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By J. Burns Read, Charles H. Fulton

A previous article1 by the authors contained a general description of the new roasting furnace herein described but it did not go into detail as to the metallurgical behavior or the results obtained. Believing that such information would be of great value, they have elaborated on the subject and have given many unpublished details. The furnace described applies the principle of roasting finely divided zinc-sulfide ores, now produced in large quantity by the flotation process, in gaseous suspension; that is, the ore particles are carried, in suspension, in a current of air and gaseous products of the roast. The relatively great fineness of flotation concentrate presents difficulties and problems of roasting in furnaces of the ordinary type; the fine ore is forwarded through the furnace in the form of a shallow bed and its very fineness leads to dense impervious bedding which prevents oxygen from reaching the interior of the bed, thus unduly lengthening the time of roasting and preventing the elimination of the last of the sulfur. The fineness of the concentrate, normally, should lead to a rapid and complete roast, for the speed of roasting is a function of the surface exposed to oxygen, which surface is greatest, per unit of weight, in very fine material. The difficulty in bed roasting is to get the oxygen to the particle. If the fine ore, during the roasting, could be freely suspended in oxidizing gases, full advantage could be taken of the great surface conferred by its fineness. This fundamental idea, of course, is not new, for the Stedtefelt furnace, familiar to the older metallurgists, is an example of it; but the manner in which this is accomplished may be new. The numerous efforts to roast in gaseous suspension show that the idea is attractive; in fact, an analysis would indicate that it is the most reason-

Jan 1, 1925

By A. Hellawell

Specitlrens of the Al-Ge eutectic alloy have been frozen unidivectionally at rates between 2.5 x 10-6 and 2.5 x 10-4 cm per sec and the structure examined by optical and X-ray methods. There is no epitaxial relationship between phases, the aluminum having random orientation and the germanium a preferred (011) fiber textuve. Lamellar colonies which are BINARY eutectic alloys occur between either silicon or germanium with the metals aluminum or silver. common in this alloy are constructed from axial and nonaxial (111) plates of germanium which are related by a variety of twin configurations. Irregular or globular regions of the microstructure are composed of continuous single crystals of each phase, the germanium being heavily twinned. There is limited solid solubility in these systems, and the eutectic phases all involve diamond cubic with fcc crystal structures. In the microstructures of these eutectic mixtures the silicon and germanium crystals exhibit an almost infinite variety of shapes which are notably sensitive to

Jan 1, 1968

By Wayne E. Glenn, R. W. French, Lincoln F. Elkins

The Lance Creek Sundance reservoir provides a case history of ro years performance of a reservoir in which unit operation has permitted effective utilization of gravity drainage augmented by primary pressure control with injection of gas into top structural wells. Detailed performance of the reservoir is presented by means of maps of Well status, reservoir pressure, individual well recovery, etc., and by pool-performance charts. Analysis of reservoir performance indicates only minor water encroachment, so that gravity, injected gas, and expansion of gas are the main oil-expulsive agents. A simplified theory of regional drainage of oil from upstructure location to downstructure location due to gravity is presented and checked by means of comparison of "reservoir" permeability and "well" permeability from the pool performance. Good order of magnitude agreement was obtained. Individual well performance and overall reservoir performance indicate possibility that maintenance of pressure makes ineffective those parts of the reservoir in which permeability is too low to permit effective drainage of oil by action of gravity. Oil from these parts can be recovered only when pressure is reduced locally by selective withdrawal or when overall reservoir pressure is finally reduced.

