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By William C. Brice

Minnesota is involved in planning controversies related to taconite and potential copper-nickel mining. Mine facility planning includes the Reserve dining on-land tailings disposal issue and the potential for a new copper-nickel mining district. Both provide a unique opportunity for innovative planning in the attempt to be responsive to public and private interests. Concerns that emanate as a result of mineral resource activities include environmental protection, land use competition, land exchanges, highway and utility extensions, and legal constraints on public or private lands. The purpose of this newly-developed planning approach is to anticipate such issues and provide a rational information base for dealing with them. The result will be a framework plan for guiding public planning, and an impact assessment for reviewing the implications of industrial project proposals. The approach uses a computer-stored resource inventory of natural and cultural information. Geographic data is mapped and entered into a computer storage and retrieval system. This enables systematic analysis of mineral resources along with environmental and land use considerations. Computer mapping describes the relationship of each activity and allows identification of potential conflicts; it also shows geographical extent in the form of statistical compilations. Resource data is being collected and compiled using a standard metric grid (Universal Transverse Mercator). Individual cells are 100 m. squares and represent areas of about 2.5 acres. The study area contains about 145,000 cells. Data inventories are being compiled in 25 natural and cultural resource categories. Geologic variables include Bedrock Geology, Taconite Reserves and Potential Resources, Depth to the Duluth Complex Contact and two soil inventories. Topographic and hydrologic variables include elevation, slope, slope orientation, surface hydrology, and watersheds. There are also 6 biological data variables and 7 land use inventories.

Jan 1, 1977

By T. Egleston

SOME months ago samples of black oxide of copper and of pig copper from Colorado were sent to me to examine for arsenic and

Jan 1, 1882

By Robert A. Colten, Frederick C. Hull, Robert F. Mehl

It is known that pearlite forms from austenite by a process of nucleation and growth, and that the rate of formation of pearlite may be described by a rate of nucleation and a rate of growth.l,2 The manner in which these two quantities operate to produce the observed isothermal reaction curve has been analyzed in a paper published in I939.3 Two types of process were described: (I) that in which nucleation occurs at the grain boundaries of the parent phase, with the nodules growing toward the centers of the grains, initially as hemispheres and then after impingement as roughly radial-columnar structures; and (2) that in which nucleation occurs generally, with the nodules growing to full spheres until impingement with other growing nodules restricts growth. Both cases are met in the formation of pearlite from austenite (Fig. I);2,4 the former, occurring near the knee of the S-curve, has been named "grain-boundary transformation," and the latter, occurring at temperatures near Ael, has been named "group-nodule transformation." In developing our knowledge of the factors that determine the rate of formation of pearlite from austenite, it is important1,2 to obtain data on the rate of nucleation and the rate of growth of pearlite. Such data, when obtained near the knee of the S-curve, will furnish information of use in understanding the factors that affect hardenabil-ity; when obtained at higher temperatures, such data will be useful in understanding the behavior of steels that during heat-treatment react to pearlite.2 It is the purpose of this paper to present data on the rate of nucleation and the rate of growth of pearlite in dependence upon composition, grain size, temperature, and the degree of homogeneity of the parent austenite. The studies are restricted chiefly to plain carbon commercial steels." Previous Data on Rate of nucleation and rate of Growth Data on the rate of nucleation and the rate of growth of pearlite have been published by Scheil and Lange-Weise,5 by Mirkin and Blanter,6,7 by Meh1,l and by Dorn, De Garmo and Flanigan.2, It is difficult to interpret the data, for in most cases too little information is given on austenitizing temperatures and times, the state of homogeneity of the austenite (presence or absence of carbide, etc.), austenite grain size, and mode of formation of pearlite at the temperatures given. Except for the approximations of Mehl and the work of Dorn, austenite grain size was disregarded, though it is well known

