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By N. Van Wingen

EFFective sand permeabilities can be ascertained from core analysis if the laboratory data are compensated to allow for the presence of connate or residual water. Such adjustments can be made by applying empirically derived correction factors. Effective sand permeabilities can be estimated also from analytical studies of field depth-pressure measurements. In one method the time rate of pressure build-up after a well is shut in from steady-state flow is required, and in the other the direct measurement of a steady-state rate of flow and the corresponding equilibrium pressure. The results of the investigation discussed in this paper demonstrate that these methods for determining mean effective sand permeabilities can be correlated. Introduction In recent years many investigators have demonstrated the practical value of an accurate knowledge of the physical and dynamical characteristics of reservoir sands containing oil and gas. Of these factors, which serve to completely define a porous medium as a container or carrier of fluids, the dynamical characteristics are of particular interest to the production engineer because they afford a direct measure of the rate at which the oil or gas content of a reservoir will become available. The constant that defines dynamically the porous medium as the carrier of a homogeneous fluid in viscous motion is the "permeability." Coke-analysis Method The generally accepted practice in com-piling permeability data has been to analyze in the laboratory core samples taken in the course of drilling through the productive horizon, and to obtain the mean measure of the productive ability or permeability for the interval open to production by graphical integration of the permeability profile. An average permeability ascertained in this manner, however, is useful to the production engineer only for comparisons of wells drilled in the same horizon, as permeabilities determined in the laboratory are measures of only the ability of a porous medium to transmit a single fluid. As a result of many investigations, it has been shown, however, that under actual reservoir conditions water is coexistent with the petroleum and that its presence greatly reduces the permeability of the sand to oil. Empirical relationships showing the effect of the presence of any immiscible fluid A (such as water) in a porous medium on the permeability of the medium to a fluid B (such as oil) have been established separately by Hassler,1 Dunlap,2 and the writer (Fig. I),3 so that the average specific or dry-core permeability as determined in the laboratory can be corrected to give the true measure of the ability of the horizon penetrated to transmit oil, provided the percentage of pore space occupied by connate water is known accurately.

Jan 1, 1942

By E. H. Lee, F. J. Fayers

Problems in reservoir analysis can usually he cupressed in terms of a system of nonlinear partial difjerential equations. A rnethod for .setting physically reasonable boundary conditions for these systerrls by ayplication of the theory of characteristics is discussed. A short description i.c. given of the technique for finding chnmcteristics of general first order and second orrler equations. Specific examples are quoted jrorn eqrrations occurring in theoretical reservoir studies. The princip1e. ossocicred wit11 the use of chnracteristic to set physically realistic boundary conditions me developed, and thr method is discussed in terms of boundary condition for the noncupillary, compressible, two-phase flow problen: jor the cupillary, ir~cowlpressible, two-phase flow problems for the tlrtergent flooding prohlenl; as for the compressible. noncapillary, two-phase flow pro11letn. INTRODUCTION In most problcms in reservoir analysis the physical situation is described by a system of nonlinear partial differential equations. The general solution to the set of equations usually comprises a wide range of functions ancl a particular solution is normally selectetl by applying suitable boundary conditions to the problem. In some cases it is clear from the physical situation what form the boundary conditions should take, but it is usually desirable to have an independent mathematical check of the suitability of the chosen conditions. From the mathematical standpoint, a system of partial differential equations with boundary conditions is said to be properly set if the combination determines a unique solution which is continuously dependent on the equation and the boundary conditions. Such a solution is sometimes termed "reasonable". In investigating the properties of the mathematical representation, it is useful to determine the structure of the system by the application of the theory of characteristics. This theory determines in the space of the independent variables, lines or surfaces which play a special role in thc system's behavior. The characteristics determine the possibility and nature of the propagation of discontinuities in the derivatives of the dependent variables. Along the characteristics certain differential relations hold which for some problems allow a so- lution to be obtained analytically. In the case of hyperbolic equations the characteristics can bc used as 3 basis for a numerical solution. If a complicated nonlinear system is to be solved, a study of behavior of the characteristics will indicate what boundary conditions should be chosen. By using the method of characteristics, several advances have rccently been made in solving reservoir engineering problems. Sheldon, Zondek and Cardwell' have discussed how the the method may be used grap-phically to solve the incompressible two-phase displaccmerit problem when the gravity term is included in the equations. Fayers and Perrine' have applied the method to study the equations representing detergent flooding. When compressibility and solution-gas effects are introduced into the two-phase flow problem, the equations and their characteristics become more complicated. It will be seen that in this problem the characteristics are useful for indicating a reasonable set of boundary conditions but cannot readily be used to compute a numerical solution. This problem has been solved on the IBM 701 using normal finite difference methods hy West, Garvin and Sheldon." The material to be prcscntcd in this report is divided into three sections. The first discusses the determination of the characteristics of first and second order partial differential equations; the second describes the selection of suitable boundary conditions by the application of the principle that the future cannot affect the past; the third discusses the use of characteristics for setting the boundary conditions of the two-phase solution-gas flow problem. A useful introduction to the method of characteristics has been given by Hildebrand.' A summary of the method will be given in this section of the paper. The First Order Equation The quasi-linear equation of first order is It is linear in the partial derivations of z. The properly linear equation has the form The characteristics of are curves along which the

