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By James Norman, E. W. Gieseke

Spodumene is a lithium-bearing pyroxene, and is an important source of lithium compounds. Because of its high alumina and lithia content, it might be a desirable constituent of glass batches. The use of spodumene in ceramics will undoubtedly increase, as it has been shown that a mixture of the proper proportions of this mineral with soda feldspar and potash feldspar has a much lower maturing temperature upon firing than has any one of the three components. The mineral spodumene seldom occurs as pure mineral, but ordinarily with feldspars, mica and quartz. All spodumene-bearing rocks tested contained these minerals as gangue. Small amounts of iron and manganese oxides also were present, usually as stains on the silicate grains. Mica associated with the spodumene carried a considerable amount of lithia. This was discovered in flotation tailings, which, although virtually free of spodumene grains when examined microscopically, showed 0.4 to 0.5 per cent Li²O on chemical analysis. The lithia content of micas picked from the North Carolina spodumene rock was variable. Some samples contained little lithia, others more than 3 per cent. In 1938, under the supervision of Oliver C. Ralston,S the Bureau of Mines, in cooperation with the Tennessee Mineral Products Corporation, undertook to study the beneficiation of North Carolina spodumene by froth flotation. The Bureau had previously published investigations on the beneficiation of spodumene.2,3The methods described in the second publication3 did not give good results with badly weathered spodumene rock, so that more thorough investigation of the subject was warranted. Study of Method of Flotation Separation Most of the work on concentration of spodumene was done with rock from near King's Mountain, North Carolina. Rock from two

Jan 1, 1942

By AIME AIME

OCTOBER will be western month for the Institute. With meetings at Spokane, Tulsa, Los Angeles, and San Francisco, and with a large number of American Institute of Mining Engineers members and their families in the party sailing out through the Golden Gate to Japan on the afternoon of the tenth, the major activities of the Institute will, for this month at least, be west of the Mississippi. Despite cancellations due to necessity, most of the officers of the Institute will be present and taking part in some one or more of the Western meetings. Prof. Robert S. Richards, our senior past-president, will attend both the Spokane and San Francisco meetings and then go to Japan. President Bradley will preside at the San Francisco meeting and then head the party going to Tokyo. At Tulsa and Los Angeles, the principal officers of the Petroleum Division will be present and active and at all the meetings, directors, ex-directors and -present and past officers will be on the job and keeping things moving.

Jan 1, 1929

By Tibor Stefansky, John E. Dorn

MOTT and Nabarro1-5 were first to illustrate the importance of the flexibility of dislocations in accounting for the strengthening that metals undergo due to the presence of internal-strain centers. Such strain-centers might arise from a number of causes such as radiation damage, the presence of semicoherent and coherent precipitates and clusters, as well as individually dispersed interstitial and misfit substitutional solute atoms. Each strain-center induces positive and negative shear stress fields on the slip planes of the surrounding alloy matrix. In order to effect plastic deformation, therefore, the alloy must be subjected to sufficiently high applied shear stresses to push dislocations past all such internal stress fields. If dislocations were inflexible and moved as rigid lines, they would be equally pushed and pulled by internal stress fields. At this extreme the strengthening would be vanishingly small. Dislocations, however, are not rigid; they are flexible and extensible. They wiggle between positive and negative strain-centers, thus increasing their line energy at the expense of their interaction energy with strain-centers. cottrel16 and Friedel7,8 have independently presented lucid reviews of the significance of the Mott-Nabarro dislocation-flexibility concept to the strain-center strengthening of alloys. Their analyses however were only semi-quantitative. There is evidence in the recent literature of renewed interest in a more rigorous analysis of flexibility. Thus, Gleiter9 and Gerald" have shown that the calculated strain-energy interaction between a dislocation and the stress fields of coherent precipitates can be seriously in error if the flexibility of the dislocation is not taken into account. This report will be concerned with a more detailed analysis of the problem based on the following approximations: 1) Although many types of strain-centers exist, the following analysis will be limited to the case of solute-atom strain-centers in fcc substitutional alloys. 2) To facilitate the analysis by avoiding statistical considerations, the strain-Centers are assumed to be in regular arrays on the slip plane. Although the quantitative results are somewhat dependent on the type of array that is assumed, the qualitative trends are similar for various arrays that were studied. 3) An adjustment of the results from those for square arrays to those for the more realistic case of a random distribution of strain-centers is accomplished by adopting the interesting statistical theory first introduced by Kochs,11,12 elaborated on by Dorn, Guyot, and stefansky,13 and analyzed by Foreman and Makin14 in their computerized experiments. 4) For simplicity the dislocation lines are taken to wiggle about their edge orientation and no correction is applied to their line energy for deviations from edge configurations or for the elastic interaction between segments of the now curved dislocation. It will be shown that for extremely low concentrations of atomic strain-centers the strengthening increases with the square root of their concentration. For slightly higher concentrations the strengthening rate becomes less rapid. At a critical concentration a maximum strength is obtained and a decrease in the strengthening takes place as the concentration of solute atoms is further increased. These trends are a direct consequence of dislocation flexibility. They arise from changes in the amplitude of the waviness of the dislocation line at the yield stress with solute atom concentration. Despite the simplifying assumptions that were made, the results agree qualitatively with appropriate experimental data. I) STRESS FIELDS ON SLIP PLANES Internal stresses are introduced in a lattice whenever a host atom of radius ro is replaced by another that has a different atomic radius. According to the classical theory of linear elasticity,15 the stress field about a solute atom at the origin of a spherical coordinate system is given by arr=-4G€(?_0)3 ffflfl ="W =2G€{t) f°rr^ro(l+e) UJ where G is the shear modulus of elasticity and Y, = ro(l + E) is the radius in situ, of the substituted atom. As shown by ~shelb~,'~ this approximation assumes that the bulk modulus of elasticity of the substituted atom is identical with that of the host species. ~abarro'~ suggested that the strain E can be deduced

