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By Paul Merica

ONE of the most useful, and at the same time least commonly used, methods of thermal analysis for the determination of transformations in metals and alloys consists in the recording of the tune intervals required for successive increments of temperature change during heating or cooling, the temperature of the furnace containing the specimen being altered at a uniform rate. The curve obtained by plotting these time intervals as a function of the mean temperature of the specimen during the interval is called the inverse-rate curve. It is probably due to the fact that no simple and convenient method has apparently been available for the measurement of the successive time intervals that this method has not been so generally used as, for example, the differential method, for which several tykes of automatic or semi-automatic apparatus have been designed. Whenever this method has been used, the intervals have usually been measured with the use of a chronograph; its operation as practised at the Bureau of Standards' is as follows: The temperature of the specimen is measured by a thermocouple and a dial potentiometer. The operator sets the potentiometer at successive values of the electromotive force differing by equal increments, usually 0.02 millivolt, and records the exact instant on the chronograph, by pressing a contact key, at which the galvanometer coil passes through its null position. Two-second intervals are also recorded on the chronograph record, and the number of 'seconds elapsing between successive signals is afterward counted from the record and plotted as a function of the electromotive force or of the temperature. This is an admirable method and by it most minute thermal arrests may be detected, but it requires a good chronograph, which is generally difficult to obtain, and the time of one operator during the recording and, subsequently, to read the intervals from the record; the latter operation often takes from one to two hours.

Jan 7, 1919

By J. D. Dixon

Procedures are given for calculating stresses in underground tunnel supports which accounts both for the structural behavior of the support and that of the adjacent rock mass. Stresses in the support are caused by service loads and rock reactions. Service loads are due to rock pressures, hydrostatic and hydraulic pressures, selfweight of the support, or other utilitarian-type loads. Rock reactions, equal and opposite those in the support, are due to the deformational interaction that results as service loads deform the tunnel support against the adjacent rock mass. The procedures developed for solving this problem are an application of matrix structural analysis. The principles involved in this method allow for the consideration of the deformable characteristics of most tunnel support systems and an iterative solution procedure is applied to determine the areas of support-rock interaction. Numerical results of example problems are given.

Jan 1, 1972

By F. A. Forward, A. H. Ross, J. Halpern

IN treating carnotite ores by carbonate leaching it is often necessary to subject the ore to a prior roast. Among the advantages that may result from roasting are: 1) improvement in settling and filtering characteristics of the ore; 2) destruction of carbonaceous impurities that would otherwise contaminate the leach solution and consume carbonate reagent; and 3) substantial increase in extraction of vanadium, which is usually low when the un-roasted ore is leached. Recovery of vanadium may be an important factor in processing carnotite ores, and the fact that vanadium is usually recovered in good yield by acid leaching has often been an economic advantage over results obtained with carbonate leaching. It has been found that response of an ore to carbonate leaching, following roasting, depends primarily on its composition and on the conditions of the prior roast treatment, particularly with regard to the roasting temperature, the atmosphere maintained above the charge during roasting and cooling, and the presence of certain reagents. These factors, especially the last, virtually determine the extractions of uranium and vanadium attainable by carbonate leaching, as well as the reagent consumption on leaching, whereas adjustment of the leaching conditions has only a limited influence. These variables were examined systematically to elucidate roasting and carbonate leaching of carnotite ores and to establish a treatment yielding high recoveries of both uranium and vanadium. Tests were conducted on samples of four different Colorado Plateau ores, described in Table I. Roasting Procedure: The roasting tests were conducted in an electrically heated furnace in which the temperature was controlled to +15oC. The ore (usually a 500-g charge) was ground to —100 mesh, mixed with the desired reagent, and spread in a silica tray to a bed depth of about 1/2 in. During the roast the charge was rabbled at intervals of 15 min. To provide free access of air the furnace was usually ventilated; however, in a few experiments a controlled atmosphere such as carbon dioxide or hydrogen was maintained above the charge. Leaching Procedure: The pulp, generally comprising 500 g of ore and a 2000-cc solution containing 80 g per liter of Na2CO3 and 20 g per liter of NaHCO3, was agitated in an autoclave at 120°C, under 30 psi O2. Samples were withdrawn periodically, and the solution and ore residue were analyzed. Under the conditions employed, maximum attainable extractions were generally achieved in 4