Jan 1, 1949

By E. H. Fahmy, L. C. Uren

During recent years, oil producers have observed with interest the practical success which has attended the application of water as a medium for displacement of oil from its reservoir sands in the Bradford field of northern Pennsylvania and southern New York. Here, according to various authorities, additional recoveries of frorn 2,000 to 12,000 bhl. of oil per acre have heen secured by this method, after ordinary flowing and pumping. rnethods of production had practically reached the lower limit of economic operation. Notwithstanding the success which has attended the practical use of the flooding process in the Bradford field, oil producers in other regions are skeptical of its value when applied under physical conditions differing markedly from those which characterizc the Bradford field. Its usc would probably he construed as illegal in most of the oil-producing states. This general relnctance on the part of oil producers in other regions to accept the flooding process is due in large part to lack of infor-n~ation regarding the factors that influence its operation and efficiency. With the purpose of clarifying to some extent the issues involved, and of determining when the flooding proccess may or may not beeffee-tivcly ernployed, the writers have conducted a serics of laboratory exper-imentments under carefully controlled conditions, designed to indicate, the influence of various physical, chemical arid lithologic factors. These experments have not been conducted under conditions identical with those which exist at depths far below the earth's surface, so that direct quantitative comparisons with field results are not justified, hut it is believed that the experimental results at least warrant qualitative inter-pretations that may he applied to field conditions. The methods employed in the conduct of these experiments are briefly explained, and the results, together with the conclusions based thereon, arc presented. FactoRs Influencing Displacement of Oil froM SaNdS by WAteR- flooding Before presenting the experimental data, it, will he desirable to con-sider the manner in which the residual oil is retained within the oil sand

Jan 1, 1928

By J. Parke Channing

THESE days of great industrial and social problems in America produce many suggested solutions and great changes. The practical engineer and employer of labor views these problems differently from the labor leader or the social reformer, but as never before he is sincerely interested in solving them in a way that will be just to all. The inevitable tendency of the day is toward "industrial betterment," "safety," "industrial education," "efficiency," and the many other things' which have become so familiar to progressive employers. There is no longer any question that these things are worth while from both the hu¬man and economic standpoints. They "pay" in dollars and cents. The very center of final success in improving conditions and increasing the efficiency of workingmen must be the spirit of fairness and a knowledge on the part of the employer of how to deal sympathetically and intelligently with his employees. Every progressive employer knows how greatly he desires foremen, superintendents, managers and others who possess these qualities. On the other hand, we are all familiar with serious mistakes made by young graduates of engineering schools who have had no opportunity to develop these qualities, and who have no real appreciation of the worth of the workers. Indeed, one wonders whether much ill-feeling, labor difficulties, and many strikes could not be avoided if such men had the right attitude. Is there any way of remedying this condition? If this particular difficulty can be solved, if these young engineers, many of whom are our coming leaders of industry, can be given the right perspective and the right understanding of these other problems in addition to fair, sympathetic methods of handling men, many of our other problems will be solved-not at once, but gradually and permanently, as these men make good and become influential in paths of industrial righteousness and industrial peace. Many progressive employers of to-day have enlarged their own perspective and realize the great importance of enlarging the perspective of those who shall follow them.

Jan 3, 1915

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Jan 1, 1938

By Arthur Phillips, E. S. Bunn

During the past few years considerable interest has been shown in the study of fiber, and its effect, in wrought metals. Fiber has recently been defined as a "condition of parallelism of important lines or details in the structure."' Briefly stated, two distinct types of fiber are commonly encountered. One results from the alignment in the direction of working of constituents, more or less segregated, such as slag, oxides, carbides and dendritic formations. The second, and least understood, type is produced by working the metal below the recrystallization temperature in such a way as to develop a parallelism of the grains. This condition is readily recognized by the pronounced elongation of the grains in the direction of working. Under certain deformational treatments the grain fragments produced by cold working tend to orient in certain definite directions with respect to the axis of extension. Furthermore, even in metals that have been annealed after cold working preferred orientations may be present. It is perhaps logical to assume that such marked parallelism of structural elements would be manifested by directional properties in the metal. As a matter of fact, tests on many kinds of materials have shown differences in varying degrees. In recognition of this condition, proper design, for many purposes, places the fiber axis in such a way as to present the direction of maximum strength to the greatest applied stress. Earlier Investigations Howe2 has written at considerable length regarding the causes and practical significance of fiber in steel and wrought iron. His studies showed that wrought iron and the puddled steel sheets (materials of plastic origin) were weaker transversely than longitudinally. The transverse deficit ranged from 5 to 29 per cent. The longitudinal tests

