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By N. J. Grant, D. Carne, J. B. Seabrook

IT is unnecessary to review much of the literature on hydrogen embrittlement of steel since several excellent reviews and bibliographies exist.1-3 Hot acid pickling and cathodic charging have been known to cause hydrogen embrittlement of steel and have been used as laboratory methods to charge steels with hydrogen.4-8 Experimental Procedure The problem of prime concern in all instances, except in the work of Sims and coworkers,10 is that at no time was there a definite known hydrogen value reported which could be related to a particular value of the degree of embrittlement. It was the purpose of this research to determine the relationship between hydrogen content and degree of em-brittlement quantitatively. The 1020 stock used for the specimens was hot-rolled 7/16 in. diam rod of the following analysis: 0.19 pct C, 0.40 pct Mn, 0.012 pct P, 0.036 pct S' Vacuum-fusion analyses for nitrogen and oxygen gave 0.014 pct O2 and 0.0011 pct N2. Cathodic charging was used to cause embrittle-ment. The advantages of this method were that no quenching was necessary, the impregnation was reasonably controllable, and representative samples for analysis could be prepared simultaneously with the charging of the tensile bars. Analyses for hydrogen were made in a vacuum-fusion type of apparatus which extracted gas from the samples by fusion in a molten tin-iron bath' This apparatus, which has recently been described in detail elsewhere, will not be discussed here.". " Consecutive samples can be analyzed every 15 min with an accuracy of 0'03 ppm. A A from an electrolytic or pickling bath can be charged for analysis in about 3 min, and analysis completed in 15 min. Samples of as-received 1020 stock were analyzed and found to contain a negligible amount of hydrogen (0.06 ppm). Preliminary pickling and electrolytic charging gave highly variable results. Cold-worked samples showed higher values but ranged from 0.6 to 6.0 ppm of hydrogen. Charging at 90°C gave higher values of charged hydrogen, but troublesome films on many of the specimens resulted. It was not until a few drops of a catalytic poison, prepared from 2 g of yellow phosphorus dissolved in 40 ml of carbon disulphide,8 was added to the electrolytic cell that fairly consistent high values of hydrogen could be charged into the as-received 1020 steel at room temperature. The cell used is sketched in fig. 1. The anode and fixture for the tensile specimens were fastened to the cell cover as shown, and the specimen was screwed in place, centrally located with respect to the anode. At first, anodes of lead and graphite were tried, but they contaminated the electrolyte and gave a slight deposit on the specimen. Later, a platinum wire was used in the form of a uniform helix. A current of 2 amp, corresponding to about 0.5 amp per sq in. of cathode, was used for most specimens. The electrolyte was 4 pct H2SO4 solution. Fig. 1 shows the form of the special tensile bar, the main portion of which was an ordinary 1/4 in. diam, 1 in. gauge length test bar, except that two to four small cylinders of stock were left attached by small links to the bottom end of the tensile bar for the purpose of providing samples for hydrogen analysis. Thus the bars and samples were charged with hydrogen simultaneously and an analysis could be made while the bar was being tested mechanically. Experiments were performed to determine how representative the test cylinders were of the middle of the test bar proper. While the bar center was being analyzed, the small cylinder was stored in dry ice, since it had been shown that such storage prevents loss of hydrogen for many hours.12 The results of these checks are shown in table 1. The checks are very good (0.3 ppm) and indicate that it is permissible to use the small end cylinders to establish the hydrogen content of the tensile test bar proper-

Jan 1, 1951

The members of the Institute have probably seen in the daily papers notices of the plans of the Secretary of the Navy to. form an Advisory Board to assist the Government to make available the latest inventive genius of the country. Secretary Daniels has appointed Mr. Thomas A. Edison Chairman of this Advisory Board and has officially invited the Institute to secure the selection of two of its members to serve. on this Board. The Secretary in his letter states: "I feel that the work your Institute has done has been such as to give it the right to be in a way officially represented, and the Navy Department desires in this way to testify to its own appreciation of the splendid work for our country that your Institute has done. I have the emphatic approval of Mr. Edison, and he agrees entirely with me that your Institute should he represented in this way and that no better method of getting the kind of men we need could be devised." The invitation of the Secretary of the Navy has been officially accepted and steps have been taken to nominate the two members. Since the Constitution provides for no meeting of the Board of Directors until September, and as Secretary Daniels urged early action, the matter was discussed at a special meeting of the Executive Committee of the Institute, at which were present as many members of the Board of Directors as were in New York City at the time. Invitations were also extended to other members of the Institute who happened to be in the vicinity. At this meeting it was decided to submit the matter by a special letter-ballot to the Board of Directors and in doing so to suggest or nominate five members of the Institute, accompanying this nomination with the statement that the Directors might vote for two of the members so nominated or for any other members of the Institute not so nominated. It was voted at this meeting that it. was the sense of those present that in view of the fact that this committee was an advisory one the type of men to be chosen should be men of administrative or executive ability, cap-

