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By William D. Klopp, Joseph R. Stephens

Chromium alloys were coated with silicon, alumi-nuw, and boron by pack cementation. None of these simple coatings provided adequate nitridation/oxida-tion protection for a Cr -0.17pct Y alloy substrate as shown by a substantial Increase in the ductile -brittle transition temperature after air exposure for 100 hr at 2100°F. Iron-modified silicide coatings afforded good protection, holding the transition temperature of air-exposed specimens to 350° F compared to 200° F for uncoated unexposed specimens and 800°F for un-coated exposed specimens. Additional attractive cant-binations of modi-tying elements included Fe-mo, Fe-Mo-W, Fe-,Mo-W-Ti, and V-Mo-W-Ti. THE desirability of increased operating tempera-tures as a mcans of improving the performance of ad-vanced air breathing engines has resulted in emphasis on the development of materials with high operating temperature capabilities. Chromium, because of its relatively low density (7.19 g per cu cm), high melt-ing point (3410°F), and adequate strength upon alloy-ing, is a candidate material for turbine buckets and stator vanes of advanced air breathing engines. How-even, chromium is not without severe limitations, the major one being susceptibility to nitrogen embrittle-ment upon exposure to air at high temperatures.1,2 For example, a 25-hr air exposure of a Cr-5 pct W* * All compositions in wt pct. alloy at 2100°F produces a 600°F increase in the duc-tile-brittle transition temperature.' Although dilute alloying with such elements as yttrium, lanthanum, arid thorium3,4 or strong nitride formers5 has been shown capable of reducing nitrogen embrittlement, it is apparent that some additional form of surface protection, such as coatings or claddings, will be required for long time service in air breathing engines. Studies of aluiminide6 and silicide7 coatings and of nickel-base claddingsl on chromium alloys to date have suggested that these protection systems are inadequate. Of the aluminidc systems Studied,6 a simple aluminum and an Fe-Al coating on a Cr-5 pct W-0.1 pct Y alloy showed the lowest air exposure weight gains. However, the air exposures raised the ductile-brittle transition temperature of the coated specimens to above 1600°F from an initial level in unexposed specimens of about 500°F. A second in-vestigation for protection of Cr-5 pct W-0.1 pct Y employed gas pressure bonded alloy foils as protective claddings.1 An aluminized Ni-20 pct Cr-20 pct W alloy plus an unalloyed tungsten barrier layer gave the best performance with air exposure lives based on appearance and weight gains of over 600 hr at 2100°F. However, the bend ductile-brittle transition tempera-ture was increased to at least 1000°F after 100 hr at

Jan 1, 1970

By F. P. Morawski, J. E. Schelske, J. R. Geddes, B. R. Eberts, D. M. Wilson, J. D. Jeffries

"The Griffith Mine is located 200 miles northeast of Winnipeg and is 30 miles south of Red Lake, Ontario. Owned by The Steel Company of Canada Limited and managed by Pickands Mather & Co., it has an annual rated capacity of 1.5 million tons of high-grade iron ore pellets with an analysis of 66.3 per cent iron and 4.5 per cent silica.Development of the mine and construction of the plant got underway in January of 1966 and operations began in February of 1968. The orebodies outcrop on the shore of Bruce lake and run under the lake. The ore in its crude form is a metasedimentary low-grade magnetite and occurs in a highly folded banded formation. The average iron analysis of the crude is 29 per cent and the over-all weight recovery is 32 per cent.In order to mine the portion of the orebody under the lake, the soft varved clay on the lake bottom was hydraulically dredged and a dyke constructed of rock, with till used to provide an impervious seal on the lake side of the dyke, prior to dewatering.Mining is carried out by conventional open-pit tech-niques. Ore dressing is achieved by combining one crushing stage and a two-stage grinding system, with beneficiation by magnetic separation, hydroseparation and flotation. Agglomerating is done with conventional balling drums and pelletizing is carried out in shaft furnaces.Of interest and discussed in detail are the 32-foot autogenous cascade mills ."

