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By James Paul

BEGINNING in December, 1933, and continuing to the close of April, 1934, large sums of money were expended in the states of Pennsylvania, Ohio and West Virginia through the conduct of Federal and State Civil Works Administration, financed by the Government as a part of the President's recovery program to furnish employment to mine employees idle as a result of the economic depression. PURPOSE OF THE PROJECT The protection of the public health against the pollution of public water supply by acid mine drainage was the incentive that prompted the request that the sealing of abandoned bituminous coal mines be made a Federal project. A paper before the Central Section of the American Water Works Association, Wheeling, W. Va., on Aug. 24, by E. S. Tisdale, Chief Engineer of the West Virginia Department of Health, tersely says: In October, 1933, the combined experience of the U. S. Bureau of Mines and the U. S. Public Health Service and the States of Pennsylvania, Ohio, West Virginia and Kentucky resulted in a report being filed in Washington, first with the Public Works Administration and later with the Civil Works Administration, where it was favorably acted upon, calling for these governmental agencies under the direction of the U. S. Public Health Service to expend $1,500,000 in a unified effort to seal abandoned coal mines in Pennsylvania, Ohio, West Virginia, Kentucky and six other states farther down along the Ohio river. The report referred to was embodied in a petition that was signed by the chief engineers of the State Departments of Health of the several states contiguous to the drainage area of the Ohio River. The project as established under Federal supervision became interstate with respect to the several states involved, and upon the termination of the Federal project on Feb. 15, it was authorized as a State C.W.A. project, effective Feb. 20, under the supervision of the State Departments of Health and the State C.W.A. Administration, which continued to March 29, and was succeeded by the S.E.R.B. of the R.W.D. from April 2 to April

Jan 1, 1935

By William Greenawalt

The Greenawalt electrolytic copper extraction process is applicable to suitable oxide ores, sulfide ores and concentrates, and low-grade matte. The process is self-sustaining in acid on sulfide ores or concentrates, on mixed ores, on high-grade oxidized ores; and on low-grade oxidized ores the amount of acid to be purchased or manufactured is greatly reduced. The ferric iron is under easy control, and copper may be effectively deposited from solutions of any acid or iron content likely to be used in copper leaching. From 60 to 75 per cent. of the copper may be removed from the solution in passing through the electrolytic department, before returning the solution to the ore. The amount of copper requiring chemical precipitation, from the waste and foul solutions, is only about 5.0 per cent, of the total copper produced, and this 5.0 per cent. is converted into the electrolytic metal in the regular operation of the process. The entire process can be made practically automatic, and can be carried out mechanically. There is no uncertain departure of any kind in the application of the process; no unusual or unproved apparatus is used. EVER since electrolytic copper refining gave promise of success, about a half century ago, efforts have been made to apply the idea to the extraction of copper from its ores. The methods of attack have, usually, been to leach with a dilute acid and then to deposit electrolytically the copper from the resulting solution with the simultaneous regeneration of the solvent used in the process. Many efforts have been made, and many patents have been taken out, both in the United States and abroad, to give this idea practical application, but only within the past few years have the difficulties been surmounted. Leaching and electrolysis, as applied to copper ores, are among the most promising fields in modern metallurgy. New conditions are arising, which will bring the wet methods into prominence; while high freight rates and increasing cost of fuel will tend to limit smelting to highly favored localities. The possibilities offered by the installation of hydro-electric plants and the greatly enlarged range of power transmission will greatly widen the field of electrolytic methods.

Jan 1, 1924

By R. F. Mehl, M. Gensamer

Although a large number of X-ray photograms of cold-rolled steel have been published, two circumstances have led to the experimental work reported in this paper. The first is that no complete study, making use of the pole-figure method of Weverl, has been made of cold-rolled low-carbon steel. Wever has published pole figures of mild steel subjected to plane parallel deformation1, 2 and undoubtedly he has applied the method to cold-rolled mild steel, but the authors have not found these data published. Kurdjumow and Sachs3 have applied the method to the study of rolling and recrystallization textures in electrolytic iron; their results will be referred to later. The reason for this dearth of papers using the pole-figure method is obvious; a greater number of photograms and more analytical work (although this work is quite simple and straightforward) are required to construct a pole figure than most investigators have felt worth while, despite the fact that no other method of which the authors are aware will satisfactorily depict the orientations of the crystallites in a polycrystalline aggregate. The second circumstance that led to the work reported in this paper was the appearance of a paper by Wayne A. Sisson4 on the same subject. In his valuable study of the factors influencing the development of preferred orientations in cold-rolled mild steel, Sisson made one observation that required confirmation; that is, that at some stage of the rolling process the type of preferred orientation changed from the type that gives a photogram characterized as a "six-point" X-ray pattern to that known as a "four-point" pattern. A similar observation had been made by Tam-mann and Heinzel5, who studied the orientations developed in the rolling of steel by the specular reflection of light from the etched surface of rolled samples. These workers also found that the type of preferred orientation changed during the rolling process. The authors had some difficulty in seeing how this behavior could be consistent with modern views on the genesis of preferred orientations, particularly with those of Wever2