Jan 9, 1915

A rotary chambered blasthole technique has initially indicated a 30% overall improvement in drill and blast department productivity. The method, developed at several open pit copper mines in Arizona, centers around a chambering tool that can be used with existing high-speed rotary drills. The "Chamber Maker," manufactured by the Servco Div. of Smith International, Inc., produces an enlarged section or chamber near the bottom of a large diameter blasthole (Fig. 1). This enlarged cavity permits a greater concentration of explosives at the bottom of the blasthole, resulting in better fragmentation and reduced hard toe problems, and also lowers the number of blastholes required to break a bench area, says Servco's Gerald W. Laswell. Cost savings can therefore be achieved in reduced secondary blasting requirements, increased shovel efficiency, and subsequently, less shovel maintenance. All these factors would serve to lower the overall mine cost per ton figure

Jan 3, 1975

By Oren C. Baptist, Carlon S. Land

Laboratory research has been conducted to evaluute the effect of clay hydration on the permeability to gas of water-sensitive reservoir sands. Samples of a .sandstone containing trace amounts of montmorillonite and a sample of montmorillonite were .studied in the laboratory to detertnine whether swelling or dispersion was the cause of permeability reduction in these samples. Heliuin, containing various amounts of water vapor, was used to hydrate the clay minerals and to determine the gas permeability at various stages of clay hydration. The amount of water adsorbed by the samples using this method is small. The nonwetting-phase permeability at higher water saturations war investigated by saturating the with water and measuring the permeability to humid helium while decreasing the water saturation, Relative-permeability curves obtained from results of these procedures were used to estimate the effect of the swelling of trace amounts of mont/tlorillonite on the permeability of the .samples. Most of the damage to the permeability when reservoir sands containing trace amounts of montmorillonite are exposed to fresh water is due to dispersion and movement of clays. Blockage of pores by the increased volume of expanded montmorillonite is believed to result in permeability damage that is small in comparison to the observed damage to the samples tested. INTRODUCTION Studies have shown that permeability is severely damaged when sands containing only small amounts of montmorillonite are contacted by fresh water.15 When samples of sands containing large amounts of montmorillonite are placed in fresh water in the laboratory, these samples may completely disintegrate, forming an unconsolidated mass of larger volume than that occupied by the dry sample." In this case, it is apparent that the swelling of montmoril-lonite has destroyed the pore structure of the sand. If only a trace of montmorillonite is present in a sand. samples may remain intact when saturated with water, although the permeability to water is a small fraction of the gas permeability of the dry sample. Many workers in the field of water sensitivity have attributed this reduction in permeability to the blocking of pores and reduction of pore size by the increased volume occupied by expanded mont- niorillonite. if the sand contains a detectable amount of montmorill'onite or mixed-layer clay containing rnontmorillonite. Logically3 the smaller amount of montmorillonite present in a sand, the smaller should he the effect of montnlorillonite swelling on permeability; however, the quantity of montmorillonite sufficient to cause severe damage by swelling is not known. Although hundreds of samples have been tested in our laboratory, no correlation has been established between the amount of montmorillonite in samples and the permeability reduction caused by fresh water. To many petroleum engineers, the phrase "clay swelling" is synonymous with "water sensitivity", or "permeability reduction" implying that any formation damage due to the hydration of clays is caused by swelling. Although all clays adsorb water on their surfaces, montmorillonite is the only clay mineral commonly found in reservoir rocks which adsorbs water between intercrystalline layers, resulting in expansion of the clay particle. As montmoril-lonite swells, the first few layers of water adsorbed between platelets are strongly held and well oriented, and the montmorillonite retains its crystalline structure, although expanded. As swelling of sodium montmorillonite continues, the platelets become farther apart and the forces orienting the platelets in the crystalline structure become weaker, resulting in a less orderly orientation of platelets. In an abundance of water, small groups of platelets may become detached from the original monl-rnorillonite particle and may be dispersed throughout the water phase. Because of its swelling properties, sodium montmorillonite is very easily dispersed in water. Particles of other clay minerals. such as illite and kaolinite may also be dispersed in water. causing water sensitivity of sands not containing montmorillonite. The presence of an immobile layer of water adsorbed on the surface of clays has been considered a possible cause of the low permeability to water of dirty sands. Grim states that the thickness of the layer of immobile water held by sodium montrnorillonite is three nlolecular layers or 7.5 A (angstroms), with some orientation of water extending to 100 A. Assuming a very thick, immobile water layer adsorbed on the surface of a pore represented by a capillary tube, the maximum effect of the water layer on permeability can be calculated. Using a pore radius of 10 ' cm and an immobile water layer of 50 A. the calculation shows the permeability to be reduced only 2 per cent. Similar calculations can be used to show that the effect of electro-osmotic counterflow is of the same order of magnitude as that of bound water. The reduction of the permeability to water by either an immobile water layer

