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By W. C. Winegard, W. J. Bratina

Internal friction characteristics and temperature dependence of the torsion modulus for iodide zirconium containing 2.4 pct Hf were investigated, using a low frequency pendulum technique. The internal friction curve consists of a background which increases as the temperature increases, a maximum at 860°C apparently a background due to the al-lotropic transformation, a maximum due to grain boundary relaxation with an associated heat of activation of 58,000 cal per mol, and an anomaly below 350°C which may be associated with a precipitation perphenomenon, Oxygen in below small amounts reduces the grain boundary maximum substantially. The variation of the torsion modulus at 20°C was found to be 3450 Kg per mm2 for the zirconium used in the present work. IT is well known that small amounts of certain solutes materially affect the ductility of zirconium. Lely and Hamburger,&apos; as early as 1914, found that high purity zirconium exhibited a remarkable ductility, while Fast&apos; has shown that oxygen and nitrogen can cause substantia1 embrittlement. Treco" has recently demonstrated that the ductility decreases sharply with the oxygen content, and that 2 atomic pct O2 embrittles zirconium to such an extent that cold working is impossible. The marked decrease in ductility is difficult to understand in view of the fact that Domagala and McPherson4 report the solid solubility of oxygen in zirconium to be 29 atomic pct at 500 °C. Another metal which behaves much the same as zirconium in this respect is titanium. Pratt et al." investigated the internal friction characteristics of titanium and the effect of oxygen on the internal friction values. It is evident that internal friction measurements are of value for studying grain boundary segregation, as shown by Pratt et al. for oxygen in titanium, by Pearson for oxygen in copper, and by Maringer and Schwope for oxygen in molybdenum. With this in view, the internal friction characteristics of zirconium and the qualitative effect of oxygen on the grain boundary relaxation phenomenon were investigated. Materials and Experimental Procedure The zirconium used in the present work was supplied by the Foote Mineral Co. in the form of wire 0.05 in. diam. The analysis supplied by the manufacturer indicates the amount of hafnium as 2.4 pct, less than 0.01 pct O less than 0.01 pct N,, less than 0.02 pct H,, and less than 0.001 pct C. Additional spectro-graphic analysis indicates the other main impurities as follows: 0.01 pct Fe, 0.05 pct Si, 0.008 pct Cu, <0.005 pct W, <0.001 pct Al, <0.05 pct Mg, <0.001 pct Ni, <0.02 pct Ca, and <0.01 pct Ti. Microscopic examination of the material in the as received condition revealed very fine grains with numerous twins. Specimens were annealed either in situ in the internal friction apparatus or in evacuated silica tubes in an auxiliary furnace. When the specimens were annealed in the auxiliary furnace, they were wrapped in identical zirconium wire to prevent contamination by the container. Metallographic sections were taken in all cases. Some were taken from the specimens used for internal friction measurements after completion of the experiments, while others were taken from control specimens at intermediate stages of the experiments. lnternal friction values were obtained by measuring the free decay of a low frequency torsion pendulum (1 cycle per sec), the suspension of which was

Jan 1, 1957

By F. D. Rosi, C. A. Dube, B. H. Alexander

WHEN a deformed polpcrystalline metal is heated to a sufficiently high temperature, a recrystallized structure develops which consists of small, essentially stress-free grains. This transformation is referred to as primary recrystallization. Under certain conditions, on prolonged annealing of the specimens, a type of grain coarsening occurs in which a small number of grains commence to grow at various points by devouring the neighboring finegrained primary structure, which, in itself, exhibits a marked stability toward normal grain growth. This grain coarsening process has been referred to by Burgers&apos; as "secondary recrystallization" or "exaggerated grain growth." Although much work has been done on recrystallization and growth processes, present knowledge of the factors which determine the occurrence and growth of secondary grains is inadequate for the advancement of a theory which accounts for the observed characteristics of this recrystallization phenomenon. In this respect, it would be important to make measurements of the velocity of growth of these large secondary grains. The early work of Feitnecht2 on aluminum showed that the size of secondary grains increased with temperature and time, suggesting that such measurements would be possible. More recently, Burgers1 found that the growth velocity of these grains in aluminum was constant over a large time interval, as is generally found for the growth velocity of primary grains in a uniformly deformed test piece.3-5 It is reasonable to expect that the determination of the activation energy of the secondary growth process might lead to a better understanding of the underlying atomic mechanism. This investigation, therefore, is one of a series primarily designed to measure the growth velocity of secondary grains at various temperatures for silver, copper, and aluminum. It is hoped that these studies along with those of orientation relationships, will establish a sound basis for theorizing as to the origin and nature of the secondary transformation. Experimental Procedure The metal used in the present investigation was high-purity silver (999.9 fine), which was supplied in the form of cold-rolled plates 0.250 in. thick. These plates were annealed at 500°C for 1 hr and then straight-rolled to a thickness of 0.04 in. in three reductions of approximately 45 pct, followed in each case by an anneal at 450°C for 1/2 hr. The 0.04 in. sheets were given a final reduction of approximately 50 pct, which resulted in a thickness of 0.02 in., thereby insuring two-dimensional crystal growth. Individual specimens of this material about 1x3 cm were used for all heat treatments, unless otherwise noted. The annealing was carried out under an atmosphere of argon in an Inconel tube furnace whose temperature was controlled to within -+2°C. Metallographic examination of the secondary transformation was accomplished by mechanically polishing the specimens on one side to approximately one half their thickness through 2/0 metallographic emery paper, and then electrolytically polishing in a solution of potassium ferrocyanide and sodium cyanide. With a current density of approximately 20 amp per sq dm, the time required to obtain a satisfactory surface varied from 3 to 5 min. Standard potassium bichromate was used to etch the electrolytically polished surfaces. A heavy etch with this solution produced a sharp contrast between the secondary grains and the fine-grained primary structure, darkening the latter while leaving the large secondary grains bright. All area measurements of the secondary crystals were made with a planimeter on enlarged tracings of the grains.

