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By CYRIL W., William Campbell, Henry M. Howe

THIS paper gives the results of an investigation of the behavior of the argentiferous cobalt-nickel arsenides of Temiskaming, 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 (Ag6 Sb), argentite (Ag2S), pyrargyrite (Ag3SbS3)-smaltite (CoAs2), chloanthite (NiAs2) 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 laboratory-work

Jan 1, 1907

By Carl Lee

WITH the modern trend toward motor drive in coal mines, more careful forethought should be given to future layouts than has usually been done in the past. Both top and bottom equipment of future new mines is likely to differ radically from those of a decade ago. No one is able to predict very far ahead, but provisions can be made to allow for uncertainty. One thing stands out: the mine of the future will be laid out for long life compared to that of the small mine of the past, where an inexpensive top plant, simple equipment, a small timbered shaft, small cars, light rail, hand loading and mule haulage all contributed to a short economical life.

Jan 1, 1933

By E. E. Donath

Application of the coal hydrogenation process for the production of chemicals is described. It has been estimated that a plant to produce 31,090 bbl per day of chemicals and fuels would cost $326,- 000,000. These products would consist of 6.1 pct by weight tar acids, 50.8 pct aroma tics, 16.4 pct LPG, and 26.7 pct gasoline. THE coal hydrogenation process is well known as a means for the production of liquid fuels from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aro-matics and of tar acids and tar bases. The relative amounts of heavy and middle oil—boiling above and below, e.g., 325°C—can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.' Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydrogen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catchpot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1953

By E. E. Donath

Application of the coal hydrogenation process for the production of chemicals is described. It has been estimated that a plant to produce 31,090 bbl per day of chemicals and fuels would cost $326,- 000,000. These products would consist of 6.1 pct by weight tar acids, 50.8 pct aroma tics, 16.4 pct LPG, and 26.7 pct gasoline. THE coal hydrogenation process is well known as a means for the production of liquid fuels from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aro-matics and of tar acids and tar bases. The relative amounts of heavy and middle oil—boiling above and below, e.g., 325°C—can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.' Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydrogen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catchpot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1953

By AIME AIME

PRESIDENT BASSETT'S gavel called the Annual Business Meeting to order shortly after 10 a. m. on Tuesday. On motion of Eugene McAuliffe, reading of the minutes was dispensed with and Mr. Bassett read his annual report of the year's activities as follows : During the year I have visited eighteen of the twenty- seven sections, making an average of GG 2/3 per cent. The invitation to come again has always been extended, but in only one case have I been able to visit the same section twice. Chicago entertained the president twice during 1930. Mrs. Bassett accompanied me on visits to ten sections. Everywhere we have found the most cordial hospitality and a gratifying enthusiasm for the Institute. If anyone had fault to find with the management or felt dissatisfied with what was being done, it was carefully concealed. I am happy to report to you an agreeable, helpful and progressive spirit in each of the sections visited.

Jan 1, 1931

By Euzebio De Oliveira

ONE of a recent batch of samples from the Serra da Baliza, in the state of Parana, Brazil, contained asphalt and a dark heavy oil; and workmen on the railway from Porto União to Uruguay discovered asphalt, coming from eruptives that outcrop along the Rio de Peixe. The occurrence f asphalt in the triassic eruptives of southern Brazil, however, has been known a long time, according to Dr. Gonzaga de Campos. It is generally believed that the Botacatú sandstone is always a hard vitrified rock, from the metamorphic action f. the overflowing eruptive contacts. In this region, however, the contact metamorphism is almost nil; the sandstone is slightly hardened in a narrow zone about 20 to 30 cm. wide. In many places, the sandstone is so friable as to be easily reduced to sand, which is used-.in, mortar for building in Guara-puava and Palmas. South and west from Porto União,. this bench of sandstone is about. 50 m. thick, and is capped by a heavy bed. f basic eruptives, many of which are amygdaloids. Dr. Geo: P. Merrill, after studying the triassic eruptives collected by the Coal Commission, reached the conclusion that. "All these rocks are of typical basalt-diabases, not in any essential different other than in structure. An interesting mineralogical phase is its paucity in olivine, which in many cases is completely lacking. Professor Hussak, who carefully studied these rocks and their accessory minerals, decided that in the dikes they are granular (diabase) and, that in the lava sheets, porphyritic (augite-porphyrite or melaphyre), and that the latter pass evidently to normal diabases and are always typical of effusive rocks. The examination f many slides from dikes and sheets leads us to adopt the opinion of Professor Hussak; the rocks of the dikes are of ophitic structure, while that of the sheets show a great variety f structure and may vary from almost granular to basaltic. The great paucity in olivine had been noted by Hussak, who classes as melaphyres, the porphyritic triassic rocks in Brazil which contain olivine.