Jan 1, 1966

By M. Van Siclen

THE outstanding fact in connection with dust disease in the United States at present is the growing recognition of its seriousness by state officials and by the more progressive operators of mining, metallurgical and allied industrial plants. The same may perhaps be said of labor in some of its better organized centers, but the average independent non-union workman continues, .as of yore, to suffer the toll of disability and even of death from dust inhalation without realization of the source of his ill-being. Progress in the betterment of the handling of sufferers from dust disease and of the conditions creating dust hazards in mining and allied industries is pursuing a course similar to that of the now widespread campaign against accidents, in which the risk is more obvious, more severe, and was naturally recognized sooner. The coming on of dust disease is generally relatively slow and its immediate effects not infre-quently masked by or attributed to other diseases. Marked exceptions to this general rule have occurred in districts where the dust is particularly pernicious, such as the Rand and Joplin; yet such exceptions, unhappy in themselves, opened the eyes of medical men, and of those in other localities charged with the responsibility for the welfare of industry, to the much more widespread if less spectacular hazard existing from the inhalation of dust in all rock-excavating operations and all industrial operations creating inorganic dust, whether it be crushing and grinding, sand-blast-ing, granite-cutting, or what not. Advancement to date in the United States in prevention and treat-ment has been slow, yet the record shows that quantitative methods for determining the degree of hazard and means for decreasing it were being developed as far back as 25 years ago; and that more rapid progress may be looked for from now on. In 1908, in this country; F. L Hoffman?(1) discussed the mortality from consumption in dusty trades, especially brass foundries; and in 1913 E. R. Hayhurst(2) described the effects of inhalation

Jan 1, 1933

THE morning session on non-metallic minerals was opened briefly by the chairman, Oliver Bowles, giving the usual instructions and then turning immediately to the introduction of the speakers. "Min-ing and Preparation of the St. Peter Sandstone in' Arkansas" by D. D. Dunkin was first presented by W. M. Weigel, mining technologist for the Missouri Pacific R. R. The paper covered a discussion of the geology of the sandstone, correlating it with the sand-stones at Klondike, Mo., and at Ottawa, III. Its physical appearance, structural characteristics and thickness; the mining methods, blasting, loading, haulage and classification were taken up. A series of slides aided in clarifying the details. The discussion consisted of questioning Mr. Weigel on operating details. The second paper, "Geology and Mining of Diaspore and Flint Fire-Clays of Missouri," written by H. S. McQueen, geologist with the Missouri Bureau of Geology and Mines, and C. R. Forbes, professor of mining, Missouri School of Mines and Metallurgy, was presented by Mr. Forbes. It thoroughly covered the geology, stressing the peculiar sink formations in which all diaspore clay deposits of the region occur. The crudeness of the mining methods was mentioned and believed justifiable because of the small size of the indi-vidual deposits. It was stated that the diaspore and flint clay deposits of Missouri were confined to an area 60 mi. square and it was found in a survey that the average deposit had dimensions comparable to the fol-lowing: 100 ft. long, 75 ft. wide and 50 ft. deep. The largest deposit found was 800 ft. long. 500 ft. wide and 20 ft. deep. It is estimated that the known reserve of clays is from 750.000 to 1,500,000 tons. Mr. Forbes stressed the fact that in mining clays the major problem is entirely one of sorting. This is done under the supervision of a pit foreman trained to make this classification by eye. The mine-run clays are sepa-rated into diaspore clay ranging in alumina content from 70 to about 85 per cent, first grade Burly clay 00 to 70 per cent, and Flint clay 52 to 60 per cent. Discussion of the paper consisted in questioning Pro-fessor Forbes on labor. cost, haulage, drilling, and geology.

Jan 3, 1928

By N. J. Grant, E. Gregory

The creep rupture properties of wrought aluminum powder products made from five grades of sintered aluminum powder were investigated at temperatures from 400° to 900°F for rupture times up to 1000 hr. The effect of stress concentrations on materials of this type was investigated by means of notched creep rupture tests. A tentative correlation was obtained between the creep rupture properties and the structure as revealed by electron micrographs. SEVERAL papers have been published recently concerning the production and properties of wrought aluminum powder products and their possible high temperature applications. Most of the published work in this field has come from abroad, notably Switzerland, and articles by Irmann and his colleagues were summarized in English recently.'.' Most of the papers published by Dr. Irmann are principally concerned with the retention of properties (by a product which is produced from extremely fine flake powder and is subsequently hot extruded) after heating to high temperature for prolonged times. The powder may be in atomized or flake form, and during hot working the applied pressure is reported to plastically deform the aluminum powder, thus breaking the oxide skin and welding the particles together. Irmann attributes the remarkable properties to the dispersion of oxide inclusions. Specifically, the product described by Irmann is one labeled SAP (Sintered Aluminum Powder) in which the initial flake powder is so fine that at least 50 pct of the flakes have one dimension of 2 microns or less. The composition of the starting aluminum shows in percent, Fe, 0.18; Si, 0.19; Zn, 0.06; Ti, 0.03; Cu, Mn, Mg, all nil; balance Al, approximately 99.5 pct. Aluminum is not the only material that has been found to have increased resistance to deformation at elevated temperatures when produced by powder metallurgy. It has been reported by Middleton, Pf eil, and Rhodes- hat platinum has a higher recrys-tallization temperature when produced by powder metallurgy and exhibits peculiar properties, many of which are similar to those of the aluminum powder products. Difficulties were encountered in explaining the reason for the strengthening in the case of platinum since the existence of the oxide is doubtful. The authors attributed the special properties to "a small amount of suitably dispersed porosity." This theory was supported by von -~eer-leder4 in the discussion to the paper, and the similarity between this method of hardening and that suggested by Rohner in his theory of age hardening was pointed out. R. de Fleury5 attempted to explain some of the properties in terms of the modulus of elasticity and elastic limit of alumina and aluminum while von Zeerleder examined the relationship between the yield strength and the reciprocal of the powder particle size. Boenisch and WiderholtQ dealt mainly with the corrosion resistance of the powder aluminum material and compared it with other aluminum alloys. The diffusion rates of other metals in SAP and pure aluminum have been compared by Seith and Lop-mann.' They showed that the alloying metals diffuse particularly quickly in SAP possibly due to the very fine grain size. The properties of the Alcoa products were given by Lyle.' The creep rupture properties of SAP and two of the Alcoa experimental powder products were compared by Gregory and Grant hnd it was shown that these products are vastly stronger at 900°F than are the best cast and wrought alloys at 600°F. Since the publication of these data, the authors have investigated two further aluminum powder products and it is the object of this paper to show how the high temperature creep rupture properties of the five materials vary with oxide content and with the structure as revealed by electron microscopy. Materials One of the five products, SAP, a sintered aluminum product, was supplied by the Societe Anonyme pourl Industrie de l,Aluminium, Neuhausen a/RHF, Switzerland, through Dr. R. Irmann, while the others, M276, M257, M293, and M255 were supplied by the Aluminum Company of America as experimental powder metallurgical products. M255- and M293 were made from coarse and fine atomized powders, respectively. The other materials were made from flake powders with significant differences in oxide content, the details of the type of powders used in the manufacture of these materials

