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By W. G. Lidman, H. J. Hamjian

' I HE fabrication of many materials from powders involves a sintering process. A mass of powder will sinter because of the excess free energy over the same mass in the densified state caused by the higher total surface area of the powder. An understanding of the kinetics and mechanism of sintering should assist in improving the properties of such materials. The present investigation conducted at the NACA Lewis laboratory deals with the sintering of chromium carbide. Dry sintering (sintering at a temperature below the melting point) was divided into two stages by Shaler:' the first stage, during which the particles preserve much of their original shape and the voids are interconnected, and the second stage, during which densification occurs and the pores are isolated. The mechanism of forming interfaces between particles, or welding together of particles, has been investigated by Kuczynski2 and may be described by any one or a combination of the following mechanisms: viscous flow, evaporation and condensation, volume diffusion, or surface diffusion. The mechanism by which pores are closed or eliminated (densification) during sintering, is of interest. Grain growth observed during sintering may be attributed to the variation in the surface energies of individual grains, causing some grains to grow at the expense of others. Grain boundary migration occurs presumably by a diffusion process, therefore the rate of grain growth would be expected to increase exponentially with increasing time and temperature. Thus, for practical sintering times of less than 1 hr, a certain minimum temperature may exist at which major structural and property changes will occur. Densification and kinetics of grain growth during sintering under pressure of chromium carbide were investigated to provide additional information which will aid in describing more accurately the sintering process and the mechanisms involved. This material was selected for this study because of the current interest in high strength, oxidation resistant refractory materials, such as carbides, which are sintered to produce solid, dense materials from powders. Sintering under pressure is a process where the heat and pressure are applied to the compact simultaneously, specimens for this work were prepared by sintering under pressure at different temperatures and for various time periods. Experimental Procedure Preparation of Specimens: Chemical analysis of the commercial chromium carbide used in this investigation was as follows: Cr 86.19 pct, C 12.14 pct, and Fe 0.2 pct. X-ray diffraction powder patterns gave characteristic diffraction lines of Cr3C2 crystal structure. Powder particle size was determined microscopically and the average initial particle size was 6 microns with 85 pct between 2 and 10 microns. Specimens sintered under pressure were formed in graphite dies3 heated by induction. Sintering temperatures were measured with an optical pyrometer by sighting into a 3/8-in. hole drilled 1 in. deep at the midsection of the graphite die. A load of approximately 1 ton per sq in. was applied to the powder. The die assembly was heated in 20 min to the highest temperature (2500°F') at which no increase in grain size could be observed, and less than 2.5 min were required to heat from this temperature to the maximum temperature (3000°F). Sintering temperatures and times for the specimens of this investigation are indicated in Table I. Analysis of Specimens: Specimens polished with diamond abrasives were etched to reveal the grain boundaries with a 1:1 mixture of 20 pct potassium hydroxide and 20 pct potassium ferricyanide heated to 160°F. Representative areas of each sample were photographed at 1000 diameters. The largest diameters of all well-defined grains were measured, but only the measurements of 15 of the largest grains were averaged in order to determine an index of grain size on the assumption that they were among the first to begin growth. Densities were determined from differential weighing of the samples in air and water. The reported density values are considered correct within ±0.01 g per milliliter. Results and Discussion Metal compacts have exhibited grain growth when sintered at temperatures about two-thirds of the absolute temperature of their melting point.' Grain growth also occurs during the sintering of chromium carbide and is illustrated by the micrographs shown in Fig. 1. These micrographs were prepared from specimens sintered for 90 min at temperatures ranging from 1371°C (2500°F) to 1648°C (3000°F). Average grain size and density measurements of specimens investigated are presented in Table I. The relationship between grain size and sintering tem-

Jan 1, 1954

By Charles E. Lundin

The character of the Er-D system was established by determining pressure-temperature-composition relationships. A Sieuerts&apos; apparatus was employed to make measurements in the temperature range, 473" to 1223"K, the composition range of erbium to ErD3, and the pressure range of 10~s to 760 Torr. The system is characterized by three homogeneous phase regions: the nzetal-rich, the dideuteride, and the trideuteride phases. These phases and their solubility boundaries were deduced from the family of isotherms of the system zchich relate the pressure-temperature-composition variables. The equilibrium plateau decomposition relationships in the two-phase regions were determined from can&apos;t Hoff plots to be: The differential heats of reaction in these two regions are AH = - 53.0 * 0.2 and -20.0 *0.1 kcal per mole of D2, respecticely. The differential entropies of reaction are AS = - 36.3 * 0.2 and - 31.0 * 0.2 cal per mole D2. deg, respectively. Relative partial molal and intepal thermodynamic quantities were calculated from the pure metal to the dideuteride phase. The study of the Er-D system was undertaken as a logical complement to an earlier study of the Er-H system.&apos; The primary interest was to compare the characteristics of the two systems and relate the difference to the isotopic effect. Studies of rare earth-deuterium systems by other investigators have been very limited in number and scope. Furthermore, there is even less information available wherein an investigator has systematically compared a binary rare earth-hydrogen system with the corresponding rare earth-deuterium system. The available information consists primarily of dissociation pressure measurements in the plateau pressure region of a few rare earths. Warf and Korst&apos; determined dissociation pressure relationships for the La- and Ce-D systems in the plateau region and several isotherms for each system in the dideuteride region. They compared these data with those of the corresponding hydrided systems. The study of these systems as a whole was very cursory and did not give sufficient data for a thorough comparison of the effect of the hydrogen vs the deuterium in the respective rare earths. The heat capacities and related thermodynamic functions of the intermediate phases, YH, and YD2, were determined by Flotow, Osborne, and Otto,~ and the investigation was again repeated for YH3 and YD3 by Flotow, Osborne, Otto, and Abraham.4 This investigation studied only these specific phases. Jones, Southall, and Goodhead5 surveyed the hydrides and deu-terides of a series of rare earths for thermal stability including erbium. They experimentally determined isotherms of selected hydrides and plateau dissociation pressures for deuterides. These data allowed comparison of the enthalpy and entropies of formation of the dihydrides and dideuterides. To date, no one rare earth has been selected to thoroughly establish the complete pressure-temperature-composition (PTC) relationships of binary solute additions of hydrogen and deuterium, respectively. The objective in this investigation was to provide the first comparison of a complete family of isotherms of a rare earth-deuterium system with those of a rare earth-hydrogen system. This would allow one to determine what differences exist, if any, in the various phase boundaries and the thermodynamic relationships in various regions of the systems. I) EXPERIMENTAL PROCEDURE A Sieverts&apos; apparatus was employed to conduct the experimental measurements. Briefly, it consisted of a source of pure deuterium, a precision gas-measuring buret, a heated reaction chamber, a mercury manometer, and two McLeod gages (a CVC, GMl00A and a CVC, GM110). Pure deuterium was obtained by passing deuterium through a heated Pd-Ag thimble. A 100-ml precision gas buret graduated to 0.1-ml divisions was used to measure and admit deuterium to the reaction chamber. The reaction unit consisted of a quartz tube surrounded by a nichrome-wound furnace. The furnace temperature was controlled by a recorder-controller to . An independent measurement of the sample temperature in the quartz tube was made by means of a chromel-alumel thermocouple situated outside, but adjacent to, the quartz tube near the specimen. Pressure in the manometer range was measured to k0.5 Torr and in the McLeod range (10~4 to 10 Torr) to *3 pct. The deuterium compositions in erbium were calculated in terms of deuterium-to-erbium atomic ratio. These compositions were estimated to be *0.01 D/Er ratio. The erbium metal was obtained from the Lunex Co. in the form of sponge. The metal was nuclear grade with a purity of 99.9+ pct. The oxygen content was reported to be 340 ppm and the nitrogen not detectable. Metallographically the structure was almost free of second phase (<i vol pct). A quantity of sponge was arc-melted for use as charge material. The solid material was compared with the sponge in the PTC relationships. They were found to be identical. Therefore, sponge material was used henceforth, so that equilibrium could be attained more rapidly. The specimen size was about 0.2 gr for each loading of the reaction chamber. The procedure employed to obtain the PTC data was to develop experimentally a family of isothermal curves of composition vs pressure. First, a specimen

