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By S. E. Bretherton

Discussion of the paper of S. E. BRETHERTON, presented at. the San Francisco meeting, September, 1915, and printed in Bulletin No. 104, August, 1915, pp. 1595 to1599. ANTON EILERS, Brooklyn, N. Y. (communication to the Secretary*). While the advantages in the use of high-line siliceous slags in lead smelting which Mr. Bretherton discusses in this paper are obvious under certain economical conditions, he gives me credit for the introduction of such slags when it does not belong to me. It is true I did considerable experimental work, off and on, for the purpose of finding such slags, while at the Germania in 1877 and 1878, but I did not have occasion to introduce any such slags for regular work, because I had no ores which fitted the economical conditions for using high silica and high lime, except in isolated cases for very brief periods. On the contrary, the ores I had to treat were mostly very ferruginous and very low in silica, so that, economically, I was compelled to run nearly always on slags, which allowed me to use the abundant flux I had without cost. It was August Raht who first had occasion to establish and use for long periods a slag high in silica and line, and low in iron. This was when he was confronted with the task of smelting the. Horn-Silver ores at the smelting works at Franklin, Utah, with as little expenditure for fluxing material as possible. I was at that time in Leadville, Col., where, in the new works I had built, the Billings and Eilers smelters, I had occasion to use profitably many slags, but never anything as high in the earthy bases and in silica as Mr. Raht had to use.

Jan 12, 1915

By H. P. Greenwald

THIs paper brings forward a discussion that was prepared for the meeting of the Coal Division in Chicago in 1938.1 War in Europe less than a year after that meeting, followed by our defense preparations and entry into the conflict, caused general cessation of large-scale experimentation on the subject, and it is best to confine this paper to events in the United States during the five-year period since the preceding paper was written. The views of members of the Coal Division's Committee2 on Rock-dust-ing for 1943 were obtained before this paper was written and the manuscript was reviewed by them. Extent of Rock-dusting Statistics on the use of rock dust in the United States during the years 1930-1933, appearing on page 97 of Volume 139 of the Transactions are extended in Table I herein through the year 1941. The results through 1933 did not appear encouraging, but there has been improve-ment since that date. It has always been true that the larger operations were the ones that used rock dust. In 1941 only 10 per cent of the mines in the country used rock dust, but they produced 57 per cent of the coal, employed just under 50 per cent of the miners, and accounted for 52 per cent of the man-hours. Unfortunately, collection and compilation of these statistics are slow procedures, and figures dealing with the tremendous war expansion of the industry are not likely to be available for a year or more. In 1941 the five leading states in regard to percentage of man-hours worked in mines using rock dust were: Utah, 92.1; Wyoming, 79.3; Alabama, 77.4; New Mexico, 72.5; West Virginia, 65.3. The first four states were the same as in 1933, but West Virginia displaced Washington in fifth place. On the basis of pounds of rock dust used per ton of coal, the five leading states in

Jan 1, 1944

By H. P. Greenwald

THIs paper brings forward a discussion that was prepared for the meeting of the Coal Division in Chicago in 1938.1 War in Europe less than a year after that meeting, followed by our defense preparations and entry into the conflict, caused general cessation of large-scale experimentation on the subject, and it is best to confine this paper to events in the United States during the five-year period since the preceding paper was written. The views of members of the Coal Division's Committee2 on Rock-dust-ing for 1943 were obtained before this paper was written and the manuscript was reviewed by them. Extent of Rock-dusting Statistics on the use of rock dust in the United States during the years 1930-1933, appearing on page 97 of Volume 139 of the Transactions are extended in Table I herein through the year 1941. The results through 1933 did not appear encouraging, but there has been improve-ment since that date. It has always been true that the larger operations were the ones that used rock dust. In 1941 only 10 per cent of the mines in the country used rock dust, but they produced 57 per cent of the coal, employed just under 50 per cent of the miners, and accounted for 52 per cent of the man-hours. Unfortunately, collection and compilation of these statistics are slow procedures, and figures dealing with the tremendous war expansion of the industry are not likely to be available for a year or more. In 1941 the five leading states in regard to percentage of man-hours worked in mines using rock dust were: Utah, 92.1; Wyoming, 79.3; Alabama, 77.4; New Mexico, 72.5; West Virginia, 65.3. The first four states were the same as in 1933, but West Virginia displaced Washington in fifth place. On the basis of pounds of rock dust used per ton of coal, the five leading states in

