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By W. M. Bertholf

To establish the minimum or break-even efficiency of a preparation plant it is necessary to determine the ratio of production costs per ton of run-of-mine coal to sale price per ton of clean coal. This ratio is then divided by the percentage of plant recovery. Assume, for example, that washability data indicate that 80 pct of the run-of-mine coal may be recovered as clean coal selling for $5.50 per ton. If the same plant incurs $4.00 per ton mining costs and $0.25 per ton preparation costs, the cost to sale price ratio would be 4.25/5.50, or 77.3 pct. Since the plant is capable of recovering 80 pct of the run-of-mine coal the minimum plant efficiency would be 77.3/80, or 96.6 pct. If the plant efficiency were increased to 100 pct the limit on preparation costs would be increased to $0.40. Therefore, the washing operation must be accomplished at a cost of $0.25 to $0.40 per ton and the efficiency must be 96.6 pct or higher. By plotting a curve of efficiency vs preparation costs and taking into consideration the plant cost, feed rate, operating costs, and yields of the various flowsheets it is possible to select a financially sound process. Table I classifies preparation processes according to their nature of separation. It must be remembered that what is thought to be ideal does not always prove practical under actual operation. An outstanding example is the work done on the plunger-type jig. It was determined by the law of equivalence that this unit could treat satisfactorily only sizes differing by no more than a ratio of 2. Yet these same plunger-type jigs are successfully treating sizes considerably greater than this ratio.

Jan 12, 1957

By Francisco Cadena

THE construction of Norris Dam, built by the Tennessee Valley Authority on the Clinch River, a tributary of the Tennessee River, involved the production of coarse and fine aggregate for approximately 1,000,000 cu. yd. of concrete. A hammer-mill plant for the manufacture of sand from quarried rock was indicated as the most economical method of providing this material. The abrasive character of the feed as compared to the average hammer-mill feed made it necessary to control operations rather closely, and this resulted in the accumulation of many data bearing on production and maintenance. This paper will deal only with three specific sets of data, accompanied by such general information as may be necessary to explain the conditions under which they were obtained and followed by discussions on the relation of silica content to hammer wear, comparative costs of slugger and stirrup hammers, and comparative costs of tool-steel and manganese-steel grate bars. Coarse Aggregate Aggregate for the concrete poured at Norris Dam came from a dolomite quarry within 2000 ft. of the west abutment of the dam. Geologically this rock is known as a Knox dolomite. A typical chemical analysis is given in Table 1. TABLE 1 .-Typica.1 Chemica1 Analysis [PER CENT H20,1100F ............................................ 0.0'2 Ignitionloss ............................................. 43.56 MgO .................................................. 19.19 CaO .................................................... 29.07 FezO .................................................... 0.39 A1203 .................................................... 1.94 FezO .................................................... 0.39 A1203 .................................................... 1.94 ..................................................... 5.75 SO2.. .................................................. Tr.] Rock was carried by 12-yd. dump trucks to a 42-in. gyratory crusher set at 6 1/2 in. The product of the primary crusher was taken by a belt conveyor to a double-deck vibrating screen followed by a 5 1/2-ft. cone

Jan 1, 1937

By John Blatchford, H. O. Hofman

The leading antimony mineral is stibnite. In smelting stibnite ore two processes are available, precipitation and roasting-reduction. The former is suited only for high-grade ores. As low-grade ores are more common than high-grade, roasting-reduction is of greater importance than precipitation. In the roasting process the aim may be to leave the oxidized antimony in the ore, or it may be to volatilize as much of the antimony as possible, collect the volatilized oxide as a rich intermediary product and smelt it for antimony, leaving the gangue poor enough to be considered a waste product. Whichever way the roast is conducted certain difficulties inherent in stibnite are encountered. These are: 1. The low melting point of stibnite which, according to Pélabon,' is 550°C., according to Wagemann2 540°C., and according to Borgstroma 546°C. 2. The ignition temperature: According to Friedrich,4 stibnite, if heated in air, begins to oxidize at 290°C. if the size of a grain is 0.1 mm. in diameter; at 343", if 0.1 to 0.2 mm.; and 430" if 0.2 mm. 3. The fusibility of a mixture of Sb2S33 and Sb203 which in the form of kermesite (Sb2S3)z.Sbz03 melts at 517°C.6 4. The volatility of Sb2Ss and SbzOs, for which no numerical data appear to exist, although practical experience has shown that they are volatile at low temperatures. As regards the oxidation of metallic antimony, we have the experimental evidence of C. F. Plattner6 that when fused and brought to a red heat, it burns with a bluish-white flame to Sb2Oa which passes off as a