Jan 1, 1969

By J. R. Bell, W. J. Childs, J. H. Bucher, G. A. Wilber

A technique for determining recrystallization times as short as 0.10 sec was developed utilizing the "Gleeble", a commercially available testing system designed for the study of short-time, high-temperaLure themal and mechanical processes. The procedure consisted of heating a small tensile specimen to a given temperature of hot deformation, loading to a given reduction in area, unloading, delaying various intervals at temperature, and then reloading- to failure. The magnitude of the ultimate load obtained upon reloading decreased with delay lime as recrys-lallization proceeded. The technique was applied to austenite recrystallization in AISI 1010 and AISI 1010 uith 0.02 pct Cb steels. For each steel the reduction in area given the specimen on the first pull was mainlairred at 30 ± 5 pct and recrystallization times deterntined at various temperatures. The results indicaled a significantly slower rate of recrystallization for the columbium-modified composition, suggested the presence of- a recovery stage in the softening process , and indicated a greatly increased softening rate at a temperatuve where significant allotropic transformation to a partially ferritic Structure could occur. In recent years increasing attention has been paid to the fact that the process of recrystallization of austenite deformed at elevated temperatures is far from instantaneous at many practical hot-working temperatures.1-3 This realization has given rise to such terms as hot cold-working1 or warm-working,2 These terms generally describe processes where the recrystallization rate at the temperature of deformation is slow enough to have an appreciable effect on mechanical properties despite a relatively high deformation ternperature. The mechanical properties of interest can be either the properties at the deformation temperature as in hot-workability studies4 or the room-temperature properties after cooling as in the many recent studies of various thermomechanical processes172 where heat treatment and deformation are intentionally combined to give a unique set of room-temperature properties. Because of this interest in processes where the austenite recrystallization kinetics can be an important variable, the development of quantitative methods of following the course of short-time, high-temperature recrystallization has received increasing attention.l,3,5 The experimental methods to date have, in general, relied upon rapidly deforming the austenite, holding at temperature for various brief intervals, quenching as G.A.WILBER and W. J. CHILDS, Members AIME,are Research-Fellow and Professor, respectively, Rensselaer Polytechnic Institute, Troy, N. Y. J. R. BELL and J. H. BUCHER, Member AIME, are Research Engineer and Research Supervisor, respectively, Graham Research Laboratory, Jones & Laughlin Steel Co., Pittsburgh, Pa. Manuscript submitted March 13, 1968. IMD. rapidly as possible, and then using room-temperature measurements to follow the recrystallization process. Although such methods can be successfully applied to certain alloy steels, the existence of the allotropic transformation during cooling of plain-carbon or low-alloy steels tends to obscure the results. Thus, such room-temperature measurements as hardness and X-ray line widths do not correlate well with the extent of austenite recrystallization before quenching,5 and results based on room-temperature microstruc-tural observations are dependent upon the success in correlating the observed structure with the prior aus-tenitic grain structure.1,3,5 The purpose of the present work was to develop a quantitative method for the determination of short-time, high-temperature recrystallization rates, based on measurements made at the temperature of deformation. EXPERIMENTAL TECHNIQUE The basic technique consisted of heating a small tensile specimen to a given temperature of hot deformation, loading to a given reduction in area, unloading, delaying various intervals at temperature, and then reloading to failure. The data were obtained in the form of traces of load and elongation as a function of time. Due to the high deformation temperature, the strain hardening introduced during initial loading was progressively annealed out with holding time after unloading and the loads obtained upon reloading decreased as this softening proceeded. Although the value of the second load at any Consistent point On the load-elongation curve could have been used as a measure of the degree of softening, the most convenient to use was the ultimate load. The softening indicated by the decrease in the second ultimate load with time is essentially a process of annealing of cold-worked material at a high deformation temperature. Although some recovery grain growth may contribute to such a softening process, it is generally considered that the major softening which must take place to achieve complete removal of substantial Strain hardening will occur by the formation of new, stress-free grains. As the results of this work indicate that essentially complete removal of strain hardening did in fact occur. the primary softening process will be attributed to recrystallization, and specific reference made where it appears that other mechanisms may be contributing to the total observed softening. It would, of course, be of interest to attempt to correlate the results of this work with the actual austenite fraction recrystallized as determined by other techniques. This was not attempted in the present work because it would have required running a large number of additional specimens and, as discussed previously, there is limited assurance that the results would accurately reflect the prior austenite fraction recrys-

Jan 1, 1969

By Charles E. Lundin

Pressure-temperature-composition data were obtainedfor the Er-H system. Measurements werecar-ried out in the temperature range of 473° to 1223°K, the composition range of erbium to ErH,, and the pressure range of 10-5 to 760 Torr. Solubility relationships were established from these data throughout the system. Three solid-solution phases were delineated: metal solid solution, dihydride phase, and trihydride phase. The trihydride Phase decomposes at about 656°K and 1 atm pressure. The dihydride phase is stable to about 1023°K, but becomes more deficient in hydrogen above this temperature. The equilibrium decomposition pressure-temperature relationships in the two-phase regions, erbium solid solution plus dihydride and dihydride plus trihydride, were deter- The differential heats of reaction in these two regions are AH = - 52.6 * 0.3 and - 19.8 i 0.2 kcal per mole of Hz, respectively. The differential entropies of reaction are AS = - 35.2 * 0.3 and - 30.1 * 0.4 cal per mole HZ.deg, respectively. Relative partial molal and integral thermodynamic quuntities were calculated in the system to the dihydride phase. RARE earth metal-hydrogen systems have been the subject of general survey,1"4 and all have been found to form hydride phases. The heavy rare earths, of which erbium is a member, form dihydride and trihydride phases with different crystal structures, whereas the light rare earths form only a single-phase dihydride which expands without structure change, as hydrogen is added, to the trihydride composition. These materials are of interest primarily because of their theoretical properties, such as bonding, defect structure, and thermodynamic and electronic characteristics. Erbium has been studied in several previous investigations.5, 6 It was deemed desirable to more thoroughly and accurately define the system, both for the phase equilibria and the thermodynamic properties. I) EXPERIMENTAL PROCEDURE A Sieverts&apos; apparatus was employed to conduct the experimental measurements. Briefly, it consisted of a source of pure hydrogen, a precision gas-measuring buret, a heated reaction chamber, a mercury manometer, and two McLeod gages (a CVC, GM 100A and CVC, GM 110). Pure hydrogen was obtained by passing hydrogen through a heated Pd-Ag thimble. The hydrogen was analyzed and found to have only a trace of oxygen and nitrogen. A 100-ml precision gas buret graduated to 0.1-ml divisions was used to measure and admit hydrogen to the reaction chamber. The reaction unit consisted of a quartz tube surrounded by a nichrome-wound furnace. The furnace temperature was controlled by a recorder-controller to ±1°K. An independent measurement of the sample temperature in the quartz tube was made by means of a chromel-alumel thermocouple situated outside, but adjacent to, the quartz tube near the specimen. Pressure in the manometer range was measured to ±0.5 Torr and in the McLeod range (10-4 to 10 Torr) to ±3 pct. The hydrogen compositions in erbium were calculated in terms of hydrogen-to-erbium atomic ratio. These compositions were estimated to be ±0.01 H/Er. The erbium metal was obtained from the Lunex Co. in the form of sponge. The metal was nuclear grade with a purity of 99.9 pct +. The oxygen content was reported to be 340 ppm and the nitrogen not detectable. Metallographically the structure was almost free of second phase (<1 vol pct). A quantity of sponge was arc-melted for use as charge material. The solid material was compared with the sponge in the pressure-temperature-composition relationships. They were found to be identical. Therefore, sponge material was used henceforth, so that equilibrium could be attained more rapidly. The specimen size was about 0.2 grain for each loading of the reaction chamber. The procedure employed to obtain the pressure-temperature-composition data was to develop experimentally a family of isothermal curves of composition vs pressure. First, a specimen of erbium was wrapped in a tungsten foil capsule to prevent contact with the quartz tube. After loading the specimen, the system was evacuated to less than l0-6 Torr, flushed several times with high-purity hydrogen, and evacuated again ready for the start of the experiment. The furnace was then brought to the desired temperature. A measured amount of hydrogen was admitted into the chamber. Equilibrium was allowed to be attained, the pressure read, and the process then repeated many times until 1 atm of gas pressure was finally reached. Other isotherms were then developed in the same manner. The partial pressure plateaus were determined by another manner. In the solid solution-dihydride region a composition of approximately 1.0 H/Er was selected on the plateau. The temperature was varied throughout the range of interest. At each temperature level, equilibrium was achieved, the pressure read, and the next temperature attained. The temperature was cycled both up and down. In the dihydride-trihy-dride region, the plateaus were determined in the 473" to 651°K range only by heating to the desired temperature and not by both heating and cooling. The data were much more reproducible in this manner. Equilibrium required long periods of time. Specimens were initially hydrided to 2.8 H/Er, so that at the higher

