods for deter-mination of effective grain densities of minerals have been evaluated for accuracy and precision, and their applicability to various types of petroleum reservoir minerals tested. Consideration was given to the effect of consolidation, swelling clay, and wettability on these grain-density determinations. Procedures with helium displacement, a modified low-pressure Boyle's law porosimeter, and liquid displacement (water, n-decane, and n-octanol) were tested. The helium-displacement procedure was used primarily as an independent reference for which the effects of fluid-solid interaction, e.g., adsorption and wettability, were negligible. The procedures with the Boyle's law porosimeter and with liquid displacement are the methods in common use. Minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The number of samples tested, while not large, was adequate to permit application of statistical methods. Grain-density measurements on calcite (Iceland spar) provided a basis of comparison for the accuracy and precision of the procedures under investigation for a material with a high degree of chemical and physical homogeneity and for which fluid-solid interactions were at a minimum. Liquid-displacement procedures (water or n-decane) provided the greatest reliability and precision for measurement of the grain densities of the limestone tested. Gas-displacement procedures (helium or Boyle's law porosimeter) provided the greatest reliability and experimental convenience, if not the greatest precision, for the measurement of the grain densities of the swell- ing clay, Wyoming bentonite, and the shah sandstones which -contained appreciable amounts of swelling, in-terstitial clays. These experiments were designed to evaluate the applicability of the grain-density procedures in common we to some of the less tractable minerals—tight limestones, shaly sandstones, and swelling clays. The results should provide a useful basis for a selection of the method most suitable for application to the various petroleum reservoir minerals encountered and especially for use in the estimation of formation porosity. INTRODUCTION These experiments were undertaken to evaluate the accuracy and precision of several commonly used methods for determination of effective grain densities of minerals, and to test their applicability to various types of petroleum reservoir minerals. Consideration was also given to the effect of consolidation, clay, and wettability on these grain-density determinations. Procedures used included measurements with helium displacement, with a modified low-pressure Boyle's law porosimeter, and with liquid displacement (water, n-decane, and n-octanol). The minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The accurate determination of the porosity of petroleum reservoir formations, in particular those of low porosity, has received much attention. Both bulk-volume and grain-volume measurements necessary in the evaluation of porosity have been examined by many investigators with the objectives of improving both the accuracy and the precision of these determinations. In this investigation statistical criteria for selection of the most reliable and suitable procedure for use with a given type of mineral are demonstrated. The grain-volume measurement procedures appear to be the most susceptible to improvement.

Jan 1, 1958

By N. A. Stockett

Southeast Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. Tons World production................. 2,000,000 United States Production .........- 460,000 Southeast Missouri production..... 142,000 The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country's production. The largest previous year's in in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averaging over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. I, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,980,000 short tons of pig lead. • About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of st. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in st.Francois county, Prospecting In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jack-hamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling—100-ft. centers of holes, and sometimes less—is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more. To date, geophysical and other methods of prospecting, apart from diamond and Mining Practices of the St. Joseph Lead Company in Southeast Missouri

