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Lead-zinc production in Canada accounted for 19% of the total value of metals and minerals produced in 1976, says Keith C. Hendrick, president of Noranda Sides Corp. Mine production of recoverable zinc w as 1. 158 million toils of 27.4% of free world production in 1976. Slab zinc pro¬duction was placed at 472,000 tons that year. Canadian mine production of recoverable lead was 247,000 tons or 10.6% of the free world production. Refined lead that year was at 177,000 tons.

Jan 11, 1977

By R. Wang, N. J. Grant, B. C. Giessen

By crystallographic and X-ray methods, the existence and isonzorphism of Ti3Rh5 and Hf3Rhs were confirmed. Both phases are of the orthorhombic Ge3Rh5 type; lattice parameters and refined positional parameters are given. The structure is related both to the filled-up NiAs-B8 and Cu-AI types. An analogous phase with zirconium does not exist; the effect of ternary substitutions for titanium ad hafnium suggests a size factor limit to be active. A recent survey of phase diagrams of the T4 metals titanium, zirconium, and hafnium with the T, noble metals rhodium and iridium indicated the existence of the A3B5 phases Ti3Rhs, ZrsRhs, and HfsRhs. Ti3Rhs and Hf3Rh5 were found to be isostructural, based on the line-rich powder patterns which had not been analyzed. Zr3Rh5 was considered to have a substructure of the NbRu type (orthorhombically distorted B2-CsCl type).&apos; Because, in combinations with other transition metals, hafnium and zirconium are generally more likely to form isostructural phases than hafnium and titanium (with the significant exception of the Ti2Ni-"E93" type phases based on T4 metals2), the reversal of this relation for the A3B5 phases was of interest. As shown in the following, the nonexistence of Zr3Rhs has been established, the structures of Ti3Rh5 and Hf3Rh5 have been worked out, and crystal chemical relationships and stability criteria are reported. EXPERIMENTAL METHODS AND RESULTS Alloy Preparation and Phase Diagram Work. Alloys were prepared from high-purity (99.99+ pct) elements by arc-meltin3,4.Heat-treated alloys were annealed in a vacuum of 3 x X torr for 24 hr at 1300DC. Metal-lographic samples were etched electrolytically in concentrated HCl with 5 v ac for 5 min.3 X-ray diffraction powder patterns were taken on a GE XRD-5 dif-fractometer with Cum radiation at low scanning rates (0.2 deg per min for 28). It was confirmed that Ti3Rhs and Hf3Rh5 have similar diffraction patterns, and that an alloy with the composition Zr3Rhs has a different pattern. Six Zr-Fh alloys with 59 to 69 at. pct Rh were therefore prepared and investigated in the as-cast state by X-ray diffraction and metallography. Alloys at 59 and 61 at. pct Rh were found to be a single phase, with the distorted B2-CsC1 type structure typical for the off-stoichio- metric region of the phase (Zr,-,Rh,)Rh. This phase forms a eutectic with ZrRhs at about 66 at. pct Rh: accordingly, alloys between 61 and 69 pct at. pct Rh consisted of two phases. There is no evidence for the existence of Zr3Rh5. Based on the results in Rafs. 1 and 5, on the present work on Zr-Rh, and on several additional alloys investigated, the portions between the AB and AB3 stoi-chiometry for Ti-Rh, Zr-Rh, and Hf-Rh are as follows: Further, several ternary alloys near Ti3Rhs and Hf,Rhs were prepared in which it was attempted to replace titanium and hafnium partly by zirconium, niobium, tantalum, and germanium. The results will be discussed in a later section. Structure Determination of Ti3Rh5. Since Ti3Rh5 and Hf3Rh5 are isostructural, the following discussion will largely deal with the former. Although the powder pattern of TisRhs is complex, as found previously,1 it could be indexed by comparison with other structures of A3Bs stoichiometry. Ti3Rh5 was found to be isostructural with Ge3Rh5, whose orthorhombic structure had been elucidated by Geller.9 As both the sizes and atomic numbers of germanium and titanium are comparable, the unit cell volume and the peak intensities could be expected to be similar; however, significant differences exist in the atomic positions, as will be shown. All lines in the powder patterns of Ti3Rh5 and Hf3Rhj could be indexed with primitive orthorhombic unit cells with the lattice constants: The fractional errors are 10 The low-angle portion of the indexed powder pattern of Ti3Rh with sin2 8 < 0.30 is listed in Table I. The extinction laws Okl only with k = 2n and hOl only with h - 2n are compatible with the space group Pbo2 and the more symmetrical space group Phnm of Ge3Rh5. Finally, the positional parameters of Ti3Rh5 and HfsRhs were refined under the assumption that titanium and hafnium occupy the germanium positions in Ge3Rh5. Integrated intensities were obtained from the diffraction patterns by planimetry. Intensities of overlapping reflections were separated by an iteration process incorporated into the least-squares positional refinement program according to a method described previously. The intensities of Ge3Rh5 were used in the first separation cycle, while the atomic parameters of Ge3Rh5 were used as starting values in the first refinement cycle. Absorption due to specimen

Jan 1, 1970

By W. C. Knopf, G. Samsel

For several years International Minerals & Chemical Corp. has used a radiation method to assay potassium content of products from potash and feldspar beneficiation. The procedure is rapid, accurate, and inexpensive and is easily handled, if necessary, by nontechnical personnel. Data are presented to show the accuracies that may be expected if the technique is used for control of pilot plants or large- scale plants. Natural potassium is composed of three isotopes -K39, K40 and K41. Five other isotopes, artificially produced, have been detected. In natural potassium only the K40 isotope, with a half life of 1.4 x 109 years, is radioactive. Its modes of decay are beta and gamma rays, positrons, and x-rays. Only the more abundant beta rays, however, are important in radiation measurements using geiger tubes.

