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By J. R. Boyle

The Bureau of Mines developed cost estimates fur the disposal of phosphate rock washer slimes by pond settling, from a study of the method used at the International Minerals a Chemical Corp., Moralyn Phosphate Operations, Polk County, Fla. Data were obtained by basing phosphate production and slime generation statistics on plant capacity rather than on actual company records. Cost estimates, which were prepared as a guide in evaluating alternative disposal methods and in identifying needed areas of research, could be applicable to any Florida plant using the same disposal method. To conserve mineral resources and to improve environmental conditions, the Bureau recommends further research directed toward developing alternative methods of disposal, including the recovery of water and P205 values from the slimes.

Jan 1, 1969

By Olman Hee

This study investigates the identity and relative importance of factors affecting the future demand for phosphate rock, potash, and nitrogen. The main objective is to analyze demand relationships for these chemical raw materials for some specified past period, and to utilize this information to make projections of consumption into some designated future period. The end-use approach is used, which divides total consumption of each chemical raw material into agricultural, industrial, and export use. Multiple regression analysis is employed to statistically measure the relative effects of the different factors on consumption in each end use. The general method centers on the construction of a consumer demand model, the fitting of the respective equations in the model, and the interpretation of the statistical results. Direct and cross price elasticities of demand are computed for each end use of the chemical raw materials. These give an insight into expected changes in consumption with respect to given changes in price. The results of this study indicate that price, consumer income, and level of technology are factors which measurably affect consumption of chemical raw materials. For phosphate rock and potash, the agricultural and industrial end uses showed an inelastic demand, whereas for nitrogen, all end uses (including export use) exhibited an elastic demand. Among the chemical raw materials, average annual growth of consumption of nitrogen for agricultural and export uses to 1980 is expected to be notably higher than that for phosphate rock and potash.

Jan 1, 1969

By Robert E. Baker

Cortez Gold Mines, the United States' third largest primary producer of gold, commenced continuous operations on January 10, 1969. The decision to proceed to production was made in March of 1968 and construction of the mill and stripping operations for the pit began in April and July, respectively. Anomalous conditions on the slope of Mt. Tenabo along the Roberts Mountain thrust fault zone were discovered by the U.S.G.S. while conducting geochemical surveys in the old Cortez silver district. Following the discovery of gold an intensive program of drilling was organized. Drilling outlined an orebody with 3.5 million tons of ore averaging 0.28 ounces of gold per ton. It was on the basis of this reserve that a 1700 t. p.d. cyanide plant was designed. Needless to say, with such a limited ore reserve, economies in design and construction would have to be observed. Cortez Gold Mines is a joint venture with American Exploration & Mining Co., The Bunker Hill Company, Vernon F. Taylor, Jr., and Webb Resources, Inc. , as partners. American Exploration & Mining Co. is the operating partner.

Jan 1, 1969

By Richard W. Amerman

The final cost and quality of a project employing equipment, labor, and materials is dependent upon the expediency and extent to which each of these parameters are used. An ideal solution then, would be one in which three solvable equations were given for each particular situation. The equipment, labor, and materials could then be solved for, and the perfect job would result. In reality, however, the ideal and most economical solution is seldom attainable by solving three given equations. Therefore, knowledge, experience, and sometimes guesswork must be relied upon when correlating equipment, labor, and materials. Drilling and blasting, in particular, is one operation which normally involves more uncertainty than other operations. It is also an operation in which the outcome is extremely critical for two reasons. First, the cost of the operation that follows drilling and blasting is dependent upon how well the material is fragmented. Second, once the drilling and blasting has taken place, it is impossible to return to the area, without considerable expense, and correct any mistakes that might have been made. Therefore, what is desired is a method by which drilling and blasting operations can be performed yielding optimum results at the lowest cost; this can best be accomplished by having the relationships between equipment, labor, and materials prior to their use. For obtaining best results, the selection of these three relationships must be based on knowledge, experience, and as little guesswork and uncertainty as possible.

