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By W. F. Netzeband

THE zinc-lead mines of the Eagle-Picher Lead Co. are situated in the Tri-state district of Oklahoma-Missouri-Kansas. The company is operating, at the present time, seven mines in the brecciated deposits of the Picher, Okla., camp; two in the water-course ground of the Treece, Kans., camp; two in the open, boulder ground of the Crestline, Kans., camp; and one in the sheet ground of the Pierce City, Mo., camp. The accompanying map (Fig. 1) shows the relation of the rich narrow runs to the other ore-bodies of the district. The runs are designated by cross-hatching so as to distinguish them from narrow drifts that have been driven as prospect drifts or haulage drifts. Figs. 2, 3 and 4 are cross-sections showing the type of formation encountered in the operation of the drills. The Picher camp is in the brecciated type of deposit with some water-course ground encountered, usually near the edge of the deposit. These deposits are flat and fairly uniform so that they can be mined systematically. However, scattered between these deposits are narrow runs that are usually very rich. Up to the present time, most of the prospecting has been done from the surface with churn drills, supplemented with some prospect drifts in the ground, once the mine is opened up. Prospect drifts are expensive, do not give much information except the presence or absence of ore and are therefore not used to any great extent. In the early days of the camp only the larger deposits were found and mined, with an occasional narrow run which was drilled out more or less by sheer luck. Later, more of these narrow rich runs were found and mined, until today many of the properties that were formerly considered worked out are being leased and re-drilled. It is very evident that many of these narrow runs, which are often only 20 ft. wide, can easily be missed by drilling from the surface unless very close drilling is practiced. This, of course, becomes very expensive as there are from 150 to 250 ft. of

Jan 11, 1926

By George A. Roberts, Robert F. Mehl

WHEN austenite first forms from aggregates of cementite and ferrite, it is not homogeneous.1 This inhomogeneity, consisting of both undissolved carbide and carbon concentration gradients, has a profound effect upon the characteristics of the austenite-pearlite reaction. The rate of formation of pearlite is increased by the presence of inhomogeneities2,3 and because of this (when the inhomogeneity is sufficiently pronounced) the hardenability of the steel is reduced,4,5 In addition to this kinetic effect, inhomogeneities will cause the direct formation of spheroidite from austenite at temperatures just below the Ae1.6-11 The present report attempts quantitatively to evaluate the effect of inhomogeneity upon the rate of the austenite-pearlite reaction, presents a method of determining the austenitizing cycle necessary to obtain "practical homogenization," and considers the effect of inhomogeneity on hardenability. EFFECT OF INHOMOGENEITIES ON REACTIONS NEAR Ae1 Few quantitative data are available representing the effect of undissolved carbide or of carbon concentration gradients upon the rate of the austenite-pearlite reaction. In procuring such data it is necessary to separate the effect of undissolved carbide from that of grain size, and this is not an easy task. The solution of carbide is always accompanied by an increase in the grain size, both effects contributing to the retardation of the reaction rate. It has been possible to make this separation and to obtain data that are independent of the grain size by the use of steels that differ only with respect to their tendency toward grain-coarsening. Steels C and D in Table I are such steels. These steels have been studied previously;1,2,12 they differ only with respect to deoxidation practice; C was deoxidized with silicon while D, teemed from a portion of the same heat, was deoxidized with additional quantities of aluminum in the mold. C therefore is what is normally termed a "coarse-grained steel" and D is a "fine-grained steel." These steels can be compared at the same grain size by heating C to a low temperature and heating D to an elevated temperature, producing a structure of austenite plus residual carbide in the former while forming homogeneous austenite in the latter; in such

Jan 1, 1943

By N. M. Parikh, T. J. Koppenaal

The strengthening mechanism of fiber-reinforced silver has been investigated as a function of fiber density and fiber material. Stress-strain curves were determined in the range 2 x 10-6 to 2 x 10-3 plastic styain and slip lines were examined. The yield strength at 0.2 pct permanent strain is markedly dependent upon fiber density but the stress necessary to initiate plastic deformation is independent of fiber density. The strengthening mechanism of the fibers is shown to be malogous to grain boundary strengthening in poly crystalline metals. The variation in strengthening with different types of fibers is also noted and discussed. In recent years, considerable progress has been made in the understanding of the mechanical properties of two-phase systems, particularly in the classical dispersed-phase alloys where the separation between the dispersed phases is 0.01-0.1µ. However, little work has been done on fiber-reinforced metals where the dispersed-phase separation is considerably larger than this. Parikh1 investigated the mechanical properties of many fiber-reinforced metals and found that two general relationships are always observed, as follows: 1) A fibrous network incorporated into a second weaker metal strengthens the latter, and the amount of strengthening increases with fiber concentration. 2) At a corrstant fiber concentration, the amount of strengthening in a given matrix can vary considerably, depending upon the type of fiber employed. The object of the present investigation was to examine the fuiidamental factors controlling these two observations. procedure: Fig. 1 shows the initial step in the fabrication of the specimens. The sieve is shaken so that the fibers fall into a mold with the longitudinal axes of most fibers in the X-Z plane. The fibers are then compressed to a predetermined density, thus forming a "felt", and the necessary amount of matrix metal is added to the top of the felt. The mold is heated, in vacuum or hydrogen, to above the melting point of the matrix metal; the molten metal flows into the felt, and the entire assembly is cooled. This produces a "composite" that is essentially free of voids. A number of composites were prepared in this manner using 1/4-in. kinked lengths of mild steel

Jan 1, 1962

By K. L. Meissner

It is well known that the so-called pure aluminum contains noticeable amounts of impurities, chiefly iron and silicon, and many investigators have studied the forms in which these impurities exist. Hanson and Archbutt1 state that iron exists in aluminum as FeA13 and silicon as elementary Si. The solubility of FeA13 in solid aluminum is practically zero, or at least so small that the smallest trace of this compound is always visible as a separate constituent. Under the microscope an untrained eye can hardly distinguish, without etching, the two constituents FeA13 and Si, but they can be differentiated by suitable etching reagents. Anderson2 also found the same results. At the same time, Merica, Waltenberg, and Freeman3 found a constituent of unknown composition. They found a small thermal effect, at 610" C., on the cooling curves of aluminum with small amounts of iron and silicon. The intensity of this effect increased with increasing silicon content, until an effect occurred at 576" C. due to the eutectic between aluminum and silicon. The authors ascribed the effect at 610" C. to a compound, which they call "X constituent." It was thought to be a ternary compound containing iron and silicon and could be observed under the microscope as dark particles. Dix4 has published unetched photomicrographs of an aluminum with 0.51 per cent. iron, 0.99 per cent. silicon, and 0.32 per cent. copper that shows three constituents: the dark Si (black in the figure), the lighter FeA13, which appears in half tone and crystallizes in needles, and a constituent of the same color as FeAL3 but of different crystal form, often resembling Chinese script. This last constituent, Dix thought, is a compound of Fe and Si; not the compound FeSi but a compound containing a relatively small amount of silicon. Therefore an alloy of aluminum. iron, and silicon (the copper should not be regarded in the following considerations) must contain the following four constituents: Al, FeA13, Si, and a compound of Fe and Si. This, however, does not agree with the laws of chemical equilibrium.