Jan 1, 1916

By Philip W. Simmons

THE Colorado Plateau uranium province is in a mining boom rivaling the most colorful days of the early West. The application of scientific skills and the use of modern and novel mechanical equipment, however, is unique. No metal has ever received such concentrated effort from geologists and mining engineers. Moreover, no other metal has had the variety of tools available for finding and mining ores. Radiation detection equipment, bull- dozers, truck-mounted wagon and core drills, jeeps, airplanes, helicopters, tractor loaders, self -propelled 3-wheeled dump cars, front-end loaders and fleets of modern trucks are some of the present-day tools of the uranium prospector and miner. Because uranium is so vital to our national defense, the Atomic Energy Commission has offered many incentives for its mining. Through a series of circulars, the AEC has established base price schedules and various incentive payments. The incentive payments for acceptable ores from domestic mines are: (1) a guaranteed base price of $3.50 per Ib for ores assaying 0.20 pct U3O8 and more; (2) premiums based on grades above 0.20 pct U3O8 as for example, ores assaying above 0.50 pct U3O8 receive $1.00 per lb premium; (3) a development allowance of 506 per Ib of U3O8 contained in ores assaying over 0.10 pct U3O8 (4) an ore haulage allowance of 64 a ton mile for a maximum of 100 miles; and (5) an initial production bonus which may amount to as much as $35,000 in addition to all other payments. The producers have been guaranteed this policy until Feb. 28, 1957. The other four will continue until April 1962.

Jan 4, 1954

By G. A. Reinhardt

THE Youngstown Sheet & Tube Co. has produced a large tonnage of 0.35 to 0.45 carbon forging steel, the acceptance of which was based on the physical properties of test specimens obtained by forging the original 5 3/4 in. (14.5 cm.) square bloom to a ¾ in. (1.9 cm.) round. Annealed and tempered specimens were required. The test bars were annealed by heating from 900 ° to 950° C. and cooling slowly in mica. The test bars were tempered by heating to 825° to 875° C., quenching in water, and drawing to 515° to 535° C. Immediately after heat treatment, the test pieces were machined to a diameter of 0.534 in. (1.38 cm.) and tested. Very good physical properties were obtained and no difficulty was experienced in meeting the specifications called for. ULTIMATE STRENGTH, ELONGATION, LB. PER SQ. IN. PER CENT. IN 4 IN. NOT LESS THAN Annealed specimens 78,230 to 92,450 18 Tempered 120,000 to 149,350 9 After experience oil this material, production of slightly higher carbon forging steel was started. The method of testing this material required that test blooms be either normalized or annealed. The normalizing consisted in heating to 850° to 900° C. and cooling in still air; the annealing, in heating to 850° to 900° C. and cooling in the furnace or in mica. From the treated bloom, the test pieces were taken either by core drilling or by sawing from points midway between the edges and the intersection of the diagonals. The cores or blocks were turned to a standard 2-in. test piece with a diameter of 0.564 in. and tested without further treatment. The physical requirements of the test pieces were:

Jan 7, 1919

By H. E. Lee, P. C. Feddersen

Blast-fuRnace operation at the Bunker Hill smelter deviates somewhat from common practice. Under existing conditions it is economical to operate the furnaces at "forced" capacity. The furnace feed consists chiefly of sinter and averages close to 50 per cent lead. Experience in smelting such material favors a low charge column attended by smaller proportions of coke and a low blast pressure. Under such conditions the gain in furnace tonnage greatly overbalances the somewhat higher slag losses and increased percentage of material fumed Furnace Charge The ingredients for the blast-furnace feed are stored in a group of 24 charge bins (3600 cu. ft. capacity). Each bin has two discharge chutes. Beneath each chute is a steel weighing hopper, suspended from a Fairbanks scale. The several hoppers are kept filled with the exact amount of material required to complete a furnace charge. The weighed material is discharged into a standard-gauge, bottom-dump charge car containing two compartments, each of which holds a complete charge (approximately 1½ tons). It is hauled to the blast furnace by a 44011 electric trolley locomotive. The proportionate parts of the various constituents of a representative blast-furnace charge are shown in Table 1. Table 1.—Representative Blast-furnace Charge at Bunker Hill Smelter Material Pounds Sinter.................................................. 2500 Limerock............................................... 0- 50 Coke................................................. 250-300 Scrap iron.............................................. 0-25 Settler skulls.......................................... 75 Undried zinc-plant residue................................ 0-200 Siliceous ore............................................ 25 Baghouse dust.......................................... 0-50 By-product slag......................................... 100 A variable stock tonnage of zinc-plant residue and return by-products results in fluctuations in the percentages of these materials in the blastfurnace feed. Accompanying such variations are corresponding increases or decreases in the amounts of coke, limerock and scrap iron necessary to obtain good furnace operation and adequate reduction.

