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By James R. Cudworth

ENGINEERING has been taught at the University of Alabama for over a hundred years. The School of Mining and Metallurgy was authorized by the Board of Trustees in 1887 and four students were graduated in 1888. In 1919 the legislature directed that all mineral industry instruction in the state should be centralized at the University and designated the department of mining of the College of Engineering as the Alabama School of Mines and made financial provisions for carrying on both instructional and research work for the benefit of the mining industry of the state and for cooperation with the U. S. Bureau of Mines, which had established its Southern Experiment Station on the campus.

Jan 12, 1950

By S. Leber

Pole figures and pole distributions were used for the quantitative detevinination of the preferred orientations in swaged tungsten rods and the effect of subsequent wire drawing on the texture. In the swaged rod, the preferred orientation could best be described as a pseudo (111-112) [110] cylindrical texture. A secondary component was assigned the indices (110) [001]. Further reduction by swaging retained these cylindrical textures. Wire drawing caused lattice rotations about the wire axis, converting the cylindrical texture into a normal fiber texture. The conversion was initiated and proceeded lnost rapidly in the center of the wire. The (110) /001] component was converted into a (110) fiber texture by wire drawing. The effective rotations were about axes contained in the lransverse plane. The preferred orientation associated with tungsten wire usually has been assumed to consist of a (110) fiber texture. This implies rotational randomness around the wire axis. Leber1 has shown that rotation about the wire axis may be restricted resulting in a preferred orientation designated as a cylindrical texture. Specific crystal planes tended to remain aligned parallel to the wire surface. This texture seemed to be the result of the swaging operation used in the intermediate stages of fabrication. Bhandary and cullity2 detected similar textures in swaged iron wires. Peck and Thomas3 suggested that the preferential alignment of crystal planes parallel to the wire surface was the result of tangential flow, characteristic of swaging. Wire drawing, following swaging, twisted the crystals about axes parallel to the wire axis, converting the cylindrical texture into a normal fiber texture.4 In this investigation, quantitative techniques were used to more accurately characterize the cylindrical texture and to study its conversion into a normal fiber texture. PROCEDURE The material investigated was lamp-quality tungsten. Three ingots were rod-rolled and swaged to 112 mils diameter, and were then drawn to 10-mil wire. Samples were obtained after each drawing pass. (110) and (200) pole figures were obtained from samples prepared as shown in Fig. 1. To form the sample shown in Fig. l(a), l-in. lengths of wire were glued side by side to form a l-in. square. The composite was ground and electropolished to form a diametral reference surface. For certain specific tests, samples were prepared as shown in Fig. l(b). This composite was made from 10-mil-thick strips prepared by grinding on parallel longitudinal planes. The polished reference surface in this case was, in essence, the wire surface. The two forms of samples [~igs. l(a) and l(b)] were related by a 90-deg rotation around the wire axis. Because of ease in preparation, most data was obtained from the diametral samples. The X-ray data were obtained using a Siemen's pole-figure goniometer. These data were not corrected for absorption or defocusing effects, since only the angular locations of the intensity maxima were of interest. Regions of the pole figure more than 80 deg from the center were not investigated. Partial monochromatization was achieved by the use of unfiltered copper radiation and a krypton-filled proportional counter. No evidence of spurious white radiation effects5 could be detected. Therefore, more elaborate X-ray techniques were not required. Intensity levels were chosen to show all pertinent details of the orientation distributions. The reference plane for the pole figures was the diametral section. The orthogonal reference directions, shown in Fig. 1, were the wire axis, the radial axis per-