Jan 1, 1969

By Jean Howard

ThE formation of the (100) [001) texture in 3-1/4 pct Si-Fe strip was first reported by Assmus ef a1.l in 1957. Since then much experimental work has been carried out with a view to establishing the mechanism involved. The papers cited above state that the (100) [001] texture was developed in strip rolled from material melted and cast in vacuum. (The impurity content of the ingot is reported as 0.005 pct.) The present note records that similar results can be obtained in material processed by powder metallurgy. A processing schedule is described.which enables the texture to be formed in strip up to 0.010 in. thick, but there seems no reason why this should not be achieved in thicker strip, provided that large grains are developed after sintering. The materials were prepared from Carbonyl Iron Powder Grade MCP (particle size 5 to 30 p) of the International Nickel Co. (Mond) Ltd. The powder contains about 0.15 pct 0, 0.01 pct C, 0.004 pct N, <0.002 pct S, $0.005 pct Mg and Si, and 0.4 pct Ni— that is, it is substantially free from metallic impurities other than nickel, which is thought to be unimportant in the present work. The silicon powder was 99.9 pct purity, or material of transistor quality (ground in pestle and mortar). The mixed powders (3-1/4 pct Si to 96-3/4 pct Fe) are heated in hydrogen at 350" and 650°C to deoxidize the iron before sintering loose at temperatures between 1350" and 1460°C (depending upon the ultimate thickness of strip required) for up to 24 hr. The object of the high-temperature sinter is to develop a large grain size at this stage. Alternatively, the loose sintering can be done at a lower temperature followed by rolling or pressing and then annealing at temperatures between 1350" and 1460°C. Both methods produce large grains, which remain large throughout the process. The compact is then hot-rolled to approximately 1/8 in. with high-temperature interstage anneals if necessary. This step is taken to avoid intercrystalline cracking which would occur if the material of such large grain size were cold-worked. The bar is then annealed at 1050°C and reduced to its final thickness by approximately 50-pct reductions and 1050°C interstage anneals. Throughout the process the dew point of the hydrogen furnace atmosphere is maintained at about -40°C. Samples were annealed in hydrogen at various temperatures and times. Secondary recrystalliza-tion to (100) [001] was developed on the thinner material (i.e., up to 0.002 in.) by annealing in hydrogen at 1050" to 1200°C with a dew point of - 40°C or in vacuum (10-5 Torr) at 1050°C. With the thicker materials (i.e., up to 0.010 in.) the best results were obtained by annealing in hydrogen at 1200°C with a dew point of - 55°C. Complete secondary recrystal-lization to (100) [001] textures was obtained. Above these temperatures secondary recrystallization to (110) [001] tended to develop. The final annealing of samples was normally carried out with the samples placed between recrystal-lized alumina plates, but some experiments were performed with the samples suspended so that their surfaces were not in contact with anything except hydrogen, and these were equally successful in developing secondary crystals. An approximate determination of the proportion of material (before secondary recrystallization took place) having crystals with the (100) or (110) planes in or near the rolling plane showed that 11 pct of the sample had (100) and 16 pct (110). The method used for the determination is described below. A sample was annealed at a temperature just below the secondary recrystallization temperature and etched to reveal the (100) planes. The approximate area covered by crystals having (100) or (110) in or very near the surface was measured on the screen of a Vickers projection microscope. This was repeated for twenty positions chosen at random and a mean of the results calculated. The main hindrance to developing the secondary crystals in the thicker materials was the difficulty of obtaining a large enough initial primary grain size before secondary recrystallization. This was overcome by increasing the particle size of the silicon powder used. During the course of the work, it had been observed that the larger the grain size after sintering the more likely it was that the material would be successful in developing secondary crystals at a later stage. An experiment was therefore carried out to determine whether the material with the larger grain was more successful in developing secondary crystals due to the large grain produced at the sintering state per se or whether it was due to the greater reduction of silica brought about when the sintering temperature was raised in order to increase the grain size. A comparison was made between two compacts, one of which was made with silicon powder of 60 to 100 mesh, the other with silicon powder which was finer than 200 mesh. F?r this experiment, use was made of a phenomenon previously observed that the larger the particle size of the silicon powder employed in making a compact, the larger is the grain size of the compact. The silicon powder was ground

Jan 1, 1964

By A. A. Collins

When we speak of high copper on a lead blast furnace we think in terms of 4 to 5 pct, or. any lead charge carrying over 1 pct. Any copper on charge will produce its corresponding troubles such as lead well, extra slag losses, drossing problems, and the working up of the dross. This is indeed a very interesting subject and one that used to give the old-time lead metallurgists such as Eiler, Hahn and lles many worries, not so much in the actual operation of the hlast furnace but in the working up of the copper. When the American nletallurgists commenced with the American rectangular-shaped lead blast furnace in the 1870&apos;s and got away from the reverberatories such as were in use in Germany and other parts of the world, they went to greater tonnages, as 80 to 100 tons per day in comparison to the 20 to 30 tons per day in the other processes. With the greater tonnages along with insuficient settling capacity, the silver losses in some cases were increased. Hence the lead-fall was low, for there were no leady concentrates in those days to assist the metallurgist to gain lead or an absorber for the precious metals; and in some cases copper sulphides were added intentionally to the charge to produce a copper matte to lessen the silver losses through the dump slag. The operators in those days thought that where some copper was always present in the lead ores the copper should not enter into the reduced lead and alloy with it. This, by the way, is just the reverse of our present-day practice, when we try to put all of the copper into the blast furnace lead and to remove the same through the drossing kettles. Therefore the furnace was operated to produce a certain amount of matte or artificial sulphides, since, due to the great affinity of copper for sulphur, any copper present would enter the matte almost completely. Thus, the lead bullion produced was practically free from copper. The products of the furnace were metallic lead or lead bullion, containing 05 to 95 pct of the lead and about 96 pct of the silver which were in the ore—a lead-copper-iron matte which contained nearly all the copper in the ore and the slag, the waste product. In the United States, up through the year 1092, we find the small furnace 100 X 32 1/2 in. with 12 tuyeres, some 6 on each side, plagued with a small amount of poorly roasted sulphides— either from heap or hand roasters that produced matte. This matte was roasted and if poor in copper was returned for the ore smelting. Otherwise it was smelted either alone or with additions of rich slags or argentiferous copper ores, the products being lead and a highly cupriferous matte, the latter being subsequently worked up for its copper. The lead metallurgists kept trying and improving on furnace and roasting equipment designs until we find blalvin W. Iles constructing at the old Globe Plant at Denver what came to be the modern furnace. That is, in 1900 he built a furnace of 42 in. width by 140 in. at the tuyeres with a 10 in. bosh and a 16-ft ore column. This type has been more or less standard to the present time, though modified in width and length to meet the demand for large tonnages and improvements in structural details. In 1905 at Cananea, Mexico, Dwight and Lloyd developed the present down-draft sinter machine that has meant so much in producing a well-processed material for the lead blast furnace. In 1912 Guy C. Riddell came forth with double roasting at the East Helena Plant of the American Smelting and Refining Co., which removed the "zinc mush plague." Incidentally, with the introduction of double roasting, which most lead plants were forced into after 1924, when lead flotation came into its own, less matte or no matte was produced. When this stage arrived, the copper was forced into the dross and the casting of lead at the blast furnace lead-wells was stopped. In plants with a fair copper carry 1 pct or better on the blast furnace charge, the lead wells became inoperative once the production of matte stopped. The copper drosses clogged the lead wells and even with bombing, either water or dynamite, the operators could not keep them open. Thus, the lead wells were abandoned in some plants, such as at the El Paso and Chihuahua smelters of the American Smelting and Refinillg Co., and all lead taken out through the first settlers. The elimination of sulphur, espccially sulphide sulphur, from the blast furnace charge and the nonproductiori of matte resulted in a great saving of tinie, energy and equipment in the recirculation of the copper, With the copper content in the dross and dross-fall ranging in quantities from a few percent up to 60 pct, such as at El Paso, a drossing problem was created. As the old-time operators hated dross and buried the same in the shipping bullion, the modern metallurgists from 1925 on decided that with increasing dross-falls they would have to adopt the lead refiner&apos;s ideas of drossing kettles with subsequent treatment of the lead with a sulphur addition to have the shipping lead of 0.01

Jan 1, 1950

By Warren D. MacEvoy

INTRODUCTION Good ventilation bulkheads (stoppings) can be obtained only by conscientiously adhering to four basic principles: carefully selecting the site for the bulkhead, adequately preparing the site, properly constructing and sealing the bulkhead, and checking the results with a smoke tube before leaving the area. If all these guidelines are followed during each ventilation project, a poor job will result only from the use of improper materials and cannot be blamed on carelessness or oversight. SITE SELECTION A perfectly constructed bulkhead in the wrong location can be completely worthless. Conceivably, a bulk-head in the wrong location could cause dangerous ventilation conditions that are difficult to identify and isolate. If the suggestions herein are followed, a considerable amount of work, time, and material may be saved. Perhaps the single most important step is always to select the exact site for a bulkhead before starting construction. Although the latitude in selecting a site may be limited by instructions or operating conditions, it is common to find poor bulkheads built within a few meters (feet) of a site that would have been far superior but was overlooked during the planning process. The ideal site for a bulkhead should have as many of the following features and conditions as possible: 1) To provide a solid bulkhead, the selected site should be in firm and unbroken ground. 2) To minimize the amount of work and material required and to minimize the danger of later damage to the bulkhead, the site should have as small a cross section as possible. 3) The bulkhead site should not be encumbered by interferences such as pipes, wires, ditches, wire roof supports, trash, muck piles, etc. 4) The walls and timbers of the site should be free from oil, grease, or tar that would inhibit adhesion of the sealant used on the bulkhead. 5) Unless special precautions are taken, the site should not have water seepage, standing water on the floor, or water-carrying ditches. 6) To expedite construction of the bulkhead, the site should have reasonable access to transportation, supplies, communication facilities, and compressed-air lines. 7) The site should have a reasonably level floor, allowing direction of the bulkhead door swing to be reversed at a later time if so desired. In a steeply sloping location, it may be possible to open the door in one direction only. SITE PREPARATION Once a suitable site has been selected for the bulk¬head, it must be prepared properly. All site preparation work should be completed before starting any construction work on the stopping itself. Unfavorable site conditions can be identified during the course of thepreliminary site preparation, saving time, effort, and materials that otherwise might be wasted. The follow¬ing preparation steps help assure the construction of a good stopping: 1) If wire mesh has been used at the site, a strip 457 mm (18 in.) wide should be cut and removed from the walls and roof at the selected location. 2) The exposed strip of rock should be barred down thoroughly to provide a smooth surface. 3) All obstructing materials should be removed, including old timbers, pipes, rockbolts, wires, etc. If a conduit must cross the bulkhead area, it should be located or relocated away from the floor, walls, and roof to allow a 6.28-rad (360°) seal around the juncture between the conduit and the bulkhead structure. 4) All loose muck should be cleaned from the site and a trench about 152 mm (6 in.) deep should be dug from wall to wall in the floor. The trench must be wide enough to accommodate the entire bulkhead, including the posts. 5) The rock surfaces of the walls and roof should be cleaned with a wire brush to remove as much loose surface material as possible. Thorough cleaning promotes adhesion of the bulkhead sealant to the surfaces of the walls and roof, thus promoting an airtight seal. 6) It is quite difficult to seal landing mats that cross a bulkhead. If such a crossing cannot be avoided, the bulkhead should be placed between the end and the first hole in the steel so at least one side of the bulk-head can be sealed easily and completely. That may have to be done prior to actual construction if the end is located on the opposite face from the seal coating of the bulkhead. BULKHEAD CONSTRUCTION The three principal considerations in bulkhead con¬struction are the type of bulkhead, materials to be used, and construction method to be employed. For many projects, the bulkheads are specified by the requesting agency, with no latitude for independent choice of the type, materials, or construction method. In such cases, any deviations from the specifications, for any reason, must be approved in advance by the proper department or by the project senior ventilation engineer. Types and Materials When a choice of type, materials, or method is allowed, consideration should be given to factors such as cost, required useful life, proximity to blasting concus¬sions, availability of materials, direction of permissible air leakage, and degree of airtightness required. Other factors to be considered include the amount of time available, accessibility of transportation, potential for interference with operations or production, ambient water conditions, availability of connections to com¬pressed-air lines, etc. Despite the multitude of factors to be considered, most stoppings can be analyzed easily and the proper choices can be made without much difficulty. The four common classes of bulkheads utilized in