Jan 1, 1937

The Mississippi river was discovered by French explorers that came southwestward, by way of the Great Lakes, from eastern Canada. Vignan, Joliet, De Champlain, and others of the French pioneers in the first half of the seventeenth century, dreamed of a short cut to China by means of the great waterways they explored. In a geographical book published in London in 1726 by Daniel Coxe an account is given of "a new and curious discovery and relation betwixt the river Meschachebe [Mississippi] and the South Sea, which separates America from China, by means of several large rivers and lakes". Louis Joliet, a fur-trader, and Jacques Marquette, a Jesuit missionary, reached the Mississippi and paddled their canoes on its broad waters on June 17, 1673.* They descended the river as far as the entry of the Arkansas tributary, and then returned overland to Canada, being deterred from going farther south by reason of Indian hostility. Several years later Robert de La Salle, a French trader, starting from Quebec, went westward to Lake Michigan and thence to the Illinois river, which he and his comrades descended in their canoes to the junction with the Mississippi, and then followed it to the sea. They reached the Gulf of Mexico on April 9, 1682. Thus the great central waterway of North America was made known. These French-Canadian voyageurs, or boatmen, traded with the Indians for furs in the Upper Mississippi valley, and when in need of bullets they noticed the outcrops of lead ore, from which, probably in the last decade of the seventeenth

Jan 1, 1932

By Teder R. I., M. M. Protodyakonov

In order to find an empirical relation between a quantity F and (m) independent variables or factors, each of which take (n) different values or levels, it is necessary to conduct nm different experiments (all possible combinations of the factors), each of which has to be repeated a few times (usually five) due to the scattering of the data. The total number of such experiments is very large, thus for example, when m = 4 and n = 5, it is equal to 5.54 = 3125; and very rarely is it possible to conduct such a number of experiments. Various possible methods of planning partial experiments are illustrated in Fig. 1. Each method shows a large combinative square consisting of five columns and five rows of middle squares, each of which, in turn, is further divided into five columns and five rows of cells. Such a partition corresponds to a plan of an experiment with four factors, each of which takes five different levels. The blackened cells indicate the combination of factors in a partial experiment. The total number of experiments is reduced on the basis of the following considerations: a) The effect of only a few levels of some factors is studied (Fig. la). Such an investigation gives no information on the effect of some factors, therefore it cannot be accepted as satisfactory; b) By reducing the number of levels of each factor; in such a case it is not possible to obtain an empirical relationship, but only whether some factors have an effect. This is evidently inadequate;

Jan 1, 1971

By Edward Halse

The occasional occurrence in metalliferous veins of rounded fragments of rock, matrix or ore, lying loose, embedded in clay, or enclosed in some kind of cement, may be attributed to four causes:— I. They have been washed in from the surface, or from an upper portion of the vein.. II. They are of concretionary origin. III. They have been produced by movements in the country-rock or in the walls of the vein. TV. They have been formed in situ, by the upward, downward or lateral flow of water in the vein itself. In this paper the word " conglomerate " is confined to a rock composed of rounded fragments or pebbles cemented together, as distinguished from a " breccia," in which the rock-fragments are angular. * I. Boulders and Pebbles which have been Washed in from the Surface, or from an Upper Portion of the Vein. In this type it is presupposed that the vein at one time communicated by a fissure or open space with the surface, or with the upper portion from whence the fragments have been washed. One well-authenticated occurrence was described long ago by Fournet. Owing, no doubt, to later dislocations in the lode, pebbles from an old alluvium and sands containing titaniferous iron, as well as fragments of wood, were found in a vein at Huelgoet, in France. " Toutes les parties tendres du filon de Pranal ou ces phenome'nes sont les plus prononces ont 6th excaves jusqu'a d'aasez grandes profondeurs par I' impetuosite des torrents, qui out depose la matiere alluviale.'"

Jan 1, 1906

By Henry M. Howe

This paper gives the results of an investigation of the beha vior of the argentiferous cobalt-nickel arsenides of Temiskam-ing, Ontario, in roasting, made in the metallurgical laboratories of the School of Mines of Columbia University in the City of New York. The ore was kindly given by the owners of the La Rose and Trethewey properties at Cobalt, Ontario, and Mr E. J. Hall, Tutor in Assaying in Columbia University, has helped us much. I. Object of the Investigation. The object of the investigation was to learn: 1. The temperature at which the arsenic is most rapidly expelled ; 2. The thoroughness with which it is expelled by prolonged roasting at this temperature; 3. The effect of adding charcoal (a) near the end of the roast and (b) at. the beginning of the roast. II. Nature of the ORe. The important ores mined in the Temiskaming deposits are: native silver—with small amounts of dyscrasite (Ag,Sb), ar-gentite (Ag,S), pyrargyrite (Ag,SbS,)—smaltite (CoAs,), chlo-anthite (NiAs,) and niccolite (NiAs). Mispickel (FeAsS) and cobaltite (CoAsS) also occur in smaller quantities. The average composition of the ore shipped from this district for the first six months of 1905 was: silver, from 4.1 to 4.8 per cent.; cobalt, from 6.9 to 8.2 per cent.; nickel, from 3 to 4.7 per cent.; and arsenic, from 30.9 to 34.6 per cent. The ore which we treated consists chiefly of smaltite. In our 1aboratory-work