By R. W. Smith. Discussion by D. Watson, R. M. Manser

D. Wotson, R. M. Monser (Watten Spring Laboratory, Stevenage, Herts., U. K.) - This is a valuable and interesting paper and will make an important contribution to the development of a general theory of silicate flotation. In particular the dominance of surface reactions which produce fluosilicic acid and its ions has been convincingly demonstrated. In a paper to be published shortly, however, we offer some evidence which is not consistent with the feldspar activation theory proposed by Prof. Smith. This theory, given in Eqs. 17-20, suggests that activation takes place through the exchange of SiF6 ions for OH- at aluminum sites. This results in a negatively charged site facilitating adsorption of RNH3 Firstly, we have determined the flotation response (using the vacuum flotation technique) and the adsorption of dodecylamine on a natural feldspar (albite) and on the same feldspar after washing with perchloric acid at pH3. This pre-treatment was shown to remove surface adjacent aluminum atoms. It was found that although the acid washed feldspar floated much less easily than the untreated sample, the function of fluoride ion - giving activation over the pH range 4-6.5-was preserved. Moreover, the amount of dodecylamine adsorbed either with or without fluoride present is little affected by acid-washing, despite the depression caused by this treatment. This suggests that surface aluminum atoms can be of little importance in the fluoride activation mechanism. Secondly, we have determined the changes in solution concentration of F- and H+ (or OH-) accompanying reaction of the surface with fluoride ion. The ratio of H+ lost from solution to F- lost is high, ranging from 6.9 at pH4 to 1.0 at pH 7.5. This is consistent with reaction of HF (6 molecules for every Si removed) at the surface, producing SiFi-ions, but not with the re-adsorption of these ions.

Jan 1, 1967

By M. J. Swan, W. C. Foshee, R. R. Klimpel

The large volume of water used in coal preparation plants makes water recycling a necessity. Economical cleaning of dirty water usually requires flocculation with an efficient organic polyelectrolyte. This paper discusses identification of optimum flocculant systems. Supporting laboratory data with on-site tests and full-scale field trails supplies information necessary for matching the polymer to the plant.

Jan 1, 1983

By J. W. Dougherty

THE Hollinger gold mine is in the Porcupine mining division, District of Cochrane, in the northern part of the Province of Ontario. The adjacent town of Timmins, with a population of 25,119, lies 490 miles by railway north of the city of Toronto. GEOLOGY The property is situated on the northwest limb of a major syncline, which pitches northeast at approximately 50°. The principal rocks of the Hollinger area are of pre-Cambrian age and consist of altered, schistose, Keewatin lava flows intruded by stocks of schistose, quartz-feldspar porphyry generally assigned to the Algoman period. The structure of the Keewatin series is extremely complex as a result of close folding and some faulting. The schistosity, trending north 70° east and dipping steeply to the southeast, is most highly developed along a subsidiary anticline in which the major porphyry bodies occur. The ore bodies, which exhibit three principal structures, consist of quartz veins and associated pyritized wall rock. Some lodes are com-posed of en echelon veins, others exhibit a main quartz body with branch-ing stringers and a third consists of a single definite lead. Gold, in a coarse visible form, may be confined to quartz in some ore bodies but in others it is finely divided and is found not only in quartz but also asso-ciated with pyrite in the adjacent wall rock. In many veins the dis-tribution of gold is such that there are several ore sections, separated by areas of low-grade material, in the same vein although its physical appearance remains unchanged.

Jan 1, 1940

By R. Schuhmann

Distribution of material in the fine sizes of a comminution product generally is well represented by the empirical equation' y = 100 (x/k)a [1] in which y — cumulative percent finer, x = particle size, a -= distribution modulus, and k = size modulus. Charles3 found that the energy consumption in comminution is usefully expressed by another empirical relation, E = Ak(1-D) [2] in which E = energy input per unit volume of material, A = a constant, k = size modulus based on Eq. 1, and n = a constant; (1-n) is the slope of a plot of log E vs log k. Holmes3 has presented energy equations similar to Eq. 2. The constants a and n in Eqs. 1 and 2 have been shown to depend both on the nature of the material and on the comminuting device. Moreover, Charles showed that within experimental error a and n are a — n+1 = 0 [3] Combining Eqs. 2 and 3, E = A k-a [4] In the first sections of this article it is shown that the energy equation, Eq. 4, can be derived directly from the size distribution equation for the fine sizes, Eq. 1. The derivations are made without assuming any of the specific relationships between energy and particle size which have been common in previous literature. For comminution processes in which Eqs. 1 and 4 adequately represent the experimental data, the constant A in Eq. 4 is found to be a simple and useful inverse measure of grindability. That is, A is the energy consumption per unit volume of comminution product finer than unit size as determined from the straight line portion of the log-log plot of the size distribution. These considerations all lead to a unifying hypothesis of comminution mechanism from which both Eq. 1 and Eq. 4 can be derived. Finally, it is pointed out that this hypothesis raises serious questions as to the significance of the Rittinger hypothesis, the Kick hypothesis, and other theories in which energy numbers are systematically assigned to various size fractions of comminution products in order to calculate theoretical energy consumptions. Derivation of the Energy Equation from the Size Distribution Equation: For simplicity, consider the comminution of 100 volumes of a feed material of relatively uniform particle size. The comminution process may be considered as the summation of many individual and independent comminution events. The extent of comminution is most easily expressed as the number of comminution events, z. In the first derivation, the key assumption is that the characteristics of the comminution events in a given crushing or grinding process are substantially constant and do not vary with the progress of the comminution process. Accordingly the characteristics of an average comminution event may be defined. In one such event, a quantity of energy $E is applied to a single particle of size f and volume $v. The crushing of this particle produces fine particles with a size distribution similar to that given by Eq. 1: yw=100(x/ka)a0 [51 In this equation yo, a0, and k0 are used to characterize the product of an individual comminution event rather than the product of the comminution process as a whole. In using Eq. 5, we will not be concerned with values of x close to the feed size f and will therefore assume only that the equation is applicable to the finest sizes of the material. In 100 volumes of total product, the actual volume of product finer than x from a single comminution event, or dy, is given by The total volume of material below size x, resulting from z events, is then given by y = z(dy) =z(dv) (x/ka)a0 =" Eq. 7 reduces to Eq. 1 when we let a, = a and [8a] z =100/dv (ka/k )1 or k = ka (zdv/100)-1/a [8b] Eq. 8a shows that the distribution modulus of the comminution product is the same as for the product of an individual comminution event. Eq. 8b shows how the size modulus of the comminution product k varies with the extent of comminution as measured by the number of events, z, or as measured by the fraction of the feed actually subjected to com- minution1 zdv/100. The energy input to 100 volumes of total feed, or 100E, is the sum of the energy inputs for all the comminution events: 100E =z (dE) [9]

