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By H. F. Mills

THE Iron King mine is 12 miles east of Prescott Arizona, in low foothills of the Agua Fria mining district. It was operated in 1906 and 1907, using gravity methods of concentration, mostly on oxide ores. In 1923 and 1924 shipments of sulphide ores were made to the Humboldt smelter. It remained inactive and stripped until 1936, when it was unwatered and sampled to the 400-ft level, the bottom at that time. In 1937 the Iron King Mining Co. purchased the mine and shipped oxide ores. During 1938 a bulk flotation plant of 140 tons daily capacity was erected. The mill has been enlarged and operations have been continuous since the mill first started. In July 1942, the Shattuck Denn Mining Corporation purchased the physical assets from the Iron King Mining Co., and since that time it has operated as the Iron King Branch of the Shattuck Denn Mining Corporation. Economic metals recovered are gold, zinc, silver, lead, a little copper, and fluxing pyrite. The ore occurs as a series of northward-dipping shoots arranged in echelon pattern, the series extending over a length of 3500 ft. Strike lengths of shoots vary from 60 to 600 ft, and widths from 3 ft to as much as 14 ft. The ore occurs in a sheared zone in pre-Cambrian chloritic schist. This schist belt is about 6 miles wide, and the ore zone is about 4 miles from the pre-Cambrian granites to the west. No intrusive rocks have been found in the mine, nor is there evidence of any on surface that might indicate a genetic connection with the ore occurrence (Fig I). The schists strike N23°E and dip 75° to the northwest, which might indicate an overturned thrusting from the granites. In the upper levels, the echelon pattern in which the ore occurs was quite regular, no disturbance of the enclosing schist, or of any faulting that might contribute to the formation of the ore pattern was noted. There is a possibility that the ore zone may be on the axis of an isoclinal fold. Another interesting feature is the more or less typical zoning of minerals along the strike in each of the ore shoots (Fig 2). The north end of each shoot is enclosed by schist, while the south ends usually extend out at full width beyond the economic mining limits in a pyrite-quartz low-grade material. The plane of demarcation between ore and schist is very sharp, with little or no impregnation of sulphide in the schist, especially on the footwall side. The footwall schists are usually firm and strong, and vary from dioritic phases to fine-grained, lighter colored bands, almost silky in texture. The hanging wall for a width of 50 to 8o ft consists of alternating sheetings of chloritic and pyritic schists. The mine is now partly developed to the 92o-ft level, with some diamond drilling from the 1150-ft station of No. 6 shaft. Economically there has been little change in nature or grade of ore from the top of the sulphides, about 200 ft below surface, to the bottom levels. There have been a few echelons in depth, just as there are in plan, and while a few shoots have had

Jan 1, 1947

By H. F. Mills

The Iron King mine is I2 miles east of Prescott Arizona, in low foothills of the Agua Fria mining district. It was operated in 1906 and 1907, using gravity methods of concentration, mostly on oxide ores. In 1923 and 1924 shipments of sulphide ores were made to the Humboldt smelter. It remained inactive and stripped unti1 1936, when it was unwatered and sampled to the 400-ft level, the bottom at that time. In 1937 the Iron King Mining Co. purchased the mine and shipped oxide ores. During 1938 a bulk flotation plant of I40 tons daily capacity was erected. The mill has been enlarged and operations have been continuous since the mill first started. In July 1942, the Shattuck Denn Mining Corporation purchased the physical assets from the Iron King Mining Co., and since that time it has operated as the Iron King Branch of the Shattuck Dcnn Mining Corporation. Economic metals recovered are gold, zinc, silver, lead, a little copper, and fluxing pyrite. The ore occurs as a series of northward-dipping shoots arranged in echelon pattern, the series extending over a length of 3500 ft. Strike lengths of shoots vary from 60 to 600 ft, and widths from 3 ft to as much as 14 ft. The ore occurs in a sheared zone in pre-Cambrian chloritic schist. This schist belt is about 6 miles wide, and the ore zone is about 4 miles from the pre-Cambrian granites to the west. No intrusive rocks have been found in the mine, nor is there evidence of any on surface that might indicate a genetic connection with the ore occurrence (Fig I). The schists strike N23°E and dip 75° to the northwest, which might indicate an overturned thrusting from the granites. In the upper levels, the echelon pattern in which the ore occurs was quite regular. no disturbance of the enclosing schist, or of any faulting that might contribute to the formation of the ore pattern was noted. There is a possibility that the ore zone may be on the axis of an isoclinal fold. Another interesting feature is the more or less typical zoning of minerals along the strike in each of the ore shoots (Fig 2). The north end of each shoot is enclosed by schist, while the south ends usually extend out at full width beyond the economic mining limits in a pyrite-quartz low-grade material. The plane of demarcation between ore and schist is very sharp, with little or no impregnation of sulphide in the schist, especially on the footwall side. The footwall schists are usually firm and strong, and vary from dioritic phases to fine-grained, lighter colored bands, almost silky in texture. The hanging wall for a width of 50 to 80 ft consists of alternating sheetings of chloritic and pyritic schists. The mine is now partly developed to the 920-ft level, with some diamond drilling from the 1150-ft station of No. 6 shaft. Economically there has been little change in nature or grade of ore from the top of the sulphides, about 200 ft below surface, to the bottom levels. There have been a few echelons in depth, just as there are in plan, and while a few shoots have had