Jan 1, 1958

By William M. Kester

INTRODUCTION The Coal Research Bureau of the School of Mines at West Virginia University is presently conducting laboratory-scale tests to determine the technical feasibility of beneficiating pulverized coal and coal fines with high-intensity electromagnetic fields. Interest in magnetic processes for cleaning fine coals was stimulated by results obtained by Yurovsky, et a1 in 1958.1 This work, while not new in concept,2,3 indicated that pulverized coal which had been thermally treated in a rotary drum in the presence of superheated steam and air underwent thermo- chemical reactions. Films of the ferromagnetic minerals magnetite (Fe2O3), hematite (Fe3O4), and pyrrhotite (FeS[3]) were reported to be formed on the surfaces of the pyrite grains associated with fine coal during the foregoing treatment at temperatures ranging from 120 to 360°C. After thermal treatment the coal was magnetically separated in an experimental magnetic device having a field strength of 10,000 oersteds.

Jan 5, 1965

By Linn Bradley, W. W. Strong, H. D. Egbert

Marked differences of opinion have been expressed by engineers interested in cleaning iron blast-furnace gases for use in hot-blast stoves and under boilers, in reference to the advantages of a hot-dry method over a cold-wet method. One point at issue involves the sensible heat energy in the moisture contained in the gas. Some advocates of the cold-wet methods claim that the condensation and resultant removal of the greater portion of this contained moisture by wet scrubbing, spraying or similar methods, results in a saving of some of this sensible heat energy, by reason of the fact that water vapor has a high capacity for sensible heat energy and may carry from the exit of a hot-blast stove, for example, more heat units than are sacrificed or lost when the gas is cleaned by this cold-wet method. Other advantages claimed for the latter method are: That gas burns more readily when it is free from moisture in any form; that because gas is made denser by cooling and removing the moisture it has a higher calorific value than hot gas carrying moisture; and that higher flame temperatures are obtained when the gas is cleaned by the cold-wet method. A search through the available literature fails to disclose any extensive calculations or records of conditions obtained in practice, bearing upon these phases of gas cleaning. This paper deals with these problems from the standpoint of the economy of using a gas of higher flame temperatures, of improved stove design, and of economy in the gas-cleaning department. Calculations have been made which show that by cleaning the gases by a cold-wet method the sensible heat energy of the blast-furnace gases is greatly reduced; and, in general, this loss of heat energy is far greater than that lost from the stoves or boilers due to the sensible heat capacity of the water vapor if carried away by the exit gases. By making use of the

Jan 1, 1917

By J. H. Kittel

THE properties of the metal molybdenum have been the subject of recent investigations1,2 = which have included studies of the changes that occur in the metal when it is annealed after having been cold worked. Most of the data which have been reported have pertained to only one aspect of annealing, that is, the conditions under which recrys-tallization has been observecl. The process of recovery which may precede recrystallization docs not appear to have been investigated, and it is the purpose of this note to report observations on the recovery process in cold-worked molybdenum as determined by changes ill the thermoelectric power which occur as the metal is annealed. The measurements were made on commercially pure molybdenum wires which, after annealing at 1035°C in dried hydrogen for 1 hr, were swaged to give a series of reductions up to a maximum of 84.5 pct. The variously cold-worked wires were then annea1c.d in dried hydrogen for periods of 16 hr at progrc:ssively highel. temperatures from 200" to 1000 c with a final annealing treatment of 70 hr at. 1100°C. After each annealing treatment the ther.ma1 emf's were determined against a length of original unwo~,ked material that had received the initial hydrogen anrit,aling treatment. The difference in temperature between the hot and cold junctions was maintained at about 75'C. and. the thermal emf's were measured with a potentiometer that could be read. to 0.01 microvolt. Fig. 1 shows the thermoelectric power. (dE/dT) in microvolts per C between annclalcd and cold-worked molybdenum as a function of the degree of cold work. The effect of annealing is shown in Fig. 2. The general shape of the curves in both figures is similar to results which have been obtained for copper." It was observed that after annealing at temperatures as low as 200°C recovery was well under way. The rapid changes irt thermoelectric power observed near 900 C are probably associated with recrystallization, since such a relation has been observed with copper. Beyond 900°C the thermal emf's changed in polarity. indicating that from this point or1 the specimens were more highly annealed than the standard. Annealing treatments could not be given at temperatures higher than 1100°C due to limitations of the furnace, and it is evident that, since equilibrium values of thermoelectric powers were far from having been attained, temperatures considerably higher are required to fully anneal molybdenum. References Robert M. Parke: Molybdenum, A New High-Temperature Material. Metal Progress (1951) 60, pp. 81-96. * R. A. Long, K. C. Dike, and H. R. Bear: Some Properties of High-Purity Sintered Wrought Molybdenum Metal at Temperatures up to 2400 °F. NACA TN 2319 (March 1951): G. W. Brindley: A Thern-io-Electric Study of the Cold-Rolling and Heat-Treatment of Copper, Report of a Conference on the Strength of Solids. Physical Society, London (1948) pp. 95-106.

