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By H. J. de Haan, J. van Lookeren

In view of their size and favorable characteristics, Shell's heavy-oil fields on the eastern coast of Lake Maracaibo, Venezuela — known as the "Bolivar Coast" — are obvious candidates for the application of thermal recovery methods. During the last decade various methods have been tested, such as steam drive,', steam soak and in-situ combustion.3 Steam soak was discovered as a promising production method rather accidentally in 1969, during early steam drive testing in the Mene Grande Tar Sands1 When steam erupted at the surface due to breakdown of the overburden, the injection wells were back-flowed to relieve the reservoir pressure. This resulted in high oil production rates, all the more impressive because the reservoir is unproducible by primary means. It was concluded that injection of limited amounts of steam might be a very effective method for stimulation of heavy-oil wells. To obtain information that would be more widely applicable, testing of the process was continued in the eastern part of the Tia Juana field (Fig. 1). Here even more favorable results were obtained than in Mene Grande. This created sufficient confidence to prompt a large-scale project, which was considered essential for an adequate evaluation of ultimate recovery, steam requirements, mechanical problems and economic prospects. To obtain an early answer on the ultimate recovery a fairly depleted area was selected in the western part of the same field ("A" in Fig. 1). The first steam was injected in March, 1964. This paper describes the performance until the end of 1966. The production mechanism and well inflow performance are discussed in some detail. In view of the favorable results obtained so far, steam soak operations have expanded considerably since the start of this project. Presently, five other projects are under way, of which two are about the same size as the one under discussion, with further extensions being programmed. Description of the Project Reservoir Data Shell's part of the Main Tia Juana reservoir has a proven area of 8,800 acres and an average net oil sand thickness of 130 ft. It contained an initial quantity of 2,750 million bbl of stock tank oil (STOIIP), with an API gravity ranging from 10 to 15 API and a viscosity of 100 to 10,000 cp (at 122F). As a geological unit it is known locally as the Lower Lagun-illas member of the Lagunillas formation, which is early Miocene in age. The sand bodies are believed to be distributary channel sands deposited in a lower coastal plain. Most of the channel sands have lateral and some vertical communication. The field was developed mainly in the period from 1936 to 1950. The ultimate primary recovery is estimated at 18.1 percent of STOIIP, of which 12.5 percent STOIIP had been produced by the end of 1963 from some 540 wells. By then the average pressure had decreased from an initial value of 960 to 550

Jan 1, 1970

By T. G. Sieber, T. D. Tiemann

The extraction of quartz from siliceous iron ores by dissolution in sodium hydroxide solution has been described in detail in AIME Transactions. l923 data reported covered the temperature range from 230-416°F, where a continuous increase in the amount of silica extracted with increase in temperature was found. It is the purpose of this paper to describe some unexpected results of more recent work exploring principally the range of 500600°F where higher rates and greater amounts of silica extraction were antici-p ted. In brief, the experimental procedure consists in digesting the ore under pressure in solutions of sodium hydroxide, filtering the suspension and weighing and analyzing the dried residue for iron content. The amount of extraction is calculated from the weight loss or from the iron analysis of the residue and that of the original ore.

Jan 1, 1969

Who's Who in Mineral Engineering - The 1979 Directory of the Society of Mining Engineers of AIME