Jan 1, 1969

After the minim operation, most raw materials that occur in the earth's crust require some form of processing or refining before they can be converted into a final end product. In the mineral industry these remarks apply to materials such as iron ore, bauxite, limestone, copper ore and many others that are found in Australia in large quantities. Processing plants for these raw materials operate more efficiently, however, if the feed to them is consistent in both physical and chemical characteristics. Such uniformity rarely occurs in nature so that some form of homogenisation, or blending, is required ahead of the processing plant. Bending also assists the mining operation itself by reducing; the need for selective mining and, by combining high and low grade materials, a more uniformly graded, commercially acceptable product can be obtained, thereby increasing the commercial life of a mine or quarry. Bed blending is the most efficient of the processes available, and following its development in the United States in 1905, over 100 plants have been installed, or are under construction, all over the world. The original process, the Robins--Nessiter system, has been the subject of continued improvements and refinements, so that economical capacities are possible from less than 100 l.t.p.h. up to 10,000 l.t.p,h. and beyond.

Jan 1, 1969

By H. C. Fiedler

X HE development of the cube-on edge secondary re-crystallization texture in Si-Fe strip requires that normal grain growth be restrained. It has been shown that the degree of restraint and hence the completeness of secondary recrystallization depends upon the size and number of second-phase particles, which in turn is dependent upon the prior processing history.1y2 The purpose of this note is to show that, for heats in which manganese sulfide particles are providing the restraint to grain growth, the choice of hot rolling temperature depends upon the manganese content. The making and processing of the heats to the final gage of 0.012 in. has been described.3 The compositions are given in Table I. Apparent in Fig. 1 is the decrease in the ability of strips hot-rolled from 1175°C to undergo secondary recrystallization as the manganese content increases. It has been shown that 1175°C is below the solubility temperature of 0.014 pet S in even the 0.038 pct Mn alloy: and the observed behavior is attributed to an increasing fraction of the sulfur forming large manganese sulfide particles at the heating temperature for hot rolling. This fraction of the sulfur is thus unavailable to subsequently form the small, uniformly dispersed particles which are needed to restrain normal grain growth. Since the sulfur is completely in solution at 1325°C,3 strips from all three alloys show strong secondary recrystallization behavior when hot-rolled from that temperature.

Jan 1, 1969

By A. T. Janssen

Production planning of direct-shipping ore from a number of relatively small deposits serves to sequence development and mining of these deposits so that both long- and short-range demand can be met while the timing of development cost is such that the average annual rate is minimized. Hand-computed methods have the disadvantage that they require substantial effort and time and cannot be exhaustive. The application of operations research and computers not only overcomes these disadvantages, but opens up additional applications, such as feasibility studies involving alternative mining strategies and changes in the ore market. The method employed concerns linear programming and specifically the Big-M algorithm applied to the variant on the simplex technique with penalties applied to deviations from the desired ore grade. Acceptable 20-year production schedules could be generated in relatively little time, i. e. , in less than 200 seconds for the central processor of the Control Data Corporation 6400 system of the University of Colorado in Boulder.