Jan 1, 1982

By J. B. Hess, C. S. Barrett

TO reach equilibrium between different phases in cobalt-rich alloys requires prohibitively long annealing cobalt-richalloystimes when temperatures are below about 700°C. The fact that a transformation from face-centered cubic to close-packed hexagonal readily tered takes place at temperatures below this in the cobalt-rich solid solutions is not an indication that thermally activated processes occur at an appreciable rate, for the transformation is well established as martensitic in nature. Wide divergence between heating and cooling experiments and high sensitivity to prior heat treatment make it difficult to judge temperatures of equilibrium between the phases.&apos; One object of the present work was to see if the information object of on the relative stability of phases could be gained by substituting plastic deformation for thermal agitation. Procedures were worked out that led to the determination of a diffusionless type of phase diagram, which represents the temperature of of phase equal stability for phases of the same composition, and the technique was applied to the Co-Ni system. Another object of the work was to see whether or not deformation would generate frequent stacking faults when these were thin lamellae of quentstackingfaultsa phase having higher free energy than the parent phase. The alloys were prepared in 80 to 100 g melts from cobalt (with metallic impurities estimated spectrochemically as follows: Ni, 0.05 pct; Fe, 0.001 pct.; Mg, Si, Cu, Cr, Al, < 0.001 pct) and Mond Car-bony1 nickel (with Fe, 0.05 pct; Si, 0.003 pct; C, 0.61 pct.; Cu, 0.001 pct; Co, Cr not detected, < 0.01 pct). The metals were melted in pure Al2O3 crucibles. An atmosphere of argon, that had been purified by passing over hot magnesium chips, was used for the alloys that, by analysis of the portions of the ingots actually used, were found to contain 15.3, 25.7, and 35.0 pct Ni, and vacuum melting (after degassing) was used for those containing 29.4 and 31.5 pct Ni. After induction melting the alloys were allowed to solidify in the crucible, and slices % in. thick x ½ in. in diam were annealed 12 hr at 1350°C for homogenization. These same specimens were used throughout the series of experiments, with annealing treatments of 4 hr at 900°C in purified hydrogen followed by furnace cooling, alternating with the deformation and X-ray tests discussed below. Results Spontaneous transformation was observed on cooling to room temperature in all alloys containing 29.4 pct Ni or less and by cooling the 31.5 pct alloy to — 195°C but was not observed in the 35 pct alloys after cooling to —195°C. These results are in satisfactory agreement with the cooling experiments of Masimoto.4 From these data it is clear that the temperature of beginning transformation M,,, drops to 20°C with the addition of about 30 pct Ni. The test for spontaneous transformation was metallographic. Specimens were thermally polished by annealing 10 hr in hydrogen at 1350°C, then furnace cooled; if trans- formation had occurred there were relief effects visible on the thermally polished surfaces. These markings were narrow straight lines, usually resolvable at high magnification as clusters of fine lines that resembled slip lines. It was concluded that they resulted from displacements on (111) planes, for the number of directions in individual grains often reached but never exceeded four, and lines could always be found parallel to the thermally etched (111) boundaries of annealing twins. The markings were thus consistent with the idea that the transformation occurs by (111) plane displacements (Shockley partial dislocations moving on (111) planes). This was further confirmed by X-ray tests for stacking disorders. Using an oscillating crystal technique previously employed to detect strain-induced faulting in Cu-Si alloys," streaks indicative of the stacking faults were looked for and found on X-ray films of the spontaneously transformed 25.7 pct Ni alloys, as expected by analogy with Edwards and Lipson&apos;s results on pure cobalt." The streaks were much intensified after rolling at room temperature. Transformation induced by plastic strain was investigated as a function of alloy composition and temperature of deformation. A series of tests was made to determine suitable straining and X-raying techniques. Filing was found inferior to abrasion in converting cubic samples to hexagonal, and abrasion was less effective than peening in producing smooth unspotty Debye rings in the X-ray patterns. Because the diffraction lines were broad, Geiger-counter spectrometer records of filings were less sensitive in revealing small amounts of transformed material than X-ray patterns recorded on films in a small diameter camera. After these exploratory tests the following methods were adopted. Specimens that had been annealed at least 4 hr at 900°C and furnace cooled were mounted in a block of aluminum, brought to temperature, and peened thoroughly with a mullite pestle preheated to the same temperature. The specimens were then quenched to room temperature. In peening, a circular area of % in. diam was given 500 blows. A few control tests showed that an additional 1000 blows did not detectably change the proportions of the phases present. The amount of transformation was judged by X-ray reflection patterns from the peened surface, using the innermost four lines of the cubic and the hexagonal patterns with filtered CoKa radiation,

Jan 1, 1953

By P. A. Laxen, H. R. Spedden, A. M. Gaudin

WHEN a mineral particle is fractured, bonds between the atoms are broken. The unsatisfied forces that appear at the newly formed surface1 are considered to be responsible for the adsorption of ions at the mineral surface. A knowledge of the mechanism and extent of ion sorption from solution onto a mineral surface is of interest in the development of the theory of flotation.2,3 Study of the adsorption of sodium from an aqueous solution on quartz offers a simple approach to this complicated problem. The availability of a radioisotope as a tracer element meant that accurate data could be obtained.4,5 Three main factors which appeared likely to affect the adsorption of sodium are: 1-concentration of sodium in the solution, 2-concentration of other cations in the solution, and 3-anions present in the solution. Hydrogen and hydroxyl ions are always present in an aqueous solution. By controlling the pH, the concentration of these two ions was kept constant. The variation in the amount of sodium adsorbed with variation in sodium concentration was then determined under conditions standardized in regard to hydrogen ion. The effect of concentration of hydrogen ions and of other cations was also measured. A few experiments were made to get a preliminary idea on the effect of anions. The active isotope of sodium was available as sodium nitrate. Standard sodium nitrate solutions were used throughout these experiments except when the effects of other anions were studied. It was found that sodium adsorption increased with sodium-ion concentration, but less rapidly than in proportion to it. Increasing hydrogen-ion concentration, or conversely decreasing hydroxylion, brings about a comparatively slight decrease in sodium-ion adsorption. Increasing the concentration of cations other than hydrogen or sodium decreases somewhat the adsorption of sodium ion. It would appear as if the kind of anion is a secondary factor in guiding the amount of sodium ion that is adsorbed. Materials and Methods Quartz The quartz was prepared as in previous work in the Robert H. Richards Mineral Engineering Laboratory4 except for the refinement of using de-ionized distilled water for the final washing of the sized quartz, prior to drying5 To minimize the laborious preparation of quartz, experiments were made to determine whether the sodium-covered quartz could be washed free of sodium and re-used. The experiments were successful as indicated by lack of Na&apos; activity on the repurified material and by its characteristic sodium adsorption. Table I gives the spectrographic analyses of the quartz used. The quartz ranged from 16 to 40 microns in size, averaging about 23 microns (microscope measurement), and had a surface of 1850 sq cm per g (lot I), 2210 (lot II) and 2000 (lot III) as determined by the Bloecher method.6 Radioactive Sodium Method of Beta Counting for Adsorbed Sodium: Na22, the radioisotope of sodium, possesses convenient properties.7 It has a half-life of 3 years, thus requiring no allowance for decay during an experiment. On decay it emits a 0.575 mev ß radiation and a 1.30 mev ? radiation. The decay scheme is illustrated in the following equation: [Y Nam S. - &apos;Net 3 years] The ß radiation is sufficiently strong to penetrate an end-window type of Geiger-Mueller counting tube. This, in turn, makes it possible to use external counting, a great advantage in technique. Furthermore, it permits the assaying of solids arranged in infinite thickness, while assaying evaporated liquors on standardized planchets. The equipment used was standard and similar to that employed by Chang8 The original active material was 1 ml of solution containing 1 millicurie of Na22 as nitrate. This active solution was diluted to 1000 ml. Five milliliters of this diluted active solution was found to give a quartz sample a sufficiently high activity for accurate evaluation of the sodium partition in the adsorption measurements. Also, 1 ml of final solution gave a sufficiently high count for precision on the liquor analyses. The sodium concentration of the diluted active solution was 1.2 mg per liter, so that 6 mg of sodium for 60 ml of test solution and 12 g of quartz was the minimum amount used. The active solution was stored in a Saftepak bottle. Procedure for Adsorption Tests: The method consisted of agitating 12 g of quartz with 60 ml of solution of known sodium concentration for enough time to establish equilibrium between the solution and the quartz surface. The quartz was separated as completely as possible from the solution by filtering and centrifuging. The activity on the quartz and in the equilibrium solution was measured and the partition of the sodium was calculated from the resulting data. The detailed procedure for the adsorption test is set forth in a thesis by Laxen5 In brief, it included the following steps: 1-Ascertainment of linearity between concentration of Na22 and activity measured. 2-Evaluation of factor to translate activity on solid of infinite thickness in terms of activity on an evaporated active film of minute thickness, on the various shelves of the counter shield. 3-Taking precautions to avoid evaporation of water during centrifuging.