Jan 1, 1931

GENTLEMEN Herewith are transmitted reports from the Treasurer and of the principal standing committees of the Institute. To these special reports members are referred for details as to the year's work. Despite the unfavorable business conditions obtaining throughout the year, the Institute was able to carry on its various activities without curtailment and without drawing on the surplus accumulated through previous years. In fact, small additions were made to the Life, Member¬ship and various other funds. It is highly desirable that such additions should continue to be made, especially to the Life Membership fund, for reasons reported last year. At present, money must be used from current receipts in order to enable the Institute to fulfill its obligations to those who on joining the organization commuted their dues by a single payment. In addition, with the passage of years the number increases of those who have paid dues forty years or more and who, by reason of age or dis¬ability, are unable longer to practise their profession. These men have supported the Institute through their active professional life and it would be a pity to lose them as members through resignation or for failure to keep up their dues. In accordance with the By-laws the Board has authority to advance such members, on application, to the Honor Roll of Senior Members and to relieve them from further payment of dues. It has been the policy of the Board to do this liberally, but to keep up this, as well as to meet other obligations, it is necessary for money to be provided. It has been estimated by the Treasurer that nearly $50,000 additional should be placed in the Life Membership fund as soon as possi¬ble to meet these obligations without using current income and to that end it is necessary, not only to avoid running behind currently but to earn, if possible, some surplus each year. The small amount transferred to the Life Membership fund from surplus this year was, as a matter of fact, made possible by certain members paying personally bills that were properly chargeable to the Treasury. Such generosity is common among those active in Institute work and probably no year would have closed with a surplus except for it.

Jan 1, 1923

By W. M. Peirce, R. K. Waring

Zinc of high purity offers definite advantages in certain fields. A process by which zinc of 99.99 + per cent purity is produced by pyro-metallurgical methods is described in this paper. The process consists of a fractional distillation following the primary reduction; this fractional distillation employs the principles of rectification for the separation of lead and other high-boiling impurities and cadmium and other low-boiling impurities. Theoretical Considerations Involved in Production of High-purity Zinc by Distillation Fractional distillation, fractional condensation, and rectification are recognized methods of separating mixtures of liquids. In the field of organic liquids these methods are widely used but not commonly to effect as complete a separation of liquids as is done in the problem under consideration. Zinc boils at 905" C., cadmium at 778" C. and lead at about 1620" C. Zinc may contain from several hundredths of one per cent to over one per cent each of cadmium and lead, and the problem is to reduce these impurities to a few thousandths of one per cent. For lead and zinc, the spread in boiling points is substantial, 715° C., while for zinc and cadmium it is only 127" C. The basic limitation of any separation by distillation may be found from the relation between the equilibrium composition of the vapor and the liquid for all mixtures of the two substances involved. If a mixture of constant boiling point is found, or if a stable compound that vaporizes without dissociation occurs, there is a definite theoretical limit to the degree of separation that is possible when operating at atmospheric pressure with respect to that mixture. Otherwise, any degree of separation is theoretically possible. The equilibrium composition of vapor in contact with liquid mixtures of zinc and cadmiurn at the boiling point has been determined experi-