Jan 1, 1936

By H. C. Schultz, F. K. Middleton Hunter

Certain local conditions were known to govern in large measure the successful adaptation of liquid-oxygen explosives to the large-scale blasting at Chuquicamata. The wide variation in hardness of the rock at this mine makes necessary the use of several types of explosives. A locally manufactured, relatively cheap black powder is used in blasting the softer waste and capping material, where a thorough displacement breaks the ground sufficiently. Before the introduction of L. 0. X., an ammonia dynamite of about 65 per cent. strength was being used exclusively in the harder underlying orebody, where a strong disruptive as well as a displacement effect is required for breaking the ore. The L. 0. X., as developed for quarry work in the United States, has a practically pure carbon cartridge material, and the explosive has an extremely high rate of detonation, which should therefore cause it to develop usefully its full disruptive effect in hard ground. The individual blasts at Chuquicamata arc large, black-powder shots which dislodge masses of rock averaging 250,000 tons each, and dynamite shots which dislodge masses averaging 80,000 tons each. It was desirable, therefore, to attempt to displace with L. 0. X. the faster, higher-cost ammonia dynamite used in the smaller blasts. It was not considered practical to attempt to displace the low-cost black powder with 1,. 0. X., as estimated costs showed no probable saving if this were accomplished. Since it was desirable to continue shooting relatively large blasts for effective operation, it was recognized that larger storage facilities than had been in use would be needed for the liquid oxygen. Because of the difficulty of transporting and discharging large storage containers of efficient design, the better plan appeared to be storage and discharge of the liquid at the place of manufacture, and transportation of the filled soaking boxes to the blast. Present Liquid-oxygen Plant An experimental unit with a rated capacity of 75 liters per hour was erected during the latter part of the year 1926 to prove the effectiveness of L. 0. X. at this mine, its cost, and possible efficiency of large-scale storage of the liquid. With this experimental unit 200,000 tons of ore

Jan 1, 1928

By R. F. Mehl, M. Gensamer

Although a large number of X-ray photograms of cold-rolled steel have been published, two circumstances have led to the experimental work reported in this paper. The first is that no complete study, making use of the pole-figure method of Weverl, has been made of cold-rolled low-carbon steel. Wever has published pole figures of mild steel subjected to plane parallel deformation1, 2 and undoubtedly he has applied the method to cold-rolled mild steel, but the authors have not found these data published. Kurdjumow and Sachs3 have applied the method to the study of rolling and recrystallization textures in electrolytic iron; their results will be referred to later. The reason for this dearth of papers using the pole-figure method is obvious; a greater number of photograms and more analytical work (although this work is quite simple and straightforward) are required to construct a pole figure than most investigators have felt worth while, despite the fact that no other method of which the authors are aware will satisfactorily depict the orientations of the crystallites in a polycrystalline aggregate. The second circumstance that led to the work reported in this paper was the appearance of a paper by Wayne A. Sisson4 on the same subject. In his valuable study of the factors influencing the development of preferred orientations in cold-rolled mild steel, Sisson made one observation that required confirmation; that is, that at some stage of the rolling process the type of preferred orientation changed from the type that gives a photogram characterized as a "six-point" X-ray pattern to that known as a "four-point" pattern. A similar observation had been made by Tam-mann and Heinzel5, who studied the orientations developed in the rolling of steel by the specular reflection of light from the etched surface of rolled samples. These workers also found that the type of preferred orientation changed during the rolling process. The authors had some difficulty in seeing how this behavior could be consistent with modern views on the genesis of preferred orientations, particularly with those of Wever2