Jan 1, 1953

By R. L. Fleischer, W. F. Hosford

Tensile data for coarse grained aluminum Polycrystals suggest that the "grain size" effect is not due to dislocations piled up at grain boundaries but rather is primarily a relative size effect due to surface crystals being weaker and less confined. STUDIES directed at interpreting hardening of poly-crystalline metals normally identify their strain hardening properties with those in some particular type of single crystal.1"4 The recent recognition in face centered-cubic metals of a nearly linear stage with rapid hardening occuring at comparable rates for both polycrystals and single crystals, suggested that the same process or processes determine both cases and hence that there exists some justification for the use of single crystals to understand polycrystals. Further evidence for the above view may be found by an approach initiated by Chalmers:5 By using bicrystals of controlled orientation it is possible to begin to assemble a polycrystal and also to study grain boundary effects in detail. In this way it has been found that a single grain boundary affects easy glide but not the subsequent stage II hardening.6 This result suggests that a sensitive way to observe grain boundary effects in polycrystals would be to vary grain size and measure easy glide. As will be seen, easy glide is only possible for coarse-grained samples, and hence the results will serve to fill in the gap in measurements between single crystals and bicrystals on one hand and fine-grained polycrystals on the other. One problem inherent in comparing single crystals with polycrystals is the uncertainty as to what slip systems are acting in a polycrystal. To compare the two types of samples, rates of shear hardeninn---L. on the acting -planes are needed. and these may be computed only if it is known what particular systems are active. The acting systems were examined for a coarse-grained polycrystal and it will be shown that the systems supplying the preponderance of slip can be determined with little ambiguity. EXPERIMENTAL PROCEDURE Twelve samples of aluminum were prepared by chill casting into a heated graphite mold, followed by annealing at 635° ± 5°C for 24 hr with an 8-hr fur- nace cool, and finally either etching7 or electropol-ishing.' The samples, with a 7 to 10 cm length between grips and 4.4 by 6.6 mm in cross section, were deformed at a strain rate of about 3 10 -3 . per min in a tensile device which has been described elsewhere.5 The composition was reported by Alcoa as 99.992 pct Al, 0.004 pct Zn, 0.002 pct Cu, 0.001 pct Fe, and 0.001 pct Si; nine samples were deformed while immersed in liquid helium and three in air at room temperature. The stress-strain curve for one of the samples (P-1) deformed at 4.2 "K has been reported previ~usl~.~ This sample was selected for determination of active slip systems. Eighteen of the crystals were examined by optical microscopy to determine the angles of slip line traces and by X-ray back reflection to determine orientation. By this means the slip planes were determined and the resolved shear stress factors for possible slip systems could be computed. Finally each sample was sectioned so that after etching, the number of crystals could be counted for each of ten newly exposed surfaces. The average of these ten values will be termed n, the number of crystals per cross section. Values of 11, varied from 1.9 (nearly bamboo structure) to 12.7. Sketches of typical cross sections appear in Fig. 1. RESULTS AND DISCUSSION: SLIP SYSTEMS 1) Determination of Acting Slip Planes—The stress axis orientation and operative slip planes in eighteen crystals of sample P-1, as determined by slip line traces and crystal orientation, are summarized in Fig. 2. For one of the crystals two planes had a common trace. so that the traces alone did not distinguish which plane or planes were slipping. However it was found that the stress resolving factor for the primary system was 0.386, .while that for the most stressed system in the other plane (indicated bv the dotted arrow) is 0.138. It will be assumed tgerefore that only the primary plane acted. Since the orientations were determined after extending the samples 4 pct, the stress axes may be rotated from their original value by as much as 2 deg in some cases. It is interesting to note that in five crystals only one slip plane acted, in eight two acted, and in five three planes were observed—an average of two slip

