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Discussion of the paper of Earl S. Bardwell, presented at the Butte meeting, August, 1913, and printed in Bulletin No. 79, July, 1913, pp. .1429 to 1441. H. O. HOFMAN, Boston, Mass. (communication to the Secretary*) :-It is pleasing to the originators of the planimetric determination of oxygen in refined copper to see that the method has been taken up by a large smelting plant to be used in every-day work after it has been simplified to suit the new conditions. Several years ago Huntington and Desch 1 had improved our mode of working. They projected the developed negative on to a screen, traced the outlines of the picture with a pencil, drew a border, and measured one constituent with. the planimeter. In order to give the work greater precision, they divided the area into squares of 1 cm. side, shaded the

Jan 11, 1913

By D. S. Newton

Introduction Historically the production of zinc dust has been based upon residual and secondary zinc. Using horizontal retorts filled with diecasting scrap, galvanizers drosses and sweater billets, dust has been produced by condensation into static condensers on a 24 hour cycle. Although fairly flexible as regards input materials the process is not amenable to close control of the product, is labour intensive and unless carefully run can cause fume problems. With a steadily increasing demand for zinc dust of consistent properties and higher quality there is a demand for an improved method of manufacture in which dust can be produced continuously and which is capable of close control thus ensuring a minimum amount of oversize or unsaleable material. The Process in use in the works of Imperial Smelting Corporation (Alloys) Ltd. in England, and in Canada and Holland, satisfies the criteria stated above, and has proved to be easy to control with a minimum labour demand.

Jan 1, 1970

By J. D. Forrester, Erich Sarapuu, T. C. Cheasley

John G. Tripp-—The concept of converting fuel deposits in-situ to useful forms of energy and chemical raw materials has important possibilities as a means of stretching out our fuel resources. The authors have worked in this field for years and in fact are among the pioneers in developing in-situ techniques based on underground electrocarbonization. Their efforts have aroused great interest in this subject and their contributions will undoubtedly gain even more significance as time goes on. The 4 to 5 billion tons of petroleum are proved reserves, that is, they are completely defined and could be produced economically with present methods of recovery. Reserves of coal, tar sands, and oil shale shown in Table I are not equivalent to proved reserves as the term is used in the oil industry. Incidentally, the 4.3 billion tons of oil shown in the tabulation is equal to about 28 billion barrels of oil and, therefore, presumably does not include reserves of natural gas liquids estimated at about 5 billion barrels. The relative comparisons would be more complete if these liquids together with the reserves of natural gas were included in the tabulation. It is stated in the report that production costs of the order of 10c per million Btu's could be expected from a large industrial electrocarbonization installation. The authors state that the operation probably could be operated successfully and at a profit. I would like to express my view that for the operation to be profitable extremely favorable conditions would have to prevail. For example, the coal seam would have to be thick and close to the surface in order to minimize drilling costs; the deposit should be dry and so situated that there would be little, if any, inflow of ground water; and the seam would have to be relatively gas tight to avoid excessive gas leakage. Notwithstanding the tremendous strides that have already been made, it is my hope that the authors plan to continue their development work. Experiments on underground electrolinking and initial carbonization at Gorgas, Ala., indicate a need for improved control over the operation. Subsequent examination of the underground system at Gorgas has shown that the gasification zone did not always follow a direct path between the electrodes. Undoubtedly the control of the in-situ thermal processes can be improved by further development work. With respect to the electrocarbonization of oil shale it may be well to point out that the cost of mining oil shale is estimated to be 50c to 60c per ton. These are low mining costs as compared to coal. Thus it would appear that there is less economic incentive for applying in-situ thermal methods to oil shale than there is for applying these methods to coal. As is the case with in-situ methods for petroleum, the product from the shale having the most economic interest would be liquid oil rather than gas. The authors point out that for distances up to several hundred miles it is cheaper to transmit energy as electricity than it is to ship energy as coal. This is a very important point, and with coal shipping rates rising periodically, it could prove increasingly important in the future. I believe that the authors deserve great credit for their outstanding work on underground electrocarbonization. The knowledge resulting from their efforts is of great value to our fuels technology. James L. Elder—The experimental work conducted by the authors on the electrolinking-carbonization of carbonaceous materials in situ is of great interest. The method is of great importance in the development