Jan 7, 1979

By Charles E. Wait

IT is said by some that the occurrence of a deposit of sulphide of antimony in Southwestern Arkansas has been known for fifteen or twenty years. Whether or not such is the case I am not prepared to say, but I am not able to find any record of such a discovery, or any analysis of antimony ore obtained from that section, published at so early a period. The present discoveries, that seem to be attracting some attention, date back to the winter of 1873-74. At that time a vein of ore was found by Mr. Robert Wolf, in honor of whom the vein was named, and still is called, "the Wolf lode." At the time of the discovery the ore was unknown to the prospector, and its composition was not thoroughly understood in that locality until samples were sent to several analytical chemists, who pronounced it sulphide of antimony-stibnite. Since the discovery of this ore there have been three mines opened, and a number of interesting minerals of the antimonial series have been found. I have had an unusually good opportunity to collect specimens from these mines; and it is owing to the constant inquiry concerning the character of these ores that I have collected for publication the results of quite a number of analyses, sufficient I trust to clearly point out their composition. This is one of the few localities in the United States where antimony ore is found in workable quantities; I say workable quantities, because two different shipments of ore have been made to English reduction works, and in both cases excellent returns were made. The discovery of these deposits will, it is hoped, give rise to a prosperous and remunerative industry at no distant day, and when fully developed they may yield ore in sufficient quantity to supply the regulus for the home demand, thus adding wealth not only to those interested, but also to the State of Arkansas. The three mines are situated in the northern part of Sevier County, and may be reached by the St. Louis, Iron Mountain and Southern Railway to Fulton, thence by wagon-road to Columbus, Nashville, Centre Point, and to the mines. During most seasons of the year the

Jan 1, 1880

By J. C. Bierlein, R. A. Dodd

Endurance strengths at 10' cycles, fatigue-hardening rates, and endurance strength/0.2 pct proof stress ratios have been determined jbr a range of Cu(Ni), Cu(Si), and S.R.0. Cu(Au) solid solutions. Some douht is cast on simple cross slip models of fatigue hardening in view of opposite composition dependencies of hardening displayed by Cu(Si) and Cu(Au). The temperature dependencies of hardening also are the opposite of predictions made on the basis of a cross slip model. A correlation apparently exists between the fatigue strength/0.2 Pc~ proof s1.re.s~ ratios and rates of fatigue hardening. An increase in PS/PS due to alloying or temperature change is accompanied by a decrease in hardening rate, and vice versa. In recent years there has been much interest in the determination of the dislocation structure of fatigued metals and alloys. The accumulated evidence, e.g., Refs. 1 to 5, suggests that the structure may be dependent on the stacking fault energy, 7, of the fatigued metal in the same way that fatigue hardening rates have also been shown to apparently depend on u .6' 7 The above research followed the various earlier theories relating crack nucleation to ease of cross slip, e.g., Refs. 8 to 131 so "ggesting that y may indeed be the parameter of principal significance in all facets of the fatigue process. However, comparatively little attention has been paid to correlating engineering fatigue data with observations of the above type. Certainly, it would be useful if potential engineering fatigue performance could be assessed from a knowledge of easily determined alloy properties, and the present research originated from this standpoint. TO investigate the widest Possible range of 7 would require the use of two solvent bases, e.g., aluminum and copper, but a reasonable coverage can be provided by copper-based solutions alone. Therefore, it was decided to work with Cu(Ni) and Cu(Si) solid solutions, the approximate stackillg fault energies of which are given in Table I. The y range extends from low, Cu(7.5 at- Pet Si), to moderately high in Cu(2-5 at. ~ct ~i) and two of the Cu(Ni) alloys. The values listed in Table I should be regarded as qualitative only, being derived as follows. Dillamore and smallman14 quote a value of 85 i 30 erg.cm-2 for the stacking fault energy of pure copper, based on an earlier value due to Howie and swannl5 corrected by Brown's formula.'' Since the ratios (alloy)h(pure copper) have been reported17,18 for Cu(Ni) alloys containing up to 30 pct Ni, approximate ) values for these alloys can be computed, and a rough estimate of 7 for Cu(50 at. pct Ni) obtained by extrapolation. The relatively low y value obtained in this way for Cu(50 at. pct Ni) coincides with the observation of Nakajima19 that the stacking fault probability is a maximum at this composition. Likewise, the y values for the three ~u(~i) alloys are estimates based on values given by Swann and Nuttingo corrected on the basis Of Brown's estimate that the true 7 values are probably 2.3 times greater than those originally computed. In addition to the above alloys it was decided to investigate short-range ordered (s.R.O.) CU(AU) alloys containing up to 25 at. pct Au. This last alloy has been shown to have a well-defined planar arrangement of dislocations when deformed,21,22 probably due to cross slip being restricted by the S.R.O. Engineering fatigue data was to be represented by the determination of endurance strengths, and these were to be correlated with fatigue hardening and mechanical property data. EXPERIMENTAL I, order to study the desired properties and property changes, the following alloys were prepared: Cu(2.5 at. pct Si), Cu(5.0 at. pct Si), Cu(7.5 at. pct Si), Cu(5.0 at. pct Ni), Cu(25.0 at. pct Nil, Cu(50.0 at. pct Ni), Cu(5.0 at. pct AU), Cu(15.0 at. pct AU), Cu(25.0 at. pct AU). The copper and gold were zone-refined, while the silicon was semiconductor grade. The nickel was of 99.95 p,t. purity.* All alloys were induction-melted in a *Kindly supplied by the International Nickel co. helium atmosphere, appropriate precautions being taken to avoid segregation in the Cu-Au series. Rod stock was obtained by rolling and swag,ng. A few Bridgman single crystals were grown for fatigue-hardening studies, but most material was machined into polycrystalline fatigue speciments of the design shown in Fig. 1, and into polycrystalline tensile and fatigue-hardening specimens of simple cylindrical design. All specimens except Cu(Au) were annealed; the latter were quenched from above T, to produce short-range order. A few of the quenched alloys were examined for long-range order by step-scanning over

