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By R. B. Snow

THIS paper describes a technique of polishing and etching specimens of open-hearth furnace slags or hearth aggregates for identification of the crystalline constituents-lime (CaO), tricalcium silicate (3CaO•SiO2), dicalcium silicate (2CaO-SiO2), monticellite (CaO•MgO-SiO2), or forsterite (2MgO•SiO2), with especial emphasis on the mineral merwinite (3CaO-MgO.2SiO2). With proper standardization, this identification does not require the use of the petrographic microscope. The composition of basic open-hearth slags and furnace bottoms falls, almost without exception, within systems containing CaO, MgO, "FeO," MnO and SiO2, in which the number of basic molecules so greatly exceeds the orthosilicate ratio (two molecules of base to one of silica) that free basic oxides, and combinations between them such as aluminates or ferrites, are present in cooled specimens. Orthosilicates of (CaO + MgO) are the most common in such specimens, since in nearly all cases, except premelt slags, the molecular ratio of (CaO + MgO) to SiO2 is more than 2 to r. When sufficient lime is available it combines with the silica to form dicalcium silicate (2CaO•SiO2), which contains little, if any, MgO, FeO or MnO in solid solution whereas the latter oxides combine to form the oxide solid solution known as periclase. If the lime present is insufficient to form dicalcium silicate (2CaO•SiO2) it combines with MgO to form either merwinite (3CaO•MgO.2SiO2) or monticellite (CaO-MgO•SiO2); these minerals take little if any FeO or MnO into solid solution and the remaining MgO, FeO and MnO combine as periclase. This generalization seems to be valid for basic slags and furnace bottoms, since minerals such as CaO-MnO•SiO2 and CaO-FeO-SiO2 are found only in slags in which the lime-silica ratio is less than 2 and are not observed in specimens from furnace bottoms. The identification of crystalline constituents in such materials, especially of fine crystals in the groundmass, is difficult under the petrographic microscope. They are often masked by their neighbors because of their small size in relation to the thickness of the thin section and because of the presence of opaque or colored constituents. The indices of retraction and the optical sign of the mineral are sometimes difficult to determine because of the small size or because of twinning or of inclusions within the crystal. Moreover, the positive identification of merwinite (3CaO•MgO.2SiO2) from its optical properties is usually difficult in the presence of dicalcium silicate (2CaO•SiO2). CaO, MgO, 3CaO•SiO2 and 2CaO•SiO2 in open-hearth slags have been identified for a number of years in the U.S. Steel Corporation Laboratory by the usual

Jan 1, 1947

By Reinhardt Schuhmann JR

Metallurgical Engineering Volume I, by Reinhardt Schuhmann, Jr. Addison-Wesley Press. $7.50, 390 pp., 1952. -This first volume, engineering principles, of a two volume work, is intended by the author to meet a need for reorganization of instruction in extractive metallurgy. Its three main objectives are to organize the subject matter according to basic principles and unit processes; to integrate the underlying science of physical chemistry with metallurgical engineering; and to put greater emphasis on analysis and quantitative solution of engineering problems. Vol. I deals with unit processes, stoichiometry, thermodynamics, fuels, fluid flow, heat transfer, pyrometallurgical systems and refractories. Vol. II will take up the individual unit processes. Initiation and Growth of Explosion in Liquids and Solids, by F. P. Bowden and A. D. Yoffe. Cambridge University Press. $4.50, 104 pp., 1952.-The book is a study of decomposition by impact and by friction of explosive substances and deals mainly with the work of the authors and their collaborators. Research is still in progress but results thus far indicate that the mechanism of initiation is relatively simple. Findings are thoroughly discussed, and the latter part of the monograph describes the way in which a small nucleus of decomposition can grow into a large scale explosion.

Jan 1, 1952

By T. B. Massalski, Horace Pops

The occurrence and the temperature dependence of the athermal martensitic transformation in bcc Cu-Zn ß-phase alloys have been studied by cold-state microscopy, differential thermal analysis, and electrical -resistivity measurements. CinenzatograpJzic studies have shown that in the majority of alloys the transformation occurs in two stages. A thermoelastic phase, having a 'needlelike" uppearance, forms initially at the MS temperature and grows relatively slowly, chiefly in the edge (lengthwise) direction. With further cooling, an additional martensitic phase forms in rapid bursts at a lower temperature, MB, Both martensitic phases appear to have the same cry stallographic habit hut their modes of formation and growth are different. For the composition range studied, between 38.55 and 41.49 wt pct Zn, the habit planes determined are close to the (2.17 ,12) plane of the matrix, in general agreement with the prediction of the phenomenological theory of martensite formation. Thermal cycling through the MB temperature produces permanent plastic deformation in the 0 matrix and gradutally eliminates the typical burst phenomena. Thermal cycling only through the MS temperature produces no noticeable deformation effects. THE bcc Cu-Zn ß-phase alloys tend to become unstable at low temperatures and undergo a martensitic transformation,'-3 but the details of the transformation have not been completely determined. Following earlier metal log raphic and X-ray work1 Tichener and ever' determined by means of electrical-resistivity measurements the temperature range of the martensite transformation during continuous cooling. The transformation temperature was found to decrease with increasing zinc content, becoming about -130°C for an alloy containing 40.04 wt pct Zn. Hull and Garwood3 made a metallo-graphic study of Cu-Zn 0 brasses at temperatures down to -160°C, and determined the habit plane of the transformation product for an alloy containing 38.88 wt pct Zn. No metallographic studies below liquid-nitrogen temperatures have been reported. The martensitic transformation in ß-brass alloys can also be induced by deformation.1,4 The MD temperature corresponding to the appearance of the strain-induced martensite is some 300°C higher than that observed without strain, and hence the transformation can be strain-induced in alloys containing a higher percentage of zinc. Massalski and Barrett4 found that alloys containing as much as 51.89 wt pct Zn could be transformed into a faulted hcp structure by cold working at liquid-helium temperature. Because the details of the MS temperature and morphology reported in the literature are somewhat incomplete, a further study has been made of some of the above features. A design of a cryogenic stage for optical metallography5 has permitted the examination of specimens at temperatures down to 4.2oK, and the use of a cinecamera has permitted a study of the morphology on cooling and heating. The particular aim of the present work was to examine the transformation temperatures, the habit planes, and the growth morphology over a wide composition range in the ß-phase field. The effect of thermal cycling upon the subsequent transformation was also examined.

