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By Benjamin C. Craft

As predicted, during 1937 South Louisiana witnessed one of the most active drilling campaigns in the history of the area, resulting in the discovery .of 14 new fields. The economic importance of 10,000-ft. production was far-reaching and the objective depths placed on some wildcats was 12,000 feet. Most of the important discoveries and deep tests were in the delta area between the Atchafalaya and Mississippi Rivers, where the upper Miocene sands were found productive between 10,000 and 11,000 ft. The casing program on these wells usually called for a protection string of 95/8-in. casing at approximately 9500 ft. Drilling barges with the heaviest equipment were used where water transportation was available. The oil production for South Louisiana during 1937 was 62,147,690 bbl., as compared with 51,968,727 bbl. during 1936, an increase of 19.5 per cent. There were 281 oil and gas wells and 172 dry holes completed during 1937 as compared with 262 oil and gas wells and 135 dry holes during the previous period. New Fields Gibson.—The first discovery for the year was in the Gibson area, where Shell Petroleum Corporation's Realty Operators No. 1, sec. 18, 17 S., 15 E., Terrebonne Parish, was completed flowing 780 bbl. of 38° A.P.I. oil daily through a 14/64-in. choke with a tubing pressure of 1700 lb. Production is from upper Miocene sand found from 9461 to 9483 feet. Abbevil1e.—The discovery well for the Abbeville field was Continental Oil Company's Hebert No. 1, sec. 20, 12 S., 3 E., Vermilion Parish, completed flowing 50 bbl. of distillate and 2 million cubic feet of gas through a 3/16-in. choke with a tubing pressure of 2550 lb. The well was plugged back from 12,216 ft. in the Chickisawhay, and is producing through perforations from upper Miocene sand found from 7668 to 7682 ft. Later in the year, the same operators completed Brookshire No. 1, sec. 66, 12 S., 3 E., flowing 366 bbl. of 42° A.P.I. oil per day through a 3/16-in. choke with a tubing pressure of 1800 lb. This well was com-

Jan 1, 1938

By Y. H. Liu, R. Kiessling

The chromium, iron, and tungsten borides have been treated with ammonia at different temperatures. They are attacked, forming metal nitride and boron nitride, and the results are summarized in the tables. In the tungsten-nitrogen system a new phase has been observed, closely related to the known ß phase. THE present investigations were begun to determine whether any ternary phases exist in the transition metal-boron-nitrogen systems for the metals chromium, iron, and tungsten. Attempts to prepare such phases were made by using the borides of the metals as starting materials and ammonia as the nitriding agent. Although no new ternary phases have been found to exist, the results may be of some interest with regard to the technical use of the borides. General Procedure A steady stream of dry ammonia was passed through a silica reaction tube, the central part of which was kept at the reaction temperature while its ends were water-cooled. Weighed amounts of the borides were placed in a silica or porcelain boat and heated at different temperatures for a period of 10 to 24 hr. The boat was then rapidly removed from the reaction zone to the quenching zone, the water-cooled end of the tube, by means of a simple magnetic device. The nitrogen content of the products was determined by the increase in weight of the specimens, and the phase analysis was carried out by X-ray methods. For this analysis a Guinier-type camera, constructed at this Institute, was used with a bent, ground quartz crystal monochromator. The general reaction, which occurred in all the experiments, may be summarized as: metal boride + nitrogen -* boron nitride + metal nitride For the higher temperatures pure metal was formed instead of metal nitride. It is sometimes difficult to Discussi detect boron nitride among the reaction products by X-ray methods. Prolonged exposures of some specimens showed, however, that the strongest reflections of boron nitride were present. Additional evidence for its presence was given by the increase in weight of the specimens after nitriding. This increase was always greater than that corresponding to nitride formation only and was often in close agreement with the formula given above. Finally, a white powder, which was shown by X-ray methods to be boron nitride, was left if the reaction products after nitriding Fe,B at 448°C and FeB at 768°C were dissolved in diluted sulphuric acid. Ch rom iu m - Boron - N itrogen Five phases have been found to exist in the Cr-B system,' , and all were used as starting materials. Investigations on the Cr-N system have shown the existence of two nitrides with ideal composition Cr,N and CrN.".' * The results are summarized in Table I. All the borides are attacked and decomposed into chromium nitride and boron nitride, and the kind of nitride formed depends only on the temperature and not on the boride used as starting material. The lowest reaction temperature, however, is different for the different borides. Thus the 6 phase begins to react at about 735 "C, the r phase at about 800°, the S phase at about 900°, the 7, phase