Jan 1, 1952

By G. L. Schroeder, C. H. Summers, D. B. Lindsay

INTRODUCTION The requirement that is placed on owners and operators of underground mines to protect workers against the health hazard of inhaling radioactive materials which are short-lived decay products of 222Rn can be satisfied by applying a considerable variety of what we may call "engineering" solutions as well as a number of "administrative" remedies to the problem. The most obvious of the "engineering" approaches has always been that of forced ventilation, in which relatively clean (i.e., radon-free) air from aboveground is drawn or pushed through the mine workings by a system of fans and ducts. This relatively clean air, in sweeping through the drifts, stopes and haulageways, dilutes the radon and radon-daughter concentrations in the air of the mine, and performs the added beneficial function of removing the daughter-mixture quickly enought to limit grow-in of the longer-lived nuclides in the group that make up the "toxic trio" on which the Working Level (IM) unit is based. Effective as the dilution-ventilation method is for control of WL in most underground mining situations, however, the increasing strictness of control measures that have been imposed on the mining industry over the last two decades have demanded measures of even greater effectiveness. In times of poor markets for yellow-cake and other products of the mines, mine operators are pressed to reduce operating costs, and the installation of additional primary ventilation capacity can be a severe burden on a mine that is already laboring under an unfavorable earning power. When traditional dilution-ventilation systems alone cannot meet the requirement for WI, control, radiation safety engineers and ventilation engineers begin to look at alternatives and auxiliary methods. Since the radon which produces the toxic daughter products originates in the rock of the mine walls, and since, in most United States mines, that rock is a porous sandstone through which air can move under the effect of atmospheric pressure gradients, and through which radon can diffuse relatively freely, one way to help control the growth of WL would be to hinder the escape of radon from that reservior of porous rock. An appealing; method for hindering that natural flux of radon-polluted air from the walls of the mine has long been apparent; namely, to apply a low-permeability coating over the surface of the rock, thus sealing the radon in place and, in theory at least, preventing its escape into the mine air. Our 1970 report to the U.S. Federal Radiation Council on the subject of cost impacts of proposed changes in the occupational standards for exposure of underground uranium miners to airborne radon daughters noted the possibility of using polymeric wall sealants as a means of controlling radon-pollution of mine air. Since that time a number of reports have appeared in the technical literature advocating this technique for restraining the escape of radon from building materials, mill tailings, and other materials containing 226Ra, in addition to the surfaces of underground mine workings. During this period, some controversy has occurred over the question of the probable effectiveness of wall sealants in limiting the escape of radon from the rock. Our 1970 report speculated that flaws (cracks and "pinholes") in the coating might be all but unavoidable in practice, and that even a conservative estimate of the frequency of such flaws would lead to a prediction of ineffectiveness. Hammon et al, in a laboratory evaluation of radon sealants conducted by Lawrence Livermore Laboratory of the University of California in 1975 on behalf of U.S. Bureau of Mines, concluded that a wide variety of polymeric coatings would provide "nearly 100% effectiveness" in restrain¬ing escape of radon from mine wall surfaces if applied in "thicknesses between 5 and 10 mil" (125-250 [y]pm). John Franklin and co-workers at the U.S. Bureau of Mines laboratories in Spokane, Washington, have carried the experiments with polymeric sealants through additional laboratory tests and into actual mine environments, reporting that selected sealants could provide attenuation of radon flux by a factor of four (75-80% reduction). Robert Bates and John Edwards of USBM developed a computer-assisted mathematical/physical model that predicts a relatively small effect of flaws in a low-permeability coating on the radon flux from a sandstone-type matrix. FIELD TEST Since all actual experimental work with wall sealants showed some beneficial effect on radon attenuation (even if not as exciting as the "nearly 100%" predicted by Hammon), USBM was encouraged to extend its evaluation to an actual operating uranium mine, and awarded a contract for that work to Arthur D. Little, Inc. in September 1979. We were fortunate in obtaining the voluntary cooperation of Atlas Minerals Division of Atlas Corp., who operate a mill and several underground mines in and around Moab, Utah. Atlas made available for our use a small T-shaped drift in their Pandora Mine in LaSal, Utah, and provided space for instrumentation and recordkeeping by our field crew in a surface building near the mine entry. Atlas also provided electricity and water to the test site, together with assistance in establishing necessary ventilation, removing rubble from the site, conducting periodic WL surveys and furnishing auxiliary man-power for the heavy hard work of coating the walls with gunite prior to application of the polymeric sealant. The generous coopera-

Jan 1, 1981

The Annual General Meeting of the Institute was held in Kelvin House, Johannesburg, on Wednesday, 26th August, 1970, at 4.15 p.m. Mr. J. K. E. Douglas (President) was in the Chair. There were also present sixty-three Fellows, thirty-five Members, one Graduate, eight Associates, five Students and nineteen Visitors, making a total of one hundred and thirty-two. The President declared the meeting open at 4.20 p.m. OBITUARIES The President: &apos;It is my sad duty to announce the deaths of the following members of the Institute. Dr J. A. Papenfus, Fellow, who joined the Institute in 1942 and passed away on the 28th of May, 1970. Mr D. G. Beadle, Fellow, who joined the Institute in 1946 and passed away on the 17th of June, 1970. Gentlemen, Derek Beadle was very well known in this Institute. His papers on dust will be remembered and, at the time of his untimely death, he was one of our assistant editors. As a mark of respect to the memory of the deceased and in sympathy with the bereaved, I would ask you to rise and observe a few moments&apos; silence.&apos; MINUTES The President: &apos;May we confirm the minutes of the General Meeting held on 15th April, 1970, as published in the July, 1970, issue of the Journal&apos;. Agreed. WELCOME TO VISITORS The President: &apos;Ladies and Gentlemen, we are honoured this afternoon by the presence of many distinguished guests and I extend to you all a most cordial welcome. We are happy to have with us Dr A. A. von Maltitz, President of the Chamber of Mines of South Africa, who is also Honorary President of this Institute. We also have one of our Honorary Vice- Presidents, Mr T. L. Gibbs, the Government Mining Engineer; Mr D. E. Hamm, President, Institution of Certificated Mechanical and Electrical Engineers, S.A.; Mr S. C. M. Naude, Director, Witwatersrand Technical College; Mr I. R. G. Stephen, Senior Vice-President, The S.A. Institute of Electrical Engineers; Mr G. M. Tompkins, President, The S.A. Institution of Mechanical Engineers; Professor P. B. Ackermann, President of the Geological Society of S.A.; Mr A. S. Robinson, Vice-President of the S.A. Institute of Civil Engineers; Professor W. Mare, President of the Institute of Land Surveyors of the Transvaal; Mr B. D. Charlton, President of the S.A. Institute of Assayers and Analysts; Mr R. Hemp, The President, The Mine Ventilation Society of S.A.; Mr L. J. Prince, The President, The S.A. Association of Mine Managers; Mr J. Botha, The President, The S.A. Institute of Foundrymen; Mr G. Niterl, The President, The Institute of Welding; Mr M. R. Gericke, President, S.A. Council of Professional Engineers; Mr N. A. Honnet, Chairman, Orange Free State Branch; Mr P. R. C. Cooke, Chairman. The South African Chemical Institute (S. Tvl&apos; Section). Gentlemen, we are very honoured indeed, to have these distinguished gentlemen with us this afternoon, as our honoured guests. We are also pleased to have with us, one of our Honorary Fellows, Mr F. G. Hill, and several Past-Presidents. I also extend a very warm welcome to all our lady guests and to all our other visitors.&apos; MEMBERSHIP The President: &apos;I have pleasure in announcing that the names of the following candidates, having been published in accordance with By-Law 5.2.2, Council has elected them to membership in the following grades: NEW APPLICATIONS Fellows: Herbert Dalton-Brown, Stephen William Morel. Members: Clive Lester Workman-Davies, Basil James Russell Botha. Students: Timothy Nigel Watson, John William Hairbottle. I wish to welcome the new members to the Institute and to congratulate those members who have been transferred to a higher grade.&apos; ANNUAL REPORTOFTHE COUNCILAND ACCOUNTS FOR THE YEAR ENDED 30th JUNE, 1970 The President: &apos;I now have pleasure in presenting to you, the Annual Report and Statement of Accounts for the year ended June, 1970. These have been handed to you this afternoon and, as is customary, I propose they be taken as read. Before moving their adoption, however, I would like to refer to some of the salient features, leaving as is usual, the task of dealing with the finances, to our Honorary Treasurer. It is encouraging that membership has continued to grow, and now stands at 1,613, an increase of 61 over last year&apos;s total. Your Council, however, is aware that there are still people in our mining and metallurgical industries, who could qualify for membership, but who have not yet joined the Institute. A drive to increase membership was accordingly organised, and members of Council were given the responsibility for campaigning in sections of industry, and for publicising the objectives and advantages of belonging to the Institute. Up to now there has not been much reaction to this campaign, but I hope we will see results in the coming year. At the same time, Council has recognised the need for change in the conduct of the Institute&apos;s affairs in order to meet the changing needs of our membership. Our members, both mining and metallurgical, are in the first place, geographically more widely dispersed than they used to be, and secondly, with the growth of the metallurgical industry, their technical interests are now more diversified. The Institute must cope with these changing needs if we are to continue to perform a useful function. The