Jan 1, 1936

By F. H. Wilson

Copper base alloys containing various amounts of aluminum and silicon are of considerable commercial interest. In particular the alloy containing 7 pct aluminum and 2 pet silicon shows an attractive combination of high strength with excellent, machinability. Since there is no evidence ill the literature that this ternary system has been studied since the recognition by Smith1 and Anderson2 in 1939 of the kappa phase of the binary copper-silicon system, the determination of the equilibrium phase relationships in the copper corner of the ternary diagram has been undertaken to provide a fundamental basis for understanding the behavior of these alloys. Phase boundaries have been determined by the micrographic examination of quenched samples while points on the liquidus surface have been obtained by thermal analysis. The results, of sufficient precision to serve their major purpose of providing a guide for the control of the manufacture of alloys in the region covered, are presented in a series of both isothermal and vertical sections of the diagram. Alloys StVdied For a rough survey of the copper corner of this ternary system the compositions listed in Table I (Series A) were employed. The results of examinations of these alloys indicated that the compositions listed in Table 2 (Series B) would further clarify regions of greater complexity. All alloys were prepared as 1200 g heats, the copper being melted under charcoal, and then first silicon and then aluminum were added. An excess of 0.05 pet silicon was allowed to cover deoxidation losses. Two small bars 5/8 by 1 1/4 by 5 1/4 in. were cast using Durville type casting equipment. Ailalyses were made on all alloys using material which was hot-rolled at 800 or 850°C and annealed 17 hr at 650°C. All analyses were found to be within 0.05 pet of the nominal composition. Since the precision of analysis is not much better than this, the points of both isothermal sections and vertical sections at fixed aluminum and silicon contents have been plotted at the compositions indicated by the nominal composition.

Jan 1, 1949

By C. H. Wilson, J. W. Daly, J. J. Jakosky

Meteor Crater, Arizona, is a natural wonder which for years has been the subject of considerable discussion and study as to its origin and age (Fig. 1). Of the various theories advanced regarding the origin, two have been considered as most probable by a majority of investigators. The first theory is that the crater was formed by a meteorite or a swarm of meteoric material striking the earth at a high velocity and burying itself. The second theory is that the crater was formed by a "steam explosion" from hot solutions or gases coming from underneath the present sedimentary beds which overlie the area. In order to obtain more detailed information regarding the conditions existing at the crater, the present management decided to have a detailed geophysical examination made. The origin of the crater is of considerable scientific importance and interest. More or less active mining operations have been carried out during the past 20 years by various groups who believed that the crater was of meteoric origin, and who hoped that sufficient quantities of such material had been buried to be commercially valuable. Fragments of meteoric material found on the surface of the ground in the debris around the rim gave analysis of approximately 92 per cent iron and 8 per cent nickel, with some platinum and iridium. The material having a gross value of approximately $50 per ton, mining would be commercially profitable if sufficient quantities of the material existed in condition for mining. In the early work numerous drill holes and shallow shafts were put down, mainly in the northern portion of the crater. Pulverized material and debris caused considerable difficulty, and in an effort to overcome this the present management started a 1500-ft., two-compartment shaft on the south rim of the crater and outside of the fill zone. The intention was to sink the shaft in the solid rock outside of the crater, and then to crosscut toward the crater at a depth of 1500 ft. The work was finally stopped when a depth of 650 ft. was reached, because water poured into the shaft through large cracks and fissures in the rock. The enormous force responsible for the crater had also broken

Jan 1, 1932

By P. D. Frost, H. A. Robinson, J. R. Doig, M. W. Mote

The mechanism of hardening in heat-treatable zirconium alloys was foUNd to be analogous to that for titanium alloys. Zirconium containing a relatively large addition of a ß -stabilizing element such as molybdenum or columbium can be hardened by the following transformation: Lean alloys, having insufficient alloy content to retain ß at room temperature are hardened by the following transformation: Application of these findings in Zr-Mo-Sn and Zr-Nb-Sn alloys produced strengths as high as 190,000 psi with reasonable ductility. PRIOR research on zirconium alloys has been concerned with development of greater strengths and creep resistance by solid-solution hardening or by dispersion hardening. Although solution and aging heat treatments had been applied earlier to zirconium alloys, quenching frequently produced low ductility. The possibility that the ß-to-w transformation, discovered earlier in titanium alloys,' might also occur in zirconium alloys and cause low ductility was considered, and, indeed, was found as predicted2 to be the case. In the earliest experiments, the heat-treatment response of titanium, too, was disappointing. However, by avoiding the formation of the embrittling w phase, it became practical to obtain room-temperature strengths higher than 180,000 psi, with elongation values of 10 pct.3 Based on the present concept of titanium heat treatment, the principal requirement for a heat-treatable zirconium alloy is that it contains a certain minimum amount of one or more ß -stabilizing elements. Only molybdenum, columbium, and tantalum, when present in sufficient amounts, are known to stabilize ß zirconium to room temperature during rapid cooling from the ß field. Tantalum was undesirable because of its high thermal-neutron cross section. Aluminum and tin are effective a stabilizers, but aluminum has been shown to seriously decrease the corrosion resistance of simple zirconium alloys in hot water. Therefore, for the present study, tin was used as the stabilizer addition. The alloys selected for this evaluation are presented in Table 1 along with their analyses and ß-transus temperatures. The analyses indicated that intended compositions were usually realized. EXPERIMENTAL PROCEDURES All of the alloys were melted from sponge zirconium and fabricated to sheet for heat treatment

