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By G. E. Pellissier, P. H. Salmon Cox, B. G. Reisdorf

Banding that occurred in plates rolled from the early production heats of 18Ni(250) maraging steel is described and related to the segvegation of certain alloying elements (nickel, molybdenum, titanium), the extent of which was quantitatively evaluated by means of electron-microprobe analysis. The effect of banding on mechanical properties is discussed, with particular reference to observed directional differences in plane-strain fracture toughness of plates. It is shown that banding originates as interdendritic segvegation during ingot solidification and persists in some degree through normal soaking and hot reduction to plate. The results of the study showed that heating sections of small laboratory-cast ingots at 2200°F for 4 hr was sufficient to markedly reduce microsegregation and to considerably improve mechanical properties. Hot rolling of 7-in.-thick ingot sections to 1/2-in.-thick plate effected a similar reduction of microsegregation, but resulted in even greater increases in ductility and toughness than that obtained by homogenization treatment alone. DURING the past few years, considerable attention has been directed towards the low-carbon, high-alloy maraging steels and in particular towards the 18Ni-8Co-5Mo-0.4Ti alloy. The steels of this group, having an excellent combination of high strength and toughness, have a number of advantages over their more conventional medium-carbon low-alloy, quenched-and-tempered counterparts. In the annealed condition, the maraging steels are in the form of a ductile marten-site; aging at a relatively low temperature, typically 900°F for 3 hr, increases greatly the strength through the precipitation of intermetallic compounds. One problem in the early production heats of maraging steel was that the finished plate frequently displayed a banded structure. Previous work on other steels1-' had established that banding in wrought products is either a direct or an indirect consequence of chemical segregation, which occurs during solidification and persists to some extent through normal thermal and mechanical treatments. For example, Smith and others: in a study of low-alloy steel, were able to correlate the severity of banding in the wrought product with the degree of interdendritic segregation of nickel and chromium in the as-cast ingot. The effect of banding on the mechanical properties of steels is usually considered to be detrimental, although there is only limited evidence to suggest that a marked improvement in properties can be obtained with less heterogeneous structures. Comparison of the longitudinal and transverse tensile properties of banded and of homogenized 4340 steel showed that only the transverse ductility was improved by homogenization, but even then the improvement was not commercially significant.' Conversely, homogenization of through-the-thickness tension specimens of quenched-and-tempered steel plate, containing 1.47 pct Mn, increased the strength by as much as 10 pct and the tensile ductility by at least a factor of twos5 This improvement was related to the elimination of manganese-rich bands, which also are one of the factors responsible for cold cracking in the heat-affected zone of metal-arc welds.7 In the present study the nature and severity of banding in early commercial 18Ni(250) maraging steel plate and in laboratory-melted 18Ni(250) maraging steel plate was determined. The effects of banding on plane-strain fracture toughness and the effects of thermal homogenization treatments on the strength, tensile ductility, and toughness of 18Ni(250) maraging-steel as-cast ingots and rolled plate were evaluated. In addition, the effects of hot deformation by rolling on the mechanical properties of ingots were determined. 1) STUDIES OF BANDING IN EARLY PRODUCTION PLATE The chemical composition of the steel (A) used in this part of the investigation is shown in Table I. Banding was not clearly evident in either as-rolled or annealed* plate, but annealed and agedc** plate had a banded structure. The typical banded condition, Fig. 1, consists of layers of unetched austenite (white) and dark-etching martensite in a light-etching martensitic matrix. X-ray diffraction measurements showed that this steel contained more than 6 pct austenite. An electron-probe X-ray microanalyzer (using a focused beam of electrons) was used to determine the composition of the bands and of the material between the bands with respect to the main alloying elements— nickel, molybdenum, titanium, and cobalt. The recorded X-ray intensities were converted to concentration values with the use of a standard of similar composition. To facilitate probe positioning, all analyses were conducted on specimens that had been given a light etch. The influence of this etching on the analytical results was negligible; analyses made on the identical area before and after etching yielded essentially the same concentration values. The results of the electron-microprobe analyses at selected points revealed that the layers of austenite and adjacent dark-etching martensite contained greater amounts of nickel, molybdenum, and titanium than did the surrounding matrix, Table 11. The austenite layers

Jan 1, 1968

By L. W. Casteel

This is a story of progress through research, invention and innovation-progress that made a small mine in Missouri into a large and prosperous corporation. The St. Joseph Lead Co. was founded in Borne Terre, Missouri, in 1864. At that time, the mine consisted of a narrow trench eight feet deep; the mill was a hand-operated jig; and the smelter, a charcoal oven with a sloping hearth. During the first year, production was suspended for two months because of an invasion by the Confederate army. There have been few interruptions since that time.