Jan 1, 1969

Jan 1, 1967

By E. H. Jr. Dix

THE importance of aluminum-silicon alloys in the light alloy field is now generally recognized. Where silicon was once considered detrimental to the properties of aluminum, useful alloys now contain as much as 13 per cent. Furthermore, silicon is present as an impurity in aluminum of even the purest grades. Iron is another important impurity in aluminum and like silicon is found in small quantities in the purest aluminum available today. The manner of occurrence of iron and silicon in commercially pure aluminum and many of its alloys exerts, a very pronounced influence upon their properties. The effect of large quantities of iron in aluminum-silicon alloys is so detrimental that it has been found necessary to limit the allowable maximum percentage to as low a figure as is consistent with quantity production and satisfactory physical properties. The intimate relation existing between iron and silicon in aluminum and aluminum alloys makes necessary a more complete knowledge of this ternary system. This paper is divided into two principal parts, dealing respectively with aluminum-silicon solubility equilibria and the constitution of aluminum-iron-silicon alloys.

Jan 1, 1927

By H. R. Hanley

The characteristics of alloyed anodes and their influence on the products of electrolysis and power consumption have been noted previosly ously in the literature.' This paper presents data in continuation of the subject given in an earlier paper by the authors.2 As noted in the authors1 previous paper, the objectives of this work are the reduction in the cell voltage and the purity of the cathode product resulting from the use of alloyed lead anodes. The fundamental facts developed in the previous paper were: (I) that the presence of a small amount of calcium lowers the anode potential approximately 50 per cent. below that of pure lead; and (2) that thallium when present to the extent of 4 per cent. rendered the anode practically stable, thereby lowering the contamination of the cathode by lead to a very insignificant amount. The specific features determined in this recent work are as follows: 1. The lowest limit of calcium in the lead which will still give maximum lowering of the anode potential. 2. The characteristics of the thallium-calcium-lead anode. 3. The characteristics of the silver-calcium-lead anode. 4. The characteristics of the thallium-silver-calciurn-lead anode. It was determined that 0.1 per cent. calcium in the anode was sufficient to lower the anode potential approximately 50 per cent. Table 1 shows the characteristics of alloyed anodes tested. The anode composed of 0.1 per cent. calcium, 4 per cent. thallium, and 95.9 per cent. * Professor of Metsllurgy, Missouri School of Mines. t Professor of Metallurgy and Ore Dressing, Hea.d of Department, Missouri School of Mines. Assistant Professor of Metallurgy, Missouri School of Mines. 1 Among others, see C. G. Fink and Li Chi Pan: Insoluble .Anodes for the Electrol-ysis of Brine [Trans. Amer. Electrochem. Soc., (1926) 49, 83-1341 and other papers by these authors. U. CJ. Taintori, 8. G. Taylor arid H. P. Ehrlinger: Lead Alloys for Anodes in Electrolytic Production of Zinc of High Purity. Truns. A. I. M. E. (1929) 192-200. 2 H. R. Hanley, C. Y. Clayton, D. F. Walsh: Investigation of Anodes for Production of Electrolytic Zinc. Trans. A. I. M. E. (1930) 275