Jan 1, 1955

By H. M. Strong, R. A. Oriani

THE technological interest attaching to light, age-hardening alloys for structural uses has been pointed out to one of us.1 A potentially interesting alloy would be titanium-rich Ti-Mg alloy, provided that sufficient solid solubility exists. or could be induced at high pressure. and provided also that age hardening can be induced by proper temperature and/or pressure annealing. It was decided therefore to explore the feasibility of producing a Ti-Mg alloy in the high-pressure apparatus. Experimental. Three high-pressure runs have been carried out. In each case the geometry of the sample was that of a cylinder of titanium of commercial purity, into which a narrow hole had been drilled along the axis; this hole was filled with magnesium wire,

Jan 1, 1967

SULFURIC ACID U.S. 4,070,260 - Sulfuric acid leaching of willemite, hemimorphite, or other zinc silicate ore. Ore is leached with at least a stoichiometric amount of a IN to 6N sulfuric acid solution at a temperature near its boiling point to form a gelatinous mass of hydrated silica and zinc sulfate, the water in the mass partially evaporated to crystallize all of the silica, the mass treated with hot water to dissolve substantially all of the zinc sulfate, the suspension filtered, and zinc values recovered from the filtrate by electrolysis. N. Dreulle, assigned to Compagnie Royale Asturienne des Mines. Jan. 24, 1978. 3 pp. (204-119). Filed: 2-10-76 (656,966) . Priority: France, 2-14-75 (75/04594) .

Jan 1, 1979

By C. A. Sobotowski, J. Eagan

Computer programs applicable to coal mining have been available for some time, especially in the academic sector. However, the computer has not routinely been applied to actual mining operations. This paper discusses how a computer system was set up as an important tool in mining design and decision making. The project was completed within the allotted timeframe of two months by taking advantage of existing technology. Key points include the selection of programs to meet the specified needs of the project, conversion of the programs to be compatible with a computer of a different manufacture, simplification of the data entry process, development of procedures for using these programs, and an explanation of how the reports generated from the programs were used for mine planning and decision making.

Jan 1, 1983

By W. E. Newberry

The Aspen Mining District is situated at the eastern edge of the system of stratified rocks of western Colorado, where this edge meets the ridge of metamorphic granite which divides the State into two unequal parts. In following the valley of the Roaring Fork westward from the continental divide towards Aspen, one passes through a country of granite and gneiss, with no sedimentary rocks until the town is nearly reached. At this point the Cambrian quartzites first make their appearance, lying on the granites, with a dip of from 30' to 45 to the northwest. Beyond these quartzites and conformably upon them lie dolomites, limestones, shales, porphyries and sandstones, gradually flattening in general dip as one proceeds westward, but much disturbed by local foldings and faultings.

Jan 1, 1890

By Arthur F. L. Bell

Discussion of the paper of ARTHUR F. L. BELL, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 105, September, 1915, pp. 1769 to 1799. WILLIAM A. WILLIAMS, San Francisco, Cal.-Is the Union Avila plant run as a topping plant or as a dehydrating plant? A. F. L. BELL, San Francisco, Cal.-Both. It takes off an average of 20 per cent. water besides topping the oil. Part of the crude oil is run through an electrical separator before running to the topping plant, but the entire crude averages about 20 per cent. when it enters the topping plant. DAVID T. DAY, Washington, D. C.-I suppose most of the work contemplated in these large topping plants is simply to deal with topping the oils with only a small percentage of water in them. A. F. L. BELL.-Not more than 2 per cent. of water can be handled in ordinary stills without causing trouble. At our Gavotte refinery, where the oil runs from 15 to 30 per cent. water, we carry 20 lb., pressure oil our stills to hold the framing down, we can do that with small stills, with large one's it would not be safe; but with a retort, the quantity of water contained in the oil does not affect its working. It simply means additional fuel to evaporate the water.

