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By M. S. Azun

M.S. Azun I have many objections to the content of the author's paper. Before discussing it, however, I would like to repeat the property of semivariogram function. Second order stationary properties of regionalized variables (ReV's) such as semivariogram function ?(h) are perfectly known in geostatistics. Also, the kriging equations in the language of mathematical statistics using second order stationary properties are well understood. However, the way to use the sample (estimated) semivariogram function in any one of the kriging procedures is vague. The sample semivariogram function is given as follows: [1 N-hy*(h) = 2(N h) i21 {Xi-Xi+h}Z, h=0, 1, N-1] where N is the total number of samples, Xi is the sample value at the i - th location, X i+h is the sample value at the i +h - th location, and h is the distance among the samples. An estimation variance of sample semivariogram function of first lag is smaller than that of higher order lag. The theoretical semivariogram function reaches the variance of samples asymptotically. But this is not easily observable because of the larger variation involved in the estimate of semivariogram function. In general, an estimation procedure is done for h = 0, 1, 2,…., up to the greatest integer less than N/2, even though sample semivariogram function can be computable through N-1. After estimating semivariogram function, the critical question of how to model sample semivariogram function arises. As seen in the above equation, sample semivariogram function is discrete and can be smoothed by the model being selected. Therefore, modeling of sample semivariogram function is the most important step in geostatistics. It not only smoothes a discrete function but also affects the results of the kriging procedure. When the only aim is to model the semivariogram function, which is the basic point of the author's paper, one can employ any fitting techniques, such as curve fitting, or any ar¬bitrary functions, which are called submodels in the paper. The term "arbitrary function" is used rather than "submodel" because there is no basic understanding of developing them. The author suggests that the sum of those submodels can also be used for the modeling of sample semivariogram function. The combination of any arbitrary functions brings many problems instead of giving an insight of the domain structure considered. The author used two arbitrary functions and the nugget effect in response to sample semivariogram function (Fig. 10). For the same example, he stated that the parameters involved in the mixed arbitrary function model can be accepted when the discrepancy between sample semivariogram function and the model is small visually. For verifying the fitting behavior of any selected model, one should not be contented with the visual satisfactory. Some statistical measure such as goodness of fit has to be used. The author's practice is no more than an exercise in curve fitting without any fundamental understanding or conceptualization of the underlying physical mechanism. Furthermore, the selection of any model is not an easy task if the purpose is the search for the "best" response to the observed second order properties of ReV's. I suggest that the Markovian model (Azun, 1983), on the basis of a theoretical understanding of underlying mechanism, which gives more information about the occurrence of regionalized variables, is used to respond all properties of ReV's. There are a lot of problems for modeling of onedimensional sample semivariogram function. Thus, it is not appropriate to go to higher order dimensional sample semivariogram function modeling. In the meantime, I would recommend that one can connect the values of standardized sample semivariogram function rather than simple values of semivariogram function in the two-dimensional estimation. The standardized values can be computed in dividing the semivariogram function value by the number of sample pairs involved in each lag regardless of the directions. In conclusion, geostatistics is an interdisciplinary area in mining that uses the principles of mathematical statistics. Thus, it should not violate any probabilistic and statistical rules. When Matheron was developing the theory of geostatistical study in the early years of geostatistics, many mining people had a reservation accepting the geostatistical tools. However, this does not mean that we, the geostatisticians, might try to convince those people using some "strange" tools or rules as some authors implied (Baafi and Kim, 1984). Instead, we have to develop and explain the geostatistical tools staying only in the framework of statistical concepts and properties. ? References Azun, M.S., 1983, "Stochastic Process Modeling of Spatially Distributed Geostatistical Data," Columbia University, Ph.D. Thesis. Baafi, E.Y., and Kim, Y.C., 1984, "Discussion - Comparison of Different Ore Reserve Estimation Methods Using Conditional Simulation," Mining Engineering, Vol. 36, No. 3, p. 280. Reply by J.M. Rendu The interactive method proposed by Rendu allows practitioners to develop semivariogram models that take into account not only the numerical information obtained by sampling, but also highly significant additional information that often cannot be quantified. The geology of the deposit - including hypotheses concerning its genesis, sampling methods, assaying methods, and mathematical methods used to calculate the semivariograms - all have an influence on the numerical results obtained and on how these results should be interpreted. If all the information concerning the spatial distribution of values in a mineral deposit was contained in the sample values, it could be argued that statistical techniques alone would produce optimum models. However, this is rarely, if ever, the case. Methods that allow the user to take into account his experience and his geologic understanding of the deposit should not be rejected for the sake of theoretical statistical purity. ?

Jan 1, 1986

By J. A. Solomon, H. E. Shafer

As a result of the great demand for metallic aluminum and the scarcity of domestic bauxite, numerous processes have been proposed and developed to extract the oxide of this metal (Al2o3) from clays, shales, and other low-grade raw materials.1-4 An exploratory study was made to extract alumina with sulfuric acid from relatively impure coal-associated draw-slate and to establish an optimum calcination temperature for maximum recovery. Draw-slate is the term used to describe the hard, slaty material directly overlying many coal seams and may range from a few inches to a few feet in thickness. Alumina content of these draw-slates may range from as low as 15% to over 35%. Although the following results are limited in scope, some of the data should prove beneficial for further work. Coal-associated clay, shale, and gob heretofore have been considered nuisance products; any successful alumina extraction process would greatly enhance the worth of these almost limitless resources. This research demonstrated that an optimum calcination temperature for alumina extraction could be established for a coal-associated draw-slate and that this temperature was lower than those suggested in previous work with unspecified clay types. It should be noted that slightly higher acid concentrations and somewhat finer particle sizes were used in this series of tests as compared to previous work. EXPERIMENTAL WORK Essentially, alumina extraction proceeded in four steps: 1) grinding, 2) calcining, 3) acid leaching, and 4) precipitating of aluminum sulfate. An initial series of reference tests to determine the optimum temperature of solubility for alumina was run using relatively pure kaolin. Kaolin forming clays are hydrous aluminum silicates of the approximate composition 2H2O A12O3 2SiO and kaolinite is the mineral that predominates in most kaolins. 5 The kaolin was ground to -30 mesh and subsequently calcined at temperatures ranging from 100°C to 700°C. Each sample was calcined for 1 hr in a muffle furnace and in turn subjected to sulfuric-acid leaching (H2SO4, 9 molar) for a 2-hr period. The filtrates were analyzed for the amount of dissolved alumina recovered.637 Also, each sample of leached or barren residue was