Jan 4, 1921

Jan 1, 1967

By Harry P. Hohenadel

DURING the past few years the amazing developments of the chemical industry have inspired so much publicity that the feature writers assure us that we are entering a "Chemical Age," industrially as important as the "Steel Age" and the "Electric Age," so-called. Whether or not these assurances are overstatements, it is a fact that the expansion of the chemical industry during the past 25 years has been enormous. The Chemical Bureau of the War Production Board calculates the value of chemicals produced during 1944 at $8,300,000,000, no small sum even in inflated dollars. As concerns us of the Southwest oil and gas country, four significant trends of the chemical industry are most important. (1) Many of the recently developed chemical products are new creations, not substitutes,. as new and original as the invention of the light bulb, and with a field for exploitation almost as wide. (2) Many of these chemical products will enter the mass consuming markets, which require enormous tonnages of products, and such markets are setting up an industrial demand for chemicals on a mass volume basis, compared to the relatively high-priced low-volume basis ordinarily considered as the chemical outlet of the past. (3) Most of the processes involved in producing these chemicals are adapt. able to the use, all or in part, of natural gas, oil, or refinery gases as raw mate-

Jan 1, 1945

By Robert M. Yerkes

The following is a brief account of the methods of measuring intelligence especially prepared for use in the U. S. Army, of typical results, and of some of their immediately practical applications. It has been prepared for the assistance of army examiners and for the information of all who are interested in the relations of scientific placement to military efficiency. Purpose of the Intelligence Tests Under the direction of the Division of Psychology, Medical Department, and in accordance with provisions of War Department General Order No. 74, mental tests are given recruits during the 2-wk. detention period. These tests provide an immediate and reasonably dependable classification of the men according to general intelligence. Their specific purposes are to aid: 1. In the discovery of men whose superior intelligence suggests their consideration for advancement; 2. In the prompt selection and assignment to development battalions of men who are so inferior mentally that they are suited only for selected assignments; 3. In forming organizations of uniform mental strength where such uniformity is desired; 4. In forming organizations of superior mental strength where such superiority is demanded by the nature of the work to be performed; 5. In selecting suitable men for various army duties or for special training in colleges or technical schools; 6. In the early formation of training groups within regiment' or battery in order that each man may receive instruction and drill according to his ability to profit thereby; 7. In the early recognition of the mentally slow as contrasted with the stubborn or disobedient; 8. In the discovery of men whose low-grade intelligence renders them either a burden or a menace to the service.