Jan 1, 1965

By John Chipman

Published data on the equilibria of carbon in binary Fe-C austenite with H2-CH4 and CO2-CO gas mixtures are used to obtain the constants of an equation repre -senting the activity coefficient of carbon throughout the stable austenite range of temperatutre mid compositiotl. Calculated values for the solubility of graphite are found to be in agreement with the best-published direct observations. Its heat of solution is 10,680 calper g-atom. The free energy of formation of cementite is culculated from the equilibrium compositions of austenite and of gas. Its entropy and heat of formation are also obtained. BASIC knowledge of the high-temperature properties and treatment of steels is contained in the Fe-C diagram and its extensions for the effects of alloying elements. The application of thermodynamics to the Fe-C system, with addition of alloying elements, can serve to simplify and systematize this knowledge. The points of beginning are the binary fee solution, austenite, concerning which our information is reasonably complete, and the binary carbide, cementite. Further studies must include the other phases of the binary system, a and liquid, and for these an accurate knowledge of the ? phase boundaries is essential. These studies should provide a firm base for systematic study of the effects of alloying elements on all phases of the system, their transformations, and precipitation phenomena. With the aid of the simplifying thermodynamic concepts of activity coefficients and interaction parameters it is to be hoped that the results of these studies will be amenable to computer solution thus making the information on multicomponent systems more readily available than would be possible in multidimensional diagrams. Studies of the thermodynamic properties of austenite have utilized equilibrium measurements on the reactions:

Jan 1, 1968

Jan 1, 1910

CLARENCE N. FENNER.-Mr. Gelstharp, chief chemist of the Pitts-burgh Plate Glass Co., has directed my attention to the fact that that company was using optical pyrometers obtained from the Leeds & Northrup Co. several months before the members of the Geophysical Laboratory arrived at Charleroi. I am glad to make this correction. The chief object of my paper was to emphasize the necessity of careful temperature control in the making of optical glass and to describe the kind of tests to which an optical pyrometer should be subjected at a glass plant in order to obtain information regarding the closeness with which its readings correspond with true temperatures under the condi-tions which prevail in each particular case.

Jan 12, 1919

The following members were appointed on the Committee Advisory to the U. S. Bureau of Standards: Arthur S. Dwight (Lead). John Fairfield Thompson (Nickel). The reports of the Committee in charge of the Arizona Meeting and the Committee on Transportation to the Arizona Meeting were accepted with the thanks of the Board. The By-Laws of the Nevada Section of the Institute were approved. The subscription price of the Bulletin to non-members of the Institute was increased to $12, per year beginning with January, 1917. This increase does not affect the reduced price of $5 on extra copies of the Bulletin which are sold to members, libraries and sister societies.

Jan 7, 1916

By V. H. Wilhelm

The outstanding event in the California petroleum industry during 1931 was the continuance of curtailment of crude oil production, which directly reduced drilling and well repair activities. Although all objectives were not attained, a very close balance between supply and demand was maintained during the period of maximum requirements, but the decline in intercoastal and export shipments caused an overproduction during the last half of the year, which indicated that California production would necessarily suffer further curtailment after the end of the year. A new peak in potential crude oil production of 1,187,600 bbl. per day was reported in August and at the close of the year the California potential was 1,069,000 bbl. per day, the shut-in light oil amounting to practically 425,000 bbl. per day and the shut-in heavy oil amounting to about 150,000 bbl. per day. Fig. 1 depicts these conditions and also shows the production and curtailment situation since the inception of proration in California. The December, 1931, potential figure of 1,069,-000 bbl. per day was arrived at after the most careful deliberation by a number of committees, selected to check the potential of practically every well in the state. Continued overproduction in the first three months of 1931 and the inadvisability of building more storage, together with the inability to obtain the proper amount of curtailment in town-lot fields, such as Long Beach, Santa Fe Springs and Playa del Rey, prompted the major oil companies to inaugurate a price reduction in crude oil. This cut caused prices to reach the lowest levels since 1915, and instigated the formation of an oil sales agency, composed of independent operators, which is known as the Oil Producers Sales Agency. The purpose of this organization is to procure a market for its members at reasonable prices, advise them of market conditions and aid them in controlling the amount of oil available for sale. Marketing of oil produced by members began on June 1 and independents controlling" about 160,000 bbl. per day of production had become members by the end of the month.