Jan 1, 1942

By Louise Reber

THE town of Jerome is located in Yavapai County in north central Arizona. It has a population of over 6000 people and the two important mines of the district, the United Verde and the United Verde Extension, lie almost within its limits. Perched high on the southwest side of the Verde Valley, at elevations of 4800 and 5500 ft.. (1463 and 1676 m.), both mines have long tunnels from their lower levels through which ore is hauled to their respective smelters. The two smelter towns of Clarkdale and Verde, out in. the center of the valley and about 2000 ft. (609 m.) below, form part of the wide panorama that meets the eye at Jerome. This panorama and the topographic and surface features and the geologic formations are shown in a separate pamphlet. In the vicinity of Jerome, the great southern escarpment of the Arizona plateau forms the northeast side of the Verde valley. The general level of this escarpment, or "the rim" as it is called, is about 4000 ft. above the Verde River. A corresponding elevation is reached only by the, highest parts of the Black Hills, which bound the valley to the southwest. The two lava-capped mesas, known as Mingus and Woodschute Mountains, form the culmination of the Black Hills. That part of the old Black Hills mining district which lies between their crests -and the Verde River is now known as the Jerome or Verde copper district. However, if the smelters are not included, a strip about 7 mi. long and 3 mi. wide (11 by 5 km.) embraces practically all the properties belonging to the Jerome district. This strip lies parallel to and along the side of the Verde valley from about First View, 2 mi. northwest of Jerome, to the neighborhood of Allen Spring, near the south end of Mingus. Mountain. The rank of the district in copper production, as well as features of peculiar geologic interest in connection with the ore occurrences, entitle the district to much more consideration than it has received in the literature of copper mining. Arizona stands preeminent as a copper-producing state. In 1918, it produced four-tenths of the total amount produced in the United States, and nearly equaled the, combined production of its three chief competitors, Montana, Michigan, and Utah. The production of the Jerome district places it in the sixth place among the copper

Jan 8, 1920

By C. K. Leith

The question as to what grades of ore it pays to conserve for the future, and the valuation of low-grade reserves, are becoming immediate and definite as applied to the individual ore deposits, and seems to call for some sort of quantitative answer.

Jan 1, 1915

Organization Place Date 1917 American Institute of Architects Philadelphia., Pa. Dec. 26-29 American Society of Mechanical Engineers New York City. Dec. 4-7 American Mining Congress State Chapter Phoenix, Ariz. Dec. 26-29 1918 American Society of Civil Engineers New York, N. Y. Jan. 22-25 American Institute of Mining Engineers New York, N. Y. Feb. 18-21

Jan 12, 1917

Jan 1, 1935

By A. E. Back, S. F. Ravitz

When manganese ores are leached with sulphur dioxide, a large part of any zinc in the ore usually is extracted with the manganese.1 In the dithionate process,2,3 in which the manganese ore is leached with dilute sulphur dioxide gas and the manganese is subsequently precipitated by adding lime to the pregnant solution, the zinc is precipitated with the manganese. These facts suggested the possibility of applying the dithionate process to the recovery of zinc from oxidized ores or calcined sulphide concentrates. Accordingly, an investigation was begun, and preliminary tests were made on several ores and concentrates. The results were encouraging, but the need to devote available funds and personnel to other projects made it necessary to drop the work before the various factors involved in the process could be studied in detail. A brief mention of the process,4 however, elicited a number of inquiries, so that it appeared desirable to report the results of the preliminary work. The dithionate process as applied to zinc may be summarized briefly as follows: The ore or calcined concentrate is leached with dilute SO2 gas to dissolve the zinc, largely as zinc sulphate, in accordance with the following equation in which [ZnO] represents the "oxide zinc" in the ore or calcine: [ZnO] + SO2(g) + 1/2 O2 = Zn++SO4— [1] If, in the leaching step, the ore or calcine is suspended in calcium dithionate solution, the sulphate ion, as it is formed, is precipitated immediately as calcium sulphate, which is subsequently filtered off with the insoluble ore residue: Zn++SO4— + Ca++S2O6— = CaSO4(s) + Zn++S2O6- [2] An alternative procedure is to suspend the ore in water, filter off the insoluble ore residue after leaching, add calcium dithionate to the resulting zinc sulphate solution, and then filter off the calcium sulphate precipitate. In either event the zinc is obtained in the form of a pregnant solution of zinc dithionate, from which it can be precipitated as relatively pure zinc hydroxide by adding milk of lime: Zn++S2O6— + Ca(OH), = Zn(OH)2(s) + Ca++S2O6- [3] The zinc hydroxide precipitate is calcined to form the final zinc oxide product: Zn(OH)2 = ZnO(s) + H2O(g) [4] Theoretically the process is completely cyclic with respect to dithionate ion, the calcium dithionate required for reaction 2 being replaced by that formed in reaction 3. In practice, of course, small amounts of dithionate would be lost in the various filter cakes, depending on the economic washing limits. In the leaching step, however, some of the SO2 is oxidized to dithionale instead of sulphate, accord- ing to the following overall reaction: ZnO + 2SO2(g) + 1/2 O2(g) = Zn++S2O6-, [5] so that the dithionate losses are made up, at least in part. Ores and Concentrates Tested The analyses of the ores and concentrates tested are summarized in Table 1, which also includes the analyses of the calcines produced from the concentrates. The concentrates were roasted in a laboratory muffle furnace at the temperatures indicated until evolution of SO2 could no longer be detected; shallow clay dishes ordinarily were used; but calcines 2a and 2c were prepared in iron dishes, with the result that these two calcines were badly contaminated with iron scale. The "complex" concentrate, sample 1, consisted essentially of sphalerite grains containing inclusions of pyrite and other sulphide minerals too minute to be liberated by grinding within economic limits. In the " marmatitic" concentrate, sample 2, the iron was present largely as marmatite (that is, as iron sulphide in solid solution in zinc sulphide) rather than as pyrite inclusions. The zinc was present largely as the carbonate in the two "oxidized" ores, samples 3 and 4, and as the silicate in the "willemite" ore, sample 5. Leaching Tests The leaching cell was a 3-liter glass beaker placed in an electrically heated water bath manually controlled to maintain a temperature of 35°C in the leach slurry. The slurry was agitated by means of a flat paddle-type stirrer