Jan 1, 1953

By Harold L. Overton, Leonard B. Lipson

The first paper in this series1 outlined practical methods for applying the theory of steady-state flow of an ideal Bingham plastic liquid through a circular pipe and axially through a stationary concentric annulus to the enginekring analysis of friction loss problems. In the present paper the properties of another useful rheological model, the pseudoplastic generalized Newtonian liquid, are considered. The terminology applied to the rheological models is derived from the following classification of rheological models. The term "generalized Newtonian" is a class designation applied to models which do not have yield points but which exhibit a dependence on shear rate. The term "pseudoplastic" applies to a sub-group of models within this class which exhibit a decrease in "viscosity" with increasing shear rate. The term "power model" refers to a mathematical model proposed for describing the behavior of the pseudoplastic liquid. This model is of interest since certain of the salt saturated, oil emulsion, and "low solids" drilling fluids, inverted emulsion- and oil-base drilling fluids, aqueous gels, gelled crudes and blocking agents employed in hydraulic fracturing operations are of this type. The present treatment considers the equations describing steady-state Poiseuille flow through a circular pipe and a stationary concentric annul us, and Couette flow between concentric rotating cylinders for a particular pseudoplastic model. As in the previous paper&apos; it is demonstrated how these equations can be applied to engineering calculations of friction losses. Graphical procedures for recovering the various flow curves and cxample calculations are included. A method for simplifying turbulent-flow correlations is also proposed. PROPERTIES OF PSEUDOPLASTIC GENERALIZED NEWTONIAN LIQUID In contrast to the Bingham plastic the generalized Newtonian liquid is yield point-free. However, in the flow region the relation between stress and rate of shear is not linear as it is with ordinary Newtonian fluids. If the stress increases with shear rate at a less than linear rate the system is called pseudoplastic. While there is no yield point in this system, the Bingham advocates&apos; coined the term pseudoplastic to distinguish this kind of behavior from Bingham plastic behavior. For the pseudoplastic a plot of flow rate vs friction loss or rpm vs torque, from pipe flow or rotational viscometer measurements, respectively, generally has three qualities: (1) it can be clearly extrapolated toward the origin; (2) there is very little slope at the origin. This accounts for the high apparent viscosities at low mixing and pumping rates; and (3) the flow curve possesses a continuous curvature which gradually diminishes as the shear increases. Rheological measurements on a pseudoplastic liquid can be easily misinterpreted as indicating Bingham plastic behavior. A typical case in point is illustrated in Fig. 1. These data were obtained from measurements on an oil-emulsion mud using a commercially available rotational-type viscometer (Model 35 Fann V-G meter). Applying the "two-point"* method3 gives a plastic viscosity of 17 cp and a yield point of 24 lb/100 ft2; at the same time weighting material settles very easily in this system. This illustrates that it is not possible to distinguish between the pseudoplastic and the Bingham plastic from only two data points. It is possible to determine qualitatively which model is more appropriate by a combination of dynamic and static measurements. Experience indicates that the simplest criterion for the Bingham plastic liquid is that the calculated dynamic yield point should be of the same magnitude as the measured gel strengths. For the oil-emulsion drilling fluid illustrated in Fig. 1, a value of 4 lb/100 ft2 was obtained for gel strengths measured

By James E. Lawver, James L. Wright

This paper describes the design of a cell used to measure the electrical conductivity, or the reciprocal resistivity, of granular materials. It also establishes a quantitative relationship between the electrical conductivity and the electrical separation of selected mineral samples. It is estimated&apos; that the free world produces about 13 million tons of mineral concentrates a year by electrostatic or electrodynamic methods. At least 95% of these concentrates are produced by corona discharge type machines that separate minerals by exploiting the differences in their electrical conductivity. But, what is meant by the electrical conductivity of a mineral? How large a difference in the electrical conductivity of two mineral species is necessary to effect a separation? Just what is the role of conductivity in electrical separations with regard to capacity and selectivity? There is a considerable amount of information in the literature on both the mechanisms of conduction and the values of the electrical conductivity of pure single-crystal mineral specimens. In addition, some insight into the role of mineral conductivity can be obtained by referring to a Bureau of Mines publication&apos; in which 95 minerals have been grouped as conductors or insulators as a function of temperature. The classification was made on the basis of the percent of weight that reported as "conductors" in an electrical separator. But, as is often the case in the mineral industry, practical application leads theory — and there is little useful information in the literature giving any kind of quantitative relationship between electrical conductivity and electrical separations. The problem is a bit complex because electrical conductivity per se — which can be rather easily measured on large, single grains — is not sufficiently informative to permit quantitative predictions of the separability of the mineral system. Practical "high-tension"* separations are made at such feed rates that the band of minerals on the rotor is multilayered in thickness. Thus, the effective conductivities of minerals as seen by a high-tension machine include particle-to-particle contact resistance, which is often a controlling factor in making a separation. This is particularly true when the mineral grains are coated with slime or with a dielectric surface film. From a high-tension separation viewpoint, one is actually concerned with the time required for corona-charged grains to lose enough charge so that the centrifugal force acting on the particles exceeds the image force holding the grains to the rotor. This calculation requires a knowledge of the effective mineral conductivity s. (The conductivity of the metal rotor is sufficiently greater than that of the minerals so that it need not be considered in charge decay calculations.) The charge density at time t can be approximated by the relaxation equation.3 where t 5 charge density at time t r, - charge density when t = 0 cr e total electrical conductivity £ = permittivity The time required for the charge density to fall to l/e of its initial value is called the relaxation time and is numerically equal to €/n. AS defined here, u is the conductivity of an element of homogeneous grains making contact with each other and with a grounded rotor. This paper deals with the design of a conductivity cell used to measure a, or its reciprocal p, the electrical resistivity. CELL DESIGN Initial test work was performed with a cell recommended by ASTM.4 Since the reproducibility with the ASTM cell was not satisfactory, it was decided to

Jan 1, 1970

By R. J. Schaefer, M. E. Glicksman

Direct, in situ observation of metallic alloys during solidification reveals that in some systems crystal multiplication occurs by means of a dendrite remelt-ing process, without the necessity of independent nu-cleation events. The solidification is observed on optically clean surfaces of supercooled molten alloys. In one system (Sn-3 wt pct Bi) , a fine-grained equi-axed structure is produced by the complete disintegration, via remelting, of transient initial dendrites. In contrast, several other metallic systems show little or no evidence of remelting activity. The behavior of these metallic systems is consistent with that expected on the basis of published observations of dendrite remelting in transparent organic alloy systems. It is concluded that dendrite remelting is an important crystal multiplication process in some metallic alloys, but is velatively unimportant in some other alloys. The detachment of dendrite branches from the primary stem by a remelting process has been observed by Jackson, Hunt, Uhlmann, and seward1 during the solidification of some transparent organic alloy systems. The branches released by this remelting process can drift free of the primary stem and serve as seeds for the formation of numerous independent crystals. This proliferation of new crystals does not require repeated independent nucleation events, but only modification of the initial solidification structure. The mechanism of dendrite remelting, as described by Jackson et a1.1 and by Tiller and O&apos;&apos;Hara,2 is dependent on the transport of both heat and solute and is, therefore, expected to operate only in alloys, and not in pure substances. It was found in the transparent organic alloy systems that remelting occurred primarily in the constricted regions near the base of dendrite branches, where the branches had grown through the solute-rich liquid layer surrounding the primary dendrite stem. It was suggested that impure solid had formed in these constricted regions at a relatively low temperature and had later become unstable as further solidification of purer material raised the temperature. Jackson et al. proposed that the equiaxed zone of metal alloy castings originates from a similar remelting process, and they demonstrated the operation of this mechanism in "ingots" poured from saturated salt solutions. Although these substances were especially selected to show solidification behavior similar to that of metals,3 the remelting mechanism has, until now, been subject to the objection that its operation has not been directly observed in a metallic system. Considering the fact that thermal properties such as diffusivity may differ by as much as two or three orders of magnitude between metals and organic compounds, this objection was considered to be possibly serious. A method has now been developed by which it is possible to make direct optical observations of metals during solidification. This method has revealed transient solidification processes which would not be detected by metallographic examination of totally solidified specimens. In particular, a grain-refinement process in a metallic alloy has been observed to be a direct consequence of the total disintegration of an initial dendritic structure. The influence of an initial, transient solidification structure on the final solidification structure is demonstrated here for the first time in a metallic system. I) EXPERIMENTAL The technique of using a transparent flux to maintain an optically clean metal surface during solidification has been described by us elsewhere.* The