Jan 1, 1949

By U. F. Kocks

SINGLE slip and a single parallel array of edge dislocations have been obtained in silicon single crystals by homogeneously bending them in a four-point dead-loading device at 1000°C around the [211] axis with [253.] as the tensile axis which encloses an angle of 40° with the glide plane. Other orientations or lower temperatures proved unsuitable. The homogeneity of the bending was checked by the method shown in Fig. 1. The chemically polished specimen was exposed to parallel light from a microscope-stage lamp. The sharpness of the focus of the reflected light is an approximate measure of the circularity of the sample. This method permitted the determination of the actual radius of bent specimens within 10 pct accuracy. The etching solution developed to show up dislocations consisted of the following volume parts: 2 HF, 1 HNO,, 2 CH,COOH, 1 a solution of 5 wt pct of CuNO, in water (Rosi'). The acetic-acid content was adjusted to produce fine well-defined etch-pits in about 2 min at room temperature. The effectiveness of the etch did not depend on the crystal-lographic orientation of the face etched. The number of etch pits produced after a given deformation was checked in the usual way against the Cahn formula' and showed good agreement. As it is to be expected from the orientation of the primary system there are slip steps on the top and bottom faces but not on the side faces (perpendicular to the bending axis), whereas etch pits appear on the side faces but not on the top and bottom faces. This is different only for occasional dislocations of a secondary glide system. All the micrographs included have been taken in places where the most of secondary glide could be seen. From this it is evident that in the homegeneously deformed region the number of secondary dislocations was less than 1 in 1000 of the primary type. Dislocation Distribution—A series of tests with varying amounts of deformation is shown in Figs. 2(a-c). An observation that can readily be made from these pictures is that the linear density of dislocations within slip lines is relatively constant and independent of the amount of deformation. "Slip line" in this context is understood to mean a line that is a straight connection of individual etch pits. The heavily pitted bands which can be seen in each of these three pictures may be resolved fairly definitely, at higher magnifications, into many "slip lines" the distance between them being of the order of 0.5p The distance between dislocations in slip lines is of the order of 2p and it is also fairly constant in going from the neutral zone outward. The higher over-all dislocation density in the outer regions of any sample and the higher total number in a more heavily deformed sample, are effected by a larger number of "slip lines." The relative constancy of the dislocation distance within an individual slip line is surprising. The absence of pile-ups" may imply, if there is no rear- rangement on unloading," that there are no substantial obstacles to slip in this case. It seems that the equilibrium distribution of the dislocations in each active slip plane under the higher external stress on

Jan 1, 1959

By H. R. Stahi

THE ore of the Southeast Missouri lead district consists essentially of galena in dolomitic limestone. The galena usually is in a very finely disseminated condition. The experience of recent years in the concentrating plants of the St. Joseph Lead Co. has shown that dry crushing carried to a point where about 90 per cent of the ore passes a 14-mesh screen liberates the larger portion of the galena, and minimizes further necessary reduction in rod or ball mills. Concentration practice has attempted to carry size reduction to a point where economic unlocking of the galena is obtained, without causing undue sliming of the very friable galena. While 60 per cent of the tonnage of the district is treated by the flotation process, only 40 per cent of the total concentrates is produced by that means, as efforts have always been made to keep the grade and tonnage of flotation feed as low as possible. The milling practice of the district for some years has recognized the generally accepted idea of better selective grinding in rod mills as compared with ball mills, with the attendant decrease in production of fines. The function of rod and ball mills in the various concentrating plants is the grinding of table middlings and coarse tailings that carry lead values too high to be discarded. The simplified flowsheet in Fig. I illustrates the place of grinding mills in the circuit. The arrangement of classifiers, tables and mills constitutes a closed circuit within somewhat flexible limits. In 1937 experiments were conducted in replacing the ball charge in a 6 by 4-ft. ball mill with rods 2 in. in diameter and 51 in. long. This step was taken with some hesitancy, as it was easy to picture a mass of tangled and crossed rods. However, no difficulties developed, and after a short trial period, six more ball mills were converted to rod mills. These mills are of the spur gear and pinion, belt-driven type, using in most cases a 75-hp. motor and having a 9 1/2 -in. open trunnion discharge. As ball mills, they carried a charge of 16,000 to 20,000 lb. of balls, 2 in. in original size. The feed to the mills was dewatered by dewatering wheels and introduced at 70 to 75 per cent solids, with a single scoop feeder. One change in mill design was found advisable when rods were introduced. The existing end liners had an outward flare of 3 ½ in. in 12 in. These were replaced by linings having vertical interior faces, in order to prevent undue end travel of the rods. This change gave an effective working length of 5 2 ¾ in. inside the mill. No alterations were made in the shell liners, which are of the smooth type, made of manganese steel 2 in. in original thickness. The rods at present in use are 51 in. long and 1 3/4in. in diameter. The composition has been varied at times; at present they contain 0.70 per cent carbon and 0.70 per cent manganese. Some breakage and etching occurs as the rods become small, but this is considered preferable to using softer rods, which may kink and cause tangling of the charge. The mill charges are renovated occasionally, broken pieces being removed and the charge brought up

Jan 1, 1945

By G. S. Upadhyaya, A. D. McQuillan

HERE would appear to be a simple relationship between the group number in the periodic table of the early transition metals and the maximum amount of hydrogen which they can absorb.' Thus group IIIA metals (Sc, Y, and La) yield a trihydride in which the metal atoms are on a fcc lattice and the hydrogen atoms occupy both tetrahedral and octahedral interstices. Group IVA metals (Ti, Zr, Hf) form dihy-drides in which the metal atoms are on either a fct or cubic lattice, but in which only the tetrahedral interstices are occupied by hydrogen atoms. In group VA (V, Nb, Ta) the hydrogen-saturated metal attains a composition slightly below that of a monohydride under normal conditions. Finally the metals of group VIA (Cr, Mo, W) do not dissolve appreciable quantities of hydrogen. The manner in which hydrogen solubility disappears on alloying a group VA metal with one from group VIA has previously been investigated.2 It is necessary, in order to obtain a general picture of the reactions of alloys of the early transition metals with hydrogen, to examine a system containing metals from groups IVA and VA in which there must be a change from a fcc to a bee hydride phase. The system chosen for investigation was the pseudobinary system between titanium hydride and niobium hydride. Metallic alloys were prepared by melting iodide-prepared titanium with zone-refined niobium in an argon-atmosphere are-furnace. To ensure homogeneity each alloy was cold-swaged and then heated at 1250°C in a high-vacuum furnace until metallo-graphic examination confirmed its complete homogeneity. Small weighed specimens of the alloys were charged with hydrogen using gaseous hydrogen generated by heating titanium hydride. The apparatus has been described elsewhere.3 Throughout the charging process the hydrogen pressure was kept at about 1 atm while the specimen, initially at 800 °C, was slowly cooled to 150°C over a period of days. The total amount of hydrogen absorbed by each specimen and the room-temperature crystal structure of the hydride powders were determined. The X-ray investigation indicates that the fee hydride phase arises from alloys extending in composition from titanium to 67 at. pct Nb. After a two-phase field lying between 67 and 74 at. pct Nb in which the fee and bee hydrides coexist, all alloys richer in niobium yield a distorted bee hydride. Data derived from parameter measurements are presented in Fig. 1. The atomic volume per metal atom has been plotted against the composition of the initial metallic alloy in order to facilitate comparison of the effects of hydrogen addition in the two phases of different crystal structure. The amount of hydrogen absorbed by each alloy at saturation in terms of the hydrogen to metal ratio and alloy composition is given in Fig. 2. Over the whole range of the fee hydride phase the hydrogen content remains constant, while in the distorted body-centred hydride phase, the hydrogen content increases with increasing titanium content reaching a hydrogen/metal ratio of 1.4 at the boundary of the two-phase region. It seems likely, therefore, that the maximum hydrogen content of the fee hydrides is limited to a hydrogen/metal ratio of 2 because hydrogen atoms