Jan 1, 1919

Jan 1, 1968

By J. F. Butler, H. W. Paxton

The vapor pressures of manganese in equilibrium with several alloys in the iron-manganese-carbon system between 1200° and 1275°K have been measured using the Knudsen effusion technique in conjunction with a vacuum microbalance. The effect of orifice area of the effusion cell upon the measured pressure has been determined. The binary iron-manganese system shows small negative departures from ideality, and the system of mixed carbides, (Fe, Mn)7C3, in equilibrium with graphite behaves ideally. THIS work is a continuation of the investigations in which the Knudsen effusion method has been used to determine thermodynamic activities in systems and at temperatures of interest to metallurgists. In a previous publication,' the free energy of formation of Mn7C3 was determined and some preliminary work on the solution behavior of this carbide with the hypothetical "Fe7C3" was reported. The present work deals with this latter topic and also includes data on the binary ir-on-manganese system. EXPERIMENTAL METHOD The Knudsen effusion method was used to measure the vapor pressure of manganese in both the alloy and carbide sections of this investigation. This dynamic method of vapor pressure measurement presents a problem when studying solid alloy systems in which one of the components has a much larger vapor pressure than the others. Over-all depletion of the alloy in the most volatile component will occur during evaporation so that the pressure of that component will decrease. Even more serious than the over-all concentration change is the surface depletion of volatile component in the alloy brought about by the slow rate of diffusion of this component from the interior to the surface of the solid particle. Since knowledge of this surface composition is necessary in order to relate it to the activity determined through the measurements, changes in surface composition from the analyzed bulk composition are to be avoided in dynamic vapor pressure studies of solid alloys. The system under investigation in this study presents the problem of surface depletion of manganese since its pressure at 1230°K is 105greater than iron and 1020 greater than carbon. Since the existence of a volatile manganese carbide had been ruled out previously,' the high manganese pressure relative to iron and carbon insured that the only species leaving the effusion cell was manganese. Therefore, the effusing species required no analysis so that the manganese pressure was determined directly from the weight loss of the effusion cell. In order to detect small weight losses near the beginning of effusion, a vacuum microbalance was used to weigh the cell continually. These initial weight loss data allowed the rate of manganese effusion to be determined before the surface of the alloy became depleted in manganese. The apparatus used in this investigation is shown in Fig. 1. Temperature was measured using chro-

Jan 1, 1962

By Richard W. Markley

A centralized online data acquisition system has been developed by the U.S. Bureau of Mines Pittsburgh Mining and Safety Research Center for rapidly digitizing, storing, and processing experimental signals originating up to 1100 feet away from a central computer. This system, which services seven laboratories, is currently based on a CDC System 17 1/- computer with 56K of semiconductor memory, four disk drives (one shared online with a CDC 1700), two magnetic tape drives, high-speed A/D hardware, and other input/output peripherals. The laboratories are linked to the central computer by 15-pair cables and signal conditioners and to the computer's communications controller by modems and current loops. The A/D throughput rate is approximately 30,000 samples per second (9 bit plus sign resolution) and permits scanning about 30 instruments once every millisecond for up to 100 seconds, being limited only by disk capacity. The laboratories serviced by this facility conduct explosions research and include such facilities as an Experimental Coal Mine Explosion Facility (45 channels), a Constant Volume Combustion Laboratory (4 channels), and a Simulated Coal Mine Laboratory (15 channels). Personnel support includes one systems analyst, two applications analysts, one operator, and a hardware technician. The system has performed adequately for burst-type data acquisition, but due to a lack of long-term reliability (24 hours) of the real-time multiprogramming operating system and unpredictable power failures, slow phenomena signals are generally digitized and stored offline. This latter data is input to the computer through peripherals such as a high-speed paper tape reader, or high-speed asynchronous communications ports. Processing of data is done either in real-time (as soon as data is collected) or in batch mode. Smaller batch jobs are run on this computer, and all others are transmitted by means of the system's high-speed UT 200 terminal simulator to a CDC-6000 series computer.

