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By D. W. Fuerstenau

MEASUREMENT of zeta potentials is a useful tool to study the surface chemistry of minerals under flotation conditions.1,2 Because there is continued interest in this approach, the apparatus for obtaining zeta potentials of nonconducting solids by the streaming potential method is outlined here. Fig. 1 illustrates the streaming potential apparatus." The streaming potential cell or plug consists of two 24/40 standard ground joints (4) joined with a piece of pyrex tubing 60 mm long and 12 mm in diam (5). The electrodes are made of bright platinum disks 19 mm in diam and 1 mm thick through which 0.5-mm holes have been drilled (6). To the surface of each is welded a piece of 80-mesh platinum gauze. Each electrode is permanently mounted on the ends of the inner parts of the two standard joints by means of a platinum wire (7) which connects it to the tungsten seal at the end of the cell (8). For ease in cleaning and handling the apparatus, the streaming cell is fastened to the 500-ml reservoir flasks (1) by means of two 18/9 ball and socket joints (2). This particular arrangement permits passage of the solution in either direction through the plug of particles. Flow of solution can be stopped by a stopcock (3). One of the reservoir flasks has a large opening to permit insertion of either a thermometer or a pair of electrodes for measuring pH of solutions within the system. In making the experiments, the plug is filled with 48 to 65-mesh particles, but a layer of 28 to 35-mesh particles is placed at each electrode to prevent any of the finer particles from passing through holes in the electrodes. The assembled apparatus is shown schematically in Fig. 2. To eliminate CO2 from the solutions, all experiments are conducted in a nitrogen atmosphere. Nitrogen, used to drive solutions through the plug, is passed through a bottle of concentrated KOH solution to remove CO2 (9). A 9-liter ballast reservoir (10) is used to maintain a more nearly uniform pressure. A series of stopcocks controls the direction of flow nitrogen to the flasks (11). Tubes of as-carite prevent backflow of CO2 into the system (12). Driving pressure, which can be set at any desired value, is measured with either a water manometer (13) or a mercury manometer (14). Reservoir flasks have side arms for making pressure corrections for the difference in water levels in the flasks. Streaming potentials are measured by the circuit illustrated in Fig. 2. The electrodes from the plug are connected through mercury wells (15) to a reversing switch (16), which reverses the polarity of the electrodes depending on the direction of flow of solution through the plug. The streaming potential is measured with a Leeds and Northrup type K2 potentiometer (17). Proper choice of null instrument is important because Eq. 1 assumes that the current which escapes through the measuring instruments is negligible. An ordinary galvanometer cannot be used to determine the null point because

Jan 1, 1957

By I. Fatt

Laboratory relative permeability data on reservoir rock are obtained on samples which are not subjected to overburden pressure during the permeability measurements. These data are then used for calculating the performance characteristics of reservoirs in which the rock is under the pressure of the overburden. Recent observations have shown that the permeability and porosity of reservoir sandstones are decreased by application of overburden pressure. These observations led us to a study of the effect of overburden pressure on the relative permeability characteristics of sandstones. A previous note from this laboratory1 showed that overburden pressure, simulated by applying hydraulic pressure to the outside of a plastic mounted core. caused a reduction in permeability of the core by as much as 50 per cent at 10,000 psig. In a multiphase fluid flow system, the relative permeability at a given saturation will change if the permeability or the effective permeability changes but not if both permeability and effective permeability change by the same ratio. The tests described in this note were made to determine the effect of overburden pressure on permeability and effective gas permeability in the gas-oil system. The gas-oil system was chosen because the available equipment was best suited for studying this system. The resultant data can be applied to other systems of interest because the gas permeability in the gas-oil system is the permeability of the nonwetting phase and, as such, is equivalent to the gas permeability in the gas-oil-water system and to the oil permeability in the oil-water system. EXPERIMENTAL METHOD Cylindrical test plugs, one in. in diameter and one in. long, were cut from sandstone core samples from three different reservoirs. After extraction in toluene, the plugs were mounted in Lucite by conventional core mounting methods.3 The core properties are given in the legend in Fig. 1. The mounted cores were machined to fit the apparatus shown in Fig 4. Air permeabilities as a function of overburden pressure were measured by connecting lines (1) and (2) to a conventional air permeameter. To measure porosity changes as a function of overburden pressure, the lines leading to (1) and (2) and the core were saturated with kerosene; line (1) was capped and a small bore precision calibrated pipet was connected to (2). Changes in pore volume of the core as overburden pressure was applied were noted by reading the amount of kerosene produced into the pipet. To correct for the change in volume of the lines inside the hydraulic cell as a function of pressure, a pressure-vs-volume run was made with a solid Lucite cylinder substituted for the core. The change in volume of the lines was about 10 per cent of the change in pore volume of the core. No correction was needed for the permeability measurements because there was no measurable pressure drop in the lines at the maximum overburden pressure. Relative gas permeabilities were measured by the stationary liquid method described by Osoba, et al.' Gas saturations were obtained by allowing the kerosene from a kerosene saturated core to evaporate out. This procedure was followed