Jan 1, 1962

By J. T. Norton, N. J. Grant, A. M. Gervais

An investigation of the creep deformation of coarse-grained high-purity aluminum at temperatures approaching the melting point permitted the formulation of a theory of subgrain formation. Subgrain boundaries were found to be formed by two different processes: kinking and polygonization. Polygonization is considered as the main factor in subgrain formation. SINCE "slipless flow" was first discussed in detail by Hanson and Wheeler,' many studies have been undertaken to determine how metals deform at high temperatures. Several types of observations have been reported. Jenkins and Mellor,² working on the creep of mild steels and various grades of commercial irons, found metallographic evidence of a kind of substructure within the grains after deformation at high temperatures. Homes" observed after creep deformation of steel at high temperatures that the original X-ray spots were sharply divided into several small ones. The same phenomenon was reported by Hirst4 from his studies on lead and later by Crussard5 from his work on aluminum. The works of these investigators demonstrated beyond any doubt that the splitting of the X-ray spots was due to the fact that the grains underwent a division into subgrains during deformation at high temperatures. Since then, numerous experiments have been undertaken on aluminum in order to determine the mechanism of formation of subgrains. Research workers can be divided, for the purpose of discussion, into two different groups as regards thinking on subgrain formation. On one hand, based on the work on polygonization by Cahn,6 Guinier and Lacombe,7 Greenough and Smith," Crussard,10,11 and Servi, Norton, and Grant," it was concluded that subgrain formation was a consequence of the simultaneous effects, first, of inhomogeneous deformation which produced bending of the lattice, and second, polygonization. On the other hand, Wood and coworkers13-16 based their work on the results of an earlier report" which dealt with crystallite size and a fragmentation theory. It is interesting to note that while Greenough and Smith8 and Wood et al. performed similar experiments, their conclusions were quite different. Wood et al. did not recognize polygonization as a fundamental mechanism and said that aluminum, at the beginning of the deformation, fragmented immedi- ately into subgrains in order to permit deformation of the metal, the number of these subgrains being a function of strain rate and temperature. They concluded that deformation of grains occurred by flow along the subgrain boundaries. In view of the contradictory conclusions, it would appear that the data were not explicit enough to provide an unambiguous conclusion. It appears that the techniques by which most of the results were obtained, namely, X-ray work, were not enough by themselves to solve the problem. Another approach was needed. In the present research, therefore, an extensive metallographic study was planned to supplement the X-ray work. The importance of revealing the subgrain boundaries metallographically was realized, and this will explain the extensive development and use of etching techniques. In order that subgrains would be considerably larger and therefore more readily visible under a microscope, the creep experiments were performed at very high temperatures approaching the melting point of aluminum. Development of Experimental Technique Creep tests were run at constant load on high purity (99.995 pct) aluminum specimens having a very coarse grain size. None of the specimens was run to fracture. The specimens were originally round (diameter, 0.187 in.; gage length, 1 in.) and had parallel flats milled in the gage section to permit

Jan 1, 1954

By J. Chipman, N. J. Grant, J. C. Fulton

This paper contains data on the distribution of silicon between liquid iron-silicon-carbon alloys saturated with respect to graphite and CaO-SiO2-Al2O3 slags under 1 atm of CO at 1600°C. The ranges of slag compositions studied were extended from the dicalcium silicate saturated liquidus composition up to silica concentrations at which Sic appeared as a stable phase. IN blast furnace operation it is not to be expected that slag and metal reach equilibrium with one another. Nevertheless, the silicon content of the metal varies with slag composition and with temperature in a manner which would be predicted from equilibrium considerations. Similarly, the distribution of sulphur between slag and metal does not attain an equilibrium state, yet the influence of slag composition is strongly analogous to its effect on the distribution equilibrium. The desulphurizing power of metallurgical slags has been shown to be highly dependent upon the FeO content of the slag. Moreover, the rate of removal of sulphur from slags is influenced by the oxygen potential of the slag-metal system. Thus it was shown by Grant, Kalling, and Chipman1 that the presence of MnO in slags which are low in FeO causes a marked slowing down of the transfer of sulphur from metal to slag. This led to the hypothesis that the slow removal of sulphur by blast furnace slags of more acid composition might be due in part to the effect of SiO2 on the oxygen potential of the system. This was verified in the work of Grant, Troili, and Chipman,' who found that the desulphurizing power of the more acid blast furnace slags could be markedly improved by an increase in the silicon content of the underlying metal. Their explanation of this improvement was that the higher silicon content of the metal decreased the rate of transfer of more silicon and, along with it, of oxygen from the slag to the metal. The slowness of the transfer of sulphur from metal to slag was the result of the slow reduction of SiO2 from slag to metal. Attempts to study the rate of sulphur removal had in the past resulted in very slow rates corresponding to the rates of silica reduction. It has become evident on the basis of these studies that further experimental studies on the rate of removal of sulphur must take these factors into consideration if there is to be a clear understanding of the rate of sulphur transfer under conditions simulating those existing in the blast furnace. It will be necessary, at least in a part of such study, to employ combinations of slag and metal in which the disturbing effect of silica reduction has been eliminated; in other words, to employ slag-metal combinations which are already in equilibrium with respect to the transfer of silicon. In preparation for such studies of desulphuriza-tion, a preliminary program of research on the distribution of silicon between slag and metal has been undertaken. This will ultimately include a comprehensive survey of the effects of temperature and slag composition on the equilibrium distribution of silicon between slag and metal. The present paper is a report on experimental methods employed and on

