Search Documents

By Appendix by A. S. Goldoni, R. E. Tate, E. M. Cramer

The diffision coefficient for self-diffision of plutonium in the temperature range 350" to 440°C has been measured by using puZ3 as the tracer isotope. Autoradiopaphic techniques were used to inzlestigate the possibility of grain boundary diffusion, hut only evidence for volume diffusion was found. The least-squares fit of the data gives the .following equation for the diffision coefficient: The computer least-squares technique for fitting the nonlinear equations is outlined. DETERMINATION of the self-diffusion coefficient of the fcc 6 phase of plutonium is in principle a straightforward experimental task. However, the chemical reactivity, the intense @ activity, and the toxicity of plutonium put limitations on the experimental techniques. The technique selected included roll bonding for preparation of the diffusion couples and pulse-height analysis of the @-particle activity to determine the distribution of the PU tracer in the diffusion couples. EXPERIMENTAL PROCEDURE Couple Preparation. Cylinders about 0.5 in. in diam were cast from two special stocks of plutonium, one of which had been enriched in puZ3', as shown in the isotopic analyses listed in Table I. For each roll-bonded composite sheet, a cylinder 0.437 in. in diam and 0.190 in. thick was turned from each kind of plutonium on a lathe in a 98 pct He atmosphere. The two freshly machined cylinders were positioned face to face in a tube of commercially pure aluminum which had been sealed at one end by welding and the assembly was evacuated on a vacuum manifold overnight. The elapsed time between machining the faces of the plutonium cylinders and evacuating the loaded tube was about 15 min. After overnight evacuation of the assembly the indicated vacuum was 1 X 10"5 torr or better. The aluminum tube was then warmed and pinched off with a cold-welding tool. The pinched-off weld was also fusion-welded as an additional precaution against leakage of air into the evacuated assembly. The assembly was immediately heated for 30 min in a 250°C furnace and reduced in thickness by being passed through a rolling mill with rolls heated to 200°C. The rolling schedule (four passes of 100 mils each with a 10-min reheat after two passes) reduced the thickness of the assembly to 100 mils. The rolled assembly was allowed to cool normally in air. The rolled assembly was sheared at the edges and the aluminum peeled from the composite plutonium sheet. The elliptical sheet was about 0.060 in. thick and usually three 0.383-in.-diam disks could be punched from its central portion. The sheet was heated on a hot plate to the ductile low 0 range (140°C as measured by temperature-indicating pellets) before each disk was quickly punched. The quality of the bond in the disks was evaluated by metallographic examination of the scrap sheet adjoining the hole left by the punch. Only well-bonded specimens without oxide in the interface (as indicated by metallography) were considered satisfactory for further use. More than half of the specimens so examined contained sufficient oxide in the interface to be rejected. Diffusion Anneal. Each disk to be diffusion-annealed was wrapped in 1-mil-thick tantalum foil and sealed within a Pyrex capsule evacuated to 1 x 10~5 torr or better. This capsule was then sealed within another Pyrex capsule at a similar pressure. The diffusion anneals were carried out at temperatures between 350" and 440°C in Marshall furnaces adjusted to have a temperature gradient of not more than *1/2"C over a 5-in. length. This gradient was then further smoothed by using a nickel tube as a liner in the furnace. The liner was divided into three longitudinal cavities by a septum of nickel sheet to which two calibrated Chromel-Alumel thermocouples were attached. One thermocouple was used for controlling the furnace temperature by means of a Brown Pyrovane controller equipped with a Capaciline anticipation circuit; the second thermocouple was monitored twice daily with a Leeds and Northrup K-2 precision potentiometer.

Jan 1, 1964

By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,' was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951

By A. G. H. Anderson, A. W. Kingsbury

Silicon bronzes containing ken are used to a considerable extent in industry, under the trade name of P.M.G. alloys. Various classes of wrought alloys fall in the composition range 1.5 to 3.5 per cent silicon, and 0.5 to 2.5 per cent iron. Castings may contain as much as 6 per cent silicon and 3 per cent iron at present. The constitutional diagrams of these alloys are thus of considerable practical importance. Copper-silicon-binary alloys have been thoroughly investigated by a number of workers, the latest reports being those of C. S. Smith1 and of A. G. H. Andersen.2 Although much work has been done on iron-copper alloys,3 recorded investigations on the copper-rich copper-iron binary constitutional diagram are not numerous. Tammann and Oelsen4 etermined the solubility limits of iron in copper by means of magnetic measurements, and found that the solubility of iron in copper amounts to a fraction of one per cent at 400°C., increasing slowly to one per cent at 800°C. From 800°C., the solubility increases rapidly and attains 4 per cent at iioo°C. Hanson and Ford,5 using electrical resistivity measurements and the microscope, determined a somewhat different solubility limit. of earlier X-ray works on the copper-iron system, very little has been published. The work by Bradley and Goldschmidt6 on copper-iron-aluminum alloys includes some information on the copper-iron binary. These investigators conclude that substitution of iron in the copper lattice decreases the spacings, which is contrary to the evidence of the present work. Hanson and West? have investigated the ternary alloys of copper with iron and silicon. Although their diagrams are valuable contributions to the understanding of these alloys, they did not recognize the kappa phase,l,2,7,8 and their diagrams do not everywhere conform to the phase rule. The present work contains a check by means of X-rays of the solid solubility limit of iron in copper, and an X-ray investigation of the ternary-phase diagram, which, owing to present conditions, it became necessary to curtail considerably. Preparation of Samples Castings weighing about 75 grams were melted under vacuum. The charges were made up of ingot iron, copper cathodes from Laurel Hill, and refined silicon supplied by the Electrometallurgical Co. Alundum crucibles were generally used. The exceptions were alloys 77 and 78, which were melted in graphite crucibles. The ingots were annealed at 800°C. for one week, then samples were cut for chemical analysis. Longitudinal sections of the binary alloy ingots were hammered into plates 1/8 in. thick. Wherever possible, these plates were homogenized at temperatures ensuring