Jan 1, 1955

By James E. Lawver, James L. Wright

This paper describes the design of a cell used to measure the electrical conductivity, or the reciprocal resistivity, of granular materials. It also establishes a quantitative relationship between the electrical conductivity and the electrical separation of selected mineral samples. It is estimated' that the free world produces about 13 million tons of mineral concentrates a year by electrostatic or electrodynamic methods. At least 95% of these concentrates are produced by corona discharge type machines that separate minerals by exploiting the differences in their electrical conductivity. But, what is meant by the electrical conductivity of a mineral? How large a difference in the electrical conductivity of two mineral species is necessary to effect a separation? Just what is the role of conductivity in electrical separations with regard to capacity and selectivity? There is a considerable amount of information in the literature on both the mechanisms of conduction and the values of the electrical conductivity of pure single-crystal mineral specimens. In addition, some insight into the role of mineral conductivity can be obtained by referring to a Bureau of Mines publication' in which 95 minerals have been grouped as conductors or insulators as a function of temperature. The classification was made on the basis of the percent of weight that reported as "conductors" in an electrical separator. But, as is often the case in the mineral industry, practical application leads theory — and there is little useful information in the literature giving any kind of quantitative relationship between electrical conductivity and electrical separations. The problem is a bit complex because electrical conductivity per se — which can be rather easily measured on large, single grains — is not sufficiently informative to permit quantitative predictions of the separability of the mineral system. Practical "high-tension"* separations are made at such feed rates that the band of minerals on the rotor is multilayered in thickness. Thus, the effective conductivities of minerals as seen by a high-tension machine include particle-to-particle contact resistance, which is often a controlling factor in making a separation. This is particularly true when the mineral grains are coated with slime or with a dielectric surface film. From a high-tension separation viewpoint, one is actually concerned with the time required for corona-charged grains to lose enough charge so that the centrifugal force acting on the particles exceeds the image force holding the grains to the rotor. This calculation requires a knowledge of the effective mineral conductivity s. (The conductivity of the metal rotor is sufficiently greater than that of the minerals so that it need not be considered in charge decay calculations.) The charge density at time t can be approximated by the relaxation equation.3 where t 5 charge density at time t r, - charge density when t = 0 cr e total electrical conductivity £ = permittivity The time required for the charge density to fall to l/e of its initial value is called the relaxation time and is numerically equal to €/n. AS defined here, u is the conductivity of an element of homogeneous grains making contact with each other and with a grounded rotor. This paper deals with the design of a conductivity cell used to measure a, or its reciprocal p, the electrical resistivity. CELL DESIGN Initial test work was performed with a cell recommended by ASTM.4 Since the reproducibility with the ASTM cell was not satisfactory, it was decided to

Jan 1, 1970

By Riki Kobayashi, D. L. Katz

The conditions at which methane and water form solid hydrates have been extended from 4,000 to 11,200 pounds per sq. in. The curve at high pressure had been in doubt because of Villard's report of a critical decomposition temperature. The paper explains the nature of the hydrate curve at high pressure and its dependence on fluid phase behavior. Extropolation of the methane hydrate curve indicates a pressure of 40,000 pounds per sq. in. will cause hydrates to form at a temperature of 100" F. INTRODUCTION The conditions under which natural gases form hydrates when liquid water is present have been studied by several investigators up to pressures of about 4,000 pounds per sq. in. The early work by Villard on hydrates of methane and ethylene13, ethane'', and propane14 included references to critical decomposition temperatures of the hydrates. Villard's work raised the question as to whether the pressure-temperature curve for methane-water hydrate continued above a temperature of 70.7°F. or whether this was the maximum temperature at which hydrates would form. This paper extends the experimental data on methane hydrate to 11,200 pounds per sq. in. A discussion of phase relations in the hydrate region for the hydrocarbons and of the methane-water system at high pressures is included. PREVIOUS WORK Villard suspected that methane hydrates could not be formed at temperatures above 21.5°C. (70.7°F.)la irrespective of the pressure of the liquid-vapor system. However, he was limited in his studies by his apparatus in 1888 to pressures not greater than 300 atmospheres (4,410 pounds per sq. in.) so that there has remained some doubt as to the existence of such a maximum temperature in this region. For the case of ethylene hydrates, however, Villard does specifically state the occurrence of what he terms a "critical temperature for the decomposition of the hydrates"13. Fig. lB shows a pressure-temperature projection of the three-phase locus, hydrate-ethylene rich liquid-vapor (H-L2-V) terminating at the critical locus in which L² and V assume similar properties. Throughout this paper the following phase designations will be used: H for hydrate, Ll for the water rich liquid. L2 for the

