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By Paul Gordon

The distribution coefficient, k, of interest in zone refining is generally defined as the ratio of the solid to the liquid solubilities of one element in another at the normal melting point of the solvent. In practice, distribution coefficients are frequently calculated from solubilities at temperatures well below the melting point of the solvent, e.g., at a eutectic temperature. This is done because of the general lack of accurate data on the liquidus and solidus curves in most phase diagrams. The practice is equivalent to assuming that the liquidus and solidus curves are straight lines in the temperature range between the melting point of the solvent and the temperature at which data for the solubilities are known. It is recognized that the k values so derived may be in serious error; we have found evidence in recent zone-refining operations that a case in point is silicon in aluminum. The phase diagram found in the literature for silicon in aluminum indicates a eutectic on the aluminum-rich side at 12.5 at. pct Si and at 577°C,1 and a solid solubility of silicon in aluminum at this temperature of 1.59 pct.2 It also shows the liquidus and solidus as nearly straight lines from 577°C to the melting point of aluminum (660°C)1,2 The k value obtained from this data is 0.13. This is almost exactly the same as the k value (about 0.14)' obtained in a similar way for copper in aluminum. Yet we have found by mass-spectrograph analyses* of three bars of zone-refined aluminum that copper is efficiently removed from aluminum by zone refining but silicon is not. Two of the three bars of aluminum were zone-refined in our laboratories, the other in the laboratories of AIAG Metals, Inc. The former two bars, designated bars PG2 and PG3, were 30 in. long by 1 in. in diameter during refining; each was processed in a high-purity graphite boat* and kept under refining stage of the process consisted of thirty unidirectional zone traverses at rates of about 1 to 2 in. per hr, with a zone length of 1 to 2 in. At approximately the middle of the refining period a 6-in. piece of the impurity-laden finishing end of the bar* was cut off and replaced with new start- ing material. Following refining, the purest 20-in. section of the bar (obtained by discarding approximately 2 in. of the starting end and 8 in. of the finishing end of the bar) was leveled and then analyzed. The AIAG bar was 16 in. long and about 1.2 in. in diameter; it was purified by eight passes of a 2-in. zone at a rate of 1.6 in. per hr, the bar being contained in a sintered alumina boat lined with loose alumina powder of the highest purity. Data for the silicon and copper contents of the three refined bars are given in Table I. Derived data for the efficiencies of the zone-refining operations are listed in Table 11. It is clear from these two tables that the copper is removed much more efficiently—by a factor of 10 to 50 times—from aluminum during zone refining than is silicon. For example, in bar PG3 the thirty zone passes reduced the copper content from 10 to 0.02 ppm, i.e., by 500 times, whereas the same treatment lowered the silicon content by only a factor of about 16. It seem virtually certain, therefore, that the distribution co efficient, k, for silicon in aluminum is well above that for copper and is very likely not much below unity. This also implies that the solidus line on the aluminum-rich side of the A1-Si phase diagram is very probably appreciably curved near the aluminum melting point since the phase-diagram data indicate such curvature is unlikely in the liquidus.

Jan 1, 1965

By Zolfan F. Oszter

As exploration for new mineral deposits advances farther into the Canadian North, the more the design engineer is faced with the problems of cold weather conditions. This is especially true when designing belt conveyor systems for open-pit operations where the temperature in the winter may go to -40°F or below. Problems with the mechanical components and also with the belting will arise, which in turn may reduce the availability of the system. This paper outlines the problems encountered during cold weather operation and what precautionary measures must be taken into consideration in the design of equipment, as well as in the selection of materials, in order to ensure a system which will maintain production. THE conveying of ore and waste in the pit or to the processing plant poses problems during cold weather, when temperatures may drop to -4o?F or be-low. Troubles with the mechanical components, the belting or the supporting structure may arise, and this, in turn, will reduce the availability of the conveying system.