Jan 1, 1944

By H. R. Aldrich

This paper is not a treatise on the theory and practice of magnetic surveying. It presents a diagram upon which have been plotted observations taken with the simplest form of magnetic instrument, the lowly dip needle, over a large area astride the Lake Superior syncline of northern wisconsin. The exposures of the underlying formations are not sufficiently great in number nor fortunate in distribution to have provided the fuller understanding of the geology which has been secured by the use of the magnetic observations as an auxiliary tool or accessory in the hands of the geologist. The diagram (Fig. 2) in large part speaks for itself if studied in connection with the geological map (Fig. 1) for which it is the main control. It is presented to demonstrate the extent to which the use of such methods may aid in the solution of geological problems in a covered country. The diagram is probably unique in assembling the expression of such a wide range of formations, affected by so wide a range of secondary processes, and deformed by so many different structures in terms of magnetic variation. Few geologists outside of the Lake Superior country have had any first-hand experience in the taking of magnetic observations and the interpretation of the results in terms of geological conditions; nor have the Lake Superior men gone with the methods far afield from the mere tracing of iron formations. In more recent years the oil companies have gone heavily into investments in magnetometers, balances, and dip needles in the quest of concealed structural anomalies which are the favorable loci of petroleum accumulation. But these geophysicists come back from the fields with their collections of observations facing the question of interpreting the geological meaning of their magnetic anomalies. It is considered probable therefore, and certainly it is the hope of the writer, that the appended charts, or magnographs, which show how character of the country rock and its changes, structural strike and dip and their changes, depth of burial and its variation, contact metamorphic

Jan 1, 1929

By Leonard Larson

BEFORE direct or wet smelting of copper concentrate was adopted at the McGill smelter, in November 1932, actual furnace smelting tests had indicated the possibility of smelting between 400 and 500 dry tons of wet concentrate per furnace day. Under calcine smelting practice, solid charge up to 1165 tons per furnace day had been smelted. It was realized that in order to smelt wet tonnage in equivalent amount per furnace day, a higher combustion rate and higher temperatures would be neces-sary within the furnace. The reverberatory furnace considered in the following history of wet-smelting de-velopments is a unit 127 ft. long and 28 ft. 8 in. wide, inside dimensions (Fig. r). This furnace was in operation through all the years from 1934 to date. During 1933, the first complete year of direct or wet smelting, the plant was on a curtailed copper-production basis and the available concentrate tonnage to be smelted was limited. The average coal-firing rate in the reverberatory for that year was 124 tons per furnace day. This rate was lower than the average for years immediately preced-ing under calcine smelting practice. With this coal-firing rate, an average of 391 tons of new metal-bearing material (N.M.B.M.) was smelted per furnace day. The following year, 1934, the coal-firing rate was in-creased to 139 tons and the smelting rate increased to 448 tons N.M.B.M. per fur-nace day. In succeeding years production required that either more tonnage be smelted in the one furnace or an additional furnace be placed in operation. With this situation confronting the smelting depart-ment, it was determined to continue the program of increasing the coal-firing rate and also to intensify the temperature in the smelting zone of the furnace. In order to accomplish this, various improvements were made to aid combustion within the furnace. The burners were enlarged, in-creased primary air was supplied to the burners, and changes were made in the furnace to enlarge and streamline the out-let, thus increasing the furnace draft.

Jan 1, 1940

By R. W. Lai, I. Iwasaki

Some physical as well as chemical aspects of the methods of dispersion of various corn starches and their derivatives are investigated and their effects as depressants in anionic silica flotation of iron ores ascertained. The adsorption behavior of starches on hematite and quartz is strongly affected by their molecular sizes as inferred from viscosity measurements. The implication of this behavior on flotation and flocculation is discussed. Mechanical treatment of causticized starch solutions is shown to reduce the starch requirements in flotation appreciably. Starches and starch products have been used as depressants for iron oxides both in amine flotation of siliceous gangue and in soap flotation of activated silica from iron ores. Cooke and his associates1,2,3,4 extensively studied the effects of certain starches and their derivatives in the amine flotation of iron ores at near-neutral pH and found that although most starches were good flocculants for hematite and de- pressed that mineral more or less selectively1,3 they did not flocculate quartz suspensions. Further, that replacement of active groups in corn starch modified its behavior as a flocculant for hematite or quartz suspensions1 and as an iron oxide depressant. Schulz and cooke2 showed that many starches and their derivatives, except aminoethyl starch, were abstracted more effectively by Brazilian hematite than by quartz and that the adsorption of a starch product was strongly dependent on pH and on the presence of calcium ion. In soap flotation of calcium-activated quartz, certain starches and their products have been used to depress iron oxides.5'6 The behavior of these substances in flotation appears at times to be at variance with those previously reported and especially with results obtained in the Mines Experiment Station laboratories. This is attributed, at least in part, to differences in flotation procedure and flowsheets and in the method of preparing the depressant. Most of the investigators referred to above, solubilized the starch products by autoclaving at 120°C. Others have used acid,7 alkali8 or oxidizing agents.9 In view of the limited knowledge of the depressing action of starches and their derivatives in iron ore flotation, particularly in soap flotation of calcium-activated silica at high alkalinity, an extensive study

