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Reports on process control computer projects at the Kamioka Plant are summarized from the Japanese technical literature (see references). Fluidized Bed Roaster and Sulfuric Acid plant1 A small process control computer (Yokogawa CCS-200 with an OKITAC 5090P 8K central processor) was installed in the Kamioka smelter in the summer of 1964. A year-and-one-half installation project followed, which successfully brought the roaster and acid converters under computer control. The process plant consisted of two 130 RPD fluosolids roasters and two Monsan to acid units. The roasters are charged with lead-zinc concentrates with SO2 from the roaster processed to sulfuric acid. The computer system provides the following functions: 1) log data from the plant--the input is taken from 50 analog signals, 130 high-low digital alarm points, and 50 analog high- low alarm points; 2) set-point control on 18 control loops; 3) direct digital control (DDC) on eight control loops for which conventional controllers were difficult to adapt due to abnormal loop characteristics or delay times; 4) execution of a safe shut-down procedure

Jan 1, 1969

By Richard Akerman, Frederick Prime Jr

[THE attention now being paid both in this country and Europe the greatest economy in the working of the blast furnace, and the eagerness with which all thoughtful men in the iron business look for any new information which will tend to throw light on this subject, is a quite sufficient excuse for presenting this paper to the American Institute of Mining Engineers.] I. It must be borne in mind that when two bodies unite to form a chemical compound, heat is almost always evolved. In order to

By Richard Akerman

(Translated by FREDERICK PRIME, JR., Professor of Metallurgy in Lafayette College, Easton, Pa.) [THE attention now being paid both in this country and Europe to the greatest economy in the working of the blast furnace, and the eagerness with which all thoughtful men in the iron business look for any new information which will tend to throw light on this sub¬ject, is a quite sufficient excuse for presenting this paper to the Amer¬ican Institute of Mining Engineers.] I. It must be borne in mind that when two bodies unite to form a chemical compound, heat is almost always evolved. In order to

Jan 1, 1873

By Morris M. Fine, Norwood B. Melcher

It is out of the question, at this time, to select any one prereduction process as superior to the others. It is apparent that several share a basic similarity and that within the groups listed in Part 1, the reduction vessel is sometimes the only significant variable. Claims as to the virtues of one machine over another are difficult to substantiate: one may be rapid, another thermally frugal. Based on published data, however, all seem to be performing adequately. It would appear that processes based on carbonized pellets are most applicable to foundry iron at low production rates. Adaptation to large scale manufacture of blast furnace hot metal or to agglomeration of fine concentrates at the mine site is much less likely.