Jan 7, 1964

By MCA Woolsey

(Butte. Meeting, August, 1913.). IN metallurgical circles it is known widely, but somewhat vaguely, that the ease of: reduction of metallic oxides depends largely on the way they have been prepared. It is likewise known that different forms of carbon have different and greatly varying reducing powers. It is the purpose of this paper to show somewhat more definitely and scientifically these facts. Some years ago the writer published an account of pyrometric determinations of the reduction- temperature of zinc oxides variously prepared and of several kinds.1 In said paper it was shown that the temperature it which zinc oxide evolves zinc according to the equation Zn0. +' C = Zn + CO depends upon the ;nature of:., the.' two reacting bodies. The determinations bad a range of accuracy of from 2° to. 6° C.,whereas differences were found to. amount to an extreme. of 90° C. :.86 the differences are real ones and must have, definite cause. The equation of boiling water, (H20)4 = 4 (H2O) has a fixed temperature for equilibrium of 100° C. at 760 mm. pressure. , In general, all equations. reacting e in .the liquid or the gaseous phase have-well-defined constant physical conditions which govern the equilibrium point and reaction velocities. In a reaction where we have one or more solid phases, the temperature conditions requisite for the unbalancing of the stable system are found to vary. These variations are due to the fact that in a solid there is a very complex molecule and it is not, a question solely of the tearing away of two interlocked atoms, but also of the destruction of a complex molecule containing hundreds, or possibly thousands, of smaller molecules.

Jan 7, 1913

By A. Kenneth Schellinger, O. Cutler Shepard

Overgrinding, Or the breaking of ore particles into sizes smaller than required for liberation, is a first-magnitude problem in grinding for concentration processes. The conventional ball mill-classifier circuit used in commercial grinding produces mineral particles that are all ground to pass an upper size limit, while the proportion of very fine sizes, or slimes, is uncon rolled. Calculations based on measurements made in commercial plants which were grinding ore for flotation concentration indicate that about go pct of the energy used in grinding is consumed in useless overgrinding.1 In addition to accounting for the consumption of a large amount of energy, over-grinding is detrimental to the flotation process. Overground slime coats larger partitles and inhibits selective action by the flotation reagents on particles which by themselves could be separated very well. A further difficulty is that extremely finely ground minerals do not respond satisfactorily to flotation-collecting reagents, and both selection and recovery decrease markedly with particles finer than 5 to 10 microns.2 conventional classifier-ball mill circuits inherently tend to overgrind the valuable minerals more than the gangue minerals because most valuable minerals are of higher density and are softer and more friable than the gangue minerals. The rem- edy to this situation would seem to be a separating mechanism which would separate free valuable mineral particles regardless of size and density considerations and a mechanism which would operate in the grinding mill so that valuable mineral grains would be removed from the grinding machine as soon as they are freed. A consideration of these ideas led the authors to the conception of a simultaneous grinding and flotation mechanism. So far as the authors are aware, such a machine has never been tried, even on a laboratory scale. Development oF Apparatus and Experimental Method Apparatus development went through several stages before a really workable machine was devised. Work was started with a large cast-iron mortar 7½ in. in diameter and 8 in- deep. A cast-iron disk Was mounted on the end of a vertical shaft SO that it fitted loosely into the bottom of the mortar. On top of the disk four radial cleats ¼ in. high were bolted to agitate the ball charge as the disk, or impeller, rotated. The vertical shaft was driven at 100 rpm by a mechanism improvised from an old coffee-mill type of grinder. A hole was drilled into the bottom of the mortar through which compressed air was introduced for frothing. In operation, more charges of Ore which had been crushed to pass an 8-mesh screen were placed in the bowl along with water and suitable reagents. The impeller was then started and the compressed air turned On so that the ore was ground while being exposed to air bubbles. Mineralized froth was

