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By A. B. Dyes

In the operation of a water-driven reservoir, a free gas saturation can he established by maintaining production rates fast enough to cause the reservoir pressure to decline below the bubble point. The benefit of such a procedure on the displacement efficiency of the oil by water is illustrated for two types of sandstone samples from one reservoir. Those rock samples showing the poorest recovery to water drive in the absence of a free gas saturation give the most improvement in the presence of a free gas saturation. Employing one type of reservoir fluid (low .shrinkage) the benefit of evolved gas on oil displacement is calculated at several reservoir pressures below the bubble point. This demonstrates the presence of air optimum pressure for water displace,rnent which is .several hundred pounds per .square inch below the bubble point. Displacement of oil at the optimum pressures results in the removal of 7 to I? per cent more oil than would be obtained by displacement at the bubble point pressure. In some instance. this magnitude of increase may be worthy of consideration in establishing the maximum efficient rate of production from many water-driven fields. INTRODUCTION For many years the belief that the use of gas could be combined with that of water to result in a better recovery operation than the use of either of these phases alone has been prevalent in the oil industry. This is evidenced by the several field trials which have employed the injection of gas and water in combination.1.2.v In most cases the small amount of any additional recovery, in combination with the limited knowledge available on the older reservoirs, has left uncertain the influence of gas on recovery in these earlier attempts to combine the use of gas with water. Research studies in recent years have demonstrated through laboratory. floods the magnitude of the benefit of the presence of gas on the displacement of oil from sandstones by water.5,6,7,8,9,10,11 In addition, studies of the distributions of the phases which are present during the displacement process have developed concepts concerning the mechanism by which this benefit is obtained."." It now remains for the engineer to incorporate these findings into the general technology of reservoir operations. It is the purpose of this paper to illustrate that the production of a water-driven reservoir at pressures below the bubble point is one such operation whereby improved oil displacement efficiency can be obtained as a result of gas evolution. The establishment of a gas saturation by evolution of dissolved gas was one of the techniques used by several investigators in the laboratory studies. The possibility of obtaining the benefit of gas evolution in water-driven reservoirs by producing at pressures less than the bubble point has 3150 been pointed out previously." The desirability of this operation has undoubtedly

Jan 1, 1955

By Richard F. Link, George S. Koch

Advantages and disadvantages of deflecting (wedging) diamond-drill holes to obtain sampling data are compared with the alternative of drilling additional holes. The discussion is based on a statistical analysis of a large set of deflection data from exploratory boreholes in South African gold mines. Representative cost comparisons show the conditions under which deflections are likely to be desirable.

Jan 1, 1969

Jan 1, 1933

By F. B. Sherman, Keros Cartwright

Sanitary land filling has become one of the most widely used methods of disposing of solid refuse. A principal concern of regulatory agencies and the public itself is that landfill operations do not degrade the physical environment, including water resources, and the ground-water reservoir in particular. Knowledge of ground-water and engineering geology can guide landfill operations into suitable terranes or develop measures to compensate for natural limitations at a particular site. Experience and research in Illinois suggest four activities relating to landfill disposal that warrant attention by geologists and engineers: (1) regional delineation of favorable and unfavorable hydrogeologic conditions to facilitate planning and preliminary screening of potential landfill sites; (2) site evaluations, with considerations of geologic materials, topography, water levels, flow systems, and local occurrence and use of water resources; (3) research on aspects of the hydrogeologic environment that control effects of, or are modified by, landfills; and (4) formulation of practices in the siting, construction, and operation of landfills that prevent, mitigate, or isolate deleterious effects. The first two activities are basically in the domain of earth science, requiring the application of fundamental concepts of geology and hydrology and conventional site-exploration methods. The third activity, research, requires contributions from geology as well as other disciplines, including soil physics, sanitary engineering, and chemistry. The fourth calls for policy decisions by regulatory agencies and elected officials, using the contributions of scientists and engineers. Throughout history, man has disposed of unwanted materials by dumping. As urbanization has increased, haphazard dumping practices have given way to disposal under more controlled conditions because of increasing congestion of population and production of waste and greater concern for public health and environmental amenities. Many states and communities have already outlawed open dumping and open burning of refuse. The only practical methods of disposal of large volumes of refuse, therefore, are contained, high-temperature incineration, or burial in a sanitary landfill. In Illinois, regulation of solid waste disposal has been delegated to the Environmental Protection Agency. Each session of the legislature since 1965 has passed increasingly strict laws regulating waste diposal. As a result, the work of evaluating sanitary landfill sites has increased significantly for both the Department of Public Health, now the Environmental Protection Agency, and the Illinois State Geological Survey, which advises the Agency on matters of ground-water geology and pollution. In fact, our ground-water staff spends as much time on studies relating to waste disposal, primarily sanitary landfills, as on ground-water resource studies. Many other geological agencies are experiencing similar demands for increased assistance in solving waste-disposal problems. This paper summarizes some of the salient features of the sanitary landfill concept, describes activities of the Illinois Geological Survey in ground-water and engineering geology relating to landfills, and suggests policies that need consideration. A sanitary landfill is located and operated in such a way that vermin and pests, nuisances, and degradation of air and water are kept at acceptable levels. Some of the physical requirements of a sanitary landfill are all-weather roads for year-round access, fences to retain blowing paper, a daily cover of at least six inches of suitable earth material, and a final cover of at least 2 ft of earth material. Dumping into or adjacent to standing water generally is not allowed. Two common operating techniques are used. In the first, trenches are dug, the refuse is placed in them, and the earth removed from the trenches is used to cover the waste. In the second method, area fill, refuse is placed in low ground and covered with earth from adjacent high areas. The hydrology of the site is a prime consideration in locating sanitary landfills. Putrescible refuse, if saturated above field capacity, produces a leachate that usually has a high concentration of dissolved solids.2 As the leachate also acts as an agent for transporting bacterial pollutants, it constitutes a potential pollution hazard. To reduce the production of leachates, the topography of the landfill area should be such that surface water will not flow into or through the fill. Operations that will result in refuse disposal below or near the highest known water-table elevation may be required to take corrective or preventive measures to protect the ground water. In practice, under humid conditions such as prevail in Illinois, locations where disposal can take place above the water table are relatively few because surficial materials are commonly fine-grained, which permits slow gravity drainage and results in high degrees of saturation (100% moisture content) near the surface. At some sites, although disposal has taken place above the water table, ground-water mounds have developed, resulting in permanent saturation of the refuse. Permeability barriers usually are required to protect the ground-water reservoir from degradation by leachates. The convention in Illinois is to have a minimum of

