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By George R. Ensminger, E. Heaton Hemingway

During the past year, the Watertown Arsenal has been interested in the occluded gas and oxide content of certain ordnance steels in order to determine, if possible, whether some of the peculiar failures in their physical properties might not be traced to these causes. For the purpose of best accomplishing a study of this nature, it was decided to heat the various samples of steel in a vacuum for definite periods of time at high temperatures and carefully examine the quantity and composition of the gases evolved. By the use of a fused quartz tube fitted with a water-cooled, ground-glass stopper, it was possible to maintain a vacuum at a temperature of 1000" C. for 10 hr. without perceptible leakage being evidenced as measured by a McLeod gage. The silica tube was connected with an evacuating system so constructed that the volatilized gases could be removed from time to time and a low vacuum of 0.0002 to 0.0010 mm. of mercury continuously maintained. At no time during the period of heating or in the removal of the gases did the evacuated system come in contact with rubber stoppers or any rubber connections, making contamination from such a source, impossible. In other words, the only volatile products that could be: obtained must necessarily have come from the steel itself or from the glass and fused quartz system or from the mercury used as a sealing agent. In the carlier experiments, the steel treated was in the form of turnings, but this practice was discarded because the weight's of the turnings before and after being heated were widely inconsistent,, even when taken from the same piece of steel. This discrepancy developed largely through variation in the amount of metal volatilized with the gases; this metal could always be seen in the form of a ring where it condensed in the cooler portion of the tube in either the amorphous or crystalline condition. Because of the frequency in occurrence and the variation in the manner of deposition, this material was roughly analyzed and found to consist for the most part of iron. At the same time two samples of steel that had been

Jan 1, 1922

By E. Heaton Hemingway, George R. Ensminger

During the past year, the Watertown Arsenal has been interested in the occluded gas and oxide content of certain ordnance steels in order to determine, if possible, whether some of the peculiar failures in their physical properties might not be traced to these causes. For the purpose of best accomplishing a study of this nature, it was decided to heat the various samples of steel in a vacuum for definite periods of time at high temperatures and carefully examine the quantity and composition of the gases evolved. By the use of a fused quartz tube fitted with a water-cooled, ground-glass stopper, it was possible to maintain a vacuum at a temperature of 1000" C. for 10 hr. without perceptible leakage being evidenced as measured by a McLeod gage. The silica tube was connected with an evacuating system so constructed that the volatilized gases could be removed from time to time and a low vacuum of 0.0002 to 0.0010 mm. of mercury continuously maintained. At no time during the period of heating or in the removal of the gases did the evacuated system come in contact with rubber stoppers or any rubber connections, making contamination from such a source, impossible. In other words, the only volatile products that could be: obtained must necessarily have come from the steel itself or from the glass and fused quartz system or from the mercury used as a sealing agent. In the carlier experiments, the steel treated was in the form of turnings, but this practice was discarded because the weight's of the turnings before and after being heated were widely inconsistent,, even when taken from the same piece of steel. This discrepancy developed largely through variation in the amount of metal volatilized with the gases; this metal could always be seen in the form of a ring where it condensed in the cooler portion of the tube in either the amorphous or crystalline condition. Because of the frequency in occurrence and the variation in the manner of deposition, this material was roughly analyzed and found to consist for the most part of iron. At the same time two samples of steel that had been

Jan 1, 1922

Secretary's Note.—M. Beutter's introductory remarks, being simply a resume of Prof. Hone's paper, with a disclaimer of the intention to criticise it, have been omitted, and the remainder of this contribution lias been somewhat condensed, without omitting any essential statements. M. Beutter, St. Etienne, France* (communication to the Secretary†):—Professor Home observes in $ 47 of his paper that the fluid-compression of steel diminishes piping by forcing the liquid and viscous metal, while the pipe is forming, or after it has formed, into the space so produced, and proceeds to study the different systems of compression, alluding to the four principal ones: Whitworth, Illingmorth, Williams, and Harmet. Having now for many years had in use the last-named process, that of M. Henri Harmet, I shall attempt to explain the difference between it and the three other processes named. The Harmet process does not diminish or close the pipe after it has formed, but prevents it from forming; and I may add that it is the only one of the four which produces this result. It is true that the Whitworth process diminishes the interior hollow by localizing it around the central axis of the ingot, which is afterwards removed by trepanning the hollow forg-ings for which this process has been, I believe, always exclusively used. The Illingworth and Williams processes, which, in my opinion, are applicable only to small ingots, of necessity allow the pipe to form, or (to use the expression of Professor Howe) they allow the surface of the lake of liquid steel to sink into the interior of the ingot, since they involve waiting a certain time before compression, so that (in the case of the Williams process) the ingot-mold can be opened without danger, or (in the case of the Illingworth process) so as to avoid the risk that the steel may enter the grooves produced by the removal of the distance-bars. During the time required for