Jan 1, 1937

By N. H. Emmons

(Canal Zone Meeting, November, 1910.) AN interesting development of copper blast-furnace construction has been brought about in adapting the blast-furnace to be a "burner" for sulphuric acid making. When the Tennessee Copper Co. first decided to construct an acid-plant, the standard type of brick-top furnace, supported by structural steel, was the only one in use at this plant. All the tests for temperature and strength of gas had been made on these furnaces, and had been satisfactory. When, however, the acid-plant was put on the flue, and the flue had to have a damper put in it to force the gas into that plant, troubles began. The furnaces were fairly tight, and for a few months the work was quite satisfactory., Fig. 1 shows the old type of furnace-top used at the start. It was soon found that this top would not stand the temperatures, particularly when dampered back, as was necessary to force the gas into the Glover towers. The structural steel, of which the furnace skeleton was constructed, warped and twisted so badly that it was not safe to use the furnaces. This effect is shown by Fig. 2, which is a photograph of old No. 4 furnace, after the brick-work had been removed. It became apparent that a new type of top was necessary and the engineering force was started oil the design of a new furnace-top, with the result that a low top, with brick-lined flues at each end below the feed-floor, leading to the main concrete dust-chamber, was constructed. This furnace, No. 7, is shown in Fig. 3. The charging-doors are made of cast-iron sections, three sections to a door, and three doors to a side. A door to the furnace was made of cast copper, but the heat was so great that the copper bent readily, due to the jarring of its * General Manager, Tennessee Copper Co.

Feb 1, 1911

Jan 1, 1969

By Gopalan Ramadorai

Tailings water from primary flotation concentrators usually contains minor amounts of pollutants such as heavy metals, cyanide and solubilized molybdenum, which are solubilized in the flotation process. A review of various techniques to reduce pollutants to acceptable levels is presented. Generally, molybdenite ores are processed by conventional size-reduction techniques, followed by flotation to produce a metallurgical-grade concentrate of 88% to 92% MoS2. Reagents commonly used in the milling process include: vapor oil (collector); pine oil, MIBC (frother); Dowfroth 250 (water-soluble frother); lime (rougher pH control); and sodium cyanide (Fe and Cu depressor). For lead depression, Nokes reagent is stage-added to the regrind mills and cleaners. Flocculant is added to obtain clear overflows in the intermediate thickeners.

Jan 9, 1978

By Dae S. Young

A new probabilistic approach is introduced for slope stability analysis including adverse impact of blasting vibrations. The material strength within a slope area is randomized in this bi-variate joint probability analysis. To be a completely general engineering method, the new probabilistic approach employs the random variable transformation technique: the Hermite model of the Gaussian transformation function, which transforms the experimental histogram of strength values to the standard Gaussian variables. Because bi- normal joint probability is analyzed on the true probability region projected on the Gaussian transformed variable plane, it is an exact solution of slope stability based on the available sample data. Details of the probabilistic approach are given through a case study on an iron ore mine. The case study demonstrated that the probabilistic approach is effective and simple enough to be a routine engineering practice for slope analysis.