Jan 1, 1965

By T. L. Myron

In recent years increasing attention has been given to improving both the chemical and physical properties of sinter. The first step toward this goal was the production of a self-fluxing-sinter. More recently, blast-furnace operators have found that significant improvements in blast-furnace performance can be achieved by improving and controlling the physical size of the sinter. The results of full-scale blast-furnace tests have shown that blast-furnace production can be improved by using a closely sized agglomerate. The improvements obtained by the use of pellets, a closely sized agglomerate, are well known. In contrast, blast furnaces charged with sinter having a wide size spectrum have generally not yielded results as satisfactory as those from furnaces 1) * charged with pellets. Beginning in 1958, Appleby-Frodingham charged plus 3/8-inch sinter to their blast furnaces. Further tests by other companies in Canada, 2) the United States, 3) and Australia showed that blast-furnace production could be improved by about one percent when the plus 3/8-inch material in the burden was increased by one percent. Because of the promising results obtained with screened sinter, an extensive test program was initiated to determine an effective means of producing sized sinter in U. S. Steel's sinter plants. This paper describes the work done by the Applied Research Laboratory in this program.

Jan 1, 1965

By R. A. Spurling, C. G. Rhodes

SATISFACTORY metallographic sample preparation of very soft metals, such as lead and its alloys is generally difficult. The prime requisite of any technique must be that the result gives an undis-torted microstructure for the microscopist to examine. A small amount of mechanical polishing followed by a chemical or electrolytic polish is usually the most desirable way to obtain an undis-torted surface. Several chemical-4 and electrolytic3-' polishing solutions have been developed for dilute lead alloys. Perchloric acid mixtures (with acetic anhydride, ethyl alcohol, or water) are among the most prominent electropolishing solutions used for lead; however, the presence of bismuth in the alloy precludes the use of any perchloric-containing solution. The other solutions1-7 were found to be unsatisfactory on alloys ranging from 10 to 65 wt pct Bi in lead. With increasing bismuth content, the microstructure shows a lead (terminal solid solution), 0-6 mixture, E (peri-tectically formed hexagonal phase), and E bismuth mixture (eutectic at 56.7 wt pct Bi).9 The metallographic samples were mounted in "Araldite" epoxy (the heat generated during polymerization does not alter the microstructure), ground by hand on well-waxed silicon carbide papers (400 and 600 grit), and polished with 3- and 0.25-CL diamond paste on billiard and microcloths, respectively. The use of the various polishing and etching solutions reported in the literature resulted in the formation of irremovable reaction products on the sample surface when applied to "as-ground" or "as-polished" surfaces. The E phase was the most difficult to clean chemically and in the development of an etchant for this system several solutions which satisfactorily etched the bismuth or a phase were unacceptable because of their reaction with the E. It was found that a mixture of 50 ml lactic acid 30 ml nitric acid 20 ml (30 pct) hydrogen peroxide (Solution #1) was a satisfactory etchant for the a-matrix alloys. The samples were prepared as before and etched after 1 min of polishing with 3-p diamond paste. The etchant was applied by swabbing (light pressure) for 30 sec to 1 min and the sample was then rinsed in running water. The E has a slight stain and the a is fairly bright, Fig. 1.

Jan 1, 1965

Jan 1, 1965

By Hugh M. Roberts

In the spring of 1915, then a 30-year old geologist in the employ of the E. J. Longyear Co., of Minneapolis, Minn., I accompanied prospectors to ex- amine outcrops of supposed nickel ore situated a mile or two in from the shore of a lake in the Kenora district of northwestern Ontario. The deposit proved to be bog iron ore containing traces of nickel. We were stormbound there for three days, a circumstance which gave rise to a tale that was told at our fire one night. It seems that Sandy and Jock, two prospectors, were crossing the bay of a large lake in a canoe. They were bucking headwinds; the waves grew higher. Jock called out from the stern, "Sandy, can ye na pray a little." Sandy pressed his knees a little closer into the bow and, between strokes of his paddle, sought for words, which came haltingly, "Save us this time . . . Oh Lord . . . and we promise . . ." when Jock, peering through the spray sang out, "I would na commit yourself, Sandy, I think I see lond ahead."

Jan 1, 1965

By W. E. Young

This study was made to present the mining methods and costs of a uranium mine typical of other mines in the highly productive Westwater Canyon member of the Morrison formation in New Mexico. Four mining methods have been used at the Section 23 mine: the retreat-room-and-pillar method, a sublevel-slicing method (also called top-slicing), the horizontal-cut-and-fill method, and a modification of the ring-drill method. The application of the methods at this mine and at other mines in the area should be of benefit to operators with similar problems. Ore bodies in the Section 23 mine are irregularly shaped and vary in size, in rock strength, in moisture content, and in uranium concentrations; different mining methods are required and mining costs are not constant. A 6-month period of operation at the Section 23 mine was analyzed and mining costs, not including amortization, depreciation, or Federal taxes, averaged about $6.80 per ton.