Jan 1, 1952

By W. R. Hudspeth

AS an outgrowth of its spodumene recovery operation at Kings Mountain, N. C., Foote Mineral Co. has been recovering a heavy mineral by-product. Foote leased this idle plant in 1951, reactivated it, using a new spodumene recovery process, and purchased plant and properties in October 1951. While the operation at Kings Mountain is primarily concerned with the production of spodumene concentrate, pilot plant work determined that the pegmatites also contained heavy minerals including cassiterite. Plans were made to recover the heavy minerals as a by-product and the flowsheet incorporated these facilities when the mill was modified for the new spodumene recovery process. The orebodies consist of spodumene, feldspar, quartz and mica. Apatite, tourmaline, and beryl are present in small quantities. The wall rock is pre- dominantly hornblende shist. The heavy minerals, including cassiterite, columbite, pyrrhotite, monazite, pyrite, and rutile represent about 0.2 pct of the ore. The fine-grained heavy minerals are disseminated throughout the dikes, apparently unassociated with the spodumene. The pegmatites are quarried and secondary breakage is by mud-capping and block-holing. Power shovels load into trucks transporting the ore to a coarse ore bin. A Telesmith 10x36-in. apron feeder delivers the ore to an 18x36 in. Traylor Jaw crusher adjusted to discharge -3 in. product to a primary conveyor. The conveyor delivers to a 4x5-ft Tyrock single deck vibrating screen using 3/4 in. cloth. The screen undersize is elevated to the crushed ore bin. Screen oversize goes to an Allis-Chalmers Hydrocone Crusher fitted with 4 in. concave and set to deliver approximately 66 pct minus 3/4 in. The crusher discharge returns to the primary conveyor. The crushing and screening installation has a capacity of about 60 tons per hour. Spirals The crushed ore is delivered at a rate of 350 tons per day to two 6x8-ft Hardinge Pebble Mills, equipped with 20 mesh Ton-Cap trommel screens. The screen oversize is pumped to a 12-in. hydroclone for primary desliming. The hydroclone underfl spirals. There is no heavy mineral loss in the hydro-clone overflow. The spirals bank consists of eight 5-turn Model 24-A Humphreys Spirals. The top port and the last four ports of each spiral are blanked, the remaining nine port splitters are adjusted to remove about 5 pct feed weight. The heavy mineral rougher concentrates are upgraded on a Deister Overstrom table. The spiral concentrates contain approximately 4 pct heavy mineral, and the spiral reject, which goes to another section of the plant for spodumene recovery, contains about 0.03 pct heavy mineral. There is an interesting feature in the spirals installation. An adjustable splitter mounted on the discharge boxes splits out a mica fines product containing very little heavy mineral. The mica product is cleaned by spiralling and screening. Thus the spirals recover two products; mica, and a heavy mineral rougher concentrate. Table Treatment The rougher spiral concentrate goes to a Deister Plato table, modified to receive a Deister-Overstrom No. 6 rubber cover with sand riffles. The table is operated with a 5/8 in. stroke, 270 strokes per minute, and a slope of 1/2 in. per ft from feed to tailings side. There is no slope adjustment from motion to concentrate end. Wash water consumption is relatively high, since the large spodumene grains tend to report with the fine heavy minerals. A middling band about 4 in. wide is maintained in order to produce clean concentrate. The middling, representing about 10 pct of table feed, is recirculated by air-lift. A band of concentrate grade coarse spodumene occurs just below the middling. This is removed and delivered to concentrate storage. The table tailing, containing approximately 0.7 pct heavy minerals, is returned to the spodumene feed preparation circuit. The heavy mineral table concentrates are approximately 45 pct cassiterite, 33 pct columbite, 14 pct pyrrhotite and 8 pct monazite, together, with some rutile, pyrite, and copper from blasting wire. Concentrate is collected at 24 hour intervals. and dried. If the concentrate remains in wet storage appreciably longer surface oxidation takes place which seriously interferes with the subsequent magnetic separation process. About 150 lb of heavy mineral concentrate is produced per 24 hours and shipped to the company's plant at Exton, Pa. for final separation into tin and columbium concentrates.

Jan 1, 1952

By Etienne A. Ritter

INTRODUCTION. THE Evergreen mine, located at Apex, in the northern part of Gilpin county, Colorado, has opened a very peculiar and interesting copper-deposit, in which both bornite and chalcopyrite occur as rock-minerals. The country-rocks are crystalline schists cut by dikes of granulite and of pegmatite. At the Evergreen property they have been cut by a dike of a new kind of eruptive rock, to which I have given the name " Evergreenite" The rock is composed of quartz, alkali feldspars, orthoclase and albite (often interlocked as microperthite), with augite of the aegirine variety and long needles of enstatite and diallage. For reasons stated below, I believe the dike to be of Tertiary age. It is- easily traced on the surface of the ground, from a point in the bottom of Pine creek, about a mile below Apex,. to the top of Nevada hill, 1,500 ft. beyond and 600 ft. above it. (See Fig. 1.) It varies from 3 to 12 ft in width, and is bounded on both sides by contact-zones about 60 ft. wide, in which the crystalline schists have been changed into pseudo-quartzites or pseudo-gneisses, according to the injection of an excess of quartz or of feldspars through the special layer of the schists.. The most interesting feature is the presence of the pyroxenes, which are always found, though in very variable proportions from place to place, in the layers of these' metamorphosed crystalline schists. The dike has torn from its walls a large number of fragments of the wall-rock. It must have been in a viscous state when that happened, because these fragments of the wall-rock do not show any sign of resorption or of assimilation by the magma. In places they are so distinct and so numerous that the rock looks to the naked eye like a pseudo-breccia, of which, never-