Jan 1, 1968

Upper Peninsula W. O. HOTCHKISS, Chairman C. H. BAXTER, Secretary-Treasurer, Michigan College of Mining and Technology, Houghton, Mich. S. R. ELLIOTT RUDOLPH ERICSON W. H. SCHACHT Utah Meets second Thursday of each month, October to May, inclusive B. L. SACKETT, Chairman C. T. VAN WINKLE, Vice-chairman G. L. OLDRIGHT, Secretary-Treasurer, U. S. Bureau of Mines, Salt Lake City, Utah A. E. RING L. A. WALKER

Jan 1, 1932

By Harold Markus, Gerhard Derge

THE first paper1 of this series described a technique of careful surface preparation by means of which reproducible results may be obtained from potential measurements of the behavior of tin in carbonate solutions with a pH range from 8.4 to 11.2. It then went on to establish the behavior of pure tin electrodes under these conditions and showed that the metal remains active at all times, though the steady potential attained after several hours decreases from I.I2[t] volts at a pH of 12.6 to 0.6 volts at a pH of 8.4. This behavior may serve as a norm with which all other data can be compared. In the second paper,2 small amounts of other anions were added to the carbonate solutions and the conclusion was reached that the common impurities encountered in alkaline materials packaged in tin do not increase corrosion. In fact, in some cases these anions may actually promote the formation of protective films. The present paper rounds out this survey by presenting data on the influence of cations added to the carbonate solutions, as well as the effect of alloy additions to the tin. In many cases the potential data are supplemented with weight-loss measurements. Information is also presented on the effects of some additional anions, the influence of gases above the electrolyte, the behavior of high-purity tin, and the effect of atmospheric oxidation on the corrosion resistance of the above-named alloys. Analysis of the entire body of data discloses some general rules applicable to corrosion in carbonate solutions. The experimental methods used are the same as those previously described. EXPERIMENTAL DATA Cations.-The carbonates of the cations K+, Li+, NH4+, which are soluble, were studied in the same way as the anions, by adding 0.01 mol of the metal carbonate to one liter of 0.2 M sodium carbonate solution, pH 11.2, or to 0.1 M sodium bicarbonate, pH 8.4. The other metallic carbonates are only slightly soluble, of the order of 0 7-3 mols per liter or less, and the sodium carbonate solutions were saturated by adding excess reagent several days before the experiment, shaking frequently, and filtering just before use. The chemicals were c.p. grade in each case except the indium salt. This salt was prepared by solution of the metal in hydrochloric acid and precipitation by addition of Na2CO3. These cations may be divided into two classes, according to their effect on the potential behavior of the tin: (I) normal, (2) passive. To offer a basis of comparison, curves I of Figs. I and 2 are given to illustrate the behavior of tin in carbonate solutions saturated with CaCO3. These curves are the

Jan 1, 1941

By John Chipman, Helen Towers

DEVELOPMENT of a simple radioactive tracer technique for measurement of the diffusion coefficient of calcium ion in liquid slag has already been reported. The investigation was of a preliminary nature designed to explore the possibilities of using radioactive isotopes and to establish a method, and no great accuracy was claimed for the results. It was shown, however, that Ca15 could be used successfully, and the values obtained for the diffusion coefficient appeared to be of the right order of magnitude. However, it was considered that a better technique could be devised for carrying out the diffusion. The experiments were, therefore, continued to find a more accurate method, to check the calcium results, and to extend the investigation to include measurements of the diffusion coefficient of silicon in the same slag. There were two flaws in the original technique. Convection was the cause of too many failures, and the interface between the two slags in the diffusion cell was curved rather than plane, probably due to a surface tension effect caused by the addition of the tracer Ca45 in the form of chloride. Two methods of overcoming these defects were tried. Since it was planned to study diffusion of the short-lived isotope Si"' also, the development of methods was restricted to those which gave promise of being reasonably rapid. Method 1—The principle was identical to that previously used with respect to the diffusion conditions, but there were three differences in technique. Temperature control was more rigid, the tracer was added to the slag as Ca45O rather than the chloride and, finally, an effort was made to translate to high temperatures the elegant method developed by Cohen and BruinV or bringing together the two liquid layers and beginning the diffusion. A master slag was melted in graphite, ground to a fine powder, and analyzed (38.5 pct Ca0-20.9 pct Al2O3-40.5 pct SiO2). The tracer was received as Ca45C12 in an aqueous solution of CaC12 + HC1. From this, calcium oxalate was precipitated, ignited to calcium oxide, and added as such to the slag to give an activity of approximately 5 µc per g. The mixture was then melted into the form of a cylinder 3/16 in. diam and about 1 in. long. A solution identical to the tracer solution without Ca45 was given exactly the same treatment. The resulting Ca40O was mixed with that slag which was to form the tracer-free half of the diffusion cell, and this was likewise melted into a cylinder of the same size. Slag cylinders, two with and two without Ca15, were set in graphite blocks as shown in Fig. 1, and the crucible was lowered into position in the fur-

Jan 1, 1958

By D. M. Hausen

This study identifies and describes various crystalline phases of the V205-Na20 system, and relates their properties to metallurgical aspects of vanadium production. Phase equilibria and stability ranges of sodium vanadate phases of varying molar ratios of Na20/V205 were investigated in a variety of plant products, ranging from fused "black cakes" (V20 melts) to "salt roast" calcines. Crystalline compounds, Including vanadium pentoxide, V205; sodium vanadyl vanadate, 6 phase, Na2O.V2O5.5V2O5; sodium vanadyl vanadate, y phase, 5Na20.V204.12V205; sodium metavanadate, Na20 .V 05; sodium pyrovanadate , 2Na20 .V205; and sodium orthovanadate, 4Na20.~2~5, have been characterized with the aid of X-ray diffraction patterns, infrared spectra, and optical properties in addition to chemical analyses, as a guide to mineralogical "troubleshooting" of plant problems and processes in vanadium pyro- and hydrometallurgy.