Jan 8, 1966

By G. M. Yocom

Blowing acid Bessemer converters with oxygen-steam produces steel of below 0.002 pct N2 content. This method of blowing, combined with a dephosphorizing treatment in the steel ladle, results in low-carbon steels of low nitrogen and low phosphorous (under 0.035 pet) contents, which has physical properties equivalent to open-hearth steels of similar analysis. Using a 50-50 mixture of oxygen and steam, the refinitzg rate is increased 25 pct over blowing with natural air, and scrap charge increased from 3 to 10 pet. Bottom life is normal with proper tuyere area and arrangements, fumes are decreased, yields increased, and hydrogen content is normal. THE acid Bessemer plant at the South Works of Wheeling Steel Corp., consists of two 15-ton bottom blown converters with a monthly capacity of 57,000 N.T. The product of the shop is skelp billets for continuous welded pipe and slabs for ordinary drawing and forming quality sheets. Approximately 50 pct of ingot production is regular Bessemer steel of natural Phos content and the remainder is a dephosphorized grade of steel made by a special treatment of the blown metal as it is poured into the steel ladle. The low Phos grade of steel has certain advantages over the higher Phos grade but since both grades were produced by blowing natural air, the N2 content was in the range of 0.015 pct which limited its application. In 1954 it was decided to explore the possibilities of blowing with a steam-oxygen mixture for the production of steel of both low N2 and low Phos contents. The necessary equipment was installed to operate one converter in this manner and early in 1955 an experimental run of 160 heats was made by blowing with a steam-oxygen blast and excluding natural air entirely. During this period the proper operating techniques were established, such as blast pressures, steam-oxygen mixtures, valves and instrumental control equipment, tuyere arrangement in the bottoms, blowing times and production rates, and a thorough study made of the final steel quality. Also during this experimental period the dephosphorizing practice was improved by the use of a tap hole below the lip of the vessel. This provided a clean separation of the acid converter slag and blown metal which made the dephosphorizing treatment more effective. The results of this experimental run dictated further development of this practice and a second run of 720 heats was made in 1957. The quality features and conversion cost results were in line with expectations and accordingly a 400-ton per day oxygen plant is now being installed. The plant is scheduled for completion in September of this year. This will provide sufficient oxygen to operate both vessels on steam-oxygen blast and delete natural air blowing entirely. The steel will then be below 0.002 pct N2 bar content and the dephosphorized grades will be between 0.015 and 0.040 pct Phos. STEAM-OXYGEN BLOWING The steam for the process is fed to the plant at 220 psig pressure through a 6-in. line. The high-purity oxygen is compressed to 200 psig and conducted through an 8-in. line. The oxygen from the main line is valved down to 100 psig and passed through a steam heated heat exchanger. The heat exchanger is regulated to supply oxygen at 300°F to the steam-oxygen mixing station. It is essential that the incoming oxygen be held at this temperature to avoid condensation of the steam with resulting excessive erosion of the clay tuyeres in the vessel bottom. Oxygen is admitted to the mixing chamber by a 6-in. hydraulically operated valve driven by the ratio control regulator on impulse from the flow of steam. Steam is admitted to the steam-oxygen mixture station through a 2 1/2-in. hydraulically driven valve. The ratio control regulator acts to increase or decrease oxygen input as the steam flow increases or decreases with changing positions of the Blower's control lever. The important point to note here is that steam flow always precedes the oxygen flow as a safety measure. The control valves have sufficient capacity to afford protection should blow pipe trouble develop. A 50-50 mixture for these 15-ton heats demands an oxygen flow of 3800 standard cu ft per min along with 317 lb of steam. The Blower's stations is provided with an indicating blast pressure gage, and indicating steam and oxygen flow meters. Signal and warning lights indicate the valve positions and line pressures. A control room at the real of the Blower's pulpit room houses the ratio control and pressure regulators, as well as the various meter bodies. The hand actuated wheels used to change the conditions are mounted on a panel on the front of the meter control house. The recording steam and oxygen meters used for totalizing and accounting purposes are also mounted on this panel.

Jan 1, 1962

By A. W. Hahn

USE of gold leaf goes back to biblical and even to prehistoric times. Both gold and silver, as well as other metals, were employed in illustrating or illuminating manuscripts. The medieval monks also used bronze powders. Metals were subdivided as finely as possible by mechanical methods, or by granulation and then were pounded into finely divided flakes. Substances such as honey have also been employed, since early times to keep the flakes of metal apart during grinding. Stearic acid is a more modern agent used in flaking aluminum and other metals. Finely divided "blue powder" is a by-product in retorting zinc ores, and contains from 78 to 90 per cent of zinc metal. This has been used as a precipitant for precious metals in the cyanide process and for chemical reduction processes. The making of zinc dust by atomizing is a step well known in electrolytic zinc plants. The Thermit process of Goldschmidt also requires the use of finely divided aluminum.

Jan 1, 1937

By Henry G. Morris

The use of compressed air for the transmission of power has reached so great a development that we find numerous large establishments devoted to the manufacture of machinery for its production and application, and special periodicals published for the dissemination of information on the subject. Moreover, its employment is so general in mining operations that no apology is needed for the presentation to the Institute of such a paper as the present. The admirable articles of Mr. E. A. Rix, published in Conzpressed Air, show a wide range in the mechanical efficiency of air-compressors, varying, under different conditions, from 15 to 60 per cent.; and it is evident that any