Jan 1, 1970

By Klaus W. John

The geologic factor of greatest significance in rock mechanics and rock engineering is considered to be the geologic structure represented by joints, faults, and other planes of weakness. This geologic structure differentiates between the rock element and the rock system composed of these elements. Only during the last decade has the difference of the technological properties of element and system been recognized but this appears to be more in theory than in engineering practice. If rock mechanics is to achieve real significance in engineering practice, it has to provide methods of analysis which are realistic compromises between the best representation of the actual conditions and pragmatic engineering. The rock mechanics practitioner has to face the fact that many geological engineering and rock mechanics problems may be too complex to allow rigorous analysis but at the same time are deemed satisfactory for the construction of major structures. Ultimately, the geotechnical engineer or the engineering geologist has to express the effect of geologic factors in quantitative, even if approximate, terms and provide numerical data on strength and deformability of rock systems to be utilized in construction. Qualitative evaluations, quantitative descriptions of geologic features as such, and comparisons of specific test results are always of interest but may not suffice as basis for engineering decisions and designs. The present efforts of the rock mechanics group at the Karlsruhe University, Federal Republic of Germany, are based on a systematic combination of geomechanical models and numerical analyses based on the finite element approach. This group considers that at the present stage

Jan 1, 1970

By H. B. Bell, P. C. Lidster

A study has been made of the use of ThO2-Y2O3 solid electrolytes to determine activity of chromium in Fe-Cr and Ni-Cr alloys in the temperature range 1300° to 1700°K. This method has been shown to give results which agree with the best vapor pressure measurements. SEVERAL investigations1"5 have been made of chromium activities in Fe-Cr alloys. Most of these have been made by vapor pressure measurements using knudsen cell techniques while one has been made using gas equilibration with H2/H2O gas mixtures. In the present investigation electromotive force measurements have been made on this system using a thoria yttria solid electrolyte. This system was -chosen to establish the technique of measurement at low oxygen potentials, before extending it to Fe-Ni-Cr alloys. The cell used was Pt Cr • Cr2O3 ilThO2 • Y2O3 llalloy • Cr2O3 IPt Since the oxygen pressure of the chromium-chromic oxide mixture lay in the range 10"19 to 1027 atm in the temperature range investigated, thoria yttria electrolytes were used. It was soon found during the investigation that considerable care was required to prepare satisfactory electrolytes and a study was made to find the best method of preparing pellets of TI1O2-Y2O3 solid solution of as near theoretical density as possible. Various compositions in the range 2 to 15 mole pct Y2O3 were studied but the experimental measurements were made with electrolytes containing 4 to 5 pct Y2O3. The method of preparation finally adopted was to use thorium oxalate and yttria as raw materials. The thorium oxalate was decomposed at 900°C for 6 hr to give a reactive powder. This powder was then mixed with the appropriate amount of yttria and ground in an agate mortar for about 4 hr. The powder was moistened with absolute alcohol as a lubricant and pressed in a metal die at a pressure of 7 tons per sq in. The pellets were then heated at 1100°C for 24 hr followed by 24 hr at 1250°C. After this firing cycle the material was reground and repelleted and again fired at 1100° and 1250°C followed by heating for 7 days at 1600°C. It was found in later experiments that a further firing of 4 hr at 2000°C improved the density further and gave pellets of only 2 pct porosity. After firing, the pellets were polished on emery paper and finally with the 2 µ diamond paste. The polishing was followed by a final firing of 24 hr at 1500°C. Investigation showed that this final treatment minimized reaction between the electrolytes and chromium oxide. It was believed that this was because of a lowering of the surface energy of the electrolyte surface. Two types of investigation were carried out to check that the pellets were satisfactory oxygen ion elec-

Jan 1, 1970

By J. H. C. Scrimgeour, T. Toong, R. E. Hamilton

"The principles involved in the use and application of mathematical models as an aid to the development of advanced process control computer systems are described briefly. This is followed by a brief survey of known models of this kind for the simulation of mining industry processes.The main part of the paper describes a dynamic model of the flotation process developed by Canadian General Electric. Using flotation rate constants for each species of mineral and gangue, the model provides a numerical solution of the differential equations describing cell behaviour. The cell mode] is used repeatedly as a subroutine in the •over-all-plant model. The features of the cell and plant models are described.Simulation runs from the plant model show stream .assays and other indications of plant behaviour printed typically in 1-to 10-minute steps for several hours of •Operation following typical disturbances such as changes in feed rate or reagent addition rate. The simulation can :Show expected behaviour for both uncontrolled and computer-controlled plants."