Jan 1, 1960

By Maurice E. Peloubet

This discussion of accounting will describe the statements and the information that the accounting system produces, from the point of view of those who use such systems rather than of those who prepare them and who do the detail and technical accounting work. In any well organized mine, quarry, or other enterprise exploiting a mineral deposit, no matter how small, some clerical and accounting work must be done. Miners and other employes must be paid, supplies must be purchased and issued, and various tax and information returns, which even the smallest enterprise must file, have to be prepared. In this chapter it is assumed that the enterprise has employes of this type and that they understand the fundamentals of record keeping and accounting. It would be impossible here to give sufficiently full explanations to enable a man with no previous clerical and accounting training to set up and operate an accounting and cost system for even the simplest extractive operation. Rather, we shall hope first, to tell the investor and the operator, from the chief engineer or president down to a subforeman, what to expect from the accounting statements and records and how to use this information in his daily work; and second, that it will enable the man with some knowledge of accounting or bookkeeping, but with little or no experience in any extractive industry, to set up and operate a satisfactory system for a mine or other extractive enterprise. For readers who wish to go further, the bibliography at the end of this chapter contains many references. The emphasis has, therefore, been placed on the statements to be produced and the purposes for which they are to be used rather than the underlying books and records. These are, with a few exceptions which will be described later, essentially what might be found in any industrial enterprise and would probably, in the extremely small enterprise, consist of handwritten journals, ledgers, analysis books, payroll books, and stores ledgers. In the larger enterprise, various types of mechanical accounting would be introduced in proportion to the complexity of the operation.

Jan 1, 1959

By C. O. Worden, E. K. Landgraf, C. A. Zapffe

Following the discovery of Parke and Ham that deoxidation control of cast molybdenum can be predicated upon simple fractographic examination, a special study of that metal was undertaken to investigate those patterns ascribed to forge-ability and nonforgeability. An elaborately developed system of cleavage patterns immediately rewarded the study; and they are reported here as a necessarily preliminary contribution calling attention to information which is both new in type and in origin. In general, the present observations confirm those of Parke and Ham, and Wood-side; but they also disclose a wealth of detail and correlated phenomena which greatly expand the earlier information. For example, the oxide pattern of nonforgeability is found to be complex, perhaps involving as many as three distinctive patterns, And the nature of the carbide seems to be at least twofold. In addition, transgranular facets are here shown for the first time. Elaborately complex, but in a characteristic manner, these facets depict distortion in original crystal growth which provides truly extraordinary patterns. No carbide and oxide forms display themselves transgranularly, except in profile as exceedingly thin superficial films at the grain boundaries. Crys-tallographic features are also rare—a condition undoubtedly resulting from the great substructural distortion; but occasionally registrations are found of cleavage on {00I}, and faulted areas believed to be Neumann-type deformation on I I121. Introduction Parbe and Ham,' and again Woodside,2 have reported that the forgeability of molybdenum cast by their Vacuum-electric-arc Process can be predicted with great dependability by a simple fractographic observation. They state that nonforgeability is the result of a grain boundary oxide which can be readily identified on the fracture facet at high magnification; and they convert the nonforgeable condition to a forgeable one by increasing the carbon content of the melt until the oxide structures subsequently observed in the fracto-graph become replaced by a second strongly marked pattern characteristic of carbide and coincidentally indicative of forgeability. Considerable importance immediately attaches to such observations: (I) because of their direct commercial application to one of metallurgy's inviting and relatively unexplored metals; (2) because of a general scientific curiosity regarding the nature of these characteristic markings; and (3) perhaps more important, because of