Jan 1, 1950

By G. P. Walters, W. C. Fuller

THE production of thin films of beryllium became essential early in the irradiation program at Harwell in order to study the fundamentals of irradiation damage in this metal. In common with other metals, electron-microacope specimens of beryllium can be produced by different techniques. The techniques used to produce thin-film specimens varied according to the starting material. Most of the starting material was -0.060 in. thick. Large-area specimens (1 in. long by 0.5 in. wide) were chemically thinned to -0.005 in. thick in a solution containing 85 pct orthophosphoric acid, 10 pct chromium trioxide, and 5 pct sulfuric acid at 70°C prior to electropolishing. Small-area specimens, Fig. 1, had to be mechanically thinned prior to electropolishing because chemical thinning considerably reduces the area as well as the thickness. Mechanical thinning tends to produce a worked layer about 0.002 in. deep and hence this method cannot be used to thin bulk specimens below about 0.005 in. thick. Mechanical thinning is carried out by mounting the specimen on perspex then carefully polishing on wet grinding papers. Polishing is continued until about half the initial thickness is removed; the reverse side is then polished in a similar manner. After the bulk specimens have been mechanically or chemically thinned to -0.005 in. they are elec-tropolished in the solution shown in able I at 50" to 80°C. This solution should be prepared by adding the chromium trioxide to the orthophosphoric acid and then the glycerol last. The glycerol should be added slowly because a vigorous effervescence can occur. Electropolishing is carried out by holding the specimen in stainless-steel tweezers and gently agitating in the solution. Masking or "window" techniques are not required for beryllium, good microscope specimens being obtained from the edges of elec-tropolished foils. A stainless-steel beaker should be used, acting as the cathode and solution container. A closed circuit voltage of 30 v is used for polishing. Too low a voltage produces a matt surface and pitting occurs when it is too high. The solution temperature is important. If it is too low, the solution is viscous and bad polishing results and, if too high, etching of the specimen occurs. After electropolishing, the foils are thoroughly

Jan 1, 1963

By A. S. Richardson

VENTILATION of the Butte mines has long been a rather difficult problem because of the natural high temperature of the rock. With increase in mining depth, higher rock temperatures have been encountered, and this has caused a constantly growing demand for more effective ventilation measures. During recent years the hazards of dust in mine air have been more clearly recognized, and have necessitated the adoption of dust-prevention methods. To meet these ventilation problems in the mines of the Anaconda Copper Mining Co., a mines ventilation department was organized in 1918, to act under the direction of the general superintendent of mines. At the present time, under normal operating conditions, the force employed includes the ventilation engineer, two chief assistant ventilation engineers and eight assistant ventilation engineers. The activities of the department are, briefly: (1) planning and supervising operation of the general ventilation system; (2) planning and supervising the operation of dust-prevention measures, together with dust sampling and related microscopic work for the quantitation of the dust samples and determination of particle-size distribution; (3) the design and development of air- conditioning methods to meet present exceptionally severe temperature conditions and in anticipation of future requirements. To a large extent the technical features of the ventilation methods have been described in earlier papers by the author. This paper is written mainly to summarize past accomplishments bearing most closely on health and safety, with a somewhat more detailed account of the dust- prevention measures that have been developed comparatively recently. FACILITATING FLOW OF AIR As a basic requirement for the safety of the men, all ventilation plans are subject to a ruling that the main operating shafts must be maintained as inlet air courses. Under this condition, a safe, fresh-air escapeway is assured if a fire occurs within the mine, and the shaft is available as a base for fire-fighting operations. Control of the direction of air flow is