Jan 1, 1969

By P. Chiotti, J. T. Mason

Thermal, X-ray, metallographic, and resistivity data were obtained to establish the phase diagram for the Yb-Zn system. Six intermetallic compounds and five eutectics have been identified. The compounds position at 695°C. No evidence for the compound YbZn,, was observed. Whether this compound is stabilized or inhibited by small amounts of impurities is uncertain. SEVERAL aspects of the Yb-Zn system have been reported in the literature. Much of this work deals with the crystallographic identification of some of the compounds. The YbZn compound has been reported by Iandelli and palenzonal and the YbZn, structure and thermal data for the composition range between YbZn and Yb3Znll have been reported by Michel et al. A compound of uncertain stoichiometry in the range 60 to 68 wt pct Zn with a cubic structure has been reported by Kuz'ma et aL4 The YbzZn17, YbZn,,, and YbZn13 compounds have been reported by both Kuz'ma et a1 and Iandelli and Palenzona.' YbnZn17 has also been identified by Laube. This investigation was undertaken to establish the phase diagram of this system. Ytterbium in many respects behaves as an alkaline earth rather than a rare earth metal6 and it is of interest to note the resemblance between the Yb-Zn system, the Ca-Zn,' and typical rare earth-zinc systems.g'10 MATERIALS AND EXPERIMENTAL PROCEDURES The materials used in this investigation were Ames Laboratory ytterbium and Bunker-Hill slab zinc, 99.99 pct pure. Analyses of the ytterbium showed 38 ppm Ta, 82 ppm 0, and 15 ppm N with Ca, Cu, C, Mg, Al, Si, Cr, Fe, Ni, Sc, Y, Er, Tm, and Lu all less than 50 ppm. The ytterbium was dehydrogenated by heating in tantalum under vacuum for 8 hr at 900°C. The metal was kept under argon except when being cut with shears and when being weighed. Tantalum was found to be a suitable container for alloys in the composition range between ytterbium and Yb2Zn17. With higher zinc concentrations the tantalum was penetrated by the alloy and failed after several days at temperatures of 600" to 700°C. Approximately 20 g of zinc and ytterbium metal were sealed under argon in *-in.-diam tantalum cruci- bles equipped with thermocouple wells. The crucibles were in turn sealed in stainless-steel jackets. The alloys were equilibrated in an oscillating furnace and given various heat treatments in a soaking furnace. The steel jackets were removed and differential thermal analysis data were obtained under an atmosphere of argon. The thermal analysis apparatus was calibrated against the melting points of pure zinc, aluminum, silver, and copper and found to give thermal arrests within 1°C of the accepted melting temperatures for these elements. The thermal analysis apparatus has been described in an earlier paper.g Alloys were further heat-treated as necessary and subjected to metallographic examination and X-ray diffraction analysis. Most alloys were etched with Nital (0.5 to 10 pct nitric acid in alcohol). EXPERIMENTAL RESULTS The results of the thermal analysis are summarized by the points on the phase diagram, Fig. 1. Six compounds and five eutectics were observed. The eutectic temperature and compositions in weight percent zinc are 491°C and 12 pct, 645°C and 32 pct, 687°C and 54 pct, 742°C and 67 pct, and 750°C and 77 pct. The compounds YbZn, YbZn2, Yb2Zng, Yb2Zn17, and YbZnll melt congruently at 650°, 751°, 75Z°, 754", and 755"C, respectively. The compound Yb3Znll undergoes a peritectic decomposition at 695°C. The transformation and melting temperatures for the ytterbium were observed to be 797" and 817°C. re-

Jan 1, 1969

By A. McLean, D. W. Gomersall, R. G. Ward

An experimental study has been made of the solubility of nitrogen in liquid iron and liquid Fe-C alloys using levitation melting and a rapid quenching device. Iron alloy droplets were equilibrated with nitrogen gas at 1 atm pressure, quenched, and analyzed. Previous techniques for studying the Fe-C-N system have produced data which me in marked disagreement. This disagreement is due largely to errors caused by reaction between the molten alloy and the crucible material. With the levitation procedure, errors from this source have been eliminated and precise solubility data obtained for temperatures between 1450° and 1750°C. C-N interactions in molten iron have been expressed in terms of first- and second-order free energy, enthalpy, and entropy parameters. ALTHOUGH the solubility of nitrogen in iron base alloys is in general small, the effects of nitrogen on the properties of steel may be quite profound. For most purposes nitrogen in finished steels is undesirable, particularly in the low-carbon grades, since on cooling to room temperature the solubility limit of nitrogen in the steel may be exceeded and this can lead to embrittlement and loss of ductility on aging. On the other hand, nitrogen can improve the work-hardening properties and machinability of steels while in certain stainless grades nitrogen is important in order to stabilize the austenite phase. It is, therefore, desirable that one should be able to predict the solubility of nitrogen in liquid iron alloys. To do this, information is required concerning the interactions between nitrogen and the various alloying elements which may be present in liquid iron. There have been several investigations of these effects in recent years1"7 and the interactions between nitrogen and many elements dissolved in liquid iron are now known to a high degree of precision at steel-making temperatures. Unfortunately, a number of iron alloy systems which are of interest in steelmaking have been difficult to deal with by the experimental techniques generally used for this type of investigation. Among the most important of these are the Fe-C alloys. In the past, two methods have been widely used for determining nitrogen solubilities: the Sieverts' technique, in which the amount of nitrogen required to saturate a given mass of liquid metal at a particular temperature and pressure is measured volumetrically, and the sampled-bath technique in which liquid metal held in a crucible is equilibrated with a gas phase containing a known partial pressure of nitrogen, and samples drawn from the melt are quenched and analyzed. These two methods have been discussed in detail elsewhere.5,8 With the Sieverts' technique, errors may be introduced from the following sources: i) Gas adsorption on metal films which have condensed on the cooler parts of the reaction chamber. ii) Uncertainty in the determination of "hot volume" calibrations. iii) Crucible-melt interaction, particularly if a gaseous reaction product is formed or if the melt becomes contaminated with material from the crucible walls. The sampled-bath method may also suffer from errors due to reaction between the melt and the crucible material. In addition, there is the possibility that gas may be lost from the sample during solidification and cooling. In the present investigation, the solubility of nitrogen in liquid iron alloys has been studied by means of a new technique based on the use of levitation melting equipment and a rapid quenching device. In addition to the fact that problems of the type outlined above are avoided, this particular approach has the following advantages: i) The high-frequency current induces vigorous stirring within the levitated droplet so that gas-metal equilibration is rapidly attained. ii) The gas phase surrounding the melt can be changed very quickly and is easily controlled. For example, a droplet may be levitated in helium, deoxidized in hydrogen, equilibrated with nitrogen, and quenched, within a period of 15 min. ii) Melts can be readily under cooled or superheated, thus extending the effective temperature range of an investigation and allowing temperature-dependent data to be determined with a high degree of precision. Excellent reviews of levitation melting techniques and their application to physical-chemistry studies at high temperature have been published recently by Jenkins et al.,9 Peifer,10 and Rostron.11 In the present investigation a levitation melting technique has been used to obtain data for the solubility of nitrogen in pure liquid iron and liquid Fe-C alloys at temperatures between 1450° and 1750°C. The solution of nitrogen in liquid iron can be described by the reaction:

Jan 1, 1969

By K. G. Davis

Dilute alloys of silver and of thallium in tin have been solidijzed unidirectionally under controlled conditions, to study the segregation associated with a cellular interface under conditions where both thermal and solute convection are present. Autoradiography and radioactive tracer counting techniques were combined with electron-probe microanalysis to study both macro- and microsegregation. It was found that, for concentrations giving only small amounts of constitutional supercooling, cell formation had little effect on the macroscopic distribution of solute along the specimen. At higher concentrations the effective distribution coefficient was higher than that expected for a smooth interface. Node spacing was independent of initial solute content at lower concentrations, becoming greater as keff increased. Silver content at the segregation nodes of silver in tin alloys was independent of initial concentration and considerably in excess of the eutectic composition. SINCE the investigation of cell formation at advancing solid-liquid interfaces by Rutter and Chalmers,' a large volume of work has been dedicated to the determination of solidification conditions under which a planar interface will break down into cellular form. Early experiments were explained satisfactorily by the concept of constitutional supercooling,2 but, due to poor measurement of temperature gradients in the liquid, lack of accurate data on liquid diffusion and equilibrium distribution coefficients, and uncertainty about the effects of thermal and solute convection, these experiments cannot be used as proof for the theory. More recent work, however, has shown that under conditions where convection is eliminated or can be ignored good correlation is observed.3,4 Investigations into segregation at cell caps5 and at cell nodes6-'' have been made, but no measurements appear to have been done on the overall, macroscopic segregation down a unidirectionally solidified rod of material which has solidified with a cellular substructure. This has practical importance in casting, where regions of material with cellular substructure are often encountered, and also in zone refining where the thermal conditions necessary for a planar interface are unattainable. Further, as will be shown, the macroscopic segregation can give information on the following question. Granted that a cellular solid-liquid interface develops from a planar one when the conditions for constitutional supercooling are exceeded, how much supercooling is present after the cells have formed? EXPERIMENTAL PROCEDURE AND RESULTS Specimen Preparation. Specimens 25 cm long with a square cross section 0.6 by 0.6 cm were grown in graphite boats by solidification from one end. Alloy compositions are given in Table I. Two specimens of each composition were grown. The tin was 5-9 grade and the silver and thallium both 4-9 grade. Ag110 and Tl204 were used as tracers. Each composition had the same quantity of tracer so that auto radiographs of specimens containing different concentrations of the same element could be easily compared. Thermocouples inserted through the lid of the boat into a dummy specimen showed that, over the first 10 cm of growth, thermal conditions were quite steady, with a rate of interface advance of 5.8 cm per hr and a temperature gradient in the melt ahead of the interface of 3.0°C per cm. The specimens were seeded from tin crystals of a common orientation to eliminate orientation effects. Dilution of the specimen by seed material was minimized by the provision of a narrow neck between specimen and seed crystal. Macrosegregation. After growth, the specimens were sectioned with a spark cutter. The rods of silver alloy were cut into 1-cm lengths and analyzed for Ag110 using a y -ray counter with fixed geometry. The specimens containing thallium were cut into 2-cm lengths and analyzed for T1 204 by taking 13 counts from each end of the cut lengths through an aperture in lead sheet approximately 0.4 cm square. The results are summarized in Figs. 1 and 2. To find the effective distribution coefficient for the silver in tin alloys under smooth interface conditions, the region of substructure at the bottom surface of one of the 10 ppm specimens, see Fig. 3, was removed by spark machining before counting. Autoradiography. For both alloy systems the samples were polished on sections taken alternately parallel and perpendicular to the growth direction, and autoradiographed by placing the polished surfaces in contact with Kodak "Process Ortho" film. Figs. 3 and 4 show the structures revealed. The alloy containing 10 ppm Ag showed substructure only after a few centimeters of growth, and then substructure was limited to a narrow layer at the base. The "speckled" substructure reported previously in this system4 is here clearly seen to be an intermediate stage between planar and cellular interface conditions. The other samples show a remarkable similarity considering