Jan 1, 1984

By Bernard S. Borie

THE U-A1 binary system has been studied by Kaufmann and Gordon.' They have shown that three intermetallic compounds occur in the system: UAl², UAl², and a third compound tentatively identified as UA15. UA1³ is simple cubic, a, = 4.26A. Its unit cell contains one formula weight, and it is iso-morphous with AuCu³. UA1² is face-centered cubic, a, = 7.72A, with eight formula weights per unit cell. Rundle and Wilson have shown that it is iso-morphous with Cu²Mg.² A Debye-Scherrer pattern of the Al-rich compound indicated a more complex structure than either UA1² or UA1³. The following is a report of an investigation of the crystal structure of this compound and a determination of its stoi-chiometric formula. A melt of uranium (99.9 pct pure) and aluminum (99.9 pct pure) was prepared which contained about 25 pct U by weight. It was cooled from 950" to 650°C at a rate of 500" per hr and then taken from the furnace and air cooled. An X-ray diffraction pattern of the ingot showed only lines of aluminum and the Al-rich compound. Filings from the ingot were reacted with a solution of sodium hydroxide, producing a fine black powder, the diffraction pattern of which showed no traces of aluminum. A comparison of the Debye-Scherrer pattern of our sample with the data published by Kaufmann and Gordon1 showed that it is identical with the Al-rich phase which they reported. Single crystals were obtained by cooling the melt more slowly (about 50°C per hr). After reaction with sodium hydroxide, the crystals appeared as small black needles attached to the ingot surface. Cell Size, Space Group, and Uranium Positions A series of Weissenberg photographs for rotation about two of the crystallographic axes, taken with copper radiation filtered through nickel foil, revealed an orthorhombic cell of dimensions: a = 4.41 ± 0.02A b = 6.27 ± 0.02A c = 13.71 ± 0.03A Reflections of the type hkl were observed only if: h + k + I = 2n, of the type hkO only if: h = 2n and k = 2n, of the type h01 only if: h + 1 = 2n, and of the type Okl only if: k + 1=2n. Hence, the cell is body-centered with an 001 glide plane. The evidence for the existence of the glide plane is the observed extinction of 23 possible re- flections of the type hkO with at least one index odd. There are only two space groups consistent with these data: C"" — I2ma and D28 2h — Imma.³ he possible sets of atomic positions for these space groups are: 12ma: (0 0 0; ½ ½ ½) + 4: (a) x 0 %; x % % (b) x ¼ z; x ¾ Z 8: (c) x y z; x y z; x, ½ + y, Z x, M - y, z Imma: (0 0 0; ½ ½ ½) + 4: (a) 0 0 0; 0 ½ 0 (b) 0 0 ½; 0 ½ ½ (c) ¼ ¼ ¼; ¾ ¼ ¼ (d) ¼ ¾ ¾ ; ¾ ¾ % (e) 0 ¾ Z; 0 ¾ z 8: (f) x 0 0; x 0 0; x 1/2 0; x ½ 0 (g) ¼ Y ¼; ¾ Y ¾; ¾ y ¼; 1 y ¼ (h) 0 y z; 0; ;; 0, ½ + y, z; 0, l/2 - Y, Z (i) x 1/4 z; x ¾ z; ¼ z; x ¾ z 16: (j) xy z; x y z; x y z; x y z; x, ½ + y, Z; x,½ - y, z; x, ½ - y, z; 11 1, + y,Z Though density measurements on different samples were found to vary somewhat, they were all within the range 5.7 * 0.3 g per cu cm. If it is assumed that the unit cell contains four formula weights of UAl,, it is 6.5 g per cu cm. If there were as many as eight uranium atoms per unit cell, the