Jan 1, 1902

By C. E. Lesher

Low-TEMPERATURE carbonization needs no introduction to the literature on coal. This paper will attempt no review of that literature; it tells the story of the commercial development of one of the processes for carbonizing coal at so-called low temperatures, dealing with the technology and economics of the process rather than with the design of equipment. The process used is that covered by the patents of C. B. Wisner, with improvements and changes made by the Pittsburgh Coal Carbonization Co. The important and novel feature of the process is the phenomenon of making the product in ball form (Fig. 1). Melting coal dust into smokeless solid fuel in an apparatus as simple as a revolving cylinder of ordinary mild steel has been proved to be practical. Furthermore, it has been found that the process has a wide application, for by applying a knowledge of why and how this balling action is accomplished, the apparatus can be designed and adapted to treat any coal that has a certain minimum agglutinating property. The operating plant is 20 miles west of Pittsburgh, adjacent to the Champion preparation plant of the Pittsburgh Coal Co. The coal used is cleaned minus 3/8 -in- or finer sizes. The products are low-tem-perature coke, tar and tar products. Present capacity is 7000 tons per month of low-temperature coke and 140,000 gal, of tar. There is no surplus gas for sale, and none of the light oils are stripped from the gas. The coke is marketed in two sizes, 1 to 2 in. and 1 to 6 in., through retail coal dealers for domestic con-sumption in hand-fired furnaces, and for fireplace fuel. The smaller size is bagged by dealers. Crude tar and many distillates and road tars are sold.

Jan 1, 1940

By R. J. Cowan

IN the art of cementation a controversy has been going on for years as to whether solid or gaseous carbon is the active agent in carburizing steel. More recently opinion has crystallized into a compromise to the effect that carburizing is a gaseous cementation of steel in the presence of solid carbon. The importance of this theory has a particular bearing upon the work to be described. In the art of carburizing, use is commonly made of such words as "catalytic," "atomic," "nascent" and "activated;" in an attempt to describe the process. These words are used indiscriminately. For, instance, the gas is said to be "catalytic" and carbon to be "nascent," or vice versa. In using these expressions, investigators are confirming the acceptance in their minds of the active conditions of both gas and carbon in the cementation process.

Jan 1, 1931

By J. B. Clemmer, W. L. Lennemann, J. B. Rosenbaum

Security restrictions on processing uranium raw materials to yellow cake were lifted in August 1955, coincidental with the Geneva Conference on Peaceful Uses of Atomic Energy. Numerous reports and technical papers on uranium extraction and recovery methods have appeared since that time, and it is doubtful that another review of past and current practices would add much to the technical literature. Development of some promising procedures was arrested, perhaps temporarily, by mechanical handling problems or peculiarities in the chemistry of uranium and associated elements. Some methods have been incompletely evaluated and still others that tested well in the laboratory and pilot plant are dormant because of competition from other processes, or because of their restricted applicability to particular ore types that have not reached quantity production. In view of the vast number of new ideas and procedures that have been advanced, considered, and tested, it would be futile to attempt a comprehensive survey in this article. Only a cross section of the field, based on random sampling, can be provided here. The authors have chosen, therefore, to discuss some innovations that may provide a clue to uranium ore processing techniques of the future. An effort has been made to select unpublicized new metallurgical techniques or interesting applications of established principles and procedures. With the two exceptions noted later, all the research to be described has been sponsored by the AEC. Physical Beneficiation: Individuals and firms engaged in mining and processing uranium ores, and in related research activities, have often had considerable experience in ore dressing. As might be expected, therefore, a prodigious amount of work has been done on physical beneficiation testing of uranium ores, particularly in efforts to concentrate subgrade materials. Although some success has been attained on specific ores by gravity concentration and flotation, ratios of concentration have generally been low and there has been difficulty in making a throwaway tailing.

Jan 9, 1957

By Joseph Daniels

(San Francisco Meeting, October, 1911.) I. THE FRITZ ENGINEERING LABORATORY. TEE Fritz Engineering Laboratory was built under the direction of John Fritz, and presented by him to the University. A view of the building, looking east, is shown in Fig. 1. . The building was started in 1909, and completed in 1910, although all of the equipment was not placed until later. Mr. Fritz gave his personal attention to the details of construction and equipment, and it was his custom to drive over every day to the University from his home in Bethlehem, and spend some hours watching the work, offering suggestions, making changes, and planning new work. The result is a building and an equipment which embody his practical ideas. The laboratory structure is of the steel mill-building type, of light-colored brick, 91 by 114 ft., of which a section is shown in Fig. 2 and the floor-plan in Fig. 3. The steel frame carries the roof and traveling crane-way. Ample light has been provided by numerous windows in the side and end walls, in the clerestory, and by a skylight, 84 ft. long and 9 ft. wide, in the north roof. The main aisle of the building is 49 ft. 2 in. between centers of crane-columns, and has a clear height of 40 ft. The remainder of the width is taken up by two side aisles, 18 ft. high. The laboratory consists of four sections: (1) A general testing-section, containing the testing-machinery, a small machine shop, and an office; (2) a cement-testing room; (3) a room for making and storing concrete test-specimens; (4) a hydraulic section.