Jan 1, 1964

By E. P. Klier

The work of Klier and Lyman1 on the bainite reaction has led to the full description of this reaction for medium-carbon low-alloy steels. Certain experimental data reported by Klier and Lyman appear, however, to be improbable of obtaining in very high-carbon steels. The study herein reported consists of an analysis of the transformation characteristics of a 3 per cent chromium, I per cent carbon steel by means of X-ray and metallographic methods. From the results obtained it is concluded that the bainite reaction in this steel is more complicated than that reported by Klier and Lyman for the low-carbon low-alloy steels. Henever, the mechanism of bainite formation in this steel appears to be essentially the same as proposed for the low-carbon low-alloy steels with the modification that the first volumes to transform are carbon-rich rather than carbon-poor. Experimental Procedure The analysis of the steel studied was: Cr, 2.89; C, 1.02; Mn, 0.33; Si, o.35; S, 0.012; P, 0.020. The stock was received from the Carpenter Steel Co. in rolled bars. Specimen Preparation Specimens were austenitized at 1200°C. (2192°F.) for 25 min. in purified nitrogen. The resultant A.S.T.M. austenite grain size was 0-1. Isothermal transformation was allowed by quenching the specimens into liquid metal baths controlled to 5°C. at 540°C. (1004°F.) and above, and to 2°C. at 490°C. (914°f.) and below. Following the desired degree of transformation all specimens were water quenched. Metallographic Examination Specimens 1/4 in. round by 1/4 in. were used for nietallographic examination. Etch-ants used were Vilella's reagent (I gram picric acid, 10 ml. hydrochloric acid to make 100 ml. ethyl alcohol solution) and alkalinc sodium picratc (electrolytic). Vilella's reagent was effective in revealing all microconstitucnts, while the alkaline sodium picrate developed the carbon-rich structures or carbides only. X-ray Examination Two X-ray techniques were used—the Debye-Scherrer method and a back-reflection method. 'The small specimens necessary for the Debye-Scherrer method were austenitized and then allowed to transform, or were cut from the larger metallographic specimens. The metallographic specimens were used for the back-reflection X-ray analysis. When it was desirable to determine the structure of the carbide present, sliver specimens were electrolytically etched to develop a carbide coating, then were exposed in the cameras. This technique was frequently necessary to allow positive identification of the carbide.

Jan 1, 1945

By H. Bartholomew, L. Bernstein

Experirmental bonds of Ag-In SLID to gold, copper, nickel, Kovar, Dumet, nickel-plated molybdenum, ALL-Pt vrzetallizing on ceramic, and nickel-plated Mo-Ti metallizing on Al2O3 ceramic have been made and exalnined. Metallographic taper sections were made of all bonds for Phase identification. In addition, failuve temperatltres were determined for bonds heated undev shear load. Sowe bonds were subjected to electvon-probe microanalysis. The ternary SLID system Ag-In-Sn was similarly evaluated. Plwtonticrogaphs and electron-probe data are discussed and related to over-all phase diagrams , diffusion effects, and wetting properties of the liquid. The rates of diffusion andor compound formation of gold, silver, and copper in indium and In-Sn liquids are found to descend in that order, as measured by the relatzve thickness of phase layers in the interfaces of bonds made at 200to 400°C. It is concluded that the SLID process enables one to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures, and meet most requirements for application in interconnection, silicon bonding, or hermetic sealing of electronic devices. In a previous publication by one of the authors, the theory and principle of SLID bonding in simple binary systems was discussed. SLID bonding can be defined as a joining process using a preform with a laminated structure: a low-melting material clad on a high-melting core. During the bonding cycle a metallurgical transformation occurs such that the resultant structure can withstand, without reliquefying, temperatures higher than those at which the bond was made. The phases present in the joint interface region are high-melting compounds or, if equilibrium is reached, solid solution. Properties will depend on the phases present, ultimately approaching those of the solid substrate core of the SLID preform. The high-temperature strength of bonds made in these systems was correlated to phase identification in the interfacial bond regions from metallographic cross sections and electron-probe X-ray microanalysis data. When complex electronic components are assembled, multiphase systems result at the interfaces of bond regions. In these ternary and higher-order systems very little diffusion and phase-diagram data is available with which to predict the nature of the interfacia1 region that will result from conventional fabrication processes and subsequent field use of the component. Clarke and Rhines did early work in the field using the Al-Mg-Zn system as a vehicle. Guy and co-workers studied a portion of the Cu-Zn-Ni system and some mathematical4 and general5 aspects of multiphase diffusion. irkald' and coworkerse recently studied diffusion in the Cu-Zn-Sn system. No diffusion studies have been made on ternary systems directly applicable to this investigation but some phase diagrams are available: g-u-n, u-i-n, and CU-i-n. I) DESCRIPTION AND EXPERIMENTAL PROCEDURE The elements Au, Ag, Cu, Ni, In, and Sn are found in alloy systems commonly used in fabricating and assembling electronic components. Reference to the appropriate phase diagrams9 and the previous publication will indicate that the binary systems of any of the two low-melting elements, indium and tin, with any one of the other four higher-melting elements are capable of producing SLID bonds. It is not unreasonable to assume that any ternary or higher-order alloy system containing at least one of the elements gold, silver, copper, or nickel and one or both of the elements indium and tin could be used to produce bonds which are stable at high temperatures, after having been fabricated at low temperatures. Indeed, the liquidus contours and isothermal sections of those phase diagrams available7 do so indicate. The parameters affecting the bond and the equipment used in evaluating the bond were described in an earlier paper.' The current investigation used the