Jan 1, 1954

By J. G. Richardson

The performance of laboratory water floods is compared with the flooding behavior calculated by the Buckley-Leverett techniques from steady-state relative permeability-saturation relations. Both the steady-state and unsteady-state experiments were conducted on the same sand-packed column. Relative permeabilities were calculated by the Welge technique from the unsteady-state waterflooding displacement experiments and compared with those measured by steady-state techniques. An evaluation of the various calculation procedures was made. It was demonstrated that steady-state relative permeabilities could be used to calczcJate waterflood performance. INTRODUCTION To calculate the waterflooding behavior of a given reservoir, relative permeability-saturation relations of the reservoir rock are required. These relative permeabilities are commonly measured on core samples by steady-state experiments such as the Penn State technique.' The relative permeabilities obtained in steady-state experiments are calculated from oil and gas flow rates and pressure drops measured under conditions of equilibrium distribution of oil and water in the pore spaces with slow approach to equilibrium. On the other hand, in water floods the water saturation at a given point changes rapidly with time as the flood front passes. Extensive research2 has shown that the steady-state relative permeabilities to oil and water are independent of the rate of flow and the fluid viscosities. Research has also demonstrated that the waterflooding performance of homogeneous sands uniformly contacted by water is independent of rate when capillary pressure gradients, which are important in short laboratory columns, are made negligible. However, there is little experimental data in the literature comparing relative permeabilities calculated from steady-state flow experiments with those calculated from flooding experiments. In this paper, the production data of two water floods and the relative permeabilities calculated from a series of steady-state experiments on an unconsolidated sand column are presented along with the comparisons calculated by the Buckley-Leverett and by the Welge techniques. The purpose of this study was to determine if steady-state relative permeabilities could be used to predict the waterflooding performance. This study also permitted an evaluation of the Buckley-Leverett and Welge calculation procedures and allowed an insight into the nature of microscopic displacement of oil by water. EXPERIMENTAL APPARATUS AND PROCEDURE The apparatus used in this investigation was a Lucite column 1 ft long and 11/2 in. in diameter. A drawing of the apparatus is shown in Fig. 1. Six pressure taps were evenly spaced along the top of the column to measure the oil pressures. Three pressure taps fitted with small porous disks were spaced along the side of the column to measure water pressure. Water was admitted to the inflow face of the sand through a porous disk while oil was admitted through a hole in the porous disk and distributed to the face of the sand by grooves machined in the porous disk. Retainer screens of 325-mesh stainless steel were cemented over the inlet and outlet ports and the pressure taps to prevent loss of sand. The column was packed with a clean dry sand all of which was finer than 200 mesh. Next, the sand was saturated with a solution of 150,000 ppm sodium chloride solution. The column was weighed dry and water-saturated to obtain data for the calculation of the pore volume. A 151-cp oil was then injected into

Jan 1, 1958

By B. N. Webber

During World War II the Pocos de Caldas bauxite deposits of Minas Gerais in Brazil yielded some 60,000 tons. Since then they have maintained a small but almost continuous production. Known for many years, the deposits have been reconnoitered by a number of geologists,1-4 but no dimensional study has been possible because there have not been enough exposures to show clearly the depth, bedrock, and habit of occurrence. The deposits are somewhat unorthodox in their occurrence mainly on steep slopes of mountainous terrain. Although the parent rocks are a sequence of alkalic intrusions that bauxitize readily under the proper conditions, bauxitization has not been the dominant weathering process in the area. It is limited to certain localities where important volumes of bauxite have formed by laterization of several rock types, each yielding a distinctive type of bauxite. Bauxitization may be observed in several stages and in both direct and indirect cycles of formation. The deposits are unique in being of demonstrably recent age, so that the conditions under which the bauxite formed are essentially those of the present time. The bauxitization sequence is postulated in Fig. 1. Pocos de Caldas district is situated at approximately 21" 50' south latitude and 46" 30' west longitude in southwestern Minas Gerais, near its boundary with the state of Sao Paulo. It lies within the Eastern Plateau physiographic province of Brazil, occupying a prominent highland area that rises some 2000 ft above the surrounding country. The central portion of the Pocos de Caldas highland is characterized by gently undulating topography, with generally sluggish drainage, and is surrounded by a rim of hills rising above 1000 ft above it. In cross section the highland resembles a truncated cone with a depressed central area. The rim has been sculptured into a more prominent and abrupt topographic pattern than the central area, and streams that are of low to moderate gradient in the central plateau plunge over the rim in a spectacular series of cascades and falls. GEOLOGIC SETTING The Pocos de Caldas highland owes its physiographic expression mainly to the differential erosion of a complex intrusion of alkalic rocks into gneiss and sandstone. Erosion was guided somewhat by faulting. The highland is almost circular, and its limits, except in one locality, coincide with the periphery of the intrusion. The alkalic intrusions largely control its shape and extent, aided by some subsidence through faulting of the central portion. The mountainous rim of chilled phase, the later intrusions, and the indurated intruded rocks have resisted erosion more effectively than the central portion of the intrusion, which is composed of more coarsely crystalline alkalic rocks that form a central basin in the highland. Gneiss and sandstone are found coincident in elevation with the topographically highest intrusions. BAUXITE TYPES Most of the bauxite, which varies in physical type, is on the top and steep slopes of the northern rim. The only alumina mineral is gibbsite, definitely crystalline but iron-stained unless of secondary origin. Clay particles occurring with the bauxite are kaolinite. Some types of bauxite are an index to their origin. There are four general physical types of bauxite or bauxite laterite: 1) Surface Rubble: This partly nodular and partly fragmented type, usually less than 3 ft thick, results from surface weathering of massive bauxite or may form by superficial enrichment of nodular bauxite with a clay matrix when the interstitial clay is removed by surface runoff.