Jan 1, 1932

Elected Died 1895 ABBOTT, AI ATTHUR 1908 1882 ABBOTT, ARTHUR V 1906 1905 ABE, MASAYOSHI 1909 1903 ADAMS, CHARLES C. 1905 1903 ADAMS, HARRY C 1917 1906 ADAMS, JOHN C. 1913 1917 ADAMS, LLOYD D. 1918 1905 ADAMS, WILLAMS 1909 1903 ADAMS, W. EDWARDS 1910 1884 ADDY, MATTHEW 1896 1906 AFFLECK, WILLIAM A. 1911 1889 AKERS, WILLIAMS A. 1906 1905 ALABASTER, RUPPERT C. 1911 1899 ALBERGER, LOUIS R. 1911 1895 ALLAN, THOMAS A. 1894 ALLEN R B 1896 1905 ALLEN, R. SCOTT 1906 1886 ALLISON, ROBERT 1916 1874 AMIOT, H. 1892 1886 AMSLER, CARL 1894 1898 ANDRSON, JOHN W 1905 1895 ÅNGSTROM, CARL 1901 1887 ARCHBALD, JAMES 1910 1900 ARLETT, GEORGE H 1906 1895 ARMSTRONG, JOHN F 1898 1905 ARNOLDS, LEO F. 1917 1882 ARNOLDS, HUGO 1886 1875 ASHBURNER, CHARLES A 1889 1872 ASIIBURNER, WILLIAM 1887 1883 ATKINS, C M , JR 1885 1875 ATTWOOD, GEORGE 1912

Jan 1, 1923

By H. R. Banks

The Sullivan concentrator has completed 20 years of operation. During this period a considerable amount of data has been accumulated concerning the characteristics of several types of flotation machines in their application to the problem of the differential separation of the lead sulphide, zinc sulphide and, in more recent times, iron sulphide, in the ore from the Sullivan mine. It is the author's intention to sketch briefly experiences encountered when the several types of flotation machines were introduced into the flow. Original Flotation Equipment and Ore The original flotation equipment consisted of four 18-cell lead-roughing machines, whose concentrate was cleaned in an 8-cell and recleaned in a similar 8-cell machine. Zinc concentration was carried out in four 18-cell machines. One 8-cell zinc re-treatment machine received the reground zinc middling. The 168 cells handled some 3000 tons of original daily feed. These cells were of the standard Minerals Separation type, equipped with 24-in. impellers. Spindles were driven through geared line shaft at a speed of 255 r.P.m. The impellers were the 45' type, except for the last three cells of the zinc-rougher machines, which were of sub-aeration type, with full bottom shroud and half shroud for the top side of the impellers. Four-pound air was introduced. This recognition of the benefit of intensified flotation operation for "gleaning" was an important phase in the early operation and will be discussed further on in this paper. Sullivan ore during this period is described as a finely disseminated mixture of four sulphides, totaling go per cent made up of 13.6 per cent galena, 14.4 per cent mar-matite, I per cent pyrite and 61 per cent pyrrhotite. The specific gravity of the ore was approximately 4.4. There has been a gradual change in the ore content. The 10 per cent of nonsulphide constituents has increased to between IS and 20 per cent and all three sulphides have dropped somewhat. Added equipment and changing technique have made possible the treatment of 8000 tons per day of mill feed instead of the 3000 originally handled. Special Features of Flotation at Sullivan Sullivan flotation differs greatly from customary practice. The very heavy return of lead rougher middling and lead cleaner tailing, totaling at times 125 per cent of the new feed tonnage, has been the subject of much investigation. The practice is still employed. This operating condition is mentioned because it is the author's belief that the in-