Jan 1, 1952

By W. A. Backofen, G. Mayer

Single crystals of iron, copper, and a Cu-7 wt pct A1 alloy were pulled through conical dies to simulate the constraint in a polycrystalline aggregate undergoing axisymmetric reduction. With Taylor-type hardening, dependence of the drawing stress, od, on the Taylor orientation factor, M, is predictable from the polycrystal stress-strain curve; in particular, for a power-law relationship, it should follow that d log od/d log M = (1 + n). A first-order agreement with analysis was found in the data from iron. For copper, the implied n from the observed d log od/d l°g M was -0, while for Cu-7Al it was negative. The trend was in the direction of random polycrystal behavior. Thus the idea of hardening only in response to the amount of prior slip loses validity as stacking fault energy (SFE) is lowered. Two possible explanations have been suggested: as stacking fault ribbons are widened, barriers from dislocation reactions become increasingly effective in dispersing slip and reducing the orientation dependence of the total glide strain dm that appears in alternatively, or conjointly, the polyslip shear stress, 7, acquires an orientation dependence of a kind which has the same leveling effect on M. The problem of relating the strain hardening of polycrystalline material to that of an isolated single crystal is still largely unsolved. In a new experimental approach from recent work, single crystals of different orientations have been deformed under the constraints found in an aggregate while measuring their deformation resistance. Procedures have involved drawing cylindrical crystals through conical dies1 and compressing slab-shaped crystals in plane strain.2'3 Predictions for the outcome of such experiments were made first by Taylor~ and later, in more general form, by Bishop and Hill.5'6 Taylor's example was the axisymmetric extension of an fcc crystal slipping on the usual {111}(110) systems or, equivalently, a bcc crystal undergoing 'kestricted" slip on {110}(111). In his solution, the deformation work supplied was equated to that dissipated internally in slip on all active systems. With o the single applied tensile stress, dc the resulting axial strain, and dyT the total glide strain on systems operating at resolved shear stress, 7: The orientation dependence of M was found by minimizing dyT for each orientation while activating five independent systems, Fig. l(a).? The Bishop and Hill analysis, based on a principle of maximum work, leads to essentially the same conclusion; the need for at least five active systems is recognized in the finding that either six or eight are actually brought into operation. The mean value from the entire stereo-graphic triangle in either case is M - 3.06. More recently, Hutchinson8 made a Taylor-type analysis for pencil glide in a bcc structure, from which piehlerg prepared Fig. l(b) as the counterpart in Fig. l(a); here M = 2.75. The obvious weakness in such analyses is the indifference to slip-system interactions. A condition of what might be termed "independent"

Jan 1, 1969

By S. W. Zehr, G. S. Murty, W. A. Backofen

AN observation by Squires, Weiner, and phillipsl has stimulated interest in a mechanism of deformation at high temperature (above -0.5 of the absolute melting point) that is not usually thought to be involved in the creep of metals. They found precipitate-free or "denuded" zones along grain boundaries normal to the stress axis in tensile specimens of a hydrided Mg-1/2 wt pct Zr alloy after slow straining at 450° and 500°C. Their suggestion that the zones were a result of directional diffusion of magnesium atoms was supported with calculations from Harris and Jones2 which also tended to identify the process as Nabarro-Herring (N-H) creep3,4—a process that is characterized by Newtonian viscosity, with stress (o) directly proportional to strain rate (C), and one that proceeds by lattice diffusion. Material transport by diffusion along grain boundaries is an alternative basis for Newtonian viscosity, as demonstrated by Coble,5 and is favored over N-H creep for fine grain size and lower temperature.6 In either case, the strain rate sensitivity of flow stress, defined as m = d log o/d log E (which commonly appears in the empirical a = KEW), is unity. The experiments to be described here gave metallo-graphic indications of diffusional creep which were no less clear than those just cited, but the associated m (as measured by the method of Ref. 7) was much more like that of a Bingham material. For true Bingham behavior, (a — ao) E, where oo is an initial yield stress. Therefore, even if flow after yielding should occur by diffusional transport, m must increase from 0 as < is raised to reach unity only in the limit as One result is that the resistance to tensile necking conferred by Newtonian viscosity is lost, which would become increasingly apparent through the formation of more sharply defined necks as 6 is lowered. That trend appeared in these experiments. Most of the work was done on an extremely finegrained alloy of magnesium with -6 wt pct Zn and ½ wt pct Zr (Mg ZK60); the initial mean-intercept grain diameter, L, was 0.55 µ. Shown in Fig. l(a) is a germanium-shadowed carbon replica of the surface of a specimen that was coated with silicone oil,* heated to 270°C under a helium atmosphere, and then stretched locally -200 pct at an initial E = 3.3 x 10-5 sec-1. Under

Jan 1, 1969

By H. H. Wade, N. F. Schulz

The large quantities of iron-bearing materials, including taconite, semi-taconite,* and other low-grade ferruginous materials occurring in Minnesota and elsewhere, constitute an important potential source of iron. Satisfactory grade and recovery of iron ore concentrate cannot ordinarily be obtained from these ferruginous materials by simple methods of beneficiation. Iron is distinctive in that the free metal and two of its oxides [magnetite (Fe2O3) and maghemite (gamma-Fe2O3) ] are strongly ferromagnetic. The successful magnetic separation of natural magnetite from taconite has already been established on a commercial scale. The iron in semi-taconite, however, occurs largely as goethite (Fe2O3-H4O) and hematite (Fe2O3) which do not respond to ordinary magnetic separation methods. Magnetic roasting converts these iron oxides to magnetite, which can, after liberation, be magnetically concentrated. MAGNETIC ROASTING Hematite undergoes a stepwise reduction when exposed at moderately elevated temperatures to a reducing atmosphere containing hydrogen or carbon monoxide: Fe2O3? Fe3O4 ? FeO ? Fe Since the desirable product in magnetic roasting is Fe3O4, the conversion is halted after the first stage by controlling the reduction potential of the gas mixture with water vapor or carbon dioxide. The reducing gas mixture must be such that the oxygen partial pressure at the solid-gas reaction interface will be maintained intermediately between the oxygen partial pressures in equilibrium with Fe2O3 and Fe3O4 at the prevailing temperature. Because of the rapid increase in decomposition pressure of Fe3O4 with increase in temperature, the practical upper limit of useful reaction temperature is about 1400°F, above which over-reduction usually occurs in atmospheres containing hydrogen or carbon monoxide. On the other hand, useful reaction rates usually occur only above 800°F. Goethite reacts similarly except that the combined water probably has to be driven off thermally before the reduction to magnetite occurs. Iron carbonate must also be decomposed thermally to an oxide before conversion to magnetite. Iron silicates are apparently not amenable to magnetic roasting. The rate of penetration of the reaction toward the interior of a given ore fragment is dependent on the chemical composition and physical structure of the solid. Most ore fragments tested here reduced satisfactorily to 1/4-in. depth in less than 14 min at 1200°F. Some very dense fragments, however, were reduced to less than 1/32-in. depth under the same conditions. Determination of the optimum temperature, gas composition, ore fragment size, or time of exposure