The Annual General Meeting of the Institute was held in Kelvin House, Johannesburg, on Wednesday, 26th August, 1970, at 4.15 p.m. Mr. J. K. E. Douglas (President) was in the Chair. There were also present sixty-three Fellows, thirty-five Members, one Graduate, eight Associates, five Students and nineteen Visitors, making a total of one hundred and thirty-two. The President declared the meeting open at 4.20 p.m. OBITUARIES The President: &apos;It is my sad duty to announce the deaths of the following members of the Institute. Dr J. A. Papenfus, Fellow, who joined the Institute in 1942 and passed away on the 28th of May, 1970. Mr D. G. Beadle, Fellow, who joined the Institute in 1946 and passed away on the 17th of June, 1970. Gentlemen, Derek Beadle was very well known in this Institute. His papers on dust will be remembered and, at the time of his untimely death, he was one of our assistant editors. As a mark of respect to the memory of the deceased and in sympathy with the bereaved, I would ask you to rise and observe a few moments&apos; silence.&apos; MINUTES The President: &apos;May we confirm the minutes of the General Meeting held on 15th April, 1970, as published in the July, 1970, issue of the Journal&apos;. Agreed. WELCOME TO VISITORS The President: &apos;Ladies and Gentlemen, we are honoured this afternoon by the presence of many distinguished guests and I extend to you all a most cordial welcome. We are happy to have with us Dr A. A. von Maltitz, President of the Chamber of Mines of South Africa, who is also Honorary President of this Institute. We also have one of our Honorary Vice-Presidents, Mr T. L. Gibbs, the Government Mining Engineer; Mr D. E. Hamm, President, Institution of Certificated Mechanical and Electrical Engineers, S.A.; Mr S. C. M. Naude, Director, Witwatersrand Technical College; Mr I. R. G. Stephen, Senior Vice-President, The S.A. Institute of Electrical Engineers; Mr G. M. Tompkins, President, The S.A. Institution of Mechanical Engineers; Professor P. B. Ackermann, President of the Geological Society of S.A.; Mr A. S. Robinson, Vice-President of the S.A. Institute of Civil Engineers; Professor W. Mare, President of the Institute of Land Surveyors of the Transvaal; Mr B. D. Charlton, President of the S.A. Institute of Assayers and Analysts; Mr R. Hemp, The President, The Mine Ventilation Society of S.A.; Mr L. J. Prince, The President, The S.A. Association of Mine Managers; Mr J. Botha, The President, The S.A. Institute of Foundrymen; Mr G. Niterl, The President, The Institute of Welding; Mr M. R. Gericke, President, S.A. Council of Professional Engineers; Mr N. A. Honnet, Chairman, Orange Free State Branch; Mr P. R. C. Cooke, Chairman. The South African Chemical Institute (S. Tvl. Section). Gentlemen, we are very honoured indeed, to have these distinguished gentlemen with us this afternoon, as our honoured guests. We are also pleased to have with us, one of our Honorary Fellows, Mr F. G. Hill, and several Past-Presidents. I also extend a very warm welcome to all our lady guests and to all our other visitors.&apos; MEMBERSHIP The President: &apos;I have pleasure in announcing that the names of the following candidates, having been published in accordance with By-Law 5.2.2, Council has elected them to membership in the following grades: NEW APPLICATIONS Fellows: Herbert Dalton-Brown, Stephen William Morel. Members: Clive Lester Workman-Davies, Basil James Russell Botha. Students: Timothy Nigel Watson, John William Hair-bottle. I wish to welcome the new members to the Institute and to congratulate those members who have been transferred to a higher grade.&apos; ANNUAL REPORTOFTHE COUNCILAND ACCOUNTS FOR THE YEAR ENDED 30th JUNE, 1970 The President: &apos;I now have pleasure in presenting to you, the Annual Report and Statement of Accounts for the year ended June, 1970. These have been handed to you this afternoon and, as is customary, I propose they be taken as read. Before moving their adoption, however, I would like to refer to some of the salient features, leaving as is usual, the task of dealing with the finances, to our Honorary Treasurer. It is encouraging that membership has continued to grow, and now stands at 1,613, an increase of 61 over last year&apos;s total. Your Council, however, is aware that there are still people in our mining and metallurgical industries, who could qualify for membership, but who have not yet joined the Institute. A drive to increase membership was accordingly organised, and members of Council were given the responsibility for campaigning in sections of industry, and for publicising the objectives and advantages of belonging to the Institute. Up to now there has not been much reaction to this campaign, but I hope we will see results in the coming year. At the same time, Council has recognised the need for change in the conduct of the Institute&apos;s affairs in order to meet the changing needs of our membership. Our members, both mining and metallurgical, are in the first place, geographically more widely dispersed than they used to be, and secondly, with the growth of the metallurgical industry, their technical interests are now more diversified. The Institute must cope with these changing needs if we are to continue to perform a useful function. The

By R. B. Snow

This paper describes a technique of polishing and etching specimens of open-hearth furnace slags or hearth aggregates for identification of the crystalline constituents —lime (CaO), tricalcium silicate (3CaO.SiO2), dicalcium silicate (2CaO.-SiO2), rnonticellite (CaO.MgO.SiO2), or forsterile (2MgO.SiO2), with especial em-phasis on the mineral merwinite (3CaO.-MgO.2SiO2). With proper standardization, this identification does not require the use of the petrographic microscope. The composition of basic open-hearth slags and furnace bottoms falls, almost without exception, within systems containing CaO, MgO, &apos;IFeO,,, MnO and SiOz, in which the number of basic molecules so greatly exceeds the orthosilicate ratio (two molecules of base to one of silica) that free basic oxides, and combinations between them such as alumi-nates or ferrites, are present in cooled specimens. Orthosilicates of (CaO + NgO) are the most common in such specimens, since in nearly all cases, except premelt slags, the molecular ratio of (CaO + MgO) to SiO, is more than 2 to I. When sufficient lime is available it combines with the silica to form dicalcium silicate (2Ca0.Si02), which contains little, if any, IvfgO, FeO or MnO in solid solution whereas the latter oxides combine to form the oxide solid solution known as periclase. If the lime present is insufficient to form dicalcium silicate (2Ca0.Si02) it combines with Mgo to form either merwillite or moIlticellite (SiOz); these minerals take little if any FeO or MnO into solid solution and the remaining MgO, FeO and hInO combine as periclase. This generalization seems to be valid for basic slags and furnace bottoms, since minerals such as Ca0.MnOSi02 and CaO.FeO.SiOz are found only in slags in which the lime-silica ratio is less than 2 and are not observed in &apos;pecimens from furnace bottoms. The identification of crystalline constituents in such materials, especially of fine crystals in the groundmass, is difficult under the petrographic microscope. They are often masked by their neighbors because of their small size in relation to the thickness of the thin section and because of the presence of Opaque Or colored constituents. The indices of refraction and the optical sign of the mineral are sometimes difficult to determine because of the small size or because Of twinning or of inclusions within the crystal. Moreover, the positive identification of merwinite (3Ca0.Mg0.2Si02) from its optical properties is usually difficult in the presence of dicalcium silicate (zCaO.SiO2). CaO, MgO, jCa0.Si02 and 2Ca0.SiOz in open-hearth &apos;lags have been identified for a number of years in the U.S. Steel Corporation Laboratory by the usual

Jan 1, 1948

By R. B. Snow

This paper describes a technique of polishing and etching specimens of open-hearth furnace slags or hearth aggregates for identification of the crystalline constituents —lime (CaO), tricalcium silicate (3CaO.SiO2), dicalcium silicate (2CaO.-SiO2), rnonticellite (CaO.MgO.SiO2), or forsterile (2MgO.SiO2), with especial em-phasis on the mineral merwinite (3CaO.-MgO.2SiO2). With proper standardization, this identification does not require the use of the petrographic microscope. The composition of basic open-hearth slags and furnace bottoms falls, almost without exception, within systems containing CaO, MgO, &apos;IFeO,,, MnO and SiOz, in which the number of basic molecules so greatly exceeds the orthosilicate ratio (two molecules of base to one of silica) that free basic oxides, and combinations between them such as alumi-nates or ferrites, are present in cooled specimens. Orthosilicates of (CaO + NgO) are the most common in such specimens, since in nearly all cases, except premelt slags, the molecular ratio of (CaO + MgO) to SiO, is more than 2 to I. When sufficient lime is available it combines with the silica to form dicalcium silicate (2Ca0.Si02), which contains little, if any, IvfgO, FeO or MnO in solid solution whereas the latter oxides combine to form the oxide solid solution known as periclase. If the lime present is insufficient to form dicalcium silicate (2Ca0.Si02) it combines with Mgo to form either merwillite or moIlticellite (SiOz); these minerals take little if any FeO or MnO into solid solution and the remaining MgO, FeO and hInO combine as periclase. This generalization seems to be valid for basic slags and furnace bottoms, since minerals such as Ca0.MnOSi02 and CaO.FeO.SiOz are found only in slags in which the lime-silica ratio is less than 2 and are not observed in &apos;pecimens from furnace bottoms. The identification of crystalline constituents in such materials, especially of fine crystals in the groundmass, is difficult under the petrographic microscope. They are often masked by their neighbors because of their small size in relation to the thickness of the thin section and because of the presence of Opaque Or colored constituents. The indices of refraction and the optical sign of the mineral are sometimes difficult to determine because of the small size or because Of twinning or of inclusions within the crystal. Moreover, the positive identification of merwinite (3Ca0.Mg0.2Si02) from its optical properties is usually difficult in the presence of dicalcium silicate (zCaO.SiO2). CaO, MgO, jCa0.Si02 and 2Ca0.SiOz in open-hearth &apos;lags have been identified for a number of years in the U.S. Steel Corporation Laboratory by the usual