Jan 1, 1943

By A. G. H. Anderson, A. W. Kingsbury

Silicon bronzes containing ken are used to a considerable extent in industry, under the trade name of P.M.G. alloys. Various classes of wrought alloys fall in the composition range 1.5 to 3.5 per cent silicon, and 0.5 to 2.5 per cent iron. Castings may contain as much as 6 per cent silicon and 3 per cent iron at present. The constitutional diagrams of these alloys are thus of considerable practical importance. Copper-silicon-binary alloys have been thoroughly investigated by a number of workers, the latest reports being those of C. S. Smith1 and of A. G. H. Andersen.2 Although much work has been done on iron-copper alloys,3 recorded investigations on the copper-rich copper-iron binary constitutional diagram are not numerous. Tammann and Oelsen4 etermined the solubility limits of iron in copper by means of magnetic measurements, and found that the solubility of iron in copper amounts to a fraction of one per cent at 400°C., increasing slowly to one per cent at 800°C. From 800°C., the solubility increases rapidly and attains 4 per cent at iioo°C. Hanson and Ford,5 using electrical resistivity measurements and the microscope, determined a somewhat different solubility limit. of earlier X-ray works on the copper-iron system, very little has been published. The work by Bradley and Goldschmidt6 on copper-iron-aluminum alloys includes some information on the copper-iron binary. These investigators conclude that substitution of iron in the copper lattice decreases the spacings, which is contrary to the evidence of the present work. Hanson and West? have investigated the ternary alloys of copper with iron and silicon. Although their diagrams are valuable contributions to the understanding of these alloys, they did not recognize the kappa phase,l,2,7,8 and their diagrams do not everywhere conform to the phase rule. The present work contains a check by means of X-rays of the solid solubility limit of iron in copper, and an X-ray investigation of the ternary-phase diagram, which, owing to present conditions, it became necessary to curtail considerably. Preparation of Samples Castings weighing about 75 grams were melted under vacuum. The charges were made up of ingot iron, copper cathodes from Laurel Hill, and refined silicon supplied by the Electrometallurgical Co. Alundum crucibles were generally used. The exceptions were alloys 77 and 78, which were melted in graphite crucibles. The ingots were annealed at 800°C. for one week, then samples were cut for chemical analysis. Longitudinal sections of the binary alloy ingots were hammered into plates 1/8 in. thick. Wherever possible, these plates were homogenized at temperatures ensuring

Jan 1, 1943

By M. D. Hassiallis

The claim is made in a number of patents1'2'3'4 that some compounds of the class known as aryl sulphides have collector properties. One of these patents generalizes the claim to include all aryl sulphides, whose generic formula is R-S2-R' (where x = 1,2, . . . ), with the restriction that if the aromatic radicals R, R' contain substituent groups these groups may not contain nitrogen or oxygen. Moses, Hess, and Perkins cite as evidence for their claims the results of flotation tests on Anaconda and Miami copper ores using diphenyl sulphide, ditolyl disulphide and dinapthyl disul-phide as collectors. The use of alkyl sulphides as collectors has also been reported5 with the conclusion that the alkyl sulphides are better collectors than the corresponding aryl sulphides. The experimental work cited appears to confirm this contention. In order to test these claims with respect to diphenyl sulphide, a sample, purchased from the Eastman Kodak Co., was tested against Anaconda ore. The procedure followed. was that of Moses, Hess, and Perkins. A sample of ore weighing 500 • grams was placed in a laboratory ball mill. To this was added 220 grams of water, 0.06 grams of commercial diphenyl sulphide (1/4 lb. per ton of ore), and 0.8 grams of lime (3 lb. per ton of ore). The material was ground until 93 per cent passed a 65-mesh screen. This pulp was diluted to 16 per cent solids. A sample of the diluted pulp was placed in a Minerals Separation type of laboratory flotation cell. After a a-min. agitation period, pine oil was added and the froth collected for a period of 15 min. This test recovered 68 per cent of the copper, with a ratio of concentration of 6.8:I. The tailing assay was 0.3 per cent Cu. Moses, Hess and Perkins attained a recovery of 75 per cent, with a ratio concentration of I2:I. Although these results do not compare too well with those of Moses, Hess and Perkins, subsequent tests showed an improvement, as judged by vanning of the tails. It is concluded, therefore, that the patent results are confirmed. Contact-angle Tests In order to study the response of the various minerals, found in Anaconda ore, to commercial diphenyl sulphide, some contact-angle tests were made. Polished particles of bornite, chalcodte, chalco-pyrite, pyrite and quartz were conditioned for 15 min. in a suspension of diphenyl sulphide in water. The concentration of this suspension was 0.284 grams per liter, this being the concentration of this reagent in the ball mill. The conditioned particles were rinsed with water (not rubbed with filter paper or boiled linen) and then tested against an air bubble in the bubble machine, with the following results: born-