Jan 1, 1953

By E. H. Crabtree, Neil S. Parker

The custom milling plant of the Eagle-Picher Mining and Smelting Co. is at Sahuarita, Arizona, approximately 20 miles south of Tucson. It is connected by a 2-mile railroad spur to the main line of the Southern Pacific Railroad between Tucson and Nogales. The capacity of the plant is 500 tons per day. The mill is conventional except perhaps in the rather wide variety of ores treated. These vary from straight copper ores, from which only one concentrate is produced, and lead-zinc or copper-zinc ores from which two concentrates are produced, to complex gold-silver-copper-lead-zinc ores, which require the simultaneous production of three or lour concentrates. Custom ores are received in lots varying in size from a few truckloads to several carloads. Similar ores, after crushing and sampling, may be commingled, or individual lots may be milled individually. The ores are first dumped either into one of two 200-ton railroad bins, or into one of the two 75-ton truck bins. From these bins the lot of ore is individually crushed in a 24 by 16-in. jaw crusher to 3-in. size, and then to ½-in. size in a 3-ft Symons shorthead crusher. After crushing to ½-in., the ore is conveyed to the automatic sampling plant. This consists of three Vezin samplers in series, each successively cutting out 10 pct, 10 pct and 5 pct of its feed. After No. I sampler, the material passes through a mixing barrel and is then crushed to -in. in a set of rolls before passing to No. 2 sampler. Between No. 2 and No. 3 samplers, the ore is again mixed in a mixing barrel. The final sample, consisting of one pound per ton of ore, is taken to the laboratory, where it is further crushed to 1/8-in. in a coffeemill, and then riffled down to the size required for grinding in a pulverizer. The capacity of the crushing and sampling plant is up to 100 tons per hour, depending upon the character of the ore. After sampling, the ore is stored in five ore-storage bins, consisting of four 200-ton bins and one 175-ton bin. Each of these bins is discharged by means of belt feeders and conveyor to the ball mills, so that ores may be composited for milling in any required ratio, or milled separately by themselves. Fine grinding is done in one 6 by 4-ft Allis-Chalmers ball mill and one 8-ft by 36-in. Hardinge mill. These two mills both discharge to one 54-in. Akins Simplex High weir classifier. The classifier sands can be returned to either or both mills, so that flexibility in grinding for different ores is easily obtained. Flotation equipment consists of four 66-in. Fagergren machines for copper-lead roughing and six similar machines for zinc roughing. Lead-copper bulk concentrate is cleaned and recleaned in eight No. 18-S Denver machines, and zinc concentrate is cleaned in three 66-in. Fager-grens. Copper-lead differential separation

Jan 1, 1949

By S. F. Reiter, You-Chao Liu, W. R. Hibbard

Cyril Stanley Smith in his classic 1948 Institute of Metals Lecture&apos; noted in the case of annealing twins that: "It is well known that approximately the same number of twins per grain and the same general geometry are maintained in large grains as in small ones, a fact that certainly suggests a mechanism such as the above where boundaries and twins grow proportionately together. If this view is correct, a spherical grain should have no mechanism for keeping its twins." Such a constancy of twins per grain would be of particular interest as a tool for the study of the origin of annealing twins. It has been proposed by Mathewson2 and later by Barrett3 that in face-centered cubic metals slip occurs in the {111} Plane by <112> shears which combine in pairs to produce the macroscopically observed <110> movement. This proposal is schematically inviting since <112> slip permits the atoms of one plane to move along the interatomic valleys of its neighbor rather than up the hills across the atom sites. There is strong experimental evidence? that annealing twins result from the growth of nuclei in the form of "twin faults" produced by single <112> shears. It is possible that more twin faults would form at low deformation temperatures than at high ones, because the more rigid lattice may increase the tendency to "freeze" the twin faults and prevent their dissipation in slip. This is suggested by (1) the greater resistance to slip at low temperatures and (2) greater tendency toward mechanical type twinning at low temperatures (a summary of these factors is presented by Seigle and Brick5). These considerations would suggest the following: a. Constant twin/grain ratio for specimens deformed constant amounts at a constant temperature, but annealed at various temperatures above the recrystalliza-tion temperature. b. Larger twin/grain ratios for re-crystallized specimens previously deformed constant amounts at lower temperatures. The purpose of this investigation is to test these considerations. One half in. rods of phosphorous deoxidized electrolytic copper and 70-30 alpha brass (68.36 pct Cu, 0.005 pct Pb, 0.01 pct Fe, 31.62 pct Zn remainder) were rolled to a thickness of 0.350 in., milled to specimens 0.350 X 0.437 X 2 in., and annealed at 700°C to an average grain size of 0.065 and 0.090 mm, respectively. These specimens of each metal were then rolled 50 pct reduction in thickness and annealed one hour under conditions which were all combinations of the following: Rolling Annealing Temperatures. Temperatures. °C °C -70 400 25 500 200 600 Standard metallographic techniques&apos; were used to prepare specimens. By the method of lineal analysis7 using a minimum of ten samples of fifty grains each for each specimen, the ratios of twins* per total grains, twins per twinned grain, twin families* per total grains and twins per twin family were determined. Recrystallized grain size was determined by A.S.T.M. comparison methods.8 All observations were made on the rolling plane. The results are tabulated in Table 1.

Jan 1, 1950

By Kefton H. Teague

Attempts to locate domestic supplies of sillimanite have been unsuccessful until recently. This paper describes recent discoveries of sil-limonite-bearing schists in the Southeastern States, with emphasis on geology of the deposits, mineral composition, origin, and reserves. Statements concerning possible methods of mining, milling, and utilization of sillimanite are given. Results from refractory tests on a laboratory scale are summarized. SINCE 1917, when synthetic mullite was first used in spark plug porcelains, there has been a continued search for natural sillimanite. During the recent war this search was intensified, not only for sillimanite but also for any materials which could be used satisfactorily as a substitute for the imported kyanite from India. The Indian massive kya-nite does not decrepitate during calcination as does our domestic bladed kyanite, thus a coarse grog can be obtained from it. Some of the most promising domestic materials suited for high temperatures are limited in quantity. Massive topaz from Chesterfield County, S. C., showed promise of possessing desirable refractory properties; but the action of combined fluorine, liberated during calcination, upon equipment and surroundings, as well as a limited supply of ore and the presence of impurities discouraged its use. Residual lumps and boulders of massive kyanite, similar to the material imported from India, occur in Georgia. This material, like the massive topaz, is of limited quantity. Andalusite from California and dumortierite from Nevada are satisfactory high-temperature refractory materials. Their uses have been restricted to specialized products since the location and character of the deposits are such that large production is impractical. Sillimanite, like kyanite and andalusite, has the theoretical chemical composition of Al2SiO5. It has a hardness of 6 to 7; vitreous, silky to subadamantine luster; specific gravity of 3.2 to 3.3; and is gray to bluish gray in color. Under the binocular microscope, the crystals are transparent. The mineral may occur as dense, fibrous mats (fibrolite) composed of fibrous, sometimes radiating hair-like crystals in schist which are associated with igneous intrusions. Deposits of this type have widespread distribution, but none discovered to date appears to have commercial possibilities. Sillimanite also occurs as bundles of crystals disseminated in biotite schist, as noted in the Hart-Elbert-Madison County, Ga., area and in some of the South Carolina and North Carolina deposits. This type of material has been called prismatic sillimanite by the U. S. Bureau of Mines. Deposits of this variety appear to offer commercial possibilities. When heated above 1650°C, sillimanite expands about 6.5 pct and is converted into a mixture of mullite (3Al2O3 . SiO2) and vitreous silica. This is a stable mixture which has a specific gravity of about 3.15. General Geology: Sillimanite (fibrolite) is a mineral common to the pre-Cambrian metasedi-ments of the Southeast. It occurs throughout the crystalline schists which lie between the Fall Line on the southeast and the established Paleozoic rocks on the northwest (fig. 1). In addition to the meta-sediments, this area contains pre-Cambrian igneous