Jan 12, 1915

By Campbell Hunter

PETROLEUM is found in almost every province in Persia. On the northern frontier, along the southern shore of the Caspian Sea, it is found near Anzelli and Shakhtesar and gas at Khoremabad. Oil is also found at Gumush Tepe, northwest of Astrabad, on the southeastern shore of the Caspian Sea. Further inland, to the south of Astrabad, oil is found at Schahkuh-i-balae, also on the margin of the Khorasan desert at Semnan, 115 mi. (35 m.) east of Teheran. Along the western frontier, from northwest to southeast, oil is encountered at Ouschachi, north of Lake Urumieh; in the province of Azerbaijan, at Zohab, Khanikin, and other places in the district of Kormanshah in the province, of Ardelan. Further south, in the province of Luristan, oil is found east of Mendeli and in the Pusht-i-kuh districts. Considerable quantities of oil are also obtained from Schuster, Maidan-i-Naphtun, Ram-Hormuz, Beheban, which are almost on a straight line, running northwest and southeast along the foothills of the Bakhtiari Mountains. At Ahwaz, in the province of Arabistan, oil has been found along another range of hills whose axis also lies in a northwest-southeast direction. In the Fars province, boring for oil has taken place at Daliki, and indications of oil are found at Kheri, Fasa, Darab, and other places. A gas show is also recorded at Kuhi-Sung-Atush in this province, 30 mi. (48 km.) east of Darab. In the south of Persia, oil is encountered on. Qishm Island, also at Ahmedi and other places north of Bunder Abbas. On the southeastern frontier, oil is found on the Sarhad range of hills. Thus, oil indications have been noted over a distance of approximately 1100 mi. along the western and 700 mi. along the northern frontiers of Persia.

Jan 2, 1920

By Don Simon

In the late 1960s the mining industry was in an apparent slump due to a combination of factors. Enrollment dropped significantly at schools offering mining engineering degrees, resulting in a shortage today of experienced mining graduates to staff middle management positions. How has this limited supply affected salaries? Does the shortage impair the mining industry's ability to respond to national energy needs?

Jan 12, 1979

By J. Van Steveninck, A. C. Pols, R. Feenstra

In the course of time, an increasing number of investigations on jet cutting all kinds of material, such as rock,1,2,3 metal,4,5 and wood6 have been reported to serve various applications. A number of papers have been published on these subject, 7,8,9 some of which refer to jets purposely containing abrasives, termed 'jetted particle drilling'.7 Since such abrasives complicate fluid handling considerably and do not appear to be absolutely necessary for making holes, only conventional drilling fluids have been considered. A large part of our investigation has been performed with the aid of three laboratory-type drilling machines, which permit tests on both micro-bits (1 ½ in. ) and full-scale bits (6 ½ -9 5/8 in. ) . In view of the application of jets in deep holes, care has been taken to simulate hydrostatic pressures as they exist in the field on the hole bottom. These have been found to have a major effect on the bit-penetration rate for various drilling fluids.

Jan 6, 1974

By S. Whinery

In these times of sharp rivalry, both as to price and quality, among the makers and venders of engineering explosives, it is often desirable to be able to determine the relative energy or value of the various explosives offered for sale, in order to purchase intelligently ; or, having contracted for a large amount of an explosive of a certain standard quality, to be able to ascertain if the manufacturer keeps his product up to the specified standard. The simple and inexpensive apparatus described below was devised by the writer while engaged on the improvement of the Tennessee River, at MuscleShoals, under the direction of' Major W. R. King, U. S. Engineers, in the summer of 1879. It answered the purpose so well that it is thought that a brief account of it may be of interest to other engineers. It consisted, essentially, of an old blacksmith's anvil and a common striking hammer, such as is used for driving rock-drills. The anvil was placed face downward on solid, level ground. In what was then the top of it, a vertical hole, one and one-fourth inch in diameter and about one arid three-fourths inch deep, was made with a ratchetdrill. The surface of the anvil immediately around the drill-hole was made as true and smooth as possible with a file. Next, a new striking-hammer, weighing nine pounds, with a turned and true face, was selected ; and a handle, eleven feet long and about one and a half inches in diameter, was fitted into it so that it