Jan 1, 1908

By T. A. Read, H. K. Birnbaum

STRESS-induced twin boundary motion in the AuCd ß'phase (52.5 at. pct Au 47.5 at. pct Cd having an orthorhombic structure (space group D h)' was discussed for the case of transformation twins.' Mechanical twinning, i.e., introduction of new twin orientations by the applied stress was sometimes observed in the ß' phase which contained two transformation twin orientations. (See Ref. 2 for experimental details.) The transformation twins terminated at the mechanical twin boundary; the two initial orientations having been twinned to the new orientation as shown in Fig. l. In a "hard" tensile instrument, formation of each mechanical twin was accompanied by a sharp drop in load (and an audible click) resulting in a typical serrated load-extension curve. The mechanical twins increased in width and additional twins were nucleated as the load increased until the entire specimen was occupied by the mechanical twin orientation. A restoring force2 caused the mechanical twin and transformation twin boundaries to return towards their initial configuration on releasing the load. In a stabilized specimen* the total strain introduced by mechanical twinning was recovered on releasing the applied stress. Initial and final microstructures were identical. After decreasing gradually to a critical width, mechanical twins suddenly disappeared accompanied by audible clicks and sharp increases in load (measured at a constant rate of crosshead motion in a "hard" machine). Mechanical twins could be stabilized in any position by maintaining the applied load for a sufficient time, indicating a decrease in restoring force with time similar to that observed for transformation twins.' Orientation relationships for mechanical and transformation twins were determined and are shown in Fig. 2. The mechanical twin, T3, was twin related to transformation twin, T,, by reflection in (1ll), and twin related to transformation twin, T2, by reflection in (111)T, . T, was related to T, by reflection in(ll1)T1 . The "average" mechanical twin composition plane lay several degrees from (1ll), . In every specimen which mechanically twinned, orientation T3 was most highly favored by the applied stress, i.e., it was the twin orientation which provided the greatest change in length compatible with the direction of applied stress

Jan 1, 1961

By F. E. Buch

THE Smelter is designed for a production capacity of 10,000 short tons of blister copper per month, when operating on the present concentrate grade. The Smelter lay-out is shown in Fig I. The major units of equipment comprise two reverberatory furnaces, three 13 by 30 ft Peirce-Smith converters, two straight line casting machines, one being served by a 13 by 30 ft holding furnace and the other by a ladle tilting quadrant, two converter ,aisle cranes and two converter blowers. The plant is compact and the general arrangement of standard gauge railway tracks and conveyor belts provides for a smooth flow of incoming materials and metallurgical products. Concentrate is received by conveyor belts and fluxes in standard railway trucks. The local track system is covered by an electric trolley locomotive. The Smelter treats a wet (10 pct moisture) flotation concentrate containing approximately 53 pct total copper and 0.9 pct oxide copper. The predominating minerals are chalcocite, chalcopyrite and bornite accompanied by small quantities of malachite and cuprite. The gangue is highly siliceous and requires limerock as a flux. Metallurgy would be straightforward were it not for the necessity for eliminating k bismuth which occurs as an impurity in the ore along with the copper. Directly or indirectly most of the Smelter problems can be traced to the necessity for bismuth removal. Copper recovery, based on new copper treated, averages 97.5 pct. GENERAL DESCRIPTION Flotation concentrate, containing to pct moisture, is conveyed from the filter plant to the smelter storage bins by conveyor belts, the material being weighed in transit by a revolving drum type of weigh-hopper manufactured by Samuel Denison and Son, Ltd. The weigher consists of a steel drum with dished ends carried on a horizontal shaft and rotated by an 8 hp squirrel-cage motor through a worm and spur reduction gear. A feed mouth in the drum permits of filling and discharging. The whole unit is supported on a framework resting on weighing levers, which in turn connect to transfer levers, thence to an indicator of the steelyard type situated 16 ft from the centre line of the drum. The indicator is of the "Denison" patent equilibrium controlled ticket stamping type, insuring mistake-proof records by a combination of electrical and mechanical movements which prevent the operator from printing until the cover enclosing the steelyard is closed and until the poise-weights have been set correctly to the weight of the hopper and contents. The machine is capable of weighing 30 short tons at a time but the usual load is 28 tons. After obtaining the gross weight the drum is rotated and discharged into a receiving bin situated below it. The empty drum is weighed and the net weight re-