Jan 1, 1908

By W. L. Watts

The existence of petroleum in California has been known for many years. From time immemorial the California Indians used this mineral, in the form of asphaltum, for various purposes. In the early history of the State the Catholic fathers utilized it for roofing their missions and other buildings. It is said that in 1855 or 1856 Andreas Pico distilled petroleum on a small scale for the San Fernando Mission. He obtained his crude oil from Pico canon, near Newhall, in Los Angeles county; and he was probably the first refiner of petroleum in this State. In 1856 a company commenced work at the La Brea ranch, in Los Angeles county, and tried to refine the crude oil. In 1857 an attempt was made to produce illuminating-oil from crude petroleum at Carpenteria, in Santa Barbara county; and there are records of similar attempts in other localities previous to 1860; but none of them were successful. The first scientific report on petroleum in California was made by Prof. B. Silliman, who published his researches in 1865. He spoke favorably of the possibility of obtaining petroleum in remunerative quantities in this State, and gave the results of his experiments in the fractional distillation of California petroleum. The next decade was marked by a considerable oil-excitement in California; and a great many companies mere formed for the purpose of petroleum-mining and for distilling crude oil. In most instances these companies did not meet with success; but it must be remembered that the pioneer oil-miners did not

Jan 1, 1900

By O. B. Hopkins

The total production of oil in Peru in 1940 was 12,127,135 bbl., or about 10 per cent less than in 1939. Most of the reduction can be attributed to the fact that the export market under war conditions is much restricted and naturally is more than ordinarily competitive. Development and Exploration in Older Areas As evidenced by Table I, almost all production continued to come from the three established fields in coastal northwestern Peru. Zorritos Field.—Exploration in this small field, which was purchased by the Peruvian Government in 1939, continued with that in near-by areas in the adjoining National Reserve. Several wells were drilled, regarding which details are not as yet available. It is estimated that the production rate for a total of some 45 old and 15 new wells approximated zoo bbl. per day, or about 3 bbl. per well per day. Lobitos Fields.—The Lobitos area produced 2,435,504 bbl.; about 10 per cent less than the amount for 1939. La Brea-Pari9zas.—This property of International Petroleum Co. continued to account for nearly 80 per cent of Peru's production. During the year, drilling was stepped up to 139 wells, as compared with 73 wells completed in the previous year; 123 were producers and aggregated a total of 287,867 ft. Of this total, more than 85 per cent was drilled by rotary tools, which are steadily displacing other equipment. Although most of these wells were drilled in the proved or semiproved areas, eight

Jan 1, 1941

By O. B. Hopkins

The total production of oil in Peru in 1940 was 12,127,135 bbl., or about 10 per cent less than in 1939. Most of the reduction can be attributed to the fact that the export market under war conditions is much restricted and naturally is more than ordinarily competitive. Development and Exploration in Older Areas As evidenced by Table I, almost all production continued to come from the three established fields in coastal northwestern Peru. Zorritos Field.—Exploration in this small field, which was purchased by the Peruvian Government in 1939, continued with that in near-by areas in the adjoining National Reserve. Several wells were drilled, regarding which details are not as yet available. It is estimated that the production rate for a total of some 45 old and 15 new wells approximated zoo bbl. per day, or about 3 bbl. per well per day. Lobitos Fields.—The Lobitos area produced 2,435,504 bbl.; about 10 per cent less than the amount for 1939. La Brea-Pari9zas.—This property of International Petroleum Co. continued to account for nearly 80 per cent of Peru's production. During the year, drilling was stepped up to 139 wells, as compared with 73 wells completed in the previous year; 123 were producers and aggregated a total of 287,867 ft. Of this total, more than 85 per cent was drilled by rotary tools, which are steadily displacing other equipment. Although most of these wells were drilled in the proved or semiproved areas, eight

