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By K. Tangri, M. Chaturvedi

On water-quenching from within the (a + ß) phase region Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys can undergo w transfirmation. This transformation has been attributed to the enrichment of ß Zr phase, at the solution-treatment temperature, by the solute atoms. The ß—w transformation is accompanied by a hardening 01 the alloys and in the optimum condition w-bearing specimens of the ternary alloy are about 14 pct harder than those bearing only a' phase. On aging crl reverls thermally to more stable phases, which results in a considerable softening of the specirnens, as follows: w quenched -waged + ß Zr (enriched) waged - a + ß Nb The high-temperature bcc ß Zr in certain zirconium alloys can transform to a metastable w phase which has a primitive hexagonal structure. In the Zr-Nb alloy system w phase has been observed in the composition range of 7 to 15 wt pct Nb by a number of investigators.'-' In this composition range w can form by water-quenching ß Zr or by aging. known as athermal and thermal w, respectively. Hatt and Roberts' have found that thermal w has a constant c/a ratio of 0.622 +0.002 regardless of the composition and tha: the lattice parameters are of the order of a = 5.02A and c = 3.0 ?. The actual lattice parameters depend upon composition and the temperature of aging. The lattice constants of athermal w. however, depend upon alloy composition.3 The presence of w phase in zirconium alloys can cause substantial strengthening which has been attributed as probably due to the coherency between w and parent ß Zr phase. Robinson et al.' found that the presence of w can raise the strength of Zr-5.0 Nb-2.0 Sn and Zr-5.0 Mo-2.0 Sn alloys to about 170.000 psi: however. the ductility is considerably reduced. With the growing use of Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys in the nuclear reactors, and the significant effect of w transformation on the mechanical properties of zirconium alloys studies were undertaken to study the w transformation in Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys. This paper is concerned with the formation and reversion of w phase in these alloys. 1) MATERIALS AND EXPERIMENTAL TECHNIQUES The following two alloys were studied: 1) Zr-2.5 Nb-0.5 Cu (referred to as the ternary alloy): 2) Zr-2.5 Nb (referred to as the binary alloy). The chemical analysis of the alloys is given in Table I. The alloys, in the form of 3/8-in.-diam rods and 1/8-in.-thick sheets, were supplied by the Chalk River Nuclear Laboratories of the A.E.C.L. Initial fabrication for preparation of various specimens was carried out by cold rolling and swaging with intermediate anneals at 1000°C. All the heat treatments were carried out after the specimens were wrapped in zirconium foils and encapsulated in silica tubes under a vacuum of 5 x 10-% m of Hg. For optical metallography and hardness measurements disc specimens + in. diam by + in. thick were used. After the required heat treatments the specimens were mechanically and then chemically polished in a 45 pct HNO3, 45 pct H20. and 10 pct HF solution. The hardness measurements on the chemically polished specimens were carried out on a Vickers hardness tester using a 10-kg load. For each specimen at least fifteen indentations were made in order to obtain a representative hardness value. The phase identification and structural analysis were carried out using X-rays and electron diffraction techniques. Wires of 1.5 mm diam reduced to 0.12 mm diam by chemical etching were used for making Debye-Scherrer powder patterns using copper K-a radiations in 114.6-mm-diam camera. Thin films for transmission electron microscopy were prepared by electropolishing heat-treated a by 7 by 0.005-in.-thick strips using a modified Bollmann-Window technique. The 10 pct perchloric acid-90 pct methyl alcohol electropolishing bath was kepl at -5OCC and polishing was done at 5 to 10 v. The thinned specimens were washed in ethyl alcohol at -30" to -40°C and dried between filter papers. The thin films

Jan 1, 1970

By B. D. Cullity

GOLD and beryllium form an intermediate phase composed of the two metals in equal atomic proportions and having the formula AuBe. According to Winkler,1 this phase probably exists in two modifications: beta, stable below about 600°C, and alpha, stable between 600°C and the melting point, about 740°C. Only the low- temperature beta form will be considered in this paper. EXPERIMENTAL PROCEDURE The gold used had a fineness of 999.75 to 999.85, balance mainly silver, and the beryllium purity was better than 99.8 pct. AuBe was prepared by melting the constituents in a beryllia crucible in an evacuated induction furnace. After melting and thorough mixing, the alloy was allowed to solidify in the crucible. No difficulty was encountered in obtaining a homogeneous ingot. Both chemical analysis and microscopic examination of the ingot showed that the alloy was essentially one phase, containing 50 at. pct gold. The alloy was quite brittle and powder samples could easily be pre- pared by grinding in an agate mortar. The X-ray diffraction patterns were made with CuK-alpha radiation in a Debye-Scherrer powder camera 57.3 mm in diameter. The film was placed unsymmetrically in the camera in order to afford a basis for am-shrinkage corrections. A sample homogenized at 5o0°C gave the same diffraction pattern as a sample taken from the as-melted ingot. GENERAL RESULTS The diffraction pattern of AuBe was readily indexed on the basis of a simple cubic lattice with ao = 4.659 ± 0.001kX. If the unit cell is assumed to contain four AuBe "molecules," the calculated X-ray density is 13.46 grams per cc as compared with the measured density of 13.55 gm per cc. The only missing reflections in the dsraction pattern are (100) and (220) (see Table I). Since these missing reflections are not those characteristic of body or face centering, the lattice of AuBe must be simple cubic. To locate the positions of the atoms within the unit cell, two possibilities had to be considered: I. The structure was disordered and there were eight positions to be filled by an "average" gold-beryllium atom. That the structure was disordered seemed unlikely since the lattice parameter did not vary with composition in alloys containing some- what more and somewhat less than 50 at. pct gold, indicating a fixed composition for AuBe.