Jan 1, 1938

ASHBEL WELCH, LAMBERTVILLE, N. J.: Dr. Dudley has given the wear of steel rails under four different conditions. He arrives at the conclusion that the softer rails, or those that from their composition ought to be softer, wear better than the harder. But there is another condition which has an important bearing on the subject, and, should not be overlooked,-the weight on a wheel. With the lighter weights of the past, the softer rails may have worn best; with the heavier weights of the future, the harder may wear best. Weights will probably be increased up to the capacity of steel to bear; then doubtless the harder steel will wear best. A leaden rail with ten pounds on a wheel might carry millions of tons, but with one hundred pounds on a wheel, it would be destroyed by a few thousand tons. So in the days of iron rails, my experience was that the softer rails under light machinery stood better than some of the harder; but under heavy machinery the softer were much the most rapidly destroyed. His doubtless the same with steel. The pounding motion of the wheels loosens or spreads the particles of a thin film of steel; the pull lengthwise on the rail de- * Metallurgical Review, vol. i, page 1. † The remarks as here given, as in the previous discussion on steel rails, have all been written out or revised by the participants in the discussion, and represent, therefore, their mature views. It has been thought that this plan, when it can be carried out without doing any of the speakers injustice in debate, is much to be preferred to a strictly verbatim report. The remarks of Mr. Chanute were sent to the secretary after the. meeting, and although they did not form a part of the actual discussion, there can be no doubt of the desirability of including them in this report. The papers under discussion were “Rail Specifications and Rail Inspection in Europe,” by C. P. Sandberg ; " The Wearing Capacity of Steel Rails in Relation to the Chemical Composition and Physical Properties," by C. B. Dudley, and a Rail Patterns," by A. L. Holley. T. M. D., Secretary.

Jan 1, 1881

Jan 1, 1894

By C. Altstetter, Y. Huang, E. de Lamotte

Nitrogen was introduced into pure niobium (colutn-bium) and dilute Nb- Zr alloy wires by equilibration with pure nitrogen gas at high temperatures. Room-temperature hardness was correlated with the alloy composition, heat treatment, and microstructure. Hardness was found to be most sensitive to the amount of nitrogen in solution; however, a significant hardening up to 500 Dph look place upon aging of quenched alloys. A coarse dispersion of nitride did not significantly increase the hardness of the material though the nitride was found to have a hardness of 1400 Khn. BY now the marked effect of nitrogen on the properties of bcc refractorv metals is we ll-documented. There are few studies, however, in which the state of the solute has been carefully controlled. Indeed, the composition-temperature-pressure relationships in nitrogen-refractory metal systems have been determined precisely for only niobium and tantalum.'-4 Most investigations on niobium have dealt with alloys High-nitrogen alloys cleaved on (100) planes and had negligible ductility. Precipitation was found to occur in either a discontinuous or a continuous fashion, depending on the composition and cooling rates. Upon cooling, the precipitation first proceeded discontinu-ously by the nucleation of nilride needles at subbound-aries and subsequent growth of a two-phase microcon-stituent. At lower temperatures continuous precipitation occurred in the subgrain interior ahead of the discontinuous precipitation interface. containing nitrogen, carbon, and oxygen in significant but uncontrolled and, in several instances, undetermined amounts. Thus, there has been some uncertainty regarding the presence and the distribution of precipitates. This paper presents results which relate the hardness and microstructure to the heat treatment and nitrogen content of niobium and Nb-Zr alloys. Niobium rod* produced by the Wah Chang Corp.