Jan 1, 1961

By A. T. Beckwith

This paper concerns measurements of low-velocity air currents and investigations on mine ventilation by means of chemical smoke. The chemical smoke used is produced without flame and at ordinary mine temperatures, and therefore presents no ignition hazard in gaseous mines. Mining men who have worked in open-light mines are familiar with the use of tobacco smoke in determining the direction of air travel and approximately measuring low-velocity air currents. The use of chemical smoke is merely a refinement on the use of tobacco smoke and the flameless low-temperature source of chemical smoke has the additional advantage that it can be used in gaseous mines. Ventilation smoke apparatus, Fig I, is a simple device for producing dense white smoke. The apparatus as shown consists of a rubber aspirator bulb which is used to force air through a glass "smoke tube" containing a chemical substance that produces a dense white smoke on contact with air. The apparatus was developed by engineers of the U. S. Bureau of Mines.&apos; It is inexpensive, weighs less than 3 oz, is easily carried in a pocket, and requires no skill to operate. Smoke apparatus is invaluable in practical mine ventilation work for: (I) measuring low-velocity air currents, (2) detecting air leakage, (3) observing airflow characteristics. This paper is written to show the merits of the apparatus, and is based upon findings through its extensive use, during the past six years, in mines operated by the Lehigh Navigation Coal Co. Inc. The Apparatus Certain chemicals, such as stannic chloride (SnCl4) and pyrosulphuric acid (H2S2O7) produce "white smoke" when exposed to air. Stannic chloride gives off vapors which on contact with moist air cause the formation of solid hydrates, of which SnCl4.5H20 is the most important. Pyrosulphuric acid decomposes when exposed to air with the evolution of sulphur trioxide (SO3) fumes, which become white upon contacting moisture in the air. A chemical, such as one of the above, is the active substance in a smoke tube. The glass tubes are hermetically sealed during manufacture, and are made ready for use by merely breaking off the tips at the conveniently located file cuts. When the smoke tube is connected to the aspirator, depressing the aspirator bulb forces air into contact with the chemical, and smoke discharges from the open end of the tube. A white solid (a hydrate if stannic chloride is used, or sulphur trioxide if pyrosulphuric acid is used) may occasionally form a cake in the outlet opening of a smoke tube. A small wire such as an ordinary paper clip can be conveniently employed to dislodge the cake should it seal the tube. When the assembled apparatus is not

Jan 1, 1949

By CARLE R. HAYWARDC

BEFORE discussing this subject it is necessary to define somewhat the meaning of the tern metallurgical.. When I was a student at M. I. T. ore-dressing was not thought of as metallurgy in any sense of the word, but it was considered as more closely allied to mining, enabling the miner to market an otherwise unmarketable product, or at least to market it to better advantage. Progress in ore-dressing has gradually allied it more closely with smelting, for at present the raw material received by the smelter is predominantly concentrates and smelting practice has been profoundly affected by the products of the concentrating mill. It is not surprising therefore that in many schools ore-dressing is frankly considered as metallurgy and although there may be some dissenting opinions it will be considered as such in this discussion. Twenty-five years ago at M. I. T. metallography was taught in a few optional lectures. This subject has developed rapidly and been expanded into the new and increasingly important field of physical metallurgy. To many metallurgists the -term metallurgy means only physical metallurgy. They know little or nothing about smelting and leaching and even less about ore-dressing. Having then broadened the scope of the term metal¬lurgy to cover ore-dressing, smelting, leaching and phys-

Jan 1, 1930

By M. S. Abrahams

Germanium has been rolled in the temperature range of 700o to 800°C. The thickness has been decreased by as much as a factor of four, from a thickness of 0.032 in. to a thickness of 0.008 in. For deformations below 60 pet, the true strain per pass is found to be a constant; from the temperature dependence of this slope, an activation energy of about 2.5 ev is obtained. This energy agrees with that for dislocation climb in germanium . For reductions greater than 60 pet, complete rings are seen in the Lave photographs, new grains are observed in the microstructure, considerable softening occurs, and the hole mobility is very low. This evidence indicates that the recrystallization of gertnanium has occurred. GERMANIUM has been deformed in many ways1 including tension, compression, torsion, and bending since Gallagher2 first described its plastic nature at elevated temperatures. All of these studies indicate that the glide plane in germanium is (111) and that the glide direction is (110). Rolled germanium specimens were used by Kolm, Warekois, and Kulin3 in their X-ray study of deformed semiconductors, but no information is given on the rolling itself. The present experiments deal with the rolling of germanium at various temperatures and for different orientations. In all previous deformation studies, the phenomenon of recrystallization (i.e., the transformation of a single crystal into a polycrystal) in germanium has not been observed4 despite relatively large deformations at elevated temperatures. The proposed reason4 for this was that sufficient energy could not be stored in the deformed germanium lattice. In contrast to the earlier studies this work will present evidence indicating that recrystallization occurs in germanium during rolling at an elevated temperature. I) EXPERIMENTAL PROCEDURE A) Test Specimens. The samples used for rolling were in the form of rectangular parallelepipeds measuring 0.3 in. long, 0.06 in. wide, and 0.035 in. high. They were cut from an undoped single-crystal ingot of p-type germanium with a resistivity of 24.4 ohm-cm, a Hall mobility of 2300 sq cm v-&apos; sec-l, and a hole concentration of 1.1 x 1014 cm"3 at room temperature. The surfaces of the specimens were metallographically polished prior to rolling. The initial dislocation density of the samples was about 10&apos; cm-&apos; as determined by etching in CP4. Two different specimen orientations were used. In the first case, the direction of rolling was parallel to (251), the surfaces in contact with the rolls were of the form (1021, and the normal to the third face was parallel to (211). The corresponding di-