Jan 1, 1943

By N. A. Stockett

Southeast Missouri is the largest and oldest lead-producing district in the United States. For the year 1941, the statistical picture of pig-lead production, stated in short tons (partly estimated by the Engineering and Mining Journal) is as follows. Tons World production................. 2,000,000 United States Production .........- 460,000 Southeast Missouri production..... 142,000 The consumption of primary lead in the United States in 1941 was approximately 900,000 tons, or almost double the country's production. The largest previous year's in in the United States was 718,000 tons, in 1926. The largest quantities of lead are used for cable sheathing, storage batteries and white lead. During 1941 tetraethyl lead for auto and aviation gasoline consumed 50,000 tons of lead. The entire lead production of Southeast Missouri is now mined by the St. Joseph Lead Co., whose dominant position as the largest producer in the United States of lead directly from ores is best shown by the fact that in 1941 it produced approximately 31 per cent of the lead production of the United States from its mines in southeast Missouri, where 22,000 tons of ore, averaging over 3.00 per cent lead, is mined per working day. It is known that lead was mined at Mine La Motte, Madison County, Missouri, by Renault in 1723. Other white men and Indians probably did some mining prior to that time. Since 1865, the recorded production to Jan. I, 1942, shows that the St. Joseph Lead Co. and the various other companies that have operated in St. Francois County mined lead ore, which, after milling and smelting losses produced 5,980,000 short tons of pig lead. • About 95 per cent of the present lead production of Southeast Missouri is mined in St. Francois County. The northern part of this area is 60 miles south of st. Louis. The remainder of the lead is obtained at Mine La Motte, about 25 miles southeast from the center of the producing area in st.Francois county, Prospecting In this district, most of the ore is discovered by surface and underground diamond drills and by prospect drilling underground with rock drills. Each 2-ft. length of the cuttings from these Jack-hamer prospect holes is assayed for lead. These holes are marked and the records are entered on maps. It has been found that close drilling—100-ft. centers of holes, and sometimes less—is necessary in order to locate most of the smaller commercial ore bodies, many of which previously had been missed by drilling the areas with holes spaced 200-ft. centers or more. To date, geophysical and other methods of prospecting, apart from diamond and Mining Practices of the St. Joseph Lead Company in Southeast Missouri

Jan 1, 1943

By John B. Dilwoth

This paper treats primarily of the valuation of developed coal properties by the method of capitalizing their estimated average future earnings. However, reference is also made to valuations of undeveloped coal lands and to various methods of appraisal other than by future earnings. Fundamental Valuation Principles Before discussing in detail coal property valuations, a few statements bearing on the general subject will be made to present certain of the writer's views on the question as a whole. 1. A certain property at a given time has but one true value. This is not universally admitted. The appraiser rather frequently finds that a coal owner has in mind three valuations for his holdings; one, the figure at which he feels they should be appraised for taxation purposes; another, the much higher one that should be used if a loan is to be negotiated on the property; and a third, intermediate between the other two, the price for which he would be willing to dispose of his holdings were they for sale. The last is usually nearest to the true value, and because this is so the statement is generally accepted that the fair value of such a property is the price arrived at by negotiation between a willing seller and a willing buyer who are otherwise disinterested. 2. Notwithstanding the foregoing, it is only very generally and approximately true that the proper measure of the value of a given developed' coal acreage is the unit or per-acre price for which one or more bodies of similar coal in the same district have been sold recently. To give a few reasons why such a measure of value can not be strictly applied, it may be noted: a. That sales are often forced by circumstances at times when the coal business is depressed and buyers can be found only for properties that are offered at figures far below their true value. b. That conversely, during periods of unusual prosperity, abnormally high prices are paid. Such conditions obtained several years ago when coal brokers, with very profitable contracts but no sure source of supply, were bidding against inexperienced or shortsighted operators for proper-

Jan 1, 1928

By D. A. Elgillani, M. C. Fuerstenau, M. C. Kuhn

The species responsible for flotation when xanthate is added as collector for pyrite is dixanthogen. Measured oxidation potentials of these systems show that xanthate should be oxidized to dixanthogen, and the presence of dixanthogen on the pyrite surface is confirmed by infrared absorption. Zeta potential measurements are presented and related to collector adsorption. In spite of the normal presence of pyrite in most sulfide ore deposits, only a modest amount of study has been devoted to the xanthate-pyrite flotation system in the absence of activators and depressant~.'-~ As a result, little is known about the mechanism of xanthate adsorption on pyrite. From the few studies that have been made, however, a number of significant observations have been forthcoming. For example, the dependence of flotation response on the state of oxidation of the surface was noted in two studies — one conducted by Plante and Sutherland4 and a later one by plaksin.~ In another study, Gaudin and wilkinson3 found that ferric xanthate was not present on a pyrite surface. In a later investigation, however, Gaudin' and his colleagues did extract a small amount of ferric xanthate into benzene when pyrite was ground in an evacuated mill with water, benzene, and xanthate. This quantity was apparently