Feb 1, 1912

By Edward Keller

THE present ruling principle in shop and factory, induced by conditions of. keen competition, is to do the greatest amount of work in the shortest time, or in other words, to secure the greatest output at least cost, a condition which generally necessitated the substitution of machinery for manual labor. The chemical laboratory in our industrial establishments has remained a factor of minor importance, and, for this, reason, not only has progress been permitted to lag, but the methods of analytical work have been carried on along individual traditional lines. Some works-laboratories are equipped with such conveniences as Gooch filters, suction-pumps, compressed air, shaking-machines, centrifugal machines, crushers, etc., yet there is much room for improvement, particularly in laboratories of metal smelting and refining plants, in which long series of filtrations and stirrings are performed singly by hand in a slow and laborious manner. There are also many other instances in which collective handling appears rational. As a rule the chemist wastes much time by such manual labor, which, in a modern establishment and under up-to-date management, could be more advantageously applied to useful chemical work; and such higher chemical work is gradually and surely becoming recognized as an essential extension of old-time methods of assaying. While it maybe said that in some laboratories, boys and not chemists do the manual labor, it should be borne in mind that all chemical work requires care and accuracy and in these respects boys are naturally a source of concern to the responsible chemist. Moreover, the cheapness of child-labor is largely offset by the increase in the expense-account of laboratory materials, caused chiefly by breakages resulting from care¬lessness. Having; been authorized by the Anaconda Copper Mining

Mar 1, 1905

By E. C. Wright

The following article is based on observation of college graduates entering the steel industry in technical work made during the Past 25 Years, the first five of which were spent as a college instructor in two engineering schools, and the last 20 in the employ of a large steel company that has hired hundreds of engineering graduates for steel-mill operations. The college graduates encountered during this period have come from many colleges representing schools in Eastern States, Midwestern Universities, many Southern colleges, and many smaller colleges and normal training schools mostly in western Pennsylvania and Ohio. The college training of these students for engineering work naturally has varied widely and the educational qualifications of the entrants have been in many ways different. It was found at an early date that graduates of standard engineering colleges were much more adaptable than graduates in science from nontechnical schools. The engineering students seemed to be more suited to actual work in steel plants and in general were better able to grasp a knowledge of the operations they observed. However, although the graduates of engineering schools have had somewhat better training in physics, mathematics, and engineering, it has been a general and continual observation that most of the students employed have had inadequate training in the fundamental sciences. Since this discussion relates entirely to metallurgical engineers it should be emphasized that students taking metallurgical engineering courses in college seem to be poorly trained in organic chemistry-physics, physical chemistry, thermodynamics, and any higher form of mathematics than simple calculus. It has been noted frequently that young engineers faced with problems in a mill that involve some mathematics generally flounder badly, and that they have little conception of physical chemistry. Another common deficiency lies in the young graduate's lack of knowledge of where to look for the more detailed literature on any subject. He reverts instinctively to some college textbook whose coverage is usually very elementary. It is recommended that such textbooks contain a bibliography of the source literature. and that students be taught to use the original data. Many of the students had had previous courses in college dealing with metallurgical work such as steel melting, metallograhy, etc.r but it was found that their grasp of these subjects was extremely sketchy. It was soon realized that an ordinary engineering graduate could be taught more about steel melting and manufacturing processes in a few weeks in a plant than he could learn in a college course on such subjects. A similar statement may be made regarding the ability of students to conduct laboratory work. Their lack of technique and skill in handling equipment and setting up experiments was soon apparent. It became neces-