Jan 10, 1958

By P. Farrar, H. Margolin

The Ti-Pb diagram was investigated in the region 0 to 58 pct Pb and from 500°C to liquidus temperatures. Three reactions were encountered: I—ß?a+Ti Pb at 725 10°C; 2—ß+L?Ti4Pb at 1305+ 10°C; and 3—the possible eutectic L-+Ti,Pb and y between 1200" and 1300°C. LEAD-RICH alloys have been investigated by Nowotny and Pesl,&apos; who used sintered compacts and studied the region from 37.5 to 100 pct Pb by X-ray diffraction analysis. The only phase found in addition to titanium and lead was the hexagonal compound Ti Pb. Alloy systems of lead with metals of the transition group, such as iron, chromium, tungsten, cobalt, nickel, or manganese, generally show little liquid or solid solubility.&apos; Craighead et al.,3 however, indicated that lead is soluble in a and ß titanium to at least 2.1 pct. They also found that approximately 50 pct of the lead added was lost during the arc-melting of Ti-Pb alloys. In the present investigation, are-melting also was used to prepare Ti-Pb alloys and similarly large lead losses were encountered. Experimental Procedure Alloy Preparation: Considerable difficulty was encountered in the melting of the Ti-Pb alloys and a number of experiments were performed before the method described was developed. Alternate layers of lead and titanium were wrapped with titanium sheet and compacted. This "sandwich" was annealed at 300" to 350 °C and was melted according to the procedure described by Cadoff and Nielsen.&apos; Using a low current, 150 amp, and an argon atmosphere, four to eight 10 to 20 sec melts were made on each alloy, with the button being turned over between each melt to insure homogeneity. In the high lead range, the preliminary sintering was found to be of doubtful value and was eliminated. In the region above the nominal composition of 70 wt pct Pb, the alloys prepared in this manner always consolidated into two phases. The outside appeared to be composed entirely of lead and the inside was a Ti-Pb alloy. In order to determine whether this phenomenon was caused by a miscibility gap, master alloys with a nominal composition of 40 wt pct Pb were machined and mixed with various percentages of lead sheet. This mixture was compacted and melted in the same manner as the other alloys. Although these alloys were not homogeneous, they did not show the layering that was observed

Jan 1, 1956

By A. S. Yue, A. E. Vidoz, F. W. Crossman

Tensile specimens were prepared from a single grain of an epitaxially grown Al-CuAl2 eutectic ingot. The eutectic lanzellae were oriented parallel and perpendicular to the tensile axis of the specimens. Since the composite was of the eutectic composition, the aluminum-rich matrix could dissolve up lo 5. 7 wt pct Cu in solid solution and, therefore, was amenable to strengthening by precipitation hardening. The tensile properties of the eutectic single crystals were determined at room temperature as functions of interlamel-lar spacing, platelet orientation, and thermornechanical trealment. The obserced variations in composite stress and modulus with respect to the level of&apos; composite strain are discussed in terms of premature fracture of CuAlz platelets, a distribution function for the strength of the lamellae, and unequal strains due to localized fracture of&apos; platelets. The discontinuous fiber composite model of Kelly and Tyson is modgied to account for a changing distribution of fiber lengths during composite loading. The tensile properties at elevated temperatures were determined for the direc-tionally solidified eutectic oriented with platelets parallel to the tensile axis. The observed properties are attributed to the onset of plasticity of the CuAL2 phase above 150°C. DURING the investigation of whisker- and fiber-reinforced metallic matrix composites in recent years, two major problem areas have developed: 1) The fabrication of the composite involves tedious handling techniques in order to obtain a unidirection-ally aligned and uniformly spaced set of whiskers in the metal matrix. 2) Due to weak interfacial bond strengths or because of the formation of additional embrittling phases at the metal-fiber interface during long-time exposure or fabrication at elevated temperatures, many composite systems have exhibited considerably lower strengths than those predicted by a law of mixtures analysis.&apos; These problems have been bypassed by the technique of growing whiskers and plates of high-strength materials in a ductile metal matrix by controlled unidirectional eutectic solidification.2 The tensile properties of directionally solidified A1-CuA12 eutectic are presented here. This alloy consists of a ductile aluminum matrix, containing up to 5.7 wt pct Cu in solid solution, which is amenable to precipitation hardening by heat treatment and a reinforcing high modulus CuAlz intermetallic phase. The two phases are present in the form of alternating platelets or lamellae. The microstructural stability of this unidirectionally solidified alloy at elevated temperatures has been studied extensively.3.4 and preliminary tensile and bend tests have been reported. 5-7In the present investigation the tensile properties of the A1-CuA1, eutectic have been studied as a function of several ther-momechanical variables: solidification rate. heat treatment. rolling at elevated temperatures. and lamellar orientation. It was felt that the uniformity of structure and excellent interfacial bonding would give tensile properties concomitant with the metal matrix composite theory of strengthening proposed by Kelly and coson. 8-9 The tensile properties that were obtained point to a wide distribution of strengths for the CuAlZ platelets, which leads to large deviations from the predicted mechanical behavior for this composite. EXPERIMENTAL PROCEDURE Epitaxial Growth of Eutectic Alloy. The A1-CuA1, eutectic alloy was prepared by an epitaxial growth process. Sections of a master alloy ingot (total impurity content <0.008 pct) were placed in an alundum boat, melted. and directionally solidified to obtain a multigrained plate 12 by 2 by 4 in. This plate was tapered at one end to mate with a seed crystal 1; in. long and 4 by $ in. square. Then the seed-plate combination was placed in an alundum boat which sat in a quartz tube passing through the center of a horizontal resistance wound tube furnace. A dried argon atmosphere was maintained. The temperature gradient in the furnace was such that the liquid-solid interface of the eutectic alloy was located near the end of the furnace and could be observed through the quartz tube. Single-crystal plates were formed by melting the material back to the midpoint of the seed crystal of the desired platelet orientation and then epitaxially growing the plate from the seed by withdrawing the alundum boat from the furnace at a constant rate. This technique was used to produce aluminum and CuA12 lamellae parallel and perpendicular to the transverse direction on the plate. Metallographic examination showed that both phases were continuous across the original liquid-solid interface. It was also possible to grow a plate from two seeds placed side by side: and, although the lamellae of one seed were oriented at 90 deg to those of the second seed, the interface between the two grains remained parallel to the growth direction along the entire ingot length. Maintenance of a straight intergranular boundary during the solidification process was possible as long as both seeds were oriented with their original growth direction parallel to the solidification direction of the plate. Eutectic plates were directionally solidified at rates of 0.2, 1.0. and 4.7 cm per hr and sectioned transversely to the solidification direction to determine the apparent inter lamellar spacing of the lamellae. Metallographic examination was also employed