Jan 1, 1965

By R. F. W. Pease, R. A. Ploc

A scanning electron microscope with a resolving power better then 100Å has been developed for the direct examination of surfaces. This instrument was used to study iron undergoing oxidation at 500°C. It was found that the electron current in the scanning electron microscope was low enough (about 10-atrzp) to have no observable effect on the growth of the oxide. "Armco " iron, when oxidized, exhibited an oxide film whose thickness and whiskey population varied with pain orientation; but purer iron, when oxidized, exhibited no such pain dependence and whisker occurrence appeared to be caused by impurities. UNTIL recently most surfaces of opaque specimens could either be studied with a light microscope or, if higher resolution was required, by viewing a replica of the surface in a transmission electron microscope. Direct electron microscopy of a surface has, in general, proved difficult owing to excessive foreshortening and the poor image quality obtained. The scanning electron microscope, however, offers an alternative method of directly viewing a surface without these disadvantages. At low magnification it offers a much larger depth of focus than the light microscope, and at high magnifications it offers much higher resolution (about 100Å). PRINCIPLE OF THE SCANNING ELECTRON MICROSCOPE A schematic diagram is shown in Fig. 1. The electron optical system consists of a gun followed by a series of lenses which focus the electron beam onto the surface of the specimen. The beam is scanned in a rectangular raster across the specimen surface and, by amplifying the secondary electron current from the 'pecimen, a picture of the specimen surface is built UP sequentially on the face of the display cathode-ray tube. The magnification of such a system is given by the ratio of the scan amplitude on the display cathode-ray tube to

Jan 1, 1965

By D. M. Kehn

A method has been devloped for chromatographic analysis Of the vapor and liquid phases Of a a system containing methane to components having 20 or more carbon atoms. The method uses a windowed equilibrium cell in which volumetric phase behavior of the system can be observed accurately and from which small samples of gas or liquid can be withdrawn for analysis. Analyses are made using two chromatographs, one for the lighter and one for the heavier components in a sample. Combination of the two analyses yields a detailed analysis of the gas or liquid sample. The complexity of the condensate heavy ends is evident from the chromatograms of these fractions, and the predominance of the paraffin hydrocarborn serves as a useful marker in interpreting the chromatograms. The K-values obtained in this analytical method are presented for a high-pressure condensate system and predict closely the observed volumetric behavior of the system. INTRODUCTION Quantitative analysis of hydrocarbons from natural gas reservoirs is necessary for several reasons—to calculate the amount of sales gas produced, to calculate the amount of natural gasoline produced, to plan a liquid recovery system, or to calculate the potential economic value of a reservoir produced under one or more of several different conditions. Analysis of natural gas fluids produced to the surface consists of identifying and computing the mol fraction of each component of the mixture. Although methane is the predominant component, varying amounts of ethane, propane, butane, pentanes and heavier components are also present. Materials containing up to 30 carbon atoms occur in amounts which decrease with increasing molecular weight. However, the quantities of components in the 20 to 30 carbon atom range are usually so small that their importance is negligible, and they are undetect-able in natural gas by ordinary analytical methods. All the components up to those having 20 carbon atoms may sigsficantly affect phase behavior, however. Commonly, only the methane-through-pentane fraction is analyzed quantitatively for each component, while components heavier than Pentane are lumped and repored as "hexane- plus". Expensive, tedious techniques are required for analysis of this fraction. Consequently the detailed analyses needed for prediction of reservoir behavior are usually undertaken only when major gas fields are being developed. The need for complete analyses of condensate systems is apparent when it is recalled that most gas fields are produced by pressure depletion. As the pressure declines, some of the heavier hydrocarbons are lost as liquids which are in the reservoir. In many instances the amount of liquid in equilibrium with the gas phase at high pressure constitutes only 1 or 2 mol per cent of the total system. Flash calculations generally must predict the actual amount of liquid with an accuracy of a few per cent in order to be useful. This retrograde condensation has been understood for years, but accurate correlation methods to permit quantitative prediction of phase behavior in the retrograde region are not presently available. The increasing importance of natural gas has made accurate prediction of phase behavior and composition of produced natural gas streams an economic necessity. The work reported here was undertaken to provide a rapid, economical method for obtaining the vapor-liquid equilibrium information needed to predict accurately the composition of the fluids produced from a gas reservoir throughout its life. TO develop this method, a pressure cell equipped with windows was designed and built for observing the volumes of liquid and gas present at reservoir pressures and temperatures. Use was made of established chromatographic methods for rapid and detailed analysis of both phases. This paper describes the equipment and techniques developed for obtaining vapor-liquid equilibrium data, presents the results of analyses of a condensate system, and indicates the usefulness of these data in predicting hydrocarbon phase behavior. DESCRIPTION OF EQUIPMENT USED The equipment used in obtaining the required information on phase behavior and the complete analysis of hydrocarbon mixtures through C, will be described first, followed by a discussion of the operation of the equipment. It will be helpful, however, to consider first a brief outline of the technique used. A sample of separator gas and liquid is charged to the windowed cell (see Figs. 1 and 2) where volumetric equilibrium phase behavior at reservoir pressures and temperatures can be determined. Then samples of the coexisting phases are withdrawn. The methane-through-pentane fraction is analyzed with a chromatograph equipped with a hot-wire detector, and the pentane-plus fraction is analyzed with a second chromatograph equipped