Jan 1, 1967

By B. R. Hollebone

The chemical action of molten anhydrous pyridinium chloride (pyridine hydrochloride) on oxy salts and ores of some Group IV and V metals are discussed-in particular zirconium, hafnium, niobium (columbium) , and tantalum. Laboratory-scale experiments are described whose results suggest that this reaction might provide a practicable means of converting ores of these metals to the anhydrous metal chlorides. Experimental results are given which provide some insight into the nature of the reactions and some of the compounds which could be present at intermediate stages. The treatment of ores of the more refractory metals is difficult and expensive and often demands the use of gaseous chlorine, hydrogen fluoride, or other reagents which are, if nothing else, expensive and dangerous to use. This situation is, of course, due to the strong metal-oxygen affinity resulting from the high charge and the small size of the metal ion which combine to produce such high lattice energy in the metal oxide as to defeat standard reduction methods. Thus, the characteristic of these metals which leads to one of their most important properties—corrosion resistance—is the main hurdle in obtaining the metal. Many common methods' for treating ores of zirconium and niobium (columbium), for example, proceed as directly as possible to the preparation of anhydrous halides. These halides are purified by now standard processes of solvent extraction, fractional distillation, and so on. This paper reports on preliminary stages in the development of a method of treating these ores—particularly of niobium—so as to prepare the anhydrous, volatile halides by the use of chemical reagents which are much more easily handled than those used at present. CHEMICAL PRINCIPLES The solvent action of aminium halides has been referred to periodically in the literature over several decades. The chemistry of pyridinium chloride has been discussed particularly by Audreith2 and Starke.3 However, since this is not familiar chemistry in its nonaqueous setting, it is perhaps well to point out some general metallurgical principles and applications. One can use, as point of departure, the fact that HC1 dissolved in pyridine is an acid very much the same as aqueous HC1. It thus gives essentially all the reactions of the HC1 with which we are familiar. However, when the ratio of HC1:pyridine reaches 1:l (a ratio far higher than is possible with H2O) the solution becomes solid C5F5NHC1, pyridinium chloride.* Inter- estingly, the acidic properties of HC1 persist in this medium, although they are manifest only in the molten state of the compound. Some typical reactions of divalent metal compounds which we have carried out in our laboratories are the following: 2PyHCl + Zn — (ZnCl2) + H2 + 2Py 2PyHCl + MnO — (MnCl2) + H2O + 2Py 2PyHCl + CuS — (CuCl2) + H2S + 2Py 2PyHCl + CaCO3 — (CaCl2) + H2O + CO2 + 2Py In these equations, the parentheses indicate a solvated compound which in water would be predominantly a hydra ted cation but which in molten PyHCl will more likely be a complex chloro-anion of the type MC14-. Some important physical properties of pyridinium chloride (PyHCl) are given in Table I. One sees from the data in Table I that at the temperature of molten pyridinium chloride both water and pyridine will boil away. Thus the system will be kept anhydrous. For this reason the reaction 2NbCl5 + 5H2O— Nb2O5 + 10HC1 has no counterpart in molten PyHCl. Instead, the chloride is made even more stable by the formation of a hexachloro complex: Nb2O5 + 12PyHC1 — 2PyHNbC16 + 5H2O + 10Py One interesting property of these complexes is their thermal instability which for the case of niobium can be illustrated as PyHNbCl6 — PyHCl + NbCl5 With a view to possible use of this chemistry in ore treatment, we have attempted to dissolve Pyrochlore (essentially FeO - Nb2O5) and recover the NbC15 from it.

Jan 1, 1968

By S. Y. Ogawa

The effects of sulfur (up to 0.1 pet) on the deformation and fracture characteristics of iron, in cast form, were studied at strain rates up to 100 pct pcr sec and at temperatures of 1600o to -3300 oF. The effects of oxygen and manganese additions on the behavior of Fe-S alloys were studied under comparable test conditions. Brittle fracture characteristics, evident at all strain rates, resulted from the presence of the liquid iron sulfide phase at grain boundaries. Ductility could be restored in three ways: solution of the sulfide in solid y iron at higher temperatures, spheroid-zzation of the liquid sulfide, and increase. in the melting point ot the sulfide. THE literature shows that most previous studies of deformation and fracture at hot working temperatures have been based on measurements of energy absorption, reduction of height in forging upset tests, torsion tests of bar or wire samples, and so forth,' but that relatively few tension tests have been used at high temperatures and strain rates. The present work was initiated to study the ef- fects of temperature, strain rate, composition, and structure on the deformation and fracture characteristics of iron, utilizing cast specimens tested in tension. As in a previous study,' strain rates up to 100 pct per sec were chosen for the temperature range 1600° to 2400° to provide data which might be useful in the interpretation of the deformation and fracture behavior of steels under hot working conditions. The previous work was with Fe-P solid solution al10ys;2 this work is concerned with Fe-S alloys, and with the effects of oxygen and manganese additions. MATERIALS AND PROCEDURE Cast tes! specimens were employed throughout, since most of the difficulty during hot working occurs in the initial breakdown of the ingot. Alloy Systems. Ten 25 lb. heats containing sulphur were prepared. Of these, three had manganese additions, and two had oxygen additions. The sulfur content varied from 0.023 to 0.10 pct. Manganese contents were intended to be ten to twenty times the sulfur content of the particular alloy. Oxygen, being more difficult to control in small melts, was varied by the amount of solid deoxidizer added, but poor control of the oxygen content was experienced in most instances. Table I shows the chemical analyses of the heats. Melting and Casting. Electrolytic-iron chips were melted by high frequency induction in a prefired, clay-graphite crucible lined with rammed magnesite.