Jan 1, 1949

By Riki Kobayashi, D. L. Katz

The conditions at which methane and water form solid hydrates have been extended from 4,000 to 11,200 pounds per sq. in. The curve at high pressure had been in doubt because of Villard's report of a critical decomposition temperature. The paper explains the nature of the hydrate curve at high pressure and its dependence on fluid phase behavior. Extropolation of the methane hydrate curve indicates a pressure of 40,000 pounds per sq. in. will cause hydrates to form at a temperature of 100" F. INTRODUCTION The conditions under which natural gases form hydrates when liquid water is present have been studied by several investigators up to pressures of about 4,000 pounds per sq. in. The early work by Villard on hydrates of methane and ethylene13, ethane'', and propane14 included references to critical decomposition temperatures of the hydrates. Villard's work raised the question as to whether the pressure-temperature curve for methane-water hydrate continued above a temperature of 70.7°F. or whether this was the maximum temperature at which hydrates would form. This paper extends the experimental data on methane hydrate to 11,200 pounds per sq. in. A discussion of phase relations in the hydrate region for the hydrocarbons and of the methane-water system at high pressures is included. PREVIOUS WORK Villard suspected that methane hydrates could not be formed at temperatures above 21.5°C. (70.7°F.)la irrespective of the pressure of the liquid-vapor system. However, he was limited in his studies by his apparatus in 1888 to pressures not greater than 300 atmospheres (4,410 pounds per sq. in.) so that there has remained some doubt as to the existence of such a maximum temperature in this region. For the case of ethylene hydrates, however, Villard does specifically state the occurrence of what he terms a "critical temperature for the decomposition of the hydrates"13. Fig. lB shows a pressure-temperature projection of the three-phase locus, hydrate-ethylene rich liquid-vapor (H-L2-V) terminating at the critical locus in which L² and V assume similar properties. Throughout this paper the following phase designations will be used: H for hydrate, Ll for the water rich liquid. L2 for the

Jan 1, 1949

By A. R. Calawa, T. C. Harman, M. Finn, P. Youtz

A study has been made of the growing, annealing, and diffusion parameters in PbSe, Pb1-ySnySe, and Pb1-xSnxTe. Single crystals of these materials have been grown using the Bridgman technique. For all of the above materials the as-grown crystals are p type with high carrier densities. To reduce the carrier concentration and increase the carrier mobility, the samples are annealed either isothermally or by a two-zone method. From isothermal anneals, the liquidus-solidus boundary on the metal-rich side of the stoichiometric composition has been obtained for some alloys of Pb1-xSnxTe and on both the metal- and seleniunz-rich sides for PbSe and alloys of Pbl-ySnySe. In Pbo.935 Sno.065 Se carrier concentrations as low as 5 x1016 Cm-3 and mobilities as high as 44,000 sq cm v-1 sec-1 at 77°K have been obtained. Inter diffusion parameters mere also studied. The ddiffusion experiments mere identical to the isothermal or two-zone annealing experiments except that the samples were removed prior to complete equilibration. The resulting p-n junction depths were determined by sectioning and thermal probing. Inter diffusion coefficients for various temperatures were calculated for both PbSe and Pb0.93Sn0.0,Se. RECENTLY, there has been considerable interest in the PbTe-SnTe and PbSe-SnSe alloys with the rock salt crystal structure. The unusual feature of these systems is the variation of energy gap EG with composition. Several investigations1-3 have shown that EG for the lead chalcogenides decreases as the tin content increases, goes through zero, and then increases again with further increase in tin content. The possibility of obtaining an arbitrary energy gap by selecting the composition is an especially attractive feature of these alloys for applications involving long-wavelength infrared detectors and lasers. In addition, some unusual magneto-optical, galvanomagnetic, and thermomag-netic effects should occur for alloys with low band gaps. If uncompensated low carrier density crystals can be obtained, then a small carrier effective mass, a large dielectric constant, and the resultant high carrier mobility should yield enormous effects at low temperature in a magnetic field. The relative variation of the energy gap with pressure should also be very large for these low gap materials. The primary purpose of this paper is to provide some information concerning the preparation of low carrier concentra- tion, high carrier mobility, and homogeneous single crystals with a predetermined alloy composition. I) DETERMINATION OF ALLOY COMPOSITIONS In all of the work described in this paper, the composition of lead and tin chalcogenides in the alloys was determined by electron microprobe analysis. Separate X-ray spectrometers are used to make simultaneous intensity measurements of the Pb La1 and Sn La1 lines emitted by the sample under excitation by a beam of 25 kev electrons focused to a spot about 2 µm in diam. These intensities are compared to the intensities of the same lines emitted by standards under the same conditions. The standards used are the terminal compounds of each pseudobinary system, i.e., PbTe and SnTe for Pbl-xSnxTe alloys, PbSe and SnSe for Pbl-ySnySe alloys. The composition of the sample is then obtained from theoretical calibration curves which relate the weight fractions of lead and tin in the alloy to the measured ratios of X-ray intensities for the sample and the standards. The lead and tin calibration curves for each alloy system were calculated by using corrections for backscattered electrons,4 ionization,5 and absorption,6 and assuming that the atom fraction of tellurium or selenium in the sample and standards is exactly +. Results obtained by using the microprobe are in good agreement with those obtained by wet chemical analysis. II) CRYSTAL GROWTH FROM THE VAPOR Early work on the vapor growth of PbSe was carried out by Prior.7 He used small chips of Bridgman-grown single crystals as the source material and frequently converted the whole charge of a few grams into one crystal. In the present work, vapor growth occurred using a metal-rich or chalcogenide-rich two-phased alloy powder as the source material. Small, nearly stoichiometric crystals are formed on the walls of the quartz tube. The procedure will now be described in detail. Initially, a 100-g charge containing (metal)o.51(chalco-genide)o 49 proportions or (metal)o.49(chalcogenide)o. 51 proportions of the as-received elements in chunk form are placed in a fused silica ampoule. After the ampoule is loaded, it is evacuated with a diffusion pump and sealed. The sealed ampoule is placed in the center of a vertical resistance furnace. The region containing the ampoule is heated to about 50°C above the liquidus temper-ature for the particular composition used. After about one-half hour at temperature, the elements are reacted and the molten material homogenized. The ampoule is quenched in water. The quenched ingot is crushed to a coarse powder for vapor growth experiments and to a fine powder for the isothermal annealing experiments which are discussed in a later section. Vapor growth experiments were carried out using the powdered, metal-rich or chalcogenide-rich alloys