Jan 1, 1977

By W. F. Hosford

A series of aluminum single crystals was subjected to axially symmetric flow by drawing through dies. The orientation dependence of the drawing stress, which indicates the resistance to this type of flow, compares reasonably with predictions of Taylor and of Bishop and Hill. Measured lattice rotations likewise are generally consistent with theory. The most successful analyses of the plastic behavior of polycrystalline metal and its relationship to single crystal behavior are those of Taylor1-3 and of Bishop and Hill.4-6 The purpose of this paper is to provide a critical test of some of the basic assumptions involved in these theories. Both treatments apply to fcc metals and assume the shape change of each grain in a polycrystal to be the same as that of the polycrystal as a whole. Thus for a randomly oriented polycrystal extended under uni-axial tension each grain is assumed to undergo axially symmetric flow. dey = dez = -1/2dex, deyZ = dezx = dexy = 0 [l] where x, y, and z are a set of orthogonal axes, x being the tensile axis. Although [011.] oriented grains in bcc and fcc metals may depart markedly from this ideal behavior,7,8 the assumption is probably quite reasonable for most grains. Under a uniaxial tensile stress, ox, the work dW per unit volume expended in producing an increment of axial strain dex is, dW=oxdex [21 Since this work is expended in slip, dw =STi dyi 131 where Ti and yi are the shear stress and shear strain on the active slip systems. In both analyses Ti is taken to be the same on all slip systems, and dependent only on the total prior shear strain on all systems, so dw = Tdy [41 where t is the shear stress required for slip and y is the sum of the shear strain yi on all slip systems. Combining 121 and [4] and defining M = oX/T The ratio M is a generalized Schmid factor. It relates the tensile stress required for axially symmetric flow, ox, to the basic shear stress, 7, and it also expresses the ratio of crystallographic strain, y, to the tensile strain, Ex It depends only on the orientation of the crystal. Taylor evaluated M for various orientations by finding the least value of dy/dEx which could satisfy the shape change. Bishop and Hill, on the other hand, found M by considering the relative work (1/T)dW/dEx expended by stress states which could activate enough slip systems to produce the shape changes. The results of both methods appear to be equivalent, although certain omissions were made in Taylor's original work. The orientation dependence of M, calculated by the second method,9 is shown in Fig. 1. Taylor used the average 2= 3.06 for all possible orientations to predict the tensile stress-strain curve (oxvs Ex) for a random polycrystal from the shear stress-strain curve (t vs y) of a single crystal. Changes in M from lattice rotation were neglected so points on the ox vs ex curve were simply taken at ox = 3.06t and e = y/3.06 from corresponding points on the t vs y curve. Recent extension of the analyses of Taylor and of Bishop and Hill to crystallographically textured metals has been used to relate plastic anisotropy to textures, and to predict the potential texture hardening that could result from texture control.9 Unfortunately there have been relatively few experimental tests of the underlying theory. Taylor found that the tensile stress-strain curve of polycrystalline aluminum did agree reasonably well with that predicted from a single-crystal T-y curve. Had the single crystal undergone easy glide, how-

Jan 1, 1965

By Carl Lee

OXYGEN-FREE high-conductivity copper (OFHC brand) that is now being commercially offered for the first time represents a notable achievement in electro-metallurgy and is the outcome of endeavors that have extended over a long period. Its manufacture is novel in that electrolytically refined copper is melted in electric furnaces and cast into vertical water-cooled molds. The ingots show the "pipe" characteristic of sound gas-free metal and microscopic examination even at high magnification reveals no cuprous oxide in the copper. Owing to the patent situation, the United States Metals Refining Co., the producers, cannot at this time divulge the details of manufacture, but the operations are under precise control so that the castings are of great uniformity and the copper contains no residual deoxidant. Figs. 1 and 2 show photographs of cross-sections of a wirebar and a billet, both vertically cast.

Jan 1, 1933

By Walter Miller

Hundred-octane aviation gasoiine, toluene for T.N.T. production, high-quality lubricating oils for the needs of aviation and the armed forces, and synthetic chemicals for rubber manufacture again commanded the top priorities of the petroleum refining industry in 1944, the third year of America's active participation in the war. The objective continued to be to produce more and more of these materials—to keep up with increasingly greater requirements. By the end of the year all of the new installations projected before 1944, with the exception of possibly two or three that will tail over into January or February of 1945, had been completed and put into operation. And with the completion and putting into operation of these various units and the consequent lessening of construction responsibilities and problems, the industry was put into position to concentrate on the new operations and devote much more of its time and effort looking toward maximum output, both as to quantity and quality from the new facilities. Aviation Gasoline Making high-octane aviation gasoline continued to be the prime requisite of refining activities during 1944 as it was in the two previous war years, with the sights at the end of the year set to still higher figures than those which had been previously projected. About July I the daily output had been raised to 400,000 bbl., with some few large plant installations still to be completed and put into operation. Indications were that by December production would be up to all requirements, with good inventories. However, although by the end of the year the industry was turning out something over 500,000 bbl. a day, the estimated requirements of the armed services had been raised by a considerable figure, owing to the greatly increased aerial activities both in the European and Far Eastern combat areas. By the end of the year, therefore, the picture had changed, with the prospect for a much longer continuation of the European war, so that even with the completion and putting into operation in the United States by January 1945 of the last two or three 100-octane units authorized prior to 1944, it was evident it would be necessary to make still greater efforts to increase output of existing facilities to keep safely ahead of the game. Efforts of the industry and the Petroleum Administration for War as well as the Technical Advisory Committee and other research and development groups are concentrated therefore on methods and means of further augmenting the produc. tion of all existing refinery facilities engaged in making 100-octane aviation gasoline and components entering into it. The goal will be reached.