Jan 1, 1948

By E. C. Wright

The following article is based on observation of college graduates entering the steel industry in technical work made during the Past 25 Years, the first five of which were spent as a college instructor in two engineering schools, and the last 20 in the employ of a large steel company that has hired hundreds of engineering graduates for steel-mill operations. The college graduates encountered during this period have come from many colleges representing schools in Eastern States, Midwestern Universities, many Southern colleges, and many smaller colleges and normal training schools mostly in western Pennsylvania and Ohio. The college training of these students for engineering work naturally has varied widely and the educational qualifications of the entrants have been in many ways different. It was found at an early date that graduates of standard engineering colleges were much more adaptable than graduates in science from nontechnical schools. The engineering students seemed to be more suited to actual work in steel plants and in general were better able to grasp a knowledge of the operations they observed. However, although the graduates of engineering schools have had somewhat better training in physics, mathematics, and engineering, it has been a general and continual observation that most of the students employed have had inadequate training in the fundamental sciences. Since this discussion relates entirely to metallurgical engineers it should be emphasized that students taking metallurgical engineering courses in college seem to be poorly trained in organic chemistry-physics, physical chemistry, thermodynamics, and any higher form of mathematics than simple calculus. It has been noted frequently that young engineers faced with problems in a mill that involve some mathematics generally flounder badly, and that they have little conception of physical chemistry. Another common deficiency lies in the young graduate's lack of knowledge of where to look for the more detailed literature on any subject. He reverts instinctively to some college textbook whose coverage is usually very elementary. It is recommended that such textbooks contain a bibliography of the source literature. and that students be taught to use the original data. Many of the students had had previous courses in college dealing with metallurgical work such as steel melting, metallograhy, etc.r but it was found that their grasp of these subjects was extremely sketchy. It was soon realized that an ordinary engineering graduate could be taught more about steel melting and manufacturing processes in a few weeks in a plant than he could learn in a college course on such subjects. A similar statement may be made regarding the ability of students to conduct laboratory work. Their lack of technique and skill in handling equipment and setting up experiments was soon apparent. It became neces-

Jan 1, 1948

During the war, American chemists were puzzled as to the scource of the enormous amount of sulfuric acid the Germans were able to secure. Information now in the hands of the Bureau of Mines shows. that at no time during the war was there any particular stringency in Germany's supply of this acid. During the early months of the war, before conventions could be made with neutral countries, very large shipments of pyrites were made to Germany; in fact, the importation of pyrites into Germany continued in some volume throughout the war. This reserve built up at the beginning of the war gave Germany time to find new resources of sulfuric acid. A noteworthy development of the Meggen pyrites took place and other pyrite beds were opened in Germany and Hungary. Considerable sulfur was also obtained from Asia Minor. In addition, Germany made important use of its rich beds of blende and galena. Means was found promptly to eliminate the lead dust, which has been a source of trouble in the contact process of manufacture. Kaiserite and plaster of Paris also were sources of sulfuric acid; some sulfur was also obtained by purifying gas at coke plants. As a matter of fact, sulfuric acid was so plentiful in Germany near the close of the war that restrictions on its use by industries were rapidly being lifted.

Jan 6, 1919

By Arthur F. Taggart

Some years ago, A. M. Gaudin and one of the authors published a paper showing removal of tar acids from solution by sulfides preferentially as compared to gangues (specifically by galena as compared to quartz).' The underlying phenomenon was classed as adsorption, and the paper went on to develop the general thesis that so far as water-soluble frothing and collecting agents in flotation are concerned, the phenomenon of adsorption is one of controlling importance. Adsorption was defined in that paper as "a process of rearrangement of a system, which results in establishing a difference in concentration, as between the interfacial layers and the bulk of the phases, of a substance or substances initially uniformly dispersed in one or several of the phases." The paper went on to develop the relation between adsorption and surface cnergy according to Gibbs' equation (which may be thrown into the form U/c = KdT/dc, where U = excess concentration in surface layer, c = concentration, T = surface tension, and K is a constant), and pointed out that, according to this equation, degree of adsorption and change in surface tension vary directly. The present paper offers a somewhat different definition for the term adsorption; and sets up, in sweeping terms, the generalization that simple chemical reaction underlies the functioning of the flotation reagents which control mineral collection, when these reagents are soluble in and act from solution in the water of the pulp. Adsorption According to the modified definition, adsorption means concentration at an interface between different phases in a heterogeneous system (thus far the definition runs as before), by the action of some mechanism, of which nothing is properly implied in the word, and concerning which the user of the word is probably in entire ignorance. Thus defined,