Jan 1, 1968

By Robert Hoy

If the reader finds that the basic information in a commodity chapter is insufficient, he can consult the appropriate sources in this chapter to find more detailed or more up-to-date information. In these days, technology develops so rapidly that this 4th edition will be somewhat out of date even by the time it is distributed. A comparison of this edition with the 3rd edition (1960) of Industrial Minerals and Rocks will clearly demonstrate how rapidly the scene changes. One of the best sources of new information, of course, is attendance at technical meetings. For example, the papers presented at the national and sectional meetings of AIME usually discuss new developments in the respective divisions of the society. Frequently this information is available in Preprints. In addition some are printed in Mining Engineering and/or the Transactions of the Society of Mining Engineers of AIME. Furthermore, other professional and trade journals contain articles pertinent to the field. A journal introduced in 1967, Industrial Minerals, published by the Metal Bulletin, Ltd., London, is an excellent source of information. The Mining Journal, Ltd., also in London, publishes a weekly journal, a Mining Magazine (monthly), and a Mining Annual Re- view. The latter covers the field from three aspects: (1) by commodities, (2) through technical developments, and (3) geographically. Other useful magazines and periodicals include Engineering and Mining Journal, Pit and Quarry, Rock Products, and World Mining, all published in the United States. In addition many new books related to industrial minerals have been published since the 3rd edition of Industrial Minerals and Rocks. Most of these, of course, are included in the bibliography of each chapter in this volume. Another excellent information source is the proceedings of the Forum on Geology of Industrial Minerals. This group, which held its 11th annual meeting in 1975, is sponsored by a state geological survey or another mineral agency on a rotational basis. The proceedings have been published by the various sponsors and are available as indicated in Table 1. Two major sources of basic industrial mineral and rock data in the United States, and also a good source for many foreign countries, are the U.S. Geological Survey and the U.S. Bureau of Mines. The two agencies publish many reports and maps on a variety of geo- logical and mining subjects. In addition, each agency has an indexed list of all their publications with a free service announcing new publications. (New Publications of the Geological Survey, U.S. Geological Survey, Washington, D.C. 20242) and New Publications-Bureau of Mines, Publications Distribution Branch, U.S. Bureau of Mines, 4800 Forbes Ave., Pittsburgh, Pa. 15213). The U.S. Bureau of Mines (USBM) publishes annually Minerals Yearbooks which provide statistical data on mineral products including production, consumption, imports and exports, as well as information on new developments. Another very useful USBM series is called Mineral Facts and Problems. Editions were published in 1960, 1965, and 1970. Three other major series of publications by the Bureau are Information Circulars, Reports of Investigations, and Mineral Trade Notes. The latter is particularly good for news of foreign developments. A new Professional Paper No. 820 of the U.S. Geological Survey, 1973, summarizes data on the mineral resources of the entire country. The USGS, in cooperation with USBM, other Federal and various state agencies, has also prepared summary reports on mineral and water resources of given areas which include

Jan 1, 1975

By J. Rourke, F. S. Minshall, E. G. Zukas, C. M. Fowler, O&apos

The Hugoniot curves were determined for Fe-Si alloys containing up to 7 wt pct (13 at. pct) Si. The pressure of the transition increased as the silicon content of the alloy increased. Single crystals of 2.9 wt pct Si-Fe were also studied. The pressure of the transition was not dependent on crystallo-graphic orientation. All of the Neumann bands (mechanical twins) were attributable to (112) planes but not all of the {112} planes showed twin markings. A thorough study of the iron Hugoniot (the relationship between specific volume and pressure) under plane wave shock loading revealed a pressure transition at about 130 kbar shock pressure. The results of this investigation were reported by Bancroft, Peterson, and inshall1 in 1956. At the time of this discovery, it was felt that this was probably the a, to y transition normally found in iron and many of its alloys. Subsequently a number of iron alloy systems were surveyed in which the alloying element has a considerable effect on the normal a, to y transformation. The influence of carbon and nickel and/or chromium have already been reported.2,3 At the present time, there appears to be some doubt that this pressure transition is the usual a, to y transition In this study, Fe-Si alloys containing up to 7 wt pct (13 at. pct) Si were chosen for several reasons. To the present, the transition has been found only in iron-base alloys which were originally in the a, phase (bcc). Secondly, the y loop at atmospheric pressure extends to only about 2.5 wt pct Si. If the transition were a, to y, then one might expect a rather drastic pressure effect for alloys containing more than 2.5 wt pct Si. Finally, single crystals of Fe-Si alloys large enough for shock loading studies are readily available thereby making it quite easy to determine the effect of crystal orientation on the transition pressure and on the twinning behavior of the alloy. EXPERIMENTAL PROCEDURE Fe-Si alloys containing up to 7 wt pct Si were produced by normal vacuum casting procedures. Single crystals of Fe-2.9 wt pct Si were purchased from Monocrystals Co., Cleveland, Ohio. The orientations of these crystals were determined and samples cut so that the shock wave would be parallel (to within 1.5 deg) to either the (loo), (Ill), or (112) principal orientations. Three distinct experimental testing techniques were used. First, the pin technique, described elsewhere,4 was used to determine the transition pressure for the polycrystalline alloys as well as for the (111) and (112) orientations of the 2.9 wt pct Si single crystals. Secondly, the recovery studies, described in detail in an earlier paper,2 were used for determining the effect of alloy composition and crystal orientation on the plastic II compression-plastic I rarefaction interaction zone for several specific shock pressures. Finally, measurements of pressures above the two-wave threshold were made on the polycrystalline alloys so that more complete Hugoniot curves could be constructed for this alloy system. The optical techniques described by Rice et al.5 were used to measure the shock and free surface velocities of the samples from which the Hugoniot data were obtained. This method is applicable only in the single wave region, since velocities are obtained from the measured total transit times of the disturbances through measured sample thicknesses.

