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By A. F. Crawley

The densities of some liquid Pb-Sb alloys up to 11 wt pct Sb and Pb-Sb-& alloys up to 10 pct Sb/10 pct Sh have been determined by a pycnometric technique over a temperature range of about 130°C above their melting points. The data given are accurate within 0.05 pct. Density is shown to vary linearly with temperature , and equations relating these quantities have been formulated. Molar volumes calculated from the density data indicate that volumetric deviations from ideal mixing are undetectable within the limits of experimental error. A continuing research program into some fundamental physical properties of liquid metals is being pursued at the Mines Branch, Department of Energy, Mines and Resources, Ottawa, Canada. This work has received support from the Canadian Zinc and Lead Research Committee in cooperation with the International Lead and Zinc Research Organization. This paper, which reports some density data for Pb-Sb and Pb-Sb-Sn alloys, follows previous work from this laboratory on lead, tin, and Pb-Sn alloys.' Of previous data from others, Greenaway2 and Sato and Munakata3 have reported results on Pb-Sb alloys. No previous work has been published on the ternary Pb-Sb-Sn alloys, reported here. EXPERIMENTAL METHOD Densities were measured by a pycnometric technique which has been described in detail and appraised for accuracy in earlier Mines Branch reports.475 Fig. 1 shows the densitometer with the pycnometer in position for a run. The pycnometer is also shown in some detail. The pycnometer of dense, high-purity graphite, about 14 cu cm in volume, was carefully machined to a uniform, smooth finish. The height was measured by a depth micrometer and the diameter by fitting precision gage blocks between steel balls.' In each case several readings were taken, and the final results were considered accurate within 0.01 pct. The resulting volumetric uncertainty together with small inaccuracies in the coefficients of linear expansion of graphite lead to a maximum systematic uncertainty in the method of ±0.03 pct. As shown in Fig. 1, the pycnometer lid is a threaded cap. Thus, the charge, a cylinder of the alloy, can easily be inserted and the solidified metal can readily be removed after a run. The dimensions of the cylindrical charge are chosen to ensure that, once molten, the metal will not only fill the pycnometer completely but will discharge an excess into the excess-metal float chamber. AS the temperature is increased above the melting point, the volume of metal in the excess chamber increases until the system has equilibrated at the desired temperature. At this point, the excess chamber is moved to one side by twisting the shaft F, leaving a fixed volume of liquid metal in the pycnometer. This volume of fluid is readily calculated using measured coefficients of linear expansion of the graphite which expands anisotropically. The associated weight of fluid is determined as the weight of the solidified metal removed after the furnace has cooled down. Alloys were prepared from 99.997 pct Pb, 99.999 pct Sn, and 99.999 pct Sb, being melted by an electric furnace in a graphite crucible and poured into graphite molds. Several density specimens of the same nominal size were machined from each ingot, and, by comparing specimen weights, relative differences in specimen composition resulting from segregation in the ingots could be detected. In this way, segregation was found to have occurred in Pb-Sb alloys at compositions beyond the eutectic (11.2 pct Sb) and this

Jan 1, 1969

By K. E. Brown, A. R. Hagedorn

A 1,500-ft experimental well was used to study the pressure gradients occurring during continuous, vertical, two-phase flow through 1-in., 1 1/4-in. and 1 1/3-in. nominal size tubing. The test well was equipped with two gas-lijt valves and four Mathak electronic pressure transmitters as well as with instruments to measure the liquid production rate, air injection rate, temperatures and surface pressures. Tests were conducted for widely varying liquid flow, rates, gas-liquid ratios and liquid viscosities. From these data, an accucrate pressure-depth traverse was construcred for each test in each of the three tubing sizes. From the results of these tests, correlations have beer] developed which allow the accurate prediction of flowing pressure gradients for a wide variety of tubing sizes, flow conditions, and liquid properties. Also. the correlations and equations which are developed satisfy the necessary condition that they reduce to the relationships approprate to single-phase flow when the flow rate of either the gas or the liqutid phase becomes zero. All the correlations involve only dimensionless groups. which is a condition usually Sought for in similarity analysis but not always achieved. The correlations developed in this study have been used to calculate pressure gradients for pipes of larger diameter than those upon which the correlations are based. Comparisons of these calcuclaed gradients with experimetally determined gradients for the same flow conditions obtained from the literature indicate that extrapolation to these larger pipe sizes is possible with a degree of accuracy sufficient for engineering calculations. The extent of this extrapolation can only he determined with additional data from larger pipe diameters. INTRODUCTION The accurate prediction of the pressure drop expected to occur during the multiphase flow of fluids in the flow string of a well is a wideiy recognized problem in the petroleum industry. The problem has been brought even more into prominence with the advent of tubingless or slim-hole completions which use small-diameter tubing. Many of the correlations which give reasonably accurale results in the lager tubing sizes are greatly in error when applied to small-diameter conduits. Small-diameter conduits are defined as 1 1/2-in. nominal size tubing or smaller. The study of the pressure gradients which occur during multiphase flow of fluids in pipes is exceedingly complex because of the large number of variables involved. Further difficulties relate to the possibility of numerous flow regimes of widely varying geometry and mechanism and the instabilities of the fluid interfaces involved. Consequently, a solution to the problem by the approach normally used in classical fluid dynamics based on the formulation and solution of the Navier-Stokes equation has not been forthcoming. This is primarily the result of the nonlincarities involved and the difficulty of adequately describing the boundary conditions. As a result of the foregoing, most investigators have chosen semi-empirical or purely empirical approaches in an efford to obtain a practical solution to the problem. Much of the previous work in this area was done in short-tube models in the laboratory. A number of problems arise, however, when attempts are made to extrapolate these laboratory results to oilfield conditions where a much longer tube is encountered. In those few studies where data taken in long tubes were utilized, the data covered only a limited range of the variables, and as a result inaccuracies are introduced when the correlations are extended outside the range of the original data. Also, as a consequence of the limited amount of data available for these studies, the effects of several important variables were overlooked. The problem of predicting the pressure drop which occurs in multiphase flow differs from that of single-phase flow in that another source of pressure loss is introduced, namely, those pressure losses arising from slippage between the phases. This slippage is a result of the difference between the integrated average linear velocities of the two phases, which in turn is due to the physical properties of the fluids involved. In contrast to single-phase flow. the pressure losses in multiphase flow do not always increase with a decrease in the size of the conduit or an increase in production rate. This is attributed to the presence of the gas phase which tends to slip by the liquid phase without actually contributing to its lift. Many investigators have attempted to correlate both the slippage losses and the friction losses by means of a single energy-loss factor analogous to the one used in the single-phase flow problem. In an approach of this type, hourever, many of the important variables, such as