Jan 1, 1970

By P. W. George

This paper presents geological data regarding deposits of over 7,500,000 tons of fine-grained sulphide ore in barite gangue. A series of pyroclastics and arkoses was intruded by sills of quartz porphyry in connection with batholithic intrusions of granite 3 miles from Buchans. Gentle folding, with fracturing and shearing of tuff beds and intruded quartz porphyry, accompanied and followed the intrusion of granite and porphyry. The sulphide-barite mineralization is localized primarily in fractured and sheared tuff beds, but also in the sheared quartz porphyry. Two structures have proved particularly favorable for mineralization-one, the center of an anticline; the other, a series of weak, incompetent tuff beds intruded by thin sills of quartz porphyry and located between strong beds of arkose. During the folding the weak tuff with intruded quartz porphyry was intensely sheared and contorted and subsequently mineralized by sulphides and barite. INTRODUCTION Buchans is 5 miles north of Red Indian Lake, in Central Newfound- land, at an elevation of 900 ft. above sea level and 400 ft. above Red Indian Lake, and is reached by a 37-mile private railway from Miller- town Junction. The first ore body found at Buchans was discovered some 30 years ago in the bed of Buchans River, by Matty Mitchell, an Indian woodsman employed by the Anglo-Newfoundland Development Co. Ltd. In the years following the discovery the ore was developed by shaft-sinking and drifting, with results indicating a lenticular ore body in a shear zone, containing about 100,000 tons of extremely fine-grained sulphide ore in barite gangue averaging about 0.05 oz. Au, 4 oz. Ag, 1.5 per cent Ch, 10 per cent Pb, 18 per cent Zn. Because a profitable metallurgical treatment for the ore was not found, the mine was closed down in 1911. In 1915, Mr. H. A. Guess, Vice President of the American Smelting & Refining Co., learned of the Buchans River ore body, and after metallurgical tests had been carried on from time to time in his company&apos;s testing plant a satisfactory separation of the sulphides by selective flotation was finally effected in 1925. Prospecting for additional ore bodies was begun in 1926, utilizing geophysical methods under the direction of Hans Lund-

Jan 1, 1937

By N. P. Peterson

The Castle Dome copper deposit is of the porphyry type and occurs in a body of quartz monzonite intruded into the pre-Cambrian formations and possibly into the lower part of Paleozoic limestones. The hypogene sulphide minerals include pyrite, chalcopyrite, and a little molybdenite, sphalerite, and galena. Pyrite and chalcopyrite are disseminated or occur in small closely spaced veins. The hypogene mineralization shows distinct zoning in the distribution of pyrite and chalcopyrite, so that the mineralized area can be subdivided into pyritc and chalcopyrite zones. Supergene enrichment, though not extensive, played an important part in the formation of the ore body, the chalcopyritc zone being the pro-tore. Several thin, gently dipping, diabase sills occur in the mineralized area, and the copper content of the rock in and near these sills is substantially higher than average. The formation of the ore body was caused by the combined effects of three forces: I. Zoning of the hypogene mineralization, 2. Richer copper metallization associated with the diabase sills, and 3. Supergene enrichment. Introduction The Castle Dome copper deposit is about 5 miles west of Miami, Arizona, and about 3 miles west of the Miami-Inspiration ore body. The Castle Dome open-pit mine is on the south flank of Porphyry Mountain, a prominent landmark of the region. In 1941 the deposit was being explored by the Miami Copper Co., but the exploration program was cut short when the decision was made to develop the property as a war project. The Castle Dome Copper Co., Inc., was organized as a wholly owned subsidiary of the Miami Copper Co., and arrangements were made with Defense Plant Corp. for developing and equipping the mine and for construction of a concentrating plant. Construction and development work was begun in January 1942, and milling operations started June so, 1943. Since that date, the mine has been in continuous operation by the Castle Dome Copper Co, under a lease agreement with Defense Plant Corp. producing copper at an average rate of 4,000,000 lb per month. To January I, 1946 the total production amounted to 121,088,000 lb of copper,4,271 oz of gold, and 211,755 oz of silver. A detailed study of the copper deposit and the surrounding area was undertaken by the U. S. Geological Survey in June 1943. Other members of the Survey participating in the work were C. M. Gilbert, G. L. Quick, and J. P. Albers. The results of this work will be published as a comprehensive report by the Geological Survey. General Geology The Globe quadrangle, which includes the Castle Dome area, was studied by F. L. Ransome1 of the Geological Survey in 1901 and 1902. His maps and descriptions were