Jan 1, 1949

By R. L. Templin

The increasing use of aluminum and its alloys in commercial fields tias demanded a better understanding of their machining properties. This fact is exemplified by problems that have arisen in the automotive and airplane industries, but many in other fields might be cited. As pure alunlinum and its alloys in their various commercial conditions show appreciable differences in their machining properties, it is not surprising that quite divergent solutions have been offered for the machining problems encountered. However, if the fundamental requirements of the most suitable cutting tools for these metals are understood, these machining problems lend themselves more readily to satisfactory solutions. Since the machining of free cutting brass and mild steel is understood by most persons accustomed to working these metals, it may serve our purpose better to first make a general comparison of the tools more commonly used in machining these metals with the tools most suitable for machining aluminum, then proceed to a more specific discussion of the individual tools. Comparison oF Cutting Tools Cutting tools commonly used for machining free cutting brass usually have little, if any, top and side rake; they are ground on a medium to coarse abrasive wheel and used without any cutting compound or with a cutting compound that has a paraffin base. Those ordinarily used for steel have some top and side rake, are usually ground on a medium to fine abrasive wheel, and are often used with soluble-oil cutting compounds. The proper tools for aluminum and its alloys should have appreciably more side and top rake than the tools for cutting steel; should have very keen edges obtained by grinding with fine or very fine abrasive wheels supplemented in many cases by hand stoning with an oil-stone; and should be used with suitable cutting compounds whenever possible. In many cases, tools suitable for machining aluminum and its alloys are not appreciably different from tools commonly used for cutting hardwoods. The front clearance of a tool most suitable for machining aluminum and its alloys should be about 6°, the top rake from 30" to 50°, making the total angle of the cutting edge of the tool from 35' to 55". A side

By S. D. Strauss

The marketing of nonferrous metals and of the ores and concentrates from which these metals are recovered is a fascinating trade, international in character, sensitive to every change in the economic tide, and complex in its organization. Each individual metal has its own marketing mechanism; no two are exactly alike. The differences sometimes are a matter of tradition rather than of necessity, but usually they have developed because of the very nature of the problems of producing or consuming the individual metal. This description, because of limitations of space, can do no more than indicate the major aspects of the trade and touch lightly on the marketing structure of each metal. The dictionary states that a market is a "meeting of people for selling and buying." In the case of nonferrous metals this meeting may occur on a half-dozen different occasions between the time the ore has been first mined and the time the refined metal is available for use by industry; or it may not occur at all until after the metal itself has been rolled, drawn, stamped, cast, or forged into a useful semifabricated shape. To illustrate: A Chilean miner may sell his small ore production to a custom mill, which produces concentrates that are sold to an ore dealer, who finances the shipments of the concentrates to a United States custom smelter, which buys these' concentrates for conversion into blister, which is subsequently refined into electrolytic copper and sold. Conversely, much of the production of aluminum is in the hands of integrated concerns that mine bauxite, convert bauxite to alumina, smelt the alumina to produce aluminum, and then fabricate the aluminum into semifinished or even finished products before title to the material changes hands for the first time. Some nonferrous ores are not converted into metal at all but are sold by the miners or dealers directly b the ultimate consumers. A good example would be chrome ores used by the chemical industry. And of course a substantial part of the commerce in nonferrous metals is in scrap, which is the reconversion into useful form of metals that have long since been mined and smelted. Thus, one-third of all the lead used in the United

Jan 1, 1959

By John Greenawalt

IN view of the increasing importance of sintering in the beneficiation of iron ores preparatory to their reduction in the blast furnace, the writer believes the time is opportune for an up-to-date, though brief, discussion of the general principles of sintering, as well as a discussion of some of the recent improvements and mechanical developments that have been achieved in this industry, its present trend and future possibilities. Sintering may be defined as the agglomeration of fine mineral particles into a porous mass by incipient fusion caused by heat produced by com-bustion within the mass itself. Its first successful application, in connec-tion with the treatment of lead sulphide ores, was known as blast roasting. In this process the lead ore was given a preliminary roasting in a reverber-atory furnace, then the incandescent mass was placed in a pot with a grate and an updraft was applied. It was soon discovered that much better results were obtained by cooling the ore, moistening it, and placing it upon an incandescent layer of fuel previously placed upon a grate, and then applying the updraft blast of air until the charge was converted into a more or less agglomerated mass. The fuel was sulphur and the process one of desulphurization, which was the principal result desired. The application of downdraft to blast roasting brought about tremen-dous results; the principal one of which was that an air blast of high pressure could be passed through a layer of ore deposited on a grate, or on a grate covered by a layer of coarse porous material, without disturbing the particles of which the layer is composed. The air current is compelled to filter through the pores of the charge, whereas if the same pressure applied to the top surface of the charge with downdraft were applied to the bottom of the charge with updraft, the charge would be completely blown off the grate. Another result of reversing the draft was that a flame could readily be applied to the top surface of the charge for ignit-ing purposes.