Jan 1, 1962

By Ronald Gibala

THE Au-Ni alloy system is one of many binary systems in which the supersaturated solid solutions may exhibit a multistaged precipitation behavior during aging. In addition to the equilibrium phase separation, which was studied extensively years ago in the range 400" to 600",' there exists at least one earlier stage of precipitation, i.e., preprecipitation, which occurs below 300°C in quenched alls.-This note reports on some effects of composition on the preprecipitation in Au-Ni alloys as determined from resistivity measurements. The kinetics of the preprecipitation were studied in alloys of 15 to 85 at. pct Ni which were water- were found in alloys which after various quenching-and-aging treatments were slowly heated and cooled (1Z"C per hr) between room temperature and about 300°C. Two such heating-cooling curves for a 40 pct Ni alloy are shown in Fig. 2. Similar effects were observed in other 15 to 50 pct Ni alloys. These curves are characterized upon heating by two changes in slope indicated by A and B in the figure and upon cooling by a resistivity hysteresis of approximately the size of the original decrease in resistivity after the aging treatment. The inflection at B generally falls at about the same temperature for all heating curves for a given alloy and appears to be a critical temperature (T,) for the preprecipitation for that alloy. The values of T, for most of the 15 to 50 pct Ni alloys fall in the range 200" to 220°C. The position of the inflection at A depends upon the heat treatment prior to the heating-cooling run and perhaps the heating rate, which was held constant in these runs. The preprecipitates grown in by the appropriate aging treatments seem to decrease in size as the alloys are heated from A to T,, dissolve at T,, and do not reappear after cooling below T,. When similar heating-cooling treatments were performed on 60 to 85 pct Ni alloys, an entirely different behavior was observed. Typical results are shown in Fig. 3 for an 85 pct Ni alloy. In these

Jan 1, 1964

By T. S. Plaskett

A striated structure perpendicular to the growth axis was observed by the copper-decoration tech-nique in dislocation-free, .float-zoned silicon crystals. The striations, which were spaced about 100 p apart, fitted the relationship d = f/u , where d is the spacing, f is the growth rate, and u is the crystal rotation rate. Each stria was resolved into an UNDOPED silicon crystals pulled from quartz crucibles by the Czochralski technique usually exhibit a striated structure perpendicular to the growth axis.'-' This structure has been attributed to oxygen segregation, with the oxygen being introduced from the quartz crucible. If the crucible is rotated, the level of oxygen contamination has been reported as high as 10° atoms per cu cm.10 These striations are similar to solute striations commonly observed in doped Czochralski-grown crystals. The periodic nature of the striations is caused by a periodic variation in the growth rate",12 which is attributed mainly to thermal gradients in the melt.13 A finer striated structure14 attributed to constitutional supercooling is sometimes observed between the coarse striae. The oxygen striations have been observed by infrared transmission techniques,' by the copper-decoration technique,' by X-ray diffraction microscopy,6-8 and by 9 p absorption measurements3 on crystals pulled from the melt both with and without dislocations. In this investigation float-zoned dislocation-free crystals were examined by the copper-decoration technique. The level of oxygen for float-zone material is less than 1016 atoms per cu cm the lower limit of detection by 9 p absorption measurement. EXPERIMENTAL TECHNIQUE The crystals were grown by the float-zone process with the rf heating coil outside of the quartz envelope containing the silicon. All float zoning was done under an atmosphere of purified helium. The Dash technique15 was used to grow the crystal dislocation-free. This involves growing the crystal initially with a diameter between 2 and 3 mm and at array of starlike precipitates of copper. The strucLure was not .found at the surface tor a depth of about 1.5 mm, or in a region of similar width ahead of a dislocation network. The structure is postulated to consist of vacancy clusterings or dislocation loops. very rapid rates, about 20 mm per min, for a distance of about 3 cm. The diameter of the crystal is then increased to the diameter of the source of silicon, which in this case was about 19 mm. Because of the arrangement of the apparatus, the zone was passed downward rather than upward, contrary to the standard float-zoning practice. Also, the source was rotated rather than the seed. ziegler17 has made dislocation-free crystals by a similar technique but has passed the zone upwards. The starting material was zone-refined and had a p-type resistivity of 150 ohm-cm. The major impurity was boron; the total impurity excluding the boron was reported by the supplier (Dow-Corning) to be typically less than 2 x 1013 atoms per cu cm. The crystals were examined by the Dash copper-decoration technique18'19—a method in which about 10" atoms per cu cm of copper are diffused at a temperature between 900" and 1000°C into silicon which is then quenched to room temperature. On quenching, the copper precipitates on crystalline defects which are then visible when viewed by transmission infrared microscopy. The photomicrographs shown were taken either of the infrared image tube screen or directly on infrared film. All sections prior to decorating were chemically polished and, for some sections, given a sirtlZ0 dislocation etch-pit examination. After decorating, the samples were mechanically polished. RESULTS A photomicrograph, taken in transmission of a decorated cross section, is shown in Fig. 1. The portion of the section shown is near the surface of the crystal. The entire cross section showed no dislocation etch pits after being given a Sirtl etch treatment. It is seen that the copper precipitated randomly. Each precipitate, as has been reported by others, was found to have a starlike structure.