Jan 1, 1960

By P. R. Swann, J. G. Parr

Quenched structures were studied in alloys containing up to 12.5 pct cobalt. The subsequent decomposition of a 10 pct cobalt retained-ß phase alloy was investigated using metallographic and X-ray diffraction methods. Hardness measurements also were made during the decomposition process. Precipitation of Ti2Co is by nucleation and growth; and an activation energy of 50,000 cal per mole was determined. The values of the coefficient ß suggest that the precipitate is pearlitic at temperatures between 450 and 475°C, and spheroidal between 500 and 525°C. THIS paper describes part of a series of invesligations into phase transformations in binary alloys of titanium with transition elements. The general approach is similar to that taken in work on titanium-iron and titanium-nickel alloys.' Previous investigators'' have established the titanium-rich end of the titanium-cobalt phase diagram, reproduced in Fig. 1. Orrell and Fontana' showed that alloys containing more than about 6 pct" cobalt quenched from the ß range, produced 100 pcl retained-p phase. The isothermal decomposition of alloys containing between 0.8 pct Co and 15.5 pct CO was investigated by the same workers in the temperature range 650 to 1000°C. They reported that these alloys transformed into a or Ti,Co depending on the cobalt content, but no quantitative data were given. In the work to be described a series of alloys containing 0.8 pct Co to 12.5 pct Co was examined in the quenched condition. The 10 pct Co alloy (the lowest cobalt content to retain 100 pct ß on quenching) was selected for further work on the tempering kinetics of the ß decomposition. Experimental Procedure Since our own melting equipment was not installed at the outset of this work, the Physical Metallurgy Division of the Department of Mines and Technical Surveys (Ottawa, Canada) prepared the alloys. These were made of Japanese sponge, (which when melted had a value of 103 DPH, using a 1-kg load), and electrolytically prepared cobalt. The al- loys, made up to contain 0.8, 1.6, 3.3, 5.8, 8.3, 10.0 and 12.5 pct Co, were homogenized by swaging into rods at 900°C. Filings were taken from the rods, and any iron chips from the file were separated magnetically. Size fractions of both plus and minus 200 mesh (about 75p) were shown by their constitution, after annealing just below the eutectoid temperature, to contain the same cobalt content. Consequently, it was permissible to use the —200-mesh fraction, knowing it to be representative of the rod composition. Quenching in argon was carried out in a newly designed furnace, whose features include (1) an Inconel furnace tube, (2) a positive pressure of argon maintained at all times in the furnace—even when a sample is removed or inserted. The furnace is shown in Fig. 2 and is described in the Appendix. The tempering processes were carried out on powder samples sealed in evacuated quartz capsules. Since the highest tempering temperature was 525OC, no protection against reaction with the quartz was necessary. (Tests were made on filings of iodide titanium and showed no hardness increase after equivalent heat-treatments.) A thermocouple was attached to the capsule, which was heated to the

Jan 1, 1959

By R. E. Carter, C. Wagner, F. D. Richardson

By means of inert markers of radio-platinum, it has been shown that cobalt metal oxidizes by out-ward diffusion of cobalt atoms through the oxide. Oxidation rates have been measured at various temperatures and oxygen pressures and have been found to agree with the rates calculated from the Wagner equation and the authors' values for the diffusion coefficient of cobalt in the oxide. The distribution of radio-cobalt in growing oxide loyers has been accurately measured and found to be different from that predicted from the Wagner oxidation theory. Attempts have been made to measure the change of lattice parameter of the oxide with composition. SEVERAL investigators have shown that cobalt metal oxidizes according to the parabolic law,1-3 but no detailed study has been made of the oxidation mechanism. Cobaltous oxide has a metal-deficient lattice, but the defect concentration which is dependent on the oxygen pressure is only approximately known.' From the similarities in the structures of "CoO" and "FeO" and the rate laws governing the oxidation of cobalt and iron, Gulbransen- as suggested that cobalt, like iron," oxidizes by diffusion of cobaltous ions through the oxide layer. To substantiate this hypothesis, he has attempted to measure the oxidation rate of cobalt as a function of the oxygen pressure but has been able to report only that the rate depends on a "small" power of the pressure. On the other hand, Preece," Valensi,' and Arkharov' all have suggested from indirect evidence that oxygen diffuses through the COO to the metal-oxide interface. The present authors, in a previous paper,' have shown that the rate of diffusion of cobalt in cobaltous oxide is dependent on the oxygen pressure. In that investigation, they also found that cobaltous oxide disks made by complete oxidation of cobalt metal were porous at their centers (Fig. 5L, ref. 4). Both these facts strongly suggest that oxidation of the metal proceeds via outward diffusion of cations. In order to establish the mechanism unequivocally, oxidation experiments were made with inert radioactive platinum markers, and the dependence of oxidation rate on oxygen pressure was measured. In addition, an attempt was made to determine the form of the cation vacancy gradient, which the marker experiment showed must exist across a growing oxide layer. This was done by depositing radioactive Co on the surface of a cobalt disk and then measuring the tracer distribution across the oxide layer produced by partial oxidation of the metal. Finally, an X-ray examination was made in an attempt to find the expected change of lattice parameter of COO with oxygen pressure. Experimental The apparatus and materials used were substantially the same as those previously described by the authors.4 Marker Studies: The use of inert markers to follow oxidation reactions was first attempted by Pfeil" in 1929, and radioactive markers have recently been used by Davies et al.' In the investigation reported here, the markers were applied as an (NH4)2PtCI6 slurry in several thin streaks across both faces of four disks of cobalt metal 1 mm thick and 14 mm in diameter. The disks were then oxidized almost to completion at 1200°C in pure oxygen. After oxidation, they were mounted and sectioned and auto-radiographs were taken to locate the markers. Oxidation Rate: The oxidation rate of cobalt was measured at 1148°C at oxygen pressures ranging from 0.0055 to 1.0 atm and at 1000°, 1148", and 1350°C under 1 atm of oxygen. The rate was deter-