Jan 1, 1949

[A Aall, Christian H., M49 D Mgr, American Metal Climax, Inc., 61 Broadway, New York 6, N.Y. Aaroe, S. L., A54 B Sales Mgr, The W. S. Tyler Co. of Can. Ltd., St. Catharines, Ont., Canada Abalos, Teodulo Q., J57 A Foreman, Lepanto Cons. Ming. Co., Mt. Province, Philippines Abbass, G., M55 P. O. Box 680, Hong Kong, China . Abbitt, James M., A54 770 Sole Blvd., Bartow, Fla. Abdullah, M. Y., J53 Dept. of Mines Res. Div., P. O. Box 1016, Tiger Lane, Ipoh Perak, Malaya Able, John F., Jr., J53 A Ming Engr, USA SIPRE 1215 Washington Ave., Wilmette, Ill. Abell, Leo M., M31 B Conct Supt, Phelps Dodge Corp., Morenci, Ariz. Abenius, Hakan Wilhelm, M52 A Mng Dir, Stora Kopparbergs Bergslags AB, Falun, Sweden Abenoroth, Harry F., A57 Natl. Carbon India Ltd., 18A Brabourne Rd., Box 217, Calcutta, India Abercrombie, Harry W., J56 1645 Camphor Dr., Lakeland, Fla.]

Jan 1, 1961

By Hsun Hu, R. S. Cline

The effect of rate of deformation on texture formatiotz has been studied with cube-oriented single crystals of 3 pct Si-Fe, compressed 80 pct at two widely different rates. Compression at a low rate (crosshead speed, 0.1 ipm) produces large orienta-tional changes and coarse deformation bands, whereas little change in orientation is observed, particularly at the surface of the crystal, when compressed at a high rate (impact velocity, -500 ips). Thin plates of mechanical twins are produced at the high rate, but their contribution to the deformation texture is practically negligible. The crystal deformed at a high rate has a lower hardness and a more uniform dislocation structure and is morc resistant to recrystallization. There is also a dilference in the recrystallization texture between the slowly and rapidly compressed crystals. These results indicate that plastic flow is less "turbulent" at high strain rates than at low strain ratcs. THE behavior of metals under high-speed deformation has been the subject of wide study in the past decade. Most of these works were concerned with mechanical properties during testing at high rates of loading, the resulting structures, and the theoretical aspects of the observed phenomena. The present status of knowledge and research activities in this field has been documented in recent publications.17' There is, however, very little information available in the literature concerning the effect of high-speed deformation on the texture formation in metals. The possibility of an effect of rate of deformation on texture is suggested by the microstructural differences observed between normally and very rapidly deformed samples. Aside from the strong tendency for twinning (and phase transformation in certain metals) in high-speed deformation, the slip-line patterns and the dislocation configurations show marked differences as a result of large differences in the strain rates. For instance, in mild steel in static and dynamic compression, Campbell and co-worker3,4 observed that coarse slip occurred on several systems in specimens deformed at normal strain rates, whereas specimens deformed rapidly showed only fine slip on fewer systems, the slip-line pattern being very similar to that in specimens deformed at low temperatures and at normal strain rates. The absence of multiple slip was also noticed by Dieter5 in shock-loaded nickel. The dislocation configuration in an iron shock loaded at 70 kbar pressure was shown by Leslie et al.6 to be similar to that produced by light rolling at low temperature—the dislocation lines were mostly straight and uniformly distributed. These observations suggest that the mode of deformation at high strain rates is notably different from that at low strain rates. Consequently, the nature and the extent of lattice reori-entation during deformation should also be different. This investigation was undertaken to test this idea. MATERIAL AND METHOD The remaining part of a single-crystal ingot of a 3 pct Si-Fe alloy,* prepared for an earlier investi- gation,1 was used in the present studies. Specimens 9/16 in. square and 0.365 in. thick were cut from this ingot with (001) planes parallel to the square surfaces, and the [loo] and 1010] directions parallel to the edges of the specimen, within ±1 deg. These machined crystals were etched to remove distorted metal, and annealed at 1300°C for 24 hr in a purified helium atmosphere. The annealed crystals had a hardness of 161 Dph. The crystal orientation was rechecked with X-ray back-reflection techniques. In high-strain rate experiments the crystal was compressed in a Dynapak machine to approximately 80 pct reduction in thickness (from 0.360 to 0.070 in. with an impact velocity of -500 ips). Thus, the duration of loading was approximately 6x 10-4 sec, and the average strain rate was about 103 sec-1. As a result of this rapid, severe deformation, the specimen became a roughly circular thin disc. The original shape of the crystal, however, could still be recognized by a diffusely outlined square area in the center of the disc. For compression at a low speed, the crystal was deformed in a universal testing machine at a rate of crosshead movement of 0.1 ipm. Compared with