Jan 1, 1963

By D. R. McCord

Data of a known statistical quality has been successfully used in a system of conventional fluid mechanics equations essentially free of empirical "conformance factors to prediet early detailed field 03 in a reservoir where gravity drainage is important and oil and rock properties vary con. siderably. The system is useful where comparative recovery predictions for one or more cases of natural depletion and gas cap pressure maintenance are needed and the reservoir is not too heterogeneous. INTRODUCTION Many authors, have examined various facet* of the gravity drainage-gas cap pressure maintenance problem over the last several years. Two of them. Burtchaell and Elkins, have published practical studies. In the case described in the present paper the best development and operating plan for one of the important reservoirs of the Bolivar Coastal Field in Western Venezuela was urgently needed. It was requested that sound comparative economics be presented along with an engineering evaluation of no additional drilling, maximum drilling. several cases of gas pressure maintenance, of water flooding and combination cases. A rapid analysis of the effect on recovery of the range of crude and rock properties indicated that none of the published methods using average properties would yield adequate comparative predictions. This paper covers the predictive system developed to deal with natural depletion and gas cap pressure maintenance. The large amount of data available for this field permitted statistically reliable correlations to be made of most rock and oil properties, and the evident smooth areal variations of these properties encouraged the construction of a lineal mathematical model of material balance and fluid flow equations, which could be manipulated by a modified iterative procedure. The manipulation is much more adaptable to computing machines than manually operated calculators and subsequent studies have been prepared for the IBM Card Program Calculator. A matrix as opposed to linear model has been tentatively worked out by other members of our group to deal with more heterogeneous reservoirs. It is more adaptable to computers such as IBM-701 or the Remington-Rand Univac. In 1950, when the system reported below was developed, no rapid computing machines were available to the author. Their existence and promise encouraged an initial approach by hand. Some details of oil and rock Property correlation are included because there are a surprisingly large number of medium-sized reservoirs in the world that show systematic property variations which are significant for a rigorous analycon. All large reservoirs (over half a billion barrels recovery) with which the author is familiar contain at minimum a significant temperature variation. Using the rock and oil property correlations, past pressure and production, the gas-oil ratio history of the reservoir was computed and found to be in close agreement with field measurements. The future performance under cases of natural depletion, gas injection of 100 MMcf/day, and of 130 MMcf/day, was then computed; a 70 MMcf/day case was also carried far enough to provide data for comparative economics. The 130 MMcf/day case proved to be the most attractive. A 50,000 horsepower gas turbine driven centrifugal compressor plant to take this quantity of adjacent field gas from 30 to 1,950 psia and inject it into the reservoir is under construction. The total cost of the project will exceed 20 million dollars.

Jan 1, 1953

By R. Ruka, E. A. Gulbransen

ONE of the interesting questions in the understanding of the reaction of iron with oxygen is the kinetics and the mechanism of the crystal structure changes occurring in the formation and breakdown of the oxide film. In a recent work&apos; the electron diffraction method was applied to the study of the solid phase reactions occurring internally in the oxide film on iron above 570°C and under vacuum conditions. The higher oxides which form under oxidizing conditions are reduced internally by the diffusion of iron into the oxide leaving the bulk of the oxide FeO (wüstite). This paper will ask and consider three questions. These are: (1) What is the nature of the depressed transformation temperature for the Fe3O4 + Fe ? 4Fe0 reaction in very thin oxide films?; (2) What is the mechanism of the forward transformation of Fe3O4 to FeO at or near 570°C?; and (3) What is the nature and mechanism of the slow reverse transformation of FeO to Fe3O4 and Fe below 570°C?. The composition of the oxide as well as its electrical, magnetic, mechanical, and chemical properties depends upon the kinetics of these reactions. Literature Survey The composition of the oxide film on pure iron at temperatures up to 570°C has been studied extensively by the electron diffraction method. Nelson,&apos; Jackson and Quarrell,3 and Gulbransen and Hick-man4 have shown that Fe3O4 and a-Fe2O8 are formed in the temperature range of 225" to 570°C, while y-Fe,O, is most likely formed below 225°C for long oxidation times. In very thin films FeO (wüstite) is found to form at temperatures as low as 400°C, and its existence depends essentially upon the extent of initial oxidation. FeO is not found in the formation of thick films below 570°C. On the other hand X-ray5 and micrographic8 studies show that Fe3O4 may exist as the main com-ponent in thick films up to 650°C, well above the equilibrium temperature for the reaction Fe3O4 + Fe ? 4FeO. The kinetics of the forward and reverse trans-formations of the reaction Fe3O4 + Fe ? 4FeO have not been studied in oxide films. However, analysis of the data of Gulbransen and Hickman4 on the heat-ing and cooling of iron oxide films of known thick-nesses in high vacua shows that the forward reac-tion proceeds rapidly even for a 4000 A film at temperatures of 575" to 600°C. The reverse reaction or decomposition of wüstite (FeO) occurs at tem-peratures below 450°C. Thus, there appears to be a slow process in the decomposition which is in marked contrast to the rapid forward reaction. The decomposition of a bulk sample of FeO free from the metal has been studied extensively by Chaudron, Benard and coworkers using the micro-graphic, X-ray diffraction, and thermomagnetic methods. Chaudron7,8 first observed that the de-composition of FeO (wüstite) below 570°C occurs by the reaction 4FeO ? Fe3O4 + Fe. Later work by Chaudron and Forestier5 showed that the rate of de-