Jan 1, 1970

By Harold J. Bennett

The purpose of this study was to develop methods for the financial evaluation of mineral deposits. This includes the selection of the best alternative mining and processing methods and production rates. This was done by performing a financial evaluation through computer simulation using sensitivity and probabilistic risk analysis. The criterion used to measure the relative advantages of these investment and operating alternatives is the discounted-cash-flow rate of return. Included is a description of the theory and methods used in the probabilistic analysis approach, which is based on the premise that the expression of a range of values in establishing an estimate for a parameter is more realistic than the choice of a single value. Numerous simulations are made using randomly selected values of the input parameters resulting in a frequency distribution of the rates of return and their relative probability of occurrence. The sensitivity analysis method is described and combined with the probabilistic analysis to interrelate mineral reserves, capital investments, operating costs, and production rates. The ability to vary these input parameters on successive runs has permitted the selection of the best alternative mining and processing methods and production rates for a given mineral deposit. For illustrative purposes the evaluation of a mineral deposit was performed using three alternative mining and processing methods at three different quantities of resources and various production rates and prices. The computer program used in this analysis was written in FORTRAN II for maximum compatability and should run without modification on most computers having BK (8,000-word) core memory, a card reader, and printer (120 characters per line).

Jan 1, 1970

By C. J. Delisio

The basic concept of tunnel boring has not changed since the late 1800's. R. Stanley of Great Britain obtained a Canadian patent as early as December 1891. Mr. Stanley's machine was a device that consisted of a rotating wheel equipped with drag-type teeth; it had a means of thrusting the cutterhead against the face or heading; it had a means of clamping or gripping the machine in its bore; it had a means of collecting and depositing the cuttings into a screw-type conveyor located near the invert of the tunnel. It even had a means of varying the speed of the forward motion of the machine to suit different hardnesses of rock encountered. This description essentially fits the latest tunnel-boring machines being built today. In short, there has been no significant advance in the basic concept in 70 to 80 years. It may well be that no significant change can be expected for some time into the future. Today's machines, while still basic in concept, offer many advances aimed at faster tunneling. Among these are 1 ) improved cutters, 2) guidance and steering devices, 3) dust-control devices, and 4) mechanisms to aid in installing tunnel supports. CUTTERS The most important part of a hard-rock tunnel borer is the cutter. If the cutter can cut the rock, it is a boring machine. If the cutter cannot cut the rock, no other part of the machine can. When Jarva, Inc. decided to build a machine, the first problem was to find a good cutter. In our search, we looked at most of the cutters on the market. We selected Reed Drilling Tools' cutter because the design of their cutter was aimed at hard-rock tunneling. We feel that they build the best cutter available and provide the best possible service to their customers. As tunnel-boring machine design advanced, the transition from drag bits to roller bits was natural because harder formations required a roller bit, and it is the goal of all mole users to bore harder formations. Roller bits

Jan 1, 1970

By Jack Fox

Although this is going to appear in the December Issue of &E, it is being written long before the end of the year. December, of course, is the time for a summing up of the year's activities. Perhaps, the best way to begin is to report on what went on at the SME Board of Directors Meeting in St. Louis on October 20. This won't be a chronological report, and I shall take time to comment on some of the items we cover as we go along. You should be encouraged to know that your Directors take their duties seriously. Of the 21 current Directors, 19 were present, and three of the new 1971 Directors came to observe what goes on at an SME Board Meeting.

Jan 1, 1970

By Klaus Beckmann

Gentlemen : My object reads "Longwall Rapid Advance of Coal Mining in the Federal Republic of Germany". It is true that the percentage of coal obtained in your country from longwall faces, with at present 1.2, is still rather low, but it increased considerably since 1966 with 0.4 %. The coal mines of the Federal Republic of Germany ever used longwall as the classical method of coal getting. All attempts to introduce bord and pillar mining did not lead to any wider application of this method. The principal reasons, for this appear to have been: - the deeper depth of our workings, - the wish to keep working losses as low as possible and to utilize the deposits opened up by deep and therefore expensive shafts to the furthest possible degree, - the dense sequence of seams and the mutual influencing of the working points, - the high number of disturbances in the geologically much stressed deposits, - and the necessary considerations to the protection of the densely built-upon surface.