Jan 1, 1949

By N. P. Peterson

The Castle Dome copper deposit is of the porphyry type and occurs in a body of quartz monzonite intruded into the pre-Cambrian formations and possibly into the lower part of Paleozoic limestones. The hypogene sulphide minerals include pyrite, chalcopyrite, and a little molybdenite, sphalerite, and galena. Pyrite and chalcopyrite are disseminated or occur in small closely spaced veins. The hypogene mineralization shows distinct zoning in the distribution of pyrite and chalcopyrite, so that the mineralized area can be subdivided into pyritc and chalcopyrite zones. Supergene enrichment, though not extensive, played an important part in the formation of the ore body, the chalcopyritc zone being the pro-tore. Several thin, gently dipping, diabase sills occur in the mineralized area, and the copper content of the rock in and near these sills is substantially higher than average. The formation of the ore body was caused by the combined effects of three forces: I. Zoning of the hypogene mineralization, 2. Richer copper metallization associated with the diabase sills, and 3. Supergene enrichment. Introduction The Castle Dome copper deposit is about 5 miles west of Miami, Arizona, and about 3 miles west of the Miami-Inspiration ore body. The Castle Dome open-pit mine is on the south flank of Porphyry Mountain, a prominent landmark of the region. In 1941 the deposit was being explored by the Miami Copper Co., but the exploration program was cut short when the decision was made to develop the property as a war project. The Castle Dome Copper Co., Inc., was organized as a wholly owned subsidiary of the Miami Copper Co., and arrangements were made with Defense Plant Corp. for developing and equipping the mine and for construction of a concentrating plant. Construction and development work was begun in January 1942, and milling operations started June so, 1943. Since that date, the mine has been in continuous operation by the Castle Dome Copper Co, under a lease agreement with Defense Plant Corp. producing copper at an average rate of 4,000,000 lb per month. To January I, 1946 the total production amounted to 121,088,000 lb of copper,4,271 oz of gold, and 211,755 oz of silver. A detailed study of the copper deposit and the surrounding area was undertaken by the U. S. Geological Survey in June 1943. Other members of the Survey participating in the work were C. M. Gilbert, G. L. Quick, and J. P. Albers. The results of this work will be published as a comprehensive report by the Geological Survey. General Geology The Globe quadrangle, which includes the Castle Dome area, was studied by F. L. Ransome1 of the Geological Survey in 1901 and 1902. His maps and descriptions were

Jan 1, 1949

By P. W. George

This paper presents geological data regarding deposits of over 7,500,000 tons of fine-grained sulphide ore in barite gangue. A series of pyroclastics and arkoses was intruded by sills of quartz porphyry in connection with batholithic intrusions of granite 3 miles from Buchans. Gentle folding, with fracturing and shearing of tuff beds and intruded quartz porphyry, accompanied and followed the intrusion of granite and porphyry. The sulphide-barite mineralization is localized primarily in fractured and sheared tuff beds, but also in the sheared quartz porphyry. Two structures have proved particularly favorable for mineralization—one, the center of an anticline; the other, a series of weak, incompetent tuff beds intruded by thin sills of quartz porphyry and located between strong beds of arkose. During the folding the weak tuff with intruded quartz porphyry was intensely sheared and contorted and subsequently mineralized by sulphides and barite. Introduction Buchans is 5 miles north of Red Indian Lake, in Central Newfoundland, at an elevation of 900 ft. above sea level and 400 ft. above Red Indian Lake, and is reached by a 37-mile private railway from Miller-town Junction. The first ore body found at Buchans was discovered some 30 years ago in the bed of Buchans River, by Matty Mitchell, an Indian woodsman employed by the Anglo-Newfoundland Development Co. Ltd. In the years following the discovery the ore was developed by shaft-sinking and drifting, with results indicating a lenticular ore body in a shear zone, containing about 100,000 tons of extremely fine-grained sulphide ore in barite gangue averaging about 0.05 oz. Au, 4 oz. Ag, 1.5 per cent Cu, 10 per cent Pb, 18 per cent Zn. Because a profitable metallurgical treatment for the ore was not found, the mine was closed down in 1911. In 1915, Mr. H. A. Guess, Vice President of the American Smelting & Refining Co., learned of the Buchans River ore body, and after metallurgical tests had been carried on from time to time in his company&apos;s testing plant a satisfactory separation of the sulphides by selective flotation was finally effected in 1925. Prospecting for additional ore bodies was begun in 1926, utilizing geophysical methods under the direction of Hans Lund-

Jan 1, 1937

The world&apos;s production of petroleum in 1926 amounted to nearly 150 million long tons, of which India contributed 0.72 per cent. In 1927, this figure jumped to some 172 million long tons, of which the Indian proportion, on a practically stationary production, fell to 0.64 per cent. In 1928, there was another substantial rise in the world&apos;s production, which reached the figure of over 181 million tons. In 1929, there was another jump to over 202 million tons, but in 1930 the world&apos;s production fell to about 193% million tons, in 1931 to about 187 million tons, and in 1932 to about 183 million tons, while in 1933 the production rose again to about 202 million tons, in 1934 to about 215 million tons, and in 1935 to 233 million tons1. Decreases were shown by Poland, Sarawak, Egypt, Rumania and France. All other important producers showed an increase in production, by far the largest being due to Iraq, as a result of the opening of the pipe line to the Mediterranean. The United States contributed 60.9 per cent of the world&apos;s supply in 1935, Russia 10.7 per cent, Venezuela 9.4 per cent, Rumania 3.9 per cent and Iran 3.1 per cent. In 1928, India contributed 0.64 per cent, which fell to 0.60 per cent in 1929 and rose to 0.62 per cent in 1930, 0.63 per cent in 1931, and 0.64 per cent in 1932, and fell again to 0.62 per cent in 1933, to 0.60 per cent in 1934 and to 0.50 per cent in 1935; her position on the list of petroleum-producing countries fell from eleventh in 1929 to twelfth in 1930 to 1933, her place being taken by Trinidad and to thirteenth in 1934 and 1935, owing to the production by Iraq. The production of petroleum in India (including Burma2) increased slightly from 322,025,280 gal.3 in 1934 to 322,662,336 gal. in 1935, the highest figure in the history of the industry. The increase in 1935 is due to an increase of some 4 million gallons in Assam, almost offset by a decrease of 31/2 million gallons in Burma. This increase in output in 1935 was accompanied by an increase in estimated value amounting to Rs. 22,73,550 (£170,944).