Jan 1, 1965

By L. J. Ingvalson, Roy H. Miller

IN 1948, as part of a program to expand the copper tube mill facilities of the American Brass Co. plant at Kenosha, Wisconsin, plans were formulated to convert the 100 ton capacity anode casting furnace at the Great Falls, Montana plant of the Anaconda Co. to the production of 3 in. phosphor -ized billets. The furnace was rebuilt completely and construction was started on an addition to the building. Members of the Great Falls staff visited various billet casting plants to draw upon the experience of other producers of this type of casting. Many features of other plants were incorporated into the Great Falls plant but, in addition, many new designs were made and perfected to make the plant the most advanced of its type. Construction was begun in 1949, with the intention of having the plant in production in the early part of 1951. In January 1951, as the plant was being rushed to completion, the government placed restrictions on the production of copper tubing. As a result, work was halted and the plant lay idle for two years. Interest was reactivated in May 1953 with the lifting of restrictions on copper. Plans were laid to go into production in July and the first charge was taken out July 1, 1953. Basically the plant is designed to produce from cathode copper a 3 in. diam billet, 50 in. long. weighing 110 lb, and containing 0.013 to 0.036 pct P, at a rate of 150,000 Ib per operating day. These billets are to be pierced and drawn into tubing. Furnace The furnace is a 100 ton capacity reverberatory type, gas fired furnace; 21 ft long and 9 ft wide. Gas is introduced to the furnace through two 38 hole Mettler gas burners. These burners are of chrome nickel alloy with four jets per hole. The furnace is charged with cathodes from the Electrolytic Copper Refinery plus return scrap from the casting operation by means of a Wellman Seaver Morgan Co. 7,000 lb capacity charging machine. The charge crane has a 20 ft boom and fork peel provided with an air ram to push material off the peel. The machine travels on overhead tracks and can be moved in any direction. The boom can be raised and lowered and swung through an arc of 180". With well stacked units of 6,000 lb, an experienced operator can put the first charge into the furnace in 40 min. After charging, the steel framed silica brick charge door is put in place and sealed with clay. After melting and skimming off the slag, the copper is blown until an oxygen content of 0.40 pct is reached. The metal is then heated to 2180°F, covered with coke, and poled. Poling is continued until a 3 in. diam test billet, 8 in. long, shows a flat set. The oxygen content is usually 0.030 pct at this time. At the end of poling, a temperature of 2160" to 2180°F is desired. In the side of the furnace opposite the charging door is the taphole slot, extending 36 in. upward from the bottom of the furnace. It is 4½ in. wide at the outside face and widens to 9 in. at the inside face of the furnace. It is filled with a wet mixture of sand, fireclay, and crushed coal. Flow of metal

Jan 1, 1957

By J. J. Bodmer

Although the similarity between puzzolana, or trass, and blastfurnace slag, as seen by comparison of the analyses, is a well-known fact, blast-furnace slag has not been used commercially as a substitute for those cementing materials. The reason, the writer apprehends, lies in the fact that unless such slag is disintegrated or subdivided by rolls, the process must either be too costly, or the material is not in a fit and proper condition for the purpose. In order to produce a reliable slag cement, the slag must be ground together with the lime into an impalpable powder. The subdivided slag must, therefore, be perfectly dry, and, at the same time, friable. The stronger the hydraulic properties of the lime, the more reliable the slag cement will be, and practice has proved, that the slag from a gray-iron furnace gives the best results. The slag cement which has given the results shown in the annexed table, under pressure tests, was composed of six parts of slag, from a blast-furnace producing No. 3 foundry iron, and one part of lime, of medium hydraulic properties. The above-described class of cement bears storing as long as most Portland cements, and the cheapness of its production is self-evident.