Jan 1, 1965

By P. E. Demmler

The apparatus in which the process of bright annealing of copper wire was carried out consisted of a section of iron pipe, 6 ft. long and 3 ft. in diameter. The pipe was provided with flanges to which were bolted the end plates for sealing, also with inlet and outlet tubes to allow for the displacement of the air in the pipe by natural gas. After charging with copper wire, sealing and displacing the air, the pipe was heated to 350' C. (662" F.). It was expected that the natural gas would furnish a neutral atmosphere which would prevent oxidation and give a satisfactory bright-annealed product. It was found, however, that the outer layers of wire were discolored and not suited for the use for which they were mtended. To obtain an idea of what was taking place in the annealing furnace, skeins of the hard-drawn wire were placed in a glass tube so that all changes in appearance could be observed as they were heated to different temperatures and under varying conditions. The temperature in each case was determined by means of a thermocouple placed in the tube close to the wire. Following is a summary of the results of these experiments: 1. When the wire was heated for 1 hr. in a current of natural gas at a temperature of 350") 400") or 500" C. (662", 752", or 932" F., respectively), there was a marked darkening of the wire throughout the skein. 2. When heated for 1 hr. in natural gas at a temperature of 600" C. (1112' F.), there was no coloration, the wire remaining clean and bright. 3. When heated in natural gas to 350" C. until darkened and the treatment continued with the temperature raised to 600' C., the coloration disappeared and the wire became clean and bright.

Jan 1, 1923

By P. E. Demmler

The apparatus in which the process of bright annealing of copper wire was carried out consisted of a section of iron pipe, 6 ft. long and 3 ft. in diameter. The pipe was provided with flanges to which were bolted the end plates for sealing, also with inlet and outlet tubes to allow for the displacement of the air in the pipe by natural gas. After charging with copper wire, sealing and displacing the air, the pipe was heated to 350' C. (662" F.). It was expected that the natural gas would furnish a neutral atmosphere which would prevent oxidation and give a satisfactory bright-annealed product. It was found, however, that the outer layers of wire were discolored and not suited for the use for which they were mtended. To obtain an idea of what was taking place in the annealing furnace, skeins of the hard-drawn wire were placed in a glass tube so that all changes in appearance could be observed as they were heated to different temperatures and under varying conditions. The temperature in each case was determined by means of a thermocouple placed in the tube close to the wire. Following is a summary of the results of these experiments: 1. When the wire was heated for 1 hr. in a current of natural gas at a temperature of 350") 400") or 500" C. (662", 752", or 932" F., respectively), there was a marked darkening of the wire throughout the skein. 2. When heated for 1 hr. in natural gas at a temperature of 600" C. (1112' F.), there was no coloration, the wire remaining clean and bright. 3. When heated in natural gas to 350" C. until darkened and the treatment continued with the temperature raised to 600' C., the coloration disappeared and the wire became clean and bright.

Jan 1, 1923

By JOHN R. SUMAN

OVERWHELMING proof of the importance of oil in a modern national economy is afforded by the present European War. Treat¬ies and national boundaries have been cynically violated to secure greater supplies of the precious fuel. Petroleum substitutes have been desperately, and far from successfully, sought. The whole German military theory of the drang nach Osten, the drive to the East, is directed at cutting the British supply of oil and securing a supply for Germany. This is a war of machines, and the machines of war feed hungrily on oil. In view of this fact, it is surely comforting to know that we are living today in a nation which has surpassed all the rest of the world not merely in unearthing the raw supplies of petroleum which lie beneath its surface but also in every phase of the industry in mining, refining, processing, production, and distribution.