Jan 1, 1966

By R. T. DeHoff

A new approach to the measurement of the size distribution of particulate structures imbedded in opaque bodies is developed. The method is based upon the assumption of a general two-parameter distribution curve, and the estimation of these two parameters from three well-known counting measurements made upon metallogvaphic sections. The total number of particles in the system is also a product of the analysis. Application of the method with the assumption of the logarithmiconorma1 disfribution function is developed in detail. A complete description of the geometry of a particulate structure requires the determination of the size distribution of particles. The problem of estimating the size distribution of particles of a particular phase in a multiphase system, or the grain-size distribution in a homogeneous system, has been approached by many investigators.'-'0 All of the solutions proposed by these investigators share the following characteristics. a) A minimum of several hundred particle sections in the microstructure must be examined, and some characteristic dimension recorded, such as area,3'5 intercept length,6"9 or diameter.1'2'4'10 b) The resulting data must undergo a series of fairly complex calculations to generate the empirical histogram which describes the size distribution in three dimensions. c) In order to manipulate the result, the histogram must be fitted to some assumed mathematical formula, using the attendant statistical procedures. d) With two notable exceptions,8,10 the particles must be spherical. The measurements and calculations involved are in general very tedious and time-consuming, with the logical result that much effort has been expended in the development of equipment which will perform these tasks automatically and semiautomati-cally.9,11-15 considerable success has been achieved in this area, but the equipment is in general expensive, and usually places stringent requirements On the quality of microstructure which can be reliably analyzed. In laboratories which do not possess such equip- ment, the analysis of geometry is usually limited to measuring total properties of the microstructures, such as volume fraction and interfacial area, because the measurements required are much simpler to make. The determination of size distributions rarely is undertaken. The development which is presented in this paper permits the estimation of size distributions of three-dimensional structures from the same simple counting measurements which are required to determine the surface area and volume fraction of the particulate structure, and one other counting measurement. The basic approach that is used is to assume a general mathematical form for the distribution, which is described by two parameters (as the normal distribution is described by assigning values to the mean and the standard deviation), and then estimate these two parameters from the results of the counting measurements. The introduction of a third counting measurement also permits the evaluation of the number of particles per unit volume, Nv.