Jan 1, 1938

By Charles G. Maier

SCIENCE beginning in rational observation came of age, when its devotees first began to measure and count. It has been said that the most striking aspect, of science today is its growing abstraction, and its preoccupation with mathematical symbolism. Technology with specific and concrete objectives in the satisfaction of human wants, cannot conceivably achieve the abstract unification that science seeks, but .the utility of the' scientist's method has been too well proved to require bolstering. Metallurgy is in its scientific infancy.

Jan 1, 1931

By H. S. Ten Eyck

Fertilizer normally is spoken of as having three main components: nitrogen, phosphorus and pot- ash. Certainly, however sulfur must also be considered a basic component of fertilizers, even though in many instances it does not end up as a part of the end product. In addition, with heavier cropping and the resultant drain of plant foods from the soil, we have now reached a point where the minor elements necessary for plant growth have become a major factor in the fertilizer industry.

Jan 7, 1967

By F. E. Rizzo, L. R. Bidwell, D. F. Frank

THE poor high-temperature oxidation resistance of the refractory metals becomes an important problem as higher operating temperatures are sought. A meaningful analysis of their oxidation behavior requires a knowledge of the phases that can appear during oxidation as well as their relative stability. Although several extensive investigations have been carried out to obtain this information for the W-0 system,1-10 serious inconsistencies still remain. First, the standard free energies of formation (AG°) determined in recent studies which used the solid electrolyte galvanic cell technique6,7,9 differ significantly from those obtained primarily from gas equilibration measurements.1,3,4,10 The disagreement is especially large for the highest oxides. These data have been used to predict the decomposition temperatures of WO2. 72 and WO2.90.1 A considerable extrapolation is required, resulting in a large uncertainty in the decomposition temperatures. Second, Bousquet and perachon3 have presented convincing evidence, ob- tained by gas equilibration measurements, in support of the long-contested existence of W30. Phillips and chang,ll on the other hand, were not able to observe this phase under similar experimental conditions. The purposes of this work, which is part of a continuing investigation of the W-Mo system, were to resolve the discrepancies between the AGO measured by gas equilibration and solid electrolyte galvanic cell techniques, to extend the latter measurements to lower temperatures, to redetermine the WO2.72 and WO2.90 decomposition temperatures, and to apply the more sensitive electromotive-force method to the question of the existence of W3O. I) EXPERIMENTAL PROCEDURE The measurement of ?G° of reaction by the use of calcia-stabilized zirconia solid electrolyte galvanic cells has been described previously.12 The method is based on the measurement of the difference in chemical potential of oxygen between an electrode containing the two oxides of interest and a reference electrode of known oxygen activity. Two different types of cell holders were used in this study. The first type of apparatus has been described earlier." It consisted of two solid electrodes separated by a disc of electrolyte. Both electrodes were exposed to the same stream of purified helium. With this design a gaseous transport of oxygen between the two electrodes is possible. The second type of apparatus, which has also been described earlier,14 effectively separated the two electrode atmospheres. It utilized a closed-end impervious, calcia-stabilized zirconia tube that was open to the atmosphere. The tube served as an electrolyte for the cell and provided a means for separating the anode compartment, which was held under a static vacuum, from an air reference cathode. The cells and reactions of interest are described in Table I. High-purity tungsten metal was obtained from the Fansteel Metallurgical Corp. and the Allied Chemical Corp. Table II contains an analysis of each material. WO3 was prepared by oxidizing the metal in air at approximately 600°C in high-purity recrystallized alumina boats and by the dehydration of reagent-grade tungstic acid in alundum boats. The two methods of preparing WO3 resulted in slightly different purities.