Jan 1, 1969

By T. H. Aldrich

(Chattanooga Meeting, October, 1908.) Tars paper is intended only to give a preliminary account of experiments made, and conclusions reached, concerning the treatment of certain refractory low-grade gold-ores, the profitable reduction of which may furnish a useful guide to the solution of similar mining and metallurgical problems, not only in the gold-bearing belt of the Southern United States, but perhaps in other regions also. It must be regarded as simply a ?report of progress," preceding a more elaborate and conclusive report of regular practice. The mines of the Hillabee Gold Mining Co. are located upon what is generally known locally as Hog Mountain, on the northern edge of Tallapoosa county, Ala., about 15 miles from Goodwater and 14 miles from Alexander City, stations on the Central of Georgia Railway. Gold has been known since 1839 to exist on this property, where it was discovered in that year by a man named Johnston. The property was worked for placer-gold by the old miners, and there are now the remains of four attempts to operate it by stamp-mill and plate-amalgamation. The present owners purchased it in 1896, and since that time they have experimented at frequent intervals, in order to devise a process that would satisfactorily recover the gold. In 1903 regular operations were begun. Geologically, the mountain consists of an intrusion of what has been pronounced true granite in altered sedimentary slates. The cooling of the granite produced shrinkage-cracks, which have become veins. There is considerable question as to the period of the slate formation; but it is undoubtedly, in my opinion, of Carboniferous age. The veins, about 50 in number, strike N. 60° to 80° E.; dip approximately 65° from the horizontal; vary from a few inches to 25 ft. (being in gen-

Nov 1, 1908

By L. Zwell, H. A. Wriedt

X-ray Lattice parameter and bulk density measurements were made at room temperature on solid solutions of nitrogen in purified a, iron, containing from 0 to 0.053 wt pct N. When nitrogen is dissolved in a, iron, the fractional increase in unit cell volume (X-ray diffraction) and the fractional increase in volume per gram of iron (bulk density measurement) are the same within experimental error. The two sets of results when averaged show that the unit cell edge of a, iron increases linearly by 3.2 X 10-2 A per wt pct N dissolved and that the partial gram-atomic volume of nitrogen at infinite dilution in a, iron is the same as it is in nitrogen-martensite, that is, 5.90 cm3. RECENT reviews17' of literature dealing with the lattice parameter of ferritic iron-nitrogen alloys indicate that the dilating effect of dissolved nitrogen on the bcc unit cell of a iron is not known with confidence. Five investigations3-7 either revealed no effect of nitrogen or were inconclusive. Among other investigations, where quantitative data were obtained, the results of Osawa and Iwaizumi8 indicate too large an effect, and those of Eisenhut and Kaupp9 show the lattice parameter of ferrite varying with the nitrogen content at concentrations far beyond the known solubility limit. It is not clear in Burns'10 data what value should be used for the lattice parameter of nitrogen-free ferrite in calculating the dilation. Burdese11 shares with Burns the shortcoming that the iron-nitrogen alloys were solution-treated and quenched with undissolved nitride present. The consequence is that the un- certainties in the solubility limit1 are added to those in the lattice parameter measurements when the variation of lattice parameter with nitrogen content is computed. For a system of such widespread interest, we felt that a new investigation was merited. Both X-ray diffraction and bulk density measurements were used to determine the dilation of the , a iron lattice by dissolved nitrogen. EXPERIMENTAL PROCEDURE Material. The bulk density and X-ray diffraction experiments were both made with specimens of a purified iron (denoted as "B iron")- from Battelle Memorial Institute. The impurity contents were as follows: As, C, Cu and Pb—50 ppm; Ag, Al, Co, Ga, 0, Ti-11 to 50 ppm; B, Be, Ca, Cd, Cr, Mg, Mn, Mo, N, Ni, S, Sb, Si, Sn, V, W-10 ppm or less. The vacuum-cast ingot was hot-forged and annealed. Pieces of the forged stock were machined and cold-rolled to give strip stock 0.08 and 0.002 in. thick for density and for X-ray measurements, respectively. Preparation of Specimens. Starting with a piece of the cold-rolled iron stock, the general sequence of operations, after an initial recrystallizing anneal, was to measure the density or lattice parameter, nitrogenize, remeasure the property, age or denitrogenize, and again measure the property. Duplicate analyses for nitrogen were made by a modified Kjeldahl method on portions of the actual density specimens and on pieces nitrogenized to equilibrium alongside the X-ray specimens. Annealing of the density specimens was performed by sealing the pieces with the as-rolled surfaces removed by filing into evacuated "Vycor" capsules and treating for 1 hr at 750°C followed by furnace cooling. (TO check the effect, if any, of annealing procedure, a specimen also was