Jan 1, 1965

By S. E. Bretherton

During the year 1878-79, Anton Eilers, who was then interested in the lead smelting and refining business near Salt Lake City, Utah, made a somewhat radical departure from the regular practice at that time, which was to use but little lime in the slag, with a high percentage of iron. Lime was not only a cheaper flux than iron, but it enabled the metallurgist to make a more siliceous slag, an economical advantage in smelting where the smelting companies had to purchase either iron or lime to neutraiize the excess silica, and penalize the ore shippers accordingly. The larger amount of both lime and silica in the slag also made it of lighter specific gravity, and a better separation of the metals and mattes was secured. This change in the formation of slags for lead smelting was brought about by Anton Eilers, prior to the Leadville mining excitement of 1879.. We must also give Mr. Eilers credit for the general introduction of the hollow water-cooled cast-iron jacket for the blast furnace. Again referring to the use of more lime and less iron in the formation of slags, there is no doubt but that it prevents the formation of a great many so-called "sows" in the lead crucible, such as were made in the early history of lead smelting in the Rocky Mountains; these sows consisted of lead, iron, arsenic, sulphur, copper, and other metals, including gold and silver, mixed with unconsumed fuel, and often, after vain attempts to cut them up or melt them to a suitable size for handling, were buried in the slag dumps to get them out of sight. Another advantage derived from the adoption of high-lime slags when smelting ore containing arsenic is the production of less speiss (a byproduct heavier than matte, resulting from careless operation of the furnace, in the lead being driven out of the crucible and sows built up). This speiss, while usually not as rich in precious metals as matte made at the same time, is too valuable to be thrown away; but it is difficult to treat, and it was thrown away or piled on the slag dumps in the pioneer days of lead smelting in this country. About the time of the introduction of the lower iron and higher lime slags in lead smelting, sulphide ores were encountered in Utah and Colo-

Jan 1, 1916

By Klaus Schwerdtfeger, Leo Zwell

The equilibrium between Ir-Fe or Rh-Fe alloys, iron oxide (wüstite or magnetite), and CO2-CO atmospheres has been determined at 1200°C. The data are used to derive the activities in these binary solid solutions. Both systems show negative deviations from Raoult's law. The lattice parameters are given for the investigated Ir-Fe and Rh-Fe alloys. IRIDIUM and iron form a continuous series of fcc solid solutions at elevated temperatures.' Rhodium-rich Rh- Fe alloys have fcc structure.' In the medium concentration range an ordered bcc phase is stable at temperatures up to about 1300°C. Phase relations in iron-rich alloys are not well-known. No thermody-namic data are available for these alloys. EXPERIMENTAL METHOD The experimental method used was to measure the equilibria between a gas phase of known CO2/C0 ratio, the alloy, and iron oxide (wüstite or magnetite). In one series of experiments the alloys of known composition were heated in CO 2-CO gas mixtures. After treatment (usually 1 day) the sample was quenched to room temperature and its surface examined visually to determine whether an oxide tarnish had formed. The procedure was repeated at slightly higher CO 2/CO ratios until the CO 2/CO ratio of incipient oxidation was found. Subsequently, the CO 2/C0 ratio was lowered again in small increments until the tarnish was reduced. In other experiments mixtures of alloy and iron oxide powders were pressed into pellets and equilibrated with the CO2-CO gas phase. In order to ensure that equilibrium was attained, two specimens with different starting iron content were heated side by side; in most cases, equilibrium was approached in one pellet by reduction of iron oxide and in the other pellet by oxidation of metallic iron. The sample was quenched to room temperature, and the composition of the equilibrated alloy was determined by X-ray measurements of lattice parameters and comparison of these values with calibration curves obtained from alloys of known composition. The oxides present in the specimens were identified by comparison of their diffraction patterns with those in the ASTM Card File. It may be expected from the noble character of iridium and rhodium that no appreciable amount of iridium or rhodium is dissolved in wiistite and magnetite under the present experimental conditions. The activity of iron in the alloy is then equal to that established in the iron oxide by the COrCO atmosphere. The activities of iron in wüstite and magnetite, as a function of oxygen pressure, were taken from the work of Darken and Gurry,