Jan 1, 1951

By J. O. Scott

Transient pressure behavior of wells intersected by a single vertical fracture has been examined by means of a heat pow analogy. Results are correlated in terms of dimensionless pressure change and dimensionless transient time. The resulting curves are found to lie between the dimensionless curves for a cylindrical well and a line source when effective well radius is expressed as one-fourth of the total fracture length. Results are also shown for various degrees of afterflow. Use of the curves provides a means of determining reservoir permeability, wellbore radius, and thereby fracture length, even when the final slope of the transient curve is not obtained. Superposition of curves may be used to confirm existence of vertical fractures in the reservoir adjacent to the well or to indicate a damaged zone on the fracture face. INTRODUCTION Hydraulic fracturing has become a standard well completion practice for the purpose of increasing flow. Results are normally gauged in terms of some sort of "stabilized" flow rate established before and after the treatment. This procedure may be misleading because pressures in or around the well do not become "stabilized" during the test period. Transient pressure tests on fractured wells can overcome the objections to stabilized flow tests by indicating when a stable pressure gradient is reached. In addition, the transient pressure tests can be used to determine formation flow capacity and effective wellbore radius. The effective wellbore radius may be used as a measure of the success of the fracturing operation. The slope and position of the transient pressure-log time curve may be used to determine the flow capacity and wellbore size after sufficient lapse of time so that the pressure gradient in the vicinity of the fractures becomes constant. However, in tight reservoirs or in short tests this condition may not be reached. Presence of the fractures in tight reservoirs may cause a constantly increasing slope to the transient pressure curve. If this slope is picked too soon, formation flow capacity will appear high and the fracture size will appear too small. This paper is intended to clarify the early transient behavior of vertically fractured wells. It shows how formation flow capacity and wellbore size can be determined even though the maximum slope of the transient pressure curve is not obtained during the test. Development of the techniques of transient pressure analysis for wells has been summarized by Perrine.&apos; He reviews the various definitions of wellbore effects such as skin effect, productivity ratio, damage factor and condition ratio. In the present paper, use of these terms is avoided by defining an effective wellbore size. For the fractured well this effective wellbore size is larger than the actual wellbore. Assumptions made are constant flow rate at the well, constant fluid compressibility, constant fluid mobility and uniform porosity and formation thickness. From the basic differential equations of flow, two different solutions may be obtained. The first, the line source solution, is commonly used in transient pressure analysis.&apos; It expresses the change in pressure at any radius due to withdrawal or injection of fluid at the line source from an infinite reservoir at uniform initial pressure. This equation, in oil field units: is

By P. P. Scott, George C. Howard

A field remedial procedure utilizing a kerosene-cement slurry as a water plug-off agent in fractured formations was evaluated both in the laboratory and in the field. This procedure has proved to be capable of effectively shutting off water without causing permanent impairment of the oil production. Success was attributed to the fact that an immobile cement slurry, when placed in a water-producing strata, will set and form an impermeable barrier; whereas when placed in an oil-producing section the cement will retain a relatively high permeability and may be removed by acidizing. INTRODUCTION One of the most perplexing problems facing the oil industry is the selective exclusion of water production from oil or gas-producing wells. This problem has been studied by many investigators in an attempt to develop a material that is not only capable of reducing water production but is also capable of being selective in that it will not impair oil production in either fractured or intergranular type reservoirs. A study of these two types of formations indicated that two distinct types of materials for controlling water production might be required — a completely liquid plugging agent for intergranular formations and a semi-liquid or slurry type plugging agent for fractured formations. This paper is limited to the control of water production from fractured formations. A common source of water in the vicinity of oil bearing rock reservoirs is water which previously has entered and, because of its higher density, generally lies near the bottom of the formation. When the deepest point of penetration of a well into such an oil and water-bearing formation is above the level of the water, and the dynamical gradients due to the flow of oil overbalance the difference in densities between oil and water, water production becomes a problem. Then the water level rises in the shape of a cone and is produced from the lower depths. Other investigators1,2,3,4 have developed theories which define the pressure gradients and contours of this cone in a homogeneous formation and have shown that the placement of a plug in the bottom of a well is only slightly effective in temporarily reducing the flow of water. Assuming that the manner of flow of bottom water from fractured formations to a well is generally similar to the flow in homogeneous formations, then it would be expected that some form of coning, perhaps of less symmetry, would also occur. Then, because of the similarity of the manner of flow of water, placement of a vertical plug in a fractured formation would also probably be ineffectual for controlling water production. However, as has been shown by electric model flow study,&apos; the placing of a plug in a well and an impermeable horizontal streak in the formation might prove to be a means for materially reducing or even eliminating water production in a fractured formation. An indication of the difference in effectiveness between horizontal and vertical plugs based on theory developed from study of the flow of water and oil in rock reservoirs is depicted in Fig. 1. These curves show the expected