Jan 1, 1984

By T. A. El-Bassyouni, Paul Gordon

Grain-gvowth data in zone-refined aluminum and in dilute alloys of copper with this aluminum have been obtained. The amounts of copper added were from 4 to 400 at. ppm. It was found that in both the unalloyed aluminum and the alloys grain growth was characterized by a high value of n in the isothermal growth equation 6n = Kt The inadvertent presence of 1 at. ppm Fe in the alloys was found to he more potent in slowing growth than the purposely added copper. Possible rationalizations of these observations and their general relevance to the theoretical use of gvain-grozvth data have been discussed. Grain growth data of Winegard and his co-workers' on zone-refined tin and dilute tin alloys were analyzed with some success2 in terms of approximate theoretical equations for boundary migration.2-4 In view of this success, experiments were carried out in an effort to obtain similar data on zone-refined aluminum and on dilute copper-in-aluminum alloys. The results obtained were anomalous in several respects and could not be used to test theory. A discussion of these anomalies is presented here; they have been attributed to impurity effects and serve to emphasize the sensitivity of grain growth in general—and the particularly high sensitivity in aluminum—to impurities. The resulting difficulties in the theoretical use of grain-growth data are also discussed. EXPERIMENTAL DETAILS An aluminum bar was zone-refined and leveled by methods similar to those described previously.' The degree of purity obtained is indicated in Table The data in Table I were determined by mass-spectrographic methods through the courtesy of Mr. Thomas A. Johnson of AIAG Metals, Inc.* Three dilute copper alloys with this aluminum were prepared also by methods described previously.' The alloys contained nominally 4, 40, and 400 at. ppm of Cu, respectively (0.001, 0.01, and 0.1 wt pct). Each material was fabricated by swaging and rolling into a round bar about 1/4 in. in diameter with an annealed penultimate grain size of approximately 0.003 to 0.007 cm. In order to minimize preferred orientation the fabrication was carried out in several steps, each consisting of a reduction of about 40 pct followed by a recrystallization anneal. Annealing temperatures for the grain-growth studies were attained by the use of boiling liquids up to 213°C and molten metal baths at higher temperatures. Temperatures were controlled to within 1°C. Samples for measurements were cylinders about 3/4 in. long and 1/4 in. in diameter cut from the fabricated rods. In the interests of sample economy a single sample was used for the grain-growth measurements at each temperature. Each sample was, thus, annealed for several successive periods of time, the grain size being measured at each annealing period on a transverse surface exposed by