Jan 1, 1926

By Donald E. Cummings

Certain dusts are dangerous when inhaled, but most hazardous of all dusts are quartz or other forms of pure crystalline silica. The inhalation of dusts containing silica in combination with other elements gives rise to changes in the lung which differ from those produced by pure silica. As a generality, silicates are less dangerous than pure crystalline silica and vary greatly among themselves in harmfulness. Repeated analyses have shown that approximately 70 per cent of the total number of particles involved in any dust-producing operation are below 1 to 2 microns in diameter. (A micron is approximately 1/25,000 in.) Similar studies of dusts recovered from silicotic lungs post mortem have demonstrated essentially the same size frequency distribution, except that the upper limit of size retained in the air sacs is approximately 10 microns. Experiments carried on by Gardner and the author have further demonstrated that greater changes were produced by a fixed weight of very fine quartz particles (2 to 3 microns and smaller) than by the same weight of slightly larger particles (8 to 10 microns). Any attempt to control a dust hazard should therefore be directed toward the removal from the working atmosphere of particles less than 10 microns in size, and particularly those below 3 microns. All industrial hygienists agree on this matter, but there remains considerable dispute as to the lower limit of particle size capable of causing injury. It has been generally conceded, however, that particles of harmful dusts smaller than 1/4 to 1/2, micron are not essentially concerned in the development of pulmonary fibrosis. This opinion is partly substantiated by the existence of large numbers of these small particles in practically all atmospheres that are not associated with any known hazard. Such particles are so small that they have very little mass, fail to settle even in quiet air, and probably are not easily retained in the lung. Until further research proves that they are involved in the dangers provoked by the inhalation of certain dusts, engineers will generally agree that it is better to disregard them.

Jan 1, 1937

By G. C. Waterman, W. E. Hawes

Mr. Grieves' paper on "Shaft Sinking Today --A Boring Business Tomorrow" in the Dec. 1981 issue of MINING ENGINEERING is an excellent description of recent improvements in speed and costs of shaft sinking. However, shaft boring techniques are not a recent development. In 1935-36, the Idaho Maryland Co. (gold), Grass Valley, CA, bored the vertical 1.5-m-diam Idaho No. 2 ventilation and supply shaft to a depth of 346 m. The equipment was designed and perfected by Branner Newsome and was, I believe, described in "Transactions." Pickands Mather later bored a 1.8-m-diam shaft to a depth of about 305 m using Newsome's design. The Idaho No. 2 shaft cut through hard gabbro, diabase dikes, soft serpentine, very incompetent ankeritized serpentine and a strong fault zone. The completed shaft did not require timber support; the fault zone was cemented. Equipment consisted of a rotating 1.5-m or 3-m core barrel with a slotted bottom which cut a 76-mm kerf. The cutting agent was chilled steel shot introduced into the slot as needed. The driving mechanism and core barrel were lowered into the shaft, the former secured to the wall and the inshaft "engineer" operated the motors which controlled core barrel rpm and advance. After an advance of 1.5-3 m the equipment was lifted out of the shaft, a half(?) stick of powder cut off the drilled core, and it was hoisted to the surface with a cable attached to an eye bolt at the tope of the core. A "shift" consisted of three men: hoistman, equipment operator (down the shaft), and a surface laborer. Advance was variable as equipment and techniques were perfected. Near the end of the job advance was, as I remember, 1.5-3 m per shift. Costs were, as I recall, about $115/m. Up to 4 m cores were lifted out in one piece and swung to the dump by a stiff leg derrick. The Newsome equipment was relatively inexpensive to build and operate and his method should be (more than?) competetive with the methods described by Grieves.

Jan 1, 1983

By Walter Stephen

MODERN developments in alloy steels have been so rapid and diverse that engineering practice has scarcely had time to re-appraise all items of past experience wherein conclusions became axiomatic under conditions that no longer apply. A case in point is the wet screening of abrasive ores within the fine range still looked upon as belonging exclusively to classifiers. By virtue of the development of stainless steels (18 per cent Cr, 8 per cent Ni), it is no longer true that classifiers are more economical than screens in closed circuit with large-tonnage ball or rod mills at 65 or even 100 mesh, provided a selective overgrind of the higher-gravity constitu-ents of the ore is not desired. Wet screening of ores is a highly corrosive as well as an abrasive opera-tion, because of the inevitably high degree of oxygenation of the water. Screen cloth of ordinary or spring-steel wire almost at once becomes pitted and covered with a film of corrosion products, which causes rust-blinding of fine-mesh screens and offers high frictional impedance to the flow of ore particles. On the other hand, the well-known properties of stainless steel enable it to maintain a bright surface, and so to eliminate blinding either by ore particles or by corrosion products. That a large-tonnage mill grinding hard ore to 65 mesh can be oper-ated economically in closed circuit with screens instead of classifiers has recently been demonstrated at the Copper Cliff concentrator of the International Nickel Co.; in the test to be described, a 6 ½ by 12 ½ -ft. Marcy rod mill ground from 625 to 820 tons. of ore per day to approxi-mately 65 mesh, operating in closed circuit with three 4 by 5-ft. Hum-mer screens, without any classifier.. Stainless-steel cloth gave an indicated life of several months. There was no difficulty with blinding, yet dilution and spray water could be controlled so that screen undersize averaged not less than 40 per cent solids. In contrast, ordinary carbon steel was pitted and blind with rust within 40 hours.