Jan 1, 1955

By H. Stuart, L. Zwell, N. Ridley

specimen that was subjected to 700°C for 250 hr is shown in Fig. 2(c). The precipitates in this foil appear round and exhibit only very faint strain contrast. From this evidence, along with that described above for the symmetry of the strain field, it may be concluded that this coherent precipitate is spherical, which is generally the favored shape for coherent precipitates when the lattice parameter mismatch is small.12 These observations are consistent with the assumption that this precipitate is the y&apos; (Ni3Al, Ti) phase. y&apos; is known to be spherical in the early stages of precipitation. It is fcc and is similar in composition to the matrix and thus would have contrast similar to that of the matrix as do these precipitates. Direct identification of the spherical precipitate did not prove possible because of its low volume fraction and small size. The results of this investigation suggest that the increases in yield strength and the decreases in elongation observed in 45-Fe 30-Ni 20-Cr alloys containing about 0.4 pct A1 and 0.4 pct Ti on prolonged aging at 550" to 700°C are very likely due to the presence of a coherent, spherical precipitate, thought to be y&apos;. Mi-crohardness measurements indicated that the precipitation of semicoherent M23C6 resulted in some matrix hardening. However, this precipitation process occurs much more rapidly than the changes in mechanical properties at these temperatures. 1C. L. Clark, J. J. B. Rutherford, A. B. Wilder, and M. A. Cordovi: J. Eng. Power, 1962, vol. 84, p. 258. 2 F. A. Comprelli and U. E. Wolff: USAEC Report GEAP-4745, General Electric Company November, 1964. 3C. N. Spalaris: A Monograph, USAEC Report GEAP-4633, General Electric Company, July, 1964. THERE have been many X-ray investigations of the room temperature lattice parameters of austenite which has been retained in quenched steels of various carbon contents. The results of these investigations have been collected by Wrazej,1 Wever et al.,2 and by Roberts3 and are included in Fig. 1 due to Pearson.4 The dashed line in Fig. 1 was considered by Roberts3 to most reliably describe the variation with carbon content of the lattice parameter of retained austenite. This line is given by the equation: a (Å) = 3.555 + 0.044 wt % C and recent unpublished measurements by one of the authors (LZ) support this relationship. The object of this communication is to draw attention to a relationship which describes the variation of the room temperature lattice parameter of &apos;equilibrium&apos; austenite with carbon content, and which is different from that for retained austenite. The relationship a(Å) = 3.573 + 0.033 wt % C has been obtained from lattice parameter measurements made on equilibrium Fe-C austenites at elevated temperatures, which have been extrapolated to room temperature. The room temperature lattice parameter of 3.555Å which the Roberts&apos; relationship gives for pure y-Fe is no: in agreement with the value of 3.573Å obtained when the high temperature lattice parameter data of Basinski et aL.5 and of Goldschmidt6 is extrapolated to room temperature. A linear extrapolation was

Jan 1, 1970

By M. R. Geer, H. F. Yancey

Coal washing assumed an important role in the mining industry of the Pacific Northwest long before washing practice became firmly established in the Appalachian field. A Scaife washer was operated in the state of Washington in 1887; and by 1927, the fist year for which complete statistics were compiled, nearly a third of the state&apos;s coal production was washed, in comparison with only about 5 pct for the country as a whole. Mechanical preparation was adopted in Alaska in 1922 in a plant constructed by the United States Navy at Chickaloon to provide bunker coal for naval forces operating in northern waters. Many of the coal beds mined in Washington and Alaska contained more impurities than those mined elsewhere, and this circumstance contributed to the early interest in mechanical cleaning. A much more important factor, however, was the inclination of the coal beds. With steeply pitching beds, hand sorting by the miner at the face is impossible; consequently, all material must be loaded and dealt with on the surface, just as is now proving the case with mechanical mining of flat beds. Thus "full-seam" mining afforded the same stimulus to the early development of coal washing in the Northwest that it is providing under mechanization in the rest of the country today. Objeet and Scope &apos; This report is intended to provide a general summary of the status of coal-washing practice in Washington, Oregon, and Alaska—an area in which some of the coals mined are more difficult to wash than those mined elsewhere in the country. Detailed flowsheets of plants, statistical data on production, and cost figures have been omitted, largely for the sake of brevity but also because such information is principally of only local interest. On the other hand, considerable washability data have been included because they are Washington At present Washington leads all other states in the percentage of its total production that is cleaned mechanically, 82.1 pct in comparison with the national average of 25.6 pct in 1945.&apos; The washing problems encountered in this state are highly variable because the mountain-building forces that created the Cascade Range caused such intense folding and faulting of the beds in some fields that the rank of the coal was increased to anthracitic, while in other fields more distant from the mountains the beds were relatively undisturbed, and the rank of the coal ranges down through subbituminous to lignitic. The complicated and burdensome schedule of sizes prepared in most coal fields has never been required by the Washington market. With but few exceptions, lump is prepared on a round-hole screen of about 3 in. size, egg is about 3 to 1 5/8 or 1½ in., and nut is 1 5/8 or 1½ in. to either 1 or ¾ in. Some mines screen no finer than ¾ in. and market a slack coal of that top size, but generally the coal is screened at about ¼ in. to give a stoker coal of ¾ or 1 to ¼ in., and a ¼ in. to 0 "buckwheat." During recent years the market for lump coal has largely disappeared, and lump is crushed to supplement the pro-

Jan 1, 1950

By W. C. Winegard, E. L. Holmes

The effects of the solute elements lead and bismuth on grain growth in zone -refined tin have been investigated. At low temperatures, viz. below 160°C. or at high concentrations, viz. greater than 0.03 at. pct, the temperature dependence of grain growth was found to be constant. A correlation was found to exist between the rates of grain growth in the presence of solute impurities and the factor [C Ir - 1]2 , where C is the solute concentration, r is the radius of solvent atom, and r&apos; is radius of solute atom. It is shown that the Liicke and Detert theory does not give a satisfactory explanation of the results obtained. INVESTIGATIONS of grain growth in zone-refined lead and tin and some effects of solute elements on grain growth in these metals have been reported by Bolling and winegardly2 and Holmes and winegard? The present investigation is an extension of the previous work, and was undertaken to provide additional results which might make it possible to discover the mechanism whereby the rate of grain growth is affected by the presence of foreign solute atoms. The experimental procedure was exactly the same as that described previously.3&apos;4 Figs. 1 and 2 show the results obtained with lead and bismuth additions over the same temperature range, viz. 167" to 220°C, as that used for the investigation of grain growth in zone-refined tin.3 Fig. 3 shows the results obtained for zone-refined tin and for this tin with lead solute additions over an extended temperature range. DISCUSSION OF RESULTS As mentioned previously,3 the character of grain growth in the particular zone-refined tin used in these experiments appears to change as the temperature of annealing falls below about 160°C. The grain growth became somewhat irregular and was characterized by a jaggedness of many of the grain boundaries. The reason for this change is not known, but may be due either to residual impurity effects or possibly an oxide precipitation. It was obvious that normal grain growth only occurred in the zone-refined tin through the high-temperature range 167" to 220°C, and so the effects of solute atoms on grai11 growth over the two temperature ranges will be discussed separately. a) Effect of Impurity on Grain Growth in the Temperature :Range Above 167°C. It is apparent from Figs. 1 and 2 that, for low concentrations of solute, the rates of grain growth tend towards a common value as the melting temperature of tin is approached. As the concentration of lead is increased, the rate of grain growth close to the melting temperature is also reduced, and at high concentrations the temperature dependence of the rate of grain growth appears approximately constant. It should be noteil that the effect of bismuth is greater than that of the same concentration of lead, but both these solutes have a smaller effect on the rate of grain growth than silver, as seen from an earlier investigation of Holmes and Winegard. It should