Jan 1, 1937

By R. L. Huntington, Frank P. Vance, George F. Russell, Robert Thompson

With the advent of higher pressures in the operation of natural-gas transmission lines, the removal of water vapor from the gas has become increasingly important in order to prevent condensation or formation of gas hydrate from slowing down or stopping the flow of gas. Intelligent design of these dehydration or gas-drying plants has been hampered through the Iack of experimental data on the water vapor content of natural gas at elevated pressures. In view of this need, this present investigation was sponsored by the Southern Natural Gas Co. in the Chemical Engineering laboratories at the University of Oklahoma Research Institute. Experimental results were obtained on the water-vapor content of natural gas up to 2000 lb. per sq. in. at atmospheric temperatures. The water content at 2000 lb. is approximately two thirds as much as it is at 1000 Ib. Deviations from the ideal gas laws vary directly with pressure and indirectly with temperature. Introduction The removal of water vapor from natural gas is an important operation in connection with the production and transportation of this commodity because: I. Liquid water accelerates internal corrosion of a pipe line. 2. Accumulation of water at low points in a pipe line reduces markedly its capacity. 3. Gas hydrates, icy snowlike growths, form readily under high pressure in the presence of the lower hydrocarbons and water, often plugging up the pipe line. In order to design dehydration plants for stripping the gas of its water content, it is essential that the engineer. have a knowledge of the saturated or equilibrium water-vapor content of the gas to be processed. With the gradual increase of operating pressures around gas-producing wells and pipe lines, it was observed that the quantity of water recovered from dehydration plants or condensed in colder lines was considerably greater than had been expected from calculated contents, based on vapor-pressure data taken from steam tables. This observation prompted a number of investigators, for instance, Laulhere,3 Dea-ton,l and Hammerschmidt2 to carry out experimental work at pressures up to 600 lb. per sq. in. in order to determine quantitatively the water content of various gases. Sage, Lacey, et al.4,5 have recognized more recently the need for such data at higher pressures, but their work was done at temperatures of 100ºF, and higher. Since hydrate formation usually, if not entirely, occurs at temperatures below 100ºF., the present investigation was confined to the . lower temperature range at pressures from 600 to 2000 lb. per sq. in. gauge.

Jan 1, 1945

By H. J. Rose

SIXTY-FIVE million net tons of coal were carbonized in the by-product and beehive coke ovens1 of the United States during 1924. This tonnage represented 13.4 per cent. of the bituminous coal which was mined in that year. Table 1 shows production and disposition.2 TABLE 1.-Production and Disposition of Oven Coke in 1924 BY-PRODUCT BEEHIVE TOTAL Coal charged into ovens, tons 49,061,339 15,914,310 64,975,649 Coke produced (exclusive of screenings and breeze), tons 33,983,568 10,286;037 44,269,605 Average yield of coke, per cent 69.3 61.6 68.1 Disposition of coke: PER PER PER CENT. CENT. CENT. Blast furnace 82.5 82.8 82.6 Foundry 4.6 13.3 6.6 Domestic 8.3 1.4 6.7 Water gas manufacture and all other uses 4.6 2.5 4.1 Cokes having somewhat different combinations of chemical and physical properties are desired for the various uses listed above, and these properties depend primarily upon the types of coal used. American coals have a wide range of purity and coking quality, and the chief subject of this paper will be the selection of coals for the manufacture of blast furnace, foundry, domestic, and water-gas coke, in by-product coke ovens. It will obviously be necessary to include a discussion of those physical and chemical characteristics that are generally considered essential or desirable for each type of coke.

Jan 7, 1926

By Harry C. Gatos, Frank J. Bachner

It was shown through high-pressure experiments that tin loss by volatilizatim is necessary for the degrada-tion of the superconducting transition temperature of Nb,Sn associated with high-temperature annealing. Crystallochemical analysis of the degraded Nb3Sn showed that it constitutes a new phase with ordered niobium-site vacancies, created by the migration of niobium atoms to vaccnt tin sites. This new phase was found to form when 4 pct Nb-site vacancies were present. It has a transition temperature of 6&apos;K and a lattice parameter of 5.283A. A similar degradation effect was observed in Nb,Al. Its superconducting transition temperature dropped from 16.5" to 8" K following a high-temperature annealing. The superconducting temperature degradation in these 0-tungsten structure compounds is attributed to the disruption of the interchain d bonding by the periodic interruption of the niobium atom chains. By annealing the degraded Nb, Sn at 1000 C in nitrogen its normal superconducting behavior is restored most likely due to the incorporation of nitrogen atoms causing the elimination of the ordered vacancies. HANAK et al.&apos; have observed low superconducting transition-temperature values (T, - 9"K) in some NbsSn samples deposited from the vapor phase. They attributed such low T, values to disorder in the 0-tung-sten structure. Much lower T values (down to 5.6"K) were reported by Reed et al.zC for NbsSn samples annealed at high temperatures. These authors also attributed this degradation effect to disorder (random occupation of the A and B sites by niobium and tin) but pointed out that such disorder could be brought about (by high-temperature treatment) only in samples containing niobium in excess of the stoichiometric composition NbsSn. Both groups reported that the normal superconductivity behavior could be rever-sibly restored by appropriate heat treatment. Courtney et al., also found that degradation in NbsSn requires excess niobium brought about by the loss of tin during the treatment. However, these investigators proposed that the degradation is due to niobium-site vacancies resulting from the migration of the niobium atoms to the vacated tin atom sites. They did not consider the reversibility of the effect. The present study attempts to establish the nature of the above degradation phenomenon. EXPERIMENTAL PROCEDURES All compounds prepared for this investigation were made from the powders or filings of the elements which were intimately mixed, cold-pressed into a cylindrical pellet at approximately 50,000 lb per sq in., and then submitted to the desired heat treatment. The samples annealed under high pressure were placed in a MgO sample container which was mounted in a pyrophyllite tetrahedron designed for a tetra-hedral-anvil press. Details of the experimental arrangement are given elsewhere. This setup allowed heating at 1800°C or above under pressures in excess of 30kbars for 3 hr. The samples annealed in a vacuum were prepared in a high-temperature vacuum furnace which could reach temperatures up to 2400°C under a pressure of 2 x lo-&apos; Torr. For annealing in a reactive atmosphere, a quartz tube was placed in a clamshell furnace and the desired gas ambient passed through the tube. Lattice parameters were determined using a Debye-Scherer 114.6-mm camera. Cohen&apos;s method, programmed for the IBM 7094 computer, was used to calculate the lattice parameter from the measured d spacings. X-ray integrated intensity measurements were made on several samples. These samples were ground to -400 mesh and the powder mixed with a solution of collodion in amyl acetate. The mixture was poured into a depression milled in a bakelite disc. When the mixture dried, the surface of the disc was ground flat leaving a diffraction surface defined by the face of the disc. The disc was mounted in a Philips rotating specimen holder which allowed the rotation of the sample in the plane of the diffraction surface and the integrated intensity measured using a scintillation counter and a pulse-height analysis sys-tem. The superconducting transition temperatures were determined by means of self-inductance techniques.&apos; EXPERIMENTAL RESULTS AND DISCUSSION The Role of Tin Loss in the Degradation of Super-conductivity. The loss of tin during high-temperature annealing can be effectively suppressed by annealing under high hydrostatic pressures. Accordingly, a series of experiments were performed under pressures of approximately 30kbars. This pressure was the minimum under which high-temperature experiments could be safely performed in the particular pressure apparatus employed. Experiments were also designed to test high-pressure effects on the superconductivity behavior of NbJSn. The results of the high-pressure annealing experi-ments are summarized in Table I. All samples were prepared as described earlier. They were reacted and homogenized at 1000°C for 24 hr under argon at-

