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By H. H. Wade, N. F. Schulz

The large quantities of iron-bearing materials, including taconite, semi-taconite,* and other low-grade ferruginous materials occurring in Minnesota and elsewhere, constitute an important potential source of iron. Satisfactory grade and recovery of iron ore concentrate cannot ordinarily be obtained from these ferruginous materials by simple methods of beneficiation. Iron is distinctive in that the free metal and two of its oxides [magnetite (Fe2O3) and maghemite (gamma-Fe2O3) ] are strongly ferromagnetic. The successful magnetic separation of natural magnetite from taconite has already been established on a commercial scale. The iron in semi-taconite, however, occurs largely as goethite (Fe2O3-H4O) and hematite (Fe2O3) which do not respond to ordinary magnetic separation methods. Magnetic roasting converts these iron oxides to magnetite, which can, after liberation, be magnetically concentrated. MAGNETIC ROASTING Hematite undergoes a stepwise reduction when exposed at moderately elevated temperatures to a reducing atmosphere containing hydrogen or carbon monoxide: Fe2O3? Fe3O4 ? FeO ? Fe Since the desirable product in magnetic roasting is Fe3O4, the conversion is halted after the first stage by controlling the reduction potential of the gas mixture with water vapor or carbon dioxide. The reducing gas mixture must be such that the oxygen partial pressure at the solid-gas reaction interface will be maintained intermediately between the oxygen partial pressures in equilibrium with Fe2O3 and Fe3O4 at the prevailing temperature. Because of the rapid increase in decomposition pressure of Fe3O4 with increase in temperature, the practical upper limit of useful reaction temperature is about 1400°F, above which over-reduction usually occurs in atmospheres containing hydrogen or carbon monoxide. On the other hand, useful reaction rates usually occur only above 800°F. Goethite reacts similarly except that the combined water probably has to be driven off thermally before the reduction to magnetite occurs. Iron carbonate must also be decomposed thermally to an oxide before conversion to magnetite. Iron silicates are apparently not amenable to magnetic roasting. The rate of penetration of the reaction toward the interior of a given ore fragment is dependent on the chemical composition and physical structure of the solid. Most ore fragments tested here reduced satisfactorily to 1/4-in. depth in less than 14 min at 1200°F. Some very dense fragments, however, were reduced to less than 1/32-in. depth under the same conditions. Determination of the optimum temperature, gas composition, ore fragment size, or time of exposure

Jan 1, 1961

By G. V. Jere, C. C. Patel

Chlorination of the various constituents of ilmenite by different chlorinating agents in presence of various reducing agents, have been considered on the basis of the standard free energy and standard enthalpy changes as a function of temperature. The standard free energy change considerations show that it is beneficial to chlorinate ilmenite by chlorine in the presence of carbon and also that iron constituent of ilmenite can be preferentially chlorinated by clzlorine, titanium tetrachloride or their mixture. These findilzgs have been corroborated from the published work. METALLURGICAL processes involving the use of titanium tetrachloride have gained in importance because of the use of the latter in the manufacture of titanium metal. Since ilmenite is more abundant in nature than any other titanium mineral, the future of the metallurgical processes depends on the utilization of ilmenite for the production of titanium tetrachloride. In these laboratories, investigations have been carried out on the chlorination of ilmenite under a variety of conditions.1'2 During these studies, it was noticed that 1) preferential chlorination of iron was effected at low temperatures (400° to 600°C) and at low carbon content (6 to 7 pct), 2) carbonyl chloride retarded the chlorination of iron oxides and titania perceptibly, while 3) carbon-tetrachloride, compounds of sulphur and some other catalysts favored the chlorination. Moles3 has found that oxides of iron are chlorinated in preference to titania at high temperatures, while wilcox4 has claimed the preferential chlorination of titania between 1200" and 1500°C. It has been shown in this paper that preferential chlorination of titania claimed by Wilcox is not likely to occur. Daubenspeck and coworkers5,6 have claimed the preferential chlorination of iron by chlorine or by a mixture of titanium tetrachloride and chlorine between 700° and 1050°C in the absence of carbon. Even when plain titanium tetrachloride is employed as the chlorinating agent, pascaud7 noticed the preferential chlorination of iron and other oxides. The purpose of this paper is to explain from thermodynamical considerations, the various chlorination reactions studied so far. ILMENITE CONSTITUENTS AND THEIR CHLORINATION PRODUCTS Although the general composition of the ilmenite mineral is represented as FeTiO,, most of the ilmenites found in nature have variable quantities of TiO2 (44.6 to 64 pct), FeO (4.7 to 36 pct) and Fe2O3 (6.9 to 28 pct).8 The higher content of ferric iron in ilmenites was attributed by Millerg to the presence of arizonite (Fe2O3.3TiO2). But the X-ray studies by Overholt, Vaw, and odd" have shown that arizonite is a mixture of haematite, ilmenite, anatase, and rutile. Except for the anatase, similar views have been advanced by Lynd, Sigurdson, North, and Anderson8 from magnetic, X-ray, and optical and electron microscope studies. The ilmenite ores can, therefore, be assumed to consist of mineral aggregates of ilmenite, rutile and haematite. From the free energy of formation of ilmenite (FeTiO3), it has been shown by Kelley, Todd, and King11 that ilmenite is stable even up to its melting point (1367°C) and would not undergo decomposition into its constituent oxides. Schomate, Naylor, and Boericke12 have found that in the presence of a reducing agent the iron constituent of ilmenite is selectively reduced. The reaction of chlorine with ilmenite in presence of a reducing agent can, therefore, be synonymous with that of the reaction of chlorine with the constituents of ilmenite, viz., TiO2, FeO, and Fe2O3. Most of the reaction products of chlorination of ilmenite in the presence of reducing agents will be in equilibrium with their dissociation products, depending on the temperature. The titanium tetrachloride is, however, quite stable up to 1500°C due to its covalent nature. The equilibrium for the ferric chloride system has been investigated by Kangro and Bernstorff, 13, schafer14 and Kangro and petersen,15 and the results are summarized in Fig. 1, curves a, b, and c respectively. From these results, it is clear that the ferric chloride disociates as follows: 324° to 700°C FeaCl6(g) ?2FeCl2(c) + Cl2(g) [1] 324°to 900°C Fe2Cl6(g) =2 Fe Cl2 Reaction [I] (curve a) occurs in the forward direction to about 6 pct at 400°C but falls off very rapidly with increase in temperature and beyond 600°C, it is practically negligible, perhaps due to the formation of the stable monomer, FeC13(g). As the temperature is further increased, the amount of FeCl,(g) in-