Jan 1, 1908

By M. E. de Morton

Recovery and early recrystallization of heavily deformed, 99.98 pct Cr was investigated by studying metallographic structure. X-ray line sharpening, electrical resistivity, plastic properties, internal friction, and shear modulus. Appreciable recovery of resistivity, internal friction, and shear modulus together with some hardening and relief of internal strains occurred before the visible growth of a textured substructure above 350°C (recrystallization in situ). The complex behavior of shear modulus, internal friction, and its strain amplitude dependence during annealing are discussed qualitatively in terms of the relative mobility of dislocations. BY plastically deforming fully recrystallized 99.98 pct Cr above the brittle to ductile transition temperature, at -350°C. as in wire drawing, chromium can be made very ductile at room temperature. However, this ductility is lost on annealing at high temperatures when recrystallization takes place.' The present investigation was made to determine the general pattern of the changes in a number of physical and mechanical properties during recovery and recrystallization of heavily deformed chromium as part of an effort to elucidate the reasons for lack of ductility in the fully recrystallized condition. PREPARATION OF MATERIAL Wire specimens 0.027 in. in diam were prepared from arc-melted, electrolytic chromium by extruding, hot swaging and finally wire drawing at 300" to 350°C, i.e. above the brittle-to-ductile transition temperature. The total reduction in area of the wire was 98 pct and the last 3 pct of reduction was made at 100" to 150°C before cooling to room temperature. The impurity content of the material is shown in Table I. Internal friction and modulus measurements were made on a single specimen after annealing in situ at successively higher temperatures. For all other measurements, a fresh specimen was used for each temperature and annealing of these specimens was done in evacuated (0.001 mm Hg) and sealed silica tubes for 1 hr at the various temperatures up to 700°C. EXPERIMENTAL METHODS AND RESULTS The occurrence of a. transition in some physical properties of chromium at - 40°C2 imposed limitations on the temperature region where some of the measurements could be made. The reason for this transition in chromium is at present unknown but is probably associated with an antiferromagnetic state observed below - 40°C.* Heavy deformation produces an anomalous decrease in resistivity when measured at temperatures below -40°C4 though a normal increase is observed above this temperature. On the other hand internal friction in heavily deformed chromium5 over the temperature range 40" to 50°C is invariant with temperature. Above and below this range internal friction is strongly temperature dependent, increasing with increasing temperature. A temperature in this range was therefore convenient for both resistivity and internal friction measurements and for consistency the measurements of the mechanical properties were also made at about this temperature. No structural change has, however, been observed in careful X-ray measurements6 between -195" and 50°C, i.e. departure from cubic symmetry was not greater than 3:10,000; X-ray line sharpening measurements were therefore more conveniently made at room temperature.

Jan 1, 1962

By R. Taggart, R. H. Ericksen, D. H. Polonis

Transmission electron microscopy techniques hare been used to study the spontaneous marfensite phase that forms during the thinning of Ti-Cr alloys. The structure of this phase has been found to differ. from the hcp martensite and has been identified as a clisforted fcc lattice. The spordaneous marlensile in this system is interpreted as a metastable isomorph of the equilibriunz TiCr, phase. WHEN thin-foil specimens for transmission electron microscopy were prepared from metastable alloys of the Ti-Cr system, a spontaneous transformation occurred' when the foils contained the untrans-formed 0 phase or two-phase mixtures of the 0 and w phases. The purpose of this paper is to examine the relationship that exists between the crystal structure of the spontaneous product and that of the matrix. The differences between the martensite transformation that occurs in the bulk material and the spontaneous reaction that occurs during the preparation of thin foils are compared with the observations that have been reported for similar phenomena in a commercial titanium alloy.' A spontaneous reaction that exhibits characteristics similar to a martensite transformation has been reported to occur in thin foils prepared from the retained metastable structures of several alloy systems.1'3"7 ~ull~ observed such a spontaneous reaction in 0 brass and attributed the apparent increase in the martensite transformation temperature to a decrease in the non-chemical free energy associated with bulk strain energy. He also showed that the spontaneous product did not have a specific habit plane, but that its orientation relationships to the parent matrix were dependen on the thickness of the transforming region. It has also been pointed out by Breedis6 that in thin films the absence of the constraints imposed by a bulk matrix can cause different requirements for the martensite plate interface and lattice distortion which is reflected bv a dependence of the transformation mechanism on the specimen geometry. In the case of the spontaneous reaction reported for Au-Zn alloys7 a definite habit plane was determined and shown to correspond with the habit plane calculated on the basis of the Bowles and Mackenzie crystallographic theory of the martensite transformation.'- lo EXPERIMENTAL PROCEDURE A series of titanium alloys containing 5.5, 5.9, 6.4: 7.6, 8.0, 11.3, and 18.7 at. pct Cr were prepared from high-purity (iochrome) chromium and iodide-grade titanium by levitation melting. The experimental procedure used for sectioning the alloys and for thin-foil preparation has been reported in an earlier paper.' X-ray diffraction patterns were obtained using a 114-mm Debye-Scherrer camera and Cu-Ka radiation. In order to minimize fluorescent radiation from the specimen, a strip of aluminum foil 0.002 in. thick was placed in contact with the X-ray film. After a specimen was removed from the camera: an additional X-ray experiment was performed, to insure that no spurious lines were obtained due to the presence of the aluminum foil. The interstitial impurity analysis for the alloys used in this study was as follows: oxygen, 100 ppm: hydrogen, 30 ppm: nitrogen, 28 ppm. EXPERIMENTAL RESULTS Electron diffraction patterns were obtained from several individual crystals of the spontaneous marten-

Jan 1, 1970

By Michael S. Roscoe

In order to more accurately predict longwall surface subsidence over the Pittsburgh No. 8 Coal in Eastern Ohio, North American Coal Corporation's Quarto Mining Company undertook or participated in several subsidence studies. Due to the changing roof geology and rapid variations in the amount of cover two separate areas were investigated at two different mines to determine the subsidence response if any to these changes. Data generated from these studies were compared with NCB derived,data for accuracy and then used to predict subsidence under houses, gas lines and other critical man made structures. The following report summarizes the results of these studies as well as the subsidence case histories of gas lines, transmission towers, houses and water wells. Problems that were encountered during both phases of this process (investigation and subsequent application) are also included.