Jan 1, 1968

By M. E. Wadsworth, J. S. Cho

Colloidal silica dissolved in aqueous suspensions of high surface area thoria was permitted to adsorb on the thoria surface. Silica in three forms was identified by means of infrared spectroscopy and characterized by Si-O vibrational modes in the 9.0 to 10.5 region. A band at 9. 1 was attributed to free unad-sorbed silica, while adsorbed silica resulted in bands of greatest absorbency at 9.4 or 10.3p, depending upon the character of the surface bonding. Size considerations, the amount of silica adsorbed, and the character of the infrared spectrum for strongly adsorbed silica has been interpreted as evidence of formation of chain or layer silica linkages on the thoria surface. Infrared spectroscopy has been used successfully in recent years for the identification of minerals and synthetic inorganic substances. Unfortunately, infrared studies of silicate minerals have not proceeded to the point that unambiguous assignments may be made for Si-O vibrational modes as affected by lattice substitutions and structures. Several investigators have presented infrared spectra of silicate minerals, 1,7 and their work has pointed to the potential value of infrared to identify minerals as well as to note the sensitivity of various Si-O modes to structural and substitutional environments. The strong infrared absorption of various Si-O vibrational modes makes the infrared method a very useful tool for the study of silica adsorbed on the surface of solids of high surface area. Spaepen et a18 studied the adsorption of silica on thoria surfaces from aqueous solutions of silicic acid up to 300°C. A general review of the application of the infrared method to the study of surface adsorption has been presented by Pliskin and Eischens.9 EXPERIMENTAL Du Pont colloidal silica, Ludox SM (16.36% SiO2) and Ludox HS (30.25% SiO2) in aqueous suspensions were used as the sources of silica for the adsorption studies. The thoria used for this study was supplied by Union Carbide Nuclear Co.* under the preparation *Chemical Technology Div., Union Carbide Nuclear Co., Oak Ridge, Tenn. . number D-16-650. It was fired from the oxalate at 650°C and had a surface area of 32.4 ± 0.6 m2 per g measured by nitrogen adsorption. The chemical analysis of the D-16 thoria in ppm was: CO3= (5500), NO3- (< 4), so4±PO4 (100), and Si (20). The Ludox silica was placed in contact with the thoria in a two-liter autoclave10 between room temperature and 250°C. Slurries were made by placing 1 g of thoria in one liter of distilled water containing various additions of the silica sol. Samples were removed from the autoclave by opening a small stainless steel valve. Extracted samples were centrifuged for 10 min and excess solution was decanted. The sample was then dried for several hours at 80°C. Infrared samples were prepared by thoroughly mixing 10 mg of the thoria with 400 mg KBr in polystyrene vials on a "Wig-L-Bug" amalgamator. Pellets were pressed under vacuum and had final dimensions of 1.2 cm diam and 1.2 mm thick. Infrared spectra were

Jan 1, 1963

By Richard Moldenke

Note.—At the request of the American Society for Testing Materials, this paper wau presented at the New York Meeting, February, 1923, in connection with the "A. S. T. M. Tentative Specifications for Foundry Pig Iron" and The Physics of Cast Iron and Its Bearing on All Cast-iron Products and Specifications for Cast Iron," by William R. Webster. The discussion of this paper was not published by the Institute, having been referred to the American Society for Testing Materials, as these papers were again presented for discussion at the meeting of that Society at Atlantic Cit;, June, 1923. The result of these discussions is shown in the following abstract from the Committee A3 report on cast-iron specifications: During the past year, the adaptability of the tentative specifications for pig iron for the steel and the malleable foundry, in addition to the iron foundry proper, have been studied and suitable changes and rearrangements are being made which appear to cover the situation properly. In spite of the experience of foundrymen to the contrary, there is a persistent call from consumers of castinga for defixute compositions for given lines of castings. To respond to this call for information desired by the consumer—information every modern foundryman should have and guide his procedure with—the committee has requested the Sub-committee on General Cast!rigs to take up this matter with a view of constructing tables of analyses rang? for Important lines of foundry product. These analyses ranges however, are to be given as "recommendgd practice" and not intended for actual spkcification. In this way, the consumer of the foundry product will get the information he wants; the furnace-man will be gulded in the production of his pig irons to prepare for analyses ranges which are more closely standardized and have less of "freak" requirements made by Inexperienced metallurgists; and the foundryman will not be bound by chemical requirements he knows will not work out well with his particular reglonal supphes of melting stock. Doctor Moldenke&apos;s paper is published in full as it shows clearly the good results of the Institute&apos;s work in 1895 and a comparison of the same with the present knowledge of the metallurgy of cast iron—Bradley Stoughton, Chairman, Iron and Steel Committee. In MaRch, 1895, William R. Webster contributed a carefully prepared scheme for the study of the physics of cast iron to the American Institute of Mining Engineers at its Florida meeting. This summary of the interrelation of the chemical and physical characteristics of cast iron with the operations of daily foundry practice caused a wide discussion of the then little understood though universally used material. Mr. Webster has requested the author to bring the subject up to date and, while glad to comply, he must pay that with all the knowledge that has been gained in the quarter century that has passed since the subject was brought to the attention of the Institute—and we now are pretty familiar with cast iron in all its aspects—there is practically noth-