Jan 1, 1961

By A. J. Phillips, A. A. Smith, J. S. Smart

THE preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in properties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. PREPARATION OF HIGH-PURITY COPPER The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuS04-H2SO4 electrolyte using bagged anodes, low current .density (5 amp. per sq. ft.) and low temperature (25°C. max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe 2(S04)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then refiltered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2S04 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 434 by 43a by I-in anodes cast from high-quality electrolytic wire bar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars-which would result in fouling of the contacts and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By G. Derge, L. D. Kirkbride

In recent years the problem of sulfur elimination in iron and steel-making has been of increasing importance. This interest has been due to the increasing amounts of sulfur coming into the system via raw materials. As a result, many investigations have been directed at obtaining information pertaining to the rate and mechanism of sulfur removal in the blast furnace as well as measuring appropriate thermodynamic quantities. Chang and Goldmanl as well as others2'3 showed that the process of sulfur transfer from molten carbon-saturated iron to blast furnace-type slags could be considered as two opposing first-order chemical reactions. Recently, Ramachandran et al.4 have shown that during desulfurization electrical neutrality is preserved in both phases and iron and silicon are transferred into the slag concurrently with the evolution of carbon monoxide gas. They concluded that the reaction s + c-+ (0)=(S) + CO(g) does not express the stoichiometry of the sulfur transfer process. As in all previous investigations, these authors studied the process of a net transfer of sulfur from metal to slag across a slag-metal interface. However, no experimental data have previously been obtained for the process of sulfurization. It was the purpose of this study to investigate the sulfurization process, i.e., net transfer of sulfur from slag to metal. EXPERIMENTAL PROCEDURE Apparatus—The equipment used in this investiga-tion was typical of that used by others.1-3The furnace was a high-frequency induction unit powered by a 35 kw Hg spark gap converter. Fig. 1 shows a schematic diagram of the apparatus. A two-compartment crucible assembly was employed to melt the slag and metal charges; being similar to that used by Ramachandran,4 in size and design. The atmosphere was that produced by reaction of hot graphite with air. Temperature measurements were made by W-Mo thermocouples which were calibrated against a Bureau of Standards Pt - Pt 10 pct Rh couple. Temperature control was always good to * 5°C and in general was much better than this figure. Raw materials used in the experiments were C. P. reagent grade where possible. The silica used in the preparation of the slags was in the form of highly purified silica flour. Silicon and titanium additions