Jan 1, 1938

By K. W. Smith, E. A. Thomas

Various grades of synthetic mullite have been developed in recent years to replace or supplement natural sources of mullite deriued from the mullite group of minerals consisting of sillimanite, kyanite, and andalusite. Raw materials and heat treating processes used in making synthetic mullite are described. Chemical and physical data are given for typical grades and crystalline structure is illustrated with micrographs. Use of synthetic mullite as a refractory material in the glass and metallurgical industries is discussed. Mullite (3A12O3.2siO2), the only stable compound formed in the alumina-silica system, is usually present to some degree in all aluminum silicate ceramic products. The formation of mullite is considered beneficial to give rigidity to the structure and is dependent upon the ratio of Al2O3 to SiO2 in the original composition, particle size, degree of mixing, firing temperature, cooling rate, and the presence of auxiliary glass-forming fluxes. Mullite may also be formed at the reaction interface of fire clay or alumina-type refractories in contact with glass or slag melts. The term synthetic mullite is commonly used today to identify a class of sintered and fused aggregates or grains in the alumina-silica system having a highly developed mullite structure but derived mainly from raw materials other than the sillimanite group of minerals. Within the past 15 years extensive research has been done to develop economical processes to form sintered synthetic mullite aggregate to replace calcined Indian kyanite in super-refractories. Severa1 brands of such mullite are now being produced in commerical quantity and finding extensive use in refractories. Based on the service results of such refractories in many applications throughout the metallurgical, ceramic, and glass industry these developments have been considered successful and suitable substitutes for Indian kyanite now appear assured. EARLY DEVELOPMENT The conversion of kyanite, sillimanite and anda-lusite minerals of the sillimanite group to mullite and their use in refractories and porcelain have been discussed quite extensively in the literature by peck,' Grieg,' Riddle and Foster,3 Bowen and Grieg,4 and others and will only be mentioned here for reference to compare properties with synthetic mullite. In 1928, curtis5 reported on the development of a high temperature gas-converter process for forming synthetic mullite. The raw materials were derived mainly from lumps of high alumina clay of the correct natural composition or blends of clays and alumina that was interground and briquetted to form a suitable charge to maintain a surface combustion firing within the converter. Curtis was, no doubt, the first to illustrate by micrographs in natural color the crystalline structure of mullite derived from kyanite and mullite derived by sintering clay and alumina mixtures at temperatures above cone 32 (3123°F) and by electric fusion. In 1937, sei16 was issued a patent covering the use of a mixture of alumina-silica minerals and alumina in the proportion to form a mullite-yielding material at temperatures in excess of 3100' F. During the period from 1930 to 1940, economic conditions were not favorable for the production of synthetic mullite mainly due to an adequate supply of good grades of Indian kyanite ore suitable for conversion to mullite. Uncertain conditions on availability of the Indian kyanite during the early stages of World War II fostered further study on the development of synthetic substitutes. In 1943, McVay and wilson7 reported on an extensive investigation of domestic substitute materials. Their work covered essentially the use of mixtures of electric furnace mullite, calcined topaz, and calcined domestic kyanite. Compositions were found that gave equivalent or better hot load strength than Indian kyanite in mullite-type brick compositions; however, the calcining of the topaz presented certain physical and chemical problems on the disposition of silicofluoride and hydrofluoric acid while the high cost of electric furnace mullite was a limiting factor. In this work it was pointed out that water-quenched fused mullite was found to be unstable on reheat and gave poor hot load strength due to excessive glass present whereas the slow cooled or annealed mullite contained large crystals of mullite and corundum with little glass and gave superior results.

Jan 1, 1961

By K. F. Veith, R. L. Marovelli, T. S. Chen

An analytical study is made of thermal stress distribution in a thin circular disc subjected to a peripheral thermal shock at various rates of heat transfer. The problem is of importance in predicting the thermal shock response of a rock body of finite size. The theoretical analysis is based on radial heat flow by conduction in the disc and heat exchange by convection between the disc and the surroundings. The case of constant properties and plane stress is treated. Solutions of the stress distribution are presented for both cooling and heating shocks and an average stress theory is formulated. Preliminary experimental verification was obtained from the results of shock tests on thin rock discs insulated on both flat end faces so that heat exchange took place through the exposed peripheral surface. Physical properties vital to the analysis are Young's modulus, tensile strength, coefficient of linear thermal expansion, thermal diffusivity and thermal conductivity. Plots of these properties are presented. Historically, thermal energy has been used for primary rock removal throughout the ages. Although it is not widely known, the fire-setting method of thermal rock fragmentation was still in use 100 years ago in systematic underground mining operations in Scandinavia.' There, the availability of cheap labor and abundant wood fuel made the method competitive with the early blasting powders. By 1880, as high explosives replaced powder, use of the method declined and it was finally abandoned about 1885. Only 40 years ago, some experimental fire-setting methods were used for rock removal underground at Pribram and Zinnwald in Central Europe.2 Compressed air-oil burners replaced the earlier wood fuels. About 15 years ago, gaseous oxygen-oil burners were introduced in the United States and gained acceptance for difficult blasthole drilling and some quarry opera- tions. At present, there is renewed interest in the compressed air-oil burner designs. The literature included information on thermal secondary processes for rock weakening or particle liberation3,4,5,6,7,8 on thermal spallation of rock 9,10,11,12,13 and on the thermal fracture of materials other than rock. The 1955 Symposium on Thermal Fracture14 and the later work of Hassel-man, cover recent developments in thermal shock investigations on brittle ceramics. Although the number of published analytical and experimental investigations conducted on ceramic and refractory materials is large, the literature reveals that there is a lack of information on both the theoretical and actual response of rock to thermal shock. Many of the thermal shock studies on ceramic and refractory bodies are based on the case of heat transfer at the solid's surface by convection in either liquid or air. A similar heat transfer situation was adopted for a theoretical analysis of the thermal stresses in a thin circular disc subjected to a peripheral thermal shock. Experimental thermal shock tests were then conducted on rock specimens to check the analytical results. Specially insulated quartzite, basalt and taconite discs were shocked in either liquid or still air bath at various rates of heat transfer. The work was done in order to resolve the question as to whether theoretically determined tensile stresses are actually realized in a finite rock body undergoing thermal shock. Specifically, if theory predicts that the tensile strength of a rock should be exceeded in a particular type of controlled thermal shock, will fracture occur? This information is needed by Bureau researchers working on thermal and electrical rock fragmentation methods. The object of this paper is to present the main features of the theory and procedure being used in the authors' approach to quantitative prediction of rock response to a thermal shock. THEORETICAL ANALYSIS In the analysis to follow, simple geometry of a thin circular disc is considered. The disc is assumed to be isotropic, homogeneous and perfectly elastic, and to have constant thermal and mechanical properties. The effect of radiation is neglected so that heat is transferred by conduction inside the disc and by convection with its surrounding. In addition, the end