Jan 1, 1962

By Tell Ertl

The term oil shale is defined. Foreign oil-shale developments are outlined briefly. The richest and most extensive oil-shale deposits in the United States lie in western Colorado. The Bureau of Mines is opening two adjacent areas for underground mining. in western Colorado. From the first area the oil shale is mined selectively as required by the retorting plant. The second area is being developed as a unit of a full scale oil-shale mine to ascertain the most practical methods of mining oil shale and to determine costs. In both of these mining areas, research will be carried on to develop new and improved practices for mining oil shale. Introduction Oil shale is a sedimentary rock containing a solid mineraloid of indefinite composition known as kerogen. On heating oil shale, the kerogen undergoes thermal decomposition and some of the vapor products of the decomposition can be condensed as shale oil. Oil from shale can be a major source of liquid fuels since extensive deposits of oil shale are known to exist throughout the world. The United States considers the establishment of an oil-shale industry only when doubt exists of the adequacy of the domestic supply of crude petroleum. On the other hand, oil shale is not strange to foreign oil men. The industry is an old one in other parts of the world. The French industry has been in existence since 1838, the Scottish since 1859, the Australian since 1860, the Estonian and Swedish The since World War 1, and the Manchurian industry since 1929. The most highly exploited oil-shale deposits are the Carboniferous shales of Scotland. About 20 seams ranging from 4 to I2 ft in thickness are worked. The yield during recent years in scotland has been 18 to 25 gal of shale oil per ton, from 3&"30'000 tons per year' The French and Swedish oil-shale deposits are of lower grade than the Scottish. The Estonian oil-shale deposits are 7 ft thick, and the oil yield averages 50 gal per ton. Over 1,000,-ooo tons are mined each year, half of which is used directly as fuel to substitute for coal and the other half is used for the production of oil. Immense deposits of oil shale that will yield 10 to 15 gal per ton exist in Germany. Because of the impending loss of the Rumanian and Polish oil fields and the bombing of synthetic liquid fuel plants, the Nazis in 1943 started a large-scale oil-shale program in Germany. By V-E Day, it is said, oil-shale production had reached the rate of 2500 tons per day and rapid expansion of the industry was imminent. Australian oil shale, known as torbanite, occurs in beds 2 to 6 ft thick. It is of a very high grade and on retorting yields 80 to 160 gal per ton. The oil-shale industry of Manchuria was the largest in the world during the past decade. The well-known Fushun coal deposit in Manchuria has an overburden of 500 million tons of oil shale about 450 ft thick that will yield 10 to 15 gal of shale oil per ton. The oil shale is

Jan 1, 1949

By N. O. Johnson, R. A. Westin

Polychlorinated biphenyls were the basis of non-flammable askarel dielectric liquids wed in electrical equipment made between 1929 and 1978. Although PCBs were widely used in mine electrical equipment, the toxicity and environmental persistence of this chemical led Congress to ban its manufacture and use. Bureau of Mines Information Circular 8838 summarizes the regulations imposed by the EPA on the use and disposal of PCBs, and describes the limitations of available substitutes. Recent changes in the regulations will impose additional requirements on the use of PCBs by the mining industry. This paper is an update of the material presented in the Bureau of Mines information circular.