Jan 1, 1961

By John W. Vanderwilt

The unpredictable behavior of ground movement and subsidence has complicated the problems that attend the extraction of large quantities of ore. Special studies, particularly relating to coal mining, have yielded such a voluminous literature and so many involved controversial theories that a partial review would be difficult. Limited space makes any kind of a review impractical. The features to be considered cover only a relatively small part of the broad problems of ground movement and subsidence, but it is believed that this small part is critical. The practical aspects are important, since they bear directly on safety of mine workings, on recovery of ore and on dilution of ore in block caving and related systems for extracting large quantities of rock. The ground movement to be described occurs outside the vertical boundaries of a caved block in the area that is commonly referred to as being in the "zone of draw." "Draw" is a term that originated in the subsidence problems related to coal mining, and it is defined by a line drawn from the margin of the area caved underground to the most distant fracture at surface on the same side of the caved area as shown in Fig. I.' A line thus drawn is called the cave line, and its angle with respect to the horizontal is the cave angle or angle of draw. It is understood that the line is taken normal to the limit of mining, and in a vertical plane. The prevailing theories as to draw and angle of draw assume that appreciable movement occurred along the cave line, which has been described as a fracture resulting from the shearing action brought about by the weight of the overlying load. Fig. 3 shows diagrammatically the mechanics of ground movement adjacent to an area of subsidence according to the prevailing theory of draw (A, from Royce2) and, for comparison, ground movement observed in the Climax mine (B). The text in Peele's Handbook2 referring to Fig. 2 does not state the meaning of the "original position of top of workable ore" in the rectangular space above "ore in place," and the arrows are not explained. However, this presentation is most concerned with the zones outside the rectangle. According to the prevailing theory, as shown at the extreme left under A, Fig. 2, the vertical tension cracks at surface change at a shallow depth to shear fractures forming the cave line, and it is assumed that appreciable movement takes place along the cave line toward and into the subsiding caved block. The mechanics of ground movement observed in the Climax mine, as shown under B, Fig. 2, does not accord with the prevailing theory, particularly as regards the cave angle and draw. The vertical tension cracks seen at surface die out at depths of 150 to 225 ft. and shear fractures do not develop. Movement is confined at surface to a mantle of rock 50 to roo ft.

Jan 1, 1949

By W. J. Locher

One important means of reducing steel consumption in grinding mills is not mentioned in S.G. Malghan's paper. It is simply to reduce the oxygen content in the mill and pulp. While oxygen dissolved in pulp is not readily reduced without additives, reduced aeration and reduced ventilation of grinding mills are often feasible. It is not necessary to completely eliminate the oxygen to achieve substantial benefits, since corrosion rates vary with oxygen content in a manner analogous to combustion rates as oxygen content increases. It is difficult to generate indisputable quantitative data on the relationship of oxygen reduction in a milling system to changes in consumption of grinding steel. Perhaps this accounts for the absence of technical papers on the effects of reducing oxygen content in grinding mills by reducing aeration of pulp and ventilation of grinding mills. One qualitative observation is that mills operating at a lower percent of critical speed will tend to have lower media consumption for similar fineness of grind without necessarily having an equivalent reduction in power consumption per ton of product. Reduced mill speed would also tend to reduce both ventilation of the mill and entrainment of air in the pulp. Larger grinding mills tend to be more media efficient because they operate at a greater ratio of charge volume to pulp surface area, which will tend to reduce the aeration per unit of pulp volume. The mechanical steps required to reduce aeration of grinding mill pulps depend on the configuration of the grinding circuit and related process. Reply by S.G. Malghan Mr. Locher stated that my paper did not mention the reduction of oxygen content of the pulp as a potential method of decreasing the steel consumption. I would like to bring to the attention of Mr. Locher that an indirect reference was made to the fact that pulp oxidation potential controls the corrosion wear of steel. Though dissolved oxygen is one of the factors that controls oxidation potential, additional discussion was deliberately avoided for the reasons mentioned by Mr. Locher. The most important reason being the difficulty of decreasing and controlling the oxygen concentration of the pulp in a commercial mill.