Jan 1, 1947

By H. R. Banks

The Sullivan concentrator has completed 20 years of operation. During this period a considerable amount of data has been accumulated concerning the characteristics of several types of flotation machines in their application to the problem of the differential separation of the lead sulphide, zinc sulphide and, in more recent times, iron sulphide, in the ore from the Sullivan mine. It is the author's intention to sketch briefly experiences encountered when the several types of flotation machines were introduced into the flow. Original Flotation Equipment and Ore The original flotation equipment consisted of four 18-cell lead-roughing machines, whose concentrate was cleaned in an 8-cell and recleaned in a similar 8-cell machine. Zinc concentration was carried out in four 18-cell machines. One 8-cell zinc re-treatment machine received the reground zinc middling. The 168 cells handled some 3000 tons of original daily feed. These cells were of the standard Minerals Separation type, equipped with 24-in. impellers. Spindles were driven through geared line shaft at a speed of 255 r.P.m. The impellers were the 45' type, except for the last three cells of the zinc-rougher machines, which were of sub-aeration type, with full bottom shroud and half shroud for the top side of the impellers. Four-pound air was introduced. This recognition of the benefit of intensified flotation operation for "gleaning" was an important phase in the early operation and will be discussed further on in this paper. Sullivan ore during this period is described as a finely disseminated mixture of four sulphides, totaling go per cent made up of 13.6 per cent galena, 14.4 per cent mar-matite, I per cent pyrite and 61 per cent pyrrhotite. The specific gravity of the ore was approximately 4.4. There has been a gradual change in the ore content. The 10 per cent of nonsulphide constituents has increased to between IS and 20 per cent and all three sulphides have dropped somewhat. Added equipment and changing technique have made possible the treatment of 8000 tons per day of mill feed instead of the 3000 originally handled. Special Features of Flotation at Sullivan Sullivan flotation differs greatly from customary practice. The very heavy return of lead rougher middling and lead cleaner tailing, totaling at times 125 per cent of the new feed tonnage, has been the subject of much investigation. The practice is still employed. This operating condition is mentioned because it is the author's belief that the in-

Jan 1, 1947

NEW MEMBERS The following list comprises the names of those persons who became members during the period Aug. 10. 1918, to Sept. 10, 1918. BATCHELOR,. HARRY D., Laboratory Director, National Carbon Co., Inc., Cleveland, Ohio. BROWNING, C. P., Gen'I Supt., Britannia Min. & Smelt. Co., Ltd., Britannia Beach, B. C., Canada. COMSTOCK, GEORGE F., Met., Chg. of Physical Test Laboratory, Titanium Alloy Mfg. Co., Niagara Falls, N. Y. CONCKLIN, BERT M Chief Engr., Arthur lron Mill. Co., Hibbing, Minn. COWAN, W. A., Asst. Chief Chem., National Lead Co., 129 York St., Brooklyn, N. Y. DAVIDSON, PHILIP Met., Scovill Mfg. Co., Waterbury, Conn. DAVIS, Louis L., Mgr. & Treas., Commonwealth Min. Co., 911 Foster Bldg., Denver, Colo. DAY, P. W Chem. Engr., Western Cartridge Co., 207 E. 12th St., Alton, Ill. DECKER, HAROLD DEBIT, Co. A, 27th Engineers, A. P. 0. 714, A. E. F., Care Postmaster, N. Y.

Jan 10, 1918

By H. Landsberg

IN a previous report1 it was pointed out that a successful attack on roof troubles has to be preceded by extensive scouting. As Lord Kelvin once said, scientific progress can be made only if accurate data are available: "unless you measure, you do not know.? THE CONVERGENCE RECORDER For the observation of roof movements in mines the convergence recorder has shown that it will enable us to get some of the necessary information. Results with convergence recorders were first published by Winstanley and other English investigators for rapidly moving longwall faces. In their investigations the speed of work and the heavy over-burden produced a considerable amount of absolute values of convergence in a short time. Under the conditions frequently encountered in our investigations in Central Pennsylvania, under shallow, overburden and in mines with slowly proceeding extraction, the movements observed were much less in absolute value, for an equal interval of time. This was partly because the mines in which our studies were carried on frequently had idle days, sometimes four or five in succession. Therefore continuous records were not employed and a simple convergence gauge was built. In its first models, it consisted only of two telescoping tubes pressed against roof and floor by a coil spring. At the side of the lower tube a rule divided into 1/-mm. divisions was fixed and a knife-edge, which was attached to the upper tube, was slid over the scale in case of convergence between roof and floor. While the larger motions could be read on this device, it seemed to be desirable to increase the accuracy by inserting between the two tubes a dial meter reading in 1/1000 in. Such a gauge was first built in April 1937 and installed for experimental purposes in a bituminous coal mine in Pennsylvania (Fig. 1). It was read at least once daily, 24 hr. apart, and if feasible at shorter intervals. After several months of experience it can be said that this type of gauge answers the scientific as well as the practical needs. It is easier to handle than the recorder; no clock is used, there are no pen troubles. The price of