Jan 1, 1965

By Harold L. Overton, Leonard B. Lipson

The first paper in this series1 outlined practical methods for applying the theory of steady-state flow of an ideal Bingham plastic liquid through a circular pipe and axially through a stationary concentric annulus to the enginekring analysis of friction loss problems. In the present paper the properties of another useful rheological model, the pseudoplastic generalized Newtonian liquid, are considered. The terminology applied to the rheological models is derived from the following classification of rheological models. The term "generalized Newtonian" is a class designation applied to models which do not have yield points but which exhibit a dependence on shear rate. The term "pseudoplastic" applies to a sub-group of models within this class which exhibit a decrease in "viscosity" with increasing shear rate. The term "power model" refers to a mathematical model proposed for describing the behavior of the pseudoplastic liquid. This model is of interest since certain of the salt saturated, oil emulsion, and "low solids" drilling fluids, inverted emulsion- and oil-base drilling fluids, aqueous gels, gelled crudes and blocking agents employed in hydraulic fracturing operations are of this type. The present treatment considers the equations describing steady-state Poiseuille flow through a circular pipe and a stationary concentric annul us, and Couette flow between concentric rotating cylinders for a particular pseudoplastic model. As in the previous paper' it is demonstrated how these equations can be applied to engineering calculations of friction losses. Graphical procedures for recovering the various flow curves and cxample calculations are included. A method for simplifying turbulent-flow correlations is also proposed. PROPERTIES OF PSEUDOPLASTIC GENERALIZED NEWTONIAN LIQUID In contrast to the Bingham plastic the generalized Newtonian liquid is yield point-free. However, in the flow region the relation between stress and rate of shear is not linear as it is with ordinary Newtonian fluids. If the stress increases with shear rate at a less than linear rate the system is called pseudoplastic. While there is no yield point in this system, the Bingham advocates' coined the term pseudoplastic to distinguish this kind of behavior from Bingham plastic behavior. For the pseudoplastic a plot of flow rate vs friction loss or rpm vs torque, from pipe flow or rotational viscometer measurements, respectively, generally has three qualities: (1) it can be clearly extrapolated toward the origin; (2) there is very little slope at the origin. This accounts for the high apparent viscosities at low mixing and pumping rates; and (3) the flow curve possesses a continuous curvature which gradually diminishes as the shear increases. Rheological measurements on a pseudoplastic liquid can be easily misinterpreted as indicating Bingham plastic behavior. A typical case in point is illustrated in Fig. 1. These data were obtained from measurements on an oil-emulsion mud using a commercially available rotational-type viscometer (Model 35 Fann V-G meter). Applying the "two-point"* method3 gives a plastic viscosity of 17 cp and a yield point of 24 lb/100 ft2; at the same time weighting material settles very easily in this system. This illustrates that it is not possible to distinguish between the pseudoplastic and the Bingham plastic from only two data points. It is possible to determine qualitatively which model is more appropriate by a combination of dynamic and static measurements. Experience indicates that the simplest criterion for the Bingham plastic liquid is that the calculated dynamic yield point should be of the same magnitude as the measured gel strengths. For the oil-emulsion drilling fluid illustrated in Fig. 1, a value of 4 lb/100 ft2 was obtained for gel strengths measured

By D. D. Porter, H. G. Carlevato

Blasting to prepare orebodies for in situ leaching usually involves extraordinary conditions which sometimes require special and innovative techniques. To date several unusually large blasts have been made for leaching with results that are very encouraging. Among the factors considered when designing these large blasts are orebody shape and depth, rock properties, vibration and damage potential, loading logistics, and safety. All of these factors, and others, are discussed with an effort made to put each of them into its proper perspective.

Jan 1, 1974

By R. H. Adams, A. M. Khan

The Huntington Beach oil field is on the Pacific Coast, southeast of the City of Los Angeles (Fig. 1). It lies both onshore and offshore. Most of the onshore section is operated by Standard Oil Co. of California, WOI. The Tar reservoir is of upper Pliocene age, about 200 ft thick, and consists principally of fine-grained, unconsolidated, somewhat shaly sand, with thin inter-bedded shale stringers throughout (Fig. 2). The reservoir is a broad, highly faulted, elongated anticline, with an areal extent of about 370 acres. Most of the faults bisecting the structure are normal, trend north-south, and are the main cause of reservoir discontinuity (Figs. 3 and 4). From 1964 to Dec., 1967, 259 steam stimulations were performed on a total of 125 Tar sand wells. Eighty-six new wells were drilled and steam stimulated. Of the total, 96 have been stimulated twice, 34 three times and 3 four times. During this same period, a two-injector steam drive pilot has been in progress. The response obtained from this project has been compared with the response to cyclic stimulation. This paper presents an analysis of the field observations for the two methods of thermal recovery. History of Development Drilling to the Tar pool commenced in 1924 with an initial well production of 40 to 50 B/D of 12o API gravity oil. Complete primary development of the pool has been spread over several years. Approxi- mately 40 wells were drilled during the first phase of development, which was completed in 1945. The subsequent primary development started in 1960 with initial well productions of 30 to 40 B/D oil. Thirty-seven wells were completed in the Tar pool during this phase. For the most part, slotted, gravel flow packed liners have been used in the wells in this pool. A cyclic steam stimulation pilot was initiated in March, 1964. Based on the very successful stimulation in the pilot area, the cyclic stimulation project was expanded to include all of the Tar pool wells producing at the end of 1965 (Fig. 5). Also, a development drilling program was begun at this time. To date, 86 new wells have been drilled under this program. The number of wells drilled each year in this secondary phase of development is also shown in Fig. 5. New Well Completion Practices Most of the new wells have been completed to produce from both the Upper and Lower Tar zones. Generally, a casing stub is cemented from the top of Lower Tar to the base of clean Upper Tar sands to exclude intermediate water-bearing sands. The water string is then cemented from the top of Upper Tar to about 1,500 ft with neat cement and 30 percent silica flour. The annulus from 1,500 ft to surface is then filled with a petroleum-based gel through a high-temperature port collar. Once again, a history of sand-free production dictated the use of 60-mesh gravel flow packed liners. The Upper and Lower Tar