Jan 1, 1983

By B. B. Wood, M. J. Rzasa, E. W. Hough

An apparatus for the determination of fluid-fluid interfacial tension by the pendant drop method has been constructed. The apparatus is refined beyond those previously described in that the samples are introduced into an evacuated windowed cell without contacting air or mercury. Interfacial tension data are reported for the water-methane system between 74 and 280°F and 15 and 15,000 psi. The variation of wettability of the stainless-steel dropper tip with pressure and temperature was observed incidentally to the measurements. INTRODUCTION The most refined previous apparatus --for the determination of fluid-fluid interfacial tension at reservoir conditions was built by Hauser and Michaels.' These authors used the pendant drop method, previously investigated by Andreas, Hauser, and Tucker.' Recently, Fordham3 has made the pendant drop method an absolute one by numerical integration of the differential equation of drop shape. It is necessary to know the difference in density of the two fluids and the acceleration due to gravity in order to evaluate the interfacial tension from measurements of drop dimensions. Contact angle is not involved in the measurements by this method. Some precise tests of the method have been made at atmospheric pressure and 77°F by Douglas," who found agreement with established values to within about 0.1 per cent for water and air, cyclohexane and air, benzene and air, and benzene and water. No values of interfacial tension from the recent pendant drop apparatusJ have been published by Hauser and Michaels. However, values for the water-benzene and water-decane systems are given in Michaels' thesis5 or Dressures from 15 .to 10,000 psi and temperatures from 73 to 268ºF. Some determinations on gas-oil and gas-water systems in the range of 15 to 4,000 psi and 78 to 178°F have been made by Hozott,' by the drop-volume method. The capillary rise method has been used to investigate the interfacial tension in gas-oil systems at 88°F to several thousand psi by Swartz.7 Other determinations in gas-oil systems at pressures under 1,000 psia have been made by Jones: and Beecher and Parkhurst.9 The scarcity of data for pressures above 5.000 psi is apparent. APPARATUS An assembly drawing of the working section of the interfacial tenqion apparatus is given in Fig. 2. 'The endanant drop (A) is housed in a pressure chamber having glass windows (B). An agitator (6) is provided. The metal parts of the apparatus coming into contact with the sample are made of AISI: Type 316 steel. Drain grooves are provided around the whdows so that the sample in contact with the O-rings is not returned to the working section when the pressure is reduced. A schematic arrangement of the apparatus is given in Fig. 3. The working section containing the pendant drop (A) is filled by samples from bombs (B) with the aid of the vacuum system (C). The O-ring sealed pistons (D) used to separate the sample from the hydraulic fluid are shown together with the pressure production and measurement system (E). A front view of the apparatus is shown in Fig. 1. Most of the hydraulic system is at the top of the panel. The pump and displacement piston are at the lower right. The Variacs for the air bath heaters. the camera. and the vacuum gauge are a1so visible on the panel. The working section together with a window closure and a drop-forming tip closure are shown in Fig. 9. The carbon arc light source with filter is visible in the upper part of the picture. Two sides of the air bath with the impeller and a part of the convection shield can also be seen. The assembled air bath is shown in Fig. 10.

Jan 1, 1951

By E. W. Hough, B. B. Wood, M. J. Rzasa

An apparatus for the determination of fluid-fluid interfacial tension by the pendant drop method has been constructed. The apparatus is refined beyond those previously described in that the samples are introduced into an evacuated windowed cell without contacting air or mercury. Interfacial tension data are reported for the water-methane system between 74 and 280°F and 15 and 15,000 psi. The variation of wettability of the stainless-steel dropper tip with pressure and temperature was observed incidentally to the measurements. INTRODUCTION The most refined previous apparatus --for the determination of fluid-fluid interfacial tension at reservoir conditions was built by Hauser and Michaels.' These authors used the pendant drop method, previously investigated by Andreas, Hauser, and Tucker.' Recently, Fordham3 has made the pendant drop method an absolute one by numerical integration of the differential equation of drop shape. It is necessary to know the difference in density of the two fluids and the acceleration due to gravity in order to evaluate the interfacial tension from measurements of drop dimensions. Contact angle is not involved in the measurements by this method. Some precise tests of the method have been made at atmospheric pressure and 77°F by Douglas," who found agreement with established values to within about 0.1 per cent for water and air, cyclohexane and air, benzene and air, and benzene and water. No values of interfacial tension from the recent pendant drop apparatusJ have been published by Hauser and Michaels. However, values for the water-benzene and water-decane systems are given in Michaels' thesis5 or Dressures from 15 .to 10,000 psi and temperatures from 73 to 268ºF. Some determinations on gas-oil and gas-water systems in the range of 15 to 4,000 psi and 78 to 178°F have been made by Hozott,' by the drop-volume method. The capillary rise method has been used to investigate the interfacial tension in gas-oil systems at 88°F to several thousand psi by Swartz.7 Other determinations in gas-oil systems at pressures under 1,000 psia have been made by Jones: and Beecher and Parkhurst.9 The scarcity of data for pressures above 5.000 psi is apparent. APPARATUS An assembly drawing of the working section of the interfacial tenqion apparatus is given in Fig. 2. 'The endanant drop (A) is housed in a pressure chamber having glass windows (B). An agitator (6) is provided. The metal parts of the apparatus coming into contact with the sample are made of AISI: Type 316 steel. Drain grooves are provided around the whdows so that the sample in contact with the O-rings is not returned to the working section when the pressure is reduced. A schematic arrangement of the apparatus is given in Fig. 3. The working section containing the pendant drop (A) is filled by samples from bombs (B) with the aid of the vacuum system (C). The O-ring sealed pistons (D) used to separate the sample from the hydraulic fluid are shown together with the pressure production and measurement system (E). A front view of the apparatus is shown in Fig. 1. Most of the hydraulic system is at the top of the panel. The pump and displacement piston are at the lower right. The Variacs for the air bath heaters. the camera. and the vacuum gauge are a1so visible on the panel. The working section together with a window closure and a drop-forming tip closure are shown in Fig. 9. The carbon arc light source with filter is visible in the upper part of the picture. Two sides of the air bath with the impeller and a part of the convection shield can also be seen. The assembled air bath is shown in Fig. 10.