Jan 1, 1961

By Gerald G. Griswold, James O. Greenslade, Cherie Tilley, Richard Reseigh

INTRODUCTION The Harrison Western Corporation, a leading Denver based mine contracting and engineering concern, is presently engaged in sinking two 1,006 m (3,300 ft) shafts for the Phillips Uranium Corporation at their Nose Rock Project, approximately 13 miles northeast of the small community of Crownpoint in McKinley County, New Mexico. The Nose Rock Project is the first attempt by the Phillips Uranium Corporation to tap the deep uranium reserves in what has become known as the Grants Mineral Belt. (See Figure 1) Project Description Phillips Uranium Corporation's plan for the large 2700 metric ton per day (2950 tons/day) mining facility calls for a series of deep access and ventilation shafts ranging from 4.27 m (14 ft) to 5.49 m (18 ft) in diameter to approximate depths of 1,006 m (3,300 ft). The initial pair of shafts consists of one production shaft and one ventilation shaft separated by a distance of 91 m (300 ft). The interbedded layers of sedimentary sandstones and shales to be penetrated by the shafts contain several major water producing aquifers, the deepest being the mineralized zone called the Westwater Canyon Member of the Morrison Formation. A series of temporary and permanent water pumping stations is planned. Generally, the temporary stations are located above major aquifers to facilitate water removal while sinking through the aquifer and the permanent stations constitute what, in the final mode, will be the mine dewatering system. In addition, Phillips Uranium Corporation has In- stalled and is maintaining a system of depressurization wells that temporarily pump the major aquifers and considerably reduce the water inflows during shaft construction. The major aquifers are also chemically grouted prior to sinking. Site work for the project was initiated in the fall of 1976. Full scale shaft sinking commenced in November of 1977 on the 4.88 m (16 ft) diameter ventilation shaft and on the 5.49 m (18 ft) production shaft by another contractor. Harrison Western Corporation began work on the project on November 4, 1979 wlth the production shaft at a depth of 633 m (2,076 ft) and the ventilation shaft at a depth of 474 m (1,554 ft). This paper will address only the portion of shaft sinking completed by Harrison Western. Geology and Hydrology The Nose Rock Project is located on the Chaco Slope in the southern extreme of the San Juan Basin in northwest New Mexico. The southern San Juan Basin is generally bound by the Defiance Uplift to the west, the Zuni Uplift to the south and the Nacimiento Uplift to the east. The Grants Mineral Belt occupies most of the southern portion of the San Juan Basin and this project is located on the northern extreme of the Grants Mineral Belt. The San Juan Basin is comprised of sedimentary rock of continental, marginal-marine and marine origin, that dip northward from the Zuni Uplift and Chaco Slope into the interior of the San Juan Basin. (See Figure 2) Major Formations The major geologic formations to be penetrated range from mudstone and shales to siltstones and sandstones. The sandstones are highly productive aquifers which, under static conditions, would flow artesian. Water temperatures in the aquifers are high and therefore are a force to be dealt with. Temperatures range from 18ºC (65OF) in the upper aquifers to 48ºC (118º'F) in the lower. The mudstones are generally bentonitlc. (See Figure 2) GALLUP SANDSTONE: The Gallup Sandstone is the first major regressive wedge in the San Juan Basin of the Cretaceous era and at this project is about 35 m (115 ft) thick. It is medium grained and prior to depressurization carried a hydrostatic water pressure of over 72.5 kg per cm2 (1,031 psi) which 1s artesian. Compressive strength ranges from 334.7 kg per cm2 (4,760 psi) to 421.8 kg per cm2 (6,000 psi). Water temperature is approximately 30°C (86°F).