Jan 1, 1886

By A. H. Tousley

The cement industry is on the horns of an economic dilemma. Within the last ten years, its over- capacity in the United States has varied from 139- 127% of demand (Fig. 1). The most direct effect of this is seen in cement prices, which reached a peak in 1960, retreated steadily through 1966 and only recently climbed back to the 1960 level again. With prices in a slump and production costs estimated to be up almost 30%, there has been a steady drain on cement profits. Since 1960, labor costs have increased 86% while fuel costs have risen 18%. Meanwhile, customer service costs have also soared owing to the competition for cement customers and the wider variety of available cement products. This search for sales advantage has in turn led to a higher Blaine number, which means more grinding and hence bigger mills, more power, and, once again, higher costs. New plants as well as expansions and revisions to existing plants are also costing more owing to higher

Jan 1, 1971

By H. M. Morse

This report covers the period from Jan. I, 1943 to Dec. 31, 1943. During the year, II2 wells were drilled in Mississippi, as foilows: wildcats drilled and abandoned, 54; wildcats producing oil, 4; oil wells drilled in oil fields, 26; oil wells drilled in fields, dry and abandoned, 10; sulphur-test wells drilled, 14; salt-water-disposal wells, 3; core tests, I. Prospecting Geophysical work in Mississippi during 1943 amounted to 1127 crew weeks, divided as follows: reflection seismograph, 809 weeks; gravity meter, 285; magnotometer, 30; torsion balance, 3. A considerable amount of core drilling was done over a large part of the state. The complete data on this activity are not available at the present time. Salt Domes To date, the following salt domes have been discovered in Mississippi: Midway, Edwards, Glass, Newman, Tatum, Oak-vale, Kings, Halifax, D'Lo, Hazlehurst, Byrd, Leedo, Prentiss, Carson, Moselle, Monticello, Ruth, Keno, Taylorsville. New Oil Fields Lincoln County.—On March 10, 1943, the California Company completed its Smith No. I in sec. 4, T. 7 N., R. 7 E., Lincoln County, as an oil well and produced 29 bbl. of 25" gravity oil in 24 hr. through a fi-in. choke. Two outpost wells have been drilled in this area by the California Company, and both have been abandoned as dry holes. Madison County. —Love Petroleum Co. completed its J. R. Anderson No. 2, sec. 2, T. 8 N., R. I W., Madison County, on Sept. 7, 1943. This well produced 135 bbl. of approximately 30" gravity- oil in 24 hr. through a )/4-in. choke. The production comes from a sand or porosity in the upper part of the Chalk formation of the Cretaceous age. Adams County.—The California Company drilled its National Gasoline Co. of Louisiana No. I in sec. 52, T. 7 N., R. I W., to a total depth of 10,383 ft., and at 10,280 ft, it perforated and obtained gas and a condensate. The well had several showings in the Wilcox of the Eocene age. Several of these showings were tested and the well finally was completed at 5888 ft. on Oct. 6, 1943, producing 44" gravity oil in the second sand in this formation. No other wells were completed in this field during the year. However, a number of wells are contemplated in the near future, and locations have been staked by the California Company. The Oklahoma Pipe Line Co. will market the oil through its pipe-line facilities. Wayne County.—The Gulf Refining Co. drilled Davis No. I in sec. 2, T. 9 N., R. 9 W. in Wayne County. After several stem tests 545'-in. casing was set at 6850 ft. and production was obtained in the so-called Massive Sand of the Lower Tuscaloosa. The well produced 359 bbl. of oil in 24 hr., and it Was completed on Oct. 4, 1943. Other locations have been staked ill this area and probably will be drilled in 1944 by