Jan 1, 1947

By E. A. Gulbransen, J. W. Hickman

INTRODUCTION DURING the past two decades considerable progress has been made in the art of manufacturing heater alloys. The conventional iron-chromium-nickel alloys have been improved by the addition of small quantities of other elements. Up to the present time, to our knowledge, there has not appeared a systematic study of these alloys where the newer tools of investigation have been brought to bear on the problem. It is not yet clear what roles the additional elements play in increasing life time in usage. As a first approximation one might guess that elements such as manganese, silicon, zirconium, calcium and aluminum would aid in the formation of a protective film on the alloy surface, thus retarding the oxidation rate and increasing lifetime. If these additional elements do form protective oxides in the outer surface of the oxide film, it may be possible to identify them by means of reflection electron diffraction. It is also possible that the additional elements may not diffuse to the surface but may remain at the interface between the oxide and the metal. Then, too, the major elements in the alloys undoubtedly form oxides which are stratified on the surface. If the minor elements concentrate in a layer in contact with the substrate where they undergo oxidation and if this oxide film offers resistance to the diffusion of iron, chromium and nickel ions, then the lifetime of the heater element might be expected to increase. It is also possible that preferential reduction in the diffusion rates of the several ions may occur to such a degree that oxides may form in the body of the film and on the outer surface which are different from those that would normally form if the additional elements were not present. The use of transmisson electron diffraction may aid us in interpreting these phenomena. Up to the present time all of the factors which influence the lifetime of a given heater element are not definitely known. Among these are: (I) The rate of oxidation of the alloy. This may be dependent upon the composition and the physical state of the alloy. (2) The stability of the structure of the coating which forms. Transitions from one structure to another or solid phase reactions resulting in a change of composition may occur. The tendency of the film to adhere to the substrate when heated and cooled successively will be important. (3) The evaporation of various constituents from the alloy such as the removal of carbon by oxygen in a decarburization reaction. With these possibilities in view, an electron diffraction study of the oxides occurring on six different nickel-chromium alloys was undertaken with the hope that the results of this study could be correlated with oxidation rate studies as determined by means of the vacuum microbalance method1 and with

Jan 1, 1948

By H. I. Aaronson, H. A. Domian

ELectvon-probe analgsis has been used to in7:estigatr the partition ot alloying- elements between aus-tenite and proeutectoid ferrite (or the Jerritic component of bainite) in high-purity Fe-C-X alloys, lsuully at tzco levels of carbon content fca 0.1 and 0.4 pct in ntost steels) at temperatures between the M, and the Ae3 in Si, mn, Ni, mo, Co, Al, Cr, Cu, and PI steels. No partition ous found during the early stages of transformation at any temperature studied in the Si, ,mo. Co, Al, Cr, and Cu steels. Partition did take place, Jrowel'er, in Ihe Mn, ATi, and Pt steels, occurring in lewtperature. regions below the Ae3 of ca 130°, 65", UNDERSTANDING the mechanisms through which alloying elements influence the kinetics of austenite decomposition reactions which proceed by nucleation and 35c respectively. A break was discovered in the TTT curve for the initiation oj the proeutectoid ferrite reaction in the latter steels at the temperature at which partition began. The alloy content in ferrite at the a:y bondavy remained at constart lecels, shown experimentally to be significantly above those corresponding to eqiilib+iu??l, e'en at the longest reaction times investigated (ca 1o6sec). The partition and the TTT curve observations foere rationalized on the basis of the thermodynamic treatment developed in an accompany ing paper. and diffusional growth has been a major research objective of physical metallurgy since the latter part of the 19th century. The measurements made on the dif-fusivities of carbon and of substitutional alloying elements in austenite during the 1930's and 1940's seemed to provide a useful clue as to the nature of these mechanisms. These measurements showed that the diffu-sivity of carbon is several orders of magnitude higher than that of the alloying elements at a given tempera-