Jan 1, 1964

By F. E. Pawlek, J. K. Gerlach

The chloridizing roasting of ores is applied when metal sulfides and oxides are to be converted into soluble or volatile compounds. The chlorine required is either obtained from the admixed chlorides of sodium or calcium or added in the gaseous state. In the first part of the investigations the reaction rate of the chlorides of sodium or calcium with gas mixtures of SO,-0, or SO ,-O2 ,-SO , was measured. The rate for reactions with gas mixtures SO2-O2 is ThE chloridizing roasting of ores is applied when metal sulfides and oxides are to be converted into soluble or volatile compounds. At present the process is mainly applied to produce nonferrous metals which occur in pyrite cinders in small concentrations. Thereby the nonferrous metals are converted into water-soluble, acid-soluble, or volatile compounds whereas all the iron remains as insoluble oxide. The chlorine required is either obtained from the admixed chlorides of sodium or calcium or added in the gaseous state. The reactions occurring during the roasting process can be divided into two groups: solid-solid reaction and gas-solid reaction. The reactions between solids proceed by means of solid-state diffusion and are therefore of low velocity. The heterogeneous reactions between solids and gases of the roasting atmosphere5 are high-velocity processes and determine the velocity of the chloridizing roasting. These gas-solid reactions shall be the subject of the paper presented. In order to investigate the still little-known processes which occur during the chloridizing roasting 6-&apos; the complex reaction is split into several partial steps. First the reactions of NaCl and CaCl, with gas mixtures of SO2 and 0, have been investigated at temperatures between 500" and 600°C by measuring the weight increase of the samples. The gas mixtures used in this series of experiments had first variable compositions, then the amount of SO 2 had been increased. Furthermore the influence of Fe 2 O3 admixtures upon these reactions, the behavior of pure Fe 2 O3 with the gaseous reactants, and the chlorination of the sulfides of lead, copper, nickel, and zinc have been investigated. FORMATION OF GASEOUS CHLORINE Pyrite cinders are never completely roasted and therefore contain still a small amount of sulfide sulfur. When heated again in air, this sulfur is converted into SO,. Accordingly the formation of chlorine can first be described by the reactions: dependent on the composition of the gas phase. If more than 1 pct SO 3 is added to the roasting gas, the reaction rate is determined only by the concentrations of the SO,. In the second part the reactions between chlorine and metal sulfides are discussed. The rate of formation of gaseous chlorine is higher by me order of magnitude than is the reaction rate between ZnS and chlorine. The reaction rate of NiS and PbS lies considerably below that of ZnS. The conversion rate of both pure Fe 2 O 3 and Fe 2 O 3 containing NaCl or CaCl2 when reacting with SO2-O2, mixtures with and without SO3 portions was measured at temperatures of 500", 550°, and 600°C. The weight increase of pressings was determined by means of a spiral balanceg and the reaction rate calculated therefrom according to Eqs. [ll to [31 and [5] to [7]. The prepared samples were suspended on a platinum filament in a vertically mounted tube of mullite (ID 4 cm, length 110 cm) which could be heated by a resistance tube furnace. The platinum filament was tied to the lower end of the spiral balance. A supremax glass tube (length 70 cm) was mounted gas-tight on top of the reaction tube. The unit was sealed up at its top by a ground-in stopper which was holding the spiral balance with the sample. The spiral balance therefore hung outside the high-temperature region of the furnace. Fig. 2 shows the experimental arrangement schematically. While lowering the sample into the reaction tube pure nitrogen was flowing through the reaction zone providing a protective atmosphere. After the sample had reached the reaction temperature within approximately 1 min, the protective gas was replaced by the sulfur dioxide-oxygen reaction mixture. It took about 30 sec until the mixture filled the tube homogeneously. A Ni/NiCr thermocouple placed in the center of the furnace where the sample hung during the measure-

Jan 1, 1968

By E. P. Abrahamson II

The effect of transitiorz element bitzary solid solution additions upon the recrystallization temperature of columbium has been investigated. The elements Mn, Fe, Co, Ni, W, Re, and 0s OWY the yecystallization tempel-aturye, while Ti, V, CY, zr, Mo, Ru, Rh, Pd, Hf, Ta, W, Ir, and Pt mise it. A correlation is kloted between the rate of chatzge of recyystallization tewaperature with atomic hercent solute and the free atom electron configuration of the solute element. The work of Abrahamson and Grant1 has indicated a correlation between the free atom ground-state electron configuration and the change in brittle-ductile transition temperature per atomic percent solute in chromium base alloys. A similar correlation was observed for the change in the recrystallization temperature of iron base alloys by Abrahamson and Blakeney and Abrahamson. It was also observed that the limit of rapid change in recrystallization temperature also Correlated with the electronic configuration of the free solute atom. A further study by Abrahamson4 established the generality of the phenomenon by yielding similar results for vanadium base dilute alloys. It has been inferred that a peri- odicity might be expected with changes in the free atom electron configuration of the solvent element. This study is the third set of transition base metal systems to be studied. It is the object of this and further studies on transitional metal systems to detect any systematic variations in the observed correlation which might contribute to the understanding of the electron interactions which are evidently exhibiting themselves. PROCEDURE All alloys were made using 99.9 pct Cb with 0.030 Ta, 0.016 0, 0.0025 H, 0.003 Mo, 0.021 Fe, 0.005 C, and 0.002 N. The solute elements were 99.9 pct pure. According to the published binary phase diagrams5 and metallographic examinations at X750, all additions were in solid solution. The alloys were arc melted and remelted 6 times in the form of cubic 400-g buttons under an argon atmosphere. They were then hot forged at 1200oC to 0.6-in. diameter, annealed for 3 hr at 1200o under argon, and furnace cooled. The specimens were then machined to 0.400 -in. diameter. Grain size was checked and found to remain essentially constant at 150 i 30 grains per sq mm. The specimens were then cold swaged to 0.187-in. diameter, yielding 46 i 1 pct cold work. All alloys were chemically analyzed for the major solute. Analyses of random samples indicated that the impurity content remained at the values of the starting material. Tungsten contamination was held to 0.007 pet.