Jan 1, 1947

By G. Venturello, C. Antonione, G. Della Gatta

Results from work on the effect of inferstitials on recovery and recrystallization of' very pure iron (99.995 pet) doped with nilrogen up to 400 ppm are reported. Nitrided specimens were obtained by heating the iron in a static atmosphere of NH3 + H2. The samples were cold-rolled 80 pet, subjected to a series of isochronal and isothermal anneals, and submitted to examination by X-rays, micrographs, and hardness tests. Small additions of nitrogen show a strong effect in reducing recovery of' the mechanical properties of high-purity iron. At the temperatures of. the experiments, this effect proved greater than in the case of carbon. At 400°C pure iron recovers more than 50 pet of the total hardness increase, carburized iron vecovers 25 pet, and nitrided iron only 10 pet. On the other hand. the addition of nitrogen has, similarly to carbon, a very small effect on recrystallization; the effect is, however, slightly higher than that of carbon. When the concentration Of nitrogen is above the solubility limit in a iron at the temperattue of the experiments, an increase in the frequency of nu -cleation is also observed. THE object of the present work is to improve knowledge on the effect of interstitials both on recovery and on primary recrystallization of pure iron. In fact. at present there are no available data on the effect of nitrogen on high-purity iron. The only work which at present can be somewhat related to this problem is a work of Leak et al.1 in which grain boundary internal friction at high temperature in the presence of increasing amounts of nitrogen is studied by a torsion pendulum. The present work is a continuation of a previous one2 on the effects of carbon. EXPERIMENTAL PART Preparation of the Material. Pure iron was prepared following the same methods used in the pre- vious work2 and was nitrided using controlled quantities of ammonia in an apparatus similar to that used for carburizing. The apparatus consists essentially of a gas-tight quartz tube containing the specimens. The tube, maintained at constant pressure by means of a mercury seal, is placed in a resistance furnace. For nitriding, the NH3 + H2 atmosphere with a suitable concentration of NH3 was introduced into the tube, which had been previously carefully evacuated and degassed by heating at 600°C. The hydrogen used was carefully purified by passing it through a palladium filter. The ammonia required was prepared with the following reaction: CaO + 2NH4CI —CaCl2 + H2O + 2NH3 by heating the mixture of CaO and NH4C1 in a glass flask and then collecting the ammonia in a graduated Hempel burette. For each nitriding program a given amount of NH3 prepared by this method was introduced together with the H2 into the tube previously evacuated. Nitriding of the sample was then performed at 570°C for 48 hr. After this, to ensure a homogeneous distribution of nitrogen, the samples were further heated for 72 hr at 800°C. With this method which uses a static nitriding atmosphere, carefully controlled conditions of purity are obtained. Contrarily, with the conventional continuous-flow methods, using large quantities of circulating gas, there is a greater risk of introducing impurities into the samples. Furthermore, the required nitrogen concentration in the specimen is easily predetermined and obtained. A plot of the relation observed between the initial concentration of NH3 in the gas and the quantity of nitrogen introduced into the iron samples is given in Fig. 1. The data refer to samples of 1.2-mm thickness and to the nitriding conditions previously described. Furthermore, as a comparison, the data relative to two 0.5-mm-thick samples are reported. The presence of a reservoir in the cold zone of the reaction bulb made possible the gradual dissociation of ammonia on the sample in the hot zone. Internal-friction methods were used to determine the content of nitrogen dissolved in the iron samples. Some analyses were also carried out with chemical methods. The following table, Table I, shows a comparison of data obtained with chemical and internal-friction methods. The correspondence between chemical methods and internal-friction

Jan 1, 1964

Jan 1, 1911

By Earle Schumacher

THE solidus line above the solid solution field in the lead-antimony system was originally determined by Dean and his associates1 from heating curves. They did not regard this line as having been accurately fixed and in their more recent publications2 the curves drawn do not follow closely the original data. The precise location of the solidus line is of importance in the extrusion of lead-antimony cable sheath, as the temperature of the metal in this process must be less than the lowest temperature at which any part of the alloy in the lead-press charge becomes liquid. It is very desirable, however, to operate at as high a temperature as possible, as the rate of extrusion for a given pressure is approximately doubled for an increase of 10° C. in temperature. The precise location of this line is also important, in the investigation of ternary systems of lead, antimony and a third metal. For these reasons, and because of the differences reported in the literature, data were secured on the lead-antimony solidus line by the classical quenching-test procedure.

Jan 1, 1927

By M. G. Corson

THE theory of hardening by interference with slip which has been so clearly developed by Jeffries and his co-workers requires that an alloy to be amenable to age or heat hardening should contain among its components some that will stay in solid solution at high temperatures and precipitate as a secondary phase on cooling. This secondary phase may be either a more or less pure individual element (chromium in the case of copper, anti-mony in the case of lead), or some intermetallic com-pound. Those cases of hardening which depend on the precipitation of a compound are not only the most frequent, but are also far superior in the efficiency of hardening obtained. However, the slip interference theory as stated in its most general form is not sufficient to foretell new cases of this type of hardening and also will not explain some phenomena of a more intricate nature. It is not sufficient that a secondary phase might be absorbed by the main one at high temperatures and precipitated at the lower ones. The kinetics of this precipitation and the accompanying. physical phenomena of dimensional changes play independent and highly important parts. These kinetics, while not yet sufficiently studied to he formulated in the shape of physicochemical equations, might find their expression-in a qualitative systema-tization of the phenomena of precipitation according to two different viewpoints. To begin with, we encounter the question as to the velocities of the precipitation and of the growth of the phase precipitated. To harden a metal in an efficient manner we must be able to control the precipitation on one hand and also to bring the total of the secondary phase to such a number and size of the particles pre-cipitated as, will produce a desirable hardening effect under commercially feasible conditions of. age or heat hardening. From this viewpoint six different cases may be dis-cerned.