Jan 1, 1965

By L. D. Jaffe, R. K. Pitler

IT would clearly be advantageous to produce molten titanium, suitable for alloying and casting, directly from the relatively inexpensive tetra-chloride, without using a metallic reducing agent. Accordingly, a preliminary investigation has been made of the production of titanium by hydrogen reduction of the tetrachloride in an electric arc furnace. For the reaction: TiCl4(g) + 2H2(g) ? Ti(s) + 4HCl(g), Lockhart and his colleagues' have calculated equilibrium constants at 800" to 1500°K, based on tables of Brewer.' Extrapolating these data on the assumption that the heat of reaction varies linearly with temperature, and using Brewer's value for the heat of fusion, there is obtained for the reaction: TiCl4(g) + 2H2(g) ? Ti(l) + 4HCl(g) an equilibrium constant at 2100°K (100" above the melting point) Kp = (PHCl)4/pTlcl4 (Ph2)2 = 0.167 atm. If this is correct, starting with hydrogen saturated with TiC14 at 25°C, where the vapor pressure of the latter3 is 12.6 mm, and maintaining the overall pressure at 1 atm, 99 1/4 pct of the TiC14 would be reduced to Ti at equilibrium. An arc furnace designed for the melting of titanium and lined with water-cooled copper was used for the preliminary experimental check. Its inside diameter was 2 7/16 in. and height 6 in. The water-cooled electrode was tipped with 3/4 in. diam tung-sten. In the one run carried out, the furnace was charged with a starting batch of 293.35 g of scrap titanium,' analyzing 99.24 pct Ti. After the system was twice pumped out and flushed with argon to remove air, the arc was struck in argon and kept at 400 amp dc, electrode negative, for 1 min to melt the starting batch. Commercial tank hydrogen, dried by passing over silica gel and bubbled through technical grade TiC14 at room temperature, was then admitted to the furnace. The inlet tube directed this gas downward toward the arc and melt; the gas outlet was at the top of the furnace. The quantity of gas passed through was not measured accurately but is estimated to be about 50 liters per min at a few mm of mercury above atmospheric pressure. The arc was held in the H2-TiC14 mixture at 400 amp with little difficulty. After 10 min the arc burned through the copper lining above the melt, admitting water and ending the run. (This had happened frequently in straight melting runs under argon, and is not thought due to the atmosphere used.) In the furnace were found an ingot, several small pieces, and a little metallic powder, evidently formed when water entered the hot furnace. Some titanium also clung to the electrode. The portions were weighed and separately analyzed for titanium. Their total weight was 321.76 g of 94.82 pct overall purity. Much of the impurity consisted of tungsten broken off when the titanium was removed from the electrode. No detailed impurity analysis was made because the starting materials were impure and flooding the furnace introduced further contamination. Thus, the metal recovered contained 305.08 g Ti, as compared to 291.12 g in the starting batch. Titanium could not have been carried over from previous melting runs in the furnace, as the interior was sandblasted and the electrode ground clean before the run. Evidently at least 13.96 g of Ti were produced from TiCl4. Since this would require complete reduction of 430 liters of TiCl, gas at 12.6 mm of Hg, the efficiency of the process must have been rather high. Experimental work is continuing. No reason is seen why the process could not be scaled up to the size of a 30-ton steel-melting arc furnace. In a large unit there would be a large molten pool from which liquid metal could be withdrawn for alloying and casting. The problems of electrodes and power supply are similar to those arising in arc furnaces for melting titanium. Unreacted TiC14 and the HC1 in the exhaust gases could be recovered; unreacted H2 could be dried and re-used. The melt would be saturated with hydrogen, whose solubility in liquid titanium is unknown. Small amounts of hydrogen seem to have little effect on the properties of titanium.5 If the amount introduced was so large as to impair properties or cause casting difficulties, it could be reduced by holding the melt under an inert gas or by pumping on it, prior to casting. Acknowledgment The authors would like to thank I. Preble and M. Goldman for their valuable aid in the experimental work and the thermodynamic calculations, respectively. References 1R. J. Lockhart, J. J. Ward, M. J. Hussey, and J. W. Clegg: In unpublished report, "U. S. Air Force Project Rand. Titanium and Titanium Base Alloys." Battelle Memorial Institute (1949) 37-44. 2 L. Brewer et al: Chemistry and Metallurgy of Miscellaneous Materials—Thermodynamics. Ed. by L. L. Quill. pp 13-39, 60-192. (1950). McGraw-Hill Book Co. 3 K. Arii: Scientific Reports. Tohoku Imp. Univ. (1933) 22, 182. 4 R. S. Dean, J. R. Long, F. S. Wartman, and E. L. Anderson: Transactions AIME (1946) 166, 369-381; Metals Technology (Feb. 1946) TP 1961E. * R. I. Jaffee and I. E. Campbell: Transactions AIME (1949) 185, 646-654; Journal of Metals (Sept. 1949) TP 26813.