Jan 1, 1970

By Geo. W. Goetz

The following tables show the analyses of ores from nearly all of the mines which will produce over 10,000 tons of ore each during the season of 1890. There are many small mines now in the course of development, some of which may become large producers. Many of the mines produce several different grades of ore, but the analyses given in the tables are fair averages of ore such as the respective mines can deliver. Most of these analyses were obtained from the agents of the respective ores, and are averages of the season of 1889. One can state positively that over 75 per cent. of all the iron-ores of the Lake Superior district will average over 60 per cent. of metallic iron. During the past 34 years this region has produced about 48,137,421 tons of ore, the different districts contributing about as follows: Marquette District,. 29,754,057 Menominee " .10,415,859 Gogebic " . 6,622,194 Vermilion " . 2,342,991 Miscellaneous,. .. .. 2,320 In the year 1889, the product of all the districts was nearly '1,300,000 tons. The product of the entire region for the season of 1890 may exceed 9,000,000 tons. This large amount of ore is shipped to the lower lake ports, from Escanaba, Marquette, Two Harbors and Gladstone.

Jan 1, 1891

By Shiro Ban-ya, John Chipman

The effects of many alloying eletnents on the acticity coefficient of sulfur in liquid iron have-been studied by the equilibriutn in the reaction Sfin Fe) + Hz = HzS at 1550°C'. Results are expressed in terms of a concentration variable for a nonmetallic or for a substitutional metallic solute. Activity coefficient of sulfur, defined as increased by B, Al, C, Si, Ge, Sn, P, As, Sb, Mo, W, Co, and PI. It is decreased by Cu,Au, Ti. Zr, V, h'b, Ta, Cr, ,23n, and Ni. Irulues oj. the interaction coejficient 0i = 6 In are labulated. The same interactions are expressed also in terms of atom fraction and of weight percent. The thermodynamic properties of sulfur in liquid iron have been fairly well established. Our recent paper1 reported new determinations of activity coefficient up an atom fraction of 0.12 and equations based on a careful review of all published data. The effects of alloying elements on the activity of sulfur have been studied by several investigators,2"11 especially by Morris and Williams for silicon,' by Morris and Buehl for carbon,~ and by Sherman and Chipman for manganese. phosphorus, and al~minum.~ However, the effects of some important alloying elements remain to be determined. The purpose of this investigation was to determine the effects of many alloying elements on the activity of sulfur in Fe-S-j ternary systems. EXPERIMENTAL METHOD This study was based on experimental determination of equilibrium in the reaction at 1550°C: The same apparatus and procedure as described in our previous paper have been retained, and the same corrections were applied for dissociation of H2S. The alumina crucibles used in the experiments consisted of four separate compartments. In a given experimental run. kach of three alumina crucibles held four different samples of about 3 g each which reached equilibrium in the same gas atmosphere and temperature. The charges were made up of electrolytic iron, pure iron sulfide, and desired alloying elements, which were pure metal or master alloys made in the laboratory. The weighed samples were held for 4 to 12 hr in the prepared atmosphere at 1550°C. They were then low- ered to be cooled as quickly as possible. The quenched metal beads were crushed to avoid the errors of segregation in the ingot. The sulfur content was determined gravimetrically and alloy content by appropriate chemical analysis. CALCULATIONS The apparent equilibrium constants of Eq. [I] are expressed as follows from the corrected gas ratios and sulfur concentrations: The term K" is the observed equilibrium constant in any given ternary solution, K' is the value for the Fe-S binary solution. and the limiting value of K' in the infinitely dilute solution is designated by K, which is the true equilibrium constant in Eq. [I]. In the thermodynamic treatment of nonmetallic elements in a metallic solution, it has been suggested1' that the lattice ratio has certain advantages over other variables to express the concentration of solute. In interstitial solid solutions the lattice ratio zj is proportional to the ratio of filled interstitial sites to those which remain unfilled. The equations derived for the activity of the solute using zj as the concentration variable are found also to be applicable to liquid solutions containing nonmetallic solutes when the nonmetal is treated as if it were interstitial. For this purpose we adopt the following definitions: The quantity vj which is negative for interstitial solutes is taken as -1 for nonmetallic and +1 for metallic solutes. For purposes of calculation however ; j may be assigned a value which results in a linear relation such as shown in Figs. 1 to 15. The activity coefficient of sulfur, Qs, and equilibrium constant. K(z). are defined as follows: According to a Taylor series expansion. the logarithm of the activity coefficient of sulfur in Fe-S-j ternary system is: However, the value of 6 In */6zi remains constant through a broad range of dilute solutions and the terms of higher order are negligibly small. As a consequence, Eq. [6] is simplified as follows:

Jan 1, 1970

By M. S. Azun

I do not at all agree with the basic points of the author's conclusion. The use of lognormal or normal model to respond to the attribute distribution function should be carefully questioned. If fitting a distribution function of regionalized variables is the main purpose, one may employ one of certain well-known families of distributions, such as Tukey's lambda functions. For instance, the distribution function of gold assay values studied by Krige (Krige, 1978) may fit the lognormal model well, but one should not exclude that the basic idea of using the distribution function of observed data is to have insight of the physical mechanism that gives rise to the regionalized variables. In Applied Geostatistics, there are many examples considering only lognormal or normal model for the distribution function of geostatistical data even if the observed distribution function has more than one mode. Of course, using lognormal or normal model always brings easy computation for the statistical properties of attribute under investigation. Still, I object to adopting any of those models without having any "statistical inference." As seen from the author's paper, lognormal and normal model produce the same average grade (0.746% copper) and almost the same sample variance. Therefore, which model explains the probabilistic behavior of ore deposit is always an important question that should be replied by the geostatistician using not the common sense but the statistical and probabilistic methods. For kriging procedures, such as linear kriging, one should describe either second order stationary properties or bivariate properties of regionalized variables. Second order properties, such as correlogram function or semivariogram function, are the inputs of the so-called kriging equations. Selecting one of any useable models for the observed second order properties, such as spherical model, is not easy since the models are not based on the correlations structure of the regionalized variables. How those models being used in Applied Geostatistics can be distinguished is another important problem. One may develop many fitting models to respond to the observed second order properties of regionalized variables. However, I suggest that the model should be based on the probabilistic behavior of geologic process. The author used spherical model for copper, wolfram, and silver grades from isotropic sector (Fig. 2, 4, 3b) and exponential model for silver grades obtained along raises in isotropic sector (Fig. 3a). It seems that those semivariograms given in Fig. 3b for isotropic sector and Fig. 4 may be described by the random model implying that regionalized variables do belong to renewal process (Azun, 1983). If I knew the total number of data points used in estimation, may prove that my conclusion is correct. Recalling the test for the first order sample correlogram value, the test procedure is introduced such that the independence is rejected if [Ir(1) I > Za/2 N1/2] where Za/2 is the a/2 percentile of standard normal random variable and N is the total number of samples used in estimation (Azun, 1983). For the other observed semivariogram functions I suggest the author might try to use the so-called "Markovian model" describing not only the correlation structure of regionalized variables, but also the physical mechanism that produces the regionalized variables. The Markovian model for correlogram function is, [p (h) = T 1ih , h>1 ,] The Markovian model for the other second order properties of ReV are also derived. [T veß], in the above equation, show, for example, structural change and mineralizational variation in a considered deposit, respectively (Azun, 1983). In selecting any model, it is not easy to search for the "best" response to the observed second order properties of ReV's. The Markovian model, based on a theoretical understanding of underlying mechanism, gives more information about the occurrence of regionalized variables and respond to all properties. Random model and the so-called hole effect structure can be easily defined as a special form of the Markovian model (Azun, 1983). An estimation of any second order properties of regionalized variables may be computed through (N-1) lag. However, the dependency between the regionalized variables may be deemed to have "died out" after the so-called stationarity width (range). In practice, the estimation is carried out through 25% of the total number samples available. Therefore, the large fluctuations around the zero level and variance for correlogram or covariogram function and semivariogram function, respectively, cannot be observed. Since the number of pairs involved in the estimation of higher second order properties is small, the estimation variance at those lags is large. There is no need to show higher order estimated second order properties. After using one of any kriging procedure for block estimation, the distribution function of average grades has the same mean as the drilling sample grades but