Jan 1, 1969

By L. C. Reese

The ultimate resistance against a rigid cylinder which is moved laterally in a cohesionless soil is a function of the geometry of the cylinder and the properties of the soil. An approximate method is developed for computing this resistance and is tested against results of laboratory experiments. Satisfactory agreement between the method and experiment was obtained. Not only was the ultimate resistance against the cylinder measured, but measurements were made of the shape of the rupture surfaces. These measurements should allow the development of a more rigorous computation procedure. INTRODUCTION A critical aspect in the design of offshore drilling platforms is assuring the stability of the platform during a hurricane. The large horizontal loads from waves and wind make a severe loading condition. Piles are generally employed as the foundation since they can be effective in resisting both horizontal and vertical loads. Spuds are sometimes used with a mat foundation, where the spuds are designed principally to resist horizontal loads and the mat designed principally to resist vertical loads. The research reported in this paper is related to one aspect of the problem of laterally loaded piles or spuds in sand. The complete solution to the problem of the laterally loaded pile in sand would require the prediction of soil resistance against the pile as a function of pile deflection; only the ultimate resistance against short piles is considered in this paper. A considerable amount of additional research will be necessary in order to obtain a complete solution to the problem of the laterally loaded pile in sand; however, the work reported here should be useful as a guide in the performance of some of the additional research. ULTIMATE LATERAL RESISTANCE AGAINST A LONG FALL IN SAND To aid in the understanding of the theory which is developed for a cylinder, the theory for earth pressure against a wall is reviewed. In Fig. l(a), a long wall of height H is shown embedded in soil. Soil resistance will develop as the wall is deflected, and the soil resistance will increase with deflection until some limiting value is reached. In this discussion, and those following, it is assumed that all points on the wall deflect equal amounts. A possible shape of the real curve which relates soil resistance to deflection is shown by the dashed line in Fig. l(b); however, as a means of simplifying the discussion, an idealized curve (shown by the unbroken lines) is drawn. If such a wall as this were furnishing the horizontal support for an offshore structure, the dashed curve in Fig. 1 would be the information needed in performing a foundation analysis, with the idealized curve possibly being an acceptable substitute. For the idealized curve, the soil resistance is linear with deflection for the early portion of the curve such that

By C. D. Rugen

Ground raw material as fed to the cement kiln generally is a mixture of two to four components, each of which may have widely varying physical and grinda-bility characteristics. Chemically similar materials found in the same or different deposits may also differ appreciably in physical properties, depending on their crystalline structure. The calcareous or principal cement raw material may vary from a soft chalky limestone or friable cement rock at one plant to a hard limestone or oyster shell at another plant. Argillaceous materials include clays, shales and granulated slag. Siliceous and/or iron-bearing material, including sand, iron ore and cinders, may also be required in addition for certain types of mixes. Frequently differences in grindability characteristics are not given the attention they deserve in comparing grinding results at one plant with those at another or in selecting suitable circuits or equipment. Many types of crushing and grinding units are used, with numerous open and closed circuit arrangements. Both wet and dry processes are used successfully. When rebuilding or installing a new grinding department, the choice of process or circuit in some cases may be dictated by the nature of the materials being ground but in other cases it may be the result of good salesmanship or a compromise. An over-all evaluation of wet process vs. dry process grinding should not be made without considering the effects on all other producing departments in the plant. In general, the more recent grinding installations, both wet and dry, have employed closed circuits, but many older open circuits are still in successful operation. In our experience, closed-circuit raw grinding pays, because of lower power consumption and less operating labor per ton of product. However, some dry open-circuit mills with improved equipment and operating methods compare favorably in performance with dry closed-circuit units. Character of Ground Raw Mix (Kiln Feed) Grinding in the cement plant in general requires a considerably her product than in most ore-grinding operations. A distinction between fineness of kiln feed and of cement may be made in that kiln feed preferably should be ground to a limiting size,whereas finished cement should include a range of size fractions including sufficient fine flours to give a product with satisfactory physical qualities. Grinding raw mix for kiln feed therefore is more comparable to ore grinding, although the limiting size is smaller. Most kiln feeds are ground from 85 to 95 per cent passing 200-mesh, depending on mix composition. Some cement chemists believe that raw materials cannot be too he, since finer particles theoretically combine more readily and intimately in the kiln. However, there are certain definite practical objections to extremely fine kiln feed, such as loss of kiln dust, unstable material flow through the kiln and greater dificulty in control of chemical composition due to dust loss, and the disproportion of fines from the more easily ground component. Our