Jan 1, 1982

By R. F. Mitchell, G. F. Dillon, A. F. Armington

In this paper the present methods of boron preparation are discussed with emphasis on the iodide intermediate. Several methods of boron triiodide preparation were investigated, the most satisfactory method being the preparation from the elements. A yield of 60 pct based on iodine is found for this method. Zone-refining, sublinzation, distillation, and fractional-recrystallization results are given for the boron triiodide, with distillation producing the best results. Several methods of decomposition are also discussed. The purity of the resulting iodide boron approximates the puritjl of the best available bromide boron, ELEMENTAL boron has been suggested as a possible high-temperature semiconductor by several workers,' but has never been exploited as a device material. The principal difficulty with boron is the unavailability of pure crystalline material from which accurate information on electrical properties could be obtained. Most boron crystals presently produced are very imperfect in structure and of questionable purity, particularly in relation to carbon content. Several methods of boron purification have been reported in the past few years, all of which produce material with a purity better than 99.0 pct. Most of these methods have been the subject of a recent review by Starks' and will not be elaborated upon in this report. However, of all the purification methods reported, only those using halide intermediates produce a purity approaching that usually required for electronic applications. The bromide intermediate has been most used for the preparation of high-purity boron.'y3 This material is easily prepared from the elements and can be effectively purified by distillation and decomposed by hydrogen reduction. The resulting product contains a trace of silicon, and an uncertain amount of carbon, believed to be approximately 100 ppm. It has been recently reported by Russian workers that high-purity boron can be produced using an iodide intermediate.' In the work cited, boron is reported free of spectro-scopically determined impurities, but the reported detection limits are quite high (- 100 ppm). In addition, no data is given on the carbon content of the product. In the present paper, boron triiodide was chosen as the intermediate for several reasons. First, carbon tetraiodide, which could be a major impurity, is reported to be unstable above 200" and hence could be easily separated from the boron triiodide by its decomposition, since temperatures greater than this are attained during the purification process. The low melting point (45°C) and boiling point (20B°C) and the relatively high vapor pressure of boron triiodide should allow the application of any physical purification technique to the material. The possibility of a lower decomposition temperature than that used for the bromide process is another advantage which might cut down extraneous contamination. The iodide, however, does have certain disadvantages when compared with the bromide, the production cost being the most significant. This is the result of a higher halide-to-boron weight ratio, which means more intermediate must be employed. The cost of the starting material is also greater for the iodide. This cost could be considerably reduced however, by recycling the iodine byproduct. Epitaxial growth of boron, which is probably the best method of producing junctions, should be possible with either the bromide or the iodide as the intermediate. However, this has been attempted only on a limited scale up to the present time because of the unavailability of good crystals. The authors have been relatively successful in laying down a heterotaxy of boron on silicon, however. This will be reported at a later date. Several crystalline modifications have been reported for boron, four of which are now believed to be real.' These are the a! and 0 rhombohedral and the a, and 0 tetragonal. In general, the a! rhombohedral is the low-temperature form and the B rhombohedral is the high-temperature form. The tetragonal structures are detected between 1000"

Jan 1, 1964

By D. L. Albright, G. A. Colligan

An investigation has been conducted to determine the nature of the crystallographic substructure of nickel and a 1.0 wt pct Ag-Ni alloy which had been undercooled 105°C prior to solidification. A rotating back-reflection X-ray technique and modified Weissmann diffractometer were used to orient single-crystal sections from these poly-crystalline ingots and to determine the substruc-tural features of these single crystals, The sub-grain size in the pure nickel ingot is 0.5 mm diam while the silver-doped nickel subgrain size is only 0.1 mm diam. The misorientation between adjacent subgrains is approximately 1 deg of arc in both ingots, and the spread of orientation of sub-grains about the mean orientation of the crystal is 5 deg of arc in both ingots. The addition of silver results in a stable impurity substructure which is preserved during isothermal solidification and subsequent cooling to room temperature. In the absence of silver the initial impurity substructure is destroyed by dislocation interactions which produce a secondary substructure which grows to a size five times larger than the initial substructure. THE process of undercooling a metal entails cooling of the molten sample below the equilibrium freezing point without the occurrence of solidification, i.e., by exercising proper constraint over the experimental variables contributing to nucleation in the melt. The current work of walker1 and Colligan Metal reports undercooling large continuous samples of nickel by imposing appropriate restrictions upon the parameters of solidification. The silver-nickel equilibrium diagram3 reveals the presence of a monotectic reaction at 1435°C. At this temperature the maximum solid solubility of silver in nickel is approximately 3 wt pct, but this solubility decreases with decreasing temperature and the solute is rejected as a silver-rich liquid phase at temperatures below 1435°C. Thus, the 1.0 wt pct solute should be held in solution during undercooling and solidification and subsequently precipitate as a silver-rich liquid phase at grain and subgrain boundaries following solidification during cooling below 1435. This assumes no solute segregation sufficient to cause the monotectic reaction. One would expect this second phase to inhibit grain and subgrain growth by retarding dislocation motion after solidification is complete. The effectiveness of silver addition in growth retardation of high-angle grain boundaries has been demonstrated by Colligan and suprenantS4 The principal [l00] dendrite growth directions in a 2 wt pct Ag-Ni alloy undercooled 53 all radiated from the nucleation site. A similar pure nickel ingot undercooled 59°C exhibited a random orientation of [l00] dendrite directions with respect to the nucleation site. Since undoped nickel ingots do not retain any evidence of the casting or solidification texture and silver-doped ingots do retain this texture, it is reasonable to assume that considerable grain growth has taken place in the pure nickel. These particular experiments were performed in order to reveal the differences, if any, in the features of the crystallographic substructure of undoped undercooled nickel and silver-doped undercooled nickel. 1) EXPERIMENTAL PROCEDURE Data are reported on selected specimens from two massive (approximately 260 g) undercooled ingots of nickel. One ingot consisted of electrolytic nickel and the other of this same material with 1.0 wt pct addition of high-purity silver. Powder patterns were taken of both the as-received and as-solidified materials; in all cases the reflections recorded were attributable to the individual elements nickel and/or silver. Fig. 1 is a. schematic diagram of the apparatus employed for the undercooling experiments. The equipment consists in part of a fused silica crucible for containing the charge. A fused silica tube encloses the system, which is covered by a brass cap to permit partial sealing of the inert atmosphere. This cap contains a hole through which a Pt-Pt 13 pct Rh thermocouple is inserted for temperature measurement. The charge is inductively heated under a purified argon atmosphere.