Jan 1, 1972

Jan 1, 1934

By H. Furman Byars

INTRODUCTION of bottom dump hauling units into the Ray, Ariz., stripping operation of the Isbell Construction Co., was motivated by several reasons, with what appears to be debatable results. The accepted theory of truck design for use in open-pit holds that end dump vehicles are the most adaptable for the work. But, because operations of the bottom dump, under certain construction and haulage conditions, proved economically feasible, the unit was put to work in the Ray copper pit. The decision to try bottom dump was reached after considerable observation of the unit in action on construction of earth filled dams, levees, airport construction and several other similar tasks. Basic tire design also motivated the choice. All things being equal, a vehicle running on low pressure single tires will outperform another operating on dual high pressure tires, providing load carrying capacities are the same. The investment required to equip a vehicle with four single tires to handle the same load as one with dual tires mounted on two axles and single front axles is about 60 pct greater. Thus, in order to reach the break even point on tire costs, single tires must operate 60 pct longer. Comparison is made with a truck outfitted with 10 16:00x25 tires. Two other factors were considered in selecting bottom dump trucks. It was felt the bottom dump principle would work well in dumping ore into a hopper where gate design fits this particular method. Also, with the absence of hydraulic dumping, ore pollution with oil is reduced. The mechanical simplicity of the unit also lent weight to its choice. Ordinary reasoning indicated maintenance costs would be low compared with other units carrying similar loads. The bottom dumping principle is not new. It dates back to the days when horses were used to haul the same kind of rig. The unit employed at Ray holds 25 cu yd struck measure, or approximately 42 short tons. Dumping is accomplished by releasing an air cylinder opening a dog holding the doors. Doors are closed by a cable system operating off a wheel wind deriving power by friction with the trailer tire. The unit is mounted on four 27.00x33 and two 14.00x24 tires on the front axle. The power unit is a 300 hp Cummins engine. Hydraulic power boosts the steering. A straight mechanical drive and friction clutch with 10 speeds is used. Conditions Not Ideal Top performance of the truck can be expected only under the conditions for which it was designed, in particular grades under 5 pct, handling fine material, and dumping where one thin layer can be placed on top of another. The machine will handle 42 tons per haul, operating at high speed, with only seconds used for dumping. On a 2 or 3 pct grade over a one mile haul,

Jan 1, 1952

By William Loblowitz

A simplified system of flotation testing has been developed recently at the Bureau of Mineral Research of Rutgers University. The technique involves the known principle of skin flotation and can be used with minute quantities of sample and reagents in a beaker. A vessel containing the conditioned sample with added water and flotation reagents is held inclined and rotated slowly. Water-repellent particles come in contact with air and float on the surface of the liquid, while wettable particles are submerged. The float is poured off and filtered whereas the nonfloat remains in the beaker. The filtrate may be returned to repeat the process. This procedure can be made quantitative. Separations are obtained and are remarkably complete and repeatable. The effect of different reagents, optimum quantities, pH and other variables can be determined in a fraction of the time required for conventional testing. However, the method gives no information on the effect of frothers and the quality of froth to be expected in a cell, and it is not practical for particles finer than 200-mesh. Unlike other preliminary tests, separate float and nonfloat products are obtained, and their contents can be determined quantitatively by chemical analysis or grain counts. After the optimum reagent combination has been determined, the effect of fines and frothing may be verified in the conventional flotation cell. On the other hand, agglomeration-tabling can be directly duplicated from beaker tests. Procedure: Five to ten grams of sample are weighed into a 100-ml beaker. Flotation reagents and a small initial quantity of water are stirred together; additional water is then added to produce the proper water-solids ratio. The beaker is then tilted to 45" and rotated slowly. After three to five rotations, liquid and float are poured off and filtered; the filtrate may be recycled until the separation is completed. One test generally requires less than 10 min. Reagent concentration and pH remain quite constant because of the recycling of the filtrate. Two to four tests may be made simultaneously, and the effect of varied conditions may be observed by comparison. Considerable time is saved in preparation and handling since small quantities of sample suffice for a series of systematic tests. Repeatability One test was repeated four times under constant conditions. The sample used was a quartz sand containing approximately 24 pct feldspar and some clay aggregates. The +28-mesh grains had been screened out, and most of those finer than 100-mesh had been removed by hydraulic classification. The results are presented in Table I. For comparison, 500 g of the sample were separated by agglomeration-tabling using the same reagent combination and quantities as given in Table I. The weight percent float was 18.3 pct, composed almost entirely of feldspar and with only traces of quartz. Most of the remaining feldspar was recovered in a middling product with 2.2 pct by weight.