Jan 1, 1968

By W. D. Robertson, E. Scala

Electrical resistivity of a number of pure liquid metals and alloys has been measured as a function of temperature and composition. The data show a close correspondence between the liquid and solid states with respect to thermal, structural, and compositional relationships. STUDY of diffuse scattering of X-rays by liquid metals1 has demonstrated that some degree of order persists above the melting point and that the atomic constitution of liquids is more analogous to the solid state than to a gas. Consideration of the change in various thermodynamic properties that accompanies transformation from solid to liquid leads to the same general conclusion.² evertheless, specific knowledge of the constitution of the liquid state is limited when compared with that of the solid and gaseous states owing, in part, to the difficulty of interpreting the X-ray data and in part to the indirect character of deductions based on thermodynamic data. Of the structure-sensitive physical properties, electrical resistivity of liquid metals is perhaps the most easily interpretable, particularly when comparison is made with the solid state. According to the available data, most of which was obtained prior to 1914, cubic metals exhibit a normal linear and positive temperature dependence in the liquid state and the data have been accepted without question. The divalent metals, zinc and cadmium, are apparently exceptional in that resistivity is not linear with temperature and it passes through a minimum. Mercury also exhibits a nonlinear temperature dependence but the slope is always positive. Important comparisons with magnesium could not be made at the time the following work was undertaken because the necessary experimental data were not available. Data on liquid solutions are very limited and are largely from a single source."-" Based on Bornemann's work, Norbury7 pointed out that the resistivity of liquid copper alloys appeared to be dependent on the valence of the solute and that the increase due to the solute was of the same order as in the solid state. However, large extrapolations were involved and no quantitative relationship was developed. Therefore, before proceeding with additional deductions regarding the resistivity of liquid metals and interpretation in terms of structure, it appeared necessary to verify and extend the previous work with particular emphasis on divalent metals and the effect of alloying elements of different valence in dilute liquid solutions. The present work includes: 1—A determination of the resistivity of high purity liquid magnesium, tin, indium, copper, zinc, and cadmium as a function of temperature. 2—The effect of 1 atom pct of copper, cadmium, aluminum, tin, antimony, and

Jan 1, 1954

The fall meeting of the Institute of Metals Division Will be held in Philadelphia on Sept. 30 to Oct. 2. All meetings will be held in the Ritz-Carlton Hotel, Broad and Walnut Streets, which is also the hotel headquarters. As this meeting is being held in conjunction with the meeting of the American Foundrymen's Association, the members of the Institute will have the privileges of the exhibit of the Foundrymen's Association. This, it is expected, will be one of the largest exhibits made in this country. On Monday evening, Sept. 29, there will be a meeting, in the Ritz-Carlton Hotel, of former officers and members of the Executive Committee of the Institute. It is requested that all officers and Committee members, the present as well as the past, will arrange to be present.

Jan 9, 1919

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

By H. L. Talbot, R. S. Young, A. Golledge

The differentiation of oxidized forms of lead from lead sulphide in complex products by chemical analysis is of considerable importance to certain mining and metallurgical companies. A method for the separation of "oxide" lead, (non-sulphide), from sulphide lead, based on the solubility of the former and virtual insolubility of the latter in concentrated ammonium acetate solution, has been employed for many years in the industry.1,2 Unfortunately this solvent, while satisfactory for lead sulphate and carbonate, is without action on lead phosphates or vanadates, with the result that at .Rhodesia Broken Hill Development Co. where these latter minerals are present, they have counted as sulphides when using this procedure. For the control of operations in the new concentrator it became necessary to have a closer check on sulphide lead than could be obtained by the only current method of differentiating this constituent from oxidized lead. For some time this problem has engaged our attention, and after a large number of solvents had been tried, the following procedure was evolved. Like all methods depending on selective solution in a com- plex material, it will not give 100 pct separation into oxide and sulphide portions. Because of the ease of oxidation of galena this is almost an impossibility. Our procedure will, however, give a recovery of 99-100 pct of the oxidized lead, contaminated with very small quantities of lead sulphide, and a corresponding recovery of 97-98 pct of the sulphide lead. The procedure is simple and reproducible, and gives results quite .satisfactory for routine control purposes. Experimental For this work standard samples of the following pure lead minerals were obtained from Broken Hill, Northern Rhodesia. These were hand-picked specimens, and were carefully ground to —200 mesh. Since it was realized that a fair-sized sample would be necessary for this work to thoroughly test the large number of procedures we had in mind, a compromise had to be effected between a few grams of very pure minerals and a large sample of lower grade material. For this work the presence of gangue was not deleterious, so long as the oxide lead minerals did not contain lead sulphide, and vice versa. Table I shows the lead minerals used, and their total lead content, both theoretical and actual. Apart from the pyro-morphite the minerals are seen by analysis to be quite pure. Many solutions were tried in an effort to dissolve the oxidized lead minerals and