Jan 1, 1948

By J. R. Boldt, C. M. Kleemann, V. N. Mackiw, B. Meddings, J. A. MacLellan, E. J. Maney, D. E. Halter, D. J. I. Evans, J. Honkasalo, M. F. Dufour

The technology employed in the processing of nickel- and cobalt¬bearing ores is a continually developing process for utilizing the natu¬ral resources available at a given time. Most of the nickel-bearing ores of commercial importance fall under the category of sulfide or lateritic ores. While the occurrences of both types of ore have been known for over a century, until 1960 sulfide ores largely from Cana¬dian mines have constituted the chief source of production for com¬mercial nickel in the Free World. Sulfide ores are readily amenable to some physical means of concentration, but the lateritic ores are not readily concentrated, and to compete economically with the sulfide ores only the high-grade garnierite ores (a type of lateritic ore) found in New Caledonia were processed to any great extent up to the time of World War II. Around 1960, a gradual shift in emphasis towards latetitic ores as a commercial source of nickel became evident. See Fig. 1. New discoveries of sulfide ores, usually located underground, had not kept pace with the steadily increasing demand for nickel. The lateritic ores, found near the surface of the earth, could be readily surveyed and mined. Lower cost processes were being developed for the extrac¬tion of nickel from lateritic ores and for a time it appeared that, based on pre-OPEC economics, the lower grade lateritic ores-down to 1.2% nickel-could satisfy an increasing share of the world demand for nickel. The sharp increase in the price of crude oil in the 1970s, however, slapped an economic damper on the lateritic ores. Processes for treat¬ing lateritic ores consume large amounts of energy; as the nickel industry entered its deep recessionary period in 1981-83, nickel pro¬duction from lateritic ores became less and less profitable than from sulfide ores. At the same time, new sulfide ores were discovered and brought into production, notably in Australia and South Africa. The chapters in Section 17 were prepared in 1973. Recent improvements in mineral dressing techniques since then include Inco&apos;s pyrrhotite separation process which can remove additional pyrrhotite from nickel concentrates, resulting in reduced sulfur dioxide emission from the Sudbury smelter, by some 25%. The chapters in this section dealing with nickel are grouped in line with the two broad categories of nickel ores. Starting with the description of nickel and cobalt ores in Chapter 2, Chapter 3 deals with the processing of sulfide ores, and Chapter 4 deals largely with lateritic ores. The intermediate steps to produce a suitable feed for extraction plants and refineries are similar in principle within the same categories, although dissimilar between sulfide and lateritic ores. Thus Inco in Canada employs flotation and so does Western Mining Corp. in Australia, although Inco&apos;s plants were started before World War II, and that of Western Mining only recently in the late 1960s. Treatment subsequent to the ore dressing step, however, shows some interesting differences. The earlier parts deal mostly with established and conventional practices, leaning heavily on pyrometallurgy in both

Jan 1, 1985

By A. C. Watts

FOR several years, a mine in Colorado experienced considerable trouble from small fires caused by the blasting of coal. Although a well-known make of permissible powder was used, it was first thought that the powder ignited gas that might be present and that this, in turn, set fire to line brattices or to the coal. Experiments were, therefore, conducted with another make of powder, but the results convinced the superintendent of the mine, Robt. Williams, Jr., that the fires were not caused by the powder but by the high-voltage electric current used for detonating the shots. The mine "makes" gas very freely, giving off from three-fourths to a million cubic feet of methane per 24 hours. The coal is a good grade bituminous of a very free burning quality. Electric shot-firing from the outside after all men and animals were outside had been practiced for a number of years. The shooting circuit was connected with the main power circuit at the mouth of each entry. Shooting circuit switches were mounted in boxes, which were kept locked with the handle of the switch, in open position, showing through the bottom of the box. The door of the box could not be shut and locked when the shooting switch was closed. At the entrance to each room, or working place, a small switch, called the miner&apos;s switch, was placed on the shooting line. It was the duty of the miner, when entering his place at the beginning of the shift, to see that this switch was open and that it was kept open until he left the place at the end of the shift to go out of the mine. Grounded return was used for main power lines. The current was 500 volts, direct current, with 100 to 300 amp. The nearest working face was 9600 ft. from the shot-firers&apos; switch outside the mine and the most remote working face was 2 ½ miles. The various working faces were scattered over a wide area between these two points.

Jan 9, 1925

By O. C. Holbrook, George G. Bernard

A new theoretical treatment has been obtained for the behavior of pattern waterflood injection wells when closed in. Two cases are treated: Case I where oil and water are assumed to have the same properties, and Case 2 where they arc different. In applying the method, one plots log (p — p,) vs closed-in time, where p is well-bore pressure at any tims and p, is static pressure. The value of p. is determined by trial and error as that value which makes the plot linear at large time. A value for the permeability-thickness product can be determined from the intercept of this linear part, and a value of the skin factor from the injection pressure at time of closing in. Application of the method to data from water floods at three fields seems to give reasonable results. For the case of unit mobility ratio, it is proved that this new method should give the same value for permeability-thickness product as the conventional pressure build-up method. In addition, the new method gives correct values for static pressure, whereas the conventional method does not, often indicating negative static pressures. The new method may be used in cases where the surface pressure persists after closing in as well as in cases where it does not. INTRODUCTION It is of considerable interest and importance to be able to determine the characteristics of the reservoir in an area surrounding a water injection well. Thus, if we can determine early in the life of an injection well that there is a considerable "skin effect", remedial measures can be started before a full-scale pattern flood begins. Similarly, if it can be shown that a gradual buildup of skin effect is occurring with time, measures to free the water of plugging material can be taken. Determination of static pressure in the water-injection well may show that the water is entering a thief zone and not the desired reservoir. Finally, determination of the permeability of the sand around the injection well will allow estimation of the future relation between injection pressure and rate. It should be possible to determine average reservoir permeability, skin effect and static pressure from pressure fall-off data. However, at the time we began work on this subject, it was thought that no adequate theory on which to base such determinations&apos; was available. According to the conventional method which considers the reservoir to be filled with one fluid of small compressibility (see Van Everdingen, Joers2, and Nowak2), shut-in pressure is plotted vs log where is injection time, and At is closed-in time. The physical significance of injection time, may well be questioned in this case, since in a reservoir completely filled with a single fluid (as required by this theory) and with input and output rates equal, the pressure behavior after an initial transient is independent of t,. Attempts by our Tulsa area to use this theory led to negative values of static pressure in most cases. Because of these limitations of the method discussed above, it was decided to attempt to develop a new theory of pressure behavior in water injection wells, one which would apply when there is a gas saturation, as is so often the case in water floods. In the following treatment the assumptions and basic equations are given first, then the method of application of the equations. A complete example is given to clarify details of application. All difficult mathematics has been placed in the appendices so that the reader can follow the text without difficulty. However, if he wishes only to apply the results without knowing the basis for them, he can learn how to do this from reading only the sections entitled "Plotting of Experimental Results" and "Example." ASSUMPTIONS AND BASIC EQUATIONS Statement of Problem It will be assumed that a horizontal layer of constant thickness contains in its pore system a mixture of oil, gas and water. While water is being injected into this pore- system through a well at constant rate, an oil bank is built up, gas being expelled from the space taken by the oil as shown in Fig. 1. The saturations within each