Jan 1, 1967

By J. D. Verhoeven

The effectiue distriblltion coefficient has been Measured in a series of vertical, normal freezing experirtzents with large current densities passing through the solid-liquid interface. The results indicate that the effect of the current on solute redistribution is due to electvotransport in the liquid. The high currents produced extensive mixing in the liquid which was considerably reduced by solidifying in small lubing. Analysis of the convection indicates that it probably vesulls from a horizontal temperature gradient produced by the Joule heating- of the electvic crirver~t. Due to the strong dependence of this convection upon the specimen radius, it is conclnded that only for specit~ens with radii of less than somewhere between 1 and 2 mm wilt electric field freezing be getlerally effec-tire at enhancing the purification of zone-melting experittierats in loe-melting alloys. Experiments on 0.8-mm lubes illustrate some interesting potential applications of this techniqne as a means of solute control on smcrll specimens. In a number of papers published within the last few years'-4 it has been found that passage of large dc currents through the solid-liquid interface of a freezing alloy produces a change in the solute redistribution accompanying the solidification. It had been predicted theoretically by Hucke et al.s and by Pfann and Wagner that such an effect would occur as the result of electrotransport within the liquid boundary layer at the solid-liquid interface. These authors independently derived the following relation between the effective distribution coefficient and the variables of the process: Where k0 is the equilibrium distribution coefficient, V is the mobility of the solute relative to the solvent, E is the electric field intensity, D is the solute diffusion coefficient, R is the rate of interface motion, and 6 is the boundary layer thickness. Both groups of authors show that this equation predicts the possibility of extending the purification ability of zone-melting experiments by the addition of an electric current. However, there are other effects in addition to electro-transport which could be produced by the high dc current and might, perhaps, invalidate the applicability of Eq. [I]. For example, high electric current might affect the interface reaction or perhaps the equilibrium distribution which was assumed to exist at the interface. It was the purpose of this work to determine the applicability of Eq. [I] by systematically investigating a simple system for which all of the necessary parameters were known. It was of particular interest for speculating on the potential usefulness of this technique to determine the maximum practical field intensities obtainable, and the effect of these high fields upon convective mixing in the liquid. The initial work in this study was published in a previous paper3 which will be referred to as I. In that work, a current density of 2000 amps per sq cm was used with specimen diameters of 5 mm. The results gave a qualitative confirmation of Eq. [I.], and also showed that a large amount of convective mixing was produced in the liquid by the current. The present study is an extension of that work to smaller specimen diameters and higher current densities. Two points were overlooked in I and will be emphasized here: a) the value of ko has not been well-established in the Sn-Bi system and b) the observed convection could be due to thermal convection produced from the Joule heating. EVALUATION OF k0 To evaluate Eq. [ I.] it is necessary to know the value of the equilibrium distribution coefficient, k,. Tn I the value of k, was taken as 0.3 from a published phase diagram.7 According to ansen' the best data on the phase boundaries of the Sn-Bi system are those of Davidson.5 The data of Davidson give a k, value ranging from 0.21 to 0.25 for the compositions studied in this work, or an average value of around 0.23. In a recent publication, Rigaud and Tougas'10 determined ko by means of a solidification technique. For an alloy of approximately the same composition as that used in this work they obtained a ko value of 0.39. Hence, there is considerable uncertainty in the value of ko and, consequently, a series of experiments were made to determine k, more accurately.

Jan 1, 1968

By P. Bardzil, J. Gurland

An experimental study of the variation of transverse-rupture strength with composition Anexperimentaland grain studysize has shown that the strength reaches a maximum for values of the mean free path between carbide particles of 0.3 to 0.6 microns. The fracture oforiginates in and proceeds through the carbide grains mainly. Impact strength and hardness also were recorded. MOST of the physical properties of sintered carbides vary linearly with composition. The transverse-rupture strength, however, shows a unique behavior. As the amount of binder metal is varied from 6 to 25 pct by weight, the strength at first increases; then, between 15 and 20 pct Co, it reaches a maximum of nearly 400,000 psi, and finally decreases with further additions of binder metal. This behavior of the transverse-rupture strength has been reported, among others, by Englel and Sandford and Trent.' The significance of these observations has not been discussed in the literature. That it may be of more than specific importance is indicated by the very similar variation of strength with composition encountered in other systems sintered in the presence of a liquid phase, such as Tic-Ni3 and Fe-Cu.' Experimental Details All compacts were prepared and sintered according to normal industrial practice. The average diameter of WC grains and the mean free path between grains were measured on metallographically prepared samples by a method of linear and planar analysis sing the relations where d is the average diameter of dispersed grains; Nl is the number of noncontiguous grains intersected on a metallographic plane by a line of unit length; N, is the number of noncontiguous grains per unit area; P is the mean free path between grains of dispersed phase; and f is the volume fraction of dispersed phase. Approximately 1000 grains were counted on each sample. For each composition d2 was plotted against P, the resulting straight lines serving as a check on the measurements. The distribution curves of the WC powders of different average diameters were homologous, and no attempt was made to influence the grain size by blending powders, adjusting the sintering conditions, or otherwise altering the particle size distribution. Densities were measured by differential weighings in air and water. The degree of densification did not vary consistently with either composition or grain size. The density is influenced by slight amounts of impurities, specifically by 0.1 to 0.2 pct Fe which enters the powders during ball milling. As an illus- -tration of the experimental variations, a number of measured densities are listed in Table I. They are expressed in percentage of theoretical density, as calculated from the published X-ray densities of WC and Co.' For the purpose of determining the transverse-rupture strength, rectangular test specimens (3/16x 3/8x3/4 in.) were broken by loading at the center of a 9/16 in. span. The average strength of five or more samples is reported for each composition and grain size. The compacts were ground on two parallel surfaces only. The load was applied at an average rate of 6,800 psi per sec. Since the elongation after fracture of the alloys is very small, it was assumed that the compacts deform elastically to failure and the fracture stress was calculated by the conventional beam formula. The data for one alloy are presented in Table II as an example of the results and scattering ranges encountered. The precision of the test, as measured by the average difference between duplicates, is of the order of 15,000 psi. The results are strictly comparable only to compacts prepared and tested in the manner described and of similar chemical composition and grain size characteristics. Unnotched Charpy specimens were used for impact testing. Each point represents the average of 3 to 20 samples, the larger number being used in an attempt to determine the influence of grain size. Considerable scatter was encountered, the range from lowest to highest value often amounting to 30 pct of the impact strength. The hardness is reported as a Ra reading, using a 60 kg load with diamond brale indenter. Compositions are given in weight percent.