Jan 1, 1944

By H. M. Morse

This report covers the period from Jan. I, 1943 to Dec. 31, 1943. During the year, II2 wells were drilled in Mississippi, as foilows: wildcats drilled and abandoned, 54; wildcats producing oil, 4; oil wells drilled in oil fields, 26; oil wells drilled in fields, dry and abandoned, 10; sulphur-test wells drilled, 14; salt-water-disposal wells, 3; core tests, I. Prospecting Geophysical work in Mississippi during 1943 amounted to 1127 crew weeks, divided as follows: reflection seismograph, 809 weeks; gravity meter, 285; magnotometer, 30; torsion balance, 3. A considerable amount of core drilling was done over a large part of the state. The complete data on this activity are not available at the present time. Salt Domes To date, the following salt domes have been discovered in Mississippi: Midway, Edwards, Glass, Newman, Tatum, Oak-vale, Kings, Halifax, D'Lo, Hazlehurst, Byrd, Leedo, Prentiss, Carson, Moselle, Monticello, Ruth, Keno, Taylorsville. New Oil Fields Lincoln County.—On March 10, 1943, the California Company completed its Smith No. I in sec. 4, T. 7 N., R. 7 E., Lincoln County, as an oil well and produced 29 bbl. of 25" gravity oil in 24 hr. through a fi-in. choke. Two outpost wells have been drilled in this area by the California Company, and both have been abandoned as dry holes. Madison County. —Love Petroleum Co. completed its J. R. Anderson No. 2, sec. 2, T. 8 N., R. I W., Madison County, on Sept. 7, 1943. This well produced 135 bbl. of approximately 30" gravity- oil in 24 hr. through a )/4-in. choke. The production comes from a sand or porosity in the upper part of the Chalk formation of the Cretaceous age. Adams County.—The California Company drilled its National Gasoline Co. of Louisiana No. I in sec. 52, T. 7 N., R. I W., to a total depth of 10,383 ft., and at 10,280 ft, it perforated and obtained gas and a condensate. The well had several showings in the Wilcox of the Eocene age. Several of these showings were tested and the well finally was completed at 5888 ft. on Oct. 6, 1943, producing 44" gravity oil in the second sand in this formation. No other wells were completed in this field during the year. However, a number of wells are contemplated in the near future, and locations have been staked by the California Company. The Oklahoma Pipe Line Co. will market the oil through its pipe-line facilities. Wayne County.—The Gulf Refining Co. drilled Davis No. I in sec. 2, T. 9 N., R. 9 W. in Wayne County. After several stem tests 545'-in. casing was set at 6850 ft. and production was obtained in the so-called Massive Sand of the Lower Tuscaloosa. The well produced 359 bbl. of oil in 24 hr., and it Was completed on Oct. 4, 1943. Other locations have been staked ill this area and probably will be drilled in 1944 by

Jan 1, 1944

By W. R. Crane

While professiorlally engaged in the oil- and gas-fields of Kansas, in measuring the pressure and flow of gas-wells, and studying the phenomena attendant upon the production of both oil and gas, I noticed in the flow of gas a peculiar and interesting feature. That there are actual lines of flow in liquids (non-compressible fluids) discharged through an orifice, or a short section of pipe, is shown by the external shape of the discharge—the vena contracts. Such lines of flow are not observable in the discharge of gas from an orifice. It can hardly be questioned that they exist. That they are not apparent is probably due to the very small weight of the gaseous particles, which climinishes the momentum of their movement in a given direction, acquired before they issue from the orifice, and also to the expansion of the gases, which would exert a powerful influence in overcoming any such tendency in their flow. Gas flowing from an orifice, supplied by a large reservoir or blowing-engine, exhibits almost the reverse of what is noticed with liquids. Namely, the gas assumes the form of an inverted truncated cone, of large angle: with its apex-end at the orifice. (See BB, Fig. 1.) This external ahape assunled by the flow of gas shows, however, marked differences under varying conditions of volume and pressure. For instance, a large volume of gas under high pressure, flowing through a 2- or 3-in. pipe, as in the case of a natural gas-well, assumes a more definite conical form, the angle of which increases as the pressure falls. Moreover, outside of the well-defined inverted cone is a thin conical heath or zone of gas, A A, the angle of which is considerably greater than that of the main cone, and increases with +1UNIVERSITY OF KANSAS, LAWRENCE, KANSAS.