Jan 1, 1965

By R. H. Ernst, H. R. Ogden, D. J. Maykuth

AT present, no theories exist which allow prediction of the effect of alloying additions on the thermoelectric properties of metals. Nevertheless, Battelle and others1 have observed that, at high temperatures, the peak thermal electromotive-force output (relative to a platinum standard) occurs with metals in Group VI of the Periodic Chart. The authors suspected that this peak was associated with the fact that maximum electronic bond stability is achieved with these metals which have six bonding electrons per atom. On the basis of current electron-concentration theory for transition metals and alloys:' it was surmised that the addition of valency electrons to metals of Groups IV and V (accomplished by the addition of metals from Groups VI, VII, or VIII) should progressively increase the thermoelectric-power output of the resulting alloys until an alloy composition is reached at which the number of valency electrons per atom is six. A further increase in the ratio of valency electrons per atom should then decrease the thermoelectric power. In contrast, the addition of bonding electrons to Group VI, VII, or VIII metals should decrease their thermoelectric power since the electron per atom

Jan 1, 1965

By W. L. Chen

In the United States hydraulic cyclones have been used for thickening, classification and cleaning in coal preparation plants for many years. The cleaning cyclones presently in use are based on using a "heavy medium", such as a fine magnetite and water pulp. The latest addition to cleaning cyclones is the one which uses ?water only?, or simply called "Hydrocyclone". Just as was the heavy medium cyclone, the hydrocyclones were originated in the Netherlands (1, 2). Plants using hydrocyclones were built in Europe (3) and test plants were erected in Canada (4, 5, 6) and India (7). Roberts and Schaefer Company has built four plants using hydrocyclone circuits. One additional plant is in the process of construction.

Jan 1, 1965

By M. E. Volin

Reagent control for optimum concentrate yield was studied by laboratory batch flotation tests simulating the Groveland plant flotation circuit in which a rougher concentrate is cleaned twice. The reagents were a fatty acid collector, a sulphonate collector and sulphuric acid. The study included two types of flotation feed representative of the reground and deslimed tailing from the spiral concentration circuit, one when the ore mineral is predominantly specularite and the other when it is magnetite. The factorial design included three levels of fatty acid, five levels of sulphonate and five levels of H2S04, with the two types of ore in nested blocks, making up a total of 75 tests. Similarity of results and reproducibility were established in preliminary tests. The final tests were performed in random order under closely controlled conditions following the established procedure.