Jan 1, 1945

By Donald H. McLaughlin

ALTHOUGH Cerro de Pasco was well known since the early sixteen hundreds as one of the major silver districts of the Andes, its development on a modern scale did not occur until the first decade of the present century when a syndicate organized by James B. Haggin initiated the enterprise that eventually grew into the complex and widespread operations of the Cerro de Pasco Copper Corporation. Options on a few claims in Cerro de Pasco that had been brought to New York in 1900 came to the attention of A. W. McCune, a mining man from Salt Lake City, who took them to Haggin and soon succeeded in interesting that creative mining financier in the possibilities of the district. James MacFarlane, an engineer well known to both Haggin and McCune, was sent to Peru early in 1901 to make the initial examinations which promptly led to acquisition of a substantial group of claims in the heart of the mineralized area. A syndicate to which Haggin turned over his rights was organized on Feb. 26, 1902 to provide the necessary funds. The original members were J. B. Haggin, who retained a 34 per cent interest, Edward H. Clark (for Mrs. Phoebe Hearst, the widow of Haggin's old associate, George Hearst), H. McK. Twombly, H. C. Frick, D. O. Mills, and J.P. Morgan.

Jan 1, 1945

By George W. Friesen

This paper presents the historical trend and de- fines the causes of drilling cost escalation in the Gulf of Mexico during the 1970's. The three major components of escalation are: 1) inflation, 2) supply-demand imbalance (demand pull) and 3) decreases in drilling efficiency. The decade was divided into three periods. During each period one component of escalation was responsible for most of the rise in costs. From 1970 through 1973 only inflation pushed costs upward. During 1974 and 1975 a supply- demand imbalance caused most of the escalation. Since 1975, decreases in drilling efficiency have produced the major component of escalation. During any one year or period of years, the sum of the three components will give the total escalation rate. The reasons why different components contribute more toward escalation during certain years than others are shown by following the timing of oil and gas price increases, the overall quality of the acreage offered each year in offshore lease sales and the resulting drilling activity.

Jan 1, 1982

By R. M. Treco

The effect of small additions of oxygen on the hardness, density, and lattice parameters of high purity zirconium has been investigated. Precision parameter values and density of oxygen-free zirconium are given as: a,, - 3.2258 kX units, C = 5.1373 kX units, O23 = 6.507 g per cc. THE effect of oxygen on the hexagonal-phase lattice constants of pure zirconium is of interest for several reasons. The extensive hardening effect of oxygen noted by previous investigators' must be due in part to the lattice distortion accompanying its introduction and possibly to the preferred position of the oxygen atoms. De Boer and Fast' have shown that oxygen is taken into solid solution in large amounts, appearing to occupy an interstitial position. These authors also found that expansion of the lattice was not uniform since the a axis attained a constant value after the addition of 10 atomic pct while the c axis continued to expand. It was thought in the present work that this expansion of the zirconium lattice with increasing amounts of oxygen