Jan 1, 1984

By Donald L. Katz

THE Oklahoma City Wilcox sand, discovered on March 26, 1930, has produced 394 million barrels of crude oil and 819 billion cubic feet of natural gas as of July 1, 1941. The 100,000-bbl. wells, pressures of 2600 lb. per sq. in., and flows of "Wilcox" sand caused exciting moments in the early life of the field. Today the reservoir is substantially at atmospheric pressure and produces 75,000 bbl. of crude oil daily through 466 pumping wells. Early estimates of the initial crude-oil content of the "Wilcox" sand' indicated that about 600 million barrels of crude oil would remain after the pumping wells ceased to produce economically. The Oklahoma City Wilcox Secondary Recovery Association was organized in March 1939, to study the possibilities of recovering a portion of this oil. Only a very brief summary of the information available can be presented in a paper of this nature. Some simplification and generalizations are necessary to give the over-all picture in so short a space and statements made may not apply to a specific well or small area. Since the area under consideration by the Association is that north of the south line of section 22-11-3, some information will be presented for areas A, B, C, r, 2, 3 and part of 4 of Fig. 2, and some will be for the entire Wilcox zone west of the fault. This paper is essentially an abstract of an engineering report made by A. D. Small, B. T. Murphree, M. C. Sons and the author for the Oklahoma City. Wilcox Secondary Recovery Association on Sept. 5;.1940. Some information is taken from a report to the Association by C. V. Sidwell on March 1, 1940, and some data are from a recent report by A. D. Small. It gives a brief history of the Wilcox zone, estimates of the initial oil contents of the reservoir, present conditions in the reservoir, and probable results from several programs of "secondary recovery." HISTORY OF WILCOX ZONE The Wilcox sand lies on the flank of the general structure, as shown by cross section of Fig. 12.1 .4 and areal map of Fig. 2. The sand is of Ordivician age and is composed of well assorted, rounded' sand grains with no apparent cementing material. The loose texture of the sand is shown by the enormous quantities of sand production from the wells and from the soft cores. The productive sand varies from zero thickness on the east to 220 ft. maximum and to zero thickness on the west because of water. The development of the pool4 was dependent upon drilling restrictions within the city limits, which accounts for the spacing of drilling operations listed in Table I by years. In 1931, areas I through 7 of Fig. 2 were open for drilling with the exception of some west-edge properties, and all wells drilled before Feb. I, 1935, were in this portion of the field. Nearly all wells drilled from 1933 to 1937 were in areas A, B and C. Since 1939, the newly drilled wells have gradually enlarged the producing area toward the west in the northern portion.

Jan 1, 1941

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members.) Members and guests who called at Institute headquarters during the period May 10, 1916 to June 10, 1916: G. Aertsen, Philadelphia, Pa. Hennen Jennings, Washington, D. C. Frederick C. Alsdorf, Wickenburg, Ariz. H. M. LaFollette, LaFollette, Tenn. A. H. Anderson, Worcester, Mass. E. T. Lednum, Chicago, Ill. J. H. Batcheller, Mattapoisett, Mass. Francis Church Lincoln, Reno, Nev. Arthur B. Clark, Sheridan, Mont. H. Mortimer-Lamb, Montreal, Canada. J. Murray Clark, Toronto, Canada. Andrew W. Newberry, San Francisco, Cal. J. H. Collier, Oakland, Cal. C. E. Pettibone, Cleveland, 0. H. S. Emlaw, Spring Lake, Mich. Heinrich Ries, Ithaca, N. Y. E. L. Estabrook, Platteville, Wis. C. S. Robinson, Youngstown, 0. James W. Hambleton, El Paso, Tex. - M. K. Rodgers, Basin, Mont. James Henderson, London, England. E. J. Rossbach, St. Louis, Mo. G. P. Hulst, East Chicago, Ind. J. B. Tyrrell, Toronto, Canada. William F. Jahn, Riebeling, Mont. G. B. Waterhouse, Buffalo, N. Y.

Jan 7, 1916

(The following list contains the names of those members of the Institute of whose connection with military service we have only recently become acquainted; it also includes the names of a few who have recently been promoted or transferred, indicated by a *. A complete list was published in the Year Book, issued as a supplement of the Bulletin for March, 1918.) ANDERSON, AMIL A., Co. A, 309th Regiment Engineers, 84th Div., American E. F., Care Postmaster, New York. ARMSTRONG, HAROLD K., Pilot, Naval Aviation, U. S. Naval Air Station, Miami, Fla. BASSETT, ARTHUR F., Co. 6, -E. 0. T. S., Camp Humphreys, Va. BEDDALL, THOMAS H., Adjutant, 1st Battalion, 1st Gas Regiment, American E. F. BERNARD, CLINTON P., Candidate, 12th Observation Battery, F. A. C. 0. T. S., Camp Taylor, Ky. BROOKE, LIONEL, 50th Co., 13th Battalion, 5th Replacement Engineers, Camp Gordon, Ga. BROWNING, EDWARD, Corp., 1st Regiment Engineers, Co. D, American E. F. BUGBEE, EDWARD E., S. A. T. C. Headquarters, Raleigh N. C. BUTTERFIELD, G. BRUCE, CO. C, 605th Engineers, American E. F. CADOT, J. J., 1st Lieut., U. S. Air Service, American E. F., Care Post- master, New York. CARLOCK, J. B., Major, 2d Battalion, 1st Gas Regiment, American E. F., France.