Jan 1, 1947

By C. D. Rugen

Ground raw material as fed to the cement kiln generally is a mixture of two to four components, each of which may have widely varying physical and grinda-bility characteristics. Chemically similar materials found in the same or different deposits may also differ appreciably in physical properties, depending on their crystalline structure. The calcareous or principal cement raw material may vary from a soft chalky limestone or friable cement rock at one plant to a hard limestone or oyster shell at another plant. Argillaceous materials include clays, shales and granulated slag. Siliceous and/or iron-bearing material, including sand, iron ore and cinders, may also be required in addition for certain types of mixes. Frequently differences in grindability characteristics are not given the attention they deserve in comparing grinding results at one plant with those at another or in selecting suitable circuits or equipment. Many types of crushing and grinding units are used, with numerous open and closed circuit arrangements. Both wet and dry processes are used successfully. When rebuilding or installing a new grinding department, the choice of process or circuit in some cases may be dictated by the nature of the materials being ground but in other cases it may be the result of good salesmanship or a compromise. An over-all evaluation of wet process vs. dry process grinding should not be made without considering the effects on all other producing departments in the plant. In general, the more recent grinding installations, both wet and dry, have employed closed circuits, but many older open circuits are still in successful operation. In our experience, closed-circuit raw grinding pays, because of lower power consumption and less operating labor per ton of product. However, some dry open-circuit mills with improved equipment and operating methods compare favorably in performance with dry closed-circuit units. Character of Ground Raw Mix (Kiln Feed) Grinding in the cement plant in general requires a considerably her product than in most ore-grinding operations. A distinction between fineness of kiln feed and of cement may be made in that kiln feed preferably should be ground to a limiting size,whereas finished cement should include a range of size fractions including sufficient fine flours to give a product with satisfactory physical qualities. Grinding raw mix for kiln feed therefore is more comparable to ore grinding, although the limiting size is smaller. Most kiln feeds are ground from 85 to 95 per cent passing 200-mesh, depending on mix composition. Some cement chemists believe that raw materials cannot be too he, since finer particles theoretically combine more readily and intimately in the kiln. However, there are certain definite practical objections to extremely fine kiln feed, such as loss of kiln dust, unstable material flow through the kiln and greater dificulty in control of chemical composition due to dust loss, and the disproportion of fines from the more easily ground component. Our