Jan 1, 1967

By John W. Wagner, Robert K. Willardson

Single crystals of Pbl-xSnxTe have been grown from nonstoichiometric, cation-rich melts with the objective of producing as-grown, bulk material containing carrier concentrations ranging from 1016 per cu cm to 1018 per cu cm. Three specific crystal composi-tions were investigated in detail; x = 0.00, 0.10, and 0.17. Pull rates of from I to 3 mm per hr were used. Single crystals were successfully pulled from melts containing as little as 30 at. pct Te. Hall coefficients, resistivities, and carrier mobilities of these materials were determined. The relationship between the composition of the melt and the carrier concentration in the as-grown crystal has been studied for the three crystal compositions of interest. BULK single crystals of Pb,-,Sn,Te have previously been grown from stoichiometric melts.1,2 Such crystals are p-type and have relatively high carrier concentrations ranging from -9 x 1018 per cu cm for PbTe to -8 x l020 per cu cm for SnTe at 77°K. These carrier concentrations result from deviations from stoichiometry (lead vacancies) in the as-grown crystals. Since lower carrier concentrations are desirable for electrooptic device applications, these crystals are usually subjected to long-term, isothermal anneals.&apos; This paper reports on the growth of Pbl-xSnxTe single crystals from nonstoichiometric melts with the primary objective of producing as-grown material containing relatively low (1016 to 1018 per cu cm) carrier concentrations and also reports on the general characteristics of these crystals. The phase relationships in the Pbl-xSnxTe systems are such that materials solidifying from nonstoichiometric, cation-rich melts will have smaller deviations from stoichiometry than materials grown from stoichiometric melts. Fig. 1 is the T-x phase diagram for PbTe in the vicinity of the stoichiometric composition.3 A crystal grown from a stoichiometric melt will solidify at a melting point maximum at which the solid will contain -0.5002 atom fraction of tellurium. PbTe single crystals grown in our laboratories from stoichiometric melts have carrier concentrations of 9 x 10" per cu cm, indicating that the excess tellurium in the crystals is as expected from this phase diagram. However, growth of PbTe from a lead-rich melt will result in material having a more nearly stoichiometric composition. Although the addition of Sn to the melt shifts the solidus curve further toward the tellurium-rich side,4 the general discussion given for PbTe applies to the Pbl-xSnxTe systems as well. EXPERIMENTAL Single crystals of Pb1-xSnxTe have been grown in our laboratories from nonstoichiometric, cation-rich melts using the Czochralski technique and boric oxide liquid encapsulation. The details of the growth apparatus and growth technique have been reported in a previous paper on growth of these alloys from stoichiometric melts.2 In the present study, three specific crystal compositions were investigated in detail; x = 0.00, 0.10, and 0.17. Growth of alloy crystals from nonstoichiometric melts requires considerable care, and good quality single crystals were obtained in this study only by optimizing the mechanical and thermal stability of the growth system and by using pull rates of from 1 to 3 mm per hr (Pbl-xSnxTe crystals are easily pulled from stoichiometric melts at rates of from 5 to 10 mm per hr). The liquid encapsulation technique was found to yield near-ideal conditions, since the B2O3 layer increased the thermal stability at the growth interface, permitted easy attainment of near-ideal thermal gradients, and dampened vibrations at the melt surface. The hygroscopic character of the B2O3 was a slight problem and vacuum heat treating was necessary to completely remove the water from the boric oxide. During initial growth, the seed diameter was reduced and a narrow neck (1 to 2 mm diam) of several millimeters length was grown. The latter steps were found to be necessary for the growth of single crystals, i.e., if either of these two requirements were