Jan 1, 1963

By C. S. Yust, C. S. Morgan

ThIS note reports the observation of masses of dislocation etch pits around the weld necks of small single-crystal particles of calcium fluoride sintered to a cleaved face of a larger CaFz crystal. Crystal particles in the -50 +I00 mesh size range were placed on freshly cleaved CaFz surfaces and heated at 1250°C for 30 min in a tantalum container in an argon atmosphere. The sintered specimens were then etched at room temperature for 40 to 50 min in a 2 pct sulfamic acid solution which is a selective etch for dislocations in caF2.' Figs. 1 through 3 show the masses of dislocation etch pits observed around weld necks after etching. In some cases, particles were gone after removal of the specimens from the furnace although weld necks were readily visible. In other instances, no etch pits formed around a weld neck. A possible cause of concentrations of dislocations on the crystal surface is mechanical deformation of the base crystal when particles are dropped on it. If such a deformation does occur, it would be much smaller than that caused by the light punching of a crystal with a sharp instrument which results in large concentrations of etch pits. However, crystals deformed by punching with the sharp instrument and annealed at the conditions of these experiments (1250°C for 30 min) before etching showed no concentrations of dislocation etch pits. It is obvious that dislocations from the much smaller deformations, possibly created when particles are placed on the surface, would also anneal out. Etching of large crystals which had particles placed on them in the usual manner but which were not heated showed no dislocation concentrations such as shown in Fig. 1. The magnitude of dislocation etch-pit concentrations did not vary with extensive variation of the cooling rate. The appearance of many of the etch-pit clusters is typical of a well-annealed condition, indicating that the dislocation concentrations formed before the specimen temperature was lowered. Therefore, it is evident that thermal stresses in the neck area did not create the deformation indicated by the presence of the dislocations. The possibility exists that the etch-pit concentrations at places where particles had been removed may be the result of deformation accompanying the fracture of the sintered bond. That this is not so was demonstrated by breaking off particles around which no etch pits occurred. Re-etching never resulted in the large concentrations observed at sintering sites. The stress available to effect material movement during sintering of two particles will depend on the geometry at the contact point but can easily exceed the macroscopic yield stress in CaFz systems. It appears that the plastic deformation observed results from sintering or simply from the weight of the small particles. It has been previously argued that plastic flow makes an important contribution to the initial densification of oxides having the fluorite crystal structure.2p3 If plastic deformation occurs, it would begin as soon as the temperature is sufficiently high

Jan 1, 1967

By S. F. Reiter, You-Chao Liu, W. R. Hibbard

Cyril Stanley Smith in his classic 1948 Institute of Metals Lecture&apos; noted in the case of annealing twins that: "It is well known that approximately the same number of twins per grain and the same general geometry are maintained in large grains as in small ones, a fact that certainly suggests a mechanism such as the above where boundaries and twins grow proportionately together. If this view is correct, a spherical grain should have no mechanism for keeping its twins." Such a constancy of twins per grain would be of particular interest as a tool for the study of the origin of annealing twins. It has been proposed by Mathewson2 and later by Barrett3 that in face-centered cubic metals slip occurs in the {111} Plane by <112> shears which combine in pairs to produce the macroscopically observed <110> movement. This proposal is schematically inviting since <112> slip permits the atoms of one plane to move along the interatomic valleys of its neighbor rather than up the hills across the atom sites. There is strong experimental evidence? that annealing twins result from the growth of nuclei in the form of "twin faults" produced by single <112> shears. It is possible that more twin faults would form at low deformation temperatures than at high ones, because the more rigid lattice may increase the tendency to "freeze" the twin faults and prevent their dissipation in slip. This is suggested by (1) the greater resistance to slip at low temperatures and (2) greater tendency toward mechanical type twinning at low temperatures (a summary of these factors is presented by Seigle and Brick5). These considerations would suggest the following: a. Constant twin/grain ratio for specimens deformed constant amounts at a constant temperature, but annealed at various temperatures above the recrystalliza-tion temperature. b. Larger twin/grain ratios for re-crystallized specimens previously deformed constant amounts at lower temperatures. The purpose of this investigation is to test these considerations. One half in. rods of phosphorous deoxidized electrolytic copper and 70-30 alpha brass (68.36 pct Cu, 0.005 pct Pb, 0.01 pct Fe, 31.62 pct Zn remainder) were rolled to a thickness of 0.350 in., milled to specimens 0.350 X 0.437 X 2 in., and annealed at 700°C to an average grain size of 0.065 and 0.090 mm, respectively. These specimens of each metal were then rolled 50 pct reduction in thickness and annealed one hour under conditions which were all combinations of the following: Rolling Annealing Temperatures. Temperatures. °C °C -70 400 25 500 200 600 Standard metallographic techniques&apos; were used to prepare specimens. By the method of lineal analysis7 using a minimum of ten samples of fifty grains each for each specimen, the ratios of twins* per total grains, twins per twinned grain, twin families* per total grains and twins per twin family were determined. Recrystallized grain size was determined by A.S.T.M. comparison methods.8 All observations were made on the rolling plane. The results are tabulated in Table 1.