Jan 1, 1931

DURING September, the Coal Commission pre- pared for issue a series of 18 reports on varied aspects of- the bituminous coal industry; the final report, dated Sept. 22, sums up the facts and offers recommendations addressed to Congress, to the industry, and to the public. The few following paragraphs are selected: Bituminous coal is the real foundation of that great industrial and transportation structure which enables more than a hundred million people to live in America and be so well supplied with things necessary for their health, comfort; and convenience; it also furnishes domestic fuel for two-thirds of the homes of the land. The distribution of the output of the bituminous mines tells the story: 28 per cent. goes to the railroads, 25 per cent. to the boiler houses of factories and mills of all kinds, 15 per cent. to the coke ovens and gas plants, 10 per cent, to the homes, 7 per cent. to steel plants and the same percentage to power plants and street railways, 4 per cent. is exported, 2 per cent is used for power at the coal mines, and the remaining 2 per cent. goes to the seaboard for steamship fuel. Bituminous coal enters into interstate commerce on a scale approached by no other commodity; less than a fourth of the coal mined in the United States fails to enter interstate com-merce. All but one of the 45 coal producing districts in the United States ship coal outside the State in which it is mined. Three hundred miles of cars loaded with coal is the daily output of the bituminous mines of the United States. The public-welfare element in coal is seen in the dependence of public health and safety on an unfailing supply of fuel, in the close connection between the prosperity of most industries and the uninterrupted operation of the coal mines, and in the obvious fact that without coal the great network of railroads which binds together this great country would be idle. The railroads and the public utilities, themselves so clearly obligated to render what-ever public service is demanded of them that the constitutionality of their public regulation is unquestioned, are of all industries most dependent upon coal. Thus, coal makes up over 35 per cent. of the operating cost at the gas plant and over 25 per cent. at the electric power station, and in the operating expenses of. a railroad the cost of coal is the largest single item, next to labor. The practical logic that half a century ago clothed with a public interest the steam locomotive and in later years the electric-power station must recognize a large element of public service in the coal mine that furnishes the necessary energy to both locomotive and power-plant.

Jan 10, 1923

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Jan 1, 1938

By John V. Beall

Early this year at the University of Arizona in Tucson, a survey was made of student opinion about the minerals industry. Over 100 of the three page questionnaires were completed and these were analyzed by the following categories: 40 Mining Engineering students, 20 Geological Engineering with 2 Geophysical Engineering students, 15 Geology students, 7 Metallurgical Engineering, 26 Underclassmen, 29 Graduate students and a composite of 84 total students. Not all of the results of the survey were predictable. After graduation there is a strong preference toward going to work in the mineral industries. The next most popular options, but trailing the first choice greatly, was graduate work or employment in another industry. A smattering of other choices were for teaching, government or research. None checked the box for drop out.