Jan 1, 1947

By J. P. Heller

The purpose of this discussion is to comment briefly on one of the points raised in the paper. The topic is that referred to in the Conclusion 2, in which the authors note a "disproportionate increase in mixing rate" as they proceed from a displacement performed at viscosity ratio 0.998 to one at 1.002. The recovery curve of this displacement, Fig.2A, shows a quite noticeable difference between the two runs in which displaced and displacing liquids were interchanged. This difference is ascribed by the authors to the change in viscosity ratio between the two experiments. This interpretation of the experimental results must certainly be based on rather precise measurements of the fluid viscosities or, at least, of the ratio of their viscosities. The ordinary Ostwald viscometer, employed in the usual way, is only just able to distinguish between liquids whose viscosities differ by two or three parts per thousand. The experimental refinements which then must have been necessary to measure with any precision a viscosity ratio of 1.002 would be worthy of mention. Indeed, one would have expected the authors to devote at least a paragraph to the display of this technique. For the same reason - to emphasize that the details of such unusually critical experimental work should be reported and discussed in the literature — I would have liked to see some comment by the authors on the requirements for temperature control during both the viscosity measurements and the displacement experiments. The temperature coefficient of viscosity of Soltrol C at room temperature has been measured in this laboratory at about - 1.9%/1°C. How much did the coefficients for the fluid mixtures used in the experiment differ from this and from each other Even if the two fluids were identical in this respect, it would appear that a temperature difference of .l°C between them in the flow system would produce a viscosity con- trast equal to that imposed by their composition. Reference to the experimental solutions of these problems would render Conclusion 2 more credible. Published theoretical work on the stability problem contains no indication of such extreme sensitivity to the viscosity ratio in the immediate neighborhood of unity. On the contrary, perturbation calculations such as those made by Chuoke1 and Perrine2 lead to initial finger growth rates proportional to the first power of the viscosity difference. The later instability growth calculated by Scheidegger,3 using the assumption of zero pressure gradient perpendicular to the average flow, is also simply proportional to the viscosity difference. The conflict regarding the sensitivity of the dependence of instability growth or mixing rate on the viscosity contrast needs explicit recognition in the literature. In particular, it would seem that the experimental work reported here should be supported by a more detailed description of the viscosity controls. Further discussion of possible alternative interpretations of the data would also be in order. For instance, is it possible that the unconsolidstted bead pack used changed its characteristics between the runs (due, perhaps, to the handling and inverting involved in the injection of the front) Or, are the data points of Fig. 2A averages from several runs performed in a series in which the two liquids alternated as displaced and displacing fluids? To summarize, it seems to me that the relationship asserted by Conclusion 2 in the paper needs the support of more detailed experimental evidence. REFERENCES 1. Chouke, R. L., van Mews, P. and van der Poel, C.: "The Instability of Slow Immiscible Viscous Liquid-Liquid Displacements in Porous Media", Trans., AIME (1959) Vol. 216, 188.

By R. Gibala

Internal-friction measurements on hydrogen-charged iron over the temperature range 4° to 300°K are reported. Two relaxation peaks, the hydrogen Snoek peak at 48 °K and the hydrogen cold-work peak in the range 145" to 2200K, are observed at 80 kc per sec. The effects of hydrogen-charging, aging, and deformation on the internal-friction results are determined and are used to show evidence of partitioning of hydrogen between solid solution and dislocations. The hydrogen-dislocation binding energy is estimated from the behaviors of the relaxation tiwzes and relaxation strengths of the Snoek peak and the cold-work peak. Its value is approxi,mately 6400 cal per mole. MANY investigators have demonstrated the usefulness of internal-friction measurements in determining the manner in which interstitial impurities interact with dislocations in bcc metals. Part of this success has resulted from the existence in bcc interstitial alloys of two anelastic relaxation peaks—the Snoek peak' and the cold-work or Koster peak2 (designated hereafter by SP and CWP, respectively). The SP has its origin in the redistribution of interstitials in solid solution among sites made energetically nonequivalent by an applied stress. The rate at which the redistribution occurs, measured by the relaxation time for the process, is related in a simple way to the diffusion rate of the interstitial in the free solution. The relaxation strength is proportional to the concentration of interstitial in solid solution. The CWP appears to have its origin in the relaxation of an interstitial-dislocation complex for which the relaxation time at a given temperature is much longer than that for the SP. The relaxation strength depends strongly on the concentration of interstitial and the amount of deformation at relatively low concentrations and deformations.2-8 From the dependence of the relaxation strength on interstitial concentration, the SP and CWP may serve as measures of the concentrations of interstitials in free solution and bound at dislocations, respectively. Thus their behaviors have been used to investigate interstitial-dislocation interactions in Fe-C, Fe-N, and several refractory metal systems.'-' However, the Fe-H system has not been studied extensively,? even though disputes in recent years over the mechanism of hydrogen embrittlement in steels involve argument over the extent to which lattice hydrogen and hydrogen-dislocation interactions play an important role.?-'' Previous work on Fe-H indicates the internal-friction behavior to be qualitatively consistent with that for other systems. Apparently, both a SP and a CWP are observed in the temperature ranges 30" to 50°K and 100°to 140°K, respectively (at 1 cps). However, there is neither sufficient nor accurate enough information to identify convincingly these peaks with their supposed counterparts in other systems. Nor have there been any attempts to make quantitative use of these peaks to study hydrogen diffusion, aging, or interaction processes. In this paper, an attempt is made to obtain more complete information on internal friction of hydrogen in iron than presently available. Internal-friction measurements in the range 4° to 300°K on hydrogen-charged iron show that the two peaks discussed above are in fact the hydrogen SP and CWP. Several effects of hydrogen charging, aging, and deformation on these peaks are observed and are used to determine the partitioning of hydrogen between solid solution and dislocation sites in iron. EXPERIMENTAL Materials. The starting material for this investigation was a high-purity iron supplied by National Research Corp. as a 1-in.-diam rod. The following analysis was given (inwt pct): C, 0.004; N, 0.0003; 0, 0.007; P, 0.002; S, 0.005; Si, 0.006; Mn, 0.001; Cu, 0.002; Ni, 0.005; Cr, 0.001; Mo, 0.001. After an initial vacuum anneal (-5 XTorr) at 700°C, the rod was cold-