Jan 1, 1962

By E. E. Donath

THE coal hydrogenation process is well known as a means for the production of liquid fuels -from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aromatics and of tar acids and tar bases. The relative amounts of heavy and middle oil-boiling above and below, e.g., 325°C-can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.1 Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydro¬gen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catch-pot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1952

By H. Buttner, F. H. Udin, J. Wulff

GRAIN boundaries, the interface between adjacent crystals differing only in respective orientation, have been the object of much experimental and moderate theoretical attention for many years. The earlier experimental work was primarily concerned with the effect that grain boundaries have on the physical behavior of metals, while the basic nature of the boundaries themselves drew only secondary attention. A complete turnabout has been witnessed in more recent years, however, as researchers are now undertaking investigations bearing as directly as possible on the character and physical properties of the grain boundary. Quite comprehensive reviews of the past literature on the subject of grain boundaries have been reported on numerous occasions by various authors, and together these references represent a thorough coverage.&apos;-? It becomes evident in these reviews and other papers"" that the properties of grain boundaries can be explained by regarding a grain boundary as a crystalline region of transition between two unmatched grains. Studies show that grain boundaries have a definite interfacial energy. By measuring the geometry about a point where three interfaces meet in equilibrium, the energy of any two boundaries can be measured with respect to the third. If the absolute interfacial energy of one boundary is known, the absolute energy of the other two boundaries can be calculated. This apparently holds true for any system of phases and interfaces.""25 Most studies have been carried out on solid-solid or liquid-solid systems, or systems of both. However, if about the point of intersection one phase is vapor and the other two are disoriented grains, then two interfaces are surfaces, and one is a grain boundary. Investigations leading to relative grain boundary energy for this particular system have been made by Fullman,23 Greenough and King," and Bailey and Watkins." Herring" treats the system mathematically and arrives at an equation, which appears as Eq. 1, in a form consistent with the reference angles indicated in Fig. 1, ( d?1 ?n = x sina + cosa ( ------- 2 ?2 Sinß da + C0Sß (d?2/d As the system of interfaces comes to equilibrium, a groove of angle appears at the intersection of the grain boundary with the surface, an effect first observed by Rosenhain and Humfrey." Eq. 1 is essentially a summation of the vertical components in Fig. 1 set equal to zero, where ?1 and ?2 are surface tension vectors lying along the side of the groove at point 0 in the groove root. The differential vectors represent the forces tending to rotate the surface into a position that will expose a crystal cleavage surface of lowest energy. Chalmers, King, and Shuttleworth- simplify Eq. 1 by assuming the differential vectors equal to zero, ?1 = ?2= ?Surface and arrive at the following equation: ?B = 2?s cos [2] Greenough and King24 use Eq. 2 for determining the grain boundary energy of silver using prepared bi-crystals of known orientation. Bailey and Watkins25 have done the same for copper, as did Chalmers and others on lead. These authors report the grain boundary values as ratios relative to the surface energy. In the above work, the orientation of grains forming the grain boundary in all cases was controlled so

Jan 1, 1954

By C. E. Morris, S. R. Pollack

Current -vo1tage -temperature characteristics were studied for Al-A12O3-Al, Au structures. The oxide film was grown by gaseous oxidation in an 0, glow discharge. The electron-transfer mechanism was identified as tunneling and the barrier heights and thickness were determined. It was found that the barrier height at the parent aluminum-oxide interface is 1.5 ev and the built-in vloltage with an aluminum counter electrode is 0.35 v. The growth mechanism of the oxide is also discussed and it is suggested that Mott&apos;s theory is not applicable in describing the growth. Discrepancies were observed in the detailed comparison of tunneling theory, based on a trapezoidal model, with the data, and several possible explanations are discussed. THEORETICAL analyses of electron tunneling from one nonsuperconducting metal to another through an extremely thin insulating film have been presented.1-6 These calculations relate the current density, J, to the voltage, V, between the two metals, and to the temperature, T. The results of these calculations indicate that the magnitude of J and the detailed shape of the J-V characteristic will in general depend most strongly upon such properties of the insulating film as the thickness, the dielectric constant, and the structure of the electron energy barrier profile. The experimental results of many7-11 workers have corroborated the main features of these calcu- lations and have in fact been used to determine properties of the thin insulating film. It has been demonstrated, for example, that the tunneling current formulation of simmons4 is adequate to describe the observed J-V characteristic over approximately 10 orders of magnitude of current. Furthermore, from these observations and analyses, insight into the nature of the A1-A12O3 (thermally grown) interface region has been obtained.&apos;&apos; The temperature dependence of the tunnel current has also been studied and, although a self-consistent set of tunneling parameters can be chosen to describe these data at low voltages (i.e., <0.5 v), the tunneling parameters are different from those obtained from higher voltage (i.e., of the order of 1 to 5 v) measurements." We have measured the effect of temperature and voltage upon the tunnel current at higher applied voltages and find that the theory is inadequate to describe all of the effects reported here. A discussion of the origin of this inadequacy is presented following a description of the samples used for these experiments, and the experimental results. SAMPLE PREPARATION Metal-insulator-metal structures were fabricated in the following way. A 99.999 pct A1 charge was used to deposit, in vacuo, thirty films, 2000Å thick, onto a 1 by 2 in. glass substrate (7059 Corning glass). Prior to deposition the substrate was glow-discharged for final cleanup and then baked at 200°C for 2 hr at a pressure of 5 x 10-7 torr. The pressure during deposition of the metal films was 2 X 10-6 torr and the deposition rate was 50 to 100Å per