Jan 1, 1967

By A. L. Holmes

Significant technologic advances were made in open pit mining during 1973. The industry faced mounting problems on one front where expansion of stripping activities encountered enlarged public resistance and on another where manpower and materials were in short supply. These challenges, along with the challenge and opportunity to meet the increased demand for mining products including materials for energy production, placed a premium on technical developments and their application. The demands on technology also included the providing of facilities and methods to economically extract minerals from deposits of lower grade, lesser accessibility, and where other uses of land approached the value of its minerals. Detection of Failures in Slope Walls The Bureau of Mines has undertaken research directed towards providing a mine operator with the opportunity to take corrective action before a potential slide becomes a problem.

Jan 2, 1974

By AIME AIME

C. H. BENEDICT, chief metallurgist of the Calumet and Hecla Consolidated Copper Co., has pioneered for nearly half a century. Noted for his ammonia leaching process, lie has Iong been responsible for all Calumet and Hecla mill, concentrator, and reclaination plant flowsheets. His influence has spread far beyond his own organization. lie is dean of Lake Superior metallurgists and has contributed greatly toward raising his specialty-the country over-to an honored profession; not merely an honored profession but a profitable one for industry and the public. The leaching process which he developed in 1912 has, since 1915, produced for Calumet and Hecla 250,000 tons of copper from waste tailings at a cost per pound, in 1929, below five cents. It has yielded profits of $35,000,000. In the war just ended, this process proved the only one adaptable to the recovery of copper from gilding-metal¬clad steel strip, and Calumet and Hecla treated more than 50,000 tons of such scrap for the Government.

Jan 1, 1945

By Francis Lucas

ANY metal which contains even a small percentage of aluminum possesses certain peculiarities of appearance and properties which are exhibited both when the metal is melted and after it solidifies. Pure aluminum, or an alloy containing a small proportion of aluminum, can be melted without flux-except for a layer of charcoal-because a film of aluminum oxide and metal forms at the surface of melted aluminum. Although very thin, this film is air-proof, and it prevents the metal underneath from oxidizing. This oxidized film does not move easily on account of its toughness and high surface tension. One very important point in connection with this process of still casting has not been strongly enough stressed, namely, that the same kind of surface film with the same peculiarities forms over the surface of all melted alloys that contain even a small proportion of aluminum. Experienced foundrymen know how desirable it is to cast aluminum under its "skin" or-under the surface of the film which tends to remain still. In the case of red copper, when in fusion, the surface shows pure copper only. This is due to the fact that liquid copper constantly absorbs the copper oxide which forms on the surface. By closely examining melting copper the oxide can be seen dissolving in the bath, and going into solution just as pulverized sugar dissolves in water. When copper is cast in the open, either in wire bars or cakes, the surface of metal exposed to the air is covered by a film of black, oxide that cannot be absorbed by the metal.