Jan 1, 1970

By T. Egleston

The origin of gold both in placer deposits ancl in veins, and especially the origin of nuggets, has been the subject of repctated discussions and investigations, which have been recently brought to my attention by several extremely interesting specinlens sent to me for examination, and mare especially by the one exhibited at the meeting of the Institute in February, 1880.* In the year 1874 I made some exan~inations of the hydraulic mines of California, and was very nluoh struck with the distribution of the gold throughout these deep placers, which were almost invariably poor on'the surface, while gradually growing richer towards the bedrock. The constant presence of fossil wood, and the large quantity of organic matter contained even low down in these beds, was also remarkable. Not being satisfied with the various theories advanced to account for the formation of these deposits, I began an investigation early in the pear 1879 on the conditions of solubility of gold and the causes of the loss in working gold ore in a large way. The researclles which I have undertaken show that gold must be considered a soluble rather than an insoluble metal, and that the conditions of solution are such as will be found anywhere where gold is likely to occur, and the solution may take place even under the ordinary circumstuncee of surfiace drainage, and may be going on freely even where the presence of gold has never been suspected, and that there are causee enough in nature to produce the solution of the gold in sufficient quantities to account for all the phenomena of both the vein and placer formations. The general theory with regard' to the formation of these placer deposits and nuggets has been that they were the result of the deatruction of pre-existing. vein-matter, which does not accord with the fitcts as sholvn in the deep placer deposits. The gold in such case would be distributed in layers of unequal richness throughout

Jan 1, 1881

By J. Richter, D. Schulze

J. Richter and D. Schulze (Deutschen Akademie der Wissenschafte zu Berlin)—Introduction. In a recent paper R. G. Garlick and H. B. Probst reported on experimental results of investigations of room-temperature slip in zone-melted tungsten single crystals.17 In the paper it was pointed out that slip lines could be detected with an optical microscope only after about 10 pet plastic strain of the crystal. In our investigations we could observe slip lines in tungsten single crystals of defined orientations already with an elongation of 0.02 to 0.03 pet.18"9 Experimental Technique and Results. The tungsten single crystals were produced from 4 to 5 mm sintered rods* as starting material by electron- beam zone melting. With single-zone-pass melting a speed of 0.5 mm per min was used, while three-pass melting could be handled at a speed of 3 mm per min. Crystal axis orientations were located in the shaded area of the stereographic triangle, see Fig. 6. Orientation 1 is located at about 18 deg and orientation 2 at about 5 deg on the great circle from [011] to [ill]. This corresponds approximately to the orientations P and M referred to by Garlick and Probst. Our single crystals had a length of about 70 mm and were profiled solely by electrolytic means, leaving grip ends at both ends of the crystals. Between the latter, a cylindrical crystal of 45 to 50 mm length and about 2.4 mm diam was obtained. The crystals were deformed at room temperature in a commercial tensile-testing machine to obtain a strain of 0.02 to 5 pet. The average strain rate e = eP/t for all tensile tests amounted to approximately 10 -6 to 10-5 per sec, with ep representing plastic strain and t the duration of applied stress. In Fig. 7 a crystal is shown elongated by 0.03 pet. The picture was obtained by means of an optical microscope. Figs. 8 and 9 give electron-microscopic pictures of slip lines of crystals elongated by 0.07 and 1.1 pet, respectively. For crystals with the orientation 1, see Fig. 6, only the two main slip systems (101)[111] and (110)[111] were found. With the crystals of group 2 the two main slip systems are again evident, with

Jan 1, 1965

By P. H. Thornton

MaNY intermediate phases are solid solutions which have a solute-solubility range greater than 3 at. pct. These phases, which are generally very strong and often have simple crystal structures, are usually extremely brittle so that specimens of simple shape cannot be produced by the usual mechanical-deformation techniques. Furthermore, single crystals of reasonably uniform composition are difficult to grow by the Bridgman technique because the phases generally form by a peritectic reaction, which causes pronounced segregation. In this note, a technique is described for the preparation of thin-rod specimens of brittle intermediate phases, which may be used for physical-property studies such as resistivity changes' and for the conversion of such rods into single crystals. The method has been used for the preparation of rod single crystals of the phases and Ingots, of about 100 g weight and 11 mm diam, were made by melting together the appropriate amounts of high-purity materials (usually 99.999 pct) in sealed

Jan 1, 1967

By R. B. Sosman, J. C. Hostetter

It is well known that ferric oxide, Fe2O3, is paramagnetic, while magnetite, Fe3o4, is classed among the highly ferromagnetic substances. But magnetic data on oxides intermediate in composition between Fe2o3 and Fe3O4 have been almost completely lacking. Fe2O3 and Fe3O4 form a solid-solution series, according to present evidence.' In this series the properties change continuously from Fe2O3 toward Fe3O4, as the percentage of FeO increases from zero toward 31.03, which is the percentage in magnetite. It is possible that there is a break in the series near Fe3O4, but it has not yet been possible to establish the existence of such a break experimentally. The occurrence of solid solution in this series is shown by the dissociation pressure, or oxygen pressure in equilibrium with the oxides, which falls continuously over the range from Fe2O3 to Fe3O4. The oxygen-pressure curves at 1100" and 1200" are shown in Fig. 1. The existence of solid solution is also demonstrated by the continuous change in optical properties from Fe2O3 over to a composition containing about 18 per cent. FeO, at which point the opacity of the oxide becomes so great that it is impossible to obtain measurements at higher percentages of ferrous iron. Natural oxides of iron intermediate in composition between Fe2O3 and Fe3O4 are much more common than is generally supposed. If a mineral oxide is not strongly attracted by a small hand magnet and if it gives a red streak, it is usually labeled "hematite." If it is strongly attracted by the hand magnet it is usually labeled "magnetite" without further tests. As we shall show later, oxides containing from 1 up to 31 per cent. FeO can be thus erroneously lumped together as "magnetite." It is a fact, nevertheless, that the great bulk of natural oxides of iron lie fairly near either Fe2O3 or Fe3O4 in composition. The reason will be