Jan 1, 1956

By Victor Formanek, Paul Chataignon, Maurice Rey

IT is found when floating oxidized lead ores by sulphidization, that the presence of calcium salts in the water, is usually detrimental and lowers the recovery. This effect is particularly marked in dry countries such as North Africa, where the waters often carry large amounts of calcium sulphate and where the ore may even contain gypsum. The effect of calcium salts is readily visible. Whereas in their absence cerussite is quickly stained brown and then black by sodium sulphide, in their presence the mineral remains very light in color. A similar effect is produced when barium sulphide is used as a sulphidizing agent instead of sodium sulphide. Magnesium salts have little or no effect and even tend to reduce the detrimental effect of calcium salts. A study of this phenomenon indicates that it is due to the precipitation of calcium or barium carbonate in contact with the mineral simultaneously with the formation of lead sulphide. The chemical reactions can be interpreted as: PbCO3 + Na2S = PbS + Na2CO3 CaSO4 + Na2CO3 = CaCO3 + Na2 SO4 They might also be written: PbCO3 + S = + Ca++ = PbS + CaCO3 The precipitation of calcium carbonate can be followed by the lowering of the pH with which it is accompanied. Magnesium carbonate is more soluble than calcium carbonate and usually does not precipitate under the conditions prevailing. It is interesting to note that calcium salts have no effect on anglesite (lead sulphate) because calcium sulphate is soluble, but barium salts hinder the sulphidization of anglesite because of the precipitation of barium sulphate. Remedies When calcium sulphate is present in large amounts, the softening of the water with soda ash is usually too expensive to be considered, but the precipitation of the objectionable calcium carbonate can be prevented in two different ways. One is the use of sodium hydrosulphide instead of sodium sulphide. This salt gives a lower pH than sodium sulphide and does not bring about the immediate precipitation of the calcium which remains in solution as calcium bicarbonate. The other procedure is to add ammonium salts such as the sulphate or chloride which have the property of increasing markedly the solubility of calcium carbonate. Ammonium salts have other effects such as cutting down conditioning time and accelerating flotation. They should be added to the flotation cells rather than to the ball mills. Table I. Effect of Sodium Hydrosulphide and/or Ammonium Sulphate on the Flotation of Two Oxidized Lead Ores Mibladen Ore4 La Plagne Ored Con- Tall- Con- Tail-centrate ing centrate ing Reagents Pb, Pct Pb, Pct Pb, Pct Pb, Pot Without addition of CaSO, NaS 56.0 0.68 43.4 0.65 NaSH 56.2 0.60 40.4 0.50 Na2S + (NH4)2SO4d 54.6 0.56 NaSH + (NH4)2SO4d 43.0 0.66 With addition of 40 lb/ton CaSO4 Na2S 39.4 3.85 34.0 3.21 NaSH 49.1 0.70 49.6 0.88 Na2S + (NH4)2SO4d 53.9 0.85 NaSH + (NH4)2SO4d 51.0 0.45 41.1 0.78 In table I are given the results of representative tests on two different oxidized ores. They show that the strongly detrimental effects of calcium sulphate can be offset by the two procedures outlined above. Sodium hydrosulphide is now used regularly on a mill scale on certain ores. Tests are being carried out with ammonium salts. It should be noted that malachite is subject to influences similar to cerussite. One final word of caution—when the ore is rich in primary slime, which is flocculated by the calcium salts, it may be indispensable to remove these by washing or precipitation with sodium carbonate instead of keeping them in solution by the above methods. Acknowledgment We wish to thank Socibtk Miniere & Metallurgique de Penarroya and Minerais et Metaux, for permission to publish these results.

Jan 1, 1951

By D. R. Hay, E. Scala

STUDIES of structure-sensitive properties, especially mechanical behavior, have shown that grain and subgrain structure play an important role. The mechanical properties of tungsten, in particular, are sensitive to the nature of the intergranular structure. Substructure and dislocation networks in single-crystal and polycrystalline tungsten have been studied by Nakayama et al.' Various orders of substructure were observed ranging from a microscopic first order (grain diameter: 2 to 8 mm) to a microscopic second order (grain diameter: 50 to 300 p), and, within the latter, dislocation networks forming an even smaller order of substructure. In their single crystals, grown by arc fusion, the degree of misorientation in each order was small: 16'3OU, -11, and -10" for the first-, second-, and third-order substructure, respectively. To study the properties of polycrystalline tungsten, powder metallurgy tungsten is generally used. However, in a mechanical property investigation, the zone-melted or arc-fusion crystals are more desirable than the powder metallurgy product due to their higher purity and absence of porosity and other defects inherent in consolidation by powder metallurgy. Grain boundaries can also be produced in melted stock by working and recrystallizing. However, material with subgrain mis orientations of the order of several degrees (high-angle substructure) has not been reported previously and is the subject of this communication. Crystals were grown by electron-beam, floating-zone melting. The starting material, Sylvania Pure-tung welding rod, was given one zone pass at a traversal rate of -2 mm per min. Through control of the zone temperature, it was possible to influence the degree of crystal perfection. By maintaining the zone at a high degree of superheat, high-perfection crystals could be grown. However, at temperatures only slightly above the melting point, the zone-melted crystals contained a high-angle substructure. A sensitive control of the zone temperature was not possible due to the difficulty of estimating the temperature of the zone and of providing a constant supply of power to the sample. Therefore, an empirical method, using the shape of the molten zone as a criterion, was adopted as an indication of temperature. At high degrees of superheat, the surface tension of the molten zone decreases and a neck forms at the top of the zone, whereas at low zone temperatures the diameter of the zone remains reasonably uniform. Although it was not possible to obtain a continuous variation of misfit angle, the conditions could be directed toward the growth of either high- or low-angle substructure by maintaining only a slight neck in the zone (sufficient to establish that it was molten) or a well-necked zone, respectively. Mass spectrographic analyses of both types of material revealed no significant differences in the concentrations of their impurities. The degree of misorientation at high angles was obtained by measuring the angular spread of spots corresponding to a single reflection on a Laue back-reflection photograph. Fig. 1 shows a typical Laue back-reflection photograph of a crystal with a 3-deg spread. By measuring the angular deviation of the spots corresponding to a single reflection from the mean center of the spots around which constant angular deviation contours were drawn, an average angular spread of misfit could be calculated. The angular average was weighted by the number of spots observed in each angular interval. At angles greater than 5 to 6 deg the spots from different reflections begin to overlap, and cannot be associated with a particular reflection. Laue back-reflection photographs taken at different locations on samples .with approximately 3-deg spreads showed only a small difference in angular misorientation, less than 8' of arc, within individual specimens. The microstructure was examined using Berg-Barrett X-ray extinction contrast microscopy. Berg-Barrett photographs taken directly on the as-grown surface, Fig. 2, show an essentially equiaxed subgrain structure of -0.1 mm in average grain diameter in both high- and low-angle crystals. Fig. 2(a) is a photograph of a sample with a low misfit angle and Fig.