Jan 1, 1956

By Fred H. Poettmann

The vaporization characteristics of carbon dioxide in a League City natural gas - Billings crude oil system were studied at three temperatures, 38°. 120°, and 202°F and for pressures ranging from 600 to 8,500 psi. Variation of carbon dioxide concentration up to 12 mole per cent in the composite showed no effect on the equilibrium vaporization ratios (K values) of the hydrocarbon constituents or on the K value of carbon dioxide itself. It was shown that carbon dioxide is more soluble in crudes than in distillates which is contrary to the behavior of methane. A working chart of carbon dioxide K values is presented. INTRODUCTION The study of the equilibrium vaporization ratios of mixtures of paraffin hydrocarbons has been rather thorough.2,6,7,8,9 In the past few years considerable attention has been paid to the vaporization characteristics of the so-called noncondensable gases such as nitrogen, carbon dioxide, and hydrogen sulfide in mixtures of hydrocarbons. since they usually occur to some extent in most crude oils and natural gases.1,3,4,5 Knowledge of this behavior is useful to both the production and refining phases of the petroleum industry. This paper reports the equilibrium vaporization ratios (K's) of carbon dioxide in a mixture of League City natural gas and Billings crude oil, and compares them to those obtained in a natural gas-distillate system. The equilibrium vaporization ratios for the hydrocarbon components in this system had previously been studied by Roland.' In addition to the determination of the K values for carbon dioxide, the K values for methane and ethane were also determined in order to observe what effect, if any, the presence of carbon dioxide had on these K values. The concentration of carbon dioxide was also varied in order to observe the effect of this variable on the carbon dioxide K values. EXPERIMENTAL PROCEDURE The apparatus used in this study cotlsisted of a stainless steel equilibrium cell of about 2 liters capacity. The cell was mounted on trunions permitting rocking in a thermostatically controlled oil bath. Two high pressure valves fitted with steel tubing were mounted on the top of the cell. one was used for sampling the equilibrium gas phase and the other for sampling the equilibrium liquid phase by means of an induction tube within the cell. Stainless steel tubing from the bottom of the cell led to a mercury reservoir and manifold which was connected to a free-piston type pressure gauge manufac- lured by the American Instrunlent Ctr. and to a volumetric. putrip. The temperature of the oil bath was measured by means of a ralibrated mercury-in-glass thermometer. The recorded temperatures are believed to be accurate to ±0.5 °F. The pressures are correct to 22 psi. The crude oil used in this study was stock tank oil obtained from the Wilcox formation in the Billings Field, Noble County. Okla. The natural gas was obtained from the League City Field. Galveston County, Tex. The oil was treated with anhydrous calcium sulfate in order to remove the last traces of water. To insure a supply of constant composition gas at room temperature the cylinders of League City gas were cooled to about 30°F, inverted, and the condensed liquid was allowed to drain from the cylinders. The analysis of the gas and crude are tabulated in Table I. The carbon dioxide came from Pure Carbonic, Inc., and was .stated to have a purity of 99.5 per cent or better. The procedure used to obtain samples of the equilibrium liquid and vapor was similar to that employed by others making use of the rocking type equilibrium cell.6,7,8 The equilibrium cell was evacuated and calculated quantities of carbon dioxide, natural gas, and crude oil were charged to the cell to the desired pressure. In charging the equilibrium cell an attempt was made to maintain the ratio of the natural gas to crude oil as close as possible to that employed by Roland. After the cell was charged, samples of

Jan 1, 1951

By Fred H. Poettmann

The vaporization characteristics of carbon dioxide in a League City natural gas - Billings crude oil system were studied at three temperatures, 38°. 120°, and 202°F and for pressures ranging from 600 to 8,500 psi. Variation of carbon dioxide concentration up to 12 mole per cent in the composite showed no effect on the equilibrium vaporization ratios (K values) of the hydrocarbon constituents or on the K value of carbon dioxide itself. It was shown that carbon dioxide is more soluble in crudes than in distillates which is contrary to the behavior of methane. A working chart of carbon dioxide K values is presented. INTRODUCTION The study of the equilibrium vaporization ratios of mixtures of paraffin hydrocarbons has been rather thorough.2,6,7,8,9 In the past few years considerable attention has been paid to the vaporization characteristics of the so-called noncondensable gases such as nitrogen, carbon dioxide, and hydrogen sulfide in mixtures of hydrocarbons. since they usually occur to some extent in most crude oils and natural gases.1,3,4,5 Knowledge of this behavior is useful to both the production and refining phases of the petroleum industry. This paper reports the equilibrium vaporization ratios (K's) of carbon dioxide in a mixture of League City natural gas and Billings crude oil, and compares them to those obtained in a natural gas-distillate system. The equilibrium vaporization ratios for the hydrocarbon components in this system had previously been studied by Roland.' In addition to the determination of the K values for carbon dioxide, the K values for methane and ethane were also determined in order to observe what effect, if any, the presence of carbon dioxide had on these K values. The concentration of carbon dioxide was also varied in order to observe the effect of this variable on the carbon dioxide K values. EXPERIMENTAL PROCEDURE The apparatus used in this study cotlsisted of a stainless steel equilibrium cell of about 2 liters capacity. The cell was mounted on trunions permitting rocking in a thermostatically controlled oil bath. Two high pressure valves fitted with steel tubing were mounted on the top of the cell. one was used for sampling the equilibrium gas phase and the other for sampling the equilibrium liquid phase by means of an induction tube within the cell. Stainless steel tubing from the bottom of the cell led to a mercury reservoir and manifold which was connected to a free-piston type pressure gauge manufac- lured by the American Instrunlent Ctr. and to a volumetric. putrip. The temperature of the oil bath was measured by means of a ralibrated mercury-in-glass thermometer. The recorded temperatures are believed to be accurate to ±0.5 °F. The pressures are correct to 22 psi. The crude oil used in this study was stock tank oil obtained from the Wilcox formation in the Billings Field, Noble County. Okla. The natural gas was obtained from the League City Field. Galveston County, Tex. The oil was treated with anhydrous calcium sulfate in order to remove the last traces of water. To insure a supply of constant composition gas at room temperature the cylinders of League City gas were cooled to about 30°F, inverted, and the condensed liquid was allowed to drain from the cylinders. The analysis of the gas and crude are tabulated in Table I. The carbon dioxide came from Pure Carbonic, Inc., and was .stated to have a purity of 99.5 per cent or better. The procedure used to obtain samples of the equilibrium liquid and vapor was similar to that employed by others making use of the rocking type equilibrium cell.6,7,8 The equilibrium cell was evacuated and calculated quantities of carbon dioxide, natural gas, and crude oil were charged to the cell to the desired pressure. In charging the equilibrium cell an attempt was made to maintain the ratio of the natural gas to crude oil as close as possible to that employed by Roland. After the cell was charged, samples of