Jan 12, 1918

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members..) Members and guests who registered at institute headquarters during the period Dec. 10, 1915 to Jan. 10, 1916: A. R. Fletcher, Palo Alto, Cal. H. L. Hollis, Chicago, Ill. R. G. Hall,. St. Louis, Mo. Howland Bancroft, Denver, Colo. Walter E. Koch, Terlingua, Tex. G. D. B. Turner, Butte, Mont. George A. Macready, Searchlight, Nev. H. A. Wheeler, St. Louis, Mo. H. W. Edmondson, Concheno, Chili., Mex. George B. Rodgers, St. Francois, Mo. Arthur F. Taggart, New Haven, Conn. Paul S. King, Wilmington, Del. H. V. Winchell, Minneapolis, Minn. G. H. Clevenger, Palo Alto, Cal. Frank A. Ross, Spokane, Wash. J. W. Beard, Syracuse, N. Y. W. D. B. Motter, Jr., Benson Mines, N. Y. Albert De Deken, Louvain, Belgium. S. Le Fevre, Forest Glen, N. Y.. James H. Smith, Jr., Mount Carmel, Pa. E. H. Hamilton, formerly manager of the Virginia Smelting Co., West Norfolk, Va., has become consulting metallurgist to the Consolidated Mining and Smelting Co., of Canada, Ltd., Trail, British Columbia.

Jan 2, 1916

By E. A. Holbrook

MINING Metallurgy, and Petroleum Engineering department in our colleges are facing a crisis; indeed, conditions that threaten their very existence. Unless the Army, Navy, and War Manpower Commission change their present policy, within two years mineral industries education as now carried on will die, because no ablebodied students will be left in the course. If this is the decision of our responsible governmental agencies we of the mining schools must perhaps accept it as a war measure. It might be well however, for the executive of our mining metallurgical, and oil companies to look ahead a, to where they are to recruit a supply of young technically trained engineers. You can no more operate a mine, a steel plant or an oil company without trained engineers than you can operate a battleship without mechanical and electrical engineers.

Jan 1, 1943

By William Sellers

tested without knowing anything of their chemical composition. I had these pieces separately placed upon 10-inch bearings under a 7-gross ton lianlrner, a piece of 2½-inch round iron laid upon them as a fuller, and the hammer allotved to fall from 20 inches above the fuller, which, according to Haswell, gave a ldow of 67.75 gross tons. The pieces were then turned orcr, the fuller placed upon the convex surface, and the harnnler allowed to fall from 13 inches above the fuller, giving a blow of 58.46 gross tons. You will see that the rails do aot show ally bigrls of ruptnre, and their color at the points of torture prove them to have been absolutely cold when the test was made. I thirk these rails ought to be reasonably safe in the track. As you see by this piece of the head of one of these rails, I had it plarred, and then some teeth cut in it by a cold clrisel, and one-half of them pounded down with a hammer. The teeth of my rack did not break off. The analyses of these rails substquently made are: I. 11. Carbon,... 0.110 0.880 Silicon,..0.050 0.058 Phosphorus ,..0.086 0.082 Manganese,.. 0.042 0 840 In conclusion, I will say that Dr. Dudley's paper as a contribu tion to our knowledge of steel rails is valuable and interesting, but I protest against his conclusions king reoeived as manufacturing or comtnercial axioms. From its being presented in the form-of a report to the leading railroad of the country from one of its trusted officers, as well as from the tone of the concluding deductions, it is liable to be so received by railroad men. If any railroad com pany desires rails made under either of Dr. Dudley's formulas, and are willing to pay a price large enough to cover the loss in making them, dl and good; but so long as the rail makers are compelled to gwrrantee the wear of their rails for a given number of years, justice reqnires that. the composition of the steel from which these rails are made should be left to them. WILLIAM SELLERS, PHILADELPHIA: The very interesting paper upon the wear of steel rails that has just been read preseak the record of a series of investigations that are extreniely valuable, and the deduction that bas been drawn from the results noted seems to be unavoidable; the tests, however, to which it is proposed steel rails shall be subjected hereafter, with a view to determine their quality, sllould