Jan 1, 1971

By Fred D. Wright, Philip B. Bucky

FOREWORD By E. D. Gardner[$] THE present known petroleum reserves are limited, and unless important new fields are discovered the Nation will be dependent, in the not too distant future, upon imports or upon synthetic liquid fuels to supplement domestic petroleum supplies. As a national defense measure, it would appear desirable to develop a substitute source of liquid fuels within the borders of the country if new discoveries of petroleum should prove disappointing. Congress undoubtedly had this in mind when it passed the Synthetic Liquid Fuels Act (78th Congress, approved April 5, 1944). The act directed the Bureau of Mines to construct and operate demonstration plants for producing synthetic liquid fuels from coal and oil shale, and from forestry and agricultural products. As a part of this program, the Bureau of Mines has built a demonstration plant at Anvil Points, near Rifle, Colo., for retorting the oil shale, and has developed a mine to supply the plant with oil shale. At the beginning of mining operations, the physical qualities of the oil shale, which would have a bearing upon the selection of mining methods and practices for exploiting the deposits, were largely unknown. A comprehensive mining-research program has been set up to determine the best methods and practices to follow to obtain the lowest overall practicable mining cost for producing the oil shale on a large scale. Unusually low mining costs will be necessary for shale oil to be produced commercially. Consideration now is being given to exploiting a series of flat-lying beds 70 ft thick by a room-and-pillar method of three benches with the advance heading at the top. This report is one of a series giving the results obtained in research on mining problems. INTRODUCTION The structure and physical qualities of the oil shale indicate that the 70-ft interval of the oil-shale measure can be safely mined in open stopes; studies indicate that this method would be the most economical one to use.1 As labor will be a major item of expense, the largest equipment that could be operated efficiently in the workings would be required to obtain the lowest practicable mining cost. It was therefore desirable to know the maximum safe span of unsupported rooms and the size of pillars necessary to support the overburden. This paper describes the work done at the Columbia School of Mines Barodynamic Laboratory in determining the maximum safe unsupported roof spans and the minimum safe pillar dimensions for the oil-shale mine at Rifle, Colo.

Jan 1, 1947

By C. E. Gerity

Near Bunker, Mo., in the New Lead Belt, Ozark Lead Co. operates a 6000 tpd lead-zinc mine. Mined ore is transported to the surface in three mechanized and automated steps. The mine is developed by a rectangular-shaped sublevel haulage drift 15 ft high by 28 ft wide, driven on strike below the ore zones. Ore transfer raises were driven from the sublevel at locations near the shaft, 1500 ft distant, and on subsequent 1000 ft centers. These 6 x 5-ft raises are slashed to obtain maximum storage below dump points. These dump points are located on each mining level and are of steel and concrete construction. Spiral 12 X 24-ft inclines driven from the sub-level provide access to these levels for equipment and mine utilities.

Jan 11, 1972

By P. G. Hallof

Only recently has the term Induced Polarization found its way into geophysical literature. Schlumberger first mentioned the possible use of the induced polarization effect in one of his early papers. Later, induced polarization was the subject of several university theses, such as Seigel's at the University of Toronto and Bliel's at the Michigan School of Technology. In addition, a group at the New Mexico School of Mining and Technobgy has done work on induced polarization. There is very little to be found in print on the subject of induced polarization. Several papers have been presented at meetings, the 1958 AIME and SEG* conventions, for instance, on laboratory measurements of the effect and theoretical considerations useful in the interpretation of field results. This paper is the first attempt to present actual field results which show the usefulness of induced polarization as a prospecting technique. There are several phenomena that can cause polarization when electrical current is passed through the ground. In a paper presented at the 1958 SEG* meetings Professor T. R. Madden of M. I. T. demonstrated that only two of these gave rise to appreciable effects. The first is a result of the membrane and diffusion effects in a sandstone that contains appre- ciable amounts of clay minerals. The unbonded charges associated with the clay mineral forma material that passes positive and negative ions with different mobilities. When current is passed through such a system for some period of time, polarization results. The second phenomenon, which gives rise to very much larger polarization effects, is the one used in the new prospecting technique. These effects are a result of the blocking action or polarization of metallic or electronic conductors in a medium of ionic solution conduction. This electrochemical polarization, called "the over-voltage effect" by electro-chemists, occurs whenever electrical current is passed through a volume of rock which contains metallic minerals such as base metal sulphides. This polarization at metallic interfaces in ionic solutions depends upon the chemical energies necessary to allow the ions to continue the flow of current by giving up or receiving an electron from the metallic surfaces. The energy stored in this reaction isanalogous to that stored when a condenser is charged. If a d. c. current flowing through such a system is interrupted, the polarization can be detected as a small, decaying current that flows after the applied current is discontinued. The decaying potential measured is a result of the current flow caused by charges returning to their equilibrium positions from the positions they assumed under the applied potential field. Because of the polarization, there is an excess of change at each metallic interface. There is an alternate method of measurement of the induced polarization effect. The electrical