Jan 1, 1941

By L. Guttman

THE equilibrium diagram of the indium-thallium system was of interest to us in connection with a study of the superconducting properties of metallic solid solutions in progress at this Institute. For this purpose, a series of alloys was prepared covering the range from pure indium to 75 atomic pet TI, and X-ray diffraction patterns were obtained. Roughly speaking, the results indicated a region of continuous decrease in the axial ratio of the face-centered tetragonal structure from the value ca. 1.08 in pure indium to unity at about 23 atomic pct TI. From this concentration to the solubility limit, the structure was face-centered cubic, a form not reported by Hansen.1 At this point we became aware of the work of Valentiner,2 who had found the same structures at room temperature but had not investigated further the relationship between them. To study the transformation f.c.c.??f.c.t., and to clarify the phase diagram, we undertook the work reported in this paper and that which follows." Preparation of Alloys Pure indium and thallium* (both about 99.9 pct, as estimated from spectroscopic analyses) were weighed out in quantities sufficient to prepare 10 to 25 g of alloy of the desired concentration. (Occasionally indium was mixed with a previously pre- pared solution.) The metals were melted over a flame, in an open graphite crucible, stirred with a graphite rod, and poured into a graphite trough. The rough slug was hammered and swaged into a rod of 2 to 3 mm diam, and annealed in a drying oven at about 125°C for 1 to 2 days. Samples were taken from the rod for analysis, as well as for diffraction and other measurements. The thallium was determined by electrometric titration, using a modification of the method of Beale and co-workers.' The precision of analysis was generally about 2 0.2 pct of the thallium content. The rods were sometimes found to vary in thallium content as much as 1.5 pct from end to end, but since analyses were also made close to the segments used in the various studies, the composition was usually known as accurately as the analyses could be made. Where one less significant figure is given, the error is estimated to be ±0.4 pct of the thallium content. X-Ray Diffraction Measurements Three different cameras were used: (1) A 7 cm Debye camera, with oscillating specimen (manufactured by the Picker X-ray Corp., Cleveland, Ohio); (2) a 9 cm diam Debye camera of the type designed by Bradley;" (3) a 10 cm diam symmetrical focusing back-reflection camera (manufactured by Geo. C. Wyland, Ramsay, N. J.). Samples were prepared from the homogenized rods, either by filing under liquid nitrogen, or more often, in the form of wires or foils made by working at room temperature or liquid nitrogen temperature. Sharp patterns were obtained from specimens annealed at room temperature, although higher annealing temperatures were also used (cf. below). Generally, copper radiation was used; a few patterns were obtained with

Jan 1, 1951

By F. W. Glaser, W. Ivanick

A pressure-sintering method was used to produce binder-free and very dense TiC specimens. Some physical properties of these TIC bodies were determined and found to compare favorably with those of certain cemented Tic grades. It was also observed that the hot transverse rupture strength of TiC bodies remained substantially the same regardless of the amount or type of binder material used. STUDIES of the structure and physical properties of refractory materials have been intensified recently because of the urgent need for nonstrategic materials that retain their strength at high temperatures. Research aimed at determining and improving the physical properties of cemented carbides and borides has been accelerated with a view toward possible use of such materials in connection with turbine blades, rocket nozzles, and other high temperature applications. On the hypothesis that the strength requirements in connection with some of the above applications could be met only by proper choice of cementing agents for such refractory materials, the literature describing the physical properties of borides or carbides was reviewed. However, with a few exceptions,'-" references were found only to compositions containing at least one or more auxiliary binder metals. Cobalt and nickel are among the most frequently employed cementing agents. The melting point of Tic (approximately 3250°C) and therefore the sintering temperature, at which notable densification of a cold pressed Tic powder compact could be expected in the absence of a liquid binder phase, is relatively high. The present study makes use of a high temperature, pressure-sintering procedure, recently described by one of the authors in connection with the sintering of binder-free ZrB,," to produce dense bodies of sintered Tic—free of any cementing agent. During the course of this sintering study, some physical properties of dense Tic bodies produced by this method will be discussed. Materials, Preparation of Samples, Testing Methods The procedure for the forming of Tic powder consisted of mixing graphite and TiH, powders in stoi-chiometric proportions, and heating this mixture in a H, atmosphere and carbon crucible by high frequency, to temperatures ranging between 1900° and 2100°C (3452" and 3812°F). The powdered carbide was then comminuted and screened to the desired particle size. Table I shows the chemical analysis of the two grades that were employed for the production of samples during this work. Bodies of Tic, approximately 2.5xlx0.5 cm were produced in graphite molds that were heated by direct conduction. Sintering was carried out at temperatures for time intervals ranging from approximately 0 to 30 sec under a constant pressure of about 1.3 tons per sq in. An alternate method for the production of samples consisted in cold pressing the individual Tic grades at pressures ranging from 4 to 10 tons per sq in. and sintering in a hydrogen atmosphere in graphite crucibles heated by high frequency induction. Sintering temperatures ranged from 2600° to 2900°C (4715° to 5255°F). Electrical testing was done by measuring potentiometrically the voltage drop over a length of 1.5 cm for a current of 10 amp at room temperature. Cross-sectional areas as well as densi-