Jan 1, 1969

By H. D. Hoskold

It was not for the purpose of asserting any superior knowledge or authority, but simply of clearing up, in greater detail, some points casually mentioned in Mr. Scott's able paper, that the writer entered, some two years ago, into the discussion which that paper initiated. In such matters there is always room for differences of judgment, as well as for additional data, which may modify or complete the conclusions even of the best authorities. Those who are immersed in the duties of practical administration or work in the field, and who, being remote from the great scientific national libraries, are obliged to rely on their private collections, and to supplement them by their recollections of earlier studies, labor under special disadvantages in such a discussion; and it must be to the scientific and engineering world a matter for gratitude that Mr. Lyman has been willing to give the benefit of his advantages in this respect. Mr. Lyman would, however, doubtless at once disclaim the conclusion that his masterly summary constitutes " the last word " on this subject, and welcome further evidence, comment and criticism, such as the various contributors may continue to offer. This, therefore, is the motive, and must be the excuse, of the introduction by the writer of the following observations. The Miners' Dial.—Many years since, the writer employed a miners' dial, older in type than Fig. 12,* but without any attached spirit-level, made by Thomas Jones, a pupil of the great Ramsden. Jones was one of the old London makers and opticians, and enjoyed great reputation for accuracy in the con-

Jan 1, 1902

By C. W. Covington, H. C. Cook, J. F. Libsch

Sputtered aluminum thin films were prepared in each of two conventional bell-jar vacuum systems. One system utilized an inner "getter sputtering" enclosure; the second system was a standard diode sputterirlg arrangement. Consistent and repeatable film properties were obtained in both systems provided sufficient cleanup and presputter time was allowed. The various problems associated with aluminum sputtering are discussed, with pavticular attention to the vzinimization of film contamination by outgassing and oxidation. The growth and structure of the aluminum thin films were studied with the aid of electron wzicroscopy and related to deposition rate, substrate temperature, and film thickness. The resistivity of the films was correlated to film structure and surface roughness. Resistiuities as low as 3.5 microhm-cm (2.3 x bulk resistiuity) were measured for relatively thick films (20,000). THIS investigation was undertaken to explore the problems and film characteristics associated with the sputtering of aluminum. Earlier work reported on aluminum sputtering has stressed the contamination of both the cathode and film as well as abnormally low deposition rates.' Data on sputtering yields,3 however, indicate that aluminum sputtering could be practical. Recently, it was shown by Theuerer and Hauser3 that aluminum sputtering was feasible in a conventional oil-diffusion pumped vacuum system provided an inner "getter sputtering" enclosure was employed to minimize gaseous contamination. This technique employs the getter action of aluminum to produce extremely low reactive gas partial pressures in the deposition zone. Aluminum films have already found use in solid-state electronic devices such as transistors and integrated microcircuits. To the present time, most aluminum films have been prepared by evaporation due to the ease with which this metal can be evaporated. Controlled sputtering of aluminum offers a number of advantages over evaporation, however, such as 1) manufacturing compatibility with other metals which must be sputtered, 2) better control of process variables resulting in more repeatable and uniform films, 3) generally better adhesion resulting from higher-energy metal atoms, 4) built-in material supply for continuous operation, and 5) the ability to deposit alloys. The data presented in this paper are the result of two separate studies. One study utilized a small "getter sputtering" enclosure (System A) and was concerned with the structure and properties of thin aluminum films up to about 1600A thick. In this thickness range, study of the film structure was possible with transmission electron microscopy. The second study was conducted with a conventional diode sputtering apparatus (System B) and covered $ much wider range of film thickness up to about 34,000A. Emphasis was placed on developing techniques which would extend aluminum sputtering to an existing in-line continuous deposition process.4 I) EQUIPMENT AND PROCEDURE System A. Fig. 1 shows a schematic of the "getter sputtering" inner chamber used and Fig. 2 is a photograph of this chamber mounted on an 18-in. access ring of a standard liquid-nitrogen trapped bell-jar vacuum system. This chamber was designed after a similar system used by Theuerer and auser.3 The configuration allowed the glow to emanate in all directions from the cathode. Argon (99.99') was allowed to enter only at the top of the chamber such that most of the reactive gases entering with the argon were reacted with the aluminum vapor and deposited on the chilled walls of the chamber before reaching the deposition zone. Provision was also made as shown, Fig. 1, for heating and cooling the substrate from about 20" to 400°C. Two substrate materials were used: Corning 7059 glass (12 by 12 by 0.048 in.) and carbon films about