Jan 1, 1961

By P. Niessen, W. C. Winegard, C. J. Beingessner

DURING the last 10 years, several grain-growth studies have been made using zone-refined metals with controlled amounts of solute to elucidate the interaction of solute with moving boundaries. In all these studies, it was more or less implicitly assumed that the alloys used were, after recrystallization and grain growth, homogeneous within the grains with respect to solute and lattice defects. This note deals with observations made on microstructures originating from solidification of dilute alloys and from grain growth. Briefly, the experimental procedure used in these studies was the following: zone-refined cadmium and master alloys were melted and cast in Pyrex under vacuum to produce bars 14 mm in diam and about 150 mm long. These bars were cut into 8-mm-thick slices which were mechanically and chemically polished. The specimens were then deformed 30 pct in compression and given a 1-week anneal at 260°C in argon. After this anneal, a second deformation produced completely recrystallized samples 4 mm thick. The time-temperature controlled anneals were carried out in a bath of silicone oil. After the grain-growth anneal, the specimens were polished in Gil-man's' solution (33 g CrOs, 6 g NazSO, in 100 ml of water). Several etches were used depending on the alloy investigated, but mostly a mixture of concentrated HC1 and HNOj (98:2 vol) was employed. In all the alloys examined, the ease with which substructures could be revealed depended strongly on the crystallographic orientation of the surfaces of the grains. However, very frequently the microstructures to be discussed here etched up over broad areas comprising several grains. Fig. 1 is a micrograph of a Cd-0.05 at. pct Mg alloy annealed for 100 sec at 270°C. Different substructures are seen in this photograph. A denotes the now existing grain boundaries. The well-defined lines and points marked B are the remains of a solidification substructure. The lines are boundaries between cell colonies, and the points are nodes located on regular two-dimensional cells. This cellular structure has the same appearance as that found by weinberg2 for rapidly quenched Zn-Au alloys. The "ghost boundaries", marked C, are very similar in appearance to a grain boundary array in a polycrystalline sample. Repeated polishing and etching showed that all the substructures observed were three-dimensional. To date, the ghost boundaries have been clearly observed in all samples containing 0.005, 0.01, 0.05, and 1 at. pct Mg, and in samples containing 0.01 at. pct Zn. Attempts to outline these ghost boundaries in cadmium alloys containing 0.01 at. pct Ag and Au were only partially successful. In these alloys, parallel lines, having a resemblance to the ghost boundaries in the Cd-Mg and Cd-Zn alloys, were observed, but it was not possible to obtain complete arrays of ghost boundaries which extended over several grains. It is possible that a different etch than that presently employed would reveal the ghost boundaries in the Cd-Au and Cd-Ag alloys as clearly as in the Cd-Zn and Cd-Mg alloys. A close examination of the ghost structure showed that it consisted of linear etch-pit arrays, Fig. 2. The ghost boundaries were resolvable even in grains which showed over-all faceting due to the etching, as seen in the corner of Fig. 2. The general appearance of the ghost structure suggests that it originated during grain growth. This is supported by the observation that the mesh width in the ghost-boundary array generally increased with increasing final grain size. To test whether the ghost structure was formed during the long homogenizing anneal or during the grain-growth anneal, some as-cast samples were deformed and given a grain-growth anneal. This anneal was terminated by air cooling or

Jan 1, 1967

By William I. Busenbark, Elmer C. Newman

At Bingham Canyon, the world's largest open-pit copper mine, annual grease consumption is in the neighborhood of 109 000 kg (240,000 lb), all of which was 544 (120-16) purchased, warehoused, and distributed in 54-kg (120-1b) and 180-kg (400-1b) drums. While perhaps a menial and mundane chore, grease distribution shows on the ledger as a significant expense item. To improve labor and cost performance, Kennecott maintenance engineers undertook a study to find the most direct method for moving multi purpose grease (MPG) from the refinery to the point of final consumption. What they found was a direct vendor system for hulk grease so simple and flexible that long-established drum distribution is being phased out in favor of the newer method throughout 75% of the operation.