Jan 1, 1986

By William J. Coulter

WITHIN the United States the problem of meeting maximum production by our metal mines has been solved by: (1) Conservation of man power by mechanization. (2) Increasing man-power efficiency as expressed in tons per man-shift by the adoption of new and more efficient methods. (3) Production from submarginal properties made possible by some form of government subsidy. (4) Selective mining of high-grade areas. (5) Drawing on broken ore reserves and reducing advanced development work to a minimum. (6) Making maximum use of available equipment. (7) Repairing equipment that normally would be replaced. (8) Working a seven-day week on a three-shift basis to get maximum use of equipment and man power. (9) Adoption of incentive plans to increase maximum efficiency and unit production. (10) Important advancement in metallurgy, resulting in larger recoveries. (11) Improvements in safety, health, and general working and living condi-

Jan 1, 1945

Discussion of the papers of FREDERICH LAIST and HAROLD W. ALDRICH, FREDERICH LAIST and F. F. FRICK, W. L. AUSTIN, and STUART CROASDALE, presented at the Salt Lake meeting, August, 1914, and printed in Bulletins No. 91 and 92, July, and August, 1914. R. C. CANBY, Wallingford, Conn. (communication to the Secretary*). -Apropos of the experimental reduction of copper from cuprous chloride by fusion with ground limestone and coke, as described by Messrs. Laist and Frick, and also proposed for use at Chuquicamata., it might be of interest to refer briefly to the experience at Argentine, Kan., in the smelting of the suboxide of copper (as produced in the Hunt and Douglas process) containing appreciable quantities of chlorides. In the Engineering and Mining Journal of June 10, 1911, I. gave some account of what had appeared to be crucial difficulties with the Hunt and Douglas process, and how the filter-press difficulty had been so rapidly overcome after my discovery of the effect of the sodium salts in the leaching solutions. I also described the effect of the cupola furnace gases upon the lime rock with which I had replaced the coke in the absorption tower, which apparently showed the presence of considerable-chlorine, clue to the imperfect conversion of the subchloride to suboxide, as well as that clue to the difficulties of washing thoroughly the suboxide with the means provided, and also to the presence of chlorides in the cement copper which was smelted With the suboxide. The fumes from the cupola, when issuing direct into the atmosphere, were very dense and white, except when a hot furnace top caused a reddish tinge due to dust. These, fumes had a peculiarly suffocating effect, so that when they were blown over into the town the population suffered the greatest actual distress, not the mere annoyance which would have been clue to a disagreeable odor. The absorption tower had been built at the instance of the city authorities to abate this nuisance, and not with the idea of making any additional metal savings. A serious feature in connection with the Argentine experience with the Hunt and Douglas process was, that it had been implicitly assumed that there could be no metal loss in the Hunt and Douglas process itself, and that all attempts to locate the ruinous copper losses which were accumulating in the metallurgical accounts were devoted to the roasting department. It is possibly unfortunate for metallurgical advance along these particular lines that just about the time of this discovery of this previously unsuspected volatilization loss, in the smelting of the suboxide, the Kansas City company made a contract with the Western Union Telegraph Co. for its supply of copper sulphate and the Hunt and Douglas

Jan 11, 1914

By William Kent

In the paper by Mr. Fernom, on Red Charcoal, read at the first session of this meeting, it was suggested that this fuel might be used in the blast furnace with greater economy than ordinary or black charcoal. In the discussion which followed the paper, it was stated that the charcoal furnaces of the Lake Superior District have used imperfectly burned charcoal with success, and that these furnaces have given the best results in fuel economy on record. On consulting some of our well-known metallurgical authorities the writer finds that the question of the use of red charcoal, or other imperfectly burned charcoal, or charred wood, is not at all new. In Percy's late work on Fuel, pages 409-414, are given a few facts, which are here condensed, as follows:

Jan 1, 1879

By O. G. Paasche, Yuan-Shou Shen

THERE is a disagreement among the various authors about the exact manner of transformation of ZrCr2. Rostokerl and others2 stated that ZrCr2 had a C-14 (MgZn2) type of structure below 1000°C and a C-15 (MgCu2) type of structure at temperatures above 1000°C. Alisova3 and others4 reached the opposite conclusion and stated that the transformation temperature is close to the melting point of ZrCr2. A literature survey shows that various investigators3'= who homogenized the specimens at a temperature higher than 1000°C have concluded that ZrCr2 had the C-15 structure at room temperature. Meanwhile, Jordan et al.4 reached similar conclusions without annealing the specimen. Other investigators1,2,6,7 who X-rayed the specimens in the as-cast condition without annealing reached different conclusions. The investigation reported herein was conducted with the aim of exploring the exact manner of transformation of ZrCr2 by various heat treatment tests. The alloys for this examination were prepared from iodide-reduced zirconium crystal bars, 99.9 pct purity, and electrolytic chromium, 99.9 pct purity. They were melted in a nonconsumable electrode arc furnace with water-cooled copper crucible in a helium atmosphere. The melting loss of each alloy was less than 1.5 pct by weight. Chemical analysis of a randomly selected specimen indicated that there was a very close agreement between calculated and analyzed compositions. Before being heat-treated each specimen was encapsulated in a vycor or quartz tube inside which an argon atmosphere was maintained at a pressure of lower than 1 atm. In determining the crystal structure of each specimen with a Debye-Scherrer camera, the standard procedure8 for X-ray quality analysis (Hanawalt method) was followed. The different series of heat treatment tests in this investigation are tabulated in Tables I and 11. The tests in Series I, specimens from 1-1 to 1-9, which were similar to Rostoker's experiment1 indicated that the transformation temperature seemed to fall between 870° and 900°C and that the crystal structure of ZrCr2 at lower temperature seemed to be of the C-14 type. However, once the compound is transformed to C-15 type, it is impossible to reverse the transformation back to the C-14 type by first heating the specimen above 900°C and then annealing it slowly below 900°C as shown in Experiments II-1 to II-3. Thus, it appears that the specimen of ZrCr2 will transform from C-14 to C-15 structure when heated above 900°C but will not transform from C-15 to C-14 when annealed slowly passing 900° C even after the extremely slow cooling process such as indicated in the experiment of Specimen II-3. As a valid transformation temperature is a temperature at which the transformation is reversible, therefore the temperature 900°C (or other temperature close to 900°C) is not the transformation temperature for ZrCr2 and the C-14 structure is not the stable structure of ZrCr2 at lower temperatures. The C-14 structure is retained at room temperature because the transformation to C-15 structure is very sluggish and the fast cooling after melting does not allow enough time for the transformation to take place. Additional energy is required to alter the metastable condition of the C-14 structure. The sluggishness of this transformation was again demonstrated through another series of experiments. Four specimens with C-14 structure were taken. Then they were annealed at 900°C but each specimen was soaked for a different period of time, Table 11. X-ray diffraction patterns of this group indicated that the C-14 structure gradually disappeared as the soaking period was lengthened. The figures listed under the column "C-14 Structure, pct" were estimated from the intensity of the d = 2.330 line of the diffraction pattern corresponding to the structure. Notice that the intensity of this line became weaker for longer soaking periods. To determine the transformation temperature of ZrCr2, specimens with C-14 structure (as-cast condition) were annealed at 1300°, 1400°, 1500°, 1550°, and 1600°C, respectively. A final specimen was first heat-treated to 1500°C in order to transform it to C-15 structure, then heat-treated at 1600°C again. From the X-ray analyses of this series of tests, Specimen Nos. III-1 to III-6, it is evident that a transition from C-15 structure at lower temperatures to the C-14 structure occurs at some temperature between 1550° and 1600°C.

Jan 1, 1969

By William Kent

(Read at the Philadelphia Meeting, February, 1878.) IN the paper by Mr. Fernow, on Red Charcoal, read at the first session of this meeting, it was suggested that this fuel might be used in the blast furnace with greater economy than ordinary or black charcoal. In the discussion which followed the paper, it was stated that the charcoal furnaces of the Lake Superior District have used imperfectly burned charcoal with success, and that these furnaces have given the best results in fuel economy on record. On consulting some of our well-known metallurgical authorities the writer finds that the question of the use of red charcoal, or other imperfectly burned charcoal, or charred wood, is not at all new. In Percy's late work on Fuel, pages 409-414, are given a few facts, which are here condensed, as follows:

Jan 1, 1878

JOHN B. HASTINGS, Los Angeles, Cal. (written discussion *).-This, paper is so admirable for its brevity that one hesitates to enter into discussion. The cycle of eruptives makes one wonder, "Where's the basalt?" and the youthfulness of the Idaho flows suggests they may yet come. Veins and Dikes.-Veins and dikes seem to be closely aligned in the minds of some authors, while to me they appear quite distinct, the first representing quiet, long-continued action, typified by metasomatic replacement, far removed from volcanic action; the latter, sudden and cyclonic, emanating from the heart of vulcanism. The rock openings occupied by both types were formed by kindred forces, but in the one they were closed for indefinite periods before invasion by the solfataric solutions, and in the other their formation and occupation were simultaneous. Open Fissures.-I do not believe in the existence of open spaces of discission that may be occupied by veins. Occasionally they occur; I found one with. a machine drill 350 ft. below surface, fortunately in an adit; the water spouted for 12 ft. in a 6-in stream for nearly 24 hr. It was only a flattish fissure, 6 in. wide, crossing the perpendicular vein, and indicating how tabular veins of ore might be formed. The practical absence of open fissures should be a joy to miners. We all know the misgivings with which we feel about for an old winze having only 30 ft. of water in it, in an unsurveyed and inaccessible part of a mine. It is said that veins are sometimes formed in open spaces left by Protuberances of the walls, which meet after having been displaced; but I believe that in such circumstances there would be sufficient attrition and brecciated material to fill the fissure, though perhaps loosely. Parts of veins may possibly have been formed in originally open spaces, but if so, the spaces were made by solution shortly preceding the deposition of the veins. That total solution of rock adjacent to a fissure may occur under favorable conditions is proved by the existence of large bodies of sulphide which contain only a few per cent. of silica; while on the same level, and in other levels above and below, all being within the same ore shoot, assays may show as much as 50 to 60 per cent. of silica, although the gold, silver and copper assays may be almost identical in all the