Jan 7, 1928

By T. Suganuma

Mitsubishi-Cominco Smelting Co. is a joint venture of Mitsubishi Metal Mining Co. Ltd. (M.M.M.) of Japan and Cominco Ltd. of Canada. The smelter, which is located alongside M.M.M.'s Naoshima copper smelter, was completed in May, 1966 and has a capacity of 36 000 metric tons per year of refined lead. The concentrate feed for the smelter from Pine Point Mines Ltd. is high grade with low impurities; particularly silver, bismuth, antimony, and arsenic, which facilitated a simple plant layout and operation. Concentrate, fluxes, recycle granulated slag and return sinter are drawn from bins by automatic control over weigh belt feeders, sintering is carried out on a 20 m2 Lurgi updraught sintering machine, furnacing in a 3.0 m x 1 ½ m water jacketed blast furnace equipped with an Asarco continuous tapper, refining in four 120 metric ton kettles and casting on a 25 metric ton/hour automatic casting machine. The S@ gas from sintering is cleaned in a high temperature baghouse utilizing glass bags and is then delivered to the M.M.M. copper smelter acid plants. The furnace gases after cleaning in a low temperature baghouse are vented to atmosphere.

Jan 1, 1970

Steel Tape The new Lufkin Royal Ni-Clad steel tape, made in 25, 50, 75, and 100-ft sizes, is stated to cost less than any other steel tape on the market. Figures and graduations are an integral part of the steel and the nickel plated surface is rust and corrosion resistant. Circle No. 1 Lift A manually operated and propelled hydraulic lift marketed by Century Products Co. weighs only [ ] 150 lb, but the 23x24 in. platform will raise 1000 lb from floor level to 4 ft height. Circle No. 2 Scintillation Counter The Scintillator from Precision Radiation Instruments, stated to have 100 times the sensitivity of the Geiger counter, is suitable for prospecting and may be operated from plane or moving vehicle. The instrument is contained in a 2-lb probe and the belt mounted battery box weighs less than 4 lb. Circle No. 3 Generators Wincharger Corp. announces development of a Speedy-Shift wheel-barrow base type attachment for model 700, 1800 and 5000 engine-generator sets. Portability of the engine-generator sets themselves has been improved by belted construction for higher operating speed and maximum weight reduction. Circle No. 4

Jan 1, 1952

The State Mining Experiment Station, Missouri School of Mines and Metallurgy, Rolla, Mo Charles H. Fulton, Director of the School of Mines Martin H. Thornberry, Director of the Mining Experiment Station. From the State Mining Experiment Station are issued all the general and technical bulletins of the School of Mines The latest bulletin containing a complete list of publications will be sent upon application to the Director of the Station Residents of the state may obtain bulletins as issued without charge, or may ask to be placed on the mailing list. Nonresidents should write to the Director for further information concerning specific bulletins. From the long list of bulletins the following have been care¬fully selected as being most likely to interest the geologist and the mining engineer. Vol 8, No. 1 (1916), Bibliography of concentrating ores by flotation, by J Cunningham, vol 1, No 3 (1912), Some apparatus and methods for demonstrating rock drilling and the loading of drill holes in tunneling, by L E Young, vol 2, No 1 (1915), Comparative tests of piston drill bits, by C R Forbes and L M Cummings; vol 2, No 3 (1916), Cupellation losses in assaying, by H. T Mann and C. Y Clayton; vol 4, No 1 (1917), The hydrometallurgy and electrolytic precipitation of zinc, by F D. James; vol 4, No 2 (1917), The effect of additional agents in flotation, pt 1, by M. H. Thornberry and H T. Mann, vol 5, No 1 (1919), The carbonization of Missouri cannel coals, by H L. Dunlap, K. K. Kershner and V. X Smiley. Vol 5, No. 4 (1921), Coal mining methods in Missouri, by W W Weigel, vol 6, No 1 (1921), The problem of the St Peter sand¬stone, by C L Dake, 50 cents, vol 6, No. 2 (1922), Bibliography on the electrothermic metallurgy of zinc, by B M. O'Harra, vol 6, No. 4 (1923), Experiments on the distillation of zinc from complex zinc-lead-silver ores, by B M. O'Harra and E S. Wheeler, vol 7, No 3 (1924), Underground loading devices, by C. E. van Barneveld, 81; vol 7, No. 4 (1924), Briquetting of zinc ores, by B. M. O'Harra; vol. 8, No 2 (1925), A treatise of Missouri clays, by M. H. Thornberry.