Jan 1, 1905

By E. Tulcanaza

The practical significance of the in situ grade variability is usually neglected. Although recognized, often times it is either ignored or just considered as a vague guideline in many of the decisions dealing with exploration, reserve estimation, and mine planning. This paper stresses the significance of grade variability for exploration and mining, and illustrates its liaison to the structural features of the ore deposits, as well as to the mining parameters used for mine extraction. Some geostatistical results obtained from a silver mine, tungsten mine, and copper mine in South America are discussed.

Jan 1, 1985

By Frederick Burbridge

The Morning silver-lead-zinc mine of the Federal Mining & Smelting Co. is about 'two miles northwest of Mullan, Ida. The lode is a metasomatic fissure vein. The orebody is approximately 2000 ft. long within the bounds of the property and varies in width from knife edge stringers to 50 ft. It has been developed to a depth of 3600 ft. and stands nearly vertical in Revett quartzite, which .strikes north 65" west. The high-grade veins and lenses are generally mixed with waste (siderite, quartz, and quartzite). The average grade of ore to sorting plant in 1921 was 4 oz. silver per ton, 8.6 per cent. lead, and 4.1 per cent. zinc. Wall rock stands only a short time without timbering. The minimum angle of gravity flow is 45". The ratio of waste sorted out to ore is 6 per cent. No gases are generated underground and temperature has no influence on mining operations. Fresh air is forced down the air raise and up the main shaft. Drifting and Stoping Main drifts 12 ft. wide and 13 ft. high are driven every 200 ft. (vertically) and are connected by raises 125 ft. apart. These raises consist of three compartments (chute, tramway, and timber slide) and are for the purpose of ventilation, access, and hoisting supplies to stopes. Ground is stoped between raises. Chutes are placed every 25 ft. for drawing off ore broken in stopes. Waste for filling is obtained from waste raises off the stope in walls or waste is dumped from the level above down the chute compartment of raises, which is bulkheaded so that waste can be drawn off at any floor as required. Timbering Posts and caps for square sets (varying in diameter from 6 to 24 in.) are cut to length in a sawmill on the surface. No preseratives are used. Timber is taken on a flat car along drifts to a raise nearest the working place and hoisted as required. Practically no timber is salvaged for

Jan 1, 1925

By Charles Wert

THE diffusion and precipitation of carbon and nitrogen in a iron have previously been investigated using the internal friction as a measuring tool.' Most of this work has been done on rather pure iron; no effect was observed which would indicate that either of these phenomena is affected by the rather small amounts of impurity found in these samples of iron. Fastz observed, however, that both the diffusion rate and the aging properties of nitrogen in iron were sensibly changed by the addition of Vz pet Mn. The diffusion rate at a given temperature is reduced and the nucleation of nitrides is apparently changed somewhat. He observed no such changes for carbon in this alloy. Later Dijkstra and Sladek" extended these observations on nitrogen to other alloys of iron. They found that metals other than manganese also influence the behavior of nitrogen in iron; chromium, molybdenum and especially vanadium affect the diffusion and precipitation of nitrogen even more than manganese does. Their results have been verified in all essential details by this author, who finds in addition that small additions of nickel have about the same effect on the diffusion of nitrogen as the same amount of manganese. The present work was undertaken to study the effect on carbon in iron of these alloying elements. The alloys used had two sources. The material used as a "standard" (designated Fe in this paper) in the measurements was some iron supplied by J. K. Stanley, of Westinghouse Electric Corp., who reported 0.01 pct 0, as the only major impurity. He also made up an alloy of 0.26 pct Ni and one of 0.9 pct Mo using this same iron as a base. They were supplied by him in 2 lb billets, which were sawed into rods and cold formed into 0.030 in. wires for measurement. The alloys of chromium, manganese, and vanadium were prepared by the metallurgy section of the Institute for the Study of Metals, University of Chicago, by adding these metals in turn to vacuum melts of National Research Corp. iron. The small castings prepared in this way were also cold formed into 0.030 in. wires. After these wires had been prepared they were decarburized for 30 min at 730°C in wet Hz. After this treatment, no trace of carbon (as measured by internal friction) could be found. All specimens were then carburized for about 15 min at 710°C and water quenched. By this treatment the internal friction at 40°C was raised to a Q-' ~ 0.015. The diffusion of carbon in these alloys was studied by observing the shape and position of the internal friction peak at 0.9 cycles per sec. These measurements were made using a torsional pendulum in a manner described earlier.' The data are plotted in Fig. 1. It is seen that there is no apparent difference in internal friction between the various alloys. This is in marked distinction to the broadening and shift-