Jan 1, 1969

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of Clay, Gilmer, and Lewis Counties, W. Va. In 1966, almost 1.3 million tons of coal was mined in these counties, of which more than one-half was from the Pittsburgh coalbed. Washability analyses were made of 16 coalbed samples. Of these, only 11 samples could be upgraded to metallurgical quality. For steam or power generation five of the coals were of low sulfur content as received. The remaining samples were generally of medium sulfur content even after upgrading.

Jan 1, 1969

By P. J. Carroll, H. Colijn

Feeders must be considered an integral part of the over-all bin and feeder system. Improper design of either one of these parts will affect the performance of the whole system. Feeder load, material properties, feed rate, physical layout, and environment as well as first cost determine the selection of feeder type. This paper provides a new method of calculating feeder loads with some experimental data as verification. General design criteria for belt and apron feeder, rotary table and plow feeders are discussed and a special section is devoted to vibratory feeders. Feeders are used to provide a means of control for the withdrawal of bulk materials from storage units such as bins, bunkers, silos and hoppers. This control function can only be performed properly as long as the bulk materials flow by gravity to the feeder in a uniform and uninterrupted fashion. During the past few years various papers have been written and presented on feeders and their application.1-9 This paper will be confined to some specific bin-feeder design criteria such as feeder load and power requirements. Special attention is given to the basic design criteria for vibratory feeders. HOPPER AND BIN DESIGN Feeders must be considered an integral part of the over-all bin and feeder system. Improper design of either one of these parts will affect the performance of the whole system. A lot of effort has been devoted in the past decade to the development of functional design criteria for hoppers and bins.1,10 The integrated concept of bin and feeder design requires quantitative analysis of the bulk material characteristics before the design and the selection of components can be attempted. The design of a feeder system must begin with the proper dimensioning of the hopper outlet to prevent arching or ratholing. The hopper opening should be large enough to allow passage of the bulk solid at the required maximum discharge rate." A feeder can only throttle the flow. FEEDER LOAD DETERMINATION Over the past ten years, there have been various attempts to determine the exact load or pressure on feeders mounted directly under hopper openings. Many designers, however, still consider this pressure equal to the hydrostatic head of material above the opening, and because such pressure would be very