Jan 1, 1938

By George R. Mansfield

INTEREST in the reserves of phosphate rock in the United States and their proper conservation has recently been aroused by hearings held in different parts of the country by the "Joint Committee to investigate the adequacy and use of phosphate resources of the United States." This committee was appointed within a few days after a Presidential message to Congress on the same subject, dated May 20, 1938, and began to function almost immediately. Hearings were held in Washington, D. C., Pocatello, Ida., Wilson Dam, Ala., Knoxville, Tenn., and Lakeland, Fla. The resulting testimony, when published, comprised a volume of 1182 pages.1 At the earlier hearings held in Washington and Idaho the seeming disparity between the great reserves of the West and the smaller reserves in the East led to some suggestions as to the desirability of curtailing or even prohibiting the exportation of phosphate rock so that eastern producers, becoming alarmed, cooperated in making available for the use of the committee information hitherto closely guarded. This information has provided an opportunity for new studies by official agencies, for a restatement of the reserves of Florida and Tennessee, and for some modification of figures for the Western States. The writer, representing the Federal Geological Survey, was given free access to the Florida material and has prepared for publication a report,2 some features of which are summarized in this paper. The Tennessee material was studied by Dr. G. I. Whitlatch,3 of the Tennessee Division of Geology. Prof. J. Stewart Williams,4 of the Utah State Agricultural College at Logan, has published a recent study of the phosphate resources of Utah and the writer has given some further study to reserves of western phosphate from the viewpoint of including material of lower grade than that hitherto considered. Technologic advances in the phosphate industry must be credited with a large share in the expansion of reserves by making available for

Jan 1, 1940

The Free World's largest uranium reserves are in the United States. Almost 97% of the U.S. uranium reserves occur in irregular shaped sandstone formations, widely disseminated in coarse clastic sediments that are mostly of Jurassic or Tertiary age. Without doubt, the most important deposits are located in the sandstone formations of the Ambrosia Lake district of New Mexico, near the sun-scorched town of Grantswhose proud alias, as given by the city fathers, is "The Uranium Capital of the World."

Jan 8, 1974

Discussion Of the paper Of GEORGE K. BURGESS, J. J. CROWE, H. S. RAWDON, and R. G. WALTENBERG, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin NO. 93, September, 1914, pp. 2433 to 2437. ALBERT SAUVEUR, Cambridge, Mass.-The Bureau of Standards has once more rendered a public service. Manufacturers and consumers of steel rails alike should welcome the important results now laid before them by Dr. Burgess and his co-workers. Personally I welcome these results all the more that in the past, as some of the members may remember, I have never failed, when occasion arose, to call the attention of rail manufacturers to the importance of controlling the finishing temperature of their rails. The pioneer metallographic work conducted at the South Works of the Illinois Steel Co. in the early '90s clearly brought out the close relations existing between the manufacture, properties, and finishing temperature of steel rails and I think I may say without fear of being contradicted that the results of this early investigation had considerable influence in drawing the attention of manufacturers to the importance of finishing temperature and of heat treatment in general. The results now before us should be, it seems to me, of great value to rail manufacturers in their efforts to produce a better and, above all, a safer rail. It seems to be demonstrated in this paper that there is no difficulty in installing in rail mills pyrometric outfits, making it possible to record, without interfering in the mill operations, the temperature of the rails as they leave the finishing rolls, or of the ingots as they are withdrawn from the soaking pits, or at any intermediate point in the process of manufacture. The inference necessarily follows that manufacturers should see to it that such pyrometric installations are made, in order that they may actually know, instead of guessing at, the temperature of their rails;, and, for obvious reasons, rail consumers should insist upon such installations. In the rolling of heavy sections especially should care be taken to lower their finishing temperature, seeing that the present tendency is to finish them at higher temperature, whereas, owing to the slower cooling of their central portions, which makes for coarseness of grain, they should, if anything, be finished at a lower temperature than lighter rails.