Jan 1, 1970

By Roland W. Rammler

In recent years, the crude oil reserves of the world have increased at the same rate as the consumption. A Consideration of the global figures suggests that adequate supplies of petroleum will be available during the next decades. On the other hand, it in a fast of economic and political significance that the reserves in the industrialized countries increase much more slowly than in the developing countries. In Western Europe the reserves have even decreased. At the present time, about 70 % of the petroleum reserves of the world are in the Middle East and in Africa in regions in which political arises are prevalent or impending. For the industrialized countries, the discrepancies between the consumption and reserves in various regions of the world are a strong urge to investigate whether oil can be recovered from other sources. The situation will probably not be changed to a large extent by the discovery of oil in the north of Alaska. The main starting materials for the production of synthetic crude oil are coal, oil shale and tar sand. In North America, where the consumption of petroleum increases more rapidly than the reserves, there are enormous deposits of each of the three materials. This fact is another incentive toward the utilization of these unconventional oil reserves, which provide a reliable basis for a supple of energy for a long time to come.

Jan 1, 1970

By F. Daniel Rosenkranz, Peter L. Silveston

Experiments investigating the treatment of a ground wood white water waste from an Ontario pulp and paper mill by an HVCB coal are reported. Adsorption capacity for the waste, with a soluble COD contribution of 2,100 mg/I, amounted to 0.17 per cent, by weight, of the Nova Scotia coal used. Percolation of the white water waste through a coal bed indicated that soluble COD is removed. For finely ground coals, over 90 per cent of the suspended solids in the waste are retained on the coal. Plugging of the coal bed is rapid, so that any treating process using filtration would have to renew the surface of the bed frequently.

Jan 1, 1970

By M. A. Bergougnou, I. Inculet, K. I. Burgess

This paper describes the electrostatic methods of separating various minerals, reviews the principles of fluidization and outlines the technique of electrostatic sorting in fluidized beds. The application of the method to the benefication of coal is emphasized.

Jan 1, 1970

By Robert B. Scott

Acid mine drainage, discharging from coal beds, has polluted our streams and rivers since early time. These pollutants affect water quality by lowering the pH, reducing natural alkalinity, increasing total hardness, and adding undesirable amounts of iron, manganese, aluminum and sulfates, The tangible damages are the costs involved in replacing equipment corroded by the acid water, additional treatment costs at municipal and industrial water treatment plants, and damages resulting from corrosion of steel culverts, bridge piers, locks, boat hulls, steel barges, pumps, and condensers. Intangible damages, which are real and important, include destruction of biological life of the stream, reduced property values, and streams rendered undesirable for recreational uses.1 The major problems of mine drainage occur in the anthracite and bituminous coal regions in Appalachia. However, many of the western mining states have significant mine drainage problems in specific areas, but the overall problem is not as great as in the eastern states.

Jan 1, 1970

By B. D. Sartwell

Multiple-charged beams originating from a 300-kv ion accelerator are important tools in the study of metal surfaces and thin films. A knowledge of the particle range is necessary for an understanding of the interaction processes of the ions with the targets. Utilizing a theory developed by Lindhard for determining the range of low-energy ions in solids, the ranges of H, He, C, N, 0, and Ar ions in A1203, Al, Fe203, Fe304, CuO, Cu20, Fe, Cu, Sn, and W were calculated for the energy range 60 to 400 kev using a computer program written in BASIC. The range, presented in graphical form, is given in both µg/cm2 and angstroms. In addition, heavy ion ranges were calculated for comparison with published experimental values. For ions with Z > 5, the discrepancy between the calculated values and published experimental values generally ranged from 2 to 40 percent; the largest deviations were probably due to experimental error.