Jan 1, 1970

By H. W. Knott, M. H. Mueller

The crystal structures of Ti2Cu, Ti2Ni, Ti4Ni2O, and Ti4Cu20 have been determined using powder specimens examined by X-ray and neutron diffraction. Lattice constants have been determined for all four phases using X-ray powder diffraction films. Atom positional parameters of all four phases have been determined from observed neutron intensities. X-ray diffraction calculated intensity data have been presented also for the phase Ti2Cu to point out the particular suitability of neutron diffraction in this case. Interatomic distances have been determined using the positional parameters obtained from neutron diffraction. ALTHOUGH some investigations of the crystal structures have been made of these four compounds previously,&apos;-13 it was the purpose of the present investigation to expand the previous work in order to locate the various atoms, determine their coordinates, and to confirm or to correct some of the previous work. It was convenient to group these four compounds together since they are related chemicallv and/or structurally. The compound Ti2Cu is tetragonil; and Ti2Ni, Ti4Ni2O, and Ti4CU2O are all large fees of the same space group. Ti2Cu has been previously reported as a fee phase by Laves and Wallbaum;1 and Rostoker2 which was possibly the oxide phase, Ti4Cu20. Joukainen, Grant, and Floe;3 and Trzebiatowski, Berak, and Ramotow-ski4 have also reported a phase of this composition. karlsson5 has reported a small fct phase of the composition Ti3Cu which may be the presently discussed Ti2Cu phase. More recently Ence and Margolin6 have reported a small fct phase for Ti2Cu and the present authors7 together with Nevitt8 have briefly reported it to be a bet related to the fct with a co three times the length of the co of the fct and have also reported that this phase has a very limited composition. Further refinements will be reported which have varied some of the parameters of this bct structure slightly. Ti2Ni has been reported as a fee phase by Laves and wallbaum;1 Duwez and taylor;9 Rostoker;2 Poole and Hume-Rothery;10 and Yurko, Barton, and parr.11 In a later paper Yurko, Barton, and parr12 have given the complete structure of this phase based on an X-ray diffraction study which was independently confirmed with neutron diffraction by Mueller and knott.7 Additional crystal structure information will be given. Ti4Ti2O, Ti4Cu2O, and a number of other compounds including Ti4Fe2O have been reported as fcc phases by Rostoker,2 and more recently Nevitt13 has confirmed the Ti4Ti2O phase. Rostoker,2 however has reported diffraction lines for Ti4Fe2O which do not have all odd or all even indices. These lines, therefore, cannot be observed if this compound has a fee structure. This same error has crept into the diffraction results reported for TiNi2O and Ti4Cu20 in the ASTM powder data which has been credited from Rostoker&apos;s data. Complete crystal structures of these two phases will be presented. Although all four of these structures have large unit cells and hence do not lend themselves for completely resolved neutron powder patterns, a sufficient number of individual reflections was observed for solving the structure. They also serve as good examples of some of the advantages to be gained by using both neutron and X-ray diffraction techniques. EXPERIMENTAL PROCEDURE All of the alloys were prepared by arc melting. The starting metals had the following purity: Cu 99.999 pct, Ni 99.83 pct, and Ti 99.92 pct. Oxygen was introduced into the two oxide phases as chemically pure TiO2, with the remainder of the titanium coming from the above mentioned metal. All of the sample buttons were annealed in evacuated Vycor tubes, the two binary phases for 5 days at 700°C and the two oxide phases for 3 days at 900°C. Oxygen analyses were performed on all four phases by two independent laboratories with the following amounts of oxygen present in atomic percent; Ti2Cu-0.06, Ti2Ni-1.03, Ti4Ni2O-13.95, and Ti4Cu20-13.87. The stoichiometric amount for the oxide phases is 14.29 at. pct. Since all of the samples were very brittle they were easily reduced to a powder for diffraction measurements. The lattice constants given in Table I were determined for the four compounds from X-ray diffraction patterns of powder samples exposed to filtered copper radiation using a 114.59 mm diam Debye-Scherrer type camera using the Straumanis loading. None of the patterns showed a detectable amount of a second phase. The lattice constants were obtained from an IBM 704 computer program employing a least squares treatment with systematic correction terms as previously reported.14

Jan 1, 1963

By Harry L. Brown, Philip E. Armstrong

Young&apos;s modulus doto ore presented for W, Mo. Ta. V, Cr. Ni, Ti, and Zr as a function of temperature up to about 0.7 of the melting points. A plot of reduced temperature us reduced modulus produces a general correlation except for titanium and zirconium. Young&apos;s modudlus data for some representatiue commercial graphites are given up to 2400°C. All results were obtained from longitudinal resonance-frequency measzrrements of 4-in. long samples, corrected for simultaneously measured thermal expansion. Comparison of poly crystalline and single-crystal tungsten behavior indicates that all the observed modulus values are frequencv -dependent at the higher temperatures. STATIC measurements of elastic properties of materials at elevated temperatures are extremely difficult to make since the elastic behavior is obscured by relatively large first-stage creep effects. Dynamic methods which avoid this difficulty by utilizing the measurement of the resonance frequency of a simple vibrational mode have been described in the 1iterature.l-3 The authors have extended the operating temperature range of this type of measurement to above 2000°C and have described the equipment elsewhere.~ The Young&apos;s modulus data presented here were obtained with this equipment, using samples about 4 in. long and 1/4 in. diam, supported horizontally at the center and excited to the fundamental longitudinal resonance frequency. Young&apos;s modulus was calculated by the formula: E = 4f2f2p where E = Young&apos;s modulus, / = frequency, 1 = length, and p = density. Dilatometric data were obtained simultaneously by optical measurements of the change of length of the sample. For the metals tested, an attempt was made to obtain modulus values that would be representative of the pure, strain-free, randomly oriented material. All of the graphites studied exhibited a high degree of elastic anisotropy, while the method assumes an isotropic homogeneous material. However , when the values for Young&apos;s modulus obtained for AUC graphite were compared with those taken from static measurements at room temperature they were found to be only about 4 pet higher. This is excellent agreement considering the low precision of modulus calculations from stress-strain curves. The difficulty in using data of apparent Young&apos;s modulus for anisotropic materials arises when the attempt is made to use these data and shear-modulus data to obtain Poisson&apos;s ratio. The results are usually meaningless and sometimes absurd.&apos; RESULTS Table I lists the sources, impurity content, thermal history, and dilatometric constants of the metal samples that were investigated. All the metal samples were tested under a vacuum of 1 to 5 x 10-5 Torr. Where our dilatometric data agreed with previously published data, the table lists the previous values and the literature reference. Where no reference is given, the constants were determined from our dilatometric data. Table II presents the modulus data in units of millions of psi as a function of temperature in degrees centigrade. The numbers were obtained from curves fitted to the experimental data. For some types of calculations, such as those attempting to correlate creep data, the slope of the modulus curve is of interest, and this information also is reported in Table 11. It is always tempting to try to fit physical-property data into some general pattern and then use this pattern to predict the behavior of other similar materials. The general pattern for an elastic modulus of a metal seems to be a linear deoro- with increasing temperature Over the range between 0.1 and 0.4 of the melting temperature, then a progressive1y decreasing value up to the melting point. Metals appear to retain finite moduli