By J. J. Bodmer

ALTHOUGH the similarity between puzzolana, or trass, and blast-furnace slag, as seen by comparison of the analyses, is a well-known fact, blast-furnace slag has not been used commercially as a substitute for those cementing materials. The reason, the writer apprehends, lies in the fact that unless such slag is disintegrated or subdivided by rolls, the process must either be too costly, or the material is not in a fit and proper condition for the purpose. In order to produce a reliable slag cement, the slag must be ground together with the lime into an impalpable powder. The subdivided slag must, therefore, be perfectly dry, and, at the same time, friable. The stronger the hydraulic properties of the lime, the more reliable the slag cement will be, and practice has proved, that the slag from a gray-iron furnace gives the best results. The slag cement which has given the results shown in the annexed table, under pressure tests, was composed of six parts of slag, from a blast-furnace producing No. 3 foundry iron, and one part of lime, of medium hydraulic properties. The above-described class of cement bears storing as long as most Portland cements, and the cheapness of its production is self-evident.

Jan 1, 1874

By James S. Browning

The Mineral Resources Institute and State Mine Experiment Station of the University of Alabama conducted Humphreys spiral tests on fine coal waste from nine preparation plants of Alabama strip mining operations to determine the feasibility of recovering low ash and sulfur fuel meeting steam coal specifications. The ash in the samples ranged from 9 - 5l%, and the total sulfur ranged from 0.4J- 2.39%. Continuous laboratory tests using a Humphreys spiral gave good recovery of the coal with excellent rejection of the ash and pyritic sulfur. Coal recoveries of 83.6 - 94.1% were achieved from the different samples. Ash content of the clean coal products fell within a range of 5 - 12.2%, with a total sulfur content of 0.62 and 1.10%. In quality, the products were comparable or superior to those now being shipped from the preparation plants.

Jan 1, 1980

By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,' was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951

By Philip Drinker

IN THE mining and metallurgical industries, numerous problems arise requiring determinations of solid and of liquid particles suspended in air. Frequently, these problems are of local interest and involve purely economic or operating difficulties; on the other hand, toxic effects from the inhalation or the ingestion of substances suspended in air may be a matter of concern. For checking up process improvements or for determining ventilation efficiencies in problems of this general nature, various methods have been proposed. Although simpler methods are often satisfactory, precipitation combines several desirable features that other methods lack. This paper is, therefore, devoted to a discussion of portable alternating-current precipitators applicable to the quantitative determination and microscopy of dusts, fumes, and smokes in air. Small particles suspended in gases, such as air, are referred to in the literature as aerosols or suspensoids. Of these terms, suspensoids appears to be preferable as being more nearly in keeping with words in everyday use. In problems involving air pollution by small, particles-by suspensoids-it is convenient to distinguish three broad classes based on the size, the degree of dispersion, and the method by which the particles become suspended in the air. Dusts.-Particles or aggregates of particles, 150 to 1 micron in diameter, that are thrown into the air by mechanical agencies are termed dusts. Examples are silica, talc, cement, organic dusts such as hard rubber, starch, and cocoa; flocculated fume and smoke products. Fumes.-Particles, 0.2 to 1 micron in diameter, formed from chemical or physicochemical reactions are known as fumes. Examples are ammonium chloride, lead and mercury, zinc and magnesium oxides, fogs, and acid mists.

Jan 3, 1925

By G. G. Biggar

A MATERIAL contribution to the success of our Armies in the field has been the portable pipe-line system. These are the words of Brigadier General R. F. Fowler, chief of the supply division of the War Department. The portable pipe line is one of the "secret weapons" the American forces employed in their swift advances through Tunisia, Sicily, and Italy. Constructed of a light steel so flexible it can be snaked around trees, it can be laid at a rate of ten to thirty miles daily right up to the fighting fronts. It has played a major role in supplying combat troops with products varying from petroleum to water.