Jan 1, 1969

By N. Standish

Heat transfer coefficients have been measured in beds of various packings irrigated with mercury and molten fusible alloy countercurrent to hot gases. The measured coefficients for both systems were found to increase with gas velocities and liquid rates. Correlations were determined which show this dependence and also indicate that heat transfer in these systems is influenced by the liquid flow characteristics and the thermal conductivity of the gas and the solid packings. A heat transfer model has beer2 proposed which explains the various features of the experimental results. On the basis of this study, which gives an insight into the heat exchange in the melting zone of the blast furnace, it was concluded that by comparison with the furnace stack heat transfer coefficients are about 1.5 times higher in the melting zone. EACH year large tonnages of metal are produced in operations which, in part, involve liquid metal irrigation of "packings" countercurrent to hot gases. The melting zone in blast furnaces and in cupolas is a good example of packings irrigated with a liquid melt countercurrent to gases. In all instances of this kind large amounts of heat are exchanged and it is desirable to have some knowledge of heat transfer phenomena involved in these systems. So far the most common method of analyzing furnace efficiencies, fuel requirements, and the general thermal state of the furnace has been through the use of heat balances. As heat balances are essentially statements of the first law of thermodynamics they give no real indication of the factors which govern heat transfer between phases in the various zones of blast furnaces. Hence, rational improvement in production efficiency and the development of theoretical models is only possible if the heat transfer characteristics are known at every stage of the process and related to the important variables involved. This has been generally recognized for some time but it was only recently that Kitaev et al.' have produced a comprehensive treatment of heat transfer in solid-gas countercurrent systems such as the blast furnace stack and the packed bed regenerator. Using their treatment it is now possible to predict the effect of particle size, thermal conductivity, bed porosity, and the flow rates of both the gas and the solid material on the heat transfer in the blast furnace stack. However, the stack of a blast furnace is only one part of an integral unit for which the heat transfer analysis cannot be complete without also considering the heat exchange in the melting zone. The complexity of heat transfer processes in this region of the furnace has so far escaped quantitative description. Yet, the melting zone accounts for a greater amount of heat exchange than all the other zones of the furnace put together. Moreover, if the reduction of oxides in the melting zone proceeds in part in the liquid state the importance of heat transfer on furnace productivity and on the metal and slag temperatures is obvious. THEORY Heat transfer for two-phase flow in packed beds is a complex problem involving a number of heat exchange paths for which interphase areas are not known with any degree of certainty. Analytical solution is, therefore, difficult. This difficulty is emphasized by noting that Rabinovich~ and Luck have only recently solved the steady-state heat transfer for simplified two-phase heat exchangers of known area. However, useful progress can be made for the system considered by making a not unreasonable assumption that the usual heat transfer considerations apply and restricting treatment to the steady state. For these conditions the rate of heat transfer dq in a height dz of a packed bed of unit area is: dq = UaATdz [I.] Integration of Eq. [I] then gives the total heat transferred: assuming both U, the overall heat transfer coefficient, and a, the interphase area, to be independent of bed height. Since a, in these systems, is unknown it is convenient to combine this term with U. The group U, then represents the overall heat transfer coefficient on a volumetric basis. If AT is linear with q, then for a bed of unit volume Eq. [Z] can be integrated to give: is the log mean of terminal temperature differences. From Eq. [3] U, can be readily calculated as q and {AT)im are experimentally obtained quantities, but a difficulty arises in interpreting its meaning. Two approaches are possible depending on whether the effect of packing in the transfer of heat is neglected or not. If the packing is thermally decoupled then the resistance concept gives the relationship: which states that the overall resistance is the sum of the gas phase and the liquid phase resistances (assuming areas are equal throughout). Because the resistance to heat transfer in liquid metals is negligible by comparison with that of the gas,4 Eq. [4] can be simplified, i.e.:

Jan 1, 1969

Two structurally and mineralogically distinct sulphiderich veins cross-cutting the disseminated sulphides of the Nairne Pyrite Member appear to be products of local remobilization of sulphides under fracture-induced free energy gradients during regional metamorphism and tectonic deformation.The contrasting mineralogy of the two vein types may have arisen as a result of differences in the structural orientation of the veins and!or the relative ages of the veins.

Jan 1, 1969

By M. I. Jacobson, M. L. Hammond

The solid solubilities of high-purity silver, aluminum, chromium, copper, and iron in zone-refined beryllium have been determined. Diffusion couple sandwiches of beryllium with aluminum, copper, and silver foil and diffusion couples of beryllium with two-phase alloys in the Be-Cr. Be-Fe, and Be-Ag systems were analyzed by electron beam micro-probe techniques. This paper describes the material used, the experimental methods for preparing the diffusion couples and the alloys, the analytical techniques, and the results obtained. The results are compared with those of previous investigators who used materials of lower purity. ~NVESTIGATORS of beryllium phase diagrams have often been hampered in their interpretations of certain phase boundaries because of the relatively low purity of the beryllium used. This has sometimes resulted in the appearance of three phases in the regions where only two should exist. Advances in purification methods, specifically zone refining, have made available beryllium that is considerably purer than the material previously used for phase diagram studies. The primary object of this investigation was to reex-amine portions of the beryllium-rich end of the binary systems of beryllium with silver, aluminum, chromium, copper, and iron to determine more accurately the limits of terminal solid solubility. The five elements—silver, aluminum, chromium, copper, and iron—include some which are commonly found as the major impurities in beryllium, some of which are being used as solid-solution alloying elements, and some of which are used in ductile matrix alloys. They are thus of considerable importance to physical metallurgists who must work with beryllium but who must rely on the present inaccurate or incomplete diagrams. The determination of more reliable diagrams would aid researchers concerned with the problems of alloying, heat treatment, and ductility. MATERIAL The beryllium was acquired from the Franklin Institute in the form of a single-crystal, 6 in. long by 1 in. in diam, zone-refined in three passes from Pechiney SR-grade beryllium bar. The principal impurities, as determined by mass spectrography at Battelle Memorial Institute, are shown in Table I. Vacuum-melted copper, silver, and aluminum, and electron-beam zone-refined iron were obtained from the Materials Research Corp. in the form of 1/2-in.- diam bars. Iodide chromium was obtained as flakes from the Chromalloy Corp. Analyses supplied with these metals are shown in Table 11. EXPERIMENTAL PROCEDURE Preparation of Diffusion Couples. Two types of dif-fusion couples were used in this study. For the copper, silver, and aluminum systems, the couples were sand-