Jan 1, 1941

By J. D. Verhoeven

The effectiue distriblltion coefficient has been Measured in a series of vertical, normal freezing experirtzents with large current densities passing through the solid-liquid interface. The results indicate that the effect of the current on solute redistribution is due to electvotransport in the liquid. The high currents produced extensive mixing in the liquid which was considerably reduced by solidifying in small lubing. Analysis of the convection indicates that it probably vesulls from a horizontal temperature gradient produced by the Joule heating- of the electvic crirver~t. Due to the strong dependence of this convection upon the specimen radius, it is conclnded that only for specit~ens with radii of less than somewhere between 1 and 2 mm wilt electric field freezing be getlerally effec-tire at enhancing the purification of zone-melting experittierats in loe-melting alloys. Experiments on 0.8-mm lubes illustrate some interesting potential applications of this techniqne as a means of solute control on smcrll specimens. In a number of papers published within the last few years'-4 it has been found that passage of large dc currents through the solid-liquid interface of a freezing alloy produces a change in the solute redistribution accompanying the solidification. It had been predicted theoretically by Hucke et al.s and by Pfann and Wagner that such an effect would occur as the result of electrotransport within the liquid boundary layer at the solid-liquid interface. These authors independently derived the following relation between the effective distribution coefficient and the variables of the process: Where k0 is the equilibrium distribution coefficient, V is the mobility of the solute relative to the solvent, E is the electric field intensity, D is the solute diffusion coefficient, R is the rate of interface motion, and 6 is the boundary layer thickness. Both groups of authors show that this equation predicts the possibility of extending the purification ability of zone-melting experiments by the addition of an electric current. However, there are other effects in addition to electro-transport which could be produced by the high dc current and might, perhaps, invalidate the applicability of Eq. [I]. For example, high electric current might affect the interface reaction or perhaps the equilibrium distribution which was assumed to exist at the interface. It was the purpose of this work to determine the applicability of Eq. [I] by systematically investigating a simple system for which all of the necessary parameters were known. It was of particular interest for speculating on the potential usefulness of this technique to determine the maximum practical field intensities obtainable, and the effect of these high fields upon convective mixing in the liquid. The initial work in this study was published in a previous paper3 which will be referred to as I. In that work, a current density of 2000 amps per sq cm was used with specimen diameters of 5 mm. The results gave a qualitative confirmation of Eq. [I.], and also showed that a large amount of convective mixing was produced in the liquid by the current. The present study is an extension of that work to smaller specimen diameters and higher current densities. Two points were overlooked in I and will be emphasized here: a) the value of ko has not been well-established in the Sn-Bi system and b) the observed convection could be due to thermal convection produced from the Joule heating. EVALUATION OF k0 To evaluate Eq. [ I.] it is necessary to know the value of the equilibrium distribution coefficient, k,. Tn I the value of k, was taken as 0.3 from a published phase diagram.7 According to ansen' the best data on the phase boundaries of the Sn-Bi system are those of Davidson.5 The data of Davidson give a k, value ranging from 0.21 to 0.25 for the compositions studied in this work, or an average value of around 0.23. In a recent publication, Rigaud and Tougas'10 determined ko by means of a solidification technique. For an alloy of approximately the same composition as that used in this work they obtained a ko value of 0.39. Hence, there is considerable uncertainty in the value of ko and, consequently, a series of experiments were made to determine k, more accurately.

Jan 1, 1968

By A. H. Larson, R. J. McClincy

The activity of Sb,03 in PbO-Sb,03 slags containing less than 50 mol pct Sb,03 was determined by the inert-gas saturation method at 700°C. In this composition range, the activity gf SbzO3 shows a strong negative deviation from ideality. The activity of PbO in these slags was calculated by application of the Gibbs-Duhem iniegration to the Sb203 activity data. The calculated activity of PbO in slags containing more than 63 mol pct PbO was found to deviate in a positive direction from ideality uthile a negative deviation was found for slags containing less PbO. The standard Gibbs free energies of formation of Sb,03 and PbO. Sb203 have been calculated and compared with existing data in the literature. The activity of Sb203 in PbO-Si0,-Sb203 (PbO/SiO, = 2) slags containing less than 25 mol pct Sb,03 was also determined by the inert-gas saturation method at 700°C. In this composition range, the activity of Sbz03 shows a very large negative deviation from ideality. VERY little experimental work has been published in the past to determine equilibrium data in the oxide systems connected with the refining of lead. These data are of value since impurities such as antimony, arsenic, and tin must be removed from lead and recovered for further treatment. Equilibrium studies on antimony and arsenic systems are also of interest for the design of new processes for lead refining and lead dross treatment. Maier and ~incke' first determined the liquidus curves for the PbO-Sb203 system and identified the compound PbO . Sb203. They found the phase diagram for this system to be two simple eutectics located on either side of the congruent melting compound. They also determined a very limited amount of vapor pressure data for Sb406 abbve PbO-Sba3 melts at 697"~. A second phase diagram investigation on this system was reported by Hennig and Kohlmeyer' who confirmed the existence of the compound PbO . Sb203 as well as the form of the diagram. A disagreement was noticed, however, in that their liquidus temperatures over nearly the entire composition range were higher than those reported by Maier and Hincke. Barthel~ and pelze14 redetermined the liquidus curve at the PbO-rich end of the PbO-Sb@, system and agreed very closely with the results of Maier and Hincke. None of the investigators mentioned above reported any mutual solid solubility in the PbO-SbD3 system. Zunkel and Larson5 have determined the phase diagram for the PbO-rich end of the PbO-Sb203 system by slag-metal equilibrium studies in the Pb-PbO-Sb203 system and by thermal analysis studies in the PbO-Sbz03 system. A maximum solid solubility of 5.6 mol pct Sb203 in PbO was observed at the eutectic temperature of 604°C. Their results for the phase diagram agree favorably with those of Maier and Hincke. The vapor pressure of Sb2O3 in the temperature range from 470" to 800°C has been determined by Hincke, using a modification of the transportation meth~d.~ His results for temperatures below the melting point of Sba3 are the only data reported in the published literature. The predominant vapor species has been shown to be Sb,06 by Norman and staley.? Myzenkov and Klushin,8 using the boiling-point method, have determined the pressure of Sb406 above liquid SbD3 in the temperature range from 715" to 1025°C. The agreement between these two studies is not very close. A portion of the discrepancy lies in the fact that Hincke used silica crucibles, which were attacked by the liquid Sbz03 at high temperatures. This fact does not account, however. for the large difference observed at the melting point. ~aier' gives a brief summary of vapor pressure data for Sb,O, above pure liquid Sbz03 which agree quite well with the data of Myzenkov and Klushin at temperatures near the melting point. This paper describes the determination of Sb2O3 activity data in the PbO-Sb203 and Pb0-Si02-Sb203 (PbO/SiOz = 2) systems by the inert-gas saturation method. These activity data are compared with the data calculated by Zunkel and arson. EXPERIMENTAL Materials. The materials used in this investigation were analytical reagent-grade PbO (99.8 pct PbO, 0.14 pct insoluble in CHsCOOH, 0.02 pct not precipitated by HB, 0.1 pct CaO, and 0.08 pct SiOz), Sbf13 (99.6 pct Sb203, 0.004 PC~ C1-, 0.005 PC~ SO;-, 0.15 p~t AS, 0.001 pct Fe, and 0.03 pct other heavy metals such as Pb), and SiOz (chromatographic grade). Apparatus for Vapor Pressure Determinations. The apparatus used in this investigation consisted of a transportation reaction system with two separate gas trains. The argon transporting gas was first mixed with a small amount of hydrogen, metered, and dried by passage through silica gel and anhydrone drying tubes arranged in series. After this preliminary drying, the argon was passed through copper wool at 500°C to convert the residual oxygen to water vapor which was removed by three anhydrone drying tubes. A second stream of argon was metered and dried and then passed around the outside of the alumina reaction tube to flush away the volatile species to pre-