Jan 1, 1951

By J. A. Goebel, S. Rosen

IN the NiAl phase diagram the NiAl (CsC1-type) phase field extends over a large composition range. At elevated temperatures the nickel-rich phase boundary extends to a composition of about 70 at. pct Ni, a value which is within 5 at. pct of the Ni3A1 (Cu 3 Au-type) phase boundary.' At room temperature, however, the maximum nickel content is only about 60 at. pct. Experiments have shown that alloys containing greater than 63 at. pct Ni when quenched from temperatures below 1000°C contain the equilibrium phases NiAl and Ni3A1. On the other hand, when these same alloys are quenched from temperatures above 1000°C and examined microscopically, a typically martensitic decomposition product appears in the microstructure as shown in the micrograph of Fig. 1. The structure of the martensitic phase has been determined by employing powder X-ray diffraction techniques to be an "ordered" AuCu type (Strukturbericht Llo, space group P/4 mmm - DL). The diffraction pattern of this phase differs from that of AuCu in the appearance of superlattice lines. The structure is shown in Fig. 2. The open circles represent nickel atoms and the half-shaded circles represent nickel and aluminum atoms which are randomly distributed. The sites represented by half-shaded circles would be occupied solely by nickel atoms at a stoichiometry of Ni3A1. The alloys used in this investigation were prepared from 99.99 wt pct Al and 99.99 wt pct Ni by arc melting charges of varying compositions in a water-cooled copper hearth using a tungsten electrode in a gettered argon atmosphere. In all cases chemical analysis agreed within $ at. pct with the nominal compositions of the alloys. Annealing treatments were carried out in a vertical resistance furnace through which a stream of argon gas was flowing. Specimens, which were wrapped in tantalum foil, were quenched by allowing the specimens to drop into a bucket containing iced brine. X-ray diffraction patterns were obtained from -325 mesh powder specimens by using a 114.8-mm

Jan 1, 1969

By E. T. Turkdogan, W. L. Worrell

The rate of reaction of hydrogen sulfide with ferrous sulfide was studied by measuring the initial rates of sulfidation of iron strips in hydrogen sulfide-hydrogen-argon mixtures at 670°, 800°, and 900" C. The time-dependent surface sulfur activity is derived from the instantaneous rate of sulfidation with the assumption that diffusion in the sulfide layer is in a pseudo-steady state with the gas-sulfide chemical reaction. The rate of sulfur transfer from hydrogen sulfide to the surface of iron sulfide is proportional to the partial pressure of hydrogen sulfide and inversely proportional to the activity of sulfur at the surface of the sulfide layer. The derived rate equation is based on the assumption that most of the surface sites on the chemisorbed layer of iron sulfide are occupied by sulfur atoms and that the slow rate-controlling reaction is the dissociation of hydrogen sulfide on the chemisorbed layer. The experimental results are in reasonable accord with this reaction model. 1 HE slow approach to parabolic growth rate in the sulfidation of iron in hydrogen sulfide-hydrogen mixtures is a manifestation of slow approach to surface equilibrium between the gas and the surface of the sulfide layer. For example, at 800°C and Fig. 7 in Part I, the parabolic growth rate begins after approximately 1 day of sulfidation time. With decreasing temperature and decreasing partial pressure of hydrogen sulfide, the time necessary to reach gas-sulfide surface equilibrium is much longer. These observations are similar to those reported previously by Turkdogan et al.' on the oxidation of iron to wustite in hydrogen-water vapor mixtures. The slow approach to gas-sulfide equilibrium is well-demonstrated by the results in Fig. 1 where the square of the weight gain per unit area, ( g S per sq cmI2, is plotted against time for gas mixtures having PH g//>H = 1.0 with 0, 25, 50, and 67 pct Ar at 800°C. The value of 1.5 X lo-' (g S per sq cm)' corresponds to almost complete sulfidation of the iron strip (- 0.05 cm thick) to iron sulfide. The points fall on S-shaped curves. If the inflection parts of the curves are considered to be linear, thus indicating parabolic growth rate and the establishment of gas-sulfide equilibrium, their slopes would have to be the same for a fixed ratio in the gas mixture. Such is not the case, and the slopes for the "linear" parts of the S-shaped curves are lower than the value when gas-sulfide surface equilibrium is established. The subject matter of this paper is the kinetics of the surface reaction of hydrogen sulfide with iron sulfide during the early stages of sulfidation of an iron strip. EXPERIMENTAL RESULTS The apparatus and materials used were the same as those discussed in Part I. In the present experiments of relatively short duration, a purified iron strip, 5 by 2 by 0.05 cm, which was suspended in the uniform hot zone of a vertical zircon tube, reacted with a flowing gas mixture of hydrogen sulfide-hydrogen-argon. The sample was suspended from a gold chain attached to a calibrated silica spring. The amount of sulfur picked up by the iron, which formed a layer of iron sulfide, was determined by measuring the displacement of a reference point on the silica spring, using a cathetom-eter. In all cases, the degreased sample was first annealed in a stream of oxygen-free dry hydrogen for several hours to remove any impurities such as oxygen, nitrogen, or carbon which might have been present on the surface of the sample.' The rate measurements were carried out at 670°, 800°, and 900° C in hydrogen sulfide-hydrogen-argon mixtures with pH2 s/Ph2 ratios from 4 to 0.1. In a few experiments of short duration no sulfur deposition was observed in gas mixtures with (comments concerning sulfur deposition at high pH s/ph ratios were made in Part I.) Typical examples of the results obtained are shown in Fig. 2 for two temperatures and two gas compositions. With the present experimental technique, reproducible rate data could be obtained only after a uniform