Jan 1, 1949

By F. J. Tuck

The Hayden mill of the Ray Mines Division, Kennecott Copper Corporation, is now equipped with two 9 by 12-ft. rod mills having a daily capacity of 6000 tons of coarse-crushing plant product from the mine. These two mills crush a ¾-in. product to approximately 19 per cent on 14 mesh, with only one pass through the mills. Each rod mill has taken the place of four sets of 42-in. Garfield rolls with their attendant screens, and is making a product for the fine-grinding department comparable to that formerly made by rolls in closed circuit with screens. The rod mills are lined with wave-type liners of white iron, varying in thickness from 2 to 3 in. The shell and end liners last approximately 600 to 700 days. Manganese-steel lifter bars, 3? in. thick, are used, spaced about 11 in. apart, and they give a life of 350 to 450 days. Fig. 1 shows the general design and thickness of the wave-type liners and lifter bars; 1½-in. liner bolts are used to fasten the lifter bars to the shell. The shell liners are held in place by the tapered lifter bars. A ¾-in. wood backing is used between the shell and the liners. The rod-mill scoop has removable manganese-steel lips, which last 250 to 300 days. The scoop proper has shown some wear in spots, and these spots have been protected by rubber bolted over them. Water and milk of lime are added to the elevator feeding the mill, but not enough water to cause a pounding of the rods against the shell. Roughly, the water added amounts to 25 to 33 per cent of the ore. Additional water is added to the mill discharge to facilitate distribution to the classifier bowls in the fine-grinding department. Rods are charged to the mill once every four days, the mill being down about 20 min. for this purpose. Other delays are negligible, and usually are due to a loose liner bolt or possibly power trouble. However, these occasions are extremely rare. In charging the mill, a crane is used

Jan 1, 1939

By Mark E. Smith

To allow recovery of gold values from ore which cannot be economically processed by the mill, Pinson Mining Company has developed a run-of-mine heap leaching facility. In order to estimate production scale recovery rates, reagent consumption and percolation problems, a series of pilot scale tests were performed. These tests typically consisted of 3,630 metric tons (mt) (4,000 tons) leach ore at a grade of .94 to 1.56 grams Au per metric ton (g/mt) (.03 to .05 oz. Au/ton). Test heaps were loader stacked to approximately 4.3 meters (14 feet) high. Information from these pilot scale tests was employed in the design and construction of the production scale facility. Parameters such as spray rate, leach cycle, sprinkler placement, and barren solution chemistry were determined by the pilot tests.

Jan 1, 1984

By Bernard Kopelman

The particle size of tungsten metal powder used to make tungsten wire for use in radio tubes and incandescent lamps must be closely controlled if the highly desirable feature of nonsagging is to be achieved. Our knowledge of factors affecting the particle size of tungsten powder has been limited by lack of any extensive literature on the subject. There are no publications in the English language discussing this problem in any but the most general terms. In this paper the published experimental information on this subject is reviewed. Based on the published data and some experimental data obtained by the author, a general theory of factors affecting the particle size of tungsten metal powder obtained by reduction of the oxides in hydrogen is offered. The various forms of the tungsten oxides and tungsten metal used in the experiments described were those prepared by commercial processes, so that the experimental results obtained on a laboratory scale would be more directly applicable to actual commercial reduction conditions. The effects of time of reduction, temperature. and concentration of water vapor in the hydrogen were observed by counting microscopically the particle distribution obtained. Such a method is very time-consuming, but the data obtained by this method are more reliable and more fundamental than those obtained by any of the several instruments available for measurement of particle size. Review of the Literature Until the year 1912, tungsten powder was prepared commercially by reducing tungstic oxide in the presence of carbon or one of its compounds (such as glycerin or ethylene glycol), usually by firing the mixture in a closed fire-clay crucible. The resultant powder contained about 95 per cent tungsten.' When reduction of tungsten oxides by H² was introduced Commercially,²,³ several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-l3 While these many investigations were in fair agreement on the equilibria WO³ + H2 = WO2 + H2O and WO2 + 2H2 = W + 2H2O there arose considerable controversy as to the chemical composition of the oxide between WO³ and WO², because of very poor agreement on the equilibrium constant of this intermediate oxide reduction reaction. The controversy on this intermediate oxide has been in progress for more than 100 years. Thus Malguti,14 in 1835, decided it was WO2.56 In 1857, Riche15 proposed the formula W³O8. Usler,16 in 1865, confirmed the existence of WsO8 and further proposed W1O1l. In 1897, Desil7 agreed upon W²O8 but also found W5O14.

Jan 1, 1947