Jan 1, 1968

By Maurice Rey, Victor Formanek, Paul Chataignon

IT is found when floating oxidized lead ores by sulphidization, that the presence of calcium salts in the water, is usually detrimental and lowers the recovery. This effect is particularly marked in dry countries such as North Africa, where the waters often carry large amounts of calcium sulphate and where the ore may even contain gypsum. The effect of calcium salts is readily visible. Whereas in their absence cerussite is quickly stained brown and then black by sodium sulphide, in their presence the mineral remains very light in color. A similar effect is produced when barium sulphide is used as a sulphidizing agent instead of sodium sulphide. Magnesium salts have little or no effect and even tend to reduce the detrimental effect of calcium salts. A study of this phenomenon indicates that it is due to the precipitation of calcium or barium carbonate in contact with the mineral simultaneously with the formation of lead sulphide. The chemical reactions can be interpreted as: PbCO3 + Na2S = PbS + Na2CO3 CaSO4 + Na2CO3 = CaCO3 + Na2 SO4 They might also be written: PbCO3 + S = + Ca++ = PbS + CaCO3 The precipitation of calcium carbonate can be followed by the lowering of the pH with which it is accompanied. Magnesium carbonate is more soluble than calcium carbonate and usually does not precipitate under the conditions prevailing. It is interesting to note that calcium salts have no effect on anglesite (lead sulphate) because calcium sulphate is soluble, but barium salts hinder the sulphidization of anglesite because of the precipitation of barium sulphate. Remedies When calcium sulphate is present in large amounts, the softening of the water with soda ash is usually too expensive to be considered, but the precipitation of the objectionable calcium carbonate can be prevented in two different ways. One is the use of sodium hydrosulphide instead of sodium sulphide. This salt gives a lower pH than sodium sulphide and does not bring about the immediate precipitation of the calcium which remains in solution as calcium bicarbonate. The other procedure is to add ammonium salts such as the sulphate or chloride which have the property of increasing markedly the solubility of calcium carbonate. Ammonium salts have other effects such as cutting down conditioning time and accelerating flotation. They should be added to the flotation cells rather than to the ball mills. Table I. Effect of Sodium Hydrosulphide and/or Ammonium Sulphate on the Flotation of Two Oxidized Lead Ores Mibladen Ore4 La Plagne Ored Con- Tall- Con- Tail-centrate ing centrate ing Reagents Pb, Pct Pb, Pct Pb, Pct Pb, Pot Without addition of CaSO, NaS 56.0 0.68 43.4 0.65 NaSH 56.2 0.60 40.4 0.50 Na2S + (NH4)2SO4d 54.6 0.56 NaSH + (NH4)2SO4d 43.0 0.66 With addition of 40 lb/ton CaSO4 Na2S 39.4 3.85 34.0 3.21 NaSH 49.1 0.70 49.6 0.88 Na2S + (NH4)2SO4d 53.9 0.85 NaSH + (NH4)2SO4d 51.0 0.45 41.1 0.78 In table I are given the results of representative tests on two different oxidized ores. They show that the strongly detrimental effects of calcium sulphate can be offset by the two procedures outlined above. Sodium hydrosulphide is now used regularly on a mill scale on certain ores. Tests are being carried out with ammonium salts. It should be noted that malachite is subject to influences similar to cerussite. One final word of caution—when the ore is rich in primary slime, which is flocculated by the calcium salts, it may be indispensable to remove these by washing or precipitation with sodium carbonate instead of keeping them in solution by the above methods. Acknowledgment We wish to thank Socibtk Miniere & Metallurgique de Penarroya and Minerais et Metaux, for permission to publish these results.

Jan 1, 1951

By A. D. Marlin, A. J. Gentile, E. F. Jordan

Metallurgical changes in SAE 52100 ball-bearing components resulting from overload testing are described. Changes in microstructure, hardness, and resiclctal stresses crre discussed zuitlz re.ference to material cleanliness obtained by various steel-melting practices and are compared with work by otlzer investigators. Evidence is presented to show that the initialion and development of microstruc-tural alterations are characterized by two separate reactions: the appeavance of a "dark etchingJ' constituent, and "gray lines" or a light etclzing constituent. The dependency of these tzvo reactions on material cleunliness, running tirne, and contact stresses is discussed and a failure mode related to material cleanliness and microstructural transformation is proposed. THE study of ball- and roller-bearing contact fatigue has been paced by a strong emphasis on bears ing application performance. Particular attention has been paid to conditions that effect the spalling-type failure that is characteristic of rolling contact fatigue in through-hardened components. Some of the conditions investigated are lubrication and atmosphere,1-3 material characteristics and finish,475 and speed and design fa~tors."~ A typical spalling-type failure is shown in Fig. 1. The arrow shows the motion of the ball relative to the inner-ring race surface. The leading edge of the spall is usually sharper than the trailing edge. The race surface near the trailing edge also shows small dents caused by debris from the spall. In this type of testing very little metallurgical investigation is done on failed bearings. Emphasis is placed on test conditions and statistical analyses of endurance data. More basic work has been done relating micro-structural changes to fatigue performance. Dyer" and Wood, Cousland, and sargant9 have used mostly simple materials, such as single crystals and single-phase polycrystalline specimens, under simple alternating strain to identify a systematic process of fatigue damage. drutowski" was concerned primarily with the relationship between steel structure, contact stress, and energy losses in rolling contact. dones11 and Bush, Grube, and Robinson12 utilized changes in microstructure and residual stress in overload-tested rolling contact elements as a means of investigating the fatigue process. Work is being done on an ASME-sponsored contract,13 using both simple and complex materials, but there is still a long way to go before such theories as pore and void growth in simple structures can be applied to the relatively complex bearing steel microstructure. The purpose of this paper is to report on an investigation into the effect of steel cleanliness on the structural alteration and residual stress changes found in overload-tested ball bearings. Using these results and those of previous investigators, we will propose probable failure mechanisms in both overload- and normal load-tested ball bearings.14,15 PROCEDURE Ball bearings? 3208 size, were fabricated from SAE 52100 steel obtained by five different melting practices. The melting practices, chemistry, and inclusion ratings for the five lots of steel are summarized in Tables I and 11. The nonmetallic inclusion ratings were determined by the Jernkontoret method described in ASTM E45-51 Method A. This technique consists of microscopically examining a series of polished samples taken from specified locations in the ingots, billets, or bars. Each sample is surveyed at XlOO magnification and the inclusion types and sizes are compared to standard fields. Because of the nature of these ratings all values in Table I1 are rounded to the nearest half. The elec-