Jan 1, 1881

By W. L. Phillips

Nickel alloys containing approximately 0.5, 2.0, and 6.0 at. pct of Os, Pd, Ru, and Rh were Prepared by vacuum melting. Tension tests were carried out at 25°, 500°, 800°, and 1000°C; stress-rupture tests were carried out at 650° and 800°C. The room- and elevated-temperature tensile strength, as well as the stress-rupture life, increased for the same atomic percent in the order palladium, rhodium, ruthenium, osmium. The ductility decreased with increasing concentration or temperature for a given concentration. The results are discussed in terms of solid-solution theory. BOTH solid-solution strengthening and weakening have been observed in alloys. The simple rules which have been suggested to explain alloy strengthening are subject to several exceptions and deviations based on atom size and valency effects. The purpose of the present investigation was to extend the knowledge of the effect of solid-solution alloying on the mechanical properties of several Ni-Pt group metal alloys at room and elevated temperatures. The platinum group metals, osmium, ruthenium, rhodium, and palladium were chosen as the solute elements because of their different valencies and atom sizes. Nickel was chosen as the base material because of the large amount of previous literature available on nickel alloys. EXPERIMENTAL PROCEDURE Grade A Carbonyl nickel powder having the following composition: C, 0.07 pct; Fe, 0.013 pct; Mn, 0.0005 pct; Si, 0.016 pct; Mg, 0.0003 pct; S, 0.003 pct, was purchased from the International Nickel Co. The platinum-group metal powders were purchased from A. D. Mackay Co. The powders were weighed, cone-blended for 4 hr, and vacuum-melted into 1-in.-diam billets, approximately 2 in. long. The ingots were homogenized for 5 hr at 1800°F before being extruded into 1/4-in. rods at 2100°F. The alloy compositions are shown in Table I. Typical impurity values were not significantly different than that of the as-received nickel. All alloys were single phase. The lattice parameter of each alloy after the heat treatment described below is also included in Table I. Each alloy was annealed at 2200°F for 1 hr and air-quenched to comparable grain sizes (ASTM G.S. No. 4-5). The rods were then machined into test samples 0.160-in. diam and 0.750-in. gage length. Tension testing was carried out in an In-stron tension-testing machine at a strain rate of 0.02 in. per in. per min. An extensometer was used to determine the room-temperature yield stress. Stress-rupture testing was carried out in an Arc Weld stress-rupture unit. All testing was performed in air. EXPERIMENTAL RESULTS A) Room-Temperature Mechanical Properties. The 0.2 pct yield stress, ultimate tensile strength, and elongation for all alloys tested at room temperature are plotted as a function of atomic percent solute element in Fig. 1. The ultimate tensile strength for the same atomic percent increases in the order palladium, rhodium, ruthenium, osmium. The yield strength at low concentrations, -0.5 at. pct, increases in the order osmium, palladium, ruthenium, rhodium. At higher concentrations, 3.0 and 10.0 pct, the yield strength increases in the same order as the tensile strength. Both yield strength and tensile strength increase rapidly ini-

Jan 1, 1964

By M. C. Fuerstenau, A. M. Gaudin

A homogeneous suspension is viewed by X-rays. The radiation density seen, affords a measure of the extra absorption due to the solids contained. This radiation density, at a predetermined depth, varies with time. The chart of this relationship gives the desired determination. s it is frequently necessary to know the distribu-rt tion of particle sizes in various products used in industrial applications, a number of means have been devised for these determinations. Some of them include direct microscopic measurement, screening of product, extraction of samples from a settling slurry, air and liquid elutriation, adsorption of gases and liquids, and light absorption. The absorption of light as a means for particle size analysis has been known and employed for some time. X-ray absorption has not received the attention that light has enjoyed primarily because of the complex and costly instrumentation involved with X-rays. In 1954, Brown and Skrebowskil suggested the use of X-rays for this type of determination but did not supplement their suggestion with experiment. In 1958, the authors conducted size analysis experiments on suspensions of quartz with the Trans-viewer: an X-ray unit specifically adapted for sedimentation research, and Rossa conducted experiments in a similar manner in 1959 with a stable gamma emitter, AmZ4l, on suspensions of uranium oxide. To illustrate the applicability of X-ray absorption for analyzing particle size distributions, an essentially mono-energetic and well collimated X-ray beam was used as a source. The beam was made mono-energetic by placing a zirconium filter before the counting window together with feeding the pulses from the proportional counter into a reverter, a device capable of discriminating against pulses of various heights. The sketch in Fig. 1 shows the collimation arrangement in more detail. As shown, the X-ray beam was collimated by inserting a 3/8-in. ID pipe into one of the ports of the X-ray tube and further by two small steel plates with slits 3/32-in. wide and 1/2-in. long placed in front of the window of the Geiger-Mueller (G-M) tube. One of the plates was located 1/2 in. and the other 2 1/2 in. from the window of the counter; both plates were contained in an aluminum holder mounted on the box containing the G-M tube. This type and degree of collimation should eliminate any intensity due to scattered radiation; the transmitted intensity would then be solely a functior. of the absorption by the suspension at that level. Experimentally, homogeneous suspensions of finely ground quartz were prepared, Daxad (a sulfo-nated compound made from wood) was added as dis-persant, and the transmitted X-ray intensity measured as a function of time at a fixed depth in the suspension. In more detail, the experimental procedure involved the following: 1) measuring the transmitted X-ray intensity through the Daxad solution at a predetermined position or settling depth in the absence of solids, 2) placing a known amount of dry solids into the vessel and agitating thoroughly, 3) measuring the transmitted X-ray intensity at time zero (i.e., immediately upon cessation of stirring), and 4) measuring the transmitted X-ray intensity as a function of time (a 10-sec counting interval being chosen and counting being started 5 sec before the desired time). Since a linear relationship exists between percentage solid in a slurry and the logarithm of transmitted intensity for a homogeneous material, the cumu-