Jan 1, 1965

By William W. Magnus

The Eastern Magnesia Talc Company has always had the problem of adequate storage at its various mines and mills of not only crude ore and finished product but also material in process. An opportunity arose a couple of years ago with the decision to build a new mill at West Windsor, Vermont, (Figure 1) to come as close to providing adequate space for ore and the ground talc in the new plant as money and judgement would allow. Since our engineering staff did not have the time to design and engineer the new facility, an architectural firm with complete engineering staff was retained. Our original thought was to contract all phases of the construction and installation, however, and I think this is a most important point for any small firm such as ours, we found that with good supervision we, as the contractor, could do the job faster and at a lower cost than the construction firms that bid on the work. For some 50 odd years Italian talc has had a virtual monopoly in the body powder area of the cosmetic industry. Due to the purity, superior lubricity and whiteness, naturally occurring in the talc from Italy, no talc in the Western Hemisphere could capture any but a very small part of the market. When the Italian supply was cut off during World War II, the United States' largest consumer of this talc decided that it was time to develop a domestic source of a satisfactory replacement.

Jan 1, 1965

By E. L. Howard, R. S. Barney back

E. L. Howard (Chief Testing Engineer, Pacific Cement & Aggregates, Inc., San Francisco, Calif.) We have made concrete with all the materials mentioned by Mr. Barneyback, including sawdust. He has highlighted the principal problems and effects found when these light materials are used as concrete aggregate. We can only agree with the inter-relationship he has emphasized between grading, specific gravity and unit weight. Uniformity in these characteristics helps to assure good concrete. Mr. Barneyback says the design of lightweight concrete mixtures "is a complete mystery to most engineers". He is wholly right in his evaluation of our ability generally to put together a concrete using lightweight aggregate. A study of the references he has appended will yield little comfort in the matter of proportioning. Much remains to be done in this area of concrete. We believe Mr. Barneyback has treated the subject, though briefly, in an excellent manner.

Jan 1, 1965

By Jr. Joyce

This report describes sulfatization of nickeliferous laterites from Puerto Rico and the Philippines for recovery of water-soluble nickel and cobalt sulfates. Temperatures ranging from 665 C to 710 C and a 10-percent sulfur dioxide-air reaction gas were employed during batch-roasting tests and during continuous countercurrent treatment in a 2-inch-diameter shaft furnace. A maximum of 69 percent of the nickel and 76 percent of the cobalt were recovered from one sample of Puerto Rican laterite, and a maximum of 96 percent of the nickel and 91 percent of the cobalt were recovered from the Philippine laterite.

Jan 1, 1965

By Harold N. Miller

Lost time and services caused by electrical equipment breakdown or cable faults can often be substantially reduced by the use of direct-current high-voltage testing as a maintenance tool. This paper discusses the relative merits of alternating-current versus direct-current testing, pointing out the advantages in size and cost of equipment and more definitive results achieved through the use of D.C. General principles of direct-current high-volt-age testing, types of testing, methods of performing the actual test and interpreting the results are explained. ?The value of insulation resistance measurements and their relationship to high-voltage testing is discussed. Pinpointing the physical location of a cable defect using a fault locator or thumper is described. Reference is made to several organizations that have effected considerable savings with high-voltage test programs. Introduction T HE past decades have seen great advances in the field of electrical power distribution and application. Motor generators, power-operated equipment, cables, etc., have all gone through various stages of improvement both in efficiency and reliability. Un-fortunately, however, power failures and equipment breakdown still occur -frequently with disastrous effects in loss of time,

Jan 1, 1965

By A. J. Jacobs

THE purpose of this note is to draw attention to a set of tables, recently compiled in Rocketdyne Research Report No. 64-19, under the title "Crystal-lographic Data for Indexing Cubic Twin Reflections and Cementite (Fe3C) Reflections in Electron Diffraction Patterns."' These tables were an outgrowth of electron-diffraction work conducted over the past several years on steels, precipitation-hardening aluminum- and nickel-base alloys, molybdenum, tantalum, and tantalum-base alloys. The first table lists the indices of possible twin reflections for all the possible twinning planes in bcc and fcc lattices. The twin reflections correspond