Jan 1, 1968

By A. W. Schlechten, R. P. Abendroth

Equilibrium H2S/4 ratios were determined as functions of temperatunz and composition in a hydrogen recirculation apparatus. A high-temperature solid solution exists in the range two-phase regionfrom TiS 1.96, to TiS1.30, Various thermodynamic quantities were calculated from the data. COMPOUNDS in the titanium -sulfur system have not receiyed much attention in the past, probably because they do not occur naturally in the earth's crust. However, titanium-sulfur compounds have been used in various metallurgical processes. The U.S. Bureau of klines' studied the formation of ti- tanium-sulfide mattes from charges composed of rutile, pyrite, and carbon, with the resulting sulfide matte being chlorinated to form titanium tetrachlo-ride. Fishel, Roe, and Ellis' investigated the de-sulfurizing action of titanium in steels, and Schwarz and Koster studied the preparation of metallic titanium from the sulfide using aluminum and magnesium reduction. The thermodynamic properties of some of the compounds present in the titanium-sulfur system may prove to be of some use in the consideration of future processes using these sulfides, and would

Jan 1, 1960

By G. R. St. Pierre, R. D. Blackburn

Oxygen contents of' liquid-iron alloys saturated with oxides are analyzed. Minimum points observed in particular Fe-X-O systems can be predicled by a simple extension of first-order interaction methods. If minimum oxygen content occurs at N; where r is the ratio of metal to oxygen in the oxide phase. RECENTLY, wisher' reported on solubility measurements of A1203 in liquid iron at 1580°C which support the earlier work of d'Entremont, Guernsey, and chipman2 and Gokcen and Chipman. Swisher's diagram is reproduced in Fig. l. Minimum points in oxide solubilities have also been found in the Fe-Cr-0 system,4 Fig. 2, and the Fe-Ti-0 system,' Fig. 3. Minima positions can be used to confirm approximately the measured first-order interactions, &, cgr, and E&~, in liquid iron and to deduce compositions of components of constant activity in the oxide phases. Consider the solution of Alz03 in liquid iron: for which an equilibrium constant can be written as: differentiating Eq. [2] with respect to Na~, the atom fraction of &l in the metallic solution, and noting that If the activities of Al and 9 are expanded by a first-order interaction model, then:

Jan 1, 1969

By L. H. de Wald, J. Walter Scott

The removal of lead by fire refining methods from copper of electrolytic quality is growing in importance. Particularly is this true of the refining of secondary copper and copper cathodes obtained from electrolytic cells where lead is used as the anode material, as in the electrolysis of ore-leaching solutions and foul electrolyte. When investigating the removal of small amounts of lead from molten copper in a reverberatory furnace during the refining of secondary copper of otherwise electrolytic copper quality,' it was found necessary first to know something about the distribution of the lead throughout the bath. The authors believe that it is not generally known how small amounts of lead as an impurity are distributed in a molten copper bath; that is, whether the lead is concentrated at the bottom or at the top, or whether it occurs more or less uniformly throughout the bath. The data contained in this report may help, therefore, in the development of a satisfactory fire refining method for the removal of this obstinate element from a molten copper bath. The first step was the development of a method for taking samples from various locations in the bath, at the surface and at various depths. The sampling device used, shown in Fig. 1, consisted of a 10-gram fireclay assay crucible fitted into a ring on the end of a steel rod handle of suitable length. A fireclay scorifier, 2 in. dia., with a ½-in. hole bored in the