Jan 1, 1933

The Goodman Mfg. Co., Chicago, builders of underground electric mining machinery, celebrated its 50th Anniversary on April 23rd. The company has a complete line of cutting machines, loaders, conveyors, locomotives, and shuttle cars for service in both coal and metal mines. The Joy Mfg. Co. has received, under the provisions of the Economic Cooperation Administration, an initial order in excess of $1,000,000 for equipment to be used in the mechanization of iron ore mines in France. While the equipment will be used in various privately owned mines, the order was placed through the French Society for the Development of Mechanical Mining. Included in the equipment are the company's recently developed hard rock loaders and shuttle cars. American Brake Shoe Co. has consolidated all operations of its Canadian subsidiaries into one corporation, the Dominion Brake Shoe Co. Ltd., Montreal, Canada. The products of Dominion Brake Shoe include brake shoes, track equipment, manganese steel castings, automotive brake lining, air compressors, and paint spray equipment. Exhibits of more than 2000 electrical products, processes, and techniques, ranging from precise aircraft instruments to complex working models of steel mill, textile and other industry equipment, will be displayed in the "More Power To America Special" when it makes its nationwide tour this spring. C. H. Lang, Vice-President in charge of sales for General Electric's apparatus department, said that the train will visit the country's key industrial centers for inspection by utility and industrial executives and municipal leaders. The train will be hauled by an Alco¬G-E two-unit, 4000-hp., Diesel-electric locomotive which in itself will be part of the unusual series of displays. Sizing of Excavators and Hauling Equipment. The Power Crane and Shovel Association has released a 24-page bulletin dealing with the proper sizing of excavators and hauling equipment, Technical Bulletin No. 3. Rubber Conveyor Belting. "Installation, Care and Maintenance of Rubber Conveyor Belting" is the title of a booklet just published by the Carlyle Rubber Co., New York. Power Transformers. The manufacturing procedure of Allis-Chalmers small power transformers is described in a new 28-page bulletin, 61B6094A, covering the core and coil unit, no-load tap changer, tank construction, cooling methods, oil preserving systems, bushings, terminal compartments, indicators and testing of transformers. Safety Equipment. General Scientific Equipment Co., Philadelphia, has released a 46-page, fully illustrated catalog on personal protective equipment and industrial safety devices. This new catalog covers respiratory devices, eye protection, hats, gloves, carboy pumps, drum pumps, and miscellaneous safety equipment for use in mines, industries, etc. Osmosalts. The Osmose Wood Preserving Co., Buffalo, N. Y., has issued a bulletin on Osmosalts, the wood preservative which, say the manufacturers, makes timber last three to five times longer, slashes maintenace costs, stops rot, and resists wood-destroying insects. Jigs. The Dorr Co. has acquired the Pan American jigs and they are now known as the Dorrco-Pan American jigs. Originally developed as a gold-saving device for dredges, the simplicity, ease of operation. efficiency, and negligible maintenance of these jigs have resulted in wide adoption on all types of placer operations, in the closed grinding circuits of gold mills, and on many applications where a coarse bed concentrate is separated from the ore gangue.

Jan 5, 1950

By G. L. Fisher, R. Maddin

The rate of self-diffusion in silver single crystals during torsional strain was measured over a wide range of tenperatures and strain rates. The torsional strain was applied in a cyclic manner by reversing the divection of twist aftev a certain fraction of the total strain was reached. Surface roughening was substantially reduced in cyclically strained specimens compared with those strained entirely in one direction. Diffusion coefficients were determined using a special sectioning technique whereby slices could be removed parallel to the surface of a strained torsion specimen. The accuracy of the technique was first determined using roughened specinzens statically diffused to various penetration depths. Simultaneous strain-diffusion experiments were then performed over the temperature range 550' to 800 using strain rates of lo-' to 2.2 x 10' sec-'. The increase in silver self-diffusivity during torsional plastic strain was small. In only one case was the enhancement greater than twice the static value of the diffusion coefficzent. The enhancements increased slightly with decreasing tenzperature and increased with increasing strain rate. A dislocation pipe mechanism of enhancement was found to explain the present results satisfactorily. The magnitude of the enhancements and the tenzperatures at which they were observed suggests that a steady-state dislocation density of 10' to 109 dislocations cm-2 existed during the high-tempevature deformation. The diffusion coefficient in an fcc metal can be increased by 1) an excess concentration of point defects and 2) the rapid movement of diffusing atoms along grain boundaries and dislocations. Plastic deformation may be responsible for enhancements by both of these mechanisms. The results of simultaneous strain-diffusion experiments have caused a controversy over the magnitude of the effect of strain upon diffusion. Experiments reporting large enhancements have been criticized for the manner in which the diffusion coefficient was measured. Several of these experiments have been contradicted by other results obtained in a similar manner. No enhancement was reported by two investigators''' who performed their experiments at high temperatures where strain is expected to have little effect upon diffusion. A recent theoretical analysis3 indicates that strain enhancement by a vacancy mechanism will be small and exist only at low temperatures and rapid strain rates. It is doubtful whether any experiment has yet proven that strain enhancements can occur by an excess vacancy mechanism. In the present research, experiments were performed at extremes of temperature and strain rate in an attempt to measure enhancement of diffusion by strain. Self-diffusion of silver during torsional deformation was chosen since two separate investigations4j5 indicate that at least a small enhancement exists under these conditions. An accurate method of determining the diffusion coefficient, mechanical sectioning, was employed after a technique was devised to apply it to the roughened surface of a strained torsion specimen. First, the accuracy of the technique was determined for different penetrations (2fi). Then diffusion experiments were performed at temperatures between 550" and 800°C at strain rates of 10"" to 10"" per sec. I) EXPERIMENTAL PROCEDURE Preparation of Specimens. The experimental procedure detailing the growth of crystals, their treatment, and the annealing techniques during straining are contained in earlier publications.496 The dimensions and orientations of the torsion specimens are shown in Figs. 1 and 2. licatiin of Torsional Strain. The torsion procedure was changed from that used previously. The specimens were strained in cycles to reduce the gross distortion and surface roughening inherent in twisting to high strains in one direction. For all strains above 0.30, the total surface strain was obtained as follows: the specimen was twisted to 0.10 strain in a clockwise direction; the direction was reversed; the backlash in the torsion apparatus was taken up; and the specimen was twisted in a counterclockwise direction through the initial starting point to 0.20 surface shear strain in the opposite direction. The strain reversal took no more than 1 min to accomplish. The total accumulated surface shear strain was arbitrarily taken as the sum of the 0.10 strain in the clockwise direction plus 0.20 in the counterclockwise direction. Although cyclic torsional strain was beneficial, surface roughening and specimen distortion were not entirely eliminated. The variation in the diameter at various points on the specimen was often much greater than the depth of the diffusion zone. Since serious errors might result if specimens were sectioned in the usual manner, a technique of lathe sectioning was devised to allow sections to be taken parallel to planes of equal concentration.