Jan 1, 1951

By Arthur B. Cummins

Diatomite is a siliceous rock of sedimentary origin, which may vary in degree of consolidation, but which consists mainly of the fossilized remains of diatoms. These are microscopic algae of the order Bacillaria. Diatomite is a unique form of silica, there being nothing else found in nature or produced by the manufacturing arts, that has its characteristic physical structure. There are numerous sediments which contain some diatom residues, admixed with a substantial amount of other materials-clay, carbonates or silica. While these are classified as diatomaceous silts, shales, or mudstones, they are not properly diatomite, a designation which is restricted to material of such qualities that it is suitable for commercial uses. The terms diatomaceous earth and kieselgur are synonymous with diatomite. The expressions infusorial earth and tripolite are obsolete. Diatomaceous silica is a definition best used to distinguish the basic component of diatomite, that is, the substance of the silica shell itself and is the major constituent of beneficiated diatomite or processed diatomaceous products. Some highly indurated materials, such as cherty shale, porcelanite, and opaline cherts which have resulted from diagenetic changes cannot be considered as diatomite although they may have been derived therefrom. On the other hand, diatomaceous oozes or loose sediments consisting mainly of diatom residues with or without much organic matter are source materials in process of becoming diatomite. Composition and Properties Pure diatomite is composed of opaline or hydrous silica, with small amounts of associated inorganic components-alumina, iron, alkaline earths, alkali metals, and minor constituents, all of which may occur in solid solution or as an essential part of the opal complex. Crude diatomite on the other hand may contain variable amounts of organic matter and soluble salts, and the usual contaminants of sedimentary formations-particles of rockforming minerals, sand, clay, or carbonates. As occurring in nature, diatomite contains an unusual amount of free water, which may vary from 10 to 60 pct or more. Diatomite, in the dry deposits which are characteristic of most of the important world deposits, occurs as a lightweight, comparatively light colored, "chalklike" material. The apparent density (dry basis) in situ varies from 20 to 40 lb per cu ft. The structure may be either massive or finely stratified. The earth is highly porous, usually soft and easily friable. It is nonreactive with acids and may be tentatively identified by the above characterizations. Confirmation is by microscopic examination which readily reveals the nature of the material. In deposits which contain organic matter the appearance of the material is totally different. The color may vary from light tan or gray to brown, greenish or nearly black. There is frequently difficulty in distinguishing it in the field from peatlike materials, but the difference is readily apparent after calcination. Powdered diatomite or diatomite products have an apparent density (loose weight) of 5 to 16 lb per cu ft, wet densities of 10 to 30 lb per cu ft, specific gravities 1.9 to 2.35, index of refraction 1.42 to 1.48. Diatomite is essentially micro-amorphous, but does show some tendency toward orientation in structure after a cristobalite pattern. Amorphous silica has been considered as a random association of cristobalite crystallites, the size of which are only slightly larger than a unit cell.20 The prop-

Jan 1, 1960

By Eugene F. Poncelet

Glass squares compressed on edge by steel jaws in poor contact with them developed jagged "partial-contact" cracks caused by the formation of local tensile stresses. Compressed by steel jaws in perfect contact, they developed smooth "release cracks" during release of the pressure, caused by the formation of local tensile stresses during the release of the pressure. All these cracks were parallel to the pressure. A Microflash photograph of a disintegrating specimen under sufficient pressure reveals a network of fractures roughly normal to each other, also "release cracks" and a disintegration cloud. The Griffith theory is amended to account for the formation of a first crack. A new theory, based on the theory of thermal agitation and wave propagation, is proposed to account for the progress, velocity and forking of cracks. The network of fractures is shown to have been caused by reflection at a free boundary of pressure pulses emanating from a first crack. Postulating equal distribution of energy in the pulses emitted on either side by a crack in particles, the smaller fragments are shown to continue fracturing preferentially while some of the coarser fragments remain as residual pieces. As comminution of the smaller fragments proceeds, the solid is reduced to a collection of residual particles of smaller and smaller sizes, accounting for the disintegration cloud. Experimental Procedure Apparatus A crushing device was built, consisting of a steel frame and two polished, hardened steel jaws to crush plate-glass samples. This device was placed between the plates of a hydraulic press (Fig. I). For centering the pressure, the upper jaw was guided vertically and provided with a rounded top. Later it was replaced by a steel jaw ground out of a 2½-in. steel ball, the lower surface being ground to an optical flat (Fig. 2). Four rollers were used to eliminate side thrust. Screws and centering blocks served to center the specimen in the crushing device. Hard steel shims placed under the shoulder of the upper jaw limited the "follow through&apos;&apos; of the jaw after failure of the specimen. Stress distribution was first examined with a polariscope mounted on an optical bench, using monochromatic light. It was found convenient to mount polaroid, quarter wave and monochromatic plates directly on the device itself. A Microflash unit* was used as light source for the photographs. A gold-paint pattern was fused on the plate-glass specimens and connected into the spark-

Jan 1, 1947

By H. C. Jennison

Two distinct types of defects occur at times in copper wire as a result of the use of dies of improper design or undesirable wire-drawing practice. The conditions under which these defects may be produced, as well as precautions to be taken in order to prevent them, have been known to The American Brass Co. for many years. The quality of the copper wire bars and rods has too often and unjustly been held responsible for these particular defects and it is to correct any such belief that this paper is presented. An extremely high quality of electrolytic copper has been supplied to the trade by all refineries for the last 20 years at least. The purity of the copper would average well above 99.900 per cent. The casting of the wire bars has been handled in a generally satisfactory manner. The bars have been cast sound, with a flat to slightly crowning set and have been free from sloppy edges, cold sets, etc. In other words, the wire bars have met A. S. T. M. specifications and have been generally satisfactory. For the most part, they have been everything that could be desired from a quality standpoint yet most of the wire mills in this country and in Europe have at times held the quality of the copper responsible for the two types of defects described in this paper. As a matter of fact, these defects are produced entirely in the wire mills. The author has visited many of the large wire mills in the United States and in Europe to investigate these defects. In some cases the trouble has been so serious that the wire mill has ceased operations. At times the wire mills are reluctant to believe that they are responsible for the defective product. The effect of die design, wire-drawing practice, etc., upon the quality of copper wire has received little study on the part of wire mills, particularly those that have commenced operations in the last few years. Two Types of Defects One type of defect is generally known in this country as "check marks;" in Europe it is termed "crowfeet" (Fig. 1). This defect occurs in the surface of the copper wire, in the form of V&apos;s, which are always

Jan 1, 1930

By Eugene F. Poncelet

Glass squares compressed on edge by steel jaws in poor contact with them developed jagged "partial-contact" cracks caused by the formation of local tensile stresses. Compressed by steel jaws in perfect contact, they developed smooth "release cracks" during release of the pressure, caused by the formation of local tensile stresses during the release of the pressure. All these cracks were parallel to the pressure. A Microflash photograph of a disintegrating specimen under sufficient pressure reveals a network of fractures roughly normal to each other, also "release cracks" and a disintegration cloud. The Griffith theory is amended to account for the formation of a first crack. A new theory, based on the theory of thermal agitation and wave propagation, is proposed to account for the progress, velocity and forking of cracks. The network of fractures is shown to have been caused by reflection at a free boundary of pressure pulses emanating from a first crack. Postulating equal distribution of energy in the pulses emitted on either side by a crack in particles, the smaller fragments are shown to continue fracturing preferentially while some of the coarser fragments remain as residual pieces. As comminution of the smaller fragments proceeds, the solid is reduced to a collection of residual particles of smaller and smaller sizes, accounting for the disintegration cloud. Experimental Procedure Apparatus A crushing device was built, consisting of a steel frame and two polished, hardened steel jaws to crush plate-glass samples. This device was placed between the plates of a hydraulic press (Fig. I). For centering the pressure, the upper jaw was guided vertically and provided with a rounded top. Later it was replaced by a steel jaw ground out of a 2½-in. steel ball, the lower surface being ground to an optical flat (Fig. 2). Four rollers were used to eliminate side thrust. Screws and centering blocks served to center the specimen in the crushing device. Hard steel shims placed under the shoulder of the upper jaw limited the "follow through&apos;&apos; of the jaw after failure of the specimen. Stress distribution was first examined with a polariscope mounted on an optical bench, using monochromatic light. It was found convenient to mount polaroid, quarter wave and monochromatic plates directly on the device itself. A Microflash unit* was used as light source for the photographs. A gold-paint pattern was fused on the plate-glass specimens and connected into the spark-