Jan 1, 1961

By R. G. Weavind, R. S. Young, I. Wolf

ONE of the most important fields of investigation at the Diamond Research Laboratory in Johannesburg is concerned with improvements in metallurgical practices for the diamond mining companies, with particular reference to increased recoveries of the smaller industrial stones. Considerable work has been done on the possible application of flotation processes to the diamond industry. From the viewpoint of recovery processes, diamonds in their natural state may be grouped into two classes, the water-repellent diamonds, which adhere to a grease surface, and the water-avid diamonds, which, because of their wettability, will not adhere to a grease surface and must be recovered by means other than the grease tables used for water-repellent diamonds. Experiments in the flotation of small diamonds from both kimberlite and alluvial deposits indicate the following conclusions: Water-repellent diamonds: Satisfactory flotation of —16 mesh diamonds, which are naturally water-repellent, may be accomplished using either Aero-float 25 together with cresylic acid, or Du Pont B23 as frother together with kerosine as auxiliary oily conditioner or froth stiffener. The quantities of reagents required are of the order of 0.15 lb per ton Aerofloat and 0.18 lb per ton cresylic acid. The use of acid circuits is detrimental, and for best results a pH between 7 and 9 should be maintained. R. G. WEAVIND and I. WOLF are with the Diamond Research Laboratory, Johannesburg, South Africa, and R. S. YOUNG, Member AIME, is Director of Research, Diamond Research Laboratory. TN 76B. Manuscript, March 23, 1951. A flotation period of 5 to 10 min is necessary to insure that all floatable diamonds are removed. Diamonds larger than 16 mesh cannot be recovered satisfactorily by flotation. Xanthates do not act as collectors for diamonds, and this is probably associated with their inability to impart a water-repellent surface to this mineral. Water-repellent diamonds smaller than 28 mesh can be floated quite well by the addition of a frother alone, such as pine oil or Du Pont B23. Water-avid diamonds: Partial flotation of the smaller sizes of wettable diamonds can be achieved by preconditioning with fatty acid soaps, cationic amines, and similar reagents, which will impart a water-repellent film to diamonds. Washing to remove excess reagent, followed by flotation, will result in a fair recovery, but the latter is much lower than for water-repellent diamonds. Crushed boart: Recovery of crushed boart from the waste products of industrial uses is best accomplished by first conditioning the diamonds present in the mixture with fatty acids, cationic amines, etc., removing the conditioning agent by washing, and floating in a cell of the pneumatic type. Flotation reagents found to be most suitable are Du Pont B23, and Aerofloat 25 together with cresylic acid. The optimum quantities are 1.2 g Du Pont B23, and 0.55 g Aerofloat plus 1.4 g cresylic acid, per liter of pulp in the cell. A solids-to-water ratio of 1 to 4 is found to be the most suitable, and alkaline circuits are necessary for best results. Diamonds larger than 28 mesh are not recovered satisfactorily by this procedure, but for finer sizes flotation offers an excellent procedure for the reclamation of this strategic industrial material.