Jan 1, 1965

By Harvey Cline, Donald P. Ferriss

THE violent outgassing of commercial tungsten and other refractory metals when melted in an electron beam zone refining apparatus1"3 is dealt with experimentally by one or both of two approaches. One is to provide a suitable emission current control1,2 the other is to purify the metal in the solid state before melting.4 The first of these is usually sufficient, but the authors chose also to investigate the source of the troublesome gases and to devise means of solid-state purification. Some further insights into the use of tungsten as a structural material at temperatures near its melting point were also revealed in the course of the work. One may speculate on the causes of gas formation in tungsten at high temperature by inferences from the literature and an examination of the impurities in commercial wire. Davenport5 observed microporosity in both tungsten and molybdenum filaments heated to several hundred degrees below their melting points. Studying the function of oxygen in molybdenum welds, Perry, Spacil, and wulff8 attributed similar porosity to the disproportionation of Moo2 to molybdenum metal and Moo3. Tungsten dioxide also disproportionates7 above 2000oC to yield WO3 vapor at considerable pressure. Commercial tungsten contains some 5 to 20 wt ppm O and a similar concentration of carbon depending on the details and precautions of processing. Therefore, evolution of CO is also a strong possibility as a source of gas at high temperatures. Furthermore, even for activities in the order of 0.01, it may be calculated that the pressure of CO at 3000°C would be over 4000 psi, which is in excess of the tensile strength of tungsten at this temperature.9,10 Powder metallurgy tungsten contains some 0.02 pet Fe and 0.002 to 0.005 pet of the elements Ni, Si, Al, Ca, Mn, Mg, and Mo; at temperatures over 2800°c, therefore, these elements will exhibit appreciable vapor pressure, though small compared to that of WO3 and CO. Some of these impurities may react to form high-pressure monoxides such as SiO and A10. Finally, dissolved and occluded nitrogen is an ever-present source of high-pressure gas. Commercial Type 218, General Electric filament wires, 0.025 in. diam, were heated by resistance in 10 -4 mm of Hg and in argon or hydrogen at pressures from 50 µ to atmospheric. For temperature determinations in vacuo, the Jones - Langmuir8 current-temperature relationship was employed. For gaseous atmospheres, the burn-out temperature was assumed to be the same as in vacuo so that a small, constant correction could be made for temperatures below burn-out conditions (i.e., local heating to failure). Several dozen experiments may be summarized by pointing out some structural observations. At 3050oC in 1 atm of A, porosity is very evident after 30 min, as shown in Fig. 1. For the section in Fig. 2, failure occurred 200°C below the melting point and many voids have grown in the grain bound-

Jan 1, 1962

By Kefton H. Teague

Attempts to locate domestic supplies of sillimanite have been unsuccessful until recently. This paper describes recent discoveries of sil-limonite-bearing schists in the Southeastern States, with emphasis on geology of the deposits, mineral composition, origin, and reserves. Statements concerning possible methods of mining, milling, and utilization of sillimanite are given. Results from refractory tests on a laboratory scale are summarized. SINCE 1917, when synthetic mullite was first used in spark plug porcelains, there has been a continued search for natural sillimanite. During the recent war this search was intensified, not only for sillimanite but also for any materials which could be used satisfactorily as a substitute for the imported kyanite from India. The Indian massive kya-nite does not decrepitate during calcination as does our domestic bladed kyanite, thus a coarse grog can be obtained from it. Some of the most promising domestic materials suited for high temperatures are limited in quantity. Massive topaz from Chesterfield County, S. C., showed promise of possessing desirable refractory properties; but the action of combined fluorine, liberated during calcination, upon equipment and surroundings, as well as a limited supply of ore and the presence of impurities discouraged its use. Residual lumps and boulders of massive kyanite, similar to the material imported from India, occur in Georgia. This material, like the massive topaz, is of limited quantity. Andalusite from California and dumortierite from Nevada are satisfactory high-temperature refractory materials. Their uses have been restricted to specialized products since the location and character of the deposits are such that large production is impractical. Sillimanite, like kyanite and andalusite, has the theoretical chemical composition of Al2SiO5. It has a hardness of 6 to 7; vitreous, silky to subadamantine luster; specific gravity of 3.2 to 3.3; and is gray to bluish gray in color. Under the binocular microscope, the crystals are transparent. The mineral may occur as dense, fibrous mats (fibrolite) composed of fibrous, sometimes radiating hair-like crystals in schist which are associated with igneous intrusions. Deposits of this type have widespread distribution, but none discovered to date appears to have commercial possibilities. Sillimanite also occurs as bundles of crystals disseminated in biotite schist, as noted in the Hart-Elbert-Madison County, Ga., area and in some of the South Carolina and North Carolina deposits. This type of material has been called prismatic sillimanite by the U. S. Bureau of Mines. Deposits of this variety appear to offer commercial possibilities. When heated above 1650°C, sillimanite expands about 6.5 pct and is converted into a mixture of mullite (3Al2O3 . SiO2) and vitreous silica. This is a stable mixture which has a specific gravity of about 3.15. General Geology: Sillimanite (fibrolite) is a mineral common to the pre-Cambrian metasedi-ments of the Southeast. It occurs throughout the crystalline schists which lie between the Fall Line on the southeast and the established Paleozoic rocks on the northwest (fig. 1). In addition to the meta-sediments, this area contains pre-Cambrian igneous