Jan 1, 1943

By M. D. Hassiallis

The claim is made in a number of patents1'2'3'4 that some compounds of the class known as aryl sulphides have collector properties. One of these patents generalizes the claim to include all aryl sulphides, whose generic formula is R-S2-R' (where x = 1,2, . . . ), with the restriction that if the aromatic radicals R, R' contain substituent groups these groups may not contain nitrogen or oxygen. Moses, Hess, and Perkins cite as evidence for their claims the results of flotation tests on Anaconda and Miami copper ores using diphenyl sulphide, ditolyl disulphide and dinapthyl disul-phide as collectors. The use of alkyl sulphides as collectors has also been reported5 with the conclusion that the alkyl sulphides are better collectors than the corresponding aryl sulphides. The experimental work cited appears to confirm this contention. In order to test these claims with respect to diphenyl sulphide, a sample, purchased from the Eastman Kodak Co., was tested against Anaconda ore. The procedure followed. was that of Moses, Hess, and Perkins. A sample of ore weighing 500 • grams was placed in a laboratory ball mill. To this was added 220 grams of water, 0.06 grams of commercial diphenyl sulphide (1/4 lb. per ton of ore), and 0.8 grams of lime (3 lb. per ton of ore). The material was ground until 93 per cent passed a 65-mesh screen. This pulp was diluted to 16 per cent solids. A sample of the diluted pulp was placed in a Minerals Separation type of laboratory flotation cell. After a a-min. agitation period, pine oil was added and the froth collected for a period of 15 min. This test recovered 68 per cent of the copper, with a ratio of concentration of 6.8:I. The tailing assay was 0.3 per cent Cu. Moses, Hess and Perkins attained a recovery of 75 per cent, with a ratio concentration of I2:I. Although these results do not compare too well with those of Moses, Hess and Perkins, subsequent tests showed an improvement, as judged by vanning of the tails. It is concluded, therefore, that the patent results are confirmed. Contact-angle Tests In order to study the response of the various minerals, found in Anaconda ore, to commercial diphenyl sulphide, some contact-angle tests were made. Polished particles of bornite, chalcodte, chalco-pyrite, pyrite and quartz were conditioned for 15 min. in a suspension of diphenyl sulphide in water. The concentration of this suspension was 0.284 grams per liter, this being the concentration of this reagent in the ball mill. The conditioned particles were rinsed with water (not rubbed with filter paper or boiled linen) and then tested against an air bubble in the bubble machine, with the following results: born-

Jan 1, 1943

By AIME AIME

General Local Committee.-John Fritz, Chairman; A. B. de Saulles, Vice-Chairman.; R. M. Bird, Treasurer; Henry S. Drinker, Secretary; Robert H. Sayre, E. P. Wilbur, Charles M. Dodson, Abraham S. Schropp, E. M. McIlvain Archibald Johnston, A. B. Fichter, C. G. Convers, W. A. Wilbur, Garrett B. Linderman, Frederick Conlin, George Pettiuos, Albert Brodhead, Garrett L. Hoppes, M.B. Cutter, H. J. Seaman, C. A. Matcham, B. F. Fackenthal, Jr., A. L. J. Queneau, Geo. R. Elder, Eldridge Wilbur, William H. Chandler, Mansfield Merriman, Joseph F. Klein, William S. Franklin, William Esty, Joseph AN'. Richards, Howard Eckfeldt, John D. Irving. Transportation Committee.-H. J. Seaman, C. A. Matcham, B. F. Fackenthal, Jr., A. B. Fichter, A. L. J. Queneau, Henry S. Drinker. Hotel Committee. -Garrett B. Linderman, Charles M. Dodson, W. A. Wilbur, Garrett L. Hoppes, Albert Brodhead. Steering Committee.-William S. Franklin, William Esty, John D. Irving, R. M. Bird, the members of the Tau Beta Pi Society of Lehigh University. Committee on Meetings - William S. Drinker, Joseph W. Richards, Howard Eckfeldt. Entertainmment Committee.-W. A. Wilbur, E. M. McIlvain, Archibald Johnston, A. B. de Saulles, G. G. Convers,.A. L. J. Queneau, Garrett B. Linderman, Frederick Conlin, George Pettinos, Garrett L. Hoppes, Henry S. Drinker, William S. Franklin, Eldridge Wilbur, Robert M. Bird, Secretary. The opening session was held at 8.30 p.m., Wednesday, February 21, 1906, in Gymnasium Hall of Lehigh University, which had been tastefully decorated with flags and bunting. Dr. Henry S. Drinker, President of Lehigh University, and Secretary of the General Local Committee, called the meeting to order, and welcomed the Institute to the Bethlehems, where its first meeting, after its organization in May, 1871, at Wilkes-Barre, was held in August, 1871.*