Jan 1, 1962

By W. R. Johnson, M. Hansen, John M. Parks

AS part of a research project sponsored by the Signal Corps Engineering Laboratories, which had the objective of obtaining a magnet wire of good conductivity and low temperature coefficient of resistance, a comprehensive literature survey, supplemented by experimental work, revealed that a linear relationship exists for solid-solution alloys between the electrical conductivity, K, and the temperature coefficient, a, as expressed by the equation: k = a/ß where ß is constant for the solvent metal and a - per°C. tR0 It has long been known that the electrical conductivity at a given temperature and the temperature coefficient of resistance of binary alloys are related to their constitution by the LeChatelier-Guertler rules, as illustrated by Figs. 1 and 2: Rule 1—In alloy systems consisting of a heterogeneous mixture of two phases, the electrical conductivity and temperature coefficient vary as a straight line, if the composition of the alloys is given in volume percentage, Fig. 1. Rule 2—In solid solutions, the electrical conductivity and temperature coefficient are always lower than those of the solvent metal, and usually a considerable decrease occurs with the first small percentage additions of the solute metal, Fig. 2b. If the two components form a continuous series of solid solutions, the electrical conductivity and temperature coefficient curves take the form of a U-curve, Fig. 2a. That some kind of proportionality exists between electrical conductivity and temperature coefficient of resistance is implied by the LeChatelier-Guertler rules and by study of data such as those given by Smith and Palmer,&apos; Fig. 3. Dellinger2 in 1910 first recognized this relationship in a number of commercial copper wires, ranging in conductivity from 94 to 100.7 pct I.A.C.S. He gave the ratio of temperature coefficient to the percentage of conductivity as a constant, C = 0.003939. A year later, Lindeck observed that the linear relationship was valid for a wider range of conductivity in "various sorts of copper," and concluded that the product of resistivity and temperature coefficient was 6.78x10-5 1.5 pct. Since then, this relationship seems to have been entirely ignored. Conductivity-Temperature Coefficient Relationship If the electrical conductivity of copper solid-solution alloys with phosphorus, silicon, arsenic, antimony, aluminum, nickel, manganese, and iron is plotted against the temperature coefficient of these alloys, the diagrams in Figs. 4 and 5 are obtained. Similar data were found with copper-rich solid solutions containing magnesium, cobalt, and titanium,&apos;" as shown in Fig. 6. In all cases, a linear relationship exists. The point representing the highest

Jan 1, 1952

By Pierre I. Desré, Donald T. Hawkins, Ralph Hultgren

The torsion effusion method has been used to measure the vapor pressure of thallium over pure thallium in the temperature range 931" to 996&apos;k The resulting 100 cal per g-atom is in excellent agreement with previous values. Vapor pressures of T1 above seven Ag-Tl alloys ranging from 33 to 90 at. pct T1 were measured at 979K. Calculated silver activities show a positive deviation from Raoult&apos;s law, approaching ideality near the liquidus. Measured thallium activities scatter less than previous measurements using the electromotive force technique. Values for the silver component were calculated by Gibbs-Duhem integration. This paper reports the results of a study of the liquid Ag-T1 system by the torsion effusion method. The method has been discussed in detail previously1 and will be only briefly summarized here. The sample is contained in a cell which is suspended on a torsion wire. Vapors effusing from orifices on opposite sides of the cell exert a torque on the wire. The torque is related to the vapor pressure by the following relation: where D is the torsion constant of the wire, 4 the angle of torque, fl and f2 the correction factors determined by Freeman and seamy2 to account for orifice length, a1 and a2 the areas of the orifices, and ql and q2 the distances of the orifices from the axis of rotation. By using the same cell for pure thallium and the alloy, it follows that: so that most systematic errors are eliminated in determining the activities. EXPERIMENTAL 99.999+ pct T1 was obtained from the American Smelting and Refining Co. and 99.999 pct Ag was obtained from Cominco American, Inc. Seven Ag-T1 alloys, ranging in composition from x^\ = 0.33 to 0.90, were prepared by melting together weighed amounts of the pure metals in sealed, evacuated Vycor tubes and quenching the melts in water. The apparatus and graphite cells were the same as those used by Hawkins and Hultgren3 in their study of the Pb-Sn system. RESULTS Ten measurements were made on pure thallium in the temperature range 931" to 996K, and the results are presented in Table I. Values of were calculated using tabulated Gibbs (free) energy functions.4 No dependence of on temperature or orifice size was found, indicating that equilibrium was attained. Data for the Ag-T1 alloys are shown in Table 11. Values were smoothed with respect to composition by a plot of where . DISCUSSION The value = 43,520 * 100 cal per g-atom for pure thallium (95 pct uncertainty limit) is in excellent agreement with previous investigations.4 In the Ag-T1 system, this study shows positive deviations from Raoult&apos;s law at all compositions. Fig. l gives the phase diagram according to Hansen, and Fig. 2 presents the activity values measured in this study as well as those from electromotive force measurements at 950°K by Terpilowski, Kundys, and slaby.&apos;