Jan 1, 1970

By Richmond Bennett

Airborne geochemistry became a reality with the advent of a high-sensitivity airborne gamma ray spectrometer with large volume NaI (TI) crystal detectors. Small variations in the concentration of potassium (as K40), thorium (as T1208) and uranium (as B1214) along the flight lines can be determined by measuring the gamma radiation with a sensitive airborne spectrometer. Small volume crystal spectrometers are useful only for detection of major surface uranium (Bi214) variations, but the large crystal volume system is an airborne geochemical exploration method capable of locating hydrothermal mineral deposits. Radioactivity as a guide to ore has been discussed in the literature by Damon (1950), Gross (1952) and others. The theoretical basis is that potassium, thorium, and uranium are concentrated in late stage solutions during magmatic crystallization. Thorium and uranium are concentrated in late stage liquids because their large atomic radius and high ionic charge prevent them from entering into the crystal lattice of common rock-forming minerals (Rankama and Sahama, 1950). Potassium, which has a large ionic radius and small charge, also can be concentrated in the high water content late stage fluids (Heier and Adams, 1964). A large proportion of uranium and thorium in rocks occurs around grain boundaries of the essential rock-forming minerals (Hurley, 1950). Uranium and thorium substitute for zirconium in zircon, a comparatively early forming mineral. However, most of the thorium and uranium is concentrated in residuals where they can be fractionated and incorporated into allanite, monazite, xenotime, and other minerals.

Jan 1, 1970

By A. L. Mular

"This paper summarizes the present-day usage of computers in the mining-metallurgical industry. The industry appears to be following a path taken by other industries in improving the operation of processing plants, production schedules, grade control and haulage performance. A reduction in the cost of computers and computing has been a significant factor.An attempt is made to forecast the future of computers in our industry. Such developments as time-sharing, mini-computers, and easy-to-understand process-oriented languages will lead to wider usage. Considerable strides have been made in the use of computers for laboratory data acquisition. In general, the implementation of new methods, new techniques and new equipment will require plant personnel to develop new skills. The universities are meeting this challenge by re-structuring curricula and offering special courses. Most vendors of computers already offer special courses within their own facilities at a customer's plant."

Jan 1, 1970

By Nathaniel Arbiter

After almost 60 years of application in this country froth flotation is still by far the most important process for concentrating metallic ores as well as a number of nonmetallic ores including fluorspar, phosphate rock, and potash. Its use on iron ores and coal is increasing. In the metals groups the largest plants and the greatest progress are found in copper and molybdenum mills, and the section of this paper that deals with applications will be found most pertinent to that field. During its long reign the flotation process has passed through several phases of evolution and has achieved progress in economy, efficiency, and simplicity of operation. Much of today's success in the flotation of low-grade ores can be attributed to that progress. Even more important to us than our ability to cope with today's conditions are tomorrow's problems, which we can contemplate with some prescience and confidence. Our annual production of copper, lead, zinc, and molybdenum--to mention only the most important metals occurring in the U.S. as sulphides--must be held at a high level in the face of a declining grade of ore. It is probable that the tonnage of such ores mined and processed will double in this country before the turn of the century. Not only will many of the existing flotation mills be enlarged again and again, but larger mills will be built here and abroad to meet our needs. At this moment, in fact, there are at least three proposed new foreign mills or expansions that envision 100,000 tons daily milling rate on copper ores. Table I (1) shows the trend in copper ore grades in U.S. in recent years:

Jan 1, 1970

By C. R. Whitney, G. N. Maniar, D. R. Muzyka

Previous results have shown that Pyromet 860, an Fe-Ni-base heat-resistant alloy, is stable at temperatures as high as 1500°F for aging times as long as 100 hr. This Paper describes the results of long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Times as long as 37,660 hr were employed. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffraction, and microprobe techniques. phase, containing cobalt, nickel, and molybdenum, was detected after extended exposures from 1200" to 1400°F and careful study was performed to describe the kinetics of its formation in this alloy. µ phase formation apparently has little effect on the elevated-tem-perature properties of Pyromet 860. For times as long as 500 hr at 1300°F and below, with µ phase present, m significant effects on ambient temperature properties were noted. For longer times at 1300°F and after 1400°F exposure, the effects of u phase on ambient temperature tensile strength properties are not clear due to y' effects and grain boundary reactions. Electron-vacancy, N,, numbers were calculated using different methods described in literature and correlated with the present findings. In the selection of alloys for use in gas turbine applications, structural stability ranks as a primary criterion. High-temperature strength and cost are also of major concern. With these factors in mind, Pyromet 860 alloy, an Fe-Ni-base superalloy was designed. This alloy combines the cost advantages of Fe-Ni-base alloys such as A-286, 901, and V-57 with improved strength and structural stability'1,2 and no tendency to form the embrittling cellular 77 phase. A previous study3 reported on the stability of Pyro-met 860 at temperatures from 1375" to 157 5°F and times up to 100 hr. That study showed that the y' precipitates increased in size and separation and decreased in number with an increase in time or aging temperature. No deleterious phases were found to occur. In the present work, samples from four production heats were subjected to long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Various heat treatments were used on the starting samples and tests were run up to 37,660 hr. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffrac- tion, and microprobe techniques. Electron vacancy numbers, Nv , calculations were made by TRW.4 Experimental results are correlated with the Nv data used to predict occurrence of intermetallic phases such as a phase. EXPERIMENTAL PROCEDURE Mechanical Tests. Material for the present study came from four production size heats of Pyromet 860 alloy, weighing from about 3000 to about 10,000 lb. All of these heats were made by vacuum induction melting plus consumable electrode vacuum remelting. The nominal analysis for this alloy is compared with the actual analysis of the four heats in Table I. Sections of these heats were forged to 9/16-in. round bar,3/4-in. square bar, 3-in. round bar, 4-in. square bar, and a gas turbine blade forging about 16 in, long, about 6 in. wide, and weighing about 20 lb. In general, all forging of this alloy is done from a 2050°F furnace temperature. Longitudinal test blanks were cut from the centers of the smaller bars, from mid-radius positions for the 3- and 4-in. bars, and from the air foil of the gas turbine blade and heat-treated according to the procedures outlined in Table 11. Heat treatment A is the "standard treatment" recommended for this alloy for best all-around strength and ductility. Heat treatment B is a modification of treatment A for improved tensile strength at moderate temperatures. The treatment coded C was designed for treating large sections according to a procedure previously described.' Heat treatment D was developed to yield optimum stress relaxation characteristics at 1050°F for a steam turbine bolting application. After heat treatment, the test blanks were machined either to plain bar creep specimens with a gage diameter of 0.252 in., to combination smooth-notched stress-rupture bars with a plain bar diameter of 0.178 in. and a concentration factor of Kt 3.8' at the notched section, or to notch-only specimens. All specimens conformed to ASTM requirements. Metallography. Most of the creep-rupture tests were continued to failure. A few bars were fractured as smooth or notch tensiles after creep-rupture exposures. After fracturing, ordinary metallographic sections were made primarily in gage areas adjacent to fractures to represent a "high-stress" region and through specimen threads to represent a "low-stress" region. All metallographic sections were made in a longitudinal direction with respect to the test specimen axes. For optical microscopy, the samples were etched in glyceregia (15 ml HC1, 5 ml HNO,, 10 ml glycerol). For XRD analysis, the phases were extracted electrolytically in two media: 20 pct &Po4 in H20 for selective extraction of y' and 10 pct HC1 in methanol for carbides and other phases.