Jan 1, 1962

By D. T. MacRoberts

Tins paper embodies the results of theoretical studies concerning gas reservoirs, especially the effect of drilling programs of various intensities upon pressure depletion and ultimate recoveries. The primary objective has been to determine the net quantity of recoverable gas that could be obtained as a result of each additional well, in comparison with the gas that might be secured from a single well ideally placed with respect to both acreage and geological structure. No method is yet known whereby the relative merits of intensive and sparse drilling can be compared experimentally; a reservoir must either be drilled closely or developed with wide spacing, but both programs cannot be conducted simultane-ously. Hence, the analytical method seems to be the only approach to the problem. While the present state of our theoretical knowledge does not offer a precise solution to the problem of gas flow in sand bodies, it takes such appropriate cognizance of the limitations of the methods used as to restrict any answer obtained to the realm of engineering accuracy. In solving the problem for the average gas field, it was found that practically the same answers resulted as to pressure distribution, regardless of the size of the drainage radius, even though the latter was assumed to vary from a few feet as a minimum to that of the entire reservoir as a maximum. Such limits represent extreme possibilities; therefore, the practical conditions that are associated with normal development programs, in which wells are placed in the center of tracts varying in size from 40 to 640 acres, will of necessity result in less extreme variations than those indicated in the tables accompanying this paper. Stated more concisely, the amount of gas unrecovered at abandonment (of the particular field used for illustrative purposes) will lie somewhere between 4.6 and 6 per cent of the total original content, no matter how intensively the field is drilled.

Jan 1, 1938

By R. R. Byran, M. H. Kuryla

The Compania de Real del Monte y Pachuca started a 10-ton pilot plant in March, 1906. The distinctive features of the first cyanide installations at Pachuca were: grinding in cyanide solution, all-sliming and filtration of ore in which silver constituted the major value. Loreto started with a 300-ton " all-sliming" plant, using jaw crushers, grinding in stamps, Chilean mills and pebble mills in cyanide solution, concentrating with Wilfley tables and Johnson vanners, classification by cones and Dorr classifiers, intermittent thickening by decantation, mechanical agitation in flat tanks by stirrers and centrifugal pumps, filtration in Butters filters and precipitation by zinc shavings. The "San Francisco" mill No, 1 was contemporaneous, using a rather similar flow sheet. We shall trace the main developlnents in the three large mills of the district to their present practice. Developments in Large Mills of District Crushing and Grinding.—The trend of development in this part of the work has been the same as throughout the milling world; via., all increase in the degree of comminution of the ore in dry-crushing machines, the advance from pebble mill to rock mill and then to ball mill and the elimination of the stamp battery through the encroachment upon its field on the one side by finer dry crushing and on the other by more efficient wet grinding. The single-stage crushing in jaw type crushers, used at the start, has been replaced by two stages; at first, both stages by gyratory type and later the present practice, which is the same in all three mills, consisting of gyratory as primary followed by cone as secondary and delivering a product that may be rated at 56 to 1 inch. Primary wet grinding, at first performed by stamps and Chilean mills, is now by hall and/or rod mills; present practice differing widely in the three mills. Santa Gertrudis uses a 7 by 15 ft. rod mill, San Rafael