Jan 1, 1923

By W. R. Opie, O. W. Mole

By confining the electrolytic reduction of TiCl4 to the interior of a porous basket-cathode the electrolyte between the anode and the cathode can be kept free of reduced chlorides of titanium eliminating undesirable reactions of reduced titanium chlorides with brickwork or oxygen in the cell atmosphere. Semiwalls are not needed. Operating conditions are given and discussed. Titanium yields based on TiCl4 introduced are 93 pct. Cell voltage and amperage characteristics are adaptable to multiple cathode-series cell urmngements. EXPERIMENTS conducted in the National Lead Co., Titanium Division, Research Laboratories showed that titanium metal could be deposited in an electrolytic cell in which titanium tetrachloride was introduced through a tubular cathode.&apos; The reduced chlorides as formed were confined to the vicinity of the cathode. They were reduced to form a cocoon-shaped growth of sponge titanium metal at the end of the cathodic tube below the surface of a sodium chloride-strontium chloride electrolyte. No diaphragm was needed.&apos; Although high-purity, coarse crystalline metal was produced in the cocoon growth, the yields of metal removed from the cell, based on the amount of titanium introduced as TiCl4, were usually only 40 to 60 pct. The growth of the cocoon deposits was away from the cathodic tube for introduction of TiC14 toward the anode following the flu lines. The reduced chlorides of titanium diffused through the deposit and were reduced to titanium electrolytically within the deposit or on the outer surfaces. Deposition within the pores of the cocoon was detrimental to further deposition because it plugged the passages used by the reduced chlorides to diffuse away from the point of titanium introduction. As plugging due to deposition in the pores proceeded, the reduced chlorides in the center of the cocoon would force their way out by forming a channel and would escape from the vicinity of the cathode without being reduced to metal. Some work had been done previously1, 2 which indicated that if the end of the cathodic tube for introducing TiC14 was surrounded by a screen connected to the tube so that it too was cathodic, growth could be made to occur within the screen. Direction of growth was observed to be from the screen toward the point of TiCl4 introduction. Through a series of design modifications a cathode evolved which consisted of an introduction tube surrounded by a perforated metal basket as shown in Fig. 1. Modifications of this design are described in Refs. 3, 4, and 5. This basic cathode designa" was incorporated in electrolytic cells containing graphite anodes and constructed of high-silica brick refractory for containing the electrolyte (see Fig. 2). The inner crucible was surrounded by insulating brick and the entire unit contained in a welded steel shell. Suitable cooling chambers with inert gas atmospheres were devised so that the cathode could be removed from the cell without exposing the deposit to air while hot. Various alkali and alkaline earth chlorides were used as electrolytes.

Jan 1, 1961

By Richard Moldenke

Note.—At the request of the American Society for Testing Materials, this paper wau presented at the New York Meeting, February, 1923, in connection with the "A. S. T. M. Tentative Specifications for Foundry Pig Iron" and The Physics of Cast Iron and Its Bearing on All Cast-iron Products and Specifications for Cast Iron," by William R. Webster. The discussion of this paper was not published by the Institute, having been referred to the American Society for Testing Materials, as these papers were again presented for discussion at the meeting of that Society at Atlantic Cit;, June, 1923. The result of these discussions is shown in the following abstract from the Committee A3 report on cast-iron specifications: During the past year, the adaptability of the tentative specifications for pig iron for the steel and the malleable foundry, in addition to the iron foundry proper, have been studied and suitable changes and rearrangements are being made which appear to cover the situation properly. In spite of the experience of foundrymen to the contrary, there is a persistent call from consumers of castinga for defixute compositions for given lines of castings. To respond to this call for information desired by the consumer—information every modern foundryman should have and guide his procedure with—the committee has requested the Sub-committee on General Cast!rigs to take up this matter with a view of constructing tables of analyses rang? for Important lines of foundry product. These analyses ranges however, are to be given as "recommendgd practice" and not intended for actual spkcification. In this way, the consumer of the foundry product will get the information he wants; the furnace-man will be gulded in the production of his pig irons to prepare for analyses ranges which are more closely standardized and have less of "freak" requirements made by Inexperienced metallurgists; and the foundryman will not be bound by chemical requirements he knows will not work out well with his particular reglonal supphes of melting stock. Doctor Moldenke&apos;s paper is published in full as it shows clearly the good results of the Institute&apos;s work in 1895 and a comparison of the same with the present knowledge of the metallurgy of cast iron—Bradley Stoughton, Chairman, Iron and Steel Committee. In MaRch, 1895, William R. Webster contributed a carefully prepared scheme for the study of the physics of cast iron to the American Institute of Mining Engineers at its Florida meeting. This summary of the interrelation of the chemical and physical characteristics of cast iron with the operations of daily foundry practice caused a wide discussion of the then little understood though universally used material. Mr. Webster has requested the author to bring the subject up to date and, while glad to comply, he must pay that with all the knowledge that has been gained in the quarter century that has passed since the subject was brought to the attention of the Institute—and we now are pretty familiar with cast iron in all its aspects—there is practically noth-

Jan 1, 1923