Jan 1, 1947

By B. A. Cheadle, K. P. Steward

Axial tensile, ring tensile, closed end burst, and free end burst tests were done at room tempe.vature and 300°C on three batches of Zircaloy-2 sheathing zuith different textures. Knoop hardness tests were also done on all batches. The mechanical properties of the tubes were largely dependent on the percentages of cold work, but were also markedly affected by the textures, particularly with respect to deformation behavio&apos;r. The deformation behavior observed confirmed Picklesimer&apos;s predictions, zuhereas Knoop hardness results could be correlated with texture and yield strength anisotropy after the ,method of Wheeler and Ireland. From the mechanical properties, and from efjectiue strain values deterrlzined at the fractures using a photoqid technique, it zuas concluded that tubing witlz a single preferred orientation of radial basal poles best combines strength and ductility for any given deqee of cold work. THE mechanical properties required in collapsible Zircaloy-2 fuel sheathing for water-cooled power reactors are strength to resist wrinkling deformation by coolant pressure and ductility to accommodate a small amount of deformation in service without rupturing. Zircaloy-2 tubing during fabrication develops pre- ferred orientations of the a Zr grains due to aniso-tropic deformation behavior, and these textures markedly affect mechanical properties. Picklesimer&apos; had predicted the deformation behavior of tubes with various textures, but the texture required to provide the optimum strength and ductility for a given degree of cold work has not been reported. To investigate this problem, tests at three transverse to axial stress ratios were done at room temperature and 300°C on three batches of Zircaloy-2 tubing covering a wide range of textures and percentages of residual cold work. Knoop hardness values were also measured to correlate with preferred orientation and yield strength anisotropy after the method of Wheeler and relland.&apos; 1) MATERIAL For this investigation, three batches of tube-reduced tubing were chosen from the Zircaloy-2 sheathing produced for the Douglas Point Reactor. Individual tubes were 191/2 in. long, 0.600 in. OD, and 0.0165 in. nominal wall thickness. The identities of the batches, together with their textures, are shown in Table I. The tubes had the normal Zircaloy-2 composition3 of 1.5 wt pct Sn, 0.3 wt pct Fe, Ni, Cr combined with the following oxygen concentrations: Batch VII 1140 to 1390 ppm 0 Batch VIII 1400 to 1750 ppm 0 Batch IX 880 to 1320 ppm 0

Jan 1, 1968

By Eugene F. Poncelet

GLASS squares compressed on edge by steel jaws in poor contact with them developed jagged "partial-contact" cracks caused by the formation of local tensile stresses. Compressed by steel jaws in perfect contact, they developed smooth "release cracks" during release of the pressure, caused by the formation of local tensile stresses during the release of the pressure. All these cracks were parallel to the pressure. A Microflash photograph of a disintegrating specimen under sufficient pressure reveals a network of fractures roughly normal to each other, also "release cracks" and a disintegration cloud. The Griffith theory is amended to account for the formation of a first crack. A new theory, based on the theory of thermal agitation and wave propagation, is proposed to account for the progress, velocity and forking of cracks. The network of fractures is shown to have been caused by reflection at a free boundary of pressure pulses emanating from a first crack. Postulating equal distribution of energy in the pulses emitted on either side by a crack in particles, the smaller fragments are shown to continue fracturing preferentially while some of the coarser fragments remain as residual pieces. As comminution of the smaller fragments proceeds, the solid is reduced to a collection of residual particles of smaller and smaller sizes, accounting for the disintegration cloud. EXPERIMENTAL PROCEDURE Apparatus A crushing device was built, consisting of a steel frame and two polished, hardened steel jaws to crush plate-glass samples. This device was placed between the plates of a hydraulic press (Fig. 1). For centering the pressure, the upper jaw was guided vertically and provided with a rounded top. Later it was replaced by a steel jaw ground out of a 2 1/2-in. steel ball, the lower surface being ground to an optical flat (Fig. 2). Four rollers were used to eliminate side thrust. Screws and centering blocks served to center the specimen in the crushing device. Hard steel shims placed under the shoulder of the upper jaw limited the "follow through" of the jaw after failure of the specimen. Stress distribution was first examined with a polariscope mounted on an optical bench, using monochromatic light. It was found convenient to mount polaroid, quarter wave and monochromatic plates directly on the device itself. A Microflash unit* was used as light source for the photographs. A gold-paint pattern was fused on the plate-glass specimens and connected into the spark-