May 1, 1906

By AIME AIME

SECTION DELEGATES were given an opportunity to see how the machinery of Institute administration functions, on Tuesday evening, Feb. 16, when they were the' guests at the regular monthly meeting of the Directors. Of the new board of 25 members, 19 were present at the meeting, including directors from Seattle, Los Angeles, Wyoming, Oklahoma, Chicago and Pitts-burgh, the new junior past-president from Jerome, Ariz., and the new president from .Washington, D. C. The complete list of the 72 in attendance at the dinner,: held in the main dining room of the Engineers' Club, which pre-ceded the general session of the Directors'. meeting, follows:

Jan 1, 1932

By D. Y. Geng, Syd S. Peng

This paper analyzes the effects of geology and mining methods on surface subsidence factor, angle of draw and angle of critical deformation based on the results of 40 longwall subsidence profiles in the Northern Appalachian coalfield. Several equations were derived to show the relationships between those parameters. Furthermore, the equations were transferred and plotted in the form of several monographs for convenience of applications.

Jan 1, 1982

By W. Chubb

By measuring the hardness of metals at temperatures just above and just below their allotropic change point, it has been established that crystal structure has a real effect upon the strength of metals. The DPH of cobalt, iron, titanium, uranium, and zirconium have been measured at temperatures up to 1000°C. It was found that the body-centered-cubic crystal structure is always the softer structure when it is involved in an allotropic transformation. The close-packed and more complex structures are inherently harder, and may be expected, therefore, to be better base materials for high strength alloys. IT has been observed that for metals with nearly the same melting point (i.e., tin and lead, magnesium and aluminum) the metal with the more complex crystal structure has a higher tensile strength and hardness. It might be asked whether this effect is really caused by the difference in crystal structure; and, if so, just what is the contribution of crystal structure to the strength of these metals. A qualitative answer to these questions can be obtained by measuring the change in hardness produced by the change in structure in metals exhibiting allotropic forms. The evidence for changes in mechanical properties during allotropic transformations is rather meager. In 1909, Rosenhain and Humfrey' observed that "ß" iron showed much less deformation at the transformation temperature than a iron. By means of a torsion test, Lee found that iron bars were "critically plastic" at the a-7 transformation temperature. Sauerwald and Knehans have shown that the dynamic hardness of iron increases between 900" and 1000°C. In 1930, Albert Sauveur' presented data on the hardness, tensile strength, and torsional strength of pui-e iron up to 1000°C. He concluded, "At 900°C, the a iron transforms into y iron, and this is accompanied by increased strength and stiffness and decreased ductility." The same year, Schischokin" obtained data on the hardness of thallium at temperatures above and below its transformation temperature. His data are replotted on semilogarithmic coordinates as Fig. 1. The fact that his data fall on straight lines in this type of plot is believed to attest to the purity of his metal and the accuracy of his results. In 1941, Nadai and Manjoine" obtained tensile data on pure iron with an indicated increase in strength at about 900°C. These experiments make it quite evident that changes in mechanical properties occur when a metal transforms from one crystal structure to another; but, except for Schischokin's data on thallium, none of the measurements seem accurate enough to determine the relative magnitude of the mechanical property change. Materials The metals that have been examined for changes in hardness during transformation include l—as- deposited commercial electrolytic cobalt about 99.7 pct pure, 2—Armco ingot iron, 3—are-melted iodide titanium of a purity in excess of 99.8 pct, 4—uranium of a purity in excess of 99.5 pct, 5—are-melted iodide zirconium of a purity in excess of 99.8 pct, 6—annealed, 0.08 pct C, rimmed steel, and 7—commercially pure RC55 titanium. While the purity of the first five of these materials leaves something to be desired, it will be noted that the observed hardness discontinuities occurred at the accepted transformation temperatures. (These temperatures are indicated by vertical arrows in Figs. 1 and 3 through 7.) The last two materials are commercial alloys introduced to show the effect of minor alloying elements upon the hot hardness curve. Apparatus Hardnesses at elevated temperatures were determined by means of a vacuum hot hardness machine. A diagram showing the basic features of this machine appears as Fig. 2. This machine is essentially a deadweight hardness .machine in a furnace within a vacuum chamber. The sapphire-tipped indentor