By W. M. Robertson

The kinetics of grain boundary groove formation on copper surfaces immersed in liquid lead have been studied over the temperature range of 400° to 900°C. The groove widths were Proportional to the cube root of the annealing time, indicating that the diffusion of copper through the saturated liquid-lead solution is the mechanism by which grooves form. The rate constant for the process can be calculated by a theory due to Mullins. Using published data for the solubility of copper in liquid lead, for the interfacial energy of the solid copper-liquid lead interface, and for the diffusion coefficient of copper in liquid lead, the calculated rate constants almost exactly reproduce the measured values over the entire temperature range. The decay of scratches placed on copper surfaces has also been studied. The rate constant for scratch decay agrees with that for grain boundary groove growth, though scratch decay is sensitive to convection currents in the liquid. The interaction of solid and liquid metals has been studied extensively and has been found to be rather complex. Many of the studies have been complicated by a host of competing effects, including temperature gradients, concentration gradients, the formation of one or more intermetallic phases, natural or forced convection, and the presence in both the solid and liquid of considerable amounts of impurities and alloying elements. Recently theories have been developed of changes in surface profiles driven by capillary forces,&apos; which allow the interaction of the solid and liquid to be analyzed quite directly. The present paper reports a study of the formation of grain boundary grooves on pure copper immersed in liquid lead, which allows the theory to be checked quantitatively. The Cu-Pb equilibrium diagram is quite simple: there are no intermetallic compounds, copper is just slightly soluble in liquid lead, and lead is almost completely insoluble in solid copper.2 The Cu-Pb system has been studied extensively,3-9 and all of the quantities—interfacial energy, diffusion coefficients, and equilibrium solubilities-necessary to calculate the rate of groove growth by a volume-diffusion mechanism are known. The kinetics of grain boundary grooving and scratch smoothing have been studied on the noble metals and the iron group metals in a reducing atmosphere or in vacuum.10 The main interest of these studies has been the determination of surface-diffusion coefficients at metal-gas interfaces using the theories developed by Mullins.1 The present paper uses similar methods for the study of diffusion processes at the interface between two condensed phases. There has been one previous study" of the kinetics of groove growth in a solid-liquid system, which, however, was troubled by the fact that neither interface energies nor diffusion coefficients were known in the Ni-S system studied. THEORY The theory of grain boundary groove growth has been developed by Mullins for the cases of volume diffusion," surface diffusion," and a combination of the two processes.14 He has also analyzed the kinetics of the flattening of a scratched surface by these processes.l5,l6 Several assumptions and approximations were used in the derivations of the surface profile shapes. The applicability of these assumptions and approximations to the present system will be considered in the discussion. At the intersection of a grain boundary with an initially flat interface the equilibrium between the interfacial energy and the grain boundary energy establishes an equilibrium groove angle. This induces curvatures in the interface. The chemical potential of material at a curved interface is higher than at a flat interface, so that material moves away from the region of the grain boundary. Mullins&apos; calculations indicated that the groove profile would be similar to that shown schematically in Fig. 1. Small humps form above the level of the original flat surface. For a volume-diffusion mechanism the separation, w, of these humps at a time, t, is given by and where co is the equilibrium concentration of the solid in the liquid, y, the solid-liquid interfacial free energy, O the volume occupied by a solute atom in the liquid, D the diffusion coefficient of the solid in the liquid, and kT has its usual meaning. For a surface-diffusion mechanism the groove width is proportional to the fourth root of the time. For grooves forming by a combined surface and volume-diffusion mechanism the exponent of the

Jan 1, 1965

By G. W. Preckshot, J. W. Gorman

MOLTEN metals offer an excellent medium for the study of molecular diffusion and interphase transfer. In the absence of intermetallic compound formation, solutions of molten metals are solutions of elements. Therefore, complicating factors such as molecular structure, dissociation, association, polarization, and so on, are generally absent. Further, metals remain in the liquid state over a wide range of temperature. Thus, the effect of temperature on transport processes can be studied in more detail. Although some data are available for the diffusion of metals in the molten state at high temperatures,"""".&apos;!&apos; the most useful and accurate data are those for the diffusion of various elements in mercury at room temperature. The effective radius of diffusion for the various elements in mercury may be calculated from the Stokes-Einstein relation.&apos;-These calculated radii are compared with the atomic and ionic radii calculated from X-ray data on crystals." The effective radii of diffusion of the alkali and alkali-earth metals correspond to those of the neutral atom; those of cadmium, silver, lead, zinc, thallium, bismuth, and tin correspond to ionic radii; and those of copper and gold indicate larger radii due to association with mercury or more likely, faulty diffusion data. Independent evidence"&apos; supports the notion that alkali metals are uncharged in amalgams. The concept of metals moving free of their conductance electrons in the liquid state has been discussed by Eyring, et al,&apos;" in connection with studies on the viscosity of pure molten metals. Considering the approximate nature of the tabulated atomic and ionic radii and the variance in the diffusion measurements, the application of the Stokes-Einstein equation to the diffusion of metals in mercury gives gratifying results. It is noted that a number of these metals have article radii eaual to or less than those of the solvent mercury.".&apos;*,"&apos; Soba1,&apos;" sing the inaccurate Roberts-Austin20 data, indicated that the effective radius of diffusion might well be a function of temperature. Additionally in studies of mass transfer between phases, many conflicting opinions have been expressed concerning the assumption of equilibrium at the interface." ,","," The results of the present work on the diffusion of solid copper in molten lead throws light on the tempera- ture variation of the diffusion radius as well as the extent of the interfacial resistance. The theoretical background and experimental procedure are presented here in detail. Results on other systems will be presented in subsequent papers. Nomenclature The following nomenclature is used in the paper: A—cross-sectional area of diffusion column, sq cm C, C,—concentration of solution and saturated solution respectively, g per cc D,D&apos;—-diffusivity, sq cm per sec e—Naperian base h—ratio, k/D k—mass-transfer coefficient, cm per sec L—diffusion column length, cm n—series index q—flux, g per sq cm-sec r—radius, cm or A R—-gas constant t—time, sec T—temperature, K V—volume, cc w—weight of copper-lead alloy on copper cylinder WT—-total copper transferred to lead diffusion, column, g Z—distance from top of diffusion column, cm 2&apos;—distance from copper-lead interface, cm (2&apos; = L-2) u,,—roots of diffusion equation Mathematical Apparatus The model shown in Fig. 1 applies to the diffusion of solid copper into molten lead. Here Fick&apos;s first law may be written where all terms are defined in the nomenclature. It is assumed that the volume of the lead column is constant. This is justified since experimental densities compared favorably with calculated densities based on perfect interstitial mixing. Thus there is no counter diffusion of lead. It is clear that 2 in Equation [I] should be measured relative to the interface which moves relative to the diffusion cell but not to the liquid phase. Hence, the frame of reference is the plane of the copper-lead interface. The diffusivity calculated at constant volume, D", is that defined by Hartly and Crank" and is designated herein as D. No Interfacial Resistance—The two situations of the presence and absence of interfacial resistance will be treated. The simplest is the latter which re-

Jan 1, 1959

By K. -A. Björkstedt

INTRODUCTION Strassa lies in the central part of Bergslagen, a tradi¬tional mining district, on the eastern side of the Stora Valley at an elevation of about 200 m above sea level. A railway siding runs between the mine and the Stora railway station from which there are railway connections to the shipping port and iron and steel works in Oxelosund, about 224 km away. The distance to the provin¬cial capital Orebro is about 60 km. The climate is typi¬cal for this part of central Sweden and is illustrated by the diagram of monthly precipitation and temperatures for the years 1968-1975 (Fig. 1). HISTORY There is no certain information as to when the Strassa mine was first worked, but it is known from sur¬viving accounts of mine inspectors that there were smelt¬ing works in operation in nearby villages in the 12th century. An example is the Gusselhytta ore smelting works, 10 km south of Strassa, which dates from this period. Around the year 1540 there were two smelting works in Strassa, the Upper Karberg and Lower Karberg works. Ore for these smelters was probably taken from Strassa and from the adjacent Blanka mine. In the year 1624 Strassa is mentioned by the painter Jons Nils Krook in an account of the iron mines in the Linde mining district (Linde Bergslags Jarngruvor). Several mines were listed in the area, the deepest being about 30 m. An impressive power installation is mentioned in 1639, including a piston system of lashed poles for transmit¬ting power from the Stora River to the Strassa fields. Its length was 2670 m. Common ground comprising about 20.2 km2 (5000 acres) of forest was allocated in 1689 for the furtherance of mining operations. Until the beginning of this century only the rich cen¬tral parts of the ore body were mined and these yielded, after handpicking, lump ore suitable for smelter feed. An example of the ore grades from these early times is an analysis of ore from the "Big Mine" (Storgruvan) from the year 1873: 48.5% Fe, 0.008% P, and 0.06% S. This same year a total of about 18 000 t was ex¬tracted from the Strassa mine. OWNERSHIP The mine was owned and run until 1874 by a min¬ing association made up of 119 so-called "bergsman," who were homesteaders often engaged in agriculture and timber-cutting as well. In that year the Strossa Grufvebolag (Mining Co.) was founded. In 1906 it was con¬verted into a joint stock company, the Strossa Gruveaktiebolag. This was acquired in 1907 by Metallurgiska AB for the implementation of Gustav Grondal&apos;s beneficiating and briquetting methods, for which the Strassa ore was well suited. The same year saw the completion of a new ore dressing plant with an annual production of 46 000 t of ore concentrate. In 1911 the mine passed to new hands, and in 1913 it was purchased by an Austrian company. Extensive new installations were made and in 1915 a new dressing and briquetting plant was completed with twice the capacity of the old one. In 1917 the Strassa mine was acquired by Granges. Be¬cause of unfavorable business trends and technical diffi¬culties, mining operations were brought to a close in 1923. Pumping kept the mine free of water until 1933 but it was completely filled ten years later. Up to 1950 the surface buildings and installations remained intact but the large dressing and briquetting plant burned to the ground in that year. Today only the machine shop re¬mains from this earlier period of operation, now housing parts of the Mineral Processing Laboratory. The decision to take up mining operations again was made in 1955 and construction work began the follow¬ing year. Of the old installation, only the "southern shaft" could be used for some development drifting after it had been completed with a new headframe. Other¬wise, all the buildings and installations required for the operations had to be rebuilt. New installations ready by 1960 were office and personnel facilities, a new shaft and headframe, a sorting and concentrating plant, a macadam plant, settling basins, pump stations, and a railway and yard with transport equipment. The instal¬lation was completed with two plants

Jan 1, 1982