Jan 4, 1915

Jan 1, 1912

Jan 1, 1909

By S. E. Clay

In the chemical reaction control regime employed in the laboratory dissolution experiments, calcined trona ore dissolves in aqueous solutions according to a first order, irreversible reaction rate. The study showed that the reaction is first order with respect to solution NagCO3 concentration. The activation energy was determined to be 20.233 kJ/g. mol with a rate constant equal to 1235 mm/s (2917 in. per min). The dissolving particle may be described by shrinking particle behavior.

Jan 1, 1986

By K. E. Manchester, A. H. Clark

Hall measurements have been made on three groups of silicon samples, which were implanted with boron, aluininunz, and phosphorus ions. Boron and phosphorus implants show essentially bulk properties when annealed under previously determined conditions, i.e., 15 min at 80O°C for boron and 10 mirz at 600°C for phosphorus. Bulk properties were also observed in alu?rrilzum-implanted samples when ion concentrations were below 1015 cm-'; however, strange low- terrzperalure behavior and a falloff in cavrier concenlralion was observed for sarnples with ion concenlration abozle loL5 ern-'. This can be attributed to solid-solubility effects since the average bulk concentration f0.r the sample exhibiting bulk properties was below the reported solubility limit for aluminum, while the other samples were above the limit. A detailed study of the annealirzg process indicates that mobilities reach bulk c~alues in phosphorus implants at 250DC, in alutninurn ivnplanls a1 500°C, and in boron implants at 700°C. A simple rnodel has been proposed to fit the annealing data. THE technique of semiconductor doping by direct injection of energetic ions is being actively investigated at this Center. Previously published results from this laboratory have been concerned with the investigation of implanted profiles in silicon and the electrical properties of the resultant p-n structures.1'2 Diode properties have been reported for junctions produced by implantation of boron ions and aluminum ions in n-type silicon and phosphorus ions in p-type silicon. Reverse current characteristics, as well as electron diffraction data, have indicated that the damage to the structure produced by the energetic ions during the stopping process can be minimized by a gentle anneal. The time-temperature conditions for this process have been determined by sheet resistivity studies.3 Electrical profiles of implanted phosphorus ions which have been determined by a differential sheet conductivity technique are based on the assumption that the carrier mobilities and activation energies for ionization are the same as in bulk silicon. These assumptions have been substantiated experimentally by measurement of Hall constants and resistivities of these implanted structures and the results are presented herein. After establishing the bulk property equivalence of the annealed layers, a more detailed examination of the annealing process was undertaken. The sheet resistivity technique initially used to determine anneal conditions has been broadened to include Hall constants and mobility behavior with anneal conditions. PROCEDURE The three groups of samples prepared for Hall measurements were implanted with mass-separated beams of boron, aluminum, and phosphorus ions. Ion concentrations are equivalent surface concentration and they have been determined from beam current measurements during implantation. Implant conditions for the samples are shown in Table I. In all cases, the samples had previously been angle-lapped on one edge and the junction delineated with an HF-copper sulfate solution. The surfaces of the implanted regions of the samples were exposed to the delineating solution and in the case of the "n"-type phosphorus-implanted areas it was later discovered that a finite amount of surface could be etched by this solution. This is discussed in the section on results. The implanted samples were ultrasonically cut into the conventional six-probe configuration shown in Fig. l.* In the annealing studies, for which the meas- urements were taken at room temperature, the sample holder was a Bakelite jig incorporating tungsten mechanical probes. The other measurements were taken using a conventional liquid-nitrogen cryostat, in which the temperature could be varied from 77" to about 400°K. For these measurements, 10-mil aluminum dots were evaporated onto the samples and alloyed with the silicon at 530°C for 15 min. The samples were then mounted in flat-packs, and gold wires were bonded to the aluminum dots. The electrical measurements were made with either a Leeds & Northrup K-5 Potentiometer, a Keithley 147 Nanovolt Null Detector, or a Keithley 601 Electrometer. No external bias was applied to the substrate. There is an inherent self-biasing arrangement at one or the other of the current contacts (depending upon the polarity), and this suffices to limit the current flow to the implanted layer. The magnetic field was generated by an A. D. Little electromagnet. Except for occasional checks of linearity of the Hall voltage with