Jan 1, 1967

A tentative plan for the Colorado Meeting has been formulated as follows: One day will be spent at Denver, one day at Colorado Springs, one day at Cripple Creek, a trip by automobile to the top of Pike's Peak, one day at Pueblo, one day at Leadville. All the principal mines and mills of the districts mentioned will be visited, including the gold mines in Cripple Creek, the lead, zinc, and steel works. of Pueblo, the production of ferro-molybdenum by electric furnace at Leadville, etc. Special arrangements are being made for the social entertainment of ladies at all points; one evening at Colorado Springs will be devoted to a reception and dance, and the usual dinner will he given on another evening. The following papers have already been accepted for the Colorado Meeting, and some have already been published: Fireproofing Mine Shafts by the Anaconda Copper Mining Co. By E. M. Norris. (March Bulletin.) Air Blasts in the Kolar Gold Field, India. By E. S. Moore. (March Bulletin.) The Use of Coal in Pulverized Form. By H. R. Collins. (April Bulletin.) Coal Mining in Washington. By F. A. Hill. (April Bulletin.) Carbocoal. By C. T. Malcolmson. (May Bulletin.) Gaging and Storage of Oil in the Mid-continent Field. By O. U. Bradley. (March Bulletin.) An Interpretation of the So-called Paraffin Dirt of the Gulf Coast Oil Fields. By A. D. Brokaw. (April Bulletin.) The Theory of Volcanic Origin of Salt Domes. By. E. DeGolyer. (May Bulletin.)

Jan 5, 1918

By W. T. Bishop, G. A. Crowe

While the literature in the United States on general polarographic technique is extensive, very little appears to be directly applicable to the analysis of flotation tailings. For this reason, it seemed worth while to present a few polarographic methods of ore analysis that have been in constant use in the laboratories of the Hercules Experiment Station for the past few years. At the time of our initial investigation of the polarographic method, there was little or no mention of its specific application to flotation tailings. It was therefore necessary for us to establish suitable conditions for the analysis of our flotation tailings and to consider possible interfering constituents. The polarograph, or dropping mercury electrode, method was discovered in 1925 by J. Heyrovsky and M. Shikata,1 of the Charles University, Prague. This method has since received extensive development and the literature contains many articles on the use of the polarograph for the quantitative determination of metals as well as anions, oxygen in solution, and reducible organic compounds. Kolthoff and Lingane,² by the publication of their book, "Polarography," in 1941 did much to advance the knowledge and use of the polarograph. In chapter 25 of that book, methods for the polarographic analysis of brass, steel and iron products, alloys, and zinc ore are given. Aluminum,³ cadmium,³,4 cobalt,4 cop-per,³-9 gold,10 iron,3,11 lead,³,l2,l³ molybdenum,14 nickel,4,8,9 tin," and zinc³,4,5,7 in ores have been analyzed by the polarograph. However, most of the work on tailing samples has been published in Russian journals and translations are not yet readily available. In this paper we will describe the method that was developed and used in our laboratory for the determination of copper, zinc, and lead in flotation tailings. Principle OF the Method The polarograph is an instrument for applying a potential to a mercury pool and a dropping mercury electrode separated by a solution, and for measuring the resultant electrical current. The procedure is essentially a small-scale electrolysis, in which the voltage required to reduce or oxidize the material identifies it qualitatively and the current measures the concentration quantitatively. Different constituents in a sample may often be determined simultaneously provided they reduce at sufficiently different voltages. An example is the determination of copper and zinc in the same solution. The reduction potentials are quite far apart, as shown in Fig. I. The polarographic method is particularly useful in the range of concentration between those normally determined by spectographic and chemical methods. In

Jan 1, 1947

By G. A. Crowe, W. T. Bishop

While the literature in the United States on general polarographic technique is extensive, very little appears to be directly applicable to the analysis of flotation tailings. For this reason, it seemed worth while to present a few polarographic methods of ore analysis that have been in constant use in the laboratories of the Hercules Experiment Station for the past few years. At the time of our initial investigation of the polarographic method, there was little or no mention of its specific application to flotation tailings. It was therefore necessary for us to establish suitable conditions for the analysis of our flotation tailings and to consider possible interfering constituents. The polarograph, or dropping mercury electrode, method was discovered in 1925 by J. Heyrovsky and M. Shikata,1 of the Charles University, Prague. This method has since received extensive development and the literature contains many articles on the use of the polarograph for the quantitative determination of metals as well as anions, oxygen in solution, and reducible organic compounds. Kolthoff and Lingane,² by the publication of their book, "Polarography," in 1941 did much to advance the knowledge and use of the polarograph. In chapter 25 of that book, methods for the polarographic analysis of brass, steel and iron products, alloys, and zinc ore are given. Aluminum,³ cadmium,³,4 cobalt,4 cop-per,³-9 gold,10 iron,3,11 lead,³,l2,l³ molybdenum,14 nickel,4,8,9 tin," and zinc³,4,5,7 in ores have been analyzed by the polarograph. However, most of the work on tailing samples has been published in Russian journals and translations are not yet readily available. In this paper we will describe the method that was developed and used in our laboratory for the determination of copper, zinc, and lead in flotation tailings. Principle OF the Method The polarograph is an instrument for applying a potential to a mercury pool and a dropping mercury electrode separated by a solution, and for measuring the resultant electrical current. The procedure is essentially a small-scale electrolysis, in which the voltage required to reduce or oxidize the material identifies it qualitatively and the current measures the concentration quantitatively. Different constituents in a sample may often be determined simultaneously provided they reduce at sufficiently different voltages. An example is the determination of copper and zinc in the same solution. The reduction potentials are quite far apart, as shown in Fig. I. The polarographic method is particularly useful in the range of concentration between those normally determined by spectographic and chemical methods. In