Jan 1, 1969

By Walter M. Stephen

MODERN developments in alloy steels have been so rapid and diverse that engineering practice has scarcely had time to re-appraise all items of past experience wherein conclusions became axiomatic under conditions that no longer apply. A case in point is the wet screening of abrasive ores within the fine range still looked upon as belonging exclusively to classifiers. By virtue of the development of stainless steels (18 per cent Cr, 8 per cent Ni), it is no longer true that classifiers are more economical than screens in closed circuit with large-tonnage ball or rod mills at 65 or even 100 mesh, provided a selective overgrind of the higher-gravity constituents of the ore is not desired. Wet screening of ores is a highly corrosive as well as an abrasive operation, because of the inevitably high degree of oxygenation of the water. Screen cloth of ordinary or spring-steel wire almost at once becomes pitted arid covered with a film of corrosion products, which causes rust-blinding of fine-mesh screens and offers high frictional impedance to the flow of ore particles. On the other hand, the well-known properties of stainless steel enable it to maintain a bright surface, and so to eliminate blinding either by ore particles or by corrosion products. That a large-tonnage mill grinding hard ore to 65 mesh can be operated economically in closed circuit with screens instead of classifiers has recently been demonstrated at the Copper Cliff concentrator of the International Nickel Co.; in the test to be described, a 6 ½ by 12 ½ -ft. Marcy rod mill ground from 625 to 820 tons of ore per day to approximately 65 mesh, operating in closed circuit with three 4 by 5-ft. Hum-mer screens, without any classifier. Stainless-steel cloth gave an indicated life of several months. There was no difficulty with blinding, yet dilution and spray water could be controlled so that screen undersize averaged not less than 40 per cent solids. In contrast, ordinary carbon steel was pitted and blind with rust within 40 hours.

Jan 1, 1938

By P. L. Rittenhouse, M. L. Picklesimer

A rapid and seniquantitative method of determining prefered orientation on large numbers of. Zircaloy-2 specimens was desired. knoop microhardness measurerrzetzls were irvestigated as a solldtion to this pro6lem. The variation of Knoop microhardness measurerlerzts on selected planes as a function of 'irzdenle axis relutilje lo cryslallograplzic or fabrication divectals were used to corzstrrcl a polar coordinate hardness contour map. With use of an empirical relationslip between the single-crystal hardnesses and those of the polycrystalline material conentional pole figures could be constructed which compare favorably also obtained. To determine preferred oriention qualitatively from hardness data requires a minimum of twelve measurements per plane on three, preferattention to grain size, specimen prepartion, and in-rreinetzt, and analjlsis is of the order of- 45 to 60 rrin. THE design of structures from Zr alloys requires consideration of preferred orientation and the resulting anisotropy of mechanical properties. Rapid and semi-quantitative methods of evaluating anisotropy and of determining preferred orientation are needed for quality control and for examining the large number of test specimens required in development programs. The variation of Knoop microhardness with indenter orientation has been studied in single crystals of several hcp metals including titanium.' beryllium,' magneium, and zinc.4 The maximum hardness observed on any crystallographic plane other than the basal plane invariably occurred when the long axis of the Knoop indenter was either parallel or perpendicular to the projection of the [ OOOI.] direction on the plane of examination. When the major slip mode was (0001)(i2i0j the maximum hardness occurred at the parallel positio! but when the operating slip system was {10i0) (i210) the hardness was a maximum perpendicular to the [0001] projection. A minimum hardness was always observed at a rotation of 90 deg from the maximum. It follows that the orientation of the projection of the [0001] can be determined on any non-basal plane by making hardness measurements at a number of indenter orientations. The determination of the orientation of the [0001] projection on two non-parallel, preferably orthogonal, surfaces of the specimen will allow location of the [0001] direction in the specimen. It seems possible that such measurements could be used to examine, at least qualitatively, the preferred orientation existing in polycrystalline hcp materials. An investigation of the microhardness anisotropy in Zircaloy-2 was undertaken to ascertain whether these measurements could be used for this task. EXPERIMENTAL PROCEDURE Single crystals of Zircaloy-2 were grown by an a-8-a annealing sequence using electron-beam heating.= The orientation of the crystals was determined by a conventional back-reflection Laue technique. The crystals were then mounted on a goniometer head and the desired crystallographic faces were milled and chemically polished. Polycrystalline Zircaloy-2 specimens were prepared from fabricated sheets or plates. Inverse pole figures for these materials were obtained using the X-ray diffraction techniaue described by Jetter, McHargue, and illiams.' A Wolpert-Greis Micro-Reflex hardness-testing machine was used to make the Knoop microhardness measurements. The single-crystal and polycrystalline specimens were loaded to 0.5 and 2.0 kg, respectively. Determination of the scatter of hardness numbers as a function of applied load for several indenter orientations on several specimen surfaces showed that the loads selected were the lightest consistent with minimum scatter. Heavier loads did not appreciably decrease the scatter and produced hardness impressions too large to be conveniently measured with the equipment used. Seven crystallographic planes of the single crystals were examined, while six planes of examination were used in studying Zircaloy-2 polycrystals. The specimens were rotated 10 to 15 deg after each measurement and from four to eight impressions were made at each angle of rotation. RESULTS The two angles which were used to relate crystallographic directions and planes in the hcp cell to the planes of examination of the single crystals are shown in Fig. 1. 8 is the angle between the c axis. [0001]. and the normal, N, to the plane of examination. a is the angle between the long diagonal of the Knoop indenter and the projection of the c axis on the plane of examination. For exampIe, if P = 90 deg and a = 0 deg, the plane of examination is of the family