Jan 1, 1951

By R. S. French

The purpose of this paper is to present data that have been obtained during the past two years concerning the effects of prior cold-work and temperature and time of anneal upon the recrystallization and grain growth of 70-30 cartridge brass. It was desirable to study certain of these phases so that an accurate picture of the principles of the subject could be shown. The work is not intended to provide explicit annealing data, but to provide material examples that may help to clarify analogous problems concerning this alloy. Specifications often set limitations upon the grain size of annealed materials because of the importance of grain size upon subsequent manufacturing operations. It was, therefore, worth while to study the variables that affect the recrystallized grain size of this material. C. H. Mathewson and A. Phillips,l W. R, Webster,2 and others have presented annealing characteristic curves of this alloy. A recent typical curve presented by R. S. Pratt3 is shown in Fig. I. The tensile properties and grain sizes are shown as functions of the annealing temperature. Such curves serve as a useful guide in determining the physical properties of annealed material, but as they are made generally under carefully controlled laboratory conditions they do not indicate the performance of metal annealed in a mill muffle, where such conditions as amounts of metal, heating time and temperature may differ. Study of the effect of time and temperature upon grain growth and subscquent recrystallization was made with a coil of metal having the following analysis: 70.04 per cent copper; 0.007 lead; 0.007 iron; 0.00 tin; 0.00 silicon; 0.001 nickel; 0.000 phosphorus; balance zinc. The sample coil was obtained from metal that had been rerolled from hot-rolled mill stock, and was received at 0.228-in. gauge, soft, with a grain size of 0.125 mm. This material was then rolled 43.5 per cent to 0.129-in. gauge and annealed to a 0.053-mm. grain size. In this condition, samples were cut and used in all of the experimental work reported in this paper. Time The first study was of crystal growth at a constant temperature over a moderate length of time. Material was cut from the stock coil at 0.129-in. size and rolled 75 per , cent hard to 0.032-in. gauge. From this piece small samples were cut M by 2 in., suitable for grain-size determina.tions. Twelve samples were placed in an electric furnace uniformly across the width, approximately an inch from the floor. A thermocouple was wired to the center sample, so that the approximate metal temperature could be followed. At various

Jan 1, 1944

By R. S. French

The purpose of this paper is to present data that have been obtained during the past two years concerning the effects of prior cold-work and temperature and time of anneal upon the recrystallization and grain growth of 70-30 cartridge brass. It was desirable to study certain of these phases so that an accurate picture of the principles of the subject could be shown. The work is not intended to provide explicit annealing data, but to provide material examples that may help to clarify analogous problems concerning this alloy. Specifications often set limitations upon the grain size of annealed materials because of the importance of grain size upon subsequent manufacturing operations. It was, therefore, worth while to study the variables that affect the recrystallized grain size of this material. C. H. Mathewson and A. Phillips,l W. R, Webster,2 and others have presented annealing characteristic curves of this alloy. A recent typical curve presented by R. S. Pratt3 is shown in Fig. I. The tensile properties and grain sizes are shown as functions of the annealing temperature. Such curves serve as a useful guide in determining the physical properties of annealed material, but as they are made generally under carefully controlled laboratory conditions they do not indicate the performance of metal annealed in a mill muffle, where such conditions as amounts of metal, heating time and temperature may differ. Study of the effect of time and temperature upon grain growth and subscquent recrystallization was made with a coil of metal having the following analysis: 70.04 per cent copper; 0.007 lead; 0.007 iron; 0.00 tin; 0.00 silicon; 0.001 nickel; 0.000 phosphorus; balance zinc. The sample coil was obtained from metal that had been rerolled from hot-rolled mill stock, and was received at 0.228-in. gauge, soft, with a grain size of 0.125 mm. This material was then rolled 43.5 per cent to 0.129-in. gauge and annealed to a 0.053-mm. grain size. In this condition, samples were cut and used in all of the experimental work reported in this paper. Time The first study was of crystal growth at a constant temperature over a moderate length of time. Material was cut from the stock coil at 0.129-in. size and rolled 75 per , cent hard to 0.032-in. gauge. From this piece small samples were cut M by 2 in., suitable for grain-size determina.tions. Twelve samples were placed in an electric furnace uniformly across the width, approximately an inch from the floor. A thermocouple was wired to the center sample, so that the approximate metal temperature could be followed. At various

Jan 1, 1944

By R. J. Stevens

THE Roan Antelope Smelter commenced operations in October, 1931. As originally designed, its equipment consisted of one reverberatory furnace, 120 X 25 ft, two Peirce-Smith converters 12 X 20 ft, and one straight line casting machine. Since that time the following additions have been made: One reverberatory furnace 120 ft X 28 ft (1934) One reverberatory furnace 95 ft X 28 ft (1943) Two 12 X 20 ft Peirce-Smith converters (1934 and 1938) One 13 X 30 ft holding furnace 6 (1938) One straight line casting machine and 2 ladle tilting quadrants (1934) The metallurgy of the smelting process is comparatively simple. However, there are several features of operation which are uncommon to most copper smelters: (1) The high grade of concentrate treated; this has always been about 50 pct copper. (2) The high flux burden on the charge. This is necessary because of the deficiency of bases'in the concentrate and the high alumina content of the concentrate. (3) The frequent necessity of adding coal to the furnace charge to control the matte grade. (4) The high grade of matte produced. This has led' to unusual converter problems. From the commencement of operations, the ore mined has come from the Roan Basin orebody. The concentrate produced from this ore consists mainly of chalcocite and shale with small proportions of other copper minerals. As mining operations extend to the Roan Extension orebody, the proportions of bornite and chalcopyrite in the concentrate will increase with a corresponding decrease in the copper content of the concentrate. Because of the concentrate grade the capacity of the reverberatory . furnaces in terms of tons of copper produced per ton of coal burned is high.. This ratio is usually over 2.2, and on especially favourable runs has reached 2.6. Reference to Table , shows that the iron content of the concentrate is unusually low. Only part of this iron is available for slag formation, the balance going to the matte. To make up this deficiency in bases, limerock is added to the furnace charge. This flux ensures a slag that is of the correct silicate degree, is sufficiently fluid, of low specific gravity, and it counteracts the thickening effect of the alumina present. An ample supply of flux is obtainable from Ndola, 2 2 miles distant by rail. Although the reverberatory slag has a high copper content, the slag fall is low and the copper loss in the slag now rarely exceeds 1.0 pct of the total copper charged. The blister copper shipped is of such purity that only one fire refining operation has been necessary to produce a wirebar with properties comparable to electrolytic copper. Bismuth has always been the most troublesome impurity and consequently the problem of its control in the finished product has been of prime importance. Practically none is removed in the reverberatory furnace. The bulk of the elimina-