Jan 1, 1951

By H. T. Bowman

For more than 80 years the Bessemer process has depended upon the ability, skill, and judgment of the blower, although as early as the I860&apos;s it was recognized that the process would benefit by some type of instrumental contro1.l IIowever, instruments with sufficient recording speeds did not exist, so the end-point determination was always dependent upon the blower&apos;s eye. This placed an obstacle in the way of precise experimental work, because of the absence of the necessary records and reference points as reported by Work.2 The use of the photocell provided the instantaneous record of the blow that made this experimental work possible and provided more scientific control for the process as discussed by Graham,3 A brief description of the progress of the blow will illustrate the recording function of the instrument. The silicon in the iron is being oxidized during the first minutes of the blow, as pointed out by Henning4 in a table showing the order of metalloid elimination. The product of this oxidation is a solid that remains in the converter, so there is virtually no flame during this part of the blow. This low flame luminosity is illustrated by the flame recording shown in Fig. I, where the silicon blow is plainly marked. The dull flame of the silicon blow gradually gives way to the brilliant carbon flame as the increasing quantities of carbon monoxide formed inside the converter burn to dioxide upon contact with the atmosphere above the vessel. When the carbon reaches some low value under 0.20 per cent, there is insufficient menoxide formed to maintain the dioxide flame, so its intensity drops. Throughout the flame drop carbon continues to burn, until at some value around 0.05 per cent an arrest occurs in the recorded drop. This point has been designated as the end point. The period of time from this end point until the vessel is turned upon its side and blowing has stopped has been called the afterblow. This afterblow is used as a measure of the degree of metal oxidation, and uniformity demands that it be controlled within narrow limits. Iron and blowing conditions are likely to change several times during a turn, necessitating corresponding changes in end-point control. It is the purpose of this paper to discuss these changes, the factors that make them necessary, and their bearing upon the quality of steel. Carbon-FeO Relationship In the Bessemer process oxidation relationships are precise. Fig. 2 shows a graph of the carbon-FeO relationship. The familiar "bomb-test" method, described by Mccutcheon and Rautio,5 was used for obtaining these and all other dissolved FeO values herein reported, all tests being taken from the converter before deoxidation unless otherwise noted. All tests of 0.10 per. cent carbon and above were obtained from metal blown for duplexing. McGinley and Woodworth6 reported iron oxide values for blown metal, but their tests were obtained by a . different method than were those

Jan 1, 1942

By F. W. C. Boswell, R. L. Cunningham, H. M. Weld

Chemical analysis shows the partition of the magnesium addition between the metal and the graphite is independent of whether the graphite is in the form of nodules or flakes. The bright central spot observed in nodular graphite polished sections is shown to be due to the structure of the nodules. DURING the past few years numerous papers have been published on the production1-7 and heat treatment" of nodular cast irons. However, very little information is available on the structure of the nodules and the reason for their formation. It would appear that an explanation of the phenomenon of nodulation must await a detailed knowledge of the nature of the nodule. Disagreement exists among various workers on such a fundamental point as to whether or not a nodule actually contains a microscopically visible, nongraphitic nucleus.9-11 Work was initiated with a view to obtaining definite information on this and other aspects of the problem. Chemical Separation and Analysis Microscopic appearance had indicated9-11 that a nongraphitic core might exist in nodules (Fig. 1). It appeared that a chemical comparison of separated nodules and flake graphite would be profitable, for if the core is nongraphitic a relatively large amount of certain elements would be found in the nodules as compared to the flake. This comparison could best be made by obtaining nodules and flake from the same melt of cast iron, part of which had been in-noculated with a suitable addition reagent for the formation of nodules. A 300 lb melt was produced. About half of this was innoculated in the ladle with an Fe-Si-Mg alloy to produce nodules and cast into keel blocks; the remaining half of the melt had silicon added in an effort to compensate for the silicon in the innoculant used in the other half of the melt and this was cast into similar keel blocks. The analyses of the resultant irons are given in Table I. Nodules and flake were chemically extracted from 2 kg samples of metal as described in the appendix. While this method dissolved the iron and chromium carbides, it did not dissolve the titanium, vanadium, and molybdenum carbides. These latter carbides could have been removed by nitric acid, but in other experiments it was found that it attacked pools of metallic iron entrapped in the nodules which had, until the nitric acid treatment, been protected from the attack of the sulphuric, hydrochloric, and hydrofluoric acids. It will be shown in the next section that entrapped iron exists in nodules but not in flake. On microscopic examination many tiny irregular particles were observed to accompany both the nodules and the flake. These were identified by tabling a sample of nodules from which a sufficient fraction was obtained for X-ray analysis. A good pattern of titanium carbide was obtained indicating that this was the predominant compound present. Since it was not possible to determine how completely the carbides could be removed mechanically and since their removal from flake is much more difficult, it was decided not to resort to any separation as this would render further comparisons more difficult. The samples were ashed in a combustion

Jan 1, 1953

By Charles A. Stickels, Edward E. Hucke

The dihedral angle, formed by the intersection of three interfaces, is often determined by measuring a sample of apparent angles of intersection seen on a random plane of polish, then comparing the exerimental distribution of angles to the distribution calculated by Harker and Parker. Statistical tests show that the latter distribution does not satisfactorily describe the population from which samples are drawn. It is concluded that the major reason for this discrepancy is the presence of a range of dihedral angles in all specimens. When reasonable care is used experimentally, random measuring error is unimportant. It is shown that measurements made on dispersed second-phase inclusions are subject to a systematic error depending on inclusion size, which can be minimized by using adequate magnification. A dihedral angle, calculated from a sample of observed angles as though a unique dihedral angle were present, is termed an "effective dihedral angle". Experience has shown that "effective dihedral angles&apos;&apos; are reproducible quantities, useful for characterizing samples. Methods of determining an "effective dihedral angle", establishing its reliability, and making comparisons between samples are discussed. THE authors have recently reported measurements of the dihedral angle formed by liquid-lead inclusions lying in nickel grain boundaries.&apos; Di- hedral angles were measured by the statistical method first employed by Harker and parker2 and used subsequently by many other workers.3"8 Since a relatively high degree of accuracy was necessary in the authors&apos; experiments, the reliability of this method of dihedral-angle measurement was examined. Briefly, this method of measuring dihedral angles is usually performed as follows. A multiphase alloy is prepared, equilibrated under conditions which allow sufficient interface mobility to establish equilibrium, quenched to room temperature, then prepared for metallographic examination. A large number of observed angles, formed by the traces of grain boundaries and/or interphase boundaries on the plane of polish, are measured at high magnification. If all orientations of interfaces in the specimen are equally probable, Harker and parker2 showed that the population of observed angles is described by a distribution function containing a single parameter, the dihedral angle, 8. certain properties of the population, e.g., the mode or median, have been calculated from this distribution function in terms of the dihedral angle.3, 9 Thus, if the mode or median of a sample is identified with the corresponding property of the population, a unique value for the dihedral angle is determined. One defect in this procedure lies in identifying the properties of a sample of observed angles with the properties of the population from which they are drawn. If one were to proceed in a more rigorous fashion, it would be necessary to find a function of sample properties which is an estimator of the dihedral angle. Then by determining the distribution function for the estimator one could set limits on the value of the dihedral angle. The most apparent obstacle to this straightforward approach is the complexity of the distribution function assumed to describe the population. In analytical form, the distribution function may be written:2, 10