Jan 1, 1952

By Forrest F. Craig

Both early and more recent1 laboratory measurements of gas-oil relative permeabilities were made by subjecting oil-saturated cores to external gas drives. In these runs it was generally assumed that the flowing gas/oil ratio was constant at every point throughout the core. Using this assumption, the resulting equation for the gas-oil relative permeability ratio becomes A where Q is the flow rate at the producing end of the system. This relative permeability was then specified for the average saturation of the core. The assumption and resulting equation fail to recognize that in an external drive, the oil flow rate varies from zero at the injection end to a maximum at the producing end. The assumption also fails to consider the existence of a saturation gradient during an external drive. This saturation gradient is due solely to non-steady-state flow. Some authors2,3,4 have used this erroneous method of calculating relative permeability ratios from external drives. Other authors5,6,7 have used relative permeability ratios in calculating expected field performance by external drive, using Equation (1) and making the incorrect assumption that the saturation is uniform within the driven portion of the reservoir. To find the correct relation between the relative permeability. ratio at the average saturation and the produced gas/oil ratio, the insertion in Equation (1) of a factor, F, to adjust it for oil velocity gradient has been considered. The equation then takes the form Assuming that the oil velocity is directly proportional to the distance from the injection point leads to the conclusion that, for a linear system, the average oil velocity is one-half that at the producing end. Thus, the average gas/oil ratio is twice the produced gas/oil ratio, and Equation (2) is transformed into However, here again the existence of a saturation gradient is not recognized. The produced gas/oil ratio is related to the relative permeability ratio at the saturation of the outlet end of the system. It can be shown quite readily that, if the true log k,/k, saturation relationship is linear over small ranges of saturation, then d log kjko Where aaxv and u2 are the average and outlet saturations, respectively. Examination of Equation (3) shows that the factor F cannot have a single value over the whole saturation range. Another method of dealing with external drives is that of Buckley and Leverett.' Their method, which assumes no gas expansion and outlet end effects, considers fully the saturation gradient present due solely to the displacement mechanism during an external drive, and applies Equation (1) to each point along this gradient. The calculation of production history using relative permeability ratio is straightforward. However, the calculation of relative permeability ratios from production history by this method is impractical. In a recent paper, Welge,1 using an approach similar to that of Buckley and Leverett, presents a simplified method for determining the saturation at the producing end of the system. At thi; saturation, the relative permeability ratio calculated by Equation (1) applies exactly, after breakthrough of the stabilizej front. By this method, relative permeability ratios or production history may be calculated with equal ease. Use of this method as a laboratory tool in determination of relative permeability ratios by external drive requires the knowledge of the total injected fluid volume; in addition to the average saturation and producing ratio. As a preliminary test of this method of calculation, laborntory external gas drives were run on a 3% in. diameter, 11 in. long sample of Nellie Bly consolidated sandstone. This core sample had a permeability of 824 md and a porosity of 28.1 per cent. The driving fluid was air. Three different oils were used, having viscosities of 1.4, 9.8, and 125 cp, respectively. The runs were made under identical pressure differentials,

Jan 1, 1952

By G. B. Craig, G. L. Montgomery

A simple technique has been developed which reveals glide dislocations in zone-refined aluminum as etch pits. The technique has been tested quantitatively by making dislocation counts on aluminum single crystals deformed in pure bending. The method has the advantage of being insensitive to the orientation of the surface under examination. A number of etchants which will reveal dislocations in annealed aluminum have been reported.'-' These etchants apparently depend on decoration of the dislocations by an impurity (probably iron) and cannot, therefore, be used to reveal fresh glide dislocations. In addition, it is unlikely that screw dislocations will be etched because of their small attraction for impurity atoms. Amelinckx6 has reported that glide dislocations located along slip traces can be revealed by fluo-rated aqua regia. This work indicated that dislocations themselves, irrespective of decoration by impurity atoms, are responsible for the etch pits. However, as a result of additional etching experiments, Wyon and Marchin7 concluded that dislocations alone are not sufficient to explain the localization of etch pits on slip lines in aluminum using chemical etch-pitting techniques. In addition, their results show that glide dislocations are revealed only on surfaces approximately parallel to a (100) axis and that not all slip systems are attacked. These observations have been confirmed by the present authors. The technique described in this article is insensitive to the orientation of the surface, and reveals dislocations on all glide systems. Fig. 1 shows a deformed region in the neighborhood of a scratch. Dislocations can be seen along three slip traces. In the present work, single crystals of zone-refined aluminum are polished for from 2 to 5 min in a chemical polishing reagent held at 100°C, as described by Herenguel and second:' H2Sol 60 pct H3PO4 30 pct HNO3 10 pet The samples are then coated with a thin oxide film by annealing in air at 450°C for 1 hr and cooling in the furnace. After deformation, dislocation etch pits are developed by immersing the specimen in the same polishing solution which is now held at a temperature of 50°C. The formation of small hydrogen bubbles indicates that etching has occurred. The sample is immediately removed from the solution. Prolonged etching results in enlargement of the pits and, in regions of high dislocation density, the overlapping and loss of resolution of individual pits. It is the experience of the authors that contact with iron will ruinously contaminate the reagent. With careful etching, dislocations separated by half a micron can be resolved optically and the method has been shown to be sufficiently sensitive to reveal dislocations produced during the pre-easy glide region of deformation, Fig. 2. A few examples of glide-dislocation configurations, as revealed by this technique, are shown in Figs. 1 to 4.