Jan 1, 1953

By R. H. Wightman, G. H. Adams

In order to secure good results in the prevention of accidents, it is generally recognized that the desire for such accomplishment, as well as the aggressive and constructive action to achieve it, must emanate from the Top Management and permeate successively down through the "Chart of Authority" to the workmen. Several years ago, with the above as a basis and with full support of the Top Management, the Mining Department started a program of selling the foremen and bosses the idea that safety could be achieved and that it was desired and required. Using psychology, persistence and numerous other methods, the foremen and bosses were finally impressed with the idea that "It can be done" and "It will be done." With this in mind, new ideas were brought forth by the foremen and bosses regarding the caving operation and the specific jobs in the operation. These new ideas were taken up in round-table discussions and resulted in certain changes in the undercutting method and the actual drawing of the blocks. These changes resulted in increasing fragmentation of the blocks which prevented the usual hang-up areas in the blocks. With the rock smaller in size and within reasonable reach from the tapping drifts, accidents were prevented in the tapping section. At the same time, an enforced campaign of housekeeping throughout the mine was undertaken with very beneficial results. The foremen and bosses then, in turn, educated and trained the workers themselves to become safety conscious. In so doing, a constant reminder was given on all jobs assigned that the job was to be done safely as well as efficiently. No man is assigned a job who is not qualified for the type of work required. Efficiency and safety go hand in hand. Safety Rules To supplement and aid this safety conscious attitude, certain safety rules applicable to our operation, a modified block caving system of mining limestone, in addition to the established state regulations, were put into effect and enforced. The specific rules referred to above and which will be mentioned below are in most cases simply a means of applying and complying with the very adequate "Mine Safety Orders" issued by the Industrial Accident Commission of the State of California. Some of the safety rules and policies are as follows: All men are required to wear safety

Jan 1, 1950

By Alden Greninger

METALLURGISTS have long believed that martensite in steel forms as plates along the octahedral {111} planes of austenite. Much has been written about mechanisms whereby units of the austenite lattice are pictured as transforming to martensite by shearing movements initiated along the octahedral planes of austenite, supposedly resulting in plates of martensite lying parallel to these planes of shear. A critical inspection of two or three photomicrographs of quenched hypereutectoid steel led us to the conclusion that the orientation habit of martensite, at least in hypereutectoid austenite, could not possibly be octahedral. Inasmuch as recent studies30,31 of the martensite-type reaction in nonferrous alloy systems have established the irrational orientation habit as characteristic of this type of lattice transformation, the need for a thorough restudy of the crystallography of martensite formation in steel was evident. The present paper reports the results of such a study, extended to include both cementite and some of the products of constant-temperature decomposition of austenite. Also reported are a few of the results obtained from a microscopic and X-ray study of the austempering process in very high-carbon steel.

Jan 1, 1940

Reports on process control computer projects at the Kamioka Plant are summarized from the Japanese technical literature (see references). Fluidized Bed Roaster and Sulfuric Acid plant1 A small process control computer (Yokogawa CCS-200 with an OKITAC 5090P 8K central processor) was installed in the Kamioka smelter in the summer of 1964. A year-and-one-half installation project followed, which successfully brought the roaster and acid converters under computer control. The process plant consisted of two 130 RPD fluosolids roasters and two Monsan to acid units. The roasters are charged with lead-zinc concentrates with SO2 from the roaster processed to sulfuric acid. The computer system provides the following functions: 1) log data from the plant--the input is taken from 50 analog signals, 130 high-low digital alarm points, and 50 analog high- low alarm points; 2) set-point control on 18 control loops; 3) direct digital control (DDC) on eight control loops for which conventional controllers were difficult to adapt due to abnormal loop characteristics or delay times; 4) execution of a safe shut-down procedure