Jan 1, 1947

By P. Chaudhari, Michael B. Bever

The heat of solution at infinite dilution of selenium in bismuth, the heat of mixing of selenium and bismuth, and the limit of solubility of selenium in bis~rzuth have been determined at 573, 623; and 663°K by metal solution calorimetry. The heat of forrrzation of the compound Bi2Se at these temperatures has been determined from the heat effects associated with the precipitation of the compound from a saturated solution oj selenium and bismuth. The published information on the thermodynamic properties of the system Bi-Se is limited. The heat of solution at infinite dilution of selenium in bismuth at 623°K has been measured.' The heat of formation at 273 K1 and room temperature2 and the heat capacity at 80 K3 of the compound Bi2Se3 have been reported. An estimate of the heat of formation of the compound BiSe at room temperature has been published.2 Information on the phase relations in the system Bi-Se is available.' In the investigation reported here the following quantities have been determined at 573", 623", and 663°K: 1) the heat of solution at infinite dilution of selenium in bismuth, 2) the heat of mixing of selenium and bismuth in bismuth-rich solutions, 3) the limit of solubility of selenium in bismuth, and 4) the heat of formation of the compound BizSe. These quantities were determined by the addition of selenium to bismuth-rich solutions in a metal solution calorimeter. The determination of the heat of formation at the tem- perature of the calorimeter bath involved the precipitation of the compound from a saturated solution in the calorimeter. 5,6 This method differs from that commonly used which requires the addition of the compound and of a mechanical mixture of its components and yields the heat of formation at the temperature from which the additions are made (273 K EXPERIMENTAL PROCEDURE AND CALCULATIONS The solution calorimeter has been described in detail.' Pure bismuth (99.999+ pct) was used as the bath at the start of a run. The calorimeter was calibrated with small amounts of bismuth added from 273°K; the differences of the heat contents of bismuth at 273°K and the temperatures of the baths are listed in Table I. After the calibration, additions of hexagonal selenium (99.999+ pct) were made. Loss of selenium by evaporation was negligible. No unusual experimental difficulties were encountered.9 The differences in the heat contents10 of selenium at 273°K and the temperature of the bath, listed in Table I, were subtracted from the measured heat effects to give the "adjusted heat effects". The methods by which the heat of solution at infinite dilution, the

Jan 1, 1968

By O. Chanute

all of' level atid grade curve excepting Nos. 897, 898, 899, and 900, because of the impossibility of grouping them in the same nlonner, no two Iraving the chemical composition and physical prnprtiw as tho only v:iriubles. Phosphorus ~tnits have been taken to show the relatia h:wdnes. Of these 16 groups, 10 decidedly indicate slower wear firr tile harder rail. Of the remaining 6 groups, three (groups 2, 9, and 15) come well within the limits of error (.25 pound per yard) inherent in the palculation of the data as pointed out by Dr. Dndley; they catrnot, therefore, be considered tls exceptions. Group 2 and 15 arc but little outside of the limita of error. Rail 923 of group 9 is obviously abnornlal. This is probahly due to its being overheated, which the chemical analysis shows might easily be the case, and which the physical tc~ts and its low specific gravity tend to c-nfirm. We inry say, then, thnt 13 of these 16 groups fairly indicate, if they do not definitely point out, th:kt, under the same condition% tbe harder rail gives the slower wear. Of course, these comparisons are too few to enable us to arrive at positive ~?o-nclusions; but indications thus obtained are, I believe, fir more vsluitblc and tresttvc~rthy than those fhzt averages rvottld give us, mnde up from any ~lumhr of rails under intloy difi~rcal, conditions. Finally, it, seems to me, that the conclusions arrived at earlier in my remarks, together with, and confirmed by the last, show strong evidence that, under the same conditions, the harder rail will givc the slower wear. 0. C~~anute, New York CITY: We are very much shlipl, 1 ant sure, to Mr. Sandberg for his paper upn " Rail Ryaifications and Rail Inspertion in Europe." We have in thp United States bithhrto Been inspecting mils sonlewl~at haphazard, and we ore glad to gtbt tfie results of Mr. Sandberg's long experience. We recognize that he was an)ong the first, if not the very firwt, to iipply mare rittional and scientific rules to the designing of irou rails., niora recently, to adapt tlitve rules to the clesigtting of steel I':I~]R, to conform to the oapaljilities and rqniretnento of this new n1:ttcrial. Although we have generally adopted, in this country, sectinns for hteel rails which marly of our railway men think even bottar than those of Mr. Snlldlmrg, he is neverthelees the Ieat3er in foot.iito11~ we have followed ever since it has been est~blished