Jan 1, 1918

By Ray W. Ballmer

"For his leadership in developing and managing large, complex, and technically innovative mines, particularly the outstanding and successful Bougainville mine and for his lecture, 'The Moving Targets of Mine Development '. " Recipient of the 1981 D. C. Jackling Award

Jan 1, 1982

By J. W. Spretnak, R. Speiser, A. M. Adair

THERE are sufficient arguments and evidence to indicate that boron should be adsorbed to existing austenite grain boundaries during the austen-itizing treatment. Accordingly, it is possible that boron contributes to the hardenability of heat-treatable steels by the reduction of the interf acial energy of austenite grain boundaries, at which sites are nucleated heterogeneously the decomposition products of austenite. Such a reduction in interfacial energy would reduce the total energy that can be borrowed in these heterogeneous nudeation processes and thus retard the initiation of transformation. This investigation was undertaken in an attempt to determine the effect of boron on this interfacial

Jan 1, 1956

By M. E. Straumanis, J. -P. Krumme

In basic ([KOH + KCl] with a total polarity of 2) or acidic (2N H2SO4) electrolytes and at anodic current densities of more thun 2 to 4 ma per sq cnz, n-type GaAs single crystals of lozo resistivity preferentially dissol~je forming etch tunnels with triangular or civc~ilay cross sections and of a width between 0.5 arid 5 p. These etch tunnels are oriented along any one of the four possible (111) directions of GaAs. However, their growth occurs only in one direction of a given (111) whick apparently is determined by the atomic sequence Ga —As (and not the rezlerse) in respect to an individual valence bridge in the crystal. It is concluded from comparison with the cubic lattice structure of GaAs that the etch tunnels represent macroscopic evidence for the tetrahedral bonds and their polar properties. If the anodic current density is increased the tunnel fomation results in the development of a fibrous surface layer consisting of GaAs. The latter separates frorn the substrate (in an anodic s~irface disintegration process) by the growth pressure of an As,0, filnz forming in the interior of the fibrous layer, 100 to 200 µ under the surface, at more than about 50 ma per sq cni. The fibrous GaAs film has the same crystallographic orientation as the substvate and represents a skeleton of the original crystal. Since the etch-tunnel density in a separated GaAs layer is about 108 c?n-', and the etch tunnels develop only along (111) in a given polar direction, it is assurraed tlmt the dislocations have no influence on the growth of these tunnels. ElECTROLYTIC treatment of smooth surfaces of poly- and single-crystalline GaAs at high anodic current densities causes the formation of porous surface layers.' This phenomenon suggests comparison with effects being observed with magnesium,' indium,, gallium,4 and aluminum5 and known as "anodic disintegration". The purpose of the present paper is to explore and to explain the reasons for the formation of such surface layers on GaAs and, in particular, to investigate the influence of the lattice polarity of this III-V compound semiconductor in the (111) direction on the anodic dissolution behavior. GaAs SINGLE CRYSTALS For the experiments described below GaAs single crystals from the Monsanto Co., St. Louis, Mo., were used. Their impurity levels were below 1 ppm and their dopant levels between 1 and 100 ppm. They were grown in (111) using the Czochralski or the gradient-freeze technique. The crystals had n-type conductivity and electric resistivities between 1 and 5 ohm-cm. EXPERIMENTAL The GaAs single-crystal rods were cut perpendicularly to (111) into wafers of about 1 mm thickness using a wire-blade crystal slicer and an aqueous slurry of Sic or a diamond saw. The orientation of the faces of these wafers were checked by Laue back-reflection patterns. If there was a deviation from (111) the faces were abraded under a certain angle using grinding paper and distilled water. The damaged surface layer was removed from each crystal by chemical etching with a mixture of 1HF:1HNO3: 1H20 or 2HF:1HNO3:2HAc (glacial). {110) faces were obtained by mechanical cleavage, producing surfaces which did not require a further treatment. The GaAs wafers were mounted using "alligator" clamps instead of soldered electrical contacts.' Only the bare crystal surfaces were dipped into the electrolyte. The clamps were coated with insulating wax to prevent any contact with the electrolyte. The experiments were carried out in aqueous 2 N H2so4,' or in an aqueous solution of KOH and KCl1 (1 mole KOH + 1 mole KCl in 1000 cu cm solution). Anodic current densities up to several hundred ma per sq cm were applied for periods between 30 sec and 2 hr. For the purpose of investigating the initial steps of disintegration the anodic current density applied never exceeded 20 ma per sq cm. The films which partially separated from the anodic surfaces under high-field conditions were treated with KOH to further their detachment by dissolving the As2O3 formed. The washed and dried films were pasted to strips of filter paper, and Laue pictures were made. The back-reflection patterns obtained were compared with those of the original anode surface before and after anodic dissolution. Furthermore, space reciprocal lattices7 were constructed from asymmetric rotation crystal patternsa which permitted the determination of the crystallographic orientation of the detached films of the corrugated anodic surfaces. The disintegration products were identified from assymmetric powder patterns.8 The polarity of the {111) faces was determined by chemical etching with mixtures of 1HF:1H2O2(30 pct): 2H2O or 1HNO3:2H2O. Different patterns on each of two inverse (111) sides appeared.'-l8 The correlation of these patterns to the Ga{111) or the As(111) side has already been established by the use of light figures,18-20 by X-ray diffraction near the absorption edges of gallium and arsenic,'lmZ4 and by LEED measurements.25 The geometric structure of these surfaces and the interior of the anodically attacked crystals were observed and photographed with a high-power microscope using oil immersion objectives up to magnification of X1720.