Jan 1, 1943

By P. F. McIntyre

Electrolytic refining of lead was first carried out on a commercial scale at Trail, B. C., in 1903. The capacity at that time was small, and cell-changing operations were managed with chain block and monorail. Development up to 1922, utilizing crane installations and cell additions, attained a production of 100 tons per day. Successive additions from 1922 to 1926 further increased the rated capacity to 396 tons per day. Other improvements in metallurgical practice have gradually increased production, until for the year 1935 it was 448 tons per day. During the first five months of 1936, an average daily production of 504 tons was maintained without increasing the size of the plant. Lead Refinery Buildings.—The tank room and the lead-melting and casting equipment are housed in two buildings, which parallel each other and which for the greater part of their lengths are joined by a connecting aisle. All basements, walls, sumps and floors are of concrete. Where exposed to the electrolyte, the concrete has a protective coating of asphalt (220" melting point) over a coat of asphalt paint as a primer. Buildings erected before 1924 are of wood. More recent additions are made of structural steel with gunite siding. A brick building, adjoining the older section of the tank room, houses the slimes-treatment plant. The power house, containing motor generators, air compressors and rectifiers, is constructed of tile. Cell Construction.—The electrolytic cells are of reinforced concrete lined with asphalt. They are cast in pairs, the outside dimensions of a double cell being 113 in. long by 73 in. wide by 48 in. deep. The bottom is 6 in. thick and the sides, ends and center wall are 4 in. thick. A ledge 3 in. wide and 2½ in. deep is left along the top of the side walls to carry the insulators and bus bars. Reinforcing consists of ½-in. round iron rods. Cell inspection and repair work is done in conjunction with the cell-changing operations. The repair work necessary is usually confined to renewing chipped asphalt, unless a tank has been accidentally broken. Minor concrete repairs can be easily made in place. The broken concrete

Jan 1, 1937

By Galen Clevenger

THE losses of gold and silver occurring during the conversion of the precipitate, resulting from the cyanide process, into bullion may occur in two ways: first, there may be mechanical losses during the handling of the precipitate up to the time that it is charged into the melting furnace; and second, there may be losses after the precipitate reaches the melting furnace. Much of the loss during the handling of the pre-cipitate can be eliminated, and in fact, in modern plants this loss is known to be very small; particularly since preliminary acid treatment of the precipitate with the attendant extra operations has been abandoned in all but certain plants where gold predominates and this extra step is still deemed necessary. The losses in the melting furnace are from dusting and volatilization; losses in the furnace bottom and linings; floor sweepings; and slag and matte. The gold and silver in the: products which do not: go out of the flue are readily recoverable by standard methods, and while there may be considerable gold and silver tied up at times, the ultimate loss with careful "work should be small. The losses resulting from volatilization and dusting in connection with the melting of the silver slime from copper refineries have been determined by standard methods, and the possible recovery: definitely estab-lished through the installation and operation of electro-static precipitation units. This subject has not been thoroughly investigated in connection with the melting of`. cyanide precipitate; at least, there are no published accounts of such tests. Experiments have been made in the past to determine melting losses by weighing and assaying the precipitate, but this method gives results which are uncertain on account of the difficulty of accurately sampling and assaying cyanide precipitate. Attempts to ascertain these losses by bubbling a measured sample of the gas through cyanide solution or, other absorbent have likewise failed to give depend-able results.

Jan 1, 1922

lv. H. Blauvelt, Great Falls, Montana (communication to the Secretary): In his remarks on Mr. Stetefeldt's paper (Trans., xxiii., 587)) Mr. Goetz observes: " Trouble experienced with producers at Great Falls influenced me to try Taylor producers instead of those of Wellman. But recent reports show that the Wellman producers work better, besides coating nearly 50 per cent. less than Taylor producers of equal capacity. Indiana and Illinois coals cannot be used in the Taylor producers by reason of the large size and hardness of the clinkers which they form." I think that Mr. Goetz must have been misinformed regarding the work of this producer in Illinois. One of the large mauafacturing concerns in that State, the Illinois Zinc Company, situated at Peru, which uses a coal mined in the vicinity, tried one Taylor producer, some four years ago, in competition with those of an older type, which it had been using. As a result of this trial, the company has now thirteen Taylor producers, which have been in operation for about three years. A recent report from these works says that the Taylor producers have largely reduced the loss of coal through the grate, and have also improved the quality of the gas, as compared with that produced from the same coal in the producers of the older type. This Illinois coal is, perhaps, the worst in the country for making gas; since, besides containing from 20 to 40 per cent. of ash, it carries a large quantity of pyrites, so that the clinkers are large and extremely hard, and the capacity of the producer is most severely tested.