Jan 1, 1950

By Fuad S. Maayeh, Robert J. Evans, Paul M. Yavorsky

A description and capabilities of the Mine Roof Simulator at the Pittsburgh Mining Technology Center is illustrated for testing longwall roof support equipment. This unique Mine Roof Simulator has the capacity to exert 3 million lbs. of compressive force vertically and 1.6 million lbs. of force horizontally to simulate loads on hydraulic supports typically found in longwall mining. The supports that undergo testing are instrumented with strain gauges and photoelastic coatings such that critically strained areas become readily apparent. These critically strained areas are redesigned or retrofitted with appropriate reinforcement and retested. A data base will be accumulated from several support designs that will lead to an optimized design that will have the potential to reduce downtime by malfunctions of supports and thus increase productivity. A typical test procedure and analysis is given for a two leg 350 ton shield along with a description for placement of strain gauges, displacement gauges, and hydraulic pressure monitors for critical sites.

Jan 1, 1982

By Mark J. Klein

An internal-friction profile induced by nitrogen in Cr-35 at. pet Re was studied as a function of nitrogen concentration and heat treatment. From these studies, the solubility of nitrogen in this alloy was deduced. The equilibrium solubility of nitrogen in chromium does not appear to be substantially changed by the addition of 35 at. pet Re to chromium. However the precipitation kinetics of nitrogen from solution are significantly decreased. IT has been found that rhenium has a beneficial effect on the low-temperature ductility of Group VI-A metals. As part of a study to investigate the mechanism of this increased ductility, it was of interest to compare the concentration of interstitials retained in solution in one of these ductile bee alloys with the concentration retained in solution in its base metal. In this regard, a study of the solubility of nitrogen in ductile Cr-35 at. pet Re was selected for this phase of the investigation because the solubility of nitrogen in the base metal, chromium, has been determined over a fairly large temperature span.1-3 In addition, nitrogen is known to have an embrittling effect on chromium,4 but does not appear to have a comparable embrittling effect on Cr-35 at. pet Re.5 The experimental method selected for this study was the measurement of internal friction. This technique allows interstitial-concentration measurements to be made in bee metals that are sensitive to small changes in the concentration of a particular interstitial, even when other interstitials are present. When subjected to a cyclic stress, interstitial atoms in solid solution give rise to an internal-friction peak whose origin is the stress-induced ordering of interstitials into preferred lat- tice sites. These internal-friction peaks signify a dissipation of elastic energy which is greatest when the period of oscillation is comparable with the relaxation time for the attainment of an equilibrium interstitial distribution. For dilute interstitial binary alloys, the height of the internal-friction peak is proportional to the concentration of interstitial atoms in solid solutions. snoek8 has shown that the internal friction, Q-1, may be expressed by the equation where A is the relaxation strength, ? is the angular frequency, and 7 is the relaxation time. The relaxation strength, A, is proportional to the concentration of interstitials taking part in the relaxation if no interaction occurs between solute atoms. Thus values of peak height, which can be determined as a function of temperature, give a measure of the relative concentration of interstitial atoms in solution at various temperatures. If equilibrium has been attained, the peak heights will be proportional to the interstitial solubilities. The constant that relates A to the interstitial concentration can be determined experimentally from peak-height measurements as a function of concentration for specimens of constant crystallographic orientation. When this has been done, Q-1 measurements can be used to determine solubilities according to the equation C - KQ-1 where C is the soluble interstitial concentration and K is a constant that can be experimentally determined. It is possible, however, that lattice imperfections may bind interstitials to certain lattice sites. Internal friction does not measure these interstitial~, but does measure interstitials which are free to move in the normal lattice sites when subjected to an applied oscillating stress. On alloying the pure metal with a substitutional

Jan 1, 1965

By A. J. Carlson, G. M. Marincel, M. L. Hovland, J. H. Healy

Research personnel of Erie Mining Co., a pioneer taconite mining firm on the Mesabi Range, have invented a new method to make an effective 325 mesh separation at high tonnage rates over stationary screens. The company regards this development as historically significant in that it represents the first successful method to commercially screen large tonnages of ore at fine sizes. Erie, which is now completing an expansion program at its plant site near Hoyt Lakes, Minn., has incorporated this screening method as part of that expansion. When completed, the concentration plant will produce 10.3 million tons of iron concentrate, all of which will have been efficiently screened at 325 mesh.