Jan 1, 1968

By A. N. Roberts, N. W. Stump

New developments in on-stream analysis using immersed radioisotope gages including results from plant installations are described. The control of grinding and flotation using a small digital computer has been complemented by this development. A control scheme for grinding, which is based on maximum throughput at constant product size, and preliminary work in flotation control are also outlined.

Jan 1, 1975

By F. W. Schroeder

AT the annual meeting of the Institute 2 years ago, a paper,1 " Requirements of Refractories for Open Hearths," was presented by F. W. Davis and G. A. Bole of the U. S. Bureau of Mines. In a brief foreword, D. A. Lyon stated that the paper was not to report the results obtained but rather to present an outline to serve as a basis for discussion. The essential parts of an open-hearth furnace were described and the conditions under which they operate. Some constructive discussion followed the reading of the paper. One of the first fellowship investigations undertaken by the Bureau of Mines in 1924 under the cooperative agreement with Carnegie Institute of Technology, through the Metallurgical Advisory Board, was to determine service conditions of open-hearth refractories. The present paper gives the results of this work which was done in the Pittsburgh district and was in charge of the authors. Material contributions in the form of data were contributed by E. N. Bauer, J. W. Campbell, G. H. Pfeiffer and A. Grodner, Carnegie Institute of Technology research fellows. The study covered 18 mos.

Jan 7, 1926

By J. L. Wyatt

THE smelting of ilmenite to produce a slag rich in titanium, with pig-iron as a byproduct, introduces new concepts in electric smelting metallurgy. Titanium slags are characterized by low electrical resistance, thereby requiring a different type of electric furnace operation, and power supply sources substantially different from those encountered in normal steel melting and siliceous ore smelting furnaces. This paper describes special apparatus for determining specific electrical resistivity of titanium slags, and reports the values obtained on slags encountered in the process of smelting ilmenite ores. In an induction furnace under conditions approximating normal furnacing operation, 25 general heats and 6 special standardization and comparison heats were run. Results indicate relatively low resistivity. Resistivity depends primarily on slag composition, and, to a lesser degree, on temperature. During the summer of 1947 a cooperative project between the National Lead Co. and the Bureau of Mines was conducted at Boulder City, Nevada, in the Electrometallurgical Laboratories of the Bureau. The project involved smelting of ilmenite ores in electric furnaces, and has been reported in detail.' The author participated as a member of the staff of the National Lead Co. during the entire campaign. One outstanding characteristic of the titaniferous slags, their apparently excellent and variable electrical conductivity, was considered sufficiently important to warrant further study. Although little electric smelting of iron ores has been done in the United States, a certain amount of information is available for comparative purposes. Personal experience in smelting siliceous iron ores in electric furnaces furnished further information for comparison. In general, silicate slags are relatively poor conductors of electricity. Current flow during smelting operations may be maintained through a floating layer of coke on top of the slag bath, or through a bath of molten iron, beneath the slag. Silicate slags are not sufficiently conductive to furnish a path for current passage when normal furnace voltages are used. Experimental smelting of a silicate iron ore was undertaken for comparative purposes. A fluid melt was not obtained until the FeO content was reduced to 15 pct. The resistivity increased as the FeO content decreased, FeO compounds being the most conductive of the various oxides in such a normal slag system. The converse appears to be true in slags containing large percentages of TiO2. It has been found that titanium slags become molten with FeO percentages in excess of 30 pct, and that the conductivity becomes generally better as the FeO con-tent of the slag diminishes. This phenomenon was demonstrated in the furnacing operations at Boulder City. During the initial smelting period furnace electrodes could be held immersed several inches in the slag, with tap selectors set for a no-load voltage of 70 v. As the FeO content decreased, the furnace electrodes would "walk up," until at one point in the process the tips would break the surface and arc on top of the slag. This was undesirable since direct arcing caused losses of important flux additions. The slag compositions under study at that time were such that losses due to surface arcing sometimes caused viscous slags to be formed. Forcing the electrodes into the slag bath by manual control to prevent surface arcing resulted in excessive power input and lack of control. Suitable low voltages were not available. Measurement of the electrical resistivity of titanium slags at various operating temperatures and slag compositions was undertaken. It was believed that this information would be of use in the design of electric furnaces suitable for smelting ilmenite, with voltages, electrode sizes, and electrode spacing adapted specifically to titanium slags.