Jan 1, 1930

By M. F. COOLBAUGH

WHEN I was asked to speak on the subject of leaching, I did not realize that a complete summary of recent progress in leaching had been given by Stuart Croasdale. I shall try to give some other phases of the subject that were not touched by Mr. Croasdale. Not all metallurgists are in harmony as to their methods of treating metals. If they were it would probably mean lack of progress. They can be divided into two classes-the pyrometallurgists, using fire means, and the hydrometallurgists, or those using leaching methods. Conflict is always good for progress; we have it in politics, and in religion there are fundamentalists, and those who are not fundamentalists. As representing pyrometallurgy, may I hope not to be classed among the fundamentalists. The leaching of ores is not new. The leaching of ores for the recovery of metals, however, is quite new. The older leaching was simply to recover the salts. Agricola, back in 1555, I think it was, outlined a great many methods of leaching for the recovery of salts. They called them solid juices at that time. There was no real competition, however, between leaching meth-

Jan 1, 1926

By S. B. Christy

The practice of the cyanide-process of gold-extraction has brought to light many important contradictions of familiar chemical analogies, which still obscure both the theory and the practice of the art with distinctions subtler and more difficult to make or follow than those which delighted the heart of the old-time metaphysician. Yet Nature herself has drawn these distinctions; and if we hope to succeed in this modern search for the Golden Fleece, we must be able to follow her through the winding labyrinth. There are so many phases of this question that I shall attempt to touch on only one of them at this time, but it is one that lies at the root of many others. In reviewing my paper on " The Solution and Precipitation of Cyanide of Gold,"* Mr. E. B. Wilson contends† that" in the solution of gold by means of alkaline cyanides the various reactions are determined, as to their order and intensity, by the relative position of the elements concerned in the electro-chemical series, or series of voltaic tension." In a modified form this statement is probably true. That is to say, the difference of electrical potential in any closed electrical circuit determines the nature of the reactions which ensue. But the matter is not so simple as Mr. Wilson assumes. Recent investigations show that the order of the metals in the electro-chemical series depends not only on the nature of the elements themselves, but also on the chemical composition of the solution in which they are placed; its degree of concentration; its temperature; and, in the case of gases, on the pressure. Unless all these conditions are taken into account, inferences drawn from the electro-chemical series are likely to prove more

Jan 1, 1901

By R. Bakish, M. A. Badiali, N. W. Kirshenbaum

One pound of ultra pul-e molybdenum has been produced containing both metallic and nonmetallic impuvities close to or less than the limits of detection. various purification methods were investigated; althouglz the use of move than one purification step was consideved, it was found that a single, caefully-controlled sublimation of MoCl5 yielded a highly puvified product without prior treatment or recourse to repeated sublimation. Hydrogen reduction of MoC1, to metal was attempted at atmospheric pressure; however, reduced pressure was necessary to obtain substantial yields. The tubular deposits of metal were consolidated into bulk fovm by electron beam melting undev high vacuum yielding a very low gas content. Boblems involved in monitoring the puvity of these materials and analytical results obtained are also presented. THE pronounced effect of even trace amounts of impurities upon fundamental properties of materials is well known to metallurgists and solid-state physicists. Consequently, groups interested in basic studies of metals have in recent years immensely stimulated the preparation and production of numerous ultra-pure metals. Increased demand by scientists for these high purity materials has necessitated development of facilities to prepare them in significant quantities; the procedures reported here were devised to produce significant quantities of ultra-pure molybdenum. Previous work performed in the field of vapor phase purification and hydrogen reduction of several other refractory metal chlorides had demonstrated valuable techniques applicable to molybdenum.' Various purification and reduction steps were individually investigated. Those procedures which showed the most favorable results with respect both to attainment of high purity and to ease of operation were then incorporated in the process utilized to produce the metal.' STARTING MATERIALS It is well known that because of differences in volatility, chlorides may be separated by fractional distillation. It was presumed that distillation of molybdenum pentachloride offered a simple and straightforward method of purification due to its relatively low boiling point. Alternatively, sublimation of the solid chloride also appeared feasible since MoC15 has both a reasonably narrow temperature range in which it exists as a liquid (a property typical of refractory metal chlorides) and a low enthalpy of sublimation. Pertinent thermochemical data of MoC15 are given in Table I. It should be noted that this compound must be handled with care as it is extremely hygroscopic. Anhydrous MoC15 was obtained from the A Metal Climax Co. METHODS OF PURIFYING MOLYBDENUM PENTACHLORIDE Distillation. It was expected that distillation methods, while affording an efficient purification, would prove simple to control and would have a higher production rate than sublimation processes. Also considered was the possibility of effecting a high degree of purification by using both these volatilization methods in conjunction—possibly a distillation followed by sublimation of the solidified condensate. Distillation of MoC15 was investigated using a single stage distillation column packed with chemically resistant glass beads. Heating coils were wound around the column and collection tube (condenser). As-received MoCl5 was charged into a flask connected with the column using a side loading arm under an argon flow. After the column and condenser were brought to about 270" and 210°C, respectively, the apparatus was lowered until the flask was fully immersed in a constant temperature fused salt bath maintained at about 285 °C. Distillation was continued for about 10 or 15 min until 50 to 70 g of distillate had been collected. Analyses of these distillations indicated that several elements, e.g., Cu, Fe, Ni, Cr, and Mg, were lowered in quantity although not all were removed to the same extent. The occurrence of Na, B, Si, and A1 in the distillates appeared to be due to contamination, possibly from corrosion of the pyrex glass. An improved distillation system of larger capacity and longer distilling column was built. Improvements were effected in lowering the amounts of such impurities as B, Mn, Ni, Na, Mg, Cr, Cu, and Fe. These studies were pursued concomitantly with efforts to purify by sublimation; it was subsequently found that although improvements in purity were obtained by distillation, sublimation processes were simpler to control and effected a high degree of purity.