Jan 1, 1927

By John D. Sullivan, Edwin J. Rogers, Chester R. Austin

THE problem of making a building unit combining the necessary physical and mechanical properties and good thermal insulation has been foremost in the minds of architects and ceramic and construction engineers for many years. This paper presents the results of studies on thermally expanding shales or clays to produce light-weight cellular products suitable for making building units. An expanded clay block suitable for building purposes should be large enough so that substantial savings may be effected in labor costs in laying the wall. The permeability should be low and it should have sufficiently good "dry-wall" characteristics to permit exposing the exterior surface to the elements, and to permit plastering directly the inside wall surface. The thermal conductivity should be low and the mechanical properties should be adequate. Obviously, a unit possessing satisfactory qualities for constructing an outside wall would be satisfactory for interior walls and for back-up purposes. The results of studies on bloating various shales or clays† and the properties of the expanded products are reported. In another paper1 basic factors involved in bloating of clays are discussed. Manufacturers of ceramic products, particularly structural clay, may encounter bloating of the ware during burning, and precautions must be followed to avoid this phenomenon. About 1927 the C. F. Burgess Laboratories, Madison, Wis., while carrying on an investigation for the American Face Brick Research Corporation, conceived the idea of intentionally bloating clay while holding it in a restrained condition, with the hope of producing a unitary cellular mass. Work was carried on until about 1931, when studies were terminated because of business conditions. These studies were continued later by The Western Brick Co., Danville, Ill., which developed a process of "inwardly expansive bloating." The major purpose of the latter investigation was to produce back-up tile to compete with concrete blocks made from Haydite or cinder aggregate. Haydite is a light-weight aggregate formed by heating certain clays or shales rapidly in a rotary kiln. While the investigations at the C. F. Burgess Laboratories or at Western Brick Co. were not carried far enough to lead to the commercial production of material for the construction of walls, particularly outside walls, they showed that certain clays could be thermally expanded and that it was possible to produce a material of low permeability with a large percentage of the total voids or cells closed. Commencing in 1939, the Ozark Chemical Co. sponsored a research program at Battelle Memorial Institute for the purpose of determining whether it is technically feasible to make thermally expanded building units, and specifically to get answers to the following questions:

Jan 1, 1942

By Thomas T., Read

ANY discussion of State-supported schools of mining and A metallurgy needs to be prefaced by a definition, since the first school to offer a mining curriculum, the Pennsylvania Polytechnic College, was established by a grant from the State. But, so far as can be determined, it received no further State support. It would be tiresome to go into precise details,. and it will be enough to stipulate that by State schools are meant those which derive their main financial support from regular appropriations made by a State legislature. The University of Michigan was the first of these to offer a mineral industry curriculum; its story, as well as those of Wisconsin and Illinois, has been related in the preceding chapter.* Arranging the others in chronological order involves making a decision as to what weight to attach to plans for giving instruction, as contrasted with its , effective initiation. This may appropriately be illustrated by the history of mineral industry education in California. California Among those who came to California in 1849 and the following years were many New Englanders who had a keen interest in education. Some of them, mostly Congregationalists and Presbyterians, sought to establish a school of higher education around San Francisco Bay and eventually succeeded in opening the "Scientific and Classical School at Contra Costa' in Oakland, at Broadway and 5th St., on June 20, 1853. This prospered so well that it was chartered by the State as the "College of California" on April, 13, 1855. Developing so rapidly that its quarters became cramped, in 1864 it not only bought a tract of

Jan 1, 1941

By K. D. Jacob

IN the decreasing order of the tonnages involved, the uses of phosphates can be grouped conveniently into three general classes, namely, fertilizer; chemicals for military, industrial, and technical purposes; and mineral feed for livestock. The quantity of phosphate used as fertilizer, principally in the form of superphosphate, has always exceeded by far that used for all other purposes, though in recent years a marked increase has occurred in its consumption for the other two general classes of uses. Prior to the present century large quantities of superphosphate, as well as a considerable portion of the production of phosphorus chemicals, score made from bone materials which were plentiful and cheap in some areas and which could be more easily processed than phosphate rock for the manufacture of chemicals. Today, however phosphate rock has almost completely displaced bone as a raw material for the manufacture of chemically processed phosphates in nearly all countries of the world.