Jan 1, 1951

By G. L. Simard, D. J. Salley, J. Chupak

DITHIOPHOSPHATES and xanthates are the principal collectors for sulphide minerals, and consequently any knowledge of mineral-collector systems of this type is of value. In the present investigation an attempt was made to obtain information on the interaction of a typical dithiophosphate with galena. In carrying out this study, radioiso-topes, so much discussed in the past few years,', ' were extensively employed. By using radioactive dithiophosphate synthesized from radioactive phosphorus, a rapid and sensitive analytical procedure G. L. SIMARD is in the Research Division, Stamford Research Labs., American Cyanamid Co., Stamford, Conn.; J. CHUPAK, formerly in the Research Division, Stamford Research Labs., is now at Camp Detrick, Frederick, Md.; and D. J. SALLEY is in the Research Division, Stamford Research Labs. AlME New York Meeting, Feb. 1950. TP 2815 B. Discussion (2 copies) may be sent to Transactions AlME before April 30, 1950. Manuscript received Oct. 17, 1949. was at hand. This permitted determination of such important quantities as the rate of uptake of dithiophosphate by the mineral, the amount existing at equilibrium on the mineral surface and in the solution, and the desorption of the agent from the surface. Such measurements were possible even on single crystals of galena. In addition the exchange of dithiophosphate between the solution and the sorbed phase was examined, a matter which could be accomplished only by the use of isotopes. It is desired to point out at this time that throughout this paper the term "sorption" has been employed to designate the uptake of agent by mineral, without implication as to the nature of the process by which the uptake was accomplished. Experimental Materials: Galena: The galena was from the Tri-State district. For studies on ground mineral four preparations were used during the course of the investigation. These were prepared from selected large crystals by wet grinding in order to reduce surface oxidation. Alcohol was chosen as a convenient medium for this purpose. The ground mineral was then fractionated by sedimentation in alcohol, dried by evacuation, and stored in a nitrogen-filled desiccator. Data on the preparations are tabulated in table I. The size analysis indicated that the areas of the preparations were of comparable magnitude, even though the absolute values may be somewhat incorrect. Dithiophosphates: Nonradioactive dithiophbsphate (di-isopropyl or di-secondary butyl) was obtained by purification of a commercial product. An aqueous acid solution of the agent was extracted with petroleum ether, the ether layer dried, and the dithiophosphate precipitated as ammonium salt with anhydrous ammonia. Several repetitions of this process resulted in a nearly colorless, flaky product of good purity. (General formula (RO,)PSSNH,). Radioactive dithiophosphate was synthesized by heating radioactive elementary red phosphorus* • For early experiments (1943 to 1944), the elementary red phosphorus was obtained from the cyclotron group at the Crocker Radiation Laboratory of the University of California. Berkeley, through the courtesy of Dr. Joseph W. Hamilton. For more recent work (1946 to 1949). the elementary radioactive Phosphorus has been supplied by the Oak Ridge National Labarotories on allocation from the U. S. Atomic Energy Commission. with sulphur at 270" to 300°C to produce radioactive P,S,. The latter was then treated with the desired purified alcohol (isopropyl or secondary butyl) at 60" to 80°C to form the dithiophosphoric acid derivative. Purification was effected in the same manner as for the nonradioactive material. The effectiveness of the purification method was established by the isotopic dilution method." The same technique was used to show that only negligible decomposition of neutral or of carbonate solutions of the dithiophosphate took place over a period of a day; this was true whether or not galena was suspended in the solutions. Procedures: Radioactivity: The activity of a solution was obtained by counting with a small glass-jacketed, silvered Geiger counter, using a conventional scaling circuit.' Crystals and other solids were counted under a bell-shaped, mica-window counter tube. Sufficient counts were made so that the probable error of counting was of the order of +I-3 pct. The specific activity in terms of counts per minute