Jan 1, 1881

Jan 7, 1976

By E. F. Reed

CONSIDERABLE deep hole prospect drilling has been done in the last few years in the Globe-Miami mining district about 70 miles east of Phoenix, Arizona, and in the San Manuel-Tiger area about 50 miles south of the Globe-Miami region. More than 205,000 ft of churn drilling have been completed by the San Manuel Copper Corp. at their property in the Old Hat Mining District in southern Pinal County. The deepest hole on this property is 2850 ft; there are 49 holes deeper than 2000 ft. At the adjoining Houghton property of the Anaconda Copper Mining Co., where only one hole reached 2000-ft depth, there were 27,472 ft of churn drilling and 3436 ft of diamond drilling. Three churn drill holes were deepened by diamond drilling methods. Near Miami in the Globe-Miami district the Amico Mining Corp. drilled four holes by combined churn and rotary drilling methods, the total amounting to 13,879 ft, of which 2256 ft were drilled with a portable rotary rig. In the same district, besides doing a large amount of shallow prospect drilling, the Miami Copper Co. drilled two holes of 2560 and 3787 ft, respectively, which were completed by churn drilling methods. The rocks encountered in drilling at San Manuel and Tiger are described by Steele and Rubly in their paper on the San Manuel Prospect' and by Chapman in a report on the San Manuel Copper Deposit.' The rocks are well-consolidated Gila conglomerate, quartz monzonite, and monzonite porphyry. In some places these formations stand very well while being drilled, and three holes were drilled without casing, the deepest of which was 2200 ft. In other holes faulted and fractured ground made drilling difficult. In the Globe-Miami district the deep drilling was done in the down-faulted block of Gila conglomerate east of the Miami fault and in the underlying Pinal schist. The geology of this area is described by Rannome. In the Amico holes the conglomerate varied from material consisting entirely of granite boulders and fragments to a rock made up of schist fragments in a sandy matrix; in the Miami Copper Co. holes there were more granite boulders and the material was poorly consolidated. Drilling was much more difficult and expensive in the Miami area than in the San Manuel district, mainly because of the depth of the holes and the formations drilled. All the deep hole prospecting described in this paper was done with portable rigs. The churn drill rigs were of several types, of which the Bucyrus-Erie were the most popular. Bucyrus-Erie 28L, 29W, and 36L rigs were used on some of the deeper holes on the San Manuel property. A few Fort Worth spudder types were tried, and the deepest hole at San Manuel was drilled with a Fort Worth Jumbo H. The spudder type is considerably larger than most other rigs used on this work and required a larger location site. The spudders were belt-driven machines with separate power units, and time required for setting up and moving was much longer than with the more portable drills. All the churn drilling was done by contractors or with machinery leased from them. A few of the contractors had complete equipment, including most of the necessary fishing tools. Unusual and special fishing tools were obtainable from the supply companies in the oil fields of New Mexico or in the Los Angeles area. Most of the contractors used equipment with standard API tool joints, so that much of it was interchangeable. Failure of tool joints is one of the principal causes of fishing jobs. It can be minimized if the joints are kept to the API specifications and the proper sized joints are used in the various holes. The minimum sizes that should be used with various bits are as follows: 12-in. and larger bits, 4x5-in. tool joints; 10-in. bits, 31/4x41/4-in. tool joints; 8-in. bits, 23/4x 33/4-in. tool joints; 6-in. bits, 2Y4x3Y4-in. tool joints; 4-in. bits, 15/ix25/8-in. tool joints. Two rotary drill rigs were tried at San Manuel on the same hole, and a portable rotary drill rig was used on the Amico drilling for test coring the formation and for drilling in holes 3 and 4. Rotary drilling differs from churn drilling or cable tool drilling in that the bit is revolved by a string of drill pipe and the cuttings are removed from the hole by a thin solution of mud pumped through the drill pipe. The principal parts of a rotary rig are the power unit, a rotating table to revolve the drill pipe, hoists to raise and lower the pipe and to handle casing, and a pumping system to circulate the drilling liquid. The rig used on the Amico property at Miami was mounted on a truck. The larger rig used on the San Manuel property was hauled by several trucks and had separate turntable and pumping units. Diamond drill coring equipment was used successfully with the rotary rig in the holes on the Amico property. To allow for 23/8-in. drill pipe with tool joints, 31h-in. core barrels and bits were used. With the standard 31h-in. core barrel there was considerable difficulty in maintaining circulation with mud, so a barrel was designed with a smaller inner tube and a broad-faced bit. This allowed coarser material to circulate between the barrels. Rock bits of 55/8 to 3 in. were used with the rotary rig for drilling between core runs. Diamond drill equipment is much lighter than churn drill tools, so that fishing tools can usually be obtained from supply houses by air express when needed. Three churn drill holes on the Houghton property at Tiger were deepened by diamond drilling with Longyear UG Straitline gasoline-driven machines. The open churn drill hole was cased with 21h-in. black pipe. In deep hole churn drilling, casing is one of the most important items, especially in drilling in un-consolidated material like the formations drilled by