Jan 1, 1967

By C. B. Daellenbach, T. D. Tiemann

The prevention of quartz flotation by chelation of activating ions with the tetrasodium salt of EDTA in oleic acid flotation was investigated using a small vacuum flotation cell. It was found that flotation of quartz could be entirely suppressed in the presence of activating ions during complete flotation of hematite. It was further shown that the concentration of activating ions liberated from Wisconsin Gogebic taconite is sufficient to float quartz in an oleic acid system. Large tonnages of low grade siliceous iron ores occur on the iron ranges of the Lake Superior district. Although the lower grade nonmagnetic types are currently not of economic importance, they constitute a large future potential source of iron and steel, and hence have been the subject for extensive research on their beneficiation. TACONITES Of particular interest to the Dept. of Minerals and Metals Engineering at the University of Wisconsin have been the low grade nonmagnetic taconites of the Wisconsin Gogebic Range. These occur as five members of the iron formation and have been described in detail elsewhere.' Essentially they consist of an intimate mixture of hematite, goethite and quartz, with minor amounts of siderite, magnetite, iron containing silicates, and manganese minerals. A typical mean analysis based on the Bureau of Mines analyses' is: SiO2-52.50%, Fe2O3-43.40%, (Fe-30.38%), A12O3-1.15%, P2O5-0.07%, Mn2O3-0.29%, CaO-0.07%, (S-0.03%), Loss on ignition-2.00%. The quartz in these ores is of a microcrystalline variety,2 and so intimately associated with the iron oxide minerals that extremely fine grinding, in the order of minus 325 mesh, is required for liberation. During grinding and subsequent flotation, the concentration of quartz activating ions in the pulp becomes sufficiently high to activate quartz which floats along with the iron minerals in the presence of oleic acid. cook3 and co-workers concluded that oxidized iron ores released appreciable quantities of quartz-activating ions in water pulps. This is shown to be true in the present investigation. As a matter of fact, application of this phenomenon, as well as the intentional addition of activating calcium ions, is made use of in the an ionic flotation of silica from the iron oxide minerals.4,5 In view of the above, it becomes almost impossible to effect a sharp separation of quartz in the oleic acid flotation of the iron oxide minerals from these taconites, even with satisfactory liberation. This fact led to the current investigation to find a means of linking the activating ions with a chelating agent. The aim was to establish basic data for the quartz-water-oleic acid system which might not only be applicable to iron ores, but also to the flotation of other siliceous ores as well. EXPERIMENTAL METHODS Vacuum Flotation Cell: The vacuum flotation used in this investigation is similar to that used by previous investigators.6,7,8 The cell consisted of a 100 ml graduated cylinder with the lip removed. Vacuum from a water aspirator was applied to the cell through a trap; suitable tubing, and a rubber stopper inserted in the top of the cell. Constant absolute pressure was maintained by means of a manometer connected to the trap with a tee. Flotation: The required amount of activating ion solution was pipetted into a beaker. This was then diluted to 99.0 ml with water having a pH below that desired for the test, or so adjusted with HC1. After addition of 1.0 ml of oleic acid solution (2.0 mg oleic acid per ml), the pH was readjusted to the desired value with NaOH, and the entire solution transferred to the cell containing 1.5 gm of quartz. After vigorously agitating the cell and its contents for 2 min, the vacuum was applied to the cell and the estimated degree of flotation observed for a 3-min period. Activating ions studied included Ca++, Mg++, Al+++, and Fe+ + + added as chloride solutions. In addition,

Jan 1, 1964

By Frank C. Greene

Missouri has had one of the best years in history in the development of gas, the 49 completed gas wells having an average of nearly 1,000,000 cu. ft. initial open flow. Altogether 101 wells were drilled in the western part of the state, from Andrew County on the north to Vernon County on the south. Of these 49 were gas wells (including four old wells drilled deeper) with an initial open flow of 48,850,295 cu. ft., eight were oil wells (including one old well drilled deeper) with an initial capacity of 125 bbl. per day and 44 were dry holes (including five old wells drilled deeper). All the oil wells were in previously discovered pools in Jackson and Cass Counties. The outstanding discovery was a "shoestring" of a sand that is termed the Bartlesville, trending northwest and southeast across townships 48 and 49 N., R. 32 W., in central Jackson County. The sand is believed to be a narrow channel or bar, probably not over 800 ft. wide, lying at a higher horizon than the Bluejacket or true Bartlesville sand. A total of 32 wells with 47,453,080 cu. ft. initial open flow has been completed along the 6 miles of the shoestring. The largest individual well had an open flow of 4,500,000 cu. ft. The depth of these wells ranges from 350 to 635 ft., depending on surface elevation. The rock pressure ranges from 145 to 169 pounds. The Missouri Valley Gas and Oil Co. and Panhandle Eastern Pipe Line Co. have laid pipe lines into the area and most of the wells are now connected. In other parts of Jackson County and in other counties of the state there was very little activity during 1937. Of the 101 completions, 88 were in Jackson County. Cass County had five oil wells and three dry holes, Bates County one dry hole and Vernon County two dry holes. In the northern counties, Andrew and Clinton were represented by one dry hole each. At the end of 1937 drilling and leasing operations were very active and wildcatting promises to feature the coming year.

Jan 1, 1938

By C. Wert, P. Bunn

Determination of the solid solubility of gases in metals is usually done by one of two methods. The first is an additive method, in which measurement is made at temperature of the maximum amount of gas absorbed by an initially degassed piece of the metal. Gas additions are made until the dissolved gas first comes into equilibrium with a compound. This method is most useful at relatively high temperatures where the amount of gas absorbed is relatively large and where equilibration of the dissolved gas with the gas atmosphere can be achieved in a relatively short time. The second is a precipitation method. A supersaturated solution of the gas in the metal is held at temperature until equilibrium is established between the gas atoms in solution and a compound. The quantity of dissolved gas is then determined by some physical measurement which is sensitive only to the gas in solution. This method is generally useful in low temperatures. This paper describes measurement of solubility of nitrogen in tantalum whereby measurements at low temperatures using internal-friction methods are plotted together with existing measurements at high temperatures. The solubility is thereby known from less than 0.5 at. pet at 350°C to near 13 pet at 2300°C. Several measurements have been reported of the solubility of nitrogen in tantalum. These are collected in Fig. 1. Three single determinations by Ke,1 Andrews,2 and Brauer and zapp3 are plotted along with a series of measurements by Vaughn, Stewart and schwartz4 and Gebhardt, Seghezzi, and Fromm.5 Although not much doubt exists about the solubility being in excess of 10 at. pet above 2000°C, the solubility indicated at low temperatures depends on whose data are selected as being most reliable. The variation is enormous, being at least an order of magnitude at 500°C. Accordingly, a measurement was begun to examine this discrepancy. The method of measurement finally selected was that of internal friction. A solid solution of nitrogen in tantalum was prepared by heating a tantalum wire in a dilute at-

Jan 1, 1964