Jan 1, 1964

With a mine output as high as 5000 tpd and mill capacity of 7000 tpd, the uranium mining and milling complex owned and operated by Kerr-McGee Nuclear Corp. in the Ambrosia Lake area is the largest in the U.S. and is likely to remain so for some time. Next year, Kerr- McGee expects to have in production another mine in Section 19 of the Ambrosia area-and will begin ore production in 1976 at its new $15-million mine at Church Rock, located northeast of Gallup, N. M., where the company has already completed the shaft work and is in the early stages of project development. Ore from Church Rock will be transported to the company's facilities at Ambrosia Lake for processing. Kerr-McGee's existing eight mines in Ambrosia Lake go to depths of about 800 to 1500 ft to tap the various horizons of uranium-bearing sands in the Westwater Canyon of the Morrison formation.

Jan 8, 1974

By M. Prats, D. G. Russell

The performance of a well in a bounded, layered reservoir with interlayer crossflow has been investigated mathematically. The system studied comprises a centrally located well in a bounded cylindrical reservoir composed of two layers of contrasting physical properties. The reservoir contains a single fluid of small and constant compressibility. In the case of a well producing at constant pressure, the production rate of the crossflow system declines exponentially after the early transient behavior dies out. For wells which produce with constant rate, the pressure-time relationship is linear following the transient. For very early production time, the production rate of the two-layer crossflow system behaves as that of the two-layer stratified system (the case in which the layers are in communication at the well only). Except for early time, in most practical cases the performance of a two-layer reservoir with cross-flow can be duplicated by that of a single-layer reservoir. The equivalent single-layer reservoir must have the same pore volume and the same drainage and wellbore radii as in the two-layer case. In addition, the equivalent reservoir must have a "kh" (permeability x thickness) product equal to the sum of the "kh" products of the respective layers in the crossflow system. If the porosity and permeability distributions are known, the production and pressure behavior of a well with and without crossflow can be predicted. From a comparison of the observed pressure or production performance of a well and the theoretical behavior, the occurrence of interlayer crossflow can be detected. INTRODUCTION When flow is possible across the bedding plane from a low-permeability layer into an adjacent layer of moderate or high permeability, the earlier depletion of the more permeable layer will cause such flow to occur. If this situation exists, the oil recovery from tight layers can be appreciable; thus, the economic ramifications of interlayer crossflow are apparent. The possible importance and extent of flow between adjacent and connected layers — whether resulting from capillary, gravitational, or viscous forces — have been the subject of considerable speculation for many years. Jacquard1 presented a rigorous analysis of the crossflow due to single-fluid expansion occurring between two adjacent and connected layers when the well produces at constant rate. His presentation was entirely mathematical, however, and no numerical results from evaluation of the mathematical solutions were presented. Our objectives in the preparation and presentation of the present paper are essentially twofold— (1) to analyze the behavior of a well which produces a single compressible fluid from a bounded, layered reservoir with interlayer crossflow, and (2) to present practical numerical results and simplified formulas to facilitate engineering analysis of reservoirs with crossflow. The constant-terminal-pressure case was analyzed rigorously, whereas the constant-terminal-rate case was treated only for semisteady-state conditions. DESCRIPTION OF THE IDEALIZED TWO-LAYER RESERVOIR The reservoir to be studied is assumed to be bounded and cylindrical in shape, with a completely penetrating well at its center. The reservoir is composed of two adjacent horizontal layers between which fluid is free to flow. Each layer is assumed to be homogeneous, isotropic and completely filled with a fluid of small and constant compressibility. The total thickness of the reservoir is small enough