Jan 1, 1969

By L. Leibowitz, M. G. Chasanov, L. W. Mishler

A drop calorimeter system is described for use in measuring enthalpies to 3600°K. Data are presented for tungsten between 2800" and 3600°K. The enthalpy of tungsten in cal per mole between 2000° and 3600°K can be represented by the equation HºT- Hº298 = - 1.7622 X 103 + 5.7772T + 8.9861 where T is in degrees Kelvin. A tabulation of com -puted values is presented for heat capacity, entropy, and free energy function. A drop calorimeter has been constructed to carry out enthalpy measurements at temperatures to 3600°K. Samples are heated by induction1 and dropped into a commercial adiabatic calorimeter, modified for this purpose. The experimental temperature is limited by the melting point of container materials and compatibility of the container and its contents. Several high-temperature drop calorimeters have been described in the literature1-5 but none has been used at temperatures as high as those in the present work; our measurements of the enthalpy of tungsten range from 2800" to 3600°K. DESCRIPTION OF EQUIPMENT An overall schematic view of the equipment is shown in Fig. 1. Power for the induction coil is supplied by a 25-kw 250 kHz Ther-Monic generator coupled to an iron core RF transformer. The Sample capsule is suspended in the work coil by 10-mil diam tungsten wires which are wrapped around a horizontal 5-mil diam tungsten wire. The horizontal suspension wire is clamped between two massive copper electrodes which are fixed in an x-y motion device that allows adjustment of the position of the heated capsule from outside the vacuum chamber. The copper electrodes are connected by flexible copper straps to a 1250-joule (5 kv, 100 pfarad) condenser bank. When it is desired to release the capsule, the condensers are discharged through the horizontal suspension wire causing it to vaporize rapidly. Very reliable and precise release of the capsule is achieved in this manner. Experiments have shown that no heat correction is required for this discharge energy. As part of the temperature measuring system, two prism holders have been incorporated in the apparatus. The upper prism holder is in the main vacuum chamber itself, whereas the lower one is in a side arm attached to the drop tube below the gate valve. The upper prism is mounted on a rotary vacuum feed-through, and may be moved under a protective shield when not in use. This prevents deposition of vapors on the prism surfaces when temperature measurements are not being made. Similarly, the lower prism is mounted on a push-pull vacuum feed-through, and when not in use may be pulled into its side tube. The prism mountings are fitted with guides and stops so that they may be moved precisely into the desired position. The aim throughout is to minimize the time the prisms are exposed to vapors from the hot samples. At the high temperatures reported in this paper, only the lower prism was used. The upper prism holder in these cases was fitted with an additional radiation shield. By using a prism and viewport, the lower surface of the samples can be observed by an optical pyrometer. The measurements discussed in this paper were obtained with a Leeds and Northrup 8622-C-S series manual pyrometer which is estimated to be accurate to 0.5 pct. Pyrometer calibrations and prism and window corrections were carried out in the conventional manner6 using tungsten strip lamps calibrated by the National Physical Laboratory, Teddington, England. Prism corrections were rechecked after each use. All work to date has been done in vacuum, and no measurable change has been observed in the prism correction below -2300°K for the upper prism and below -2800°K for the lower one. The total time of exposure of the prisms is about 50 sec per run. At high temperature, the final temperature reading is corrected by using the final A value for the prism; see Ref. 6 for details of this procedure. The calorimeter is a modified Parr Instrument Co. (Moline, lll.), Series 1230 adiabatic calorimeter with automatic jacket control. Other authors5 have used a similar calorimeter with good results. The calorimeter jacket cover and calorimeter cover are attached to the drop tube which contains a radiation shield. This shield is a gold-plated copper disc which can be operated manually from outside the calorimeter. The receiver is attached below the radiation shield and is lined with tungsten. In a typical experiment, the calorimeter and its jacket water temperatures were adjusted to 0.000°K temperature difference. The sample was allowed to equilibrate in the furnace at the desired temperature for about 20 min. The initial calorimeter temperature was then recorded, the sample dropped, and appropriate shutters closed. After about 3 min, the drop tube and receiver were filled with helium to 60 torr. The final calorimeter temperature was recorded after it had remained constant over a 5-min period. The equilibration time in the calorimeter was about 25 min. Thermistor probes are used to operate a hot and cold water supply system to maintain the jacket temperature equal to the calorimeter temperature. For actual measurements of the calorimeter temperatures, a quartz thermometer was used (Hewlett Packard Dymec Thermometer, Model #2801A). This thermome-