Jan 1, 1965

By R. G. Knickerbocker, W. E. Brown, G. J. Vahrenkamp, M. M. Fine

THE results of a research and development laboratory and pilot-plant mineral-dressing investigation by the Bureau of Mines of the complex copper-lead-cobalt-nickel ores of southeast Missouri are reported in this paper. This investigation, in cooperation with the National Lead Co., showed that separate concentrates of lead, copper, and cobalt-nickel could be made by fine grinding and flotation. An industrial plant built subsequently by the St. Louis Smelting and Refining Div. near Fredericktown, Madison County, Mo., produced such concentrates during the war years. Present commercial production at the mill is limited to lead and copper concentrates, but research to permit economic utilization of the cobalt and nickel values is continuing. The complex sulphide deposits near Frederick-town in Madison County, Mo., have an operating history that dates back to the years preceding the Civil War. Perhaps these operations can best be summarized in terms of output which are given by Tyler: "Previous to 1900, the Mine la Motte Co. shipped cobalt ore to Swansea and in 1903 produced 120,000 pounds of oxide in a Missouri plant. Another cobalt refinery erected in 1906 by the North America Lead Co. at Fredericktown, Mo., operated intermittently until 1910. In 1909 it produced 83,384 pounds of cobalt oxide, 328,403 pounds of nickel, 8,314 tons of nickel-cobalt concentrates, 600 tons of copper concentrates, and 1,353 tons of lead concentrates. This plant was purchased at a forced sale in 1915 by the Missouri Cobalt Co., which produced a certain amount of oxide in 1918 and in 1920 recovered 102,410 pounds of cobalt oxide and cobalt hydrate, valued at $262,810." According to Buehler,2 "The ore, which consists of a complex mixture of the sulphides of cobalt, nickel, copper, lead, and iron, occurs at the contact of the pre-Cambrian porphyry and the overlying Lamotte sandstone and Bonneterre dolomite." The source of most of the cobalt and nickel is siegenite, a member of the linnaetite series of minerals. Its composition is variable, and although the chemical formula may be given as (CoNi),S,, it usually contains both iron and copper. The siegenite is characterized in this instance by an intimate association with chalcopyrite, and to a lesser extent with iron sulphides. Galena, on the other hand, while dis- seminated throughout the ore, is not closely bound to other constituents. Gangue is composed essentially of dolomite and quartz. Petrographic examination showed that fair liberation of sulphides and gangue could be attained at — 100 mesh. Complete liberation of micronsize inclusions, particularly of sulphides in each other would not have been possible at —400 mesh. Beneficiation Studies Many samples of the southeast Missouri ore were tested, but most of the work was confined to five samples of churn drill cuttings weighing 15 tons. The samples were reportedly representative of five sections of the deposit and were tested individually and as a composite. Only the results of the tests on the composite, which contained 1.28 pct lead, 2.03 pct copper, 1.06 pct nickel, 0.87 pct cobalt, 3.57 pct iron, 15.4 pct lime, and 23.9 pct silica, are presented in this report. In view of the rather complex and intimate association in the mineralogical composition of the ore, flotation was the logical choice in the selection of a beneficiation process. Other mineral dressing unit operations were considered as an adjunct to flotation, but none were beneficial. Many tests were made on these samples to determine the flotation characteristics of the mineral siegenite. As a result of this work, it was noted the siegenite was intermediate in floatability between chalcopyrite and galena on one extreme and iron sulphides on the other. The difference in floatability between siegenite and the iron sulphides was not very great and, in general, the same reagents that depressed pyrite and marcasite would also, in slightly larger quantities, depress siegenite. This tendency for siegenite

Jan 1, 1952

By Strathmore R. B. Cooke, Paul B. Queneau

The kinetics of the dissolution of scheelite in basic solutions of carbonate and fluoride were investigated. Work was also done with solutions of alkali metal chloride, hydroxide, phosphate, and mixtures of phosphate and fluoride. The study was conducted at 90 psig and at temperatures ranging from 100" to 155"C, and both natural and synthetic scheelite single crystals were used. The interaction of scheelite with carbonate solutions generally followed a parabolic rate law, and resulted in the formation of calcite crystals on the attached surface. The transport of the CO3 through the calcite to the scheelite surface was probably rate -controlling between 115" and 135°C. Positive deviations from Parabolic behavior were observed at 100" and 155?C, presumably due to the calcite grain growth, and to the formation of a noncoherent calcite layer, respectively. The leaching of scheelite with alkaline fluoride solution produced a calcium fluoride reaction-product which covered the surface as a sheet-like layer. Below 110°C the dissolution rate was parabolic; at 115" and 135°C it was linear. In the linear region, the periphery of the calcium fluoride layer lifted from the sample. Only the lower layers, braced by the scheelite substratum, remained unbroken. This bound layer, approximately constant in thickness, limited the rate at which the fluoride could attack the scheelite. The phosphate and phosphate-fluoride leaches dissolved scheelite at a linear rate; solid reaction products were respectively hydroxyapatite and fluorapatite. Sodium hydroxide and chloride were not effective leachants, and did not produce observable solid reaction products. THE feasibility of pressure leaching of scheelite pulps with basic solutions containing either carbonate or fluoride ions, as indicated by the following equations, has been established by previous investigators:1-3 200°C CaWO4s + CO37q - CaCO3s+WO4aq [1] 200°C CaWO4s + 2Faq ^ CaF2s+WO4aq [2] It is to be noted that a commercial process employing reaction [I] is in use at Union Carbide's operation near Bishop, Calif. In the earlier work referred to, it was apparent that the precipitation of the solid reaction-product on the scheelite particles sharply reduced contact of the leachant with the scheelite. We have extended this work by studying the kinetics of dissolution employing single crystals of scheelite of known exposed surface area. In addition, the effectiveness of solutions of phosphate, of phosphate with fluoride, and of chloride and hydroxide as leachants for scheelite have been investigated. EXPERIMENTAL Apparatus. The low-pressure autoclave used in this wo (100 psig maximum) is essentially that of J. Halpern4 as modified by F. A. Forward.5 Constructed entirely of 316 stainless steel, its maximum capacity is 4000 ml. The temperature in the autoclave was regulated to *0.5?C by a Wheelco thermocouple controller. A 4-in. diam, three-bladed impeller, circulated solution upward against the sample, and a strobo-scope permitted holding the stirring rate to *15 rpm. A check valve and a "pop" type safety valve were installed, a sample holder was fixed to an externally adjustable rod, and a water-cooled condenser was placed in series with the sampling valve. The stainless steel sample holder, Fig. 1, held the epoxy-mounted sample (f) five mm above the impeller. Tightening the tapered sleeve (d) positioned the epoxy-resin specimen-mount by forcing it back against the spacer (c). The mount (e) was 1 in. diam. Sample Description and Preparation. Both synthetic and natural scheelite crystals were leached. The former were single crystals of 99.95 pct purity which were leached approximately perpendicular to the "c" axis; they were supplied by the Gallard-Schlesinger Chemical Manufacturing Corp. The natural crystals, supplied by Minerals Unlimited, were transparent, analyzed 99.8 pct CaWO4, and in ultraviolet illumination exhibited the characteristic blue glow of substantially molybdenum-free scheelite. To permit exposure of an essentially constant surface area of scheelite to the leachant, the samples were mounted in Scotchcast Brand Resin No. 250 (Minnesota Mining and Manufacturing Co.). The mount-

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Jan 1, 1950