Jan 1, 1969

By W. G. Pfann

A simple method of obtaining multistage batch separations by crystallization was described recently. Known as zone-refining, it comprises passing short molten zones through a long solid charge. This technique can now be used on a continuous basis by means of the zone-void method described in this paper. Feed enters, at an intermediate point, a column down which molten zones travel, and waste and product leave at the ends. Materials move in the column through the agency of voids, which are introduced at the ends and travel toward the feed inlet. The voids and molten zones are moved by external heaters in a simple manner, and the principle of reflux is utilized. ANEW method of obtaining multistage separations by crystallization was described recently.' Named zone-refinina.,-, the method comwrises slowly passing a series of molten zones through a long solid charge. Solute becomes concentrated at one or the other end of the charge, depending on whether it raises or lowers the freezing point of the solvent. The separation increases with the number, P, of zone-passes, approaching a limit as P approaches infinity. Zone-refining has been highly effective in purifying germanium and other substances.2,3 and new applications are steadily increasing. Zone-refining is a batch method and as such it has certain limitations inherent in batch operation. If it could be made continuous, its scope and utility would be greatly broadened. This end has been achieved by the zone-void method described in this paper. In the zone-void method feed is introduced continuously at an intermediate point in a column down which molten zones travel, while impure waste and purified product leave at the ends. Both the flows of feed, waste and product, and also the travels of the zones, are actuated by external moving heaters in a simple manner; and the system utilizes the principle of reflux. The method provides, in the field of crystallization, the counterpart of the continuous fractiona-tion column in the field of distillation. The following will be discussed: apparatus and mode of operation, fundamental nature of the separation, design theory, and practical considerations. The method will be described in terms of a binary solute-solvent system in which the solute is an impurity to be removed and the solvent is the desired product. The distribution coefficient, k, defined as the ratio of solute concentration in the solid freezing out of a molten zone to that in the liquid in the zone, is assumed to be constant and less than one. The process is equally effective for k's greater than one and for ternary or higher order systems. Method and Apparatus The essential features of a continuous zone-refining process are represented in highly generalized form in Fig. 1. A series of molten zones, produced by moving heaters, travels slowly down the column or charge (to the left in Fig. 1). If there were no flows of feed, waste, or product, the process would simply be batch zone-refining, the action of the molten zones being to sweep solute down the column, solvent up the column. For the process to be con- tinuous, with stripping and enriching sections in the column, feed must enter, and waste and product must leave, as indicated. The zone-void process accomplishes both objectives, namely, the indicated movements of zones and the indicated flows of material. Zones are moved by moving heaters, just as in batch zone-refining. Materials are made to flow by creating voids at the waste and product exits and causing these voids to move to the feed inlet. Since there must be a net flow of material from the feed inlet to each of the outlets, the indicated movements of voids are in the desired directions, because movement of a void in a given direction corresponds to flow of material in an opposite direction. In order to produce the desired movements of voids, the column is folded into two vertical sections having the feed inlet in common at their upper ends. Voids are displaced upward by the liquids in the molten zones and their travel is actuated by the motions of the zones. Voids travel with the zones in the enriching section and move continuously. Voids travel opposite to the zones in the stripping section and move intermittently. Creation and travel of voids will now be examined in detail. The enriching section of a column in operation, with its void generator, is shown in Fig. 2. The column section is a vertical tube around which a series of closely fitting, regularly spaced heaters travel slowly upward. Each heater produces a molten region, the temperatures of the heaters and the cooling between heaters being controlled so as to maintain the molten zones approximately constant in size. A void is normally present atop the molten zone in each heater. As the heater rises, it continuously melts solid above it, which drips through the void into the molten zone and continuously freezes out solid below it, of concentration k times that of the liquid in the zone. When a molten zone and void reach the feed inlet, which is kept molten, the void is displaced by an equal volume of feed liquid. Generation of voids of controlled size in the enriching section is shown in Fig. 3. The void generator is a tube of small cross-section, provided with lateral heat-conducting fins which sense the position of the heater. Liquid can escape only when the entire outlet tube is within the heater. If any part of the outlet tube is outside the heater, liquid cannot escape,

Jan 1, 1956