Jan 1, 1918

By Walter E. Mingramm

The construction of rescue-apparatus on the principle of furnishing the wearer with air from a tank containing it under high pressure was given up by inventors about 20 years ago. Such an apparatus must supply continuously, for not less than two hours, nearly 50 liters of pure air at atmospheric pressure per minute, or a total of 6,000 liters (210 cu. ft.); and a cylinder containing this amount of air, under 2,000 lb. pressure, would weigh 180 lb. or more. Although apparatus has been recently constructed utilizing liquefied air, no experiments have been made to determine the regularity with which the air is generated, nor has its chemical composition been determined. Moreover, the chief objection to such an apparatus is the difficulty and cost of keeping on hand a large quantity of liquefied air. The system of furnishing the wearer of a breathing-apparatus with air which has given the best results, and has found

Jan 1, 1909

By Nicholas J. Grant, Robert F. Wilde

TAYLOR and Floyd's"" work in establishing phase diagrams based on the elements Ni-Cr-Ti-A1 has led to an understanding of the precipitation hardening mechanism in alloys based on these elements. Nordheim and Grant4 concluded that in simple alloys, and where the aluminum to titanium atomic ratio was such that less than three out of five aluminum atoms were replaced by titanium, the precipitate on aging is the face-centered-cubic Ni 3A 1 phase, called They further found that increasing amounts of hexagonal ? phase, Ni3Ti, precipitated from these alloys when the titanium content exceeded the solid solubility of both matrix and Ni3A1. For alloys of Ni-Cr-Ti-Al, in which the titanium and aluminum contents each ranged from 0 to 4 wt pct, the titanium-rich was superior for strengthening to either pure ?' or 7. It was also noted that the combined titanium plus aluminum content (atomic pct) was a direct measure of the high temperature strength and overaging temperatures for these alloys.4 The present investigation was undertaken to extend existing data on precipitation hardening in the more complex commercial alloys containing higher titanium plus aluminum, and with significant quantities of cobalt, molybdenum, and carbon. Experimental Procedure Reforging of As-Received Bar Stock—The alloys were received as ground, forged bar stock. Chemical analyses and the as-received bar diameters are shown in Table I along with the ASTM grain size after the various treatments. All stock except the Waspaloy was reforged to % in. diam to gain material and to facilitate machining of stress-rupture specimens. Forging was carried out at 2100°F, and discontinued when the bar temperature fell to 1800°F. Heat Treatments—For experixental simplicity it was desirable to heat treat all of the alloys at, the