Jan 1, 1944

By K. D. Jacob

MONTANA Phosphate Produucts Co., a subsidiary of The Consolidated Mining and Smelting Co. of Canada Ltd., operates three properties near Garrison, Mont., known as the Anderson, Graveley, and Luke mines. All three are underground operations, mining the same narrow bed at points several miles apart. The Anderson, the oldest and largest of the three, has produced about 700,000 long tons since 1929. The Graveley has produced slightly over 100,000 long tons since 1940, and the Luke, acquired in 1943, is still in an early stage of development. The great bulk of the output has been shipped to the Trail, B. C., plant of Consolidated Mining and Smelting Co. for use in the manufacture of fertilizers. The phosphate seam is the basal member of the Permian Phosphoria formation. In all three mines it has a uniform thickness of 3 to 4 ft. of oulitic phosphate, with a few shaly partings. The overlying part of the formation comprises about 50 ft. of chert and the immediate footwall consists of a few feet of shale and sandstone. underlain by the Quadrant quartzite.

Jan 1, 1944

By W. F., Dietrich

THIS paper deals with the- methods of mining the high-grade clays of California. Although the majority of the clay pits in the state are operated on a scale that is small by comparison with most metal mines, this very fact results in a diversity of methods and gives rise to problems of selection of the method best suited to given conditions. Two or three operators in California produce approximately 500 tons per day of a single kind of clay from a single pit. About five varieties of clay are mined on a scale of 200 to 400 tons per day; not over fifteen varieties are mined on a? scale of 50 to 200 tons per day; and more than 50 varieties are mined at a rate of less than 50 tons per day. It is the aim of this paper to delimit, insofar as the data at hand permit, the conditions and scale of operations that favor the selection of each dominant method of mining that is actually being applied at California properties. Details of the occurrence and utilization of the clays of California have been given in a recent bulletin and are not considered here.

Sep 1, 1928

By Richard W. Brummett, Robert L. Dubms

Located some 180 miles east of Los Angeles in Riverside County, California, the Eagle Mountain mine supplies iron ore concentrates for the Kaiser Steel Corporation steel plant in Fontana, California, and for export to Japan. Although the deposits were first discovered in the early 1890's, no production was realized from the area until 1948 when Kaiser Steel Corporation commenced operations. A part of the large Basin and Range province, the Eagle Mountain area's geologic column comprises a thick series of metasediments resting on Precambrian gneisses and schists that have been intruded by sill-like masses of porphyritic quartz monzonite. The metasediments are composed of three quartzite units that are separated by a schistose meta-arkose and by two ore zones. They have been folded into a large east-west trending anticlinal structure that extends completely across the Eagle Mountains. The iron ore deposits occur in two well-defined horizons in the metasedimentary series, and they are found only along the north limb of the major anticline. Host rocks for the ore zones were a series of limestones and dolomites with associated quartzites. Magnetite plus pyrite comprised the primary mineralization that formed many replacement lenses and stringers of ore within the ore zones. The primary ore has been oxidized to hematite and goethite in a broad zone at higher elevations in the deposits. Hydrothermal alteration formed actinolite- tremolite granofels, local phlogopite, and minor tourmaline in the ore zones. This alteration and the ore deposition seem related to the same magmatic event that formed the porphyritic quartz monzonite intrusion

Jan 1, 1968

By Wayne A. Greenwalt

A method that determines venture participation when the decision maker's level of risk aversion varies according to venture profitability and risk investment is presented. The decision maker's fundamental aversion to risk is established by the selection of a desired working interest for a venture that anticipates only a discounted payout.

Jan 1, 1982

By Nathan C. Rockwood

LIME is a very general term applied to products of limestone, in popular treatises often incorrectly, including ground or pulverized limestone used in agriculture. When used without qualifying adjective, the term usually means burned or calcined limestone, or quicklime, or calcia. The corresponding calcined product of magnesite is magnesia. If the calcined rock is relatively pure calcium carbonate, the resulting lime is a "high-calcium" lime; if the rock is dolomite, or a combination of calcium and magnesium carbonates, the lime is a "dolomitic" or a "high- magnesium" lime. There are various grades in between, depending on the percentage of magnesium carbonate and other ingredients in the raw rock. For some industrial purposes only high-calcium limes are suitable; in other processing-as, for example, neutralizing acid wastes -the relative percentages of magnesium and calcium carbonates in the raw material are not important. Limestone is burned (roasted or calcined) in furnaces known as lime kilns by direct exposure to the hot gases and flames. When heated to incandescence, the carbon dioxide content of the rock is expelled, leaving calcium and magnesium oxides, according to the formula usually written: [ ] This thermal reaction is reversible, which requires that the lime be withdrawn from the "calcining zone" of the kiln about as fast as made. Pure calcium carbonate would lose 44 pct of its weight in the calcining process; dolomite, 48 pct. Generally, the lime will retain the approximate size and shape of the piece of rock from which it is made but some few limestones tend to break down into granules or dust. Hence lime (quicklime) comes from the kilns in lumps or granules and normally is packed in water- tight containers in these forms, or is pulverized after calcination.