By Goldye Leeds, Marian Balicki

A SURVEY of literature reveals the scarcity of experimental evidence relating to work hardening and reannealing of silver.'-'" With the exception of the well-known X-ray investigation of silver and other metals by W. A. Wood? the effect of progressive cold working has not been studied. The determination of thermal stability of silver in the work-hardened state by means of isochronal or isothermal annealing has been confined apparently to very high reductions only. In the survey made, no study was encountered which endeavored to produce a complete picture of the changes in various properties due to cold working and subsequent reannealing. To fill these gaps and to assemble data that could be used for the determination of activation energies and of frequency coefficients of primary recrystallization, a systematic experimental approach, which was developed by one of the authors, has been applied to pure silver. Material and Processing The silver used was Handy and Harman fine silver, with a spectroscopic analysis at the testing stage of Cu, 0.0001 to 0.001 pct; Te, 0.0001; Pb, Si, Ca, Mg, and Mn, traces. The material was supplied in the form of a rod 0.406 in. diam and was converted into test samples according to the procedure condensed in Table I. It should be mentioned that air annealing was adopted to simulate industrial practice, though it was realized that annealing in a neutral gas or in a vacuum would be preferred. The usual precautions have been taken to eliminate any structural changes and property changes resulting from the storage of the samples prior to annealing or testing. Thus the wires were kept at the fully annealed stage, and the final wire drawing, which produced the desired degree of work hardening, was done just prior to the final annealing or testing. During the short waiting period, the samples were kept in a thermosflask filled with ice. Even with these precautions some strain-age-hardening or self-annealing could occur. To test such a possibility, wires of different reductions were prepared in the manner adopted and portions of them were immediately tested. The remaining portions were similiarly tested after different periods of storage, both at room and melting-ice temperature. Within experimental error, all samples obtained from a wire of a given percentage of reduction yielded identical values. This result qualified the material for further tests and interpretations, because it showed that either strain-age-hardening and self-annealing were absent, or that these effects fully balanced each other. The final annealing was carried out in an electric resistance furnace automatically controlled to within a 10°F. It was realized that the temperature fluctuations were greater than desired for this type of work. TO diminish the errors due to fluctuations of temperature, the hot junction of the thermocouple was placed as close to the samples as possible; the time of soaking was reduced to 15 min; and the number of samples annealed at different temperatures was increased. It will be seen from Table I that some tests were performed on the same material at rising temperature. These will be discussed elsewhere. Room temperature testing was limited to the determination of some of the mechanical properties that are known to be additive in a degree sufficient to be used for indirect study of the kinetics of the reannealing process, Tensile tests, carried out on a manually operated J. Camillon machine, accurate to within permitted the determination of the ultimate stress (U.S.1 and of the 2 in. elongation, (A,). The proof stress (d,e) has been determined from a series of bend tests carried out on a Tinius Olsen Stiffness Tester by using the offset method. This involved accurate determination for each sample of load-angular deflection curves, finding a

Jan 1, 1952

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

With either sulfonate or oleate as collector, quartz responds to flotation with moderate additions of calcium only at moderately high pH, where some portion of the activator has hydrolyzed to caOH+ . Calculations of the concentrations of various ionic and precipitated species of calcium and collectors suggest that the products of [(CaOH+) (RSO3)] and [(CaOH+)(01-)] determine whether flotation is obtained under specific conditions. Ion products on the order of 10-12 were calculated for both the sulfonate and oleate systems. The activating effect of calcium ion in nonmetallic flotation systems is of considerable interest because of the normal presence of calcium in natural water. As a result, this phenomenon has received quite some attention in the past. Kraeber and Boppel1 showed that quartz could be activated by calcium above pH 10 with sulfonate as collector. The feasibility of selectively separating quartz from hematite with calcium activation at relatively high pH was demonstrated by Clemmer, Clemmons, Rampacek, Williams, and stacy.2 Cooke and Digre3 showed with a bubble pick-up method that the minimum quantity of calcium ion required as activator for complete pick-up of particles occurs at pH 11.5 for an addition of 20 mg per liter sodium oleate. They also showed that larger additions of calcium (10-fold increase per unit decrease of pH) must be added for complete bubble pick-up as the pH is reduced. Schuhmann and Prakash,4 using a vacuum flotation technique, found that quartz could be floated with moderate additions of calcium chloride and oleic acid at neutral pH, providing the metal ion was present in stoichiometric excess over the quantity needed to form the normal soap with oleic acid. They also reported that calcium will function as an activator only in basic media. More recently, Eigeles and volova5 have shown that essentially complete flotation of quartz is obtained with 6 x 10-4 mole per liter calcium chloride and 1.7 x 10-5 mole per liter sodium oleate at pH 11.6. while no flotation is obtained at about pH 10.9 and below. The importance of adsorption of activator and collector at the air-liquid interface is also demonstrated in these systems. The important role that metal ion hydrolysis assumes in quartz activation systems was also demonstrated recently.6-8 A detailed investigation of metal activation in sulfonate flotation of quartz was undertaken in one system7 and yielded a number of interesting and important observations. Quantification of the data of this system7 to the extent desired was not possible, though, because certain species could neither be ignored nor accounted for accurately. These difficulties can be circumvented when calcium is involved as activator. This detailed analysis was undertaken to obtain a more quantitative explanation of calcium and metal ion activation in quartz flotation. EXPERIMENTAL MATERIALS AND METHODS Sodium alkyl aryl sulfonate9 mol wt 450, and pure potassium oleate were used as collectors. All other reagents used were reagent grade in quality, i.e., n-amyl alcohol as frother, KOH for pH adjustment, and calcium chloride. Conductivity water, made by passing distilled water through an ion exchange column, was used in the investigation. Quartz was prepared by leaching the sized sample (48 x 150 mesh) with HC1 until no iron could be detected in the leach liquor. The experimental equipment and procedure were the same as that described previously.6,10 EXPERIMENTAL RESULTS As the presence of precipitates was noted in all of the systems to which ca++ and collector were added, experiments were undertaken to determine the solubility products of calcium sulfonate and calcium oleate using a nephelometer. With this technique, collector is titrated into a known solution, which in this case was 5 x 10-5 mole per liter CaCl2 at pH 5.5. Upon precipitation of the calcium-col lector salt, e.g., calcium oleate, light is scattered and detected

Jan 1, 1967

Sifto Salt Div. of Domtar Chemicals Ltd. has developed a new method for installing roof bolts in the high backs of its 1-million-tpy rock-salt mine at Goderich, Ontario, on the east shore of Lake Huron. The method teams a telescoping- boom hydraulic crane with a specially developed combination auger-drill and bolt-tightening ma- chine. One man, controlling all operations from a basket supported at the end of the crane's telescoping boom, installs an average of 100 5-ft roof bolts per shift, at heights to 45 ft. The mine has very long backs that are not as stable as might be expected. The result has been that roof scaling has occupied an unusually high percentage of the underground work force. About six years ago, company officials decided to go to 100% roof bolting of all backs as a safety measure. The present roof-bolting equipment is the result of a development program instituted at that time to find a faster and more economical method for doing the job.