Jan 4, 1967

By L. F. Coffin

Monotonic tension and controlled cyclic-strain tests have been conducted on an annealed steel at various strain rates and temperatures in the weep range. Evidence of a strain-induced precipitate reaction abozle 500°C was determined from pronounced cyclic-hardening effects, increase inflow stress, inter granular fracture, drastic decrease in low-cycle fatigue resistance, and loss in tensile fracture ductility, as well as through electron-microscopy examination. It was found that strain rate as well as temperature had a pronounced effect on these observations. A parameter of the form P = T(7.95 - log ip) was determined, which was directly related to the ductility, defined either as the true strain at fracture in the case of simple tension, or as 2N 1/2 ? E p in the case of cyclic plastic strain. A highly satisfactory comparison of the cyclic life as measured and as computed from the ductility predicted by this parameter was obtained for a range of temperatures from 400° to 650°C and for crosshead speeds of 0.002 to 0.2 in. per min. MANY metals subjected to sustained loading at elevated temperatures derive resistance to creep from solid-state reactions of various alloying constituents. These reactions can be many and varied, and occur as a consequence of time and temperature according to reaction-rate principles. Strong evidence exists that many of these reactions are influenced by plastic strain, the argument being put forth that dislocations act as sites for nucleation and growth for the new phase.&apos; Many examples can be cited where plastic strain during transformation influences the structure, and as a consequence affects the properties.2 The low-alloy steels serve as particularly good examples for investigating the effect which aging reactions have on resulting properties. Alloying elements such as carbon and nitrogen, and carbide formers such as manganese, chromium, molybdenum, and so forth, can, by the particular aging reaction which occurs, produce strengthening effects at various temperatures, and so endow strength to the alloy over a broad range of temperatures. These effects have been systematically studied by Glen both during creep3 and for constant strain-rate tension testing.4,5 The work of Glen is of considerable interest in connection with the present study, particularly in regard to the effect of various alloying additions on the true stress-strain curve and on fracture ductility at various elevated temperatures. He has shown that strain-age hardening occurred during plastic straining, which was quite specific both to the temperature of the test and to the alloying element involved. When strain-age hardening was noted at a particular temperature, a .minimum in reduction of area was also obtained. Provided the temperature for the minimum reduction of area exceeded 300°C, all minimum ductility fractures were found to be inter-crystalline in nature. For carbon steels containing molybdenum, two minima in reduction of area were noted, one occurring at 200° to 250°C, the precise temperature depending on the percentage of molyb-

Jan 1, 1964

By E. L. Tucker

PREVIOUS investigations of E. L. Tucker and R. E. Head&apos; related in particular to the effect of cyanogen compounds on galena, sphalerite, and pyrite, and their behavior in the presence of such com- pounds. The present contribution deals with the float- ability of the copper minerals and of pyrite. All experiments were performed on minus 200-mesh material, the method of preparation being the same as that described in the previous article. Flotation tests were made in a small mechanically agitated machine of 50-g. capacity designed in this laboratory by Gates and Jacobsen." General Naval Stores pine oil No. 5 and potassium xanthate were used in constant amount in all of the experiments; these agents were selected because of their present wide use in the flotation of copper minerals. Lime additions were varied to secure four &apos;final hydrogen ion concentrations, namely, neutral, 0.0005 per cent CaO, 0.003 per cent CaO, and 0.02 per cent CaO. The variation in lime addition was introduced to include the range of alkalinities employed in actual flotation practice.

Jan 1, 1926

By C Gunther

The term metamorphism as commonly used means any change in a rock in either form or composition, from whatever cause. By metasomatism, according to Lindgren, is meant a metamorphism that involves a change in the chemical composition of a rock by the addition or subtraction of substance. Certain types of metamorphism are due to the action of mineralizing solutions, and are closely connected with ore deposition; they form, therefore, valuable guides in the exploration for ore-deposits. Other types of metamorphism are due to regional processes, and are not connected with ore deposition. By dynamo-regional metamorphism is meant a primary alteration of rocks over large areas under conditions of pressure, flow- age, and heat. This process produces schists and gneisses from either sediments or igneous rocks. It is thought that there is little migration of minerals or of elements in dynamo-regional metamorphism, and that the changes are due chiefly to recrysallization and rearrangement of original minerals in bands with their major axes oriented normal to the direction of greatest pressure. Under these conditions limestones are commonly altered to marble, and sandstones to quartzite, basic igneous rocks to greenstone or serpentine, while rocks of normal or acid com- position commonly yield the usual types of schist or gneiss. Dynamo-regional metamorphism, extending over large areas, has no connection with mineralizing processes, and is, therefore, no guide to ore deposits; while this process has certain features, such as characteristic mineral associations, in common with contact metamorphism, the results of the two processes may usually be distinguished without difficulty.

Jan 1, 1932

By W. M. Corse

AT THE TURN of the century the nonferrous alloy industry was awakening to the value of scientific metallurgy, and brass foundries and rolling mills began to establish their own research laboratories for scientific research and control. As the industry grew and its scope broadened it became apparent that an organization was needed that would stand in the same relation to the nonferrous industry as the American Foundrymen&apos;s Association did to the iron foundry business. The brass founders&apos; group of the foundrymen&apos;s association discussed the matter and it was finally decided to appoint a com- mittee to draw up a constitution for a new organization to be known as the American Brass Founders&apos; Association. Charles J. Caley was chairman and Dr. Richard Moldenke secretary of this committee. The object of the organization as defined by the constitution was the study of the technological development of alloying and founding non- ferrous metals, and furthering the advance of nonferrous metallurgy and the standardization of materials and operations in cooperation with the Bureau of Standards and engineering societies.