Jan 1, 1958

By E. R. Russell, N. E. Richards

The current ejyiciency of aluminum cells was derived from the metal produced over a period of time and the theoretical faradaic yield. The difference in the actual amount of aluminum in the cathode at the beginning and end of the period must be determined. The weight of aluminum in the cathode was calculated from the dilution of an added quantity of impurity metal. Use of multiple indicator metals, copper, manganese, and titanium, demonstrated that the weight of aluminum in cells can be determined to within 1 pct with routine but careful chemical analyses. Over intervals of the order of 30 days, current efficiencies reliable to within 1 pct can be obtained. INVESTIGATIONS beginning with those of Pearson and waddington ,' through the most recent published work of Georgievskii,9-11 illustrate the direct relationship between the composition of the anode gas and the applicability of analysis of anode gases to the control of alumina reduction cells. McMinn12 noted the lack of an independent method for measuring cell production efficiency over the short term. There is no doubt that changes in the current efficiency are immediately reflected in the composition of anode gases. However, the accuracy of faradaic yields calculated from gas analyses depends upon the degree of interaction between primary anode gas and Carbon.6 A conventional industrial practice of obtaining long-term current efficiency for production units from mass balances and quantity of electricity is generally insensitive to the impact of planned control of any one or more of the influential reduction cell parameters such as temperature, alumina concentration, and mean interelectrode distance. Consequently, there is a real need in the aluminum industry for a procedure to obtain the absolute cell current efficiency over a short term—10 to 30 days—both for the calibration of values obtained from gas analysis6 and for evaluating the effect of controlling specific parameters in the reduction process. The amount of aluminum produced may be determined by considering the cathode pool as a reduction of an impurity metal in aluminum. Analyses over a period will show a decreasing concentration of the impurity due to the accumulation of aluminum solvent. The increase in aluminum inferred from analyses is the amount produced by the cell during the period. Combining weights of the cell aluminum in the cathode at the beginning and end of a specific period, weights of aluminum tapped and the quantity of electricity passed during the interval will yield the current efficiency. Smart,I3 Lange;4 Rempel,15 Beletskii and Mashovets,16 and winkhaus17 have used dilution techniques to determine aluminum inventory in alumina reduction cells. A technique for determining the weight of aluminum in production cells by addition of small amounts of copper to the aluminum cathode was described by smart.13 The precision in values of the aluminum reservoir through dilution of copper in the cathode ranged from about 1 to 3 pct depending upon the quantity of copper added in the range 0.2 to 0.01 wt pct, respectively. Because the method appears so direct and apparently simple, one would not anticipate difficulties in application to industrial cells. The objective of this study was to resolve this problem associated with the trace metal dilution technique for determining the amount of aluminum in a cell. The approach in evaluating trace metal dilution as a basic factor in determining the weight of aluminum in the cell reservoir, and the absolute current efficiency of the Hall-Heroult cell, was to dilute more than one trace metal in the aluminum cathode so that we could discriminate among complications arising from physical mixing, the possibility of separation of intermetallic compounds, loss of the added elements, and chemical detection. EXPERIMENTAL METHODS These experiments are not complex but require standardized procedures. The technique involves addition of the trace metals to the cathode, knowing when these metals are homogeneously distributed in the liquid cathode, timing of the sampling, employing accurate and precise analytical methods, using reliable procedures for monitoring the amount of electricity passed through the cell, and accurate weighing of aluminum removed from the cell during the particular period. More accurate results might be obtained if the increment in concentration of the added indicator metals were of the order of 0.1 to 0.2 wt pct. The method must be applicable to production units and, hence, the contamination of the aluminum minimized. For this reason, the concentration of trace metals in the cathode was kept below 0.07 wt pct and generally at 0.04 wt pct level. Trace quantities of copper, manganese, titanium, and silicon are already present in virgin aluminum and are suitable as additives from electrochemical and analytical points of view. Concentration of silicon is quite dependent upon the characteristics of the raw materials and was not used extensively in this work. Chemical Analyses. All instrumental analyses require calibration against an absolute technique such as a gravimetric, volumetric, or spectrophotometric method which represents the ultimate in sensitivity, precision, and accuracy. On review, the best methods for copper appeared to be optical absorption without

Jan 1, 1969

By C. P. PERIN, DONALD BELCHER

T HE production of pure iron by electrolyzing solutions of its salts has been the object of scientific curiosity and research for about 80 years; and in the last two decades a realization of the unusual physical and chemical qualities of electrolytic iron has turned the attention of chemists and metallurgists toward a commercial application of this accumulated knowledge. Thus Burgess and Hambuechen in America, . Cowper-Coles in England, and Fischer in Germany- devised methods, more or less successful, for the electrolytic refining of iron, but none of these processes has yet attained large-scale operation. During the war some interesting ,work was done in France and England on building up worn or defective machine parts by electrodeposition of iron. It remained for the Société "Le Fern in France to carry on the process commercially. For six years Les Fonderies et Forges. de Sainte-Maire et Gravigny and the works of Bouchayer & Viallet at Grenoble have manufactured pure-iron boiler tubes in competition with established practice. The French process originated in the researches of Anthelme Boucher in 1910, and was, not put into operation until several years of experimentation had passed.

Jan 1, 1921

By Zay, Jeffries

THE effect of thoria (ThO2) on grain growth in tungsten was discussed in some detail in a paper presented before this Institute by one, of the authors in 1918.1 In that paper it " was assumed that the, thoria was present in the tungsten entirely as a mechanical mixture. There was no indication in the experiments described that even a trace of the thoria was in solid solution in the tungsten. Langmuir,2 however, observed that thoriated-tungsten filaments under certain conditions showed electron emissions many thousand times greater than unthoriated tungsten at the same temperature. He concluded from his studies that a slight amount of the thoria had dissociated on heating the filament to a temperature near 220°. C. At this temperature and higher, part of the thorium diffuses to the surface of the filament where it evaporates at. a much faster rate relatively, than the tungsten, and also at a rate, nearly as fast as it is brought to the surface by diffusion: If the temperature is lowered to say 1800°,. C., diffusion of the thorium atoms to the surface is more rapid than evaporation, sown adsorbed film of thorium atoms is produced on the surface of the tungsten filament. The electron emission is governed by the outside layer of atoms so the emission from such a filament might be expected to approxi¬mate that of a thorium filament at the same temperature. PRESENCE OF METALLIC THORIUM IN THORIATED TUNGSTEN If the filament containing the adsorbed film of thorium. is heated to a sufficiently high temperature, the thorium atoms evaporate: rapidly and the electron emission becomes more nearly that of tungsten. On cooling again to 1800° C., or thereabouts, the emission 'builds up gradually to a maximum. The filament containing the adsorbed layer of thorium atoms is said to be "activated." By studying the rates of activation under different conditions of prior thermal treatment and at different temperatures, Langmuir was able to arrive at an estimate of the