Jan 9, 1967

Jan 1, 1957

By M. E. Fine, A. A. Henderson

Investigation of the tensile properties of silver based aluminum alloy crystals was undertaken because it appeared attractive for studying strengthening effects due to Suzuki locking with minimum complication. Yield drops were observed in all alloy crystals (1, 2. 3. 4, and 6 at. pct Al) after strain aging at room temperature. No yield drops were found in similarly grown and tested silver crystals. The yield effects are attributed to Suzuki locking but the major portion of the solid solution strengthening to other mechanisms. INVESTIGATION of the tensile properties of single crystds of silver alloyed with aluminum was undertaken because it appeared to be a system in which segregation at stacking faults associated with partial dislocations1 would be the dominant factor in anchoring dislocations. First, silver and aluminum have closely similar atomic sizes and thus solute atom locking of a dislocation due to elastic interactions should be unimportant. Second, while both X-ray2 and thermodynamic3 investigations show short-range ordering in silver-based aluminum alloys, the degree of local order is quite small (X-ray measurements give v = EAB - 1/2(EAA + EBB) = - 0.025 ev and thermodynamic measurements give v r -0.007 ev) and should not be important in strengthening dilute alloys. Third, the stacking fault energy of silver is probably low (as indicated by the profusity of annealing twins) and is very likely diminished further and quite rapidly by aluminum additions since the A1-Ag phase diagram shows a stable hexagonal phase at only 25 at. pct Al. Also, a careful investigation in this laboratory4 has shown that the ratio of twin to normal grain boundaries in recrystallized alloys increases with aluminum content. Thus, with minimum complication from other factors, Ag-A1 alloys seem attractive for studying strengthening effects due to segregation at stacking faults of extended dislocations. EXPERIMENTAL METHOD Single crystals measuring 250 by 5 by 1.5 mm of pure Ag (99.99 pct) and Ag-A1 alloys (A1 of 99.999 pct purity) of nominal compositions* 1, 2, 3, 4, and 6 at. pct were grown in high-purity graphite molds from the melt under a dynamic vacuum (1 x l0-5 mm Hg). The technique consisted of moving a furnace having a hot zone (which melted about 0.5 cm of alloy) over a horizontal, evacuated quartz tube con- taining the mold and alloy at a rate of 3/8 in. per hr. Chemical analysis showed roughly the first inch of the crystal to be solute poor, the last inch solute rich; and the center section uniform in composition within the sensitivity of the analytical method (± 0.2 at. pct Al). The center section of the crystal was cut into five specimens. Gage lengths of reduced cross section, measuring from 1.5 to 2 cm in length, were mechanically introduced by means of jeweler&apos;s files and fine abrasive cloth with the crystal firmly held in polished steel guides. One-third of the cross section was then removed by etching and electro-polishing, the crystals were all subsequently annealed for several days at 850°C in a dynamic vacuum (<1 x 10-5 mm Hg) and furnace cooled to 200°C. The crystal orientations were determined using the usual back-reflection Laue technique. The Laue spots were sharp and of the same size as the incident beam. However, microscopic examination showed the crystals to contain substructures with subgrains of the order of a micron in diameter. The details of this substructure are presently under investigation. Tensile testing was done with a table model Instron using a cross-head speed of 0.002 in. per min. For testing at various temperatures the following media were used: 1) 415oK, hot ethylene glycol; 2) 296ºK, air, acetone, water; 3) 273ºK, ice water; 4) 258ºK, ethylene glycol "ice" in ethylene glycol; 5) 200°K, dry ice in acetone; 6) 77ºK, liquid nitrogen. EXPERIMENTAL RESULTS A) Yield Behavior—A portion of an interrupted stress-strain curve for a 6 at. pct A1 crystal of the indicated orientation tested at room temperature is shown in Fig. 1. Initially, at (a), there is a small, gradual yield drop of about 10 mg per sq mm2. However, on stopping the test, and aging for a few minutes at (b), a sharp yield drop is found. Aging for longer times at (c) and (dl results in larger yield drops (and larger AT&apos;S). At, defined in Fig. 1, is usually larger than the yield drop by about 20 pct; however, this increase in the lower yield is transient since extrapolations of the flow stress curves join as may be seen from Fig. 1. (Both Laue and low-angle scattering photographs revealed no evidence of precipitation in a strain-aged 6 at. pct A1 crystal.)