Jan 1, 1964

By AIME AIME

THE following paragraphs, constituting the concluding portion of the Annual Report of the Council for 1903, have been withheld from publication until now, in order to make them as accurate and complete as possible. They will be published in Volume XXXV. of the Transactions in their proper place at the end of the said Annual Report. Franklin Ballou was born in Pittsburg, Pa., May 29, 1845. He was the son of an old resident, Arthur Ballou, a manufacturer and wholesale dealer in vinegar. In early youth Franklin attended the Western University of Pittsburg, but left school at the age of 16 to become book-keeper for his father, upon whose retirement from business, in 1868, he associated himself with Walter C. Childs, of Pittsburg, in the manufac¬ture of furnace-grates and asbestos-cement for blast-furnaces. This firm was known as W. C. Childs & Co., and did a success¬ful business for several years. In 1869 Mr. Ballou married Miss May S. Wilson, daughter of Judge Wilson, of Lewistown, Pa. In 1876 he spent several months traveling in the West and studying the mining industry, which greatly interested him. In consequence of this journey, he wound up his business in Pittsburg and removed in 1877 to Georgetown, Colo., where for several years he conducted a sampling-works, and built up an extensive business as an agent for the sale of ores, besides engaging to some extent in mining enterprises. , It is said that he controlled at one time about one-eighth of the output of the Leadville mines. In the early 80&apos;s, he became Vice-President and General Manager of the Bimetallic Smelter at Leadville, of which Mr. David H. Moflat was the principal owner. This was practically the first successful demonstration of pyritic smelting in Colorado. Upon the sale of the works in 1897 to the American Smelting and Refining Co., Mr. Ballou retired

Jan 1, 1905

By H. J. Levinstein, W. H. Robinson

A method of chemically polishing silver for metal-lographic examination has been developed. The samples are prepared by polishing on 0, 2/0, and 3/0 paper. They are then polished on 600 micro-cut paper, followed by a final mechanical polish on a cloth containing 5µ diamond paste. The samples are then chemically polished in a solution of 100 cc of saturated chromic acid and 5 cc of a 5 pct HC1 solution. The chemical polishing is performed by swabbing with a cotton ball saturated with the solution. During the chemical polishing, the sample is rinsed frequently in running water. Polishing in this manner for 5 min is sufficient to remove the strained material from the previous polishing operations. The amount of material removed is approximately 4µ/min. The surface obtained is flat and free of pits. Fig. 1 is an interference micrograph of a silver surface polished by this technique. If the solution employed is of improper HC1 content, an interference color film will form on the sample. This film can be removed either by swabbing with a cotton ball saturated with ortho-

Jan 1, 1962

By Ralph W. Smith

DEVELOPMENT of the lime industry- in Ste. Genevieve County began in a crude way in 1840. According to information furnished by the Missouri Bureau of Geology, in the early days small vertical kilns built of stone were used, and wood was the fuel. Modern development began in 1904 when one company introduced steel shells lined with firebrick. Within a few years two more companies erected similar plants, and in 1925 a fourth company began operations. Thus there are today four lime companies at Ste. Genevieve, all operating at high capacity and with a gradually increasing production. GEOLOGY The limestone of Ste. Genevieve County, which has the chemical composition and purity required for lime burning, is the upper 80 or 90 ft. of Spergen formation. The Missouri Bureau of Geology, in its geological map of Ste. Genevieve County, gives the Spergen formation a total thickness of 160 ft., but only the upper portion is pure enough for lime burning, with an average raw-stone analysis of 98.7 per cent CaC03; 0.35 Si02; 0.3 R203; 0.35 MgCO3; 0.3 S03. The Spergen, one member of the Meramac group, Iowa series, of the Mississippian system, underlies an area approximately 12 miles long north and south, by 5 miles wide east and west (Fig. 1) in Ste. Genevieve County. The entire eastern two-thirds of Ste. Genevieve County is sedimentary, the formations dipping gently toward the east on an average grade of about 4 per cent, or 2 ½ º. Thus the outcrops of the various sedimentaries run approximately north and south. A line running west from Ste. Genevieve crosses the outcrops of the sedimentaries, ranging from the top of the Mississippian to the Ozarkian geological system in a space of 12 miles. Thus with the gentle dip of 2 ½ º the 160-ft. thickness of the Spergen formation stretches out in its outcrop so that it is approximately one mile

Jan 1, 1938

The Library of the above-named Societies is open from 9 A.M. to 9 P.M. on all week-days, except holidays, from September 1 to June 30, and from 9 A.M. to 6 P.M.. during July and August. The Library contains about 55,000 volumes, including sets of technical periodicals and the publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library can render valuable service through correspondence; letters requesting information-will receive special attention. The Library is prepared to furnish references and copies of articles on mining and metallurgical subjects; to determine the existence of mining-maps, and to furnish general information as to the geology and mineral resources of all countries: All communications should be made as definite as possible so that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will be sent more promptly and in more usable shape. The members of the Institute. can be of service to the Library by forwarding copies of mining-reports, maps privately issued, and similar material, which will he classified, indexed, and made available to other members. Suggestions for additions to the Library, either by purchase or personal solicitation as gifts, will be welcomed. It is hoped that members while in the city will use the Library freely, and assurance is given that most careful service will be rendered to them.

Jan 5, 1913