By L. D. Anderson

IN STUDYING Utah as a lead producing state one is immediately confronted by the fact that few, if any, of the ores of the state are valued for their lead contents alone. More correctly the ores from which this metal is recovered are characterized as silver lead. Even then the whole story is not told for many of these ores carry also gold, copper, zinc, bismuth, antimony, arsenic, tellurium, and other metals. It becomes apparent, therefore, that the production of lead i11 Utah is influenced by many factors. For example, i11 the early part of 1923 there was a marked increase in the production of the lead by reason of the efforts made by silver mines to produce as much silver as possible before the termination of purchases under the Pittinan Act in June, 1923. As nearly all silver ores carried more or less lead the production of that metal was increased with the increase in silver production. Very few, if any, ores of the State are mined for their lead contents alone. Important as Utah's contribution to the lead output of the country is nevertheless it is bound up to some extent with the production of gold, silver and copper.

Jan 1, 1925

By H. O. Jahns, R. A. Greenkorn, R. E. Haring, L. K. Shallenbarger

This paper is a study of the effects of heterogeneity on flow in an analog of porous media, the Hele-Shaw model. l-3 A set of experiments in heterogeneous Hele-Shaw models showed streamlines through and around heterogeneities of various sizes, shapes and levels. (A level, we define as the ratio between the transmissibility of the heterogeneity and that of the rest of the model.) The heterogeneities were restrictions or expansions of the flow stream analogous to variations in the transmissibility of porous media. The experimental data agreed well with numerical results and with an analytical solution, which we derived for a circular heterogeneity in an infinite field. This study considers the flow-stream distortion due to the shape, size and level of heterogeneities. Size and level are much more important than shape provided the heterogeneity is not long and narrow. Our analytical solution shows that a circular heterogeneity in a large field can be replaced by an equivalent circle of either zero or infinite permeability. The radius of the. equivalent circle is a simple function of size and level of the actual circle. INTRODUCTION With the availability of high-speed computers and numerical procedures to predict reservoir behavior, we are faced with an important question. How much information about the reservoir do we need to justify the cost of the computer in any given case? To answer this question, we have to know how various reservoir parameters affect flow behavior. Reservoir heterogeneity is one of these parameters. In this study, we used a simple, two-dimensional model of porous media, the hele-shaw model, to investigate the effect of heterogeneity on flow behavior. We restricted ourselves to linear, single-phase, steady-state flow in a rectangular field with a single heterogeneity at its center. The analogy between flow in Hele-Shaw models and in porous media is easily verified. Let us first consider a homogeneous Hele-Shaw model with constant plate separation h. (The Hele-Shaw model is constructed by placing two plates, usually glass, very close together and allowing liquid to flow between them. Streamlines are made visible by introducing colored fluid into the space between the plates at a number of points across the model.) We assume a cartesian coordinate system with its origin in the middle between the plates and the z axis directed perpendicular to the glass plates (Fig. 1). The fluid flow is always in a direction parallel to the glass plates and varies from a maximum value to zero in the very small distance from the middle (z = 0) to either plate (z = h/2). For slow motion of an incompressible fluid, neglecting inertia and body forces, we have the viscous flow equation: where p is the fluid pressure, p the viscosity, and v the velocity vector with components u, v and w in the x, y and z directions, respectively. In our rase. and the derivatives of 3 with respect to x and y are small as compared with the derivative in the z direction. Therefore, approximately, with Vp and v being two-dimensional vectors in the x-y plane. Two integrations with respect to z give

Jan 1, 1965

By Donald R. Mason, Daniel F. O’Kane

DIFFERENTIAL thermal analysis measurements have been used to determine the ZnTe-In2Te3 pseudo-binary phase diagram. Since ZnTe and In2Te3 are both semiconductors, any intermediate compounds formed in this system should also be semiconductors according to the rules delineated by Mooser and pearson.1 The compound ZnIn2Te4 was first reported by Hahn et a1.2 and it has subsequently been prepared and characterized electrically by several workers. A brief summary of this work has been presented by Mason and O'Kane3 who also report that the compound appeared to melt peritec-tically. The Zn-Te phase diagram has been investigated by Kulwicki4 who found that ZnTe has a melting point of 1290° + 2°C. The In-Te diagram published in Hansen' contains significant errors, and has been redetermined by Grochowski et al.6 However, both sources agree that the melting point of In2Te3 is 667°C, with the latter authors reporting the previously observed solid-solid transformation occurring at about 550°C. Hahn ef al.2 reported lattice-parameter values for the ZnTe-In2Te3 system. The 67 mole pct ZnTe-33 mole pct In2Te3 composition was the only

Jan 1, 1965

By W. Rostoker, S. A. Spachner

STUDIES of precipitation phenomena by use of X-ray diffraction effects have shown that atoms of the precipitating phase initially form lattices of limited periodicity in two or three dimensions.1, 2 Such diffraction effects are usually plotted in reciprocal space to facilitate identification. Atomic chains, or gratings possessing unlimited periodicity in only one dimension, cause uniform intensity planes in reciprocal space. Platelets, or gratings possessing unlimited periodicity in two dimensions, cause uniform intensity rods in reciprocal space. Such studies have been accomplished by use of white radiation (Laue technique) or characteristic or monochromatic radiation used with rotating single crystal or Weissenberg cameras. Each one of these techniques have associated drawbacks. If the Lque or rotating single-crystal technique is used, the results which are obtained may be ambiguous.3 Diffraction photograms made with a WeisSenberg camera do provide a direct but distorted representation of the variation of diffracted