Jan 1, 1927

By David White

THE search for potash salts in the great "Red Beds? region of the Southwest, conducted for several years by the U. S. Geological Survey, the work being carried on for a part of the time in coöperation with the Bureau of Economic Geology and Technology of the University of Texas, has resulted in the discovery, within shafting depth, of potash salts, apparently of workable thickness and commercial quality, and prob-ably of great extent. Definite information is lacking as to the exact thickness of the potash beds, the size and boundaries of the areas underlain by workable strata, and the locations of the deposits richest and most favorably situated for exploitation. Briefly to review the salient features, of the general situation: We have in the great Red Beds region of the southwestern United States, embracing portions of central Kansas, western Oklahoma, eastern New Mexico, and northern and western Texas, .a series of sandstones. shales, anhydrite beds, clays and limestones, which; through an interval of 1000 ft., more or less, carry beds of salt, estimated by Darton1 to contain over 30,000 billions of tons of rock salt. It is the greatest known salt field of the world. At some points the intercalated beds of rock salt, one of which is reported by the driller to exceed 300 ft. in thickness, aggregate, accord-ing to the drillers' records, over 1000 ft. The sedi-mentary strata are similar in composition to those carrying the potash deposits of western Europe, and they were laid down at the same time and under condi-tions which, in many respects at least, were similar The stratigraphy and character of the beds are des-cribed by Darton2 and a, part of the area and the reported aggregate thicknesses of salt are shown, with some revision after Darton, in the accompanying map Fig. 1. The assumption that in the great areas of shallow evaporation basins spread over -the vast base-level region of saline deposition in the Southwest during Permo-Triassic time, potash salts were in some places, and at different stages, thrown down in crystalline deposits associated with the beds of rock salt, anhydrite, and gypsum, is, geologically speaking, more than reason-able. They are to be expected, and the conviction that they are probably present has long been held both in the Texas Bureau of Economic Geology and Tech-nology, under Dr. J. A. Udden, and in the- U. S. Geological Survey. Accordingly, for many years, efforts to determine whether potash deposits are present in this region have been made, though under very great difficulties, such as insufficient funds for boring, hack of drilling on private initiative in the more promising regions, hack of interest at first on the part of the drillers and companies, and, hater, inadequacy both of the methods of boring and of the sampling, to reveal in definite terms the thickness-of any saline stratum of given composition.

Jan 4, 1922

By J. E. House, J. L. Drobnick, R. R. Swanson, D. W. Agers

Since the commercial acceptance of the liquid ion exchange process in the mineral processing industry, it has been predicted that eventually the hydrometallurgist would have a wide selection of commercially available chemical reagents to make separations efficiently and economically of virtually all metals in solution under a wide range of conditions. Several years ago, General Mills began a research and development program to determine if it were possible to develop a reagent to extract a specific metallic ion from solution at a cost that would allow large scale commercial application. A giant step toward reaching this objective was announced in late 1963, when development quantities of LIX®-63 reagent, a highly selective reagent for the extraction of copper, were first offered to industry. The properties of this reagent were de- scribed in a previous paper.1

Jan 12, 1965

By J. E. Johnson

The subject of blast-furnace slag is one which has had much consideration, particularly from the scientific standpoint, and several years ago technical literature contained many learned discussions on the oxygen-ratio of the acids and the bases, all on the assumption that acids and bases must be present in a ratio depending on molecular weight and chemical valency. Much work has also been don.e, sometimes in conjunction with the former, on the total heat and the temperature of initial fusion or softening of various slags. A wider knowledge of the blast-furnace now enables us to say that for practical purposes this work has been of almost no value. It is now generally admitted that on,the physical side the important point of a given slag is neither its total heat of fusion nor its softening-point, but its free-running temperature, since this is the critical temperature of the furnace. This temperature bears no definite relation to the softening-temperature, as determined by Seger cones, for instance, because some slags melt relatively like ice, with a very short viscous-range, while others melt relatively like tar, with a very long viscous-range. In one the difference between the softening- and the free-running temperature may be very small, as little as 100° F., while in another this difference may easily be 200' or 300°. The importance of this difference is so great in practice as to destroy completely the value of exhaustive investigations, even such as those of 0. Boudouard, published a few years ago.'

Jan 1, 1913