Jan 1, 1956

By A. L. Slaughter

The Homestake mine, located in western South Dakota, was discovered in 1876. The first reported production was in I 878. Total production through 1965 is 6,554,249 troy ounces of silver and 27,961,276 troy ounces of gold, worth $987,000,000 at present prices. Precambrian sedimentary formations at Lead total 20,000 feet. The Poorman Formation, the oldest, is chiefly ankerite carbonate. The Homestake Formation is iron-magnesium carbonate. The younger formations are argillaceous with some quartzites. The Cambrian Deadwood Formation unconformably overlies the Precambrian. All are cut by Tertiary intrusives. Sideroplesite schist of the Homestake Formation was converted to cummingtonite schist in the zones of higher-grade metamorphism. The Precambrian rocks show the effects of extreme isoclinal folding. A second stage of folding ( cross folds) may have been caused by the Tertiary intrusives. All folds plunge to the southeast. The Homestake ore bodies are pipe-like replacements of the Homestake Formation in zones of cross folding. It is believed that dilatation of the schists has increased permeability in these zones. Chloritization of the schists is the most widespread effect of the mineralization which is divided into four stages. Principal minerals of the first stage are quartz, chlorite, and arsenopyrite; in the second stage, quartz, ankerite, and pyrrhotite. In the third stage only pyrrhotite was deposited. The fourth stage followed the intrusions of Tertiary dikes and deposited mostly pyrite and calcite. Gold accompanies all stages and is always the last mineral to be deposited. It is most closely associated with arsenopyrite of the first stage but can be interpreted as having been deposited during the fourth stage and superimposed on the products of the earlier stages.

Jan 1, 1968

By K. Mukai, M. Ishihara

This report is a brief discussion of the impurity levels both in primary aluminum and super-purily alnminim in connection with raw materials and proc-essing methods. Particularly, truce amounls of im-purities were analyzed by introducing nittss-speclro-gruphy and nenlron-aclivalian analysis techniques. Vanadium and gallium content in primary aluminum metal corresponded to theor amounls in anode coke. but the nickel content in primary aluminum was hide-pendent oj its amount in the anode cake. Sulfur in the anode colic might result in an increase of the iron content in the molten metal in the reduction cell. The content of sodium and calcium increased with increasing bath ratio. In the holding furnacc sodium content decreased rapidly, and nonmetallic inclusions merit separated front the mollen metal. Three-layer elctrolysis was effectire in eliminating many impuri-ties with the exception of copper, aluminum oxide. aluminum nitride, and some rare-earth elements. THE amount of impurities and nonmetallic inclusions in aluminum metal depends on impurities in the raw materials and various production processes. This paper presents an investigation of the behavior of impurities and nonmetallic inclusions in aluminum during the electrolysis process, the period in the holding furnace, and the process of three-layer electrolysis. Chemical analysis and emission spectrometric analysis have generally been used as methods to determine small amounts of impurities in both primary aluminum and super-purity aluminum; however. mass spectrography and neutron-activation analysis have been recently introduced into this field, and trace amounts of impurities can accurately be determined by these latter methods. EXPERIMENTAL WORK Common impurities were determined by means of absorptiometric. polarographic, flame-photometric. and emission-spectrometric methods. However, in the determination of trace amounts of impurities and non-metallic inclusions, the following methods were applied. In the analyses of trace impurities by mass-spec- trographic analysis, samples were exposed in the vacuum spark of double-focus ing Mattauch-Herzog type mass spectrograph (Japan Electron Optics Laboratory, Ltd.). Ilford Q2 photographic plates were used as ion detectors. Fe was used as the internal standard, and the atomic concentration of each element was calculated by the following expression and converted into the weight concentration: where E, and Ei are the exposures (coulomb) when isotopes of the internal standard and impurity elements (on which the estimate is based) show the same density, X is the percent (atomic) concentration of the standard, IF and Ii are the percent abundances of the isotopes of the standard the impurity elements (on which the estimate is based), and Ms and hfi are the mass of the isotopes of the standard and impurity elements (on which the estimate is based). The coefficient of variation in this method is about 40 pct in the range of 0.1 to 1 ppm. In neutron-activation analysis, irradiations were done in the nuclear reactors TRIGA-I1 (neutron flux: 4.7 x 10 11 n per sq cm per sec; Rikkyo University) or JRR-2 (neutron flux: 2 x 1013 n per sq cm per sec: Japan Atomic Energy Research Institute). After the chemical separation, a NaI (3 by 3 in.) scintillator connected to a 256-channel y-ray spectrometer (R.C.L.) was used for counting and recording various activated impurities. The coefficient of variation in this method is about 20 pct. In the analyses of nonmetallic inclusions, aluminum-oxide determination was carried out according to Fischer's method, 3 as follows. A slice of sample was cut off and the surface was cleaned. It was dissolved in bromine-methanol. The solution was filtered and the residue was washed. The residue was fused with potassium bisulfate flux. Then it was dissolved in weak acid, and oxine solution was added. The aluminum oxinate was extracted with benzene. Finally, aluminum was determined absorptio-metrically. Aluminum nitride determination was carried out as follows. A slice of sample was cut off and the surface was cleaned. It was put in the distillation apparatus and decomposed with sodium hydroxide solution. The solution was distilled. Then ammonia was absorbed and