Jan 1, 1960

By N. H. Mannakee

SINCE the publication of the paper of Mr. Scholz, The Effect of Humidity on Mine-Explosions,' I have undertaken a study of the meager available data of barometric and temperature conditions it times of mine-explosions, and have arranged these data in a manner which may be of interest to other students of mine-explosions. This study covers the period from 1898 to 1909, during which an ever-increasing percentage of collieries has been ventilated by fans giving air-currents of high efficiency. Previous to 1898 this percentage was smaller than at any time since. The vari¬ous States have become, from time to time, more exacting in their demands upon poorly-ventilated mines. This general im¬provement in ventilation throughout the Appalachian field has undoubtedly brought about a condition which is annually the cause; .or a very important attendant, of the high percentage of fatalities in mine-explosions, through the daily passage of from hundreds to thousands of gallons of water, invisibly suspended in the air, carried out of the mines by the ventilating-currents during the existence of certain temperature- and humidity-conditions. There is a wide-spread opinion that these conditions exist from November 1 to March 31; but it is more likely that they have a much wider range, which varies from year to year. Certain years show an increase or decrease of rain-fall from the mean ; the daily temperature may fall far below or rise far above the mean established by a record of a period of years; and the daily humidity varies likewise. If mine-explosions are influenced by a lack of moisture in the mines, certainly it may be expected that the influence will be felt at times when the

Nov 1, 1909

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 E. A. Has, E. Mcl. Tittmann

Double roasting of sinter carrying a high percentage of lead concentrates, gave rise to the problem of removing the sheets of metallic lead formed in the wind boxes. The solution of the problem has been found in the water sealed wind boxes. The metallic lead is granulated and can be removed without seriously interfering with the operation of the machine and eliminates necessity of men going in wind boxes with air guns. THE practice of double sintering the charge for lead blast furnaces, which is now standard throughout the lead smelting industry, has introduced the rather difficult problem of cleaning the wind boxes on sintering machines used for the final pass. Two factors have more recently accentuated this problem: (1) the growing demand of workmen for better working conditions and less arduous labor, and (2) the growing dearth of crude lead ores and the improved grade of lead concentrates demand a charge carrying the maximum percentage of lead. One to 2 pct of such high lead charges (30 to 40) when processed on machines in reasonably good condition will pass through the grates and report in the wind boxes. One-half to three-quarters of this material will be metallic lead reduced by the coke breeze or other fuel mixed with the charge. This lead forms large cakes or chunks which are hard to remove and which substantially increase the time the machine is out of operation for cleaning the wind boxes. A high lead fall can reduce the operating time 30 pct. As a specific example, a 30 ft machine having 63 in. pallets, and equipped with three conventional wind boxes, requires 3 to 4 hr per day for removing the accumulation in the wind boxes when operated as a final pass machine. This same machine when operated on raw charge requires less than an hour per day for cleaning. To eliminate formation of large chunks of lead in the wind boxes of the final pass machines and time lost in cleaning the boxes, R. C. Rutherford of the Chihuahua smelter of the American Smelting and Refining Co., devised and patented* a wind box having a water bath to granulate the lead as it falls from the grate bars. Later, C. H. Harris of the San Luis plant made and patentedt an improvement on Rutherford's device in which the water bath seals the wind box in a manner permitting the latter to be readily cleaned without destroying the vacuum. The first machine to our knowledge to use the water bath box was at the Chihuahua plant along the lines of the Rutherford patent. In 1942, a machine was placed in operation at the El Paso plant which incorporated the features of both Rutherford and Harris. This machine is 40 ft long equipped with pallets 63 x 24 in., and having 4 wind boxes 10 ft 4 in. x 7 ft 2 in. x 51 ft 3 in. in size (fig. 1). The air from the fourth box is returned to the first three, and the gas from the first three discharged to a baghouse. The machine has conventional drive, discharge hopper,

Jan 1, 1951

By J. W. Hickman

Most of the electron diffraction studies of oxide films which form on metals and alloys have been carried out by oxidizing the specimens in an auxiliary furnace, cooling down to room temperature and then inserting the sample in the camera and taking a diffraction photograph. Prior to the investigations at the Westinghouse Research Laboratories, no systematic study of the oxidation of any metal or alloy had been made over a wide temperature range with photographs taken at elevated temperatures except the investigation of iron by Jackson and Quarrell.' In order to interpret the electron diffraction patterns of the oxides which may form on alloys, it seemed advisable to make a comprehensive study of the oxidation of the purest metals available in the bulk form. Thus far studies have been completed on iron,2 cobalt,~ nickel,= chromium,= copper,z tungsten,s molybdenum,3 beryllium,' uranium,' thorium,' titanium6 and zirconium6 while investigations are in progress on tantalum and columbium. The next step in the study is concerned with the investigation of the oxides which form on binary alloys. Some of the alloys consist of a single phase while others contain more than one phase. The identification of the oxides on the surface of a binary alloy may be more difficult than on the metals since oxides containing both metals as well as those of each metal separately may form. Furthermore, it is possible that solid solutions of the various oxides may occur. In these cases the electron diffraction method may not be able to identify the oxidation products unequivocally. Examples of solid solutions which may present difficulties are MOO* and WOp, Fe304 and FeO.CrnOa since the diffraction patterns are so similar. Since electron diffraction can determine only the structure of the oxide, the chemical composition must be inferred from the diffraction data based upon X ray diffraction investigations of specimens of known composition. It is possible in some cases to decide whether a given solid phase reaction can occur on the surface of an alloy by a study of available thermodynamic data. Table I lists the equations for the formation of most of the oxides from the elements together with values of loglo Kg for the several temperatures. AF"B = -RT In KR AF°R and KR are the free energy and equilibrium constant of the reaction. Calculations may be made using the the given in I 1 to determine whether a given solid phase reaction is possible thermodynamically. For example, a solid phase reaction should occur between aluminum and chromium oxide to form