Jan 1, 1944

By R. E. Shinkosk

This paper outlines the development of a program for increasing the life of woolen bags used for filtering Dwight-Lloyd gases by treating the bags and gases with hydrated lime. Methods and apparatus are described for determining alkalinity of dusts, acidity and breaking strength of bag cloth. Procedure and results, based on several years of operation, are presented. DURING 1939, additional facilities were constructed in the Dwight-Lloyd Blast Furnace and Baghouse departments at the Selby, California, Plant of the American Smelting and Refining Co. In order to handle adequately the increased volume of gases from the resultant increase in production, it was necessary to increase gradually the amount of water used for cooling gases ahead of the sinter machine baghouse. As a result of this increased water cooling, the average bag life dropped from 27 months in 1939 to 14 months in 1941. (Table I). This drop in life meant an increased. bag cost, as well as lower recovery of dust and some curtailment of operation. During 1941, it was found new bags showed as high as 0.3 pct acidity* after two weeks of opera- tion and as much as 2.0 pct acidity after some months of operation. This high acidity was present in spite of the fact that free oxide or relative alkalinity of the unburned dust ran from 5 to 6 pct. In view of these circumstances, a twofold program was started in Nov. 1941.t Part one of this program consisted of vigorously dipping all new bags in a weak lime solution, containing 50 lb of hydrated lime per 50 gal of water. Part two consisted of feeding fine, dry, hydrated lime into the gas stream intake of the sinter baghouse fan. Apparatus for feeding this lime is shown in fig. 1. All baghouse chambers are shaken in rotation about once each hour. On alternate hours, the baghouse operator places 50 lb of hydrated lime (one sack) into the lime feeder, starts feeder and immediately starts the bag shaking machinery. The rate at which lime is fed is set to coincide with the approximate time necessary to shake all sinter bag-house chambers, or about 15 min. It is felt this method of lime addition is most effective for getting lime into the woolen bag fabric. The amount of lime so fed averages about 600 lb per day. The amount of lime fed per day is varied to keep a minimum relative alkalinity of 9 pct in the unburned sinter dust. A daily dust sample is taken for alkalinity by allowing dust to accumulate in a sample pipe over a 24-hr period. This sample pipe, placed in any chamber cellar, is 2 in. in diam, 4 ft long, is sealed on the inner end, and capped on the outer end. It has a 1/2 in. slot cut for 18 in. along the tip end. This slot faces upward and allows the pipe to fill gradually with dust as bags are shaken. Breaking strength of bags has, in most cases, been the deciding factor in bag replacement. Bags that normally test 100 psi breaking strength when new are replaced when they test under 35 lb. The method for determining breaking strength is shown in the description accompanying fig. 2. Since the start of the liming program in 1941, bag life has increased from 14 months to an average of over 23 months, with a consequent material decrease in bag cost per year. Acidity, as per cent sulphuric acid, may be determined by means of a Beckman pH meter as follows: From a piece of bag cloth. which has been thoroughly cleaned of dust, a 5 g sample is weighed on a balance. Cut the sample into fine pieces and place in a 400 cc beaker. Add 100 cc (measured) of distilled water and stir vigorously. Filter on suction funnel, holding cloth pulp in beaker with a stirring rod. Wash cloth sample and filter wash water four additional times, each time with 20 cc distilled water, the last time squeezing cloth pulp over funnel. Discard pulp and rinse funnel and filter paper. Pour wash solution jnto measuring graduate and make up to exactly 300 cc with distilled water. Place into clean 600 cc beaker and measure the pH on meter. The per cent acid in bag cloth is read from the following table:—

Jan 1, 1951

By O. W. Simmons, L. W. Eastwood, C. M. Craighead

H. Schwartzbart and W. F. Brown, Jr.—The authors have divided the effects of recovery on the true stress-true strain curve into two types; metarecovery, which effects only the first part of the curve or the yield strength, and orthorecovery, which effects the flow stress at any strain. Both of these are said to be true recovery effects, involve no recrystallization, and are explained by the removal of two different types of imperfections caused by work hardening. However, there seems to be some question as to whether the data are sufficiently conclusive to exclude, as an explanation of the authors&apos; results, a mechanism based on the relief of residual stresses between the grains or slip bands and recrystallization. It appears that metarecovery could be interpreted in the same fashion as a customary interpretation of the Bausch-inger effect. The balanced system of internal stresses which exists between grains in a strained specimen due to varying orientation and, hence, yield strengths, of the different grains is responsible for a reduced yield strength in compression following pre-tension, and, similarly, for an elevated yield strength in tension following pre-tension. If the specimen is now heated so that the internal stresses are relieved by creep, then the yield strength in tension following tension will have been reduced and in compression following tension will have been raised. There seems to be a very strong case for the lack of recrystallization in the aluminum investigated by the authors, if one defines recrystallization as the presence of visually detectable new grains or accepts the X-ray evidence as conclusive. One must remember, however, that the appearance of spots on the back-reflection X-ray patterns cannot be taken as the time when recrystallization first started. The areas of recrystallized strain-free material must first have grown to a size large enough to give distinct spots on the patterns and this may take some time. Averbachl7 in an investigation of brass has shown that recrystallization can be detected by extinction measurements at temperatures lower than those based on hardness or X-ray line width determinations. It can be seen from fig. 10 that the rate of recrystallization is extremely low over a considerable time period at the onset of the process. Observations on the rate at which small amounts of recrystallization effect the flow stress would have given further insight as to whether undetectably small amounts of recrystallization might have been responsible for orthorecovery. Also, the question arises as to whether the effects observed in fig. 6 for various times and temperatures could not have been obtained if the time at 212°F were sufficiently long. In addition, the argument that the curve in fig. 10 is not sigmoidal seems weak in view of the scattering of the points. It is conceivable that an accurate determination of the curve for the first 100 hr would exhibit a relationship other than the one drawn. There is one point we would like to raise about the condition of the starting material. The authors annealed their material at 750°F for 15 min to remove the effects of any previous work hardening or machining strains. Reference to the work by Anderson and Mehl shows that this treatment may not have completely recrystallized the aluminum, so that the starting material may have had some strained areas. Higher temperatures or longer times may have been required to remove the effects of any small strains. We would like to mention some results of tests being conducted at the Lewis laboratory of the National Advisory Committee for Aeronautics in an investigation of the Bauschinger effect in relation to fatigue. Tests were performed on annealed electrolytic copper and several annealed brasses. Specimens were pre-strained 1 pct in tension and then tested in compression or tension with and without intermediate stress-relieving annealing treatments at 500°F for various times. Specimens heated at 500°F for 10 1/2 hr showed an elevation of the flow curve in compression and an approximately equal lowering of the flow curve in tension when compared with the curves for the un-heat treated specimens. After approximately 0.8 pct strain, all flow stresses coincided and were equal to the flow stress of the virgin material at this strain. This behavior is consistent with the metarecovery observed for aluminum by the authors and for which a residual stress model can be used. On the other hand, increas-