Jan 1, 1970

By E. Miller, K. L. Komarek, M. Ettenberg

The activity of aluminum in solid Co-A1 alloys has been measured by an isopiestic technique between 850° and 1200°C from 45 to 80 at. pct Al. The activity shows a Precipitous decrease around the stoichzornetric composition of CoAl. Free energies of mixing have been calculated over a limited composition range. Considering an antistructure-vacancy defect mechanism, the degree of intrinsic disorder, a , in CoAl was related to the alunminum activity. Excellent agreement between the calculated and experimental activity curves was obtained for a = 1.25 x 10-4. ThERMODYNAMIC properties of solid aluminum-transition metal alloy are being studied in an investigation of disordering in ordered compounds. In a continuing series of investigations, activities of solid Fe-1,' Ni-A1, kd r-A13 alloys have been measured. From the results for Fe-A1 and Ni-A1, the degree of intrinsic disorder for the equiatomic compounds was calculated2 using equations derived by Wagner and chottk. From the results for Cr-A1 the degree of intrinsic disorder was calculated from equations derived by Orr.' In this paper, the results of the study of Co-A1 alloys are described. Published activity data in the Co-A1 system has been limited to liquid alloys at 1600°C.° A heat capacity study7 of stoichiometric CoAl indicated that a second-order phase transformation occurs at 790° C, attributed to an order-disorder reaction. Oelsen and Middel,' employing the calorimetric mixing of pure liquid metals, obtained heats of formation for compositions from 6 to 90 at. pct Co. Heats of formation for 50 and 78 at. pct Co alloys have also been measured by acid solution calrimetr. The Co-A1 phase diagram, as compiled by Hansen and Anderko,lo is in good agreement with more recent X-ray evidence. The method for measuring activities of aluminum in this study is essentially that employed in the studies of the Fe-1,' i-Al, and r-A13 systems. This isopiestic method entails placing cobalt specimens, in a temperature gradient, in a sealed alumina system containing a pure liquid aluminum source of fixed vapor pressure. The specimens are equilibrated, cooled to room temperature, and their final compositions determined. From the measured temperature of the specimens and the known vapor pressure of pure aluminum the activities of aluminum in the alloy can be calculated. EXPERIMENTAL PROCEDURE The cobalt was 3-mil-thick sheet of 99.9 pct purity (herritt Gordon Mines Ltd., anada). The major impurities were 0.1 pct Ni, 0.014 pct C, 0.018 pct Fe, 0.004 pct S, and 0.005 pct Cu. The aluminum metal had a purity of 99.99 pct (Aluminum Corp. of America) and all alumina parts were 99.7 pct A1,O3 (Triangle RR Grade, Morganite Refractories, Inc.) with major impurities 0.05 pct SiOz, 0.1 pct Fe203, 0.2 pct NazO, and 0.05 pCt K20. Runs 1 to 3 were made with annular cobalt specimens (12 mm ID by 21 mm OD) punched from the sheet. The specimens were deburred and degreased in carbon tetrachloride and in acetone. The samples, each weighing about 150 mg, were then positioned along an alumina rod, a in. OD by 14 in. long, separated by alumina spacers, i in. ID by | in. OD by & in. long. The lower end of the rod was placed in a hole drilled in the center of an 80-g aluminum cylinder. This assembly was put into an alumina crucible, 1+ in. ID by 13 in. OD by 3+ in. high, and the position of each sample was measured to within 50.5 mm relative to the bottom of the crucible. An alumina tube, 28.5 mm ID by 35.5 mm OD by 14 in. long, closed at the top, was slipped over the whole assembly, so that it fitted snugly into the bottom crucible. The entire reaction assembly was tied with molybdenum wire and lowered into a mullite tube, closed at the bottom. A quartz thermocouple tube, closed at one end, containing a t/Pt-10 pct Rh thermocouple, calibrated according to the specifications of the National Bureau of standards,'' was placed along the reaction assembly inside the mullite tube. The temperature of each specimen could be determined by gradually raising the thermocouple and measuring the temperature gradient along the reaction assembly. The combined error in temperature measurement and sample position resulted in a total error of Q°C in the recorded temperature of each sample. The mullite tube was sealed at the top by a water-cooled brass head, connected to a conventional glass vacuum system. The aluminum reservoir is heated to its melting point sealing the alumina system containing the samples. During this process the pressure is maintained below 0.01 li Hg. During subsequent heating to establish the proper temperature gradient and throughout the entire run the pressure is maintained below 2 1 Hg by means of a two-stage mechanical pump. Equilibration runs lasted from 4 to 6 weeks and were terminated by air cooling. The temperature of the liquid aluminum reservoir was brought below its melting point in less than 20 min. For runs 4 and 5, alloy buttons with 49 and 69 at. pct A1 were prepared from the initial high-purity metals by arc melting under purified argon. The alloy buttons were comminuted to powder with an alumina mortar and pestle until the powder passed through a 400-mesh screen, particle size 0.0014 in. Portions of this powder weighing between 50 and 200 mg were placed in small alumina trays, 25 by 15 by 5 mm, which were then