Jan 1, 1953

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

The system Nh-Ir was investigated over the complete concentration range by metallography and X-my techniques, using forty one alloys. The solubility limits of terminal and intermediate phases and the solidus temperatures were determined. Five intermediate phases were found: a Nb3Ir, cubic, Cr3O type; tetragonal, ofecr thorhomhic, isostruc-turn1 with (ta-Rh); and a Nhlr3. cubic, AuCu, type. a Nb3lr and a Nbfr3 melt congruently; three eutectic and three pentectic reactions occur. The phase diagram of the Nb-Ir system had not been fully treated in the literature; only surveys of intermediate phases were found.1"5 In this study, the details of the phase boundaries were investigated as well as the crystallography of the intermediate phases. EXPERIMENTAL METHODS The experimental procedures such as arc melting of powder compacts, heat treatments, solidus measurements, X-ray, and metallographic observation were identical with those used in the work on the Nb-Rh phase diagram.&apos; They will therefore not be repeated here except where the conditions differed. The purity of the niobium powder was as stated in Ref. 6; the iridium powder of 99.9+ pct purity from J. Bishop and Co., Malvern, Penn., did not contain impurities exceeding 100 ppm, except rhodium (200 ppm). The melting points and vapor pressures of both elements are very similar. This fact contributed to a very small weight loss on melting and facilitated preparation of homogeneous alloys. As shown in Ref. 6 for Nb-Rh, no oxygen pick-up exceeding 200 ppm had to be considered; this was regarded as valid also for Nb-Ir. A total of forty one alloys were used in the determination of the phase diagram; their concentrations are shown in Fig. l, which presents the phase diagram. The concentration limits as determined by the weight-loss method averaged <0.2 at. pct, and never exceeded 0.5 at. pct. Heat treatments were carried out as described in Ref. 6. Depending on the concentration, only tantalum, tungsten, or iridium containers were employed, avoiding oxide crucibles altogether. Alloys from 0 to 25 and from 65 to 100 at. pct Ir were homogenized at 2095°C for 15 hr, intermediate compositions from 25 to 65 at. pct Ir for 65 hr at 1780°C. A typical annealing-time schedule is presented in Table I. Solidus points were measured as described in Ref. 6 with the modification that samples rich in niobium were held between pieces of tantalum foil and samples of high iridium concentrations were held between rhenium platelets or in iridium wire. After each run it was ascertained metallographically that no reaction with the holder had occurred. Rhenium was selected as holder material after it had been shown in separate tests that the melting points of Re-Ir alloys rise continuously from 2440°C. Metallographic examination was carried out as described in Ref. 6, and the same procedure and etchants were used successfully. While metallographic discrimination between a Nb3lr and o was easily possible, X-ray diffraction was necessary to separate al and ct2. X-ray powder patterns were taken and evaluated as for Nb-Rh6 yielding the error limits indicated in Table 111, to be introduced later. For the determination of the invariant reactions and phase boundaries, the same techniques as for Nb-Rh6 applied. The general accuracy of invariant concentrations is regarded as somewhat higher than for Nb-Rh due to the small slope of most solvus lines.

Jan 1, 1964