Jan 1, 1953

By E. F. Reed

CONSIDERABLE deep hole prospect drilling has been done in the last few years in the Globe-Miami mining district about 70 miles east of Phoenix, Arizona, and in the San Manuel-Tiger area about 50 miles south of the Globe-Miami region. More than 205,000 ft of churn drilling have been completed by the San Manuel Copper Corp. at their property in the Old Hat Mining District in southern Pinal County. The deepest hole on this property is 2850 ft; there are 49 holes deeper than 2000 ft. At the adjoining Houghton property of the Anaconda Copper Mining Co., where only one hole reached 2000-ft depth, there were 27,472 ft of churn drilling and 3436 ft of diamond drilling. Three churn drill holes were deepened by diamond drilling methods. Near Miami in the Globe-Miami district the Amico Mining Corp. drilled four holes by combined churn and rotary drilling methods, the total amounting to 13,879 ft, of which 2256 ft were drilled with a portable rotary rig. In the same district, besides doing a large amount of shallow prospect drilling, the Miami Copper Co. drilled two holes of 2560 and 3787 ft, respectively, which were completed by churn drilling methods. The rocks encountered in drilling at San Manuel and Tiger are described by Steele and Rubly in their paper on the San Manuel Prospect' and by Chapman in a report on the San Manuel Copper Deposit.' The rocks are well-consolidated Gila conglomerate, quartz monzonite, and monzonite porphyry. In some places these formations stand very well while being drilled, and three holes were drilled without casing, the deepest of which was 2200 ft. In other holes faulted and fractured ground made drilling difficult. In the Globe-Miami district the deep drilling was done in the down-faulted block of Gila conglomerate east of the Miami fault and in the underlying Pinal schist. The geology of this area is described by Rannome. In the Amico holes the conglomerate varied from material consisting entirely of granite boulders and fragments to a rock made up of schist fragments in a sandy matrix; in the Miami Copper Co. holes there were more granite boulders and the material was poorly consolidated. Drilling was much more difficult and expensive in the Miami area than in the San Manuel district, mainly because of the depth of the holes and the formations drilled. All the deep hole prospecting described in this paper was done with portable rigs. The churn drill rigs were of several types, of which the Bucyrus-Erie were the most popular. Bucyrus-Erie 28L, 29W, and 36L rigs were used on some of the deeper holes on the San Manuel property. A few Fort Worth spudder types were tried, and the deepest hole at San Manuel was drilled with a Fort Worth Jumbo H. The spudder type is considerably larger than most other rigs used on this work and required a larger location site. The spudders were belt-driven machines with separate power units, and time required for setting up and moving was much longer than with the more portable drills. All the churn drilling was done by contractors or with machinery leased from them. A few of the contractors had complete equipment, including most of the necessary fishing tools. Unusual and special fishing tools were obtainable from the supply companies in the oil fields of New Mexico or in the Los Angeles area. Most of the contractors used equipment with standard API tool joints, so that much of it was interchangeable. Failure of tool joints is one of the principal causes of fishing jobs. It can be minimized if the joints are kept to the API specifications and the proper sized joints are used in the various holes. The minimum sizes that should be used with various bits are as follows: 12-in. and larger bits, 4x5-in. tool joints; 10-in. bits, 31/4x41/4-in. tool joints; 8-in. bits, 23/4x 33/4-in. tool joints; 6-in. bits, 2Y4x3Y4-in. tool joints; 4-in. bits, 15/ix25/8-in. tool joints. Two rotary drill rigs were tried at San Manuel on the same hole, and a portable rotary drill rig was used on the Amico drilling for test coring the formation and for drilling in holes 3 and 4. Rotary drilling differs from churn drilling or cable tool drilling in that the bit is revolved by a string of drill pipe and the cuttings are removed from the hole by a thin solution of mud pumped through the drill pipe. The principal parts of a rotary rig are the power unit, a rotating table to revolve the drill pipe, hoists to raise and lower the pipe and to handle casing, and a pumping system to circulate the drilling liquid. The rig used on the Amico property at Miami was mounted on a truck. The larger rig used on the San Manuel property was hauled by several trucks and had separate turntable and pumping units. Diamond drill coring equipment was used successfully with the rotary rig in the holes on the Amico property. To allow for 23/8-in. drill pipe with tool joints, 31h-in. core barrels and bits were used. With the standard 31h-in. core barrel there was considerable difficulty in maintaining circulation with mud, so a barrel was designed with a smaller inner tube and a broad-faced bit. This allowed coarser material to circulate between the barrels. Rock bits of 55/8 to 3 in. were used with the rotary rig for drilling between core runs. Diamond drill equipment is much lighter than churn drill tools, so that fishing tools can usually be obtained from supply houses by air express when needed. Three churn drill holes on the Houghton property at Tiger were deepened by diamond drilling with Longyear UG Straitline gasoline-driven machines. The open churn drill hole was cased with 21h-in. black pipe. In deep hole churn drilling, casing is one of the most important items, especially in drilling in un-consolidated material like the formations drilled by

Jan 1, 1953

The entire War Minerals Relief Commission heard the case of the Chas. T. Pyrites & Chemical Company of Georgia on April 15 and 16. The Commission insisted on great detail with regard to the entire enterprise, although the main questions seemed to be of the amount involved. It is considered by the Commission that this claim comes unquestionably under the Act, it is one of the best examples that has been brought to the attention of the Government thus far. Testimony showed that operations were done on the property late in 1916 without request from the Government. Preparations were made to work the pyrites deposit on a comparatively small scale but , following a visit from a representative of the Secretary of Interior and a personal interview of the principal owner of the property and Secretary Lane, operations on a much larger scale were begun. The amounts expended prior to this interview were carefully separated from the expenditures thereafter. Testimony showed that it was the intention of the owners to transport their product by motor truck to the railroad-13 mi. away. This limited shipments to about 50 tons daily. Under the enlarged plan taken against the better business judgment of the owners, a railroad spur at a cost f nearly $200,000 was built to the mine. The operation included a concentrating mill with a capacity f 600 tons daily and an expensive dam to make possible the use of waterpower. With these improvements, the company was just beginning, operation under its enlarged program when the armistice was signed. This resulted in a greatly decreased demand and consequently lower prices, with all prospects indicating that the property could not operate profitably when Spanish pyrites begin to move.

Jan 6, 1919