Jan 9, 1977

By Rudolph Emmel

THE mines operated by the South American Development Co. are located in the Zaruma mining district of southwestern Ecuador. They are near the old mining town of Zaruma, which is the only important city in the canton of the same name. The district is situated in the upper end of a valley lying between two spurs of the Cordillera, one of which may be considered the Coast Range and the other an intermediate range. The mining camp proper, known as Portovelo, and the plant are 2.4 km. south of Zaruma, on the north bank of the Amarillo River, a tributary of the Tumbes River, which flows southwestward through Peru to the Pacific. Portovelo is difficult of access; it is reached from Guayaquil by means of river steamers and muleback. Embarking at Guayaquil, the route is down the Guayas River, across the Jambeli Canal, and up the Santa Rosa River to Santa Rosa, a distance of 177 km. From Santa Rosa, the road or trail follows the Santa Rosa River, then across the summit of the Coast Range into Portovelo, a distance of 74 km.-a two-day trip on muleback. The mining property of the South American Development Co. comprises 297 lode claims and 142 placer claims. The combined lode claims cover an area, roughly rectangular in shape, 9000 m. long from north to south by 4000 m. wide; the northern edge of the rectangle is about 3000 m. north of the central plaza of Zaruma. Mineral lands in Ecuador are held by virtue of an annual tax per claim paid to the central government, no surface rights being included.

Jan 1, 1925

By E. F. Adkins, R. W. Douglas

The variation of the spectral emissivity of osmium and ruthenium with temperature can be expressed by the following relations: DURING a study of the sintering characteristics of osmium and ruthenium, discrepancies in the previously accepted melting points of the metals were noted. The melting temperatures had not been measured at the time of the work, but were estimated in the literature as 2700°C for osmium and 2450°C for ruthenium.' A recent investigation by Baird2 has shown the melting temperatures of osmium and ruthenium are 3000" and 2250° C, respectively. In the present work, osmium bars sintered at temperatures as high as 2900° C showed no evidence of melting, whereas ruthenium showed definite evidence of melting at temperatures as low as 2250°C. In view of the apparent discrepancies, the melting temperatures of both metals were determined. The spectral emissivities of both metals were determined as an aid to studies of the sintering characteristics of these metals. MATERIALS AND PROCEDURES The materials used in these studies were metal powders supplied by Englehard Industries, Inc., through the courtesy of The International Nickel Co. Analytical data from three laboratories, although not in complete agreement as to the purity of the material or the major impurity elements, indicated that the maximum impurity levels were 0.5 and 1.0 wt pct in osmium and ruthenium, respectively. The metal powders were pressed to 1/4 by 1/4 by 6-in. bars at 20Tsi using carbon tetrachloride as a lubricant. The pressed bars were presintered 1 hr at 1200°C after heating 1 hr at 400°C. The presintered densities of the several bars of the metals ranged from 65 to 80 pct of ideal density. Specimens were self-resistance heated in a vacuum sintering bell. Temperatures were measured with an L&N, disappearing filament optical pyrometer. True temperatures were read at the base of an 0.30-in.-diam, 0.150-in. deep hole drilled into the center of a presintered bar. Apparent temperatures were read from the surface of the bar adjacent to the hole. MELTING POINT DETERMINATION The melting temperature of the metals was determined as the temperature at which a slight additional increase in current through the specimen resulted in a reduced temperature at the base of the hole. The apparent reduction in temperature is a result of the liquid metal filling the hole, thus altering the black-body conditions. The melting points of osmium and ruthenium, based on three deter-