Jan 1, 1969

By T. R. Ingraham

The thermal decomposition of Nickel (II) sulfate was examined by determining the total pressure of SO3, SO2, and O2 developed over a sample when it was heated in an evacuated system fitted with a Pyrex-bellows mercury manometer. The equilibrium pressures were combined with previously published data on the oxide and sulfide systems to establish a predominance volume diagranz for the Ni-S-O system over the normal range of roasting temperature and gas composition used in the treatment of nickel minerals. The protective coating of NiSO4 which forms on the oxide during roasting, and which causes the sulfation reaction to almost cease, may be disengaged readily by temperature cycling. When nickel sulfide is roasted in air, either nickel sulfate or nickel oxide may be formed by altering the experimental conditions. Because of the differing stabilities of various metal sulfates and oxides, possibilities exist for separating some of the constituents of mineral mixtures by the technique of selective sulfation and oxidation roasting. The experimental information required to make reasonable predictions of the possibilities of this technique is incomplete and, in some cases, in conflict. As part of a general program of providing some of the required information, a study EXPERIMENTAL Materials, Apparatus, and Procedure. Fisher certified reagent-grade nickel sulfate hexahydrate was used in the source material for both nickel sulfate and nickel oxide. The manufacturer's analysis indicated: 0.001 pct Fe, 0.005 pct Cu, 0.003 pct Co, 0.001 pct C1, other 0.15 pct. The material was dehydrated, before use, by heating at 420°C for 5 hr. The oxide was prepared by roasting the sulfate in an open tray in a muffle furnace for 10 hr at950°C. Preliminary experiments which were made by thermogravimetric analysis and X-ray diffraction analysis established that only one crystal form of nickel oxide and one of nickel sulfate were involved in the equilibrium shown in Eq. [I]. The apparatus used in the experiments was described previously.1,3 The main feature is a corrosion-resistant, flexible Pyrex bellows which is used to protect the mercury in a u-tube manometer. Before a run was begun, the apparatus was washed thoroughly with hot hydrochloric acid and water and dried by heating under vacuum. The mixed sulfate -oxide sample was contained in a platinum bat rest-

Jan 1, 1967

By A. U. Seybolt

Since the time this topic was originally treated in 1954, more recent French3,1 work has been published making it advisable to repeat the earlier oxygen solubility experiments, but using iron of a higher purity. Upon repeating oxygen saturation experiments with zone-refined iron, it was found that the oxygen solid solubility was at least an order of magnitude less than previously observed. SINCE the publication of an earlier paper1 (1954) on this subject by the present author, several contributions on this topic have appeared. Meijering2 in 1955 attempted to reconcile recent conflicting solubility data, without reaching any definite conclusion. sifferlen3 (1955) found that iron of high purity appeared to absorb a quantity of oxygen (0.005 to 0.025 pct) approximately proportional to the structural imperfections present, such as polygonization and grain boundary area. However, he also indicated that purity itself was a significant factor. He concluded that very pure iron nearly free of lattice imperfections would have essentially zero oxygen solubility. His second paper4 (1957) supported this contention since a zone-melted iron containing initially 0.0007 pct O analyzed only 0.0006 pct 0 after prolonged soaking at 850°C with an FeO layer on the surface. Because of the discrepancy between the results of Ref. 1 and those of Sifferlen, it seemed desirable to attempt to resolve this disagreement. EXPERIMENTAL PROCEDURE AND MATERIALS The experimental method used by sifferlen3,1 was essentially the same as that of Ref. 1. In this technique thin iron strip with a surface layer of FeO is soaked for prolonged periods at an elevated temperature in order to saturate the iron with oxygen. After two days at temperatures near 800° to 900° C, one would expect that the iron would be in equilibrium with the surface FeO. In the work reported in Ref. 1 there was evidence that two days holding at 8000to 900°C was more than sufficiently long for saturation. Sifferlen used 48 hr at 850°C. Because of the evidence presented by Sifferlen that the apparent oxygen solubility is a function of iron purity, three grades of iron were used as indicated in Table 1. The Bureau of Standards wire was used only for resistivity tests, while the other two irons were used for saturation-analysis tests of the type described above.