Jan 1, 1895

By R. K. Dann, L. W. Roberts, R. B. Benson

The mechanical properties of 300-series stainless steels were investigated in both high-pressure hydrogen and helium environments at ambient temperatures. An auslenitic steel which is unstable with respect to formation of strain-induced a (bee) and € (hcp) mar-tensile is embrittled when plastically strained in a hydrogen environment. A stable austenitic steel is not embriltled when tested under the same conditions. The presence of hydrogen causes embrittlement at the mar-lensitic structure and a definite change in the general fracture mode from a ductile to a quasicleavage type. The embrittled martensitic facets are surrounded by a more ductile type fracture which suggests that the presence of hydrogen initiates microcracks at the martensitic structure. If a steel is unstable with respecl to fortnation of strain induced martensile, plastic deformation in a hydrogen environment will produce rapid embrittlement of a notched specimen in comparison to an unnotched one. FERRITIC and martensitic steels can be embrittled by hydrogen that has been introduced into the alloys, either by thermal or cathodic charging prior to testing.1-5 However, conflicting reports exist as to whether austenitic steels that are stable or unstable with respect to formation of strain-induced martensite can be embrittled by hydrogen.8-12 A recent investigation has shown that cathodically-charged thin foils of a stable austenitic steel can be embrittled.13 An earlier investigation of a thermally charged 18-10 stainless steel revealed a significant decrease in the ductility only at the lowest test temperature of -78°C, although strain-induced bee martensite was shown to be present in one specimen tested at ambient temperatures.' When martensitic steels are tested in a hydrogen atmosphere, they are embrittled.'4-'7 It has been observed in this Laboratory that 304L steel, which is unstable with respect to formation of strain induced martensite, forms surface cracks when plastically strained in a high-pressure hydrogen environment. Work in progress elsewhere concurrent with this investigation has also established that 304L is embrittled when tested in a high-pressure hydrogen atmosphere." The objective of this investigation was to study the effect of a high-pressure hydrogen environment on the tensile properties of a stainless steel that contained strain-induced martensite (304L) and one that did not (310). EXPERIMENTAL TECHNIQUES Notched and unnotched cylindrical specimens were machined from 304L* and 310 rods that were heat- treated at 1000°C in argon for 1 hr followed by a water quench. The chemical analyses of these steels are given in Table I. The unnotched specimens had a reduced section diameter of 0.184 & 0.001 in., a gage length of 0.7 in., and were threaded with a 0.5-in.-diam. thread on each end. The notched specimens had a reduced section diameter of 0.260 * 0.001 in. and a 0.75-in. gage length, with a 30 pct 60 deg v-notch at the center. The notch had a maximum root radius of 0.002 in. The tensile bars were fractured in a hydrogen or helium atmosphere of 104 psi at ambient temperatures. The system used for mechanically testing the specimens is to be described in detail elsewhere.19 Several specimens of each type were tested in air using an Instron testing machine. The same yield strength and ultimate tensile strength were obtained in 104 psi helium with the above system as with the conventional testing machine. Magnetic analysis was employed to determine that there was a (bee) martensite in plastically deformed 304L and that it was not present in plastically deformed 310. The magnetic technique depended on allowing the material being studied to serve as the core between a primary and secondary coil. Thus, any change in the amount of magnetic material present between the annealed and plastically deformed steels will be indicated by corresponding changes in the induced voltage in the secondary circuit." The ratio of the output signal of a nonmagnetic stainless steel to a completely magnetic maraging steel was 2000 to I. Several unnotched 304L bars tested in hydrogen were analyzed for hydrogen by vacuum fusion analysis. There was an increase in the hydrogen content to approximately 2 ppm for the specimens tested in hydrogen, as compared to less than 1 ppm for the as-received material. Several thin sections cut from notched areas of 304L specimens tested in hydrogen and containing the fracture surface contained approximately 1.5 ppm H. The accuracy of these determinations was estimated to be ± 50 pct.

Jan 1, 1969