Jan 1, 1951

By J. Chupak, D. J. Salley, G. L. Simard

DITHIOPHOSPHATES and xanthates are the principal collectors for sulphide minerals, and consequently any knowledge of mineral-collector systems of this type is of value. In the present investigation an attempt was made to obtain information on the interaction of a typical dithiophosphate with galena. In carrying out this study, radioiso-topes, so much discussed in the past few years,', ' were extensively employed. By using radioactive dithiophosphate synthesized from radioactive phosphorus, a rapid and sensitive analytical procedure G. L. SIMARD is in the Research Division, Stamford Research Labs., American Cyanamid Co., Stamford, Conn.; J. CHUPAK, formerly in the Research Division, Stamford Research Labs., is now at Camp Detrick, Frederick, Md.; and D. J. SALLEY is in the Research Division, Stamford Research Labs. AlME New York Meeting, Feb. 1950. TP 2815 B. Discussion (2 copies) may be sent to Transactions AlME before April 30, 1950. Manuscript received Oct. 17, 1949. was at hand. This permitted determination of such important quantities as the rate of uptake of dithiophosphate by the mineral, the amount existing at equilibrium on the mineral surface and in the solution, and the desorption of the agent from the surface. Such measurements were possible even on single crystals of galena. In addition the exchange of dithiophosphate between the solution and the sorbed phase was examined, a matter which could be accomplished only by the use of isotopes. It is desired to point out at this time that throughout this paper the term "sorption" has been employed to designate the uptake of agent by mineral, without implication as to the nature of the process by which the uptake was accomplished. Experimental Materials: Galena: The galena was from the Tri-State district. For studies on ground mineral four preparations were used during the course of the investigation. These were prepared from selected large crystals by wet grinding in order to reduce surface oxidation. Alcohol was chosen as a convenient medium for this purpose. The ground mineral was then fractionated by sedimentation in alcohol, dried by evacuation, and stored in a nitrogen-filled desiccator. Data on the preparations are tabulated in table I. The size analysis indicated that the areas of the preparations were of comparable magnitude, even though the absolute values may be somewhat incorrect. Dithiophosphates: Nonradioactive dithiophbsphate (di-isopropyl or di-secondary butyl) was obtained by purification of a commercial product. An aqueous acid solution of the agent was extracted with petroleum ether, the ether layer dried, and the dithiophosphate precipitated as ammonium salt with anhydrous ammonia. Several repetitions of this process resulted in a nearly colorless, flaky product of good purity. (General formula (RO,)PSSNH,). Radioactive dithiophosphate was synthesized by heating radioactive elementary red phosphorus* • For early experiments (1943 to 1944), the elementary red phosphorus was obtained from the cyclotron group at the Crocker Radiation Laboratory of the University of California. Berkeley, through the courtesy of Dr. Joseph W. Hamilton. For more recent work (1946 to 1949). the elementary radioactive Phosphorus has been supplied by the Oak Ridge National Labarotories on allocation from the U. S. Atomic Energy Commission. with sulphur at 270" to 300°C to produce radioactive P,S,. The latter was then treated with the desired purified alcohol (isopropyl or secondary butyl) at 60" to 80°C to form the dithiophosphoric acid derivative. Purification was effected in the same manner as for the nonradioactive material. The effectiveness of the purification method was established by the isotopic dilution method." The same technique was used to show that only negligible decomposition of neutral or of carbonate solutions of the dithiophosphate took place over a period of a day; this was true whether or not galena was suspended in the solutions. Procedures: Radioactivity: The activity of a solution was obtained by counting with a small glass-jacketed, silvered Geiger counter, using a conventional scaling circuit.' Crystals and other solids were counted under a bell-shaped, mica-window counter tube. Sufficient counts were made so that the probable error of counting was of the order of +I-3 pct. The specific activity in terms of counts per minute

Jan 1, 1951

By E. Lancaster-Jones

THE gravity magnitudes obtained by means of observations with the Eötvös balance in the field are necessarily resultant or total effects due to all abnormalities of mass distribution, including even the effects due to the ellipticity and rotational motion of the whole earth. Since the object of the survey is to isolate the effects which arise solely from some particular subterranean feature, and to deduce therefrom the configuration and extent of this feature, the first step is to eliminate from the observed effects all those due to "disturbing" (i. e., unwanted) features, whether above or below the surface of the ground. The disturbing features have different characteristics, according to their situation relative to the center of the balance and to the horizontal plane through the foot of the balance, or station point; this diversity was recognized by Eötvös, who divided the total effects into so-called Normal, Terrain, Topographical, Cartographical and Subterranean effects. This classification has been adhered to by most subsequent investigators, but the writer prefers to employ the term "three-dimensional," which really indicates the essential character of the class of effect known as "Subterranean," at any rate from the standpoint of the computer of effects. Before disturbing effects can be eliminated, the features must be measured up or surveyed, whether by topographical, mining, or boring methods, and then the effects of each feature calculated and subtracted from-the total observed effects. After this the problem of interpreting the residual effects will itself necessitate the computation of the assumed feature, or even a series of trial features.

Jan 1, 1928

By E. Lancaster-Jones

THE gravity magnitudes obtained by means of observations with the Eötvös balance in the field are necessarily resultant or total effects due to all abnormalities of mass distribution, including even the effects due to the ellipticity and rotational motion of the whole earth. Since the object of the survey is to isolate the effects which arise solely from some particular subterranean, feature, and to deduce therefrom the configuration and extent of this feature, the first step is to eliminate from the observed effects all those due to "disturbing" (i. e., unwanted) features, whether above or below the surface of the ground. The disturbing features have different characteristics, according to their situation relative to the center of the balance and to the horizontal plane through the foot of the balance, or station point; this diversity was recognized by Eötvös, who divided the total effects into so-called Normal, Terrain, Topographical, Cartographical and Subterranean effects. This classification has been adhered to by most subsequent investigators, but the writer prefers to employ the term "three-dimensional," which really indicates the essential character of the class of effect known as "Subterranean," at any rate from the standpoint of the computer of effects. Before disturbing effects can be eliminated, the features must be measured up or surveyed, whether by topographical, mining, or boring methods, and then the effects of each feature calculated and subtracted from the total observed effects. After this the problem of interpreting the residual effects will itself necessitate the computation of the assumed feature, or even a series of trial features.

Jan 1, 1928