Jan 1, 1954

By A. C. Fraker, H. H. Stadelmaier

In the systems Mo-Fe-C, Mo-Co-C, and Mo-Ni-C the phase boumdaries of the cubic Ij carbides were determined at 1000°C and the variation of the lattice parameter with composition was measured. In the system Mo-Fe-C a single ternary carbide, Mo3Fe3C, was observed. In Mo-Co-C and Mo-Ni-C two new n phases of the type M12C were found: Mo6C06C and Mo6Ni6C. At 1000°C they coexist with the M6C phases MO3-4,CO3-2C and Mo3-4Ni3-2C, respectively. Mo3C03C and Mo4C02C are not separate phases but parts of a single M6C phase region, and the same is true of Mo3Ni3C and Mo4Ni2C. THE n carbide structure type has been known since it was determined by westgren' in 1933, yet reliable information on phase compositions of this type is ap-parently scarce. The following selection of suggested formulas illustrates the extent of the confusion con-cerning compositions: W2-3Fe4-3C,1W6Fe6C,2 W2_4Fe4-2C,3 (W,Fe)6C,4 Tj.-W4Co2C and nz-W6Co6C,5 n1-W3Co3C and n2-w4Co2C,5 W3C03C and w6Co3C2,7 MO3Fe3C,8n2-M04Fe2C,9 (MO,Fe)6C,4 MO3CO3C,8 n2-MO4CO2C.9 Many of these compositions obviously overlap, some disagree in carbon content. The use of the designations 77, and n2 is not consistent. There is uncertainty whether two carbides M6C coexist or whether there is only one M6C with a wide range of substitution of one metal for the other. The existence of M12C seems questionable altogether if one ignores the results of a neutron diffraction study of W6Fe6C supporting that particular metal to carbon ratio.'' More reliable information is available for the iso-typic oxides studied by Nevitt,11 Nevitt, Downey, and orris," and Meussner and carpenter.l3 That n car-bides and oxides are structurally identical, particularly with respect to the location of the metalloid atom, has been demonstrated clearly by Stadelmaier and Meussner14 and also by Parthe, Jeitschko, and sadagopan.15 Therefore the present paper, which attempts to establish the phase boundaries of n defini-tively for three carbon systems, has implications for the whole family of filled Ti2Ni types. EXPERIMENTAL PROCEDURE The samples were prepared in two stages. Pellets weighing 3 g were compacted from powders of the elements and presintered in a closed tube of fused silica that had been evacuated to lO-4 mm Hg. This was fol- lowed by arc melting the sintered samples under argon. Remelting the button once was sufficient to produce homogeneous specimens. The metal powders had the following minimum purities in wt pct: molybdenum 99.5, iron 99.0, cobalt 99.7, nickel 99.9, graphite 99.94. Carbon determinations by the gas volumetric method were obtained from thirty-one of the one hundred samples in the annealed condition. They were limited to compositions that were critical to placing a boundary line in the isothermal sections. The carbon losses were comparatively low and averaged less than 1.5 at. pct. For annealing, the samples were sealed in tubes of fused silica evacuated to 10-4 mm Hg. The annealing schedule was 20 hr at 1250°C followed by 150 hr at 1000" ±10°C. For the water quench the silica glass tubes were broken mechanically to speed the quench. The specimens were examined in the as-cast and annealed condition by standard metallographic techniques. Some of the as-cast and all annealed samples were studied by X-ray diffraction using a 114.6-mm powder camera with filtered Co radiation. The lattice parameters of the n phases were determined by graphic extrapolation to 8 = 90 deg on a plot against sin2 8. It is estimated that the maximum error in the lattice parameters is ±0.002A.. The phase fields were determined by the disappearing phase method, relying on X-rays for phase identification and on microscopy to detect small amounts of a phase. RESULTS Pertinent information on the binary side diagrams has been summarized by Hansen and Anderko16 and Elliott17 and will not be discussed further. Photomicrographs documenting the equilibria at 1000°C have been selected to avoid redundancy due to the similarity of the three systems. Thus there will be only one picture showing an equilibrium with Mo2C, and so forth. Molybdenum-Iron-Carbon. An isothermal section of most of the Mo-Fe-C system at 1000°C is shown in Fig. 1. No attempt has been made to distinguish between a and y iron or to determine their phase boundaries. A conspicuous absence is the phase Fe2 1Mo2C6 with the Cr23C6 structure, supporting the suggestion by Krainer4 that it decomposes by annealing at high temperatures. The only ternary phase is found in a narrow range around Mo3Fe3C (MO43Fe43C14). A microstructure with a two-phase mixture of Mo + n is seen in Fig. 2. The variation of the lattice parameter of n with the estimated composition is shown in in Table IA. The phase diagram does not agree with the results of Kuo9 who reported n2-Mo4Fe2C. Our lattice parameter Varies from 11.095A at the iron-rich end to 11.140Å at the molybdenum-richoend of the phase field whereas Kuo9reported 11.26Å for Mo4Fe2C. We are in agreement with the older work

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