Jan 1, 1949

The Carol concentrator of the Iron Ore Company of Canada was completed in 1962 and through expansions .has become one of the largest iron ore beneficiation plants in the world with a new feed capacity of 147,000 It (149,350 mt) per day. The Carol ore contains specular hematite and magnetite having a bulk density of 166 lb/cu ft (2660 kg/m3) It is crushed to 7 in. (178 mm) for feeding to autogenous mills for subsequent concentration by Humphrey’s s spirals. Mine ore is loaded into 150 It (152 mt) trucks by 10 cu yd (7.65 m3) shovels and then, at a transfer station, is loaded into side-dump rail cars of 100 It (101.6 mt) capacity. Each train is composed of twenty cars and operates completely automatically as it hauls the ore to the primary crushing station, dumps its loads, and returns to the loading station, a 11.5 mile (18.5 km) round trip. The primary crushing station is composed of two 60 in. by 89 in. gyratories installed in 1962 and 1972. Neither crusher has a grizzly ahead of it. Rail cars are dumped into 300 It (305 mt) pockets which contain splitters for spider protection. What few oversize boulders which do not go through the crushers are drilled and blasted. Liners in the dump pocket and the crushed ore pokcet under the crusher are manganese steel. Both crushers are direct driven by 700 hp (5 15 kw) motors, and the hardness of the ore causes them to pull almost their full power. Crushed ore drops into a 160 It (163 mt) pocket equipped with radioactive level control units for low-intermediate, and high level indications. The low level unit stops and starts the apron feeder, the intermediate unit controls the feeder speed, and a high-level reading stops the car dumping. Apron feeders are 72 in. (1. 82 m) wide and are variable speed from 12 to 52 fpm (3. 7 to 15. 8 mpm). They discharge to 60 in. (1.52 m) wide takeaway belts. Crushing capacity, nominal and maximum for each crusher, is 4, 000 ltph (4. 064 mtph) and 4,600 ltph (4,674 mtph). The crusher eccentric is removed by a conventional cart which travels on removable rails. Mainshaft removal and maintenance is done by 65 and 75/10 ton cranes. Mainshaft replacement requires eight hours, a usual time, but concave replacement requires only sixteen hours, a result of a fine maintenance organization. Mantle relining is done at grade next to a repair track. Zinc is used for backing both mantles and concaves. Both the electrical rooms and the dust collectors are located below grade,

Jan 1, 1978

By W. O. Philbrook, K. M. Goldman, G. Derge

T. Rosenqvist—The most interesting point in this paper is the observed transfer of iron into the slag in the initial stage of the desulphurization process, after which the iron again is reduced to the metallic state. The authors interpret this observation as showing that the sulphur enters the slag as an iron-sulphur compound which subsequently is decomposed by the slag. The present writer has previously suggested the following equation for the desulphurization process: S + O2- ? S2- + O For equilibrium in the blast furnace the oxygen potential is defined by equilibrium with graphite and CO of 1 atm pressure: C + O ? CO [2] During the desulphurization process the reactions proceed in the direction of the arrows. If one assumes eq 2 to be significantly slower than eq 1, the transfer of sulphur into the slag, in accordance with eq 1, will build up a local oxygen potential at the metal-slag interface very much higher than that corresponding to the value defined by eq 2. This is possible because the equilibrium oxygen potential in eq 1 is high as long as the sulphur content in the slag is low. This oxygen potential will again be able to oxidize some iron: Fe + O ? Fe2+ + O2- and an increase in the iron content of the slag will be observed. Adding up eqs 1 and 3 one obtains: S + Fe ? S2- + Fe2+ The net effect is thus in harmony with the experimental observation but is obtained without assuming any close ties between the sulphur and iron atoms during the process. Furthermore, it follows from eqs 1 and 2 that when the sulphur content in the slag increases, and equilibrium with C and CO is finally approached, the local oxygen potential at the metal-slag interface will decrease, and the iron in the slag will be reduced back into its metallic state. C. E. Sims-—The data and conclusions presented in this paper are thoroughly convincing in establishing the mechanism of sulphur transfer from iron to slag as in a blast furnace. The evolution of gaseous CO in step 3 of the reactions given on p. 1112 makes the process virtually irreversible. Assuming that the process is similar in slag-metal systems other than in the blast furnace, it is readily seen why free CaO and re-ducing conditions so greatly favor desulphurization. On the other hand, the very effective desulphurization obtained in oxidizing slags when strongly basic, must be attributed to the relatively high stability of CaS as compared to FeS. The ease and simplicity with which the reactions of classic chemistry agree with the experimental data and explain the mechanism is noteworthy. The concept of molecules of FeS, soluble in both phases (metallic iron is not soluble in the slag), migrating from the iron to the slag and there reacting with CaO, which is soluble only in the slag phase, is clear and uncomplicated. This is likewise true for step 3. Those who would deny the existence of molecules or molecular-type combinations in liquid iron, must strain to provide a mechanism so lucid. In the absence of molecules, the Fe and S exhibit a remarkable collusion. L. S. Darken—The investigation and interpretation of rate phenomena in the range of steelmaking temperatures is a difficult task. Most of the laboratory investigations of steelmaking reactions have been concerned with equilibrium. Having determined the equilibrium, our attention naturally focuses next on the mechanism and rate of approach to equilibrium. The authors seem to have contributed substantially to our understanding of these factors for the case of sulphur transfer. I should like to ask the authors whether they consider that the sulphur transfer reaction is diffusion controlled as many high-temperature reactions seem to be. If so, it would seem reasonable to suppose that the slow diffusion step of the process is the transfer across a pseudo-static layer or film similar to that considered in heat flow problems. As the diffusivity and fluidity are smaller for the slag than for the metal, it may tentatively be assumed that the sulphur gradient exists in a thin layer in the slag adjacent to the slag-metal interface and that the metal and the main mass of slag are each maintained uniform by convection. On this basis the amount of sulphur transferred across unit area per unit time is D p (?S%)/100 ?1, where D is the diffusivity, p the density, (?S%) the difference in percent sulphur on the two sides of the layer, and ?l is the layer thickness. At the beginning of the experiment the main body of the slag and hence one side of the layer contains no sulphur; therefore (?S%) may be replaced by (S%), the sulphur content of the slag at the slag-metal interface, which in turn is equal to L[S%] where [S%] is the sulphur content of the metal and L is the distribution coefficient. The rate of transfer thus becomes DpL[S%]/100 ?l, which the authors designate K[S%]. Equating these two quantities and setting D = 10-6 cm2 per sec, p = 3 g per cm3, L = 40, and K = lo-+ g cm-2 sec-1, it is found that ?l, the film thickness, is about 0.01 cm—a value of the order of magnitude of that found in heat transfer problems in liquids. The uncertainty of the numerical values used leaves much to be desired, but at least it can be said that this calculation tends to support the proposed model involving diffusion through a film. Although this does not seem to affect the general argument, I should like to call attention to the fact that the diffusivity3 of sulphur in hot metal is found (on conversion of units) to be about 10-4 cm2 per sec rather than 104 cm2 per sec as stated by the authors. The three equations written by the authors to express the steps in the overall process of sulphur transfer may alternatively be written ionically as only two Fe + S = Fe++ + S-- Fe++ + O-- + C (graphite or metal) = CO (gas) + Fe where the underscore is used to designate the metallic phase; ionic species are slag constituents. After the authors have so neatly demonstrated that iron and sulphur transfer together (at least initially), this fact seems almost self evident; from eq 4 it is seen that if sulphur acquires a negative charge during transfer