Jan 1, 1951

By L. N. Brown

The use of sheet and strip metal has increascd rapidly during the last few years and manufacturers have been called upon for an ever-increasing tonnage, better drawing quality, and better surface. The automobile industry is probably the most insistent in striving for a better product and a desire to reduce costs. Confronted by these demands, the mills have directed their efforts toward the delivery of material. Their personnel has been occupied largely with the problems incident to production, as any increase forced the use of new sources of raw material with their problems. These problems, combined with those met in the daily routine, have demanded immediate attention, with the result that the standardizing of heat treatments, quality, or temper, etc., have been neglected. Considerable work in standardizing has been done by many companies, but no acceptable method has been developed. The following method, therefore, is given with the hope that some method that can be accepted by the manufacturers and users may be developed. The problem of selecting a material with such properties that the losses in processing are a minimum is interesting and difficult. A description of the properties required is likewise difficult, largely because of loose terms. Another handicap is the number of methods of testing which have not been standardized and concerning which little information is available. In the selection of drawing or forming stock, it is advisable to eliminate as many variables as possible; consequently the method of testing the material is of the utmost importance. The method should be rapid and comparatively easy of application, as it is more important that a large percentage of the stock be tested with reasonable accuracy than that

Jan 1, 1923

By William D. Klopp

A study was conducted of the tensile and creep properties of are-melted and electron-beam-melted tungsten over the temperature range 2250° to 4140°F. The tensile and creep strengths vary with pain size, the finer -grained materials being stronger. The activation energy for transient creep at 2250° to 3500°F is 95,000 cal per (g)(mole), while that for steady creep at 3300o to 4000°F is 141,000 cal per (g)(mole). At 2875o to 3300°F the apparent activation energy for steady creep decreased with decreasing temperature. It is suggested that cross slip is rate controlling during transient creep, while dislocation climb is rate controlling during steady creep above 3300° F. ALTHOUGH considerable data have been generated on the high-temperature tensile properties of powder-metallurgy tungsten,1 relative few data have been published on the properties of are-melted2 or electron-beam melted tungsten.3 Furthermore, the available data show a fairly large amount of scatter at high temperatures. The effects of structure and purity have not yet been defined, aside from observations that high-purity electron-beam (EB)-melted tungsten3 and single-crystal-plasma-flame tungsten4 are weaker than less pure powder-metallurgy tungsten. The creep behavior of powder-metallurgy tungsten has been studied, but no data are available on the creep behavior of tungsten consolidated by melting. Green5 found that powder-metallurgy tungsten exhibited linear creep at 4082° to 5072°F with an activation energy of 160,000 cal per (g) (mole). The similarity of this activation energy to that of 153,000 cal per (g)(mole) for volume self-diffusion6 suggests that recovery of strain hardening by dislocation climb is rate controlling in this temperature range. In studies at 4800°F, Sutherland and Klopp7 concluded that grain size significantly affected the creep behavior of commercial powder-metallurgy materials. This grain-size effect was suggested by sherby,8 although the opposite relation had been reported for aluminum.' The purpose of the present study was twofold: first, to provide baseline data on high-temperature tensile and creep properties of are-melted and EB-melted tungsten for concurrent tungsten alloy studies, and, second, to determine the phenomenolo-gical effects of structural and purity variables on the high - temperature mechanical properties of tungsten. EXPERIMENTAL The are-melted tungsten materials were prepared by melting sintered 1-1/4-in.-diam electrodes into 2-1/2-in.-diam by 5-in.-long ingots. The are-melting facility has been described previously.' Eight ingots were melted, machined, and hot-extruded at

Jan 1, 1965

By L. N. Brown

The use of sheet and strip metal has increascd rapidly during the last few years and manufacturers have been called upon for an ever-increasing tonnage, better drawing quality, and better surface. The automobile industry is probably the most insistent in striving for a better product and a desire to reduce costs. Confronted by these demands, the mills have directed their efforts toward the delivery of material. Their personnel has been occupied largely with the problems incident to production, as any increase forced the use of new sources of raw material with their problems. These problems, combined with those met in the daily routine, have demanded immediate attention, with the result that the standardizing of heat treatments, quality, or temper, etc., have been neglected. Considerable work in standardizing has been done by many companies, but no acceptable method has been developed. The following method, therefore, is given with the hope that some method that can be accepted by the manufacturers and users may be developed. The problem of selecting a material with such properties that the losses in processing are a minimum is interesting and difficult. A description of the properties required is likewise difficult, largely because of loose terms. Another handicap is the number of methods of testing which have not been standardized and concerning which little information is available. In the selection of drawing or forming stock, it is advisable to eliminate as many variables as possible; consequently the method of testing the material is of the utmost importance. The method should be rapid and comparatively easy of application, as it is more important that a large percentage of the stock be tested with reasonable accuracy than that