Jan 1, 1951

By B. J. S. Sceresini

The Filblast Cyanidation Process incorporates the advantages of intense high shear mixing, high dissolved oxygen concentra­tion and high pressure to achieve extremely rapid gold dissolu­tion rates. This is made possible without suffering from high energy or wear rates by the unique design of the Filblast gas shear reactor. The reactor is a rugged and compact in-line device which can be constructed from a variety of wear and chemical resistant materials. High temperature tolerance is also possible so that the device can be incorporated into a pressure leach circuit with significant capital cost savings because of the high capacity to volume ratio that is an inherent feature of the device. For cyanidation applications the outer casing is protected by a polyurethane coating and the internal parts are of wear resistant polymer. The largest unit built to date has overall dimensions of 1200 mm length by 300 mm diameter and has a capacity of about 150 dry tonnes per hour at 40-45 % solids. Service life at this throughput is at least three months. Six mines are currently employing the Filblast Process and another six are conducting plant trials. The ore types range from highly reactive, almost impossible to treat, pyrrhotite/ arsenopy­rite to deeply weathered clay ore which forms a highly viscous pulp. It has been found that the effect of shear thinning has resulted in improved leaching and adsorption kinetics resulting in higher carbon loading and reduced soluble gold loss. Total tonnage treated is approximately eight million tonnes per annum. This paper presents the operating benefits and cost savings which have been achieved in four plants, two treating oxide/ sulphide ore blends and two treating highly reactive sulphide ore and concentrate. Filblast leasing and maintenance charges and pump operating costs are about ten percent of the benefits. A conceptual cyanidation circuit based on the Filblast Cyanidation Process is also discussed. The Filblast System is an in-line pressure leach aerator/ reactor which generates very high shear and greatly enhances mass transfer rate by generating extremely small gas particles where oxygen gas is required for oxidation reactions and/or utilising the high shear characteristics to minimise the diffusion boundary layer. Both of these rate limiting factors effect the rate mechanism for gold cyanidation. Initially two multi-stage Filblast aerator cartridges formed a leach train but now the trend is to install a single submersible cartridge of equivalent perfor­mance. This design simplifies installation and minimises change-out times. However the in-line concept can be employed where high pressure leaching or pressure oxidation is required. The reactor is submerged in the leach tank so that the mass of gas micro-bubbles contained in the discharging slurry is entrained in the agitator vortex and is thoroughly dispersed throughout the tank. A diagrammatic representation of a leaching circuit incorpo­rating the Filblast Reactor is shown in Figure 1. The recirculation pump takes new feed directly from the cyclone overflow trash screen either under gravity or pump fed and recirculates the balance to maintain 250 - 270 m3/h total slurry flow. All of the leach feed slurry gets at least one pass through the Filblast thereby eliminating short-circuiting. Typically a 6/4 EAH Warman pump drawing 60-70 kW is required to circulate 250 m3/h through the system. The back pressure generated by the Filblast is in the range of 400-500 kPa depending upon pumping rate, pulp density and slurry rheology. The high shearing rate effectively negates the viscous effect of slurries and the addition of a gas further reduces the pulp density by virtue of the intensely aerated, homogeneous medium. The gold leaching Filblast cartridge elements are made of polyurethane but stainless steel, ni-hard, rubber or ceramics can be used depending on the operating temperature and design duty. The efficiency of the Filblast Leach Reactor in gold cyani­dation is due to the extremely efficient mixing, oxygen dissolu­tion and surface polishing action of the Filblast design. Either air or oxygen may be used but Atomaer recommend the use of oxygen because of the rate benefits gained from cyaniding at [02] significantly > 20 ppm D O in the reactor. Very high DO concentrations have been measured; in excess of 50 ppm. There is some debate as to whether the value is a true measure of the DO or the oxygen meter sensor is measuring the effect of a mass of very fine bubbles of free oxygen. Regardless of the fact the reactor has registered some amazing gold dissolution rates commonly in excess of 80 % during transit of the pulp through the reactor. The elapsed time is less than half a second!

Jan 1, 1995

By A. E. Wells

A critical study of the wet Thiogen process for extracting sulphur from the smoke of smelters is one of several investigations related to the general smelter-smoke problem that are being conducted under the direction of the Bureau of Mines. Part of the work done in the pyrometallurgical section of the cooperative metallurgical exhibit of the Bureau of Mines at the Panama-Pacific International Exposition during 1915 related to this investigation, and at the expiration of the exposition, the work was continued in the labora- tories of the Bureau of Mines in the Hearst Memorial Mining Building of the University of California, Berkeley, Cal., where a mining experiment station of the bureau has been established under the cooperative agreement with the University of California. Early in the spring of 1915, when plans were being made to co- operate with several metallurgical interests, the Thiogen Co. proposed to the Bureau of Mines that, along with the studies of various pro- posed methods for eliminating sulphur dioxide from smelter smoke, there should be included a study of the wet Thiogen process. In the study as outlined it was proposed to determine whether it would be technically and commercially feasible to use the, process for the recovery of elemental sulphur from the sulphur dioxide in waste smelter gases. Although there had been no large-scale work with the process, either in the laboratory or at a smelter, representatives of the metallur- gical and mining industry had shown considerable interest in the proposed method, and the desire had been expressed that a better knowledge of the possibilities of the process should be obtained. Thus, cooperation with the Thiogen Co. seemed justified by the in- terests of the metallurgical industry, and by the conservation promised by the recovery of a product of market value from what is otherwise a waste, and in some instances a serious nuisance. In accepting the responsibility for directing this investigation, the officials of the Bureau of Mines were necessarily free to conduct the work in the manner they considered necessary to determine the facts. It was also understood that any information obtained was to be made available to all who might be interested and might be printed in a Bureau of Mines report. To cover the cost of laboratory equipment and supplies, and the payment of salaries of assistants, other than Bureau of Mines employees, the Thiogen Co. in May, 1915, deposited with the cooperative metallurgical exhibit fund a sum considered sufficient to warrant starting the laboratory investi- gation. The origin and organization of this fund has been described by Clevenger and the author." In outlining the program for this investigation it was hoped that ultimately a small complete plant would be erected and the investi- gation center around the operation of the plant. However, pre- liminary to the erection of the plant, a laboratory study of the proc- ess was considered necessary, as the technical features of the process could be determined, it was believed, as satisfactorily on a smaller scale as on the scale first proposed. However, it was realized at the time that it would not be possible to determine so satisfactorily or definitely the commercial possibilities of the process on the scale of work adopted as in the larger operating plant. With this fact in mind it was planned that, if the study of the technical features on a laboratory scale gave sufficient promise of the process being commer- cially feasible, an operating unit should, if possible, be constructed later, and that more definite information concerning the commercial prospects should be determined. The investigations were started in June, 1915. In June and July work was confined entirely to small-scale laboratory tests, in which a careful study of the chemical reactions involved was made. In August, tests on a larger scale were started, and these were con- tinued until December, small-scale tests being made at the same time. On December 1, 1915, all work on the Thiogen process was discon- tinued temporarily, as the close of the exposition necessitated moving the laboratories. Work on the Thiogen process was started again in January, 1916, in the laboratories of the new mining experiment sta- tion at Berkeley, Cal., and was continued during the spring of 1916 until a point was reached where it was felt that the essential parts of the process had been carefully covered, and that some definite state- ments concerning the technical features and possibilities of the process, as given in this report, were warranted.

Jan 1, 1917

By H. W. Russell, Paul D. MILLER

IT is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranular corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels have been ably discussed by Bain and co-workers1-3 and by other investigators.4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a. mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measurements, measurement of the degree of cracking produced on bending over a mandrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A-10 11 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. EXPERIMENTAL METHOD A small area of the steel under test is subjected to an anodic treatment in a cell that can be clamped onto a sample or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8-in. diameter. The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941