Jan 1, 1967

By W. A. Roper

Since 1950, several papers have been published which have described various methods for studying mobility ratio effects. The methods which have been described for studying mobility ratio effects include X-ray shadowgraph techniques, stepwise potentiometric model procedures, stepwise numerical procedures, gelatin model studies and fluid mapper model studies. The purpose of this paper is to describe a procedure for using a resistance network for studying mobility effects. DESCRIPTION OF APPARATUS The basic unit of the experimental model consisted of a network of 840 resistors fastened to a sheet of black Lucite which was mounted on a wooden frame, Fig. 1. The dimensions of the Lucite sheet were 36 X 36 in. The resistors were fastened to the Lucite sheet at mesh points by means of snaps. The mesh points were arranged in a square pattern, 30 X 30 in., spaced at intervals of l1/2 in. The snap fasteners permitted several resistors to be "stacked" in parallel. By adding additional resistors to the basic unit, the specific resistance on each side of the flood front could be varied. The square network of resistors represented one of four symmetrical elements of a five-spot well pattern. The current input was analogous to an injection well and the current output was analogous to a production well." The power supply was essentially a full wave transformer-rectifier system for converting alternating-current into direct-current. The DC voltage could be varied from 41.43 to 290 v in steps of 41.43 v by selecting the proper outlet jacks. The major components of the power supply were: a Triro power transformer, R 11-A; a dual 5Y3 vacuum tube; two gas filled OD-3 tubes; and a Triplett voltmeter, model 227-1, range 0 to 500 DC v. The voltages at the mesh points were determined with a Keithley electrometer, model 210, No. 185, manufactured by Keithley Instruments, Cleveland, Ohio. A Heathkit vacuum tube volt-

By A. B. Wilder

We study the past Because it is a guide to the present and a promise for the future. The struggle for a better world is strengthened By the hopes, ambitions, and deeds Of those who were before us. As we look backward Our attention is directed forward. ONE hundred years ago, the manufacture of steel from molten pig iron without the use of fuel first began. In the earlier part of the nineteenth century the crucible process was the principal steelmaking method. It was a costly process, producing only a few pounds of steel at a time; so, most of the ferrous metal output was in the form of wrought or pig iron. With the perfection of the converter technique it became possible to produce low cost steel by the ton, thereby completely changing the structure, not only of the ferrous metal industry, but also of industrial production in general. This was the turning point from the Iron Age to the Age of Steel. William Kelly (Fig. 2), Sir Henry Bessemer (Fig. 1), and Joseph G. Martien experimented with the process before 1856. William Kelly began in Eddyville, Ky., in 1847 and has been given credit for first discovering the principle of the pneumatic converter process. Several years later in England Henry Bessemer independently conceived a steelmaking process similar to Kelly's. Bessemer made public his invention at the annual meeting of the British Association for the Advancement of Science held at Cheltenham, England, August 1856. As a result of his paper, "On the Manufacture of Malleable Iron and Steel Without Fuel," and his progressive leadership in the years to follow, the process became permanently identified with the name, Bessemer. Credit for the commercial adaptation of the process must be given two additional persons. Robert Mushet (Fig. 3) in 1856 in England recognized the necessity of deoxidation and recarburization of the converter product and evolved the technique for adding high manganese iron following the blow. In Sweden, in July 1858, G_ F. Göranson [ ]

Jan 1, 1961