Jan 1, 1963

By H. Y. Hunsicker

A graphic method has been devised for three-di-mensional analysis of hot deformation and for correlating the amount and directionality of the deformation with resulting directional properties. Deformation is evaluated in terms of dimensional change ratios referred to three orthogonal axes. Since all combinations of the three ratios can be represented in a triangular coordinate field with logarithmic scales, a two-dimensional chart of extent of deformation and degree of asymetry is possible. The entire gamut of shape changes from upsetting through flat-rolling to rod-rolling is accommodated. The resulting coordinate system is a base upon which can be represented the properties of the wrought products measured in the directions of the axes employed fir evaluating the deformation. When property data are available for many types and amounts of deformation, a three-dimensional figure can be constructed, and the projection of this figure is referred to as a ''3d'' chart. Experience in using such charts to plan fabricating operations for a variety of thick-section forged and rolled products of heat-treated aluminum alloys has verified its practical value for optimizing directionality relationships. MechANICAL anisotropy of thick section products of heat-treatable aluminum alloys is recognized by producers and users of these products, and the extent of the directional differences is apparent in property tabulations included in handbooks, standards, and specifications.' Attention has also been directed to the existence of important directional differences in the resistance of these products to stress-corrosion cracking. Metallurgical structure factors responsible for these directional differences include, among other possibilities, shape and alignment of grains, voids and nonmetallic inclusions (when present), volume fraction and spatial distribution of secondary phase particles and solid-state precipitates, crystal-lographic textures, and Bauschinger effect. The contributions of the individual factors vary with alloy composition, heat-treated temper, type of working process (forging, rolling, extrusion), and the amount and directional nature of the deformation. In general, the cast ingot used as the starting material for producing these wrought products exhibits only a modest degree of directionality. A monotonic and continuous transition from this nearly isotropic state with progressive hot deformation would appear probable, assuming that the working temperature is sufficiently high to cause continuous dynamic recovery. Several years ago a project was undertaken to evaluate the effects of hot deformation and metallurgical structures on the directionality of thick wrought aluminum alloy products, and the method to be described was developed as an analytical tool in this investigation. DIRECTION NOMENCLATURE The nomenclature system adopted by industry for the three mutually perpendicular directions employed in testing aluminum alloy products includes four terms: "longitudinal", "transverse", "long transverse", and "short transverse". These terms are conventionally related to the external geometry of the product but also by implication to the deformation and resulting metallurgical structure. Occasions arise in which through use of unusual fabricating methods, intentional or otherwise, the structure does not have the usual relationship to external geometry or may be very complex because of inhomogeneity of deformation throughout the piece. The longitudinal direction is generally parallel to the primary rolling direction or to the direction of extrusion. In the case of forging, it is parallel to the direction of maximum extension (not maximum "working" or "flow", as frequently stated). The term transverse is applied to any direction perpendicular to the longitudinal direction in a product having symmetry about the longitudinal axis, and generally, although not always, the deformation to produce these forms is nearly symmetrical in the transverse plane. This term then may be applied to a round, square, hexagon, or other polygonal, symmetrical shape produced by extrusion or rolling or by forging, if produced by a simple, symmetrical drawing procedure. The type of microstructure generally associated

Jan 1, 1970