Jan 1, 1964

By John McGhee, Jack Newcombe, M. J. Rzasa

A series of water floods was made on laboratory prepared unconsoli-dated sand columns to study the effects on oil recovery of the solid-water-oil contact angle, the oil-water interfacial tension, flood rate, and oil viscosity. A procedure was developed for treating silica sand with silicone polymer to produce surfaces of varying degrees of wettability as evaluated by measuring the contact angle on a flat silica plate that had been simultaneously treated with the sand. Fluid interfacial tensions were changed by the use of surface active agents in the flood water. Water-wet, oil-wet, and intermediate wettability systems were studied at high and at low values of interfacial tension, at several flood rates, and with oils of different viscosities. For both oil-wet and water-wet systems and a low viscosity oil, recoveries were functions of the oil-water interfacial tension; also, increase in flood rate resulted in increased oil recoveries. High interfacial tension floods were more efi- cient than low interfacial tension floods on water-wet systems, while low interfacial tension floods were more eficient on oil-wet systems. Intermediate or neutral wettability systems were less sensitive to rate of flood advance and interfacial tension than either oil-wet or water-wet systems. The eflects of surface forces on oil recovery for high viscosity oils were not so well defined as for low viscosity oils. INTRODUCTION Reservoir rock surfaces vary in their wettability1, some being water-wet while others are apparently oil-wet. The factor of wettability enters into reservoir performance in both primary and secondary recovery, and into laboratory measurements of capillary pressure, connate water saturation, and relative permeabilities.&apos; In theory, the degree of wettability is measured by the contact angle for the system solid-water-oil. A water-wet system is defined as one in which the advancing water contact angle is less than 90". An oil-wet system is one in which the advancing water contact angle is greater than 90°.3 The surface forces in a solid-water-oil system are related by the Young-Dupree equation as follows4: These surface forces are commonly expressed as the difference in adhesion tension, or the product of the water-oil interfacial tension and the contact angle. If the contact angle is less than 90°, the adhesion tension difference is positive and oil displacement by water from a solid surface will be spontaneous and favored by a high oil-water interfacial tension. If the angle is greater than 90" the displacement will not be spontaneous but will require less energy the lower the oil-water interfacial tension. The contact angle and interfacial tension also appear in the capillary pressure equation5: PC = 2ocosejr .... (2) The quantity cos was used by Rapoport and Leas6 s a factor in the generalized form of their "sealing coefficient." Warren and Cal-houn&apos; presented the results of cos on oil recovery in oil-wet systems and correlated their data using a "scaling coefficient" suggested by Jones-Parra and Calhoun.8 The "sealing coefficients" were advanced to help correlate the effects of the variables influencing oil recovery by

Jan 1, 1956

By H. T. Bowman

For more than 80 years the Bessemer process has depended upon the ability, skill, and judgment of the blower, although as early as the I860&apos;s it was recognized that the process would benefit by some type of instrumental contro1.l IIowever, instruments with sufficient recording speeds did not exist, so the end-point determination was always dependent upon the blower&apos;s eye. This placed an obstacle in the way of precise experimental work, because of the absence of the necessary records and reference points as reported by Work.2 The use of the photocell provided the instantaneous record of the blow that made this experimental work possible and provided more scientific control for the process as discussed by Graham,3 A brief description of the progress of the blow will illustrate the recording function of the instrument. The silicon in the iron is being oxidized during the first minutes of the blow, as pointed out by Henning4 in a table showing the order of metalloid elimination. The product of this oxidation is a solid that remains in the converter, so there is virtually no flame during this part of the blow. This low flame luminosity is illustrated by the flame recording shown in Fig. I, where the silicon blow is plainly marked. The dull flame of the silicon blow gradually gives way to the brilliant carbon flame as the increasing quantities of carbon monoxide formed inside the converter burn to dioxide upon contact with the atmosphere above the vessel. When the carbon reaches some low value under 0.20 per cent, there is insufficient menoxide formed to maintain the dioxide flame, so its intensity drops. Throughout the flame drop carbon continues to burn, until at some value around 0.05 per cent an arrest occurs in the recorded drop. This point has been designated as the end point. The period of time from this end point until the vessel is turned upon its side and blowing has stopped has been called the afterblow. This afterblow is used as a measure of the degree of metal oxidation, and uniformity demands that it be controlled within narrow limits. Iron and blowing conditions are likely to change several times during a turn, necessitating corresponding changes in end-point control. It is the purpose of this paper to discuss these changes, the factors that make them necessary, and their bearing upon the quality of steel. Carbon-FeO Relationship In the Bessemer process oxidation relationships are precise. Fig. 2 shows a graph of the carbon-FeO relationship. The familiar "bomb-test" method, described by Mccutcheon and Rautio,5 was used for obtaining these and all other dissolved FeO values herein reported, all tests being taken from the converter before deoxidation unless otherwise noted. All tests of 0.10 per. cent carbon and above were obtained from metal blown for duplexing. McGinley and Woodworth6 reported iron oxide values for blown metal, but their tests were obtained by a . different method than were those

Jan 1, 1942