Jan 1, 1969

ON Oct. 5, 1926, the day before the general ses-sions of the fall meeting of the American Insti-tute of Mining and Metallurgical Engineers at Pittsburgh, a round table conference on the combus-tibility and testing of coke was held at the Bureau of Mines Experiment Station. There were about fifty present, with A. C. Fieldner, chief chemist of the Bureau of Mines, as chairman. The following organi-zations were represented: American Institute of Min-ing and Metallurgical Engineers, American Society for Testing Materials, American Gas Association, Eastern States Blast Furnace and Coke Oven Association, Gas and Fuel Division of, American Chemical Society, and Southern Ohio Pig Iron and Coke Association. In opening the proceedings, Mr. Fieldner explained that the meeting had been called at the suggestion of several members of the Institute and members of other organizations. The subject is of interest to the pro-ducer and the user of coke whether it be in a blast furnace, cupola furnace, house-heating furnace, open grate, gas producer, or in a water-gas generator. There has been much confusion on this subject largely because there is no common definition of combustibility. Does the blast-furnace superintendent, the coke-oven operator, and the fuel engineer have the same under-standing of the term "combustibility"? If a common understanding can be reached, many differences of opinion will disappear. COMBUSTIBILITY OF COKE R. H. Sweetser of Columbus, Ohio, disagreed with the statement of P. H. Royster, T. L. Joseph, and S. P. Kinney in Reports of Investigations, Serial No. 2524, of the Bureau of Mines, in which it was stated that the coke-oven op-erator cannot change coke combustibility by modifying oven practice. Mr. Sweetser held that the coke-oven man can change the combustibility of coke. Blast-furnace men know that coke that will burn easily with low pressure and will. come down in the regular way in the furnace can be pro-duced from a given mixture of coal. His idea of the combustibility of coke is the rate of flow through the com-bustion zone of the blast furnace. If the coke does not pass through in normal manner it is highly incombustible. H. J. Rose of the Koppers Co., Pittsburgh, objected to being pinned down so closely on this phase of the com-bustibility and incombustibility of coke. Coke-oven men are frequently obliged to change oven conditions to make a coke which gives blast-furnace men what they want. The size of the coke and the screening have an important bear-ing on combustibility, and there are many cases on record where by simply changing the different sizes of the coke, everything worked smoothly, and that is a much more combustible coke.

Jan 1, 1927

THE first session of this meeting was held Tuesday evening, in the chamber of the Common Council, the President, Mr. David Thomas, in the chair. Mayor Carroll, of Troy, gave a cordial welcome to the Institute, which was responded to, on behalf of the Institute, by the first Vice-President, Mr. R. W. Raymond. The Council reported the names proposed for membership with recommendation for election. The following named gentlemen were duly elected: Anthony, J., . .Williamstown, Pa. Babcock, George, . . .Troy, N. Y. Blake, Theo. A., . . . . . . Sa n Francisco, Cal. Blossom, T. M., . . . . . . New Pork. Boalt, James A., . . .San Francisco, Cal. Bowman, Amos, . . . . San Francisco, Cal. Chester, Prof. A. H., . .Clinton, N. Y. Dewey, C., . Pittsfield, Mass. Dock, Gilliard, . Shamokin, Pa. Emerson, O. D., . .New York. Endres, John J., . .Pittsburgh, Pa. Firmstone, Frank, . Easton, Pa. Fowle, W. B., . Philadelphia, Pa. Frazier, Prof. B. W., . . .Bethlehem, Pa. Gardner, George A., . New Pork. Goodyear, Watson A., . .6an Francisco, C al. Griswold, Chester, . Troy, N. P. Griswold, J. A.,* . . .Troy, N. Y. Hague, J. D., . . .San Francisco, Cal. Hahn, 0. H., . .Eureka, Nev. Harkness, T. C., . . . . . . Wilkes-Barre, Pa Harris, Samuel, . . .Hudson, N . Y. Henry, &. T., . Oxford, N. J. Holley, A. L., . .Brooklyn, N. Y. Howe, H. W., . . .Troy, N. Y. Hunt, Dr. T. Sterry, . Boston, Mass. Jannet, J., . Troy, N. Y. Knapp, John A., . .New Pork. Laughlin, Henry A., . . .Pittsburgh, Pa.

By H. L. Riley, B. W. Gandrud

A froth flotation unit was added to the DeBardeleben Coal Corporation&apos;s Empire washer at Empire, Alabama, in the fall Of I94O following an investigation of possible ways and means of recovering coal values from settling-tank overflow or slurry. Officials of the DeBardeleben corporation hoped that some practical and reasonably economical way could be found for recovering fine coal from overflow water, although there had as yet been very little progress along this line in the Alabama coal fields. The Bureau of Mines was asked to cooperate in the project through its Southern Experiment Station, at University, Alabama. This paper presents a brief description of the process and the installation that resulted from the investigation of the overflow water or slurry problem at the Empire mine. The experimental data include&apos; as a Part of this Paper were obtained during the course of the investigation in 1940 Since that time, however, the flotation unit has been running more or less continuously without significant operational changes and is still Performing pretty much in accordance with the data obtained in 1940. Flowsheet at Empire and Type of Coal Treated The Empire mine is developed on the Black Creek bed near the the border of the Warrior field. The coal in this bed is extremely low-ash and although there is an almost complete absence of bone coal and partings, the bed is so thin that, with mechanized mining, a high percentage of rock from roof and floor inevitably gets into the run-of-mine coal. The thickness of the Black Creek bed throughout the part of the Warrior field in which it is mined extensively is rarely over 30 in. and probably would average about 25 in, the coal is of the high-volatile A rank and of excellent quality, but as a result of admixture of roof and floor material, the run-of-mine product usually contains I ; to 20 pct rock by weight. he following is a proximate analysis on an "as-received " basis of a typical seam sample from the Empire mine:&apos; moisture, 3.0 pet; volatile, 34.6 fixed carbon 58.3; ash, 4.1 This sample shelved 15,070 Btu per pound and 0.9 pct sulphur on a moisture-and-ash-free basis. In the Empire preparation plant the lump sizes above 3 in. are removed and hand-picked on a Marcus conveying Screen, the 3 to ? -in. size is removed by vibrating screens and washed in two Montgomery single-cell jigs, and the ?-in. to o slack is cleaned on four diagonal

Jan 1, 1949