Jan 1, 1960

By Lewis A. Delano, Harold Rabling

It has been generally recognized that, owing to the extreme friability of galena, fine grinding has a tendency to cause excessive sliming of the mineral, so operators of lead mills have attempted to avoid this condition by commencing concentration at as coarse sizes as any mineral is freed. Jigging has been the basis of the milling process, making a clean coarse concentrate and a large amount of tailing, which was considered sufficiently low-grade to be rejected. However, developments and improvements in concentration processes are everywhere changing the low-grade tailing of yesterday into material worth re-treating today. Investigations of the work of the Hancock jig on the Bonne Terre ore have shown that the best results to be expected will give a tailing assaying 0.75 per cent. lead; the average for all conditions and grades of ore will be between 0.80 and 0.90 per cent. By crushing the jig tailings in ball-mills and retreating by tables and flotation, a tailing of considerably lower grade can be made; the problem then becomes an economic one of increased crushing costs versus higher recovery. In considering the entire elimination of jigging, the increascd smelting charges due to a greater amount of slime galena will be counterbalanced by the lower operating cost, increased recovery, and the many advantages of a simpler flow sheet. In developing these problems in the Bonne Terre mill of the St. Joseph Lead Co., a long series of tests has been carried out covering every stage of crushing and concentration, and a large number of possible flow sheets were considered and tried. Only the final results and a few comparisons will be given here. At the same time, a careful and detailed cost-keeping system has enabled us to compare milling costs with the various Bow sheets, and to calculate the economics of the problem with great accuracy. Concentration Problem The ore occurs as widely scattered deposits of galena disseminated through limestone; it has a specific gravity of 2.8 and the following composition: Pb, 4.00 per cent.; Fe, 3.00 per cent.; Zn, 0.32 per cent.; S, 3.10 per cent.; MnO2, 0.73 per cent.; SiO2, 4.20 per cent.; Al2O3, 3.20 per cent ; CaO, 28.60 per cent.; MgO, 16.85 per cent.; CO2, 36.00 per

Jan 1, 1922

By O. N. Carlson, H. A. Wilhelm, H. E. Lunt, J. M. Dickinson

On the basis of data obtained from microscopic examination, melting observations, cooling curves, X-ray analyses, and resistance measurements, phase diagrams have been proposed for the Th-Cb and Th-Ti alloy systems. Both are simple eutectic systems and have no terminal solid solubility or intermediate phases. The eutectic between thorium and columbium occurs at a composition of about 8 wt pct Cb and a temperature of 1435°C. The Th-Ti eutectic occurs at 1190°C at the composition 12 wt pct Ti. No change was observed in the transformation temperature of thorium in either system or in the titanium transformation. RECENT study of thorium and its alloys has been promoted because of the possibility of employing this metal in nuclear reactors. Their corrosion resistant properties, nuclear characteristics, and high melting points put columbium and titanium among the many metals being employed in the study of thorium alloys. Since a knowledge of the phase relationships would be important in the application of such an alloy, investigations were undertaken to propose phase diagrams for the Th-Cb and Th-Ti systems. Experimental Procedures Thorium metal sponge was specially prepared for use in this investigation. Carbon in a quantity less than 0.04 wt pct was the principal impurity. There was also less than 0.01 pct each of iron, calcium, zinc, aluminum, and nitrogen in the thorium. Columbium, both as a powder and sheet metal, was obtained from the Fansteel Metallurgical Corp. The manufacturer's specifications indicated that the metal contains less than 1 wt pct total impurities. An analysis of the metal showed approximately 0.18 pct C in the powder and less than 0.05 pct C in the sheet. The titanium used was commercial sponge, reported to be 99.5 pct Ti. An analysis showed that this metal contained 0.2 pct Fe. Preparation of Alloys—Since the metals used in this investigation are reactive and might become contaminated on melting in a refractory crucible, the alloys were prepared by arc melting. The titanium sponge was employed in the form of small lumps while the columbium additions were made either as pressed pellets of powder or as clippings from sheet. The alloying material and the thorium sponge were melted together under argon in conventional arc melting equipment employing a tungsten electrode and a water cooled copper crucible.

Jan 1, 1957