Jan 1, 1967

By D. W. Frommer, M. M. Fine

Mineral dressing research showed that iron concentrates of commercial quality could be produced from the Pea Ridge deposit near Sullivan, Mo. Magnetic separation and flotation, on a laboratory scale, yielded concentrates ranging from 60.0 to 71.4 pet Fe at recoveries of 89.9 to 97.6 pct. Early in 1957 St. Joseph Lead Co. announced discovery of three new centers of iron ore deposition in east central Missouri.' The discovery resulted from exploratory drilling in the vicinity of a magnetic anomaly or high. A deep hole, drilled into the Pre-Cambrian porphyry to determine the cause of anomaly, penetrated a magnetite-rich deposit.' The magnetic surveys that revealed the anomalies were begun by the Missouri Geological Survey in 1929 and were continued into the 1930's.3 At that time an area in Crawford County known as the Bourbon magnetic high was located. A second anomaly, similar in size and intensity, was discovered about six miles to the northeast in Franklin County in the vicinity of Sullivan. This area was not studied in detail until the early 1940's. To determine the cause of the anomalies, the USBM drilled four holes at the Bourbon site in 1943-1944.4 The most productive hole penetrated four mineralized zones having a total thickness of 127.5 ft. These zones contained magnetite in rhyo-lite porphyry at depths between 1600 and 2000 ft. Additional iron ore below 2000 ft was considered a possibility at the time. Some years later, the USGS, Missouri Geological Survey, St. Joseph Lead Co., and others cooperated in sponsoring an aeromagnetic survey of the Bourbon-Sullivan area which resulted in discovery of a third high, about eight miles distant at Pea Ridge. This deposit, with an estimated reserve of 50 to 100 million tons of iron ore, is considered the main find, although other orebodies in the same general area are of definite interest.' When this discovery was announced, St. Joseph Lead also revealed plans to exploit the deposit jointly with Bethlehem Steel Co. A new corporation, Meramec Mining Co., was established, and 1962 was set as the target date for completing physical plant.2 Annual production goals of 2 million tons of beneficiated and pelletized iron ore were proposed. Preparation of the site for shaft sinking was begun in June 1957. Orebody and Character of Samples: Drilling to date has established the Pea Ridge orebody as a crescent-shaped pipe about 300 ft wide. Some drillholes were bottomed at 2800 ft in very good iron ore.6 he orebody is predominantly magnetite, although hematite and a mixture of hematite and magnetite occur in the upper areas and peripheral walls. Drillhole cores representing ore from different areas and depths of mineralization were grouped into composites for testing. These composites consisted of: 1) medium grade mixed hematite and magnetite, 2) high grade mixed hematite and magnetite, and 3) high grade magnetite. The medium grade ore came from three holes with depths of i350 to 1900 ft. The high grade mixed hematite and magnetite cores came from the 1790 to 2812-ft interval of one hole. Partial chemical analyses of the three samples, given in Table 1, reveal that all are excessively high in phosphorus and sulfur, and sample 1 is

Jan 1, 1960

By KENNETH W. GREENAWALT, William Greenawalt

THE patent system, through which an inventor is given exclusive right to his invention for a limited period as a reward for his industry and in reimbursement of his expenditures, originated in England in the famous "Statute of Monopolies," enacted in 1623. The first patent granted in America was to Samuel Winslow, in Massachusetts, in 1641. The basis of the patent system of the United States is a provision in the Constitution giving Congress the power to secure to inventors for a limited time the exclusive use of their discoveries. The first legislative enactment was the law of 1790, which was placed on the statute book after Washington had addressed Congress in its favor. Under this law, the Secretary of State, the Secretary of War, and the Attorney General constituted the board for the examination of patent applications and the granting of patents. The first Secretary of State, Thomas Jefferson, became the first administrator of the patent sys- tem in this country. He personally examined every application filed during his term of office.

Jan 1, 1930

By W. M. Rust, W. D. Mounce

THE almost universal acceptance of electrical logging by the petroleum industry calls for a critical examination of the physical bases of the common methods. This is particularly needed for the natural potential log. The conventional explanations are based on the phenomena of electrofiltration and electro-osmosis. However, experimental data show that they fail to give a basis that is quantitatively sound. Moreover, they lead to interpretations of details of electrical logs that are erroneous. It was found experimentally that when a plug of shale is placed in a chain of dissimilar electrolytes, a current flow results. Experiments on oil-well cores and fluids similar to those existing in wells show that potentials are set up which are in reasonable agreement with those encountered in electrical logging. Doubt- less other sources of potential are important but this explanation not only accounts for much of the potential but also clarifies some fairly familiar examples of misinterpretations.