Jan 1, 1962

By M. C. Flemings, A. A. Tzavaras

Analytical and experimental procedures are descrihed for quantitative determination of volume-fraction microporosity in metals by mimorarlio-graphg. The analysis assumes spherical pores but allows for the observed fact that pores or portions of pores smaller than a given thickness do not project an image on the film. Volume-fraction microporosity was measuured in cast low-alloy steel and shown to vary from 0.6 x 10-4 to 10 x 10 depending on mode of solidification and on whether the material was air- or vacuum-cast. The aim of work described herein was to develop a method of quantitative measurement of the volume fraction of microporosity in cast metals. Microporosity, present in nearly all castings and ingots, is always interdendritic in nature and may be large enough to be seen on a polished surface with the naked eye. More generally, it is smaller in size, and its detection more difficult. Three techniques might be considered for measurement of microporosity: 1) lineal analysis of a polished metallographic surface, 2) density measurement, or 3) quantitative microradiography. As will be shown later, volume fractions of porosity in directionally solidified castings may be the order of 10-4 to 10-3; such small amounts of porosity are difficult to identify and measure on a polished surface. Density measurement is also not a suitable technique (for alloys) when the volume fraction of porosity is low. This is because the density of the base metal is often not known within the necessary accuracy, due to microsegregation or partial phase transformations. In general, it is not possible to completely eliminate microsegregation without also altering the porosity. Because of the limitations of the foregoing techniques, quantitative microradiography was employed to determine amount of porosity. In recent work, microradiography has been found to be useful for qualitative measurement of porosity, including determination of size and shape of individual pores;&apos;)&apos; however, quantitative determination of amount of porosity has not been attempted. I) CALCULATION OF VOLUME-FRACTION POROSITY The following analysis employs procedures similar to those of Cahn and Nutting3 and Hilliard.4 Major simplifications are that pores are assumed to be spherical and to be present in sufficiently small quantities that no overlapping occurs. A basic difference from the previous treatments is that the limited "sensitivity" of microradiography is considered. Assume first 1) cavities are spherical and of uniform diameter, 2) cavities are randomly distributed, 3) volume-fraction porosity and specimen thickness to pore radius ratio are sufficiently small that overlapping of the projected images of cavities is negligible, 4) sensitivity is limited (i.e., holes or portions of holes of less than a given thickness do not project an image on the film). The sensitivity, is defined as: where 5 = minimum thickness of void from which an image will be projected on the film and t = specimen thickness. Now, from Fig. 1, it is possible to distinguish between two different types of holes. These are 1) holes whose centers lie within the region t/2 > X > 6/2, where X is distance from one surface of the specimen (positive into the specimen), and 2) holes whose centers lie within the region (6 — r) < X < 6/2, Holes whose centers lie outside X = (6 -r) project no image on the film. These two types of pores are considered separately below. Type 1 Pores. When 6 is greater than 0, the image of a spherical cavity of radius r appears on the film as a circle of radius a which is smaller than r. From geometry, Fig. 1: a2=r2-52/4 [2] where a = radius of image of pore on film and r = radius of pore. Since the pores are randomly distributed and spherical V =4/3pr2Nv [3] where V = volume fraction of voids and Nv = number of pores per unit volume and the number of images of Type 1 pores per unit area of film, N&apos;A, is

Jan 1, 1965

By K. Takahashi, I. Iwasaki

The methyl stretching vibrations for a series of normal xanthates, isoxanthates and normal amines were determined with the aid of an infrared spectro-photometer, and the results were compared with published information on the corresponding alcohols. The frequency shifts of methyl stretching vibrations may be attributed to the inductive effect of polar groups. The hydrogens in the shorter chain alkyl groups are somewhat polar and can be expected to interact with water molecules by hydrogen bonding. Contact angle, surface tension lowering, solubility, and critical micelle concentration appear to be related to the induced polarity of the alkyl groups. Traube&apos;s rule states that in homologous series of compounds solubility decreases and surface activity increases regularly with the size of the hydrocarbon group. Analyzing the work of transfer of a solute from solution to surface, Langmuir&apos; interpreted this rule to mean that each CH2 group added to a molecule produced its effect independently of the others. It is also well known2 that the maximum equilibrium contact angle with sulfhydryl collectors is independent of the polar groups and of the sulfide minerals, and that it increases to a certain limit with the number of carbon atoms in the alkyl group. This observation is thought to demonstrate the orientation of the collector molecules at the sulfide surfaces. The dependence on the hydrocarbon chain length is usually explained as due to the screening of the force field of polar mineral surfaces.3-5 Here again, Langmuir&apos;s principle of independent surface action appears to be implied. Heteropolar compounds consist of nonpolar and polar groups, the former being the hydrocarbon group and the latter containing such electronegative atoms as O, N, S, P, or halogens. According to Palit6 the hydrogens in the alkyl groups are more electroposi- tive than in the paraffins owing to the negative inductive effect of the polar groups and a possibility that a hydrogen bond with water molecules ensues. Goto and Takenaka7 provided direct evidence of the inductive effect by measuring the shift of the C-H stretching vibrations of alcohols, acids, and alkyl bromides with an infrared spectrophotometer. Their approach appeared to be directly applicable to the studies of surface activity both at air-water and water-mineral interfaces encountered in flotation systems. The present article attempts to relate the C-H stretching vibrations of alkyl xanthates, alcohols, and amines with such flotation chemistry parameters as contact angle, surface tension lowering, solubility, and critical micelle concentration. MATERIALS AND METHODS Normal xanthates from methyl to octyl inclusive and the isopropyl, isobutyl, and isoamyl xanthates used in this investigation were prepared in the usual manner.8 Normal amine hydrochlorides with carbon chain lengths of 1, 2, 4, and 6 were from Distillation Products Industries, of 8 from Archer-Daniels-Midland Co., and of 10, 12, 14 and 16 from Armour and Co. Normal propylamines, pentylamines and heptylamines from Distillation Products Industries were used both as received and as hydrochloride formed by converting the amines according to the procedure described by Li9 Perkin-Elmer Model 521 and 621 infrared spectro-photometers were used to investigate the spectra in the frequency region of 3050 to 2800 cm-&apos; with frequency scale expansion. The accuracy of the frequency readings was within + 1 cm-1. The KBr micropellet technique was used to prepare the xan-thate samples for measurements, and the halocarbon mull technique was used for amines and amine hydrochlorides. EXPERIMENTAL RESULTS Fig. 1 shows the CH3 asymmetric stretching vibrations as a function of the number of carbons in the alkyl group for normal xanthates, isoxanthates and amines. Also included in the figure are data for normal alcohols and isoalcohols taken from the article