Jan 1, 1952

By J. Chipman, J. C. Fulton

Reduction of silicon from blast-furnace-type slags by carbon-saturated iron is a very slow reaction even under conditions of rapid stirring. Equilibrium under atmospheric pressure of carbon monoxide was approached from both sides, and the silica-silicon relation was established at temperatures of 1425º to 1700°C for slags containing up to 20 pct Al2O3. Silicon carbide is formed by reaction of graphite with high silica slags and the conditions for its formation were determined. Activities of SiO2 and of CaO in their binary solutions at 1600°C were determined. The effects on the activity of SiO2 were established for additions of 10 to 20 pct AI2O3 and of 10 pct MgO. STUDIES of chemical reactions between blast-*>-5 furnace slags and metal have been focussed on the transfer of sulphur from metal to slag. The important role which silica reduction plays in this process' has led to a study of the transfer of silicon from slag to metal and the equilibrium represented by the equation SiO2 (in slag) + 2C (graphite) = Si + 2CO (g). [I.] The authors2 have published an account of the experimental method employed in attacking this problem and of three series of experimental results at 1600°C. This paper contains data on some additional compositions and extends the observations to cover the temperature range 1425° to 1700°C. The data are used to determine the activity of silica in the slags. As in the earlier experiments, the atmosphere was carbon monoxide which flowed through the furnace at 150 ml per min. In certain heats designated in the tables and figures, the gas was bubbled through the melt using a graphite tube. The latter increased in porosity during a run and in some cases bubbling ceased as indicated by cessation of surging. Some results were discarded for this reason. Experimental Results The new data are shown in Tables I through V and both old and new data are plotted in Figs. 1

Jan 1, 1955

By E. J. KENNEDY

FEBRUARY 15-18 will be the outstanding dates of the month for members of the A. I. M. E., for then the 141st Meeting of the Institute is to be held in the Engineering Societies Building, at New York. What with 41 technical sessions, the Annual Business Meeting at 4 o'clock Tuesday afternoon,, two sessions of the Section and Division delegates, minor committee meetings, and the many luncheons and dinners, the Dinner-Smoker, Informal Dance, President's Reception and the Dinner-Dance, the opportunity will be limited to do- more-than cast sheep's eyes at New York's other multitudinous attrac¬tions until the meeting is over. The technical program is diverse but well organized. The sessions are almost equally divided among the four days, with ten on Monday, Tuesday, and Wednesday, and 11 on Thursday. The meeting opens Monday morning with registration. Be sure to attend to this detail. Failure to do so may have its repercussions at the meeting and throughout the year.

Jan 1, 1932

GENERAL COMMITTEE GERALD F. G. SHERMAN, Chairman. ARTHUR NOTMAN, Secretary. NORMAN CARMICHAEL, JOHN C. GREENWAY, W. L. CLARK, W. G. McBRIDE, B. BRITTON GOTTSBERGER, FOREST RUTHERFORD. General Committee on Transportation WALTER DOUGLAS, Chairman. CLEVELAND E. DODGE, Secretary. ARTHUR S. DWIGHT, JOHN C. GREENWAY, JULIUS KRUTTSCHNITT, JR. Committee at El Paso W. D. GORDON, ROBERT McCART, JR., W. W. ROSE. Committee at Santa Rita JOHN M. SULLY, Chairman.

Jan 12, 1916

By D. J. MacKinnon, J. M. Brannen

Smooth, compact, dendrite free 24-h zinc deposits have been electrowon from zinc chloride electrolyte using a diaphragm cell. The cell consisted of sealed anode compartments containing DSA anodes separated from an open cathode compartment by Dynel cloth membranes. Fresh electrolyte was fed to the cathode compartment where zinc deposition onto an aluminum cathode was aided by air sparging. The catholyte passed through the diaphragms into the anode compartments from which chlorine gas and spent anolyte were withdrawn. Standard electrolysis conditions were: 15 g/L Zn, 0.12 M HCI, I5 mg/L tetrabutylammonium chloride (TBACI) as the addition agent, 35°C, and 323 A/m2 (30 ASF) current density. The effect of variations in these conditions on the morpohology orientation, current efficiency, and energy requirement for 24-h zinc deposits was determined. The effect of total chloride ion concentration on the zinc deposit was studied by adding various amounts of NaCl to the electrolyte.

Jan 1, 1983

By Charles Catlett

(San Francisco Meeting, October, 1911.) WHILE the occurrence of phosphorus in coking-coal has assumed less importance with the development of the open-hearth method of steel-making, it may not be without interest to note the form in which phosphorus exists in one particular coal-seam. In the examination of what is known as the Big seam, which outcrops a few miles west of Columbiana, Ala., my attention was called to the distribution through the coal, in the form of minute veins and particles, of a resinous-looking substance. A small amount of this was selected, and was provisionally identified as evansite (Al6, P2 014. 18 Aq). Subsequently, through the courtesy of Dr. Sharshall Grasty of the Geological Department of the University of Virginia, I was able to secure an additional amount of material, which was purified down to about 0.3 g. This was examined by Prof. John J. Porter of the University of Cincinnati, and gave the following partial analysis

Nov 1, 1911