Jan 1, 1962

DEFENSE Materials Procurement Agency has been moving rapidly to encourage copper industry expansion programs. Although copper production is at a high level, a shortage exists on a world-wide basis as well as on the domestic scene. Projected expansion programs will not ease this current demand for most of them are 2 to 5 years off. Refining facilities are adequate but there is a shortage of ore and scrap, and it is for this reason that the expansion programs are directed at developing more sources of supply. The domestic expansion programmed thus far and understood to have been arranged with price escalation should the domestic price go to 271/20, were summarized by American Metal Markets as follows (dates of announcement are given in parenthesis: .1-Copper Cities Mining Co.'s, $15,000,000 expansion near Miami, Ariz., to be operating about 1954. DMPA will buy 22,500 tons of copper a year up to a given amount on an agreed price of 23¢ per pound, with some exceptions and depending upon salability at a higher price to other purchasers in the U. S. (September 25th). 2-An RFC loan of $60,000 to North Butte Mining Co. to be paid off on the basis of deliveries at a purchase price of 241/20 per pound (September 25th). 3-A $25,000,000 expansion program by Phelps Dodge to provide 38,000 tons per year by late 1954. DMPA would purchase it at a price of 22¢ per pound up to 112,500 tons providing other purchasers in the U. S. will not pay a higher price (September 26th). 4-Anaconda Copper Mining Co. $40,000,000 expansion in Nevada to provide more than 30,000 (might be increased to 45,000) tons per year. DMPA would purchase the copper at 250 per pound for a limited period of time if it is not salable to industrial users at above this price. Production would start around 1953 (November 14th).

Jan 1, 1952

By L. F. Pease, J. H. Brophy

A phase diagram for the Ta-Zr system is presented. The system is of the minimum-melting point type with the 0-zirconium phase decomposing monotectoidally at 785°C and 95.5 at. pct Zr. The minimum solidus temperature is 1875°C and the temperature of the top of the monotectoid loop is 1775°C. Techniques employed included X-ray diffraction and fluorescmce, electron microprobe analyses, diffusion couples, metallography, and melting-point measurements. Errors due to interstitial solutes and in melting observations are particularly common in this system, and their occurrence is discussed. SEVERAL versions of the Ta-Zr phase diagram have been reported in the literature.lm7 Williams et al.' report a diagram of the minimum-melting point type with a monotectoid reaction at 800°C and 12 wt pct Ta. The minimum in the solidus occurs at 1820°C and 25 wt pct Ta, while the top of the monotectoid gap is located at 1780°C and 80 wt pct Ta. The experimental techniques employed were metallography, electrical resistance variation with temperature, dilatometry, X-ray diffraction, and direct observation of melting by the technique of Pirani and ~lterthum.' Experience in the Nb-Zr phase diagram has shown that small changes in the interstitial content can cause large shifts in the positions of the phase boundaries. Small amounts of inter -stitials can cause similar changes in the Ta-Zr system and may be responsible for the wide variations in the phase diagrams previously reported.'-' The authors15 have found that alloys containing 0.75 wt pct 0 and 1.0 wt pct Ni with tantalum contents from 19 to 85 at. pct often contain a lamellar or cellular precipitate after annealing above 1400°C. This precipitate is very similar to that reported by pollack,12 Ralls," and Donlevy17 for the Ni-Zr system. In the present investigation, a wider variety of experimental techniques and improved alloy purity were applied to the resolution of errors in diagrams for this system as they now appear in the literature. New results have been obtained in the areas of alloy homogeneity and purity. Errors in the common techniques of direct melting observation in binary alloys have been demonstrated. In the commercially important high-tantalum region, the more accurate metallographic method of solidus determination has been employed. EXPERIMENTAL PROCEDURE Nominal analyses of the materials employed are given in Table I. The zirconium was low hafnium reactor grade iodide crystal bar, and the tantalum was in the form of high-purity sheet. Powders were impossible to use because of gas content. Alloys were melted on a water-cooled copper hearth, with a thoriated tungsten-tipped nonconsumable electrode in 2/3 atm of Zr "gettered" argon. Alloys were

Jan 1, 1963