Jan 1, 1947

By H. L. Teicliman, E. M. Sipprelle

ENACTMENT of Public Law 290 by the 78th Congress authorized the U. S. Department of the Interior, Bureau of Mines, to conduct an experimental program to develop the technology for obtaining oil from oil shale. In adopting and later extending this legislation, the Congress recognized the impending necessity of supplementing ground petroleum reserves with synthetic fuels. Under the provisions of this legislation, the Bureau of Mines, among other things, was charged with the responsibility of developing mining techniques, methods, and equipment for mining the oil shales of the Green River formation of Colorado, Utah, and Wyoming.

Jan 1, 1950

By L. W. McKeehan, W. C. Elmore

THE magnetic powder method, long used for roughly mapping magnetic fields, has recently been refined 1,2 for investigating the microscopic variations in the surface magnetization of ferromagnetic crystals. Bitter' first discovered regular powder patterns connected with the crystal structure of such specimens. Several other investigators3 have used Bitter's original technique, with slight modifications, to study the variation of the patterns with variations in the magnetizing field applied parallel to the surface, and their dependence upon the state of strain, of polish and of crystal cut. All of the explanations of these patterns on metallic ferromagnetics have been couched in general terms. In a preliminary report we have described an improvement in the powder technique which led us to the discovery of a new effect throwing considerable light on the magnetic secondary structure of alpha iron4 and of nickel' single crystals. We now report additional evidence confirming the existence and stability of a magnetic block secondary structure. SPECIMENS The following list describes the specimens used in the present investigation. DESIGNATION DESCRIPTION A1 Silicon ferrite furnished to us by Dr. W. E. Ruder, of the General Electric Co., for which he gave the following typical analysis: C, 0.05; P, 0.038; 5, 0.026; Mn, 0.15; Si, 3.24. Disk, 0.60 cm. diameter, about 0.05 cm. thick.

Jan 1, 1935

By Lawrence B. Wright

The Republic district, Washington, is of new interest because of the discovery of new gold-silver ore within a unique structural pattern. The camp was revived in 1937 fol1owing installation of a plant to treat low-grade disseminated ore at Knob Hill and further stimulation followed discovery of "cross vein" breccia ores in 1939. Previous writers 1-2 ascribed the quartz veins to a latite porphyry stock, but are in disagreement as to its precise location and extent. This study leads to the conclusion that the ores have a more profound parentage linked to a broad system of thrust faults and folds, the mechanical origin of which is related to a southward trending (Sanpoil) syncline connecting with the Lewis and Clark zone of shift described by Billingsley and Locke3 in 1939. The Republic anticliue and a cross anticline recumbent against Cretaceous granodiorite. and involving some 4000 ft of Eocene andesite flows and early Miocene lake beds, localize the ores, mainly along the east flank, in a series of openings simulating drag folds and steeper than the folded flows. These broad structural features no doubt reach deeply into the basement rocks, where at appropriate crossings and junctions it is suggested that heat effects gave rise to ore-making materials, including, in this instance, intrusive breccias that later were mineralized, and comprising the broader bodies of new ores. The breccia ore is seen crosscutting the earlier narrow quartz veins with a welding of the two at junction areas by a second surge of ore minerals. The ore mined and developed since 1937 equals district production from 1896 to 1937 The ores are typified by cherty quartz, adularia and some barite, with fine pyrite and marcasite, polybasite, pyrargyrite, tetrahedrite and gold. Selenium is present, possibly with gold, as a normal selenide. The disseminated ores, as well as the vein and breccia ores, are localized principally in one 500-ft flow (Knob Hill andesite), which has been traced around the crest of the low northward-plunging Republic anticline. The gold-silver ratio in the earlier narrow veins is about I to 4 and in the disseminated and breccia ores, I to 7. The latter higher silver ratio is deemed to reflect the character of the second surge of mineralization. Sills and dikes of the Columbia River (Miocene) basalt cut the folded structure and ore, thus placing the mineralization in the middle Miocene. Introduction The Republic district of north central Washington is of new interest because of the discovery, development and extraction of new gold-silver ore; also, because of a unique local structural pattern believed to be integral with the broader tectonic mechanism of the continental framework. This district had 40 years of modest rating following its discovery in 1896. Its narrow ore bodies, complex mineralogy. and early inadequate metallurgy, together with the apparent bottoming of ore near 1000 ft, limited production to 300,000 oz of gold and 1,000,000 oz silver between 1897 and 1914. The camp was then reduced to lease Life until 1937, when the gold price increase of 1933 to $35 per ounce