Jan 1, 1944

By A. J. May

THE Star shaft is near the north boundary of the group of mining claims belonging to the Ground Hog Unit of the American Smelting and Refining Co., near Vanadium, N. Mex. The shaft bins and surface plant are served by a siding from the Atchison, Topeka and Santa Fe railroad, and this factor of railroad transportation influenced the choice of site. This paper describes the shaft sinking only, and does not cover the surface plant or other parts of the mine or its equipment. Experience with this shaft seems of interest because of the mechanical mucking, good rate of progress, and the costs obtained at the present level of labor and material costs. The shaft has four compartments, as shown in fig. 1. Equipment: Riddell Mucker: The mucking was done by a clamshell bucket and a Riddell mucker, which, as in other shafts sunk with this machine, consisted of a carriage mounted on axles with double flanged wheels that traveled back and forth on a swinging track, parallel to the long axis of the shaft (fig. 2 to 6). Three air motors were mounted on the carriage; one hoisted the clam, one operated the bucket opening and closing device, and the third moved the carriage along the track. The carriage was designed with guide shoes and could be hoisted to the surface in either skip compartment without trouble (fig. 4). During blasting operations the clam was tied on the rails and the carriage was hoisted up a few sets to protect it from flying rock. No attempt was made to hoist the carriage and clam together lest the clam catch in the timbers. The track on which the carriage operated was built of extra heavy 6 in. pipe with 1x2 in. strap welded on top for rails. A 1/2x4 in. angle was welded on the bottom of the 6 in. pipe with a 1 in. round rod welded in the angle for a filler and additional strength. The end or cross pieces of the track which kept the track to gauge, were also made of reinforced, heavy 6 in. pipe and were bolted to the long members on which the carriage traveled (fig. 2 and 3). This section of track was used, instead of heavy railroad rails, for two reasons: (1) this section would bend before it snapped and was much safer for the men in the bottom; and (2) it was a better blasting shield, and protected the timbers better, in fact, only five wall plates were broken by blasting in 1926 ft of shaft, although 150 to 225 lb of 40 pct powder was loaded per round, depending on the ground conditions. The swinging track was supported by four 5/s in. hoisting cables anchored to the end plates. There were also four safety cables fastened two to three sets above the carriage, which would catch the carriage if one of the supporting cables should fail for any reason (fig. 7). Clamshell Buckets: Two clams were used, each of 3/s yard capacity, both manufactured by Blaw Knox, Nos. 662 and 663. The No. 663 clam was 4 in. wider and 5 in. shorter than the No. 662, but seemed to dig and load more satisfactorily. It was easier to hoist and lower when it came up for repair. It did not turn over as easily, had less spill

Jan 1, 1950

By R. J. Wygal

A method is presented by which homogeneous, isotropic, and reproducible aggregates of particles such as glass beads, sand, ground glass, etc., may be prepared simply and quickly by using a "particle distributor". Several applications of the packing method to the construction of model reservoirs are described. The flow characteristics of these packings me given. Some factors which limit the usefulness of unconsolidated packs for simulating reservoir rock are overcome through artificial cementation of the aggregates. INTRODUCTION Many laboratory studies of porous media are based on experiments using test packs of sand, glass beads and other granular materials. More confidence can be had in the results of such studies if the test packs are known to have uniform properties throughout, to be mechanically stable and to be accurately reproducible. This paper presents a method by which such packs of a variety of shapes and sizes may be constructed using a particle distributor. Some factors which limit the usefulness of unconsolidated packs as a means for simulating reservoir rock are described. A method of overcoming these limitations, which involves artificial cementation of the packs, is presented. DEVELOPMENT Particles packed by the tamping or vibrating techniques are usually either non-uniform or mechanically unstable. An invention by Currie and Gregoryl overcomes these difficulties to some extent. The invention is based on the use of a stream of falling particles impinging on and passing through a distributor matrix of several layers of closely spaced spheres. The particles are well dispersed by numerous collisions with the spheres. They become homogeneously distributed at some distance below the distributor matrix and at that position are collected in the sample container. This apparatus, however, was found to be ineffective when small particles were used since small particles accumulate on the top surfaces of the spheres. An improved distributor matrix was made, first in the form of a stack of five sieves, and then in the more adaptable form of spaced layers of wire screen. Fig. 1 shows a longitudinal view through a five-layered distributor of eight-mesh wire screen. This device gives excellent results.* Fine particles pass through the distributor with very little hold up. The fine structure of the wire matrix with its many deflecting surfaces ensures good particle distribution. There are no dead areas immediately below the screen as were sometimes observed to occur below a matrix of spheres. Using such a device, 20-30 mesh sands were packed to a porosity of 32.1 per cent at rates varying from 0.17 to 6 lb/rnin. The lowest porosity achieved by tamping small increments of similar sands into a container was 33 per cent. Motion pictures at 3,000 frarnes/sec of the surface of a growing pack of 2-3/4 mm glass beads have helped to show the mechanism by which packs of low porosity are obtained. The beads, although packed at the rate of 5 lb/min, were observed to hit the pack surface singly, for the most part, and at well spaced points of impact. Part of their energy is transferred to surface beads which are thereby