Jan 1, 1951

By C. S. Smith, K. K. Ikeuye

In an earlier paper1 one of the authors called attention to the significance of the relative free energies of grain boundaries and interphase boundaries in alloys in determining the shape and distribution of micro-constituents. The ratio of the interphase and inter-crystalline boundary energies (that is, —?12, where ?12 is the energy of the interface between a crystal of phase 1 and a crystal of phase 2, and ?11 is the energy of the boundary between two crystals of phase 1) will be denoted by F. It is this ratio that determines, by the simple triangle of forces relation, the dihedral angle, ?, of phase 2 where it adjoins a boundary between two grains of phase 1. On a metallographic sample various angles are actually obtained because of the random orientation of the plane of observation, but the statistically most frequent angle is the true one. These basic principles were discussed in detail in the earlier paper. The experiments described below show the effect of both composition and temperature on ? and T for some alloys containing a liquid phase, and provide data on the rate of approach to the equilibrium angles in both solid and liquid phases. All the alloys were melted in a graphite crucible and cast into ingots 3/4 by 11/8 in. cross-section. Some of the aluminum alloys consisted of two immiscible liquids from which uniform castings could not be obtained. The amount of liquid phase varied locally to a considerable extent and the analyses were meaningless. Nevertheless, the composition of the liquid would not differ from that in an alloy of the intended gross composition, and the synthetic composition of the alloys was therefore used in considering the surface energy results. The ingots were given initial deformation by cold-rolling to 50 pct reduction, annealed, and given a second 50 pct reduction prior to cutting into small samples for heat treatment at the times and temperatures subsequently reported. The resulting micro-samples were carefully prepared metallographically and examined at magnifications of 650, 1280, or 2500. The objectives used were 21X, 0.40 NA (dry); 41X, 0.65 NA (dry); and 80X, 1.40 NA (oil emulsion). The appropriate angles were measured by rotation of the stage of a Bausch and Lomb metallograph to align the appropriate boundaries successively with a cross-hair in a micrometer eyepiece. About 250 angles were measured on each phase. Though the angles were read to 1°, the accuracy is probably not above 3°, because of uncertainty in setting the cross-hair tangent to the sometimes curved boundary. The corners of very small particles, particularly in early stages of adjustment after cold-rolling, were difficult to measure and the results were slightly dependent on the magnification used (compare Fig 1-C and 1-D). With particles of larger size and more nearly equilibrium shape, magnification made no difference (vide Fig 1-F and 1-G). The measured angles were grouped in 10° intervals (5° if ? was less than 20°) and plotted in bar

Jan 1, 1950

By Theodore R. Butkovich, Jesse L. Yow

Geological storage of spent-fuel assemblies from an operating nuclear reactor has been underway since the Spring of 1980 at the U.S. Department of Energy's Nevada Test Site. The primary objective of this generic test is to evaluate granite as a medium for deep geological storage of high level reactor waste and to provide data on thermal and thermomechanical behavior of granite from imposed heat loads.(l) The underground installation in the Climax stock granite was sited at about 420 m below the surface and 145 m above the existing water table. As shown in Figure 1, three parallel drifts were excavated spaced on approximately 10 m centers. Seventeen storage holes were drilled at the central drift on 3 m centers in which eleven spent fuel canisters and six thermally identical electrical simulators were emplaced. Electrical resistance heaters were emplaced in vertical holes in the floor of the side drifts on 6 m centers. The thermal output of these heaters is being periodically adjusted to simulate the thermal response of a large storage array. Rock and ventilation air temperatures are being measured continuously in the drifts and throughout the rock surrounding the excavations. Measurements of drift deformation have been made routinely since the emplacement of the spent fuel. Both vertical and horizontal measurements are being taken at five locations along the heater drifts and at six locations along the central canister drift (Fig. 1). Two types of instrumentaton are being used: convergence wire extensometers which are monitored automatically, and a manually operated tape extensometer with which measurements are taken periodically. The tape extensometer measurements were initiated about 6 weeks following fuel emplacement. The lack of a temperature correcting capability for the convergence wire extensometers make that data unavailable for analysis at this time.