Jan 1, 1932

The term metamorphism as commonly used means any change in a rock in either form or composition, from whatever cause. By metasomatism, according to Lindgren, is meant a metamorphism that involves a change in the chemical composition of a rock by the addition or subtraction of substance. Certain types of metamorphism are due to the action of mineralizing solutions, and are closely connected with ore deposition; they form, therefore, valuable guides in the exploration for ore- deposits. Other types of metamorphism are due to regional processes, and are not connected with ore deposition. By dynamo-regional metamorphism is meant a primary alteration of rocks over large areas under conditions of pressure, flowage, and heat. This process produces schists and gneisses from either sediments or igneous rocks. It is thought that there is little migration of minerals or of elements in dynamo-regional metamorphism, and that the changes are due chiefly to recrystallization and rearrangement of original minerals in bands with their major axes oriented normal to the direction of greatest pressure. Under these conditions limestones are commonly altered to marble, and sandstones to quartzite, basic igneous rocks to greenstone or serpentine, while rocks of normal or acid com- position commonly yield the usual types of schist or gneiss. Dynamo-regional metamorphism, extending over large areas, has no connection with mineralizing processes, and is, therefore, no guide to ore deposits; while this process has certain features, such as characteristic mineral associations, in common with contact metamorphism, the results of the two processes may usually be distinguished without difficulty.

Jan 1, 1932

By H. H. Podgurski, H. E. Knechtel

Annealed Fe-Al alloys do not react readily to form AlN when held at 500ºC in NH3-H2 gas mixtures, but do so upon the introduction of dislocatims. Nuclea-tion of the nitride phase occurs on dislocation sites. In turn, the growth of the aluminum nitride particles causes the ferrite phase to yield plastically, generating more dislocations for the nucleation process. The nitride phase extracted from an Fe-2 pct A1 alloy nitrogenated at 500°C was identified as stoichio-metric aluminum nitride with a hexagonal crystal lattice. THIS investigation reveals the role that dislocations play in initiating and sustaining the nitriding reaction in Fe-A1 alloys. As early as 1931 the work of Meyer and Hobrock1 suggested that the initiation of the nitriding reaction could involve a nucleation controlled process. Recently Bohnenka2 depicted the gas-phase nitriding process below 600°C as one of mixed control limited by nitrogen penetration through the surface, by nitrogen diffusion, by aluminum diffusion, and by nucleation of the nitride phase, Fig. l(a). In our research in a comparable alloy (0.57 pct Al) at 575ºC, we have observed a nitrogenation which we feel is better described by Fig. l(b). In the case of a 2 pct-A1 alloy partially nitrided at 500°C we propose the profiles shown in Fig. l(c). For a complete and accurate description of the process, a concentration profile of the dislocation density in the test specimen would be needed. EXPERIMENTAL Nitrogenization was conducted between 500" and 575°C in a variety of NH3-H2 gas mixtures on three Fe-A1 alloys: 1) zone-refined iron + 0.16 i 0.2 pct Al—levita-tion melt, 2) zone-refined iron + 0.57 0.02 pct Al— levitation melt, 3) plastiron + 2 pct Al—melted by induction heating. To demonstrate the effect of dislocations on reactivity, both cold-worked and annealed samples were investigated. All nitrogenation rate studies were conducted gravimetrically with a gold-plated invar balance4 contained in a gas-flow system. To avoid contamination of the specimens in the reaction zone of the system, the reaction chamber was constructed of high-purity dense alumina. The activity of nitrogen was fixed by specific NH3-H2 gas mixtures whose compositions were continually monitored by calibrated thermal conductivity gages and checked by chemical analysis. Variations of ± 0.1 pct NH3 could easily be detected by both methods. Throughout this paper the activity of nitrogen is defined as PN3 /PH23/2 , where PNH3, and Ph2 are partial pressures in atmospheres. Electron transmission, density measurements, and chemical analyses were made on specimens before and after nitrogenating in order to reveal structural and chemical changes. Similar studies as well as X-ray diffraction studies were conducted on nitride extractions from the nitrogenated 2 pct-A1 alloy. These extractions were obtained by the use of an anhydrous bromine-methyl acetate solution which dissolves the iron and leaves the insoluble nitrides as a residue. Hardness profiles were obtained on cross-sections of partially nitrided specimens to demonstrate the extent of nitriding through the thickness of the specimens. RESULTS AND DISCUSSION The nitrogen activity in the NH3-H2, atmospheres was never allowed to reach a level capable of producing iron nitride (Fe4N). Hence, the term nitriding as used in this paper refers only to the formation of aluminum nitride whereas nitrogenation refers to the total uptake of nitrogen regardless of how it is distributed throughout the alloy. The weight increases observed during the initial stage of a nitrogenating treatment are due primarily to the solution of nitrogen in the ferrite phase, particularly when starting with annealed specimens. Because this initial nitrogenation rate in the case of the 0.57 pct A1 alloy, see Figs. 2 and 3(a), was most rapid the weight change that occurred thereafter might be attributed to the nitriding reaction with the exception of a small weight increment due to the irreversible pickup of oxygen by aluminum. The oxygen (<70 ppm) came from traces of H2O and 0, in the hydrogen and ammonia gases. On the basis of discrepancies between total weight increase and the increase in the nitrogen content of the sample as determined by chemical analysis, it was estimated and later established by activation analysis, that as much as 200 ppm of oxygen were taken up by a fully nitrided Fe-0.57 pct A1 specimen at 575°C. Most of the oxygen could have been picked up from the nitriding atmosphere on the surface of the samples during cooling to room temperature. Even 50 ppm of water in the gas phase will become oxidizing to iron before the sample has cooled to room temperature. The lack of reactivity* of these alloys in the annealed

Jan 1, 1970