By K. Sassa, I. Ito

The dynamic principal stresses induced within rock by an explosion under con fined conditions are analyzed for the case of blasting with one free face by applying the values of measured radial displacement, particle velocity and so on to equations derived from the theory of elasticity. The dynamic stresses on the free face are also calculated from the strain measured by wire strain gauges affixed on the free face. Some results obtained are briefly: 1) The maximum stress on the free face appeared at the intersection between the free face and the burden, and its magnitude was about twice as large as the magnitude of the tangential tensile stress imparted by the incident stress wave within the range related to the breakage by blasting. 2) The maximum value of the compressive stress near the free face was decreased due to the existence of the free face, while that of the tensile stress was increased. 3) At any point near the free face, the directions of the principal stresses in the r? plane using spherical coordinates with the origin at the center of the spherical charge, changed with time except in the direction of the burden. However, at another point near the explosion point where the principal stresses were mainly those stresses caused by the initial longitudinal wave, the directions of the principal stresses coincided with those of the coordinate used. 4) The maximum value of the tensile stress in the F direction was larger than those in the re plane at and near the free face. 5) The tensile stress caused by the Hopkinson effect appeared only near the burden. 6) It is presumed from the results of stress analysis that radial cracks will be produced in the rock mass near an explosion point, but with the approach of the free face, the directions of cracks curve towards a direction parallel to the free face. INTRODUCTION In order to investigate the mechanism of rock breakage by blasting, it is considered to be very im- portant to know how the stresses are generated and distributed within the rock by explosion of a confined charge. As part of a research program concerning the mechanism of rock breakage by blasting, the authors have already published papers on the detonation pressure produced at the inner surface of the charge hole1 and on the behavior of the dynamic stresses within rock caused by an explosion in the case where no free face existed.' In this study the dynamic stresses on and near the free face have been investigated for the case of blasting with one free face. The mechanism of rock breakage in blasting is discussed in the light of these studies.

Jan 1, 1967

By V. C. Williams

Some of the physical, chemical, and electrical processes for conversion of saline water to potable or industrial water are economically surveyed from an engineering viewpoint. Since all these processes require energy for drive and equipment for containment, the correlative economic factors are developed which indicate directive influences in the choice of particular regional processes. The supply of natural waters and its distance also affect decision. Any one process will probably not prove dominant in the field because auxiliary considerations such as the saline water source; types and continuing availability of fuel; electric power use or recovery; area economic status and advancement; and the political pressures of population, group demands, and land use tend equivocally to obscure capital and operation cost decisions. Basic engineering considerations, data, and economic factors are presented to assist in the direction of these decisions. An exploding world population, increasing industrialization, advancing standards of living, and the desire of less-privileged nations for betterment focus attention sharply on a major problem: water. *19 Up to now, in retrospect, people have had it relatively easy in the handling of this problem. All the better dams in the most advantageous sites, the better aquifers, the shortest aqueducts have been built. In another phase of the problem, concern is evident that wastes cannot indefinitely be disposed of merely by keeping them dilute and discharging them promiscuously. 7-9 And, perhaps, as past civilizations have done,l5 water, watersheds, streams, and irrigation may have been mismanaged or, at the least, not adequately studied.3,5,36,37 In this last is perhaps the core of the problem. As Gross states, "Ignorance and too often, indifference are contributing factors. Archaeology and theology both furnish ample testimony to the existence of rich lands where deserts now stand; it was man who ravaged his land. Unless education is a companion to water development, development might as well be forgotten. But without water, there is no beginning."13 The U.S. is showing increasing concern about its water for predictions are that by 1980 the daily withdrawals will be 494 billion gal, a figure nearly equal to the dependable supply.Is This is based on a conservative projected population of 230 million. The major categories of withdrawals are: To make available this per capita average of 2150 gal per day will require an expenditure of $219 billion over the next 20 years. The U.S. is not alone in this concern. The United Nations shows as arid zones of the world: all of Africa north of the equator and south of the 20's parallel; all of the Arabian peninsula; all of the middle east and Iran, Iraq, Pakistan, Afghanistan, northern and central India; a great band about 1000 miles wide along the 40'~ parallel from the Caspian Sea east across Russia through China to the Pacific Ocean; all of Australia except the coastal plain; the Caribbean Islands; the western nations of South America; and the western third of the United States and of Mexico. With one quarter of the earth's 57,500,000 sq miles of land thus suffering from lack of good water, increasing attention goes to the treatment of brackish and sea waters. The U.S. has been a leader in this field4,12, 16123,24 through its Office of Saline Water in the Dept. of Interior because even now some of its cities and regions are short of potable water. 11j'7,M Industrial water is also of vital concern as a result of ever higher industrialization1,14122 Other nations, among them JaPan, Israel,13188 Germany, Union of South Africa, Australia, Netherlands, France, Yugoslavia, Russia, and groups such as the Organization for European Economic Cooperation (OEEC)' are also diligent. The objective is low cost water, which means that both technology and economics have prominent roles in saline water conversion processes. TECHNOLOGY: SALINE WATER CONVERSION A number of reviews of methods have been made, principally by staff members of the Office of Saline Water (U.S. Dept. of Interior). Jenkins,31'32 Gillam,34p

Jan 1, 1962

By Roy G. Mead

BECAUSE of its magnitude, and the type of occurrence, the deposit of boron minerals in the Kramer district, Kern County, California, is unlike any other in the world. Discovery of this vast deposit has brought about many changes in the borax industry, so a discussion of the geology, and the occurrence, would not be complete without a brief history of the development of the borax industry. Until the discovery of boron minerals in the desert regions of California and Nevada some seventy years ago, borax was imported from Tibet and India, principally for medicinal purposes, at almost prohibitive prices. Following the discovery of commercial deposits of boron minerals in California and Nevada, and the subsequent development of new uses for borax and boric acid, the consumption has steadily increased until today borax is used in some form or other in every household.

Jan 1, 1933