Jan 1, 1969

The research project on size reduction, sponsored by the mining industry through financial support from individual companies, is now embarking on a second three-year program. The first 3-year program had as its objectives assimilation of the literature on comminution and development of simulation programs encompassing the basic mechanisms of grinding. This involved investigating conditions under which a particle in a mill is captured, the stress to which it is subjected, its break probability, and the resulting particle size distributions. The results were used to obtain the most representative simulation models based on current knowledge of mechanisms. As part of this work a set of computer programs has been developed for the following cases: . Batch mill, by numerical integration for completely general selection and breakage functions. . Continuous open-circuit mill by same method as above. . Continuous open-circuit mill by general numerical integration method, including transient behavior

Jan 1, 1969

By O. G. Paasche, Yuan-Shou Shen

THERE is a disagreement among the various authors about the exact manner of transformation of ZrCr2. Rostokerl and others2 stated that ZrCr2 had a C-14 (MgZn2) type of structure below 1000°C and a C-15 (MgCu2) type of structure at temperatures above 1000°C. Alisova3 and others4 reached the opposite conclusion and stated that the transformation temperature is close to the melting point of ZrCr2. A literature survey shows that various investigators3'= who homogenized the specimens at a temperature higher than 1000°C have concluded that ZrCr2 had the C-15 structure at room temperature. Meanwhile, Jordan et al.4 reached similar conclusions without annealing the specimen. Other investigators1,2,6,7 who X-rayed the specimens in the as-cast condition without annealing reached different conclusions. The investigation reported herein was conducted with the aim of exploring the exact manner of transformation of ZrCr2 by various heat treatment tests. The alloys for this examination were prepared from iodide-reduced zirconium crystal bars, 99.9 pct purity, and electrolytic chromium, 99.9 pct purity. They were melted in a nonconsumable electrode arc furnace with water-cooled copper crucible in a helium atmosphere. The melting loss of each alloy was less than 1.5 pct by weight. Chemical analysis of a randomly selected specimen indicated that there was a very close agreement between calculated and analyzed compositions. Before being heat-treated each specimen was encapsulated in a vycor or quartz tube inside which an argon atmosphere was maintained at a pressure of lower than 1 atm. In determining the crystal structure of each specimen with a Debye-Scherrer camera, the standard procedure8 for X-ray quality analysis (Hanawalt method) was followed. The different series of heat treatment tests in this investigation are tabulated in Tables I and 11. The tests in Series I, specimens from 1-1 to 1-9, which were similar to Rostoker's experiment1 indicated that the transformation temperature seemed to fall between 870° and 900°C and that the crystal structure of ZrCr2 at lower temperature seemed to be of the C-14 type. However, once the compound is transformed to C-15 type, it is impossible to reverse the transformation back to the C-14 type by first heating the specimen above 900°C and then annealing it slowly below 900°C as shown in Experiments II-1 to II-3. Thus, it appears that the specimen of ZrCr2 will transform from C-14 to C-15 structure when heated above 900°C but will not transform from C-15 to C-14 when annealed slowly passing 900° C even after the extremely slow cooling process such as indicated in the experiment of Specimen II-3. As a valid transformation temperature is a temperature at which the transformation is reversible, therefore the temperature 900°C (or other temperature close to 900°C) is not the transformation temperature for ZrCr2 and the C-14 structure is not the stable structure of ZrCr2 at lower temperatures. The C-14 structure is retained at room temperature because the transformation to C-15 structure is very sluggish and the fast cooling after melting does not allow enough time for the transformation to take place. Additional energy is required to alter the metastable condition of the C-14 structure. The sluggishness of this transformation was again demonstrated through another series of experiments. Four specimens with C-14 structure were taken. Then they were annealed at 900°C but each specimen was soaked for a different period of time, Table 11. X-ray diffraction patterns of this group indicated that the C-14 structure gradually disappeared as the soaking period was lengthened. The figures listed under the column "C-14 Structure, pct" were estimated from the intensity of the d = 2.330 line of the diffraction pattern corresponding to the structure. Notice that the intensity of this line became weaker for longer soaking periods. To determine the transformation temperature of ZrCr2, specimens with C-14 structure (as-cast condition) were annealed at 1300°, 1400°, 1500°, 1550°, and 1600°C, respectively. A final specimen was first heat-treated to 1500°C in order to transform it to C-15 structure, then heat-treated at 1600°C again. From the X-ray analyses of this series of tests, Specimen Nos. III-1 to III-6, it is evident that a transition from C-15 structure at lower temperatures to the C-14 structure occurs at some temperature between 1550° and 1600°C.