Jan 1, 1949

By Lawrence B. Wright

The Republic district, Washington, is of new interest because of the discovery of new gold-silver ore within a unique structural pattern. The camp was revived in 1937 fol1owing installation of a plant to treat low-grade disseminated ore at Knob Hill and further stimulation followed discovery of "cross vein" breccia ores in 1939. Previous writers 1-2 ascribed the quartz veins to a latite porphyry stock, but are in disagreement as to its precise location and extent. This study leads to the conclusion that the ores have a more profound parentage linked to a broad system of thrust faults and folds, the mechanical origin of which is related to a southward trending (Sanpoil) syncline connecting with the Lewis and Clark zone of shift described by Billingsley and Locke3 in 1939. The Republic anticliue and a cross anticline recumbent against Cretaceous granodiorite. and involving some 4000 ft of Eocene andesite flows and early Miocene lake beds, localize the ores, mainly along the east flank, in a series of openings simulating drag folds and steeper than the folded flows. These broad structural features no doubt reach deeply into the basement rocks, where at appropriate crossings and junctions it is suggested that heat effects gave rise to ore-making materials, including, in this instance, intrusive breccias that later were mineralized, and comprising the broader bodies of new ores. The breccia ore is seen crosscutting the earlier narrow quartz veins with a welding of the two at junction areas by a second surge of ore minerals. The ore mined and developed since 1937 equals district production from 1896 to 1937 The ores are typified by cherty quartz, adularia and some barite, with fine pyrite and marcasite, polybasite, pyrargyrite, tetrahedrite and gold. Selenium is present, possibly with gold, as a normal selenide. The disseminated ores, as well as the vein and breccia ores, are localized principally in one 500-ft flow (Knob Hill andesite), which has been traced around the crest of the low northward-plunging Republic anticline. The gold-silver ratio in the earlier narrow veins is about I to 4 and in the disseminated and breccia ores, I to 7. The latter higher silver ratio is deemed to reflect the character of the second surge of mineralization. Sills and dikes of the Columbia River (Miocene) basalt cut the folded structure and ore, thus placing the mineralization in the middle Miocene. Introduction The Republic district of north central Washington is of new interest because of the discovery, development and extraction of new gold-silver ore; also, because of a unique local structural pattern believed to be integral with the broader tectonic mechanism of the continental framework. This district had 40 years of modest rating following its discovery in 1896. Its narrow ore bodies, complex mineralogy. and early inadequate metallurgy, together with the apparent bottoming of ore near 1000 ft, limited production to 300,000 oz of gold and 1,000,000 oz silver between 1897 and 1914. The camp was then reduced to lease Life until 1937, when the gold price increase of 1933 to $35 per ounce

Jan 1, 1949

By F. E. Buch

THE Smelter is designed for a production capacity of 10,000 short tons of blister copper per month, when operating on the present concentrate grade. The Smelter lay-out is shown in Fig I. The major units of equipment comprise two reverberatory furnaces, three 13 by 30 ft Peirce-Smith converters, two straight line casting machines, one being served by a 13 by 30 ft holding furnace and the other by a ladle tilting quadrant, two converter ,aisle cranes and two converter blowers. The plant is compact and the general arrangement of standard gauge railway tracks and conveyor belts provides for a smooth flow of incoming materials and metallurgical products. Concentrate is received by conveyor belts and fluxes in standard railway trucks. The local track system is covered by an electric trolley locomotive. The Smelter treats a wet (10 pct moisture) flotation concentrate containing approximately 53 pct total copper and 0.9 pct oxide copper. The predominating minerals are chalcocite, chalcopyrite and bornite accompanied by small quantities of malachite and cuprite. The gangue is highly siliceous and requires limerock as a flux. Metallurgy would be straightforward were it not for the necessity for eliminating k bismuth which occurs as an impurity in the ore along with the copper. Directly or indirectly most of the Smelter problems can be traced to the necessity for bismuth removal. Copper recovery, based on new copper treated, averages 97.5 pct. GENERAL DESCRIPTION Flotation concentrate, containing to pct moisture, is conveyed from the filter plant to the smelter storage bins by conveyor belts, the material being weighed in transit by a revolving drum type of weigh-hopper manufactured by Samuel Denison and Son, Ltd. The weigher consists of a steel drum with dished ends carried on a horizontal shaft and rotated by an 8 hp squirrel-cage motor through a worm and spur reduction gear. A feed mouth in the drum permits of filling and discharging. The whole unit is supported on a framework resting on weighing levers, which in turn connect to transfer levers, thence to an indicator of the steelyard type situated 16 ft from the centre line of the drum. The indicator is of the "Denison" patent equilibrium controlled ticket stamping type, insuring mistake-proof records by a combination of electrical and mechanical movements which prevent the operator from printing until the cover enclosing the steelyard is closed and until the poise-weights have been set correctly to the weight of the hopper and contents. The machine is capable of weighing 30 short tons at a time but the usual load is 28 tons. After obtaining the gross weight the drum is rotated and discharged into a receiving bin situated below it. The empty drum is weighed and the net weight re-

Jan 1, 1947

By M. Kashiwada

The zinc leach residues are introduced into waelz kiln to fume volatile metals and before the end of 1967, the waelz-fume containing zinc, lead, cadmium and indium was directly recycled back to the leaching process for the production of electrolytic slab zinc. However, since 1968, we have been recovering with success those valuable metals contained in the fume separately instead of direct leaching. According to the improved process, the waelz-fume, after being mixed with chloridizing agents, is fed into the rotary kiln to be roasted, wherein most of lead and cadmium content is collected as fume and most of zinc remains in the calcine. Zinc calcine thus obtained, containing 70 to 75 per cent zinc and, less than 1.0 per cent lead is sent to zinc plant for further recovery and the fume containing 40 to 50 per cent lead and 3 to 6 per cent cadmium is further processed to recover lead, cadmium and indium. The advantage of this process can be secured to the utmost when it is combined with the following subsequent treatments. (a) Blast furnace smelting of non-magnetic waelz slag to recover copper, silver and gold as matte. (b) Gallium recovering process from magnetic waelz slag. (c) Soda process of lead bearing cake produced after removing cadmium and indium from the said fume. Thus the extractions of zinc, lead and cadmium from leach residues account for 87 per cent, 72 per cent and 85 per cent respectively.

Jan 1, 1970