Jan 1, 1970

By C. Scala, F. Bernstein

General expressions are derived relating the streaming potential to the electrochemical potential of a permeable junction separating two electrolytic solutions. By the methods of irreversible thermodynamics, these potentials are related to the flux of mobile species arising from differences in pressure and chemical composition. The flux is conveniently expressed as a transference number, the equivalents of a mobile species transferred through the junction per faraday of electricity. At constant pressure, the flux equation gives the electrochemical potential across the permeable junction. The streaming potential across the junction is obtained by imposing the condition of constant chemical composition. The familiar expression for the borehole SP is shown to be a particular solution of the general flux equation. The derived exprersions were verified in experiments with seven shale samples. Both the theory and experimental data provide additional proof of the presence and magniturle of the streaming potential in shales. INTRODUCTION In the interpretation of electric logs, there has been much concern over the correction to be made to the recorded SP for an electrokinetic or streaming potential originating from the difference in pressure between the mud column and the formation. It was long recognized by M. R. J. Wyllie that such an electrokinetic potential source mas in the mud cake opposite permeable sands.' More recently, M. Gondouin and C. Scala2 showed an additional but opposing electrokinetic source of potential to be in shale beds. Their work was supported by the very extensive and excellent work of Hill and Anderson.3 n the present contribution, the general relationships between the electrochemical potential and the corresponding streaming or electrokinetic potential are examined and clarified. A notable advance towards understanding the relation between the various sources of electrical potential in a borehole has been the application of the now common methods of irreversible thermodynamics to describe the passage of ions and water through charged electrolyte junctions such as in shales.' The advantages of these methods are twofold. Unlike classical thermodynamics, they can be applied to non-equilibrium sys- tems, i.e., systems in which flow takes place, provided the flow processes have reached a steady state. They also permit conventional thermodynamic properties to be related to the steady-state dynamic properties. These methods arc used here specifically to derive expressions relating the potential behavior of shales in terms of ion and water transport. Experimental verification of the expression for the shale streaming potential is given which in turn offers theoretical support to the existence of a streaming potential in shales.' Importantly, the relative contribution of transport parameters to the SP is clarified. The theoretical treatment is essentially that of Lori-mer, Boterenbrood and Hermans3 ut has been extended to derive the general expression for the SP.

By John M. Loveioy

EVERY producer of crude oil knows what is meant by the Rule or Law of Capture. It means that the ultimate ownership of a migratory substance such as oil is not determined until that substance is reduced to physical possession. Unless, therefore, the producer moves quickly to capture his share from the common pool, he may lose to any neighbor who is drilling and producing more rapidly than he a portion of the oil originally underlying his property. And there is no recourse open to him if his property is so drained. Under this rule it is obvious that the owner of an oil property, if he is to protect his' ownership, must be governed in his development and production policies by the activities of his neighbor rather than by his own business requirements. He must drill as densely and as fast as the other operators in the field or lose part of the oil to which he should be entitled.

Jan 1, 1936

By M. W. Bartley, Hugh M. Roberts

SUBSTANTIAL deposits of Bessemer hematite have been found recently by drilling beneath Steep Rock Lake, Ontario, which is situated in the northern part of the Lake Superior Region. It will be practicable to divert the waters flowing into this lake and develop open pits on the upper part of two large ore bodies by damming off and pumping out the water in the part of the lake in which they occur. Ultimately, the bulk of the ore will be mined by underground methods. Owing to the generally massive nature of the rocks in the area, no underground flows of major consequence are anticipated after diversion of the lake. The Steep Rock deposits are attributed in origin to hydrothermal replacement. They were formed, for the most part, along an unconformable, brecciated contact between the Steep Rock limestone and an overlying younger volcanic series. The replacing solutions came in as igneous after-effects, following upon the intrusion of basic igneous rocks that invaded the hanging-wall volcanics. It is believed that this took place in a geological period roughly equivalent to late Middle Huronian, which was the period when the most extensive iron-bearing rocks of the Lake Superior Region were formed. Comparison is made with other deep-seated iron-ore bodies in the Lake Superior Region, the origins of which are ascribed in the discussion to hydrothermal replacement.

Jan 1, 1943

By W. J. Millard

VAGUE rumors and stories have been heard, from time to time, about the diamond and gold deposits of southern Venezuela. It is perhaps appropriate, at this time of revived interest in gold mining, to publish a few facts in regard to this country, which has been undergoing exploration since the fifteenth century. Gold and diamonds are found principally in the State of Bolivar which lies in southeastern Venezuela and is bounded by British Guiana on the east and Brazil on the south (see Fig. 1). The famous Mt. Roraima is situated at a point where these three countries meet in a common point (see Fig. 2). Some gold is also found in the southern part of the territory of Amacuro. Good oil prospects exist in the northern part of this same territory. Diamonds are found on the Caroni river from Rio Paragua to the village of Guri. Another small district is on the headwaters of the Cuyuni river. Quartz veins containing gold are chiefly exploited in

Jan 1, 1931

The Army Reorganization Act, which became effective July 1, 1916, contains a provision authorizing the organization of an Officers' Reserve, in which will be included a Corps of Reserve Engineers. There will also be an Enlisted Reserve of skilled workmen in technical lines. The special provisions of the bill relating to the Engineer Officers' Reserve were formulated with the help of the Joint Committee of the several national engineering societies, which has been at work on the matter for over a year with the War Department and Committees of Congress. Recognizing that engineering science is the basis of success in modern

Jan 8, 1916