Jan 1, 1949

By AIME AIME

AN unusually interesting meeting devoted to the discussion of the ways and means of improving coal mining practice, through the larger use of machinery underground, was held in the Auditorium of the Engineering Societies Building on March 11. The meeting was organized by the Materials Handling Division of the A. S. M. E. and held under the auspices of the Metropolitan Section of that Society and the National Coal Association. The New York Section of the A. I. M. E., which had been invited to participate, found itself unable to do so formally because of a conflicting date for its March meeting but informally did its part to aasure the success of the meeting. As a result of the discussion at and preceding the meeting, the National Coal Association, through Walter Barnum, chairman of its research committee, has asked the A. S. M. E. and A. I. M. E. to join the Association in a study of the present problems of the bituminous coal industry. Messrs. Harry L. Gandy, Calvin W. Rice and H. Foster Bain have been selected to act as a committee which shall develop plans for a joint program.

Jan 1, 1926

By S. Senderoff, D. E. Couch

A PROCESS for the electrolytic preparation of molybdenum from molten salts has been described previously. This previous work centered on electrowinning and electroplating characteristics of the process. In this paper the properties of the process as a refining medium are discussed. In producing metals from ores, it frequently has proven most economical to obtain a comparatively impure metal by smelting, and to purify the product by electro refining. Direct electrowinning from molten salts is rather difficult when a porous diaphragm is required in the process, as in the case of molybdenum, since satisfactory refractory materials for such a diaphragm in molten salts have not yet been developed. In electrorefining, however, a soluble anode is used. By suitable control of anode and cathode current densities, the lower-valent molybdenum compound used in the electrolyte is not oxidized, and a diaphragm is not needed, thus avoiding difficulties which are encountered with other electrowinning processes. Electrorefining may result from two different processes in the cell: Dissolution of the molybdenum and the less noble impurities with a separation of the more noble impurities as an anode sludge; the electrodeposition of molybdenum and the more noble metals at the cathode, leaving the less noble metals in the electrolyte. The amount of separation which occurs in each process is determined by the potential of the operating electrode and the relative concentration of the various species at (or in) that electrode. Since molybdenum has a comparatively noble position in the EMF series in molten alkali halides,2 most refining would be expected to occur at the cathode. In this work only the cathodic process was studied. The objective was to determine to what extent various metallic ions, if they dissolve from the anode or are otherwise introduced, were concentrated in the electrolyte. The necessary conditions for the separation of each and the limiting concentration which may be tolerated in the electrolyte for effective refining were studied. The deposits were chipped from the cathode and analyzed spectrochemically for metallic impurities. Besides determining the major contaminant, a general qualitative analysis was obtained to be sure that other metallic ions were kept at a very low level during each series of runs and to be sure that the baths were not being contaminated accidentally. Samples of the bath, for analysis, were taken at the temperature of operation so there was no chance of selective crystallization during cooling. In this way the ratio of molybdenum in the bath to the other metal could be determined readily. These data permitted a check on the anode efficiency and any volatilization that took place during the electrolysis. Experimental Apparatus—The apparatus as shown in Fig. 1 was used to determine the effect of the various foreign ions upon electrodeposited molybdenum. The entry chamber A allowed the cathodes to be removed without cooling the bath and without allowing oxygen or moisture to enter." The cathodes were made Prom 0.25-in. tungsten rods and were rotated during the electrolysis. The balloon in the lower arm B was inflated with helium after the cathode was drawn up into the upper section for removal. A new cathode was then placed into the entrance chamber A after which the chamber was flushed

Jan 1, 1959