Jan 1, 1935

By Paul A. Bailly

2.1-1. The Exploration Function in the Mineral Industry. With regard to a new mine, exploration can be technologically defined as all the activities and evaluations necessary before an intelligent decision can be made establishing size, initial flowsheet, and annual output of the new extractive operation based on a certain mineral deposit. The activities that follow such a decision are called first development, then operation (90). Thus, in the U.S.A., exploration may continue in the technological sense after a mineral property has entered the "development stage" as defined for tax purposes. Regulations under Sections 1.615.1 and 1.616.1 of the U.S. Internal Revenue Code state that the "development stage" has been reached when "deposits of ore or other minerals are shown to exist in sufficient quantity and quality to reasonably justify commercial exploitation by the taxpayer" (95). There are, of course, many instances where additional later exploration discloses additional reserves which justify a plant much larger, more efficient and more profitable than the minimum feasible commercial operation. After a surface mine is put into operation, additional search generally will increase the reserves and thus warrant expansion of the rate of output and/or extend the life of the operation. The methods and techniques in such search are similar to those used in predevelopment exploration. This activity has produced a major part of new reserves for all mineral commodities but is not considered as exploration in the context of this chapter. The objective of exploration is, briefly stated, to find and acquire a maximum number of new economic mineral deposits with a minimum cost and in minimum time. The search must be so organized as to maximize the overall probability of discovering commercial mineral concentrations within a minimum time with the funds available. As shown by Celasun (27) these statements are neither adequate nor complete from a pragmatic point of view. Each actual exploration venture must define its objectives in terms of a minimum rate of return on investment for any deposit found

Jan 1, 1968

By J. R. Guard

Development of electrical power in coal mining has been an outstanding example of adaptbility. It has accommodated itself to new inventions, changing mining methods, increasing demands, increasing safety requirements and many other new conditions. With the appearance of the continuous miner in the mining machinery picture, those engineers interested in the application of electricity to mining have been thinking about what new comination of electrical apparatus will best suit this newcomer. It is the purpose of this paper to discuss the relative costs of supplying d-c versus a-c power to mining equipment with particular reference to continuous miner setups. Assume that a-c power will be delivered to the mine at some high voltage suitable for transmision to the various substation locations. Typical voltage for this purpose is 4000 volts. The problem then is to change the power to some kind of power suitable for driving the motors of mining equipment. For safety and other reasons the voltage to be delivered to the motor terminals must be under 600 volts.

Jan 6, 1950

Edwin A. SpeRry, Denver, Colo. (communication to the Secretary*) :—Since writing my former paper on this subject I have had several discussions concerning some of the statements contained therein, with men who have had a large experience with the old form of buddle, both in this country and in Cornwall. The present paper gives a brief statement of some of the points debated, together with the arguments and proofs in their substantiation. The first point is the question of the capacity. In my origi-

Jan 1, 1904

By Bashir Ahmed, Fred D. Wright

Numerous investigators have studied the various factors that influence the ultimate strength of model mine pillars, such as ratio of height-to-least width; restraint or friction on the top and bottom; 1,2 the effect of stress distribution in pillars on their strength;3 and the scaling factors involved in applying the results of model pillars to full-scale pillars. However, the load-bearing capacity of pillars after initial failure does not appear to have been investigated. Yet many mines employ methods in which small pillars or pillar remnants are left systematically; these pillars crush as mining progresses and, of necessity, affect the behavior of surrounding rock even after initial failure. The effect of such crushed or crushing pillars depends largely on their load-deformation characteristics. This chapter presents the results of a preliminary investigation to determine the load-deformation characteristics of a few model mine pillars to and beyond initial failure. Various investigators have also studied the elastic and viscoelastic behavior of mine structures. In such studies, computers are frequently employed to obtain numerical results by the finite difference or finite element methods. It would be entirely feasible to write a program that would approximate the load-deformation characteristics of pillars to and beyond the crushing stage if these characteristics were known. More accurate information on the induced stresses and deformations in overlying strata and on surface subsidence could be obtained, information which should result in better strata control by enabling the engineer to calculate more accurately the effects of changes in pillar spacing, size, and shape.

Jan 1, 1972

By Jay Carpenter

THIS paper deals with only one step in the treatment of ore at the West End mill; not because the other steps are repetitions of practice in other mills, but because in this particular step there is in use the Trent agitator. This device, although it has apparently failed in many mills, is here giving excellent service and has proved to be well adapted for making a thorough replacement of pregnant solution with a minimum amount of barren solution. The strong and weak points of this agitator, its present simple construction, and its use as a thickener for agitator or battery pulp are features of interest; but perhaps the point of greatest interest to the metallurgist in this day of continuous decantation is its use in a series of tanks for slime treatment by the replacement method. The agitating department of the West End mill consists of six redwood tanks, 24 ft. in diameter, 18 ft. high, each equipped with aTrent agitator, a centrifugal pump, and a motor. The pulp is transferred by a pump from the top of a flat-bottomed tank to a set of arms and nozzles in the bottom of the tank, at just sufficient pressure to cause the arms to revolve. The streams from the many nozzles keep the bottom of the tank clean, and these streams, coupled with the effect of the revolving mechanism and the ascending current, keep the pulp in constant motion and of constant gravity. .These agitating tanks hold 90 tons of dry slime and 202 tons of solution with a 1.24 pulp, our ore having a specific gravity of 2.7. This capacity is about 10 per cent. in excess of the standard 15 by 45 ft. Pachuca tank. The tanks are connected in one series for continuous agitation, the pulp for each agitator being drawn by its pump through a branch suction from near the top of the preceding tank and. delivered to the bottom of the tank by the agitator arms along with the regular pulp of that agitator. This method works automatically, since the flow through the branch suction varies directly with the difference in head of the two tanks. The chance for new pulp to pass out quickly is, therefore, much less than in many other systems of continuous agitation, since the new

Jan 8, 1915