Jan 1, 1965

By I. M. Gordon, J. Blackshaw

"Run-of-mine ore is reduced to 4 per cent on 4 mesh (3/ 16 inch), using four stages of dry crushing. The mill feed is then reduced to 2 per cent on 48 mesh and 60 per cent through 200 mesh, using one stage of ball milling in cyanide solution. During the subsequent treatment about one-tenth of the tonnage is removed as a table concentrate and ground to 77 per cent through 325 mesh. The size of the mill tailing is 66 per cent through 200 mesh.Four stages of ore reduction began when the dry crushing plant at No. 26 Shaft came into operation at a maximum rate of 440 tons an hour on July 31, 1941. A detailed description of the crushing plant was published in C .I .M. Trans., Vol. LVI, 1953.One-stage ball milling in cyanide solution came into full operation on January 11, 1938. The ball milling plant had a capacity of 4800 tons daily when reducing mill feed at 2. 7 per cent on 1/ 4 inch to 54. 3 per cent through 200 mesh. Primary grinding to 60 per cent through 200 mesh commenced May 22, 1945, when the feed was 3 per cent on 4 mesh. Under these conditions the capacity of the ball milling plant is estimated at 4300 tons daily. A description of the 11 Hollinger Crushing and Grinding Plant"" by D. C. McLaren was published in the Canadian Mining Journal, June 1944.The concentrate grinding circuit using a 7 x 15 low discharge ball mill and a 19-foot diameter bowl classifier with a 6-inch centrifugal pump to close the circuit began operating in the ball milling plant on October 24, 1939."

Jan 1, 1965

By Walter Kahn

Increasing consideration is being given to simplifying traditional methods of tracing pipelines and maintaining required temperatures of stored fluids. Because of their reduction in capital costs, virtual elimination of maintenance. ease of control and "cleanliness"; interest in electrical techniques has accelerated. 1,2 Resistance cable and other heaters have been given some attention. but less well known in the recent introduction of thermal conductive coatings. This paper is addressed to the use of thermal conductive coatings for heating fluid-transport piping and storage tanks. Emphasis will be given to the simplicity, efficiency, and versatility of design and application which their unique properties further contribute to the general economics of electrical heating.

Jan 1, 1965

By W. I. Duvall, D. E. Stephenson

A theoretical solution is given for the energy that is radiated outward when either a cylindrical or spherical cavity located underground in a uniform stress field is suddenly created or enlarged. The method of derivation shows that the stress field in the solid rock surrounding the opening does work on the rock because of elastic displacements that result when the size of the cavity is increased. The amount of this work is sufficient to account for both the increase in the strain energy in the rock surrounding the opening and the seismic energy that radiates outward. Thus, the source of the radiant seismic energy is mainly the gravitational potential energy and not the strain energy stored in the rock. The amount of the radiant seismic energy is directly proportional to the volume of the rock removed from the opening or relieved of stress. Seismic energies from rockbursts are compared with earthquake energies. Also, the amount of gravitational potential energy released by underground explosions is calculated and found to be small compared to the seismic energy generated by the detonation of the explosive. A review of the early literature on rockbursts shows that a number of investigators calculated the amount of energy released by rockbursts. 1-5 However, none of these papers give the formula used to make these calculations or a reference to the derivation of any formulas. The general impression that one obtains from these early papers is that the main source of the seismic energy released by rock-burst is the strain energy stored in the rock before it is fractured. However, a few of the early papers appear to have considered the solid rock at a distance from the mine opening as a possible source of the seismic energy. Recently Black and starfield7 gave a theoretical solution for the strain energy in a stressed plate with and without a circular hole. Also, Press and Archambeau8 gave the theoretical solution for the seismic energy released when a spherical cavity is created in rock subjected to a three-dimensional stress field. Both of the above theoretical papers start with the condition of no opening and calculate the strain energy before and after the opening is suddenly formed. Neither of these papers appear to have calculated the work done by the applied stress field as the cavity is enlarged. The rockburst problem associated with deep mining is concerned with the failure of the solid rock surrounding an underground opening. Therefore, it seems appropriate to consider theoretically the problem of suddenly enlarging the size of an existing opening. The purpose of this paper is to present the theoretical solution for the energy that is available for release as seismic energy when an underground circular tunnel or spherical cavity is suddenly enlarged in diameter. To keep the mathematics as simple as possible, a uniform radial applied stress field is assumed and the rock is assumed to be isotropic, homogeneous and perfectly elastic.

Jan 1, 1965