Jan 1, 1982

By J. Weertman

The paper of Gifkins and Snowden considers the interesting but difficult problem of determining the stress dependence of secondary (steady-state) creep at low stresses. These authors have concluded that at stresses below 250 psi (2 x 107 dynes per sq cm) the secondary creep rate of lead is proportional to the stress (viscous creep) and is not proportional to the stress raised to about a fifth power. The experimental data considered by them were obtained on tests conducted at room temperature and at 50°C. The lowest stress employed was 50 psi (3.5 X 106 dynes per sq cm). The authors pointed out the main difficulty in determining the stress dependence of creep at low stresses. The creep tests must be run for very long lengths of time. However they made no estimates of when an experimental creep rate determination must be rejected because it does not represent a true steady-state or minimum creep rate. In order to be certain that a creep curve is within the steady-state region, the total creep strain should be of the order of 0.1 to 0.2. For a creep test of a year's duration this requirement implies that a secondary creep rate smaller than about 10-3 per hr cannot be measured reliably. The corresponding creep rate for a 10-year test is 10-6 per hr. The creep rates of the tests that were considered by the authors to prove the existence of viscous creep were of the order of or less than 10-6 per hr. One can conclude reasonably that this data does not prove unambiguously that large strain steady-state creep rate of lead is proportional to the stress in the stress range of 50 to 250 psi (3.5 x 106 to 2 X 107 dynes per sq cm). Another technique can be used to obtain the stress dependence at low stress levels. The creep rate is a very sensitive function of temperature. The creep rate can be increased by very large amounts merely by increasing the temperature. We carried out steady-state creep tests on lead single crystals25 at temperatures up to 320°C. We were able to obtain creep rate data down to stresses as low as 35 psi (2.5 x 10' dynes per sq cm). Our smallest creep rate was 8 x 10-5 per hr. Thus we obtained large strain, steady-state creep rates to even lower stresses than were considered by Gifkins and Snowden. No evidence was seen for viscous creep. The creep rate was proportional to the stress raised to about a 4.5 power down to the lowest stresses. Since there is no reason to believe that changing the temperature should change the stress dependence of steady-state creep, we feel that large strain viscous creep does not occur in the stress range quoted by the authors for lead single crystals or large-grain polycrystalline samples of lead. This conclusion does not imply that viscous creep may nat occur in a lower stress range or in the same stress range for fine grain material or at creep strains very much smaller than 0.1. Support by the U.S. Office of Naval Research is acknowledged. Authors' Reply R. C. Gifkins and K. U. Snowden We thank Dr. Weertman for his discussion and although, as we hope to show, we do not agree with his reservations, we do concur in stressing the importance of ensuring that creep rates are reliably obtained. Dr. Weertman appears to be content to accept n = 1 for low stresses with fine-grained material but not for single crystals. We believe our results show that the former result cannot be accepted without also accepting the latter. We will also show that the probable errors in our minimum creep rates are insufficient to alter our conclusions, that the criterion proposed by Dr. Weertman is arbitrarily restrictive and his alternative experimental approach possibly invalid. 1) A principal result of our Fig. 1(a) is that n = 1 for polycrystalline specimens at room temperature and 50°C for stresses below -250 psi. There was evidence that crystal slip and grain boundary sliding contributed approximately equaily to the overall strain in this low-stress regime. This implies that either a) grain boundary sliding controls slip within the grains or b) both grain boundary sliding and crystal slip independently occur according to mechanisms which give n = 1. Alternative a does not seem acceptable, so we were forced to consider b. This led us to reexamine work on bicrystals by Strutt and Gifkins and plot curves Fig. l(b). Previously Strutt et al. (loc. cit.), had merged these points with others using the Zener-Holloman parameter and thus, we now believe, had been led to overlook the behavior where n = 1. Curves C and D in Fig. l(b) did appear to confirm the hypotheses that n = 1 for crystal slip at these low stresses and the sliding curve F was similarly of the expected form. It was comparatively easy to find a quantitative theory to account for n = 1 for sliding and the similarity of curves C and D to curve F (all obtained from the same set of specimens) led us to feel that the single-crystal curves were valid. 2) We believe the secondary creep rates for both the polycrystalline and single-crystal specimens to be in error by factors c2. In Fig. 6 creep curves for polycrystalline specimens of lead(1) and lead(II) are reproduced as curves a and b, respectively, and curve c is for a single crystal at 100 psi. It is clear that, although the attainment of secondary creep rate takes 2 years for a and 150 days for b, thereafter the curve is linear for periods of 7 and -1 year, respectively. The single crystal has a linear portion commencing after 20 and extending to 90 days. Creep extension was measured directly using a traveling microscope reading to 0.01 mm on gage lengths marked on the specimens; the gage lengths

Jan 1, 1968