Jan 1, 1970

By P. L. De Bruyn

The adsorption density of dodecylammonium ions at the quartz-solution interface has been Theadsorptiondensitydetermined as a function of collector concentration and pH. A ten thoushasbeenandfold range of amine salt concentration was covered at neutral pH. Experimental results show that over a thousandfold concentration range at neutral pH, the adsorption density (I) is proportional to the square root of collector concentration. Except at high concentrations, I increases with increases with increasing pH, but in general this effect is surprisingly small. . , . . A critical pH curve has been established for the flotation of quartz with dodecylammonium acetate. The conditions along the flotation curve are correlated with the adsorption measurements. THE behavior of collectors at the mineral-solution interfaces is usually explained in terms of an ionic adsorption process. Through the distribution of collector ions between the solid surface and the- co-existing solution phase the mineral is believed to acquire a water-repellent surface coating. Quantitative adsorption studies have been made on simple flotation systems1-4 only within the last few years. Such investigations were made possible by the adoption of the radiotracer method of analysis. As a consequence of these studies a new parameter has been added to aid the understanding of the flotation process. The research investigation to be discussed in this paper was undertaken to obtain a better understanding of the behavior of a cationic-type collector. This objective was approached through the determination of the distribution of dodecylammonium acetate between the quartz-solution interface and the solution as a function of the collector salt concentration and pH. To bring this investigation to focus on the more practical aspect of flotation research, an attempt was also made to correlate the adsorption results with actual flotation tests. Quartz: A —100 mesh ground crystalline quartz was infrasized; the products of the third and fourth cones were mixed together and reserved for experimental purposes. This stock material was cleaned by leaching in boiling concentrated HC1. After leaching the quartz was rinsed with distilled water until the filtrate showed no trace of chloride ian. It was then washed several times and dried. The qwrtz had a specific surface of 1400 cma per g as deterhined by the krypton gas adsorption method. Collector: The distribution of dodecylammonium acetate between the quartz surface and the solution phase was determined by the radiotracer method of analysis with carbon 14 as the tracer element. The radioactive amine salt with C" synthesized into the hydrocarbon chain5 was supplied by Armour and Co. The tracer element was located adjacent to the polar group. The radioactive salt as received had a specific activity of about 0.14 mc per g. When desired, dilution of this activity was effected by addition of non-radioactive dodecylammonium acetate also supplied by Armour and Co. ........ All other inorganic reagents used in this research were of reagent grade. Conductivity water was used for making up all solutions. Adsorption Tests: Two different experimental methods were used. In the first, to be designated as the agitation method, a weighed amount of quartz and a measured volume of amine salt solution were agitated in a 100-ml or 50-ml glass-stoppered pyrex graduated cylinder. The cylinder was filled with solution up to the stopper, since erratic results were obtained when an air space was left over the suspension. Time of agitation varied from 1 to 2 hr. Preliminary tests at different agitation times showed that the amount adsorbed remained constant for all agitation times exceeding 1/2 hr. After this conditioning period, the solids were separated from the solution by filtration through a Buechner fritted-disk funnel. The solution was re-circulated 10 times or more to allow the fused silica disk to come to equilibrium with it. Determinations of the amount of amine adsorbed on the frit itself indicated that this amount was less than 10 pct by weight of the amine acetate abstracted by 10 g of quartz. The funnel with quartz covered by a thin layer of solution was then centrifuged for approximately 5 min, at which time the moisture content of the solids was reduced to about 5 pct by weight. The wet quartz was blown into a tared beaker, re-weighed and allowed to dry at room temperature. A final weighing was then made to determine the moisture content. The second experimental method, similar to the procedure adopted by Gaudinand Bloecher,&apos; will be referred to as the column method. Two liters of solution were passed through a bed of quartz contained in a Buechner funnel attached to a pyrex separatory funnel by means of a ball and socket joint. Preliminary tests showed that increasing the volume of solution above 2 liters does not give a measurable increase in adsorption. From 4 to 4 1/2 hr were required for 2 liters of solution to pass through the column. The moisture content of the quartz was again reduced to a minimum by centrifuging. A slightly modified column apparatus was used for experimenting with alkaline amine solutions. The same basic unit was used, but the underflow from the Buechner funnel was again fed into a Separafory

Jan 1, 1956

By Alan M. Bateman

Before World War II we proudly considered that we were the nation of all the world most richly endowed in mineral resources. We knew it was no accident that those countries abundantly supplied with mineral resources became the great manufacturing nations, and the politically and militarily strong ones; and that our own great industrial cities sprang up where coal and iron met. We all reallized, especially we of the mining profession, that the energy of fuels and the solidity of metals spelled industrial growth and in turn industrial might and that other nations came to regard mineral self-sufficiency as one of the chief goalsof economic nationalism.

Jan 1, 1949