Jan 1, 1969

By Charles Prasky

The Bureau of Mines investigated the conversion of nonmagnetic iron minerals to magnetic form through reduction Toasting operations. The primary objective was to obtain a concentrate that could be used as a direct shipping material for blast furnace consumption. Crude iron materials from the Steep Rock Lakes, Ontario, area were prepared into a blend of 8 parts siliceous ore, 3 parts pyritic ore, and 1 part tailings. Experimental work included laboratory reduction roasting tests, two continuous 10-day campaigns, and one 12-hour test all in a 34-inch by 36¬-foot rotary kiln. The objective of the project was achieved in producing an iron concentrate containing about 66 percent iron with over 90 percent iron recovery. Desirable operating conditions were developed in the kiln but optimum process variables were not completely established.

Jan 1, 1969

The granulites and related "dry" igneous rocks tend to be passed over during exploration for metals. Preliminary data show that high trace concentrations of Cu, Ni and other metals of economic interest are common in orthopyroxene and some of the other granulite minerals. During retrograde metamorphism of granulites, pyroxenes are converted to amphiboles or phyllosilicates, and significant quantities of metals are released and become available for incorporat- ion into new mineral phases, or may be transported elsewhere. S--rich scapolite is the normal scapolite of granulites. Its retrogression to secondary plagioclase provides much S which scavenges Cu, Ni, etc., from pyroxenes undergoing retrogression, thus producing ore-fluids. A full analysis of a scapolite with 5.10 per cent S03 is given. Beryl is unstable in granulites but the rare Be mineral taaffeite (Al4Pf (Be,Fe)O3) with 5,50 per cent BeO occurs in central Australia as a pale green Tabular mineral easily confused for chloritoid in hand-specimen. Metamorphic differentiation and mobilization of primary ore concentrations are major factors controlling their post-granulite attitude and grade.

Jan 1, 1969

By D. Montagna

Large quantities of zinc-base die-cast scrap containing 3 to 4 percent aluminum are presently refined by mixing with other secondary zinc products such as galvanizer dross and distilling in a retort. The Bureau of Mines investigated alternate aluminum removal processes utilizing low-cost fluxes. Basing the investigation on the metallurgical principle that a reactive impurity can be removed from a less reactive matrix metal by melting under a flux consisting of a salt or oxide of a metal less reactive than the impurity, three separate flux mixtures were studied. In the first flux system, [FeCl3] + NaCI (the active component is underlined), part of the aluminum is' eliminated by the formation of volatile aluminum chloride and the rest by the creation of a high melting point iron-aluminum intermetallic compound that can be separated from the remaining molten zinc by filtration. Aluminum removal in the second system, [Fe203] + CaClz + NaCI, is effected by the formation of the iron-aluminum compound and possibly aluminum oxide. The third system, spent sal skimmings--essentially a mixture of [ZnCl2], NH4Cl, and ZnO, depends solely on aluminum chloride formation. Of the three flux systems investigated, the best results obtained were with system 3. Aluminum was reduced in the molten die-cast alloy from 4.10 percent to 0.01 percent when depleted sal skimmings were used.

Jan 1, 1969