Jan 1, 1923

By Milton E. Wadsworth, R. Ted Wimber

Cobalt sulfate solutions containing ammonium acetate and chloroplatinic acid were reduced by hydrogen in a pyrex-glass lined autoclave in the temperature range of 170o to 232°C and hydrogen partial pressure range of 115 to 830 psia. The reduction rate was directly proportional to the hydrogen partial pressure and surface area of the pyrex glass and was independent of the quantity of chloroplatinic acid added initially. Experiments involving the variation of the relative concentration of ammonium acetate indicated that the reducible cobalt complex was probably the diacetate complex of cobalt, Co(AC)4H20, or a new mononcetate complex Co Ac, which was in solubility equilibrium with a pink precipitate of CO(AC)-4HzO. THE reaction in which a metal is dissolved by an acid to produce gaseous hydrogen and a salt solution was discovered early in the history of chemistry. In 1859 Beketoff found experimentally that this reaction could be reversed; i.e., a salt solution could be reduced by gaseous hydrogen to produce a metal and an acid. A review of work done on this phenomenon since that time may be found elsewhere., The hydrogen reduction of a cobalt salt solution is facilitated by complexing the cobalt ion. An ammonia complex of cobalt has been reduced commercially in the recovery of cobalt metal. A new reducible complex of cobalt was discovered5 when it was found that a co-baltous sulfate solution containing ammonium acetate could be reduced by hydrogen at temperatures in the region of 200°C. When a cobalt sulfate-ammonium acetate solution was heated to a temperature below its normal boiling point, a violet color became apparent, indicating complex formation. The nature of this complex was investigated5 by the addition of NH4Ac to a CoSO4 solution maintained at 85o. During the first additions of NH, Ac, the pH of the solution remained fairly constant at about 5.85. However, as the ratio of NH,Ac to CoSO, approached two, the pH rose and then leveled off at about 6.05. The absorption spectra of a Co(Ac), solution and a CoSO,, NH Ac solution were obtained at 85°C and were compared and found to be the same. These findings suggested that the diacetate complex of cobalt, Co(Ac),.4H20, was formed at 85°C. When a cobalt sulfate-ammonium acetate solution was heated to a temperature above about 165o, a finely divided pink precipitate appeared. The X-ray diffraction pattern of this precipitate indicated that it was Co(Ac), - 4H,O. In addition, it was discovered that when chloroplatinic acid, H,PtCl;, was added initially to the cobalt sulfate-ammonium acetate solution, a faster reduction was obtained. The roles of the solution complex, pink precipitate and chloroplatinic acid in the reduction process were then investigated. APPARATUS The experimental work was carried out in a two-liter stainless-steel autoclave. Adetailed description of the autoclave and the auxiliary equipment used in maintaining constant temperature and pressure may be found elsewhere.= Because the stainless steel was corroded, and also because it acted as a hydrogena-tion catalyst, an all-glass liner was fabricated such that the solution came only into contact with flame-polished pyrex glass. EXPERIMENTAL PROCEDURE The solutions used in the experimental work were prepared by dissolving reagent grade chemicals in distilled water. Although variation of the brand of ammonium acetate appeared to have no effect on the experimental results, CoSO, 7H O from the J. T. Baker Chemical Co. of Phillipsburg, N. J.,was found to give faster reductions than that prepared by Allied Chemical and Dye Corp., N. Y. The former was used throughout the course of the experimental work and was weighed up at the outset of each experiment. The ammonium acetate was dissolved to form a 6M stock solution, which was stored under refrigeration. A 10 pct solution of chloroplatinic acid (J. T. Baker Chemical Co.) was diluted to a 1.15 x 1Q2 M stock solution, which was standardized by precipitation of K,PtCl, as outlined by Scott. The appropriate volume of the chloroplatinic acid, H,PtCl,, solution was pipetted into the clean, dry glass liner. The cobalt sulfate-ammonium acetate solution, which had previously been saturated with

Jan 1, 1962

By J. J. Thomas, J. H. Nead

This investigation was undertaken to determine, if possible, the relation between static and dynamic tensile tests as measured by the work required to break test specimens slowly, in a tensile testing machine, and rapidly, by means of a falling weight. It was hoped that the investigation would throw some light on the role played by ductility under different rates of application of load. In problems of design, it is usually assumed that the moduli of elasticity of all steels are equal; viz., about 30,000,000. The stress-strain diagram within the elastic limit is a straight line, as shown in Fig. 1, where OA is the curve of a hard steel and OB that of a soft steel. If the modulus of elasticity is constant, as assumed, the slope of the line OC

Jan 1, 1922