Jan 1, 1970

By Willard L. Hunter

Four solvent extraction systems were studied to determine their efficiency jor extraction and separation of tantalum and columbium. Aqueous feed solutions of varying HF-HCl concentrations and metal content were contacted with equal volumes of cyclohexanone, 3-methyl-2-butanone, and 2-pentanone and solutions of varying HF-H2S04 concentrations were contacted with equal volumes of 2-pentanone. One multistage continuous test was made in a polyethylene pulse column using cy clohexanone as the organic phase. In each system studied, columbium and tantalum purities in excess of 95 pct with respect to each other were obtained in single-stage tests at low acidities in the feed solution. Separation factors ranging from 1700 to 2400 were obtained when rising HF-HCl mixtures in the aqueous phase. Best results were obtained when a solution of HF-H2S04 was used as the aqueous phase and 2-pentanone as the organic phase. A separation factor in excess of 6000 was obtained in one stage with aqueous solution concentrations of 2 _N HF and 2N H2S0,. When acid concentrations were increaszd to 52 HF and 10 _N H2S0,, 99.9 pct of the tantalum and 98.2 pct of the columbium initially present in the feed solution were transferred to the organic phase. The separation of columnbium and tantalum obtainable by means of the solvent extraction systems presented in this paper was found to corn -pare favorably with other systems, including the HF-H2SO4-methyl isobutyl ketone system currently used by most producers for the extraction and separation of these metals. TANTALUM and columbium are always found together in minerals of commercial significance, although the proportion of the two metals in ores varies within broad limits. Columbium is estimated to be 13 times more abundant than tantalum. Five methods generally employed for the separat:ion of these metals are: 1) fractional crystallization (the Marignac process),2 2) solvent separation, 3) fractional distillation of their chlorides, 4) ion exchange, and 5) selective reduction. Of these methods, the one currently used by industry to the greatest extent is that of solvent separation. One of the early technical developments in solvent separation of tantalum from columbium was reported by the Bureau of Mines: the HF-HC1-methyl isobutyl ketone system; data were presented for both laboratory and pilot-plant experimentation.3 Of twenty-eight organic solvents tested for their ability to extract tantalum from an HF-HC1 solution of columbium and tantalum, 3-pentanone (diethyl ke-tone), cyclohexanone, 2-pentanone, and 3-methyl-2-butanone were chosen for further study. Data on the HF-HC1-diethyl ketone system has been published4 and data describing the use of cy clohexanone, 2-pentanone, and 3-methyl-2-butanone as the organic phase are included in this report. RAW MATERIAL The source of tantalum and columbium oxides for this study was ('Geomines" tin slag from the Manono Smelter, Cie Geomines, Gelges, S.A., Congo. In order to extract the valuable Ta-Cb content, the slags were carbided, chlorinated, and the sublimate from chlo-rination was hydrolized and washed free of chloride with water. The washed material was air-dried and stored in a stoppered container. Throughout the paper, "feed material" refers to this mixture of hydrated oxides which was employed because of its high solubility in aqueous solutions. Typical analysis of the hydrated oxides is shown in Table I. I) HF-HC1-CYCLOHEXANONE SYSTEM Batch Separation. Effect of Acid Concentration. To determine the effect of varying the acid concentration upon the transfer of tantalum and columbium, a series of tests was made in which approximately 2.5 g of feed material was added to 25 ml solutions of 2, 4, 6, 8, and 10 N HF and 0 through 5 N HC1. Tantalum pentoxide concentration of the solu%ons was approximately 21 g per liter and columbium pentoxide was 14 g per liter. These starting solutions were shaken with equal volumes of cyclohexanone in 100 ml polyethylene bottles for 30 min. The phases were carefully separated in 125 ml glass separatory funnels. The time of contact of the solutions with the separatory funnels was kept at a minimum to reduce silica contamination. The measured phases were separated into 400 ml polyethylene beakers and the metal contents of each were precipitated by addition of an excess of ammonium hydroxide. Precipitate from each phase was filtered on ashless filter paper, ignited at 800" to 1000°C for 45 min, weighed, and analyzed by X-ray fluorescence.5 Data tabulated in Table I1 and illustrated in Fig. 1, show that maximum separation of tantalum from columbium for each HF concentration was obtained with no HCl present. The purest tantalum product was obtained with some HCl present. The highest separation factor was obtained at 2 N HF and

Jan 1, 1970

By J. M. Glass, C. D. Sholtess

We at Hughes Tool Co. are extremely proud of the quality of the hardware and techniques introduced through our efforts in tunnel-machine development and of the ready acceptance of them by manufacturers and contractors throughout the world. All of us who attended the conference and who are represented in the book, we believe, anticipate an increasing need for improved methods of underground excavation. The development of such methods will permit the further exploitation of our underground resources plus providing underground space for transportation and habitation at a rate compatible with demand. We hope that our comments, derived from the application of Hughes Tool Co.'s rotary boring experience, may provide a better understanding of the boring method as a possible avenue through which the desired improvement in underground excavation may be attained. We hope you may also become aware of some of the problems Hughes, as a pioneer developer of raise, shaft, and tunnel-boring equipment, must face prior to further major undertakings in this very interesting field. Our task is to acquaint you with the present status of the Hughes Tool Co. development program as it relates specifically to tunnel-boring machines. We feel this task can best be accomplished by a brief review of the general sequence of events leading to and constituting an equipment development program and more specifically the manner in which these events have occurred to either influence or further our boring-machine development program. The development of a machine to accomplish a certain function or series of functions is usually a very long and tedious process to which any number of individuals must contribute, perhaps over a period of centuries. Of particular irony is the fact that often those who contribute most generously do not necessarily reap the greatest immediate benefit. A marketable ma- chine will, however, result from a sequence of events such as these: 1) A problem or need is defined. 2) An idea is born to eliminate the problem.

Jan 1, 1970