Jan 1, 1930

By R. E. Miner, J. K. Jackson, T. L. Wilson

A study has been made of the transformation kintetics and morphology in gas-quenched Fe-5 pct Ni alloys. Massive ferrite or nlurtensite was found to form at temperatures in agreement with earlier results. Surface Preparation appeared to have the greatest effect in determining the type of transformation Product formed. Grain size change, subgrain morphology, and dislocation densities of massive ferrite were essen-tinlly invariant functions of cooling rate. The mar-tens~tic structures were typical of transformation in austenite grains of the order of the sample thickness. BY introducing the idea of a massive transformation in dilute iron-base alloys, Gilbert and Owen in 1962 served to stimulate a closer inspection of phase transformations in ferrous systems.' A wealth of literature has followed concerned with the morphology,2-5 transformation mode,2'3'6-8 and thermodynamics of transformations.2,5,9 interesting controversies have resulted from the experimental observations; closer attention has been paid to the definition of massive transformations and still to be resolved is the Ms temperature of pure iron. The purpose of this note is to report some observations made in a detailed kinetic and metallographic examination of the transformations that occur in gas quenched Fe-5 pct Ni. The results are pertinent to the Ms extrapolations that have been made for pure iron and the observed substructure of massively transformed alloys. PROCEDURE The material used in this investigation was cast as a 5 lb vacuum induction melted, carbon deoxidized heat. The ingot was hot worked to a strip 0.10 in. thick, decarburized, and cold rolled to final thickness. Specimens were punched to sample shape and decarburized in wet hydrogen at 600°C. The chemistry of test specimens is indicated in Table I. Samples 1 by $ in., by thickness were resistance heated and rapidly cooled in an apparatus as illustrated in Fig. 1. Similar helium quenching apparatuses have been described previously;2,6'10 the distinguishing feature of this apparatus is the nozzle geometry. Twin nozzles with three convergent-divergent, sonic ports were mounted perpendicular to the specimen for quenching purposes. The specimen temperature was monitored with an intrinsic 3 mil chromel-alumel thermocouple spot welded to the specimen and con- nected to an oscilloscope. A single switch stopped the current flow through the specimen, opened a gas flow solenoid valve, and initiated an oscilloscope sweep. Cooling rates were read directly from a photograph of the oscilloscope trace and the quenching rates quoted later were made at a point immediately prior to transformation on the trace. All quenching studies were conducted either under a vacuum of 10"-5 torr or a helium atmosphere. The sample geometry was chosen large enough to permit optical and electron microscopy to be performed on samples. The samples were electropolished for both types of examination in a perchloric-acetic solution. Electron microscopy was conducted on a HU 11A microscope operated at 100 kv. Dislocation densities were determined at the same general operating reflection (110) on foils thick enough to produce Kikuchi patterns. RESULTS AND DISCUSSION Transformation Temperature Observations and OD-tical Microscopy. The quenching results of this study are illustrated in Fig. -2(a). Samples which were treated in the as-decarburized condition transformed in a manner similar to that reported previously—a decrease in transformation temperature occurred as the quenching rate increased until a plateau region was reached. Within the scatter of the results obtained here, there was no break in the transformation temperature-quenching rate plot. This suggests no change in transformation mode. Further metallographic examination confirmed this observation. A martensitic transformation was obtained for similarly treated samples except that the surface was first electropolished. The Ms temperature was approximately 85°C below the plateau determined for the unpolished samples and cooling rates as slow as 2000°C per sec were adequate for producing marten-site. The transformation temperatures are in gen- / STRIP SAMPLE / COPPER I SAX/-/}' / CONNECTOR-----A f, SON|C poRTS AC LEADS 3j ]j"I rofe[ \ Mf/yinK/iKj''^ THERMOCOUPLE X-(^—iie"s*c? ' LEADS 1 INCH Fig. 1-—Schematic scction of gas quenching apparatus

Jan 1, 1970

By R. A. Pallanch

SODIUM sulfite as a zinc retarding agent in the selective flotation of complex lead-zinc sulfide ores was discovered by the writer in the summer of 1919 in the testing laboratory of the U. S. Smelting, Refining & Mining Co.'s gravity concentrator at Midvale, Utah. It proved to be the first reagent to give consistently good results in the laboratory on the company's Bingham ore. In December, 1919, C. A. Lemke, concentrator superintendent, recommended that a flotation unit be added to the existing gravity mill to handle the mill slimes, using sodium sulfite as the zinc depressant. Owing to the poor lead and zinc markets and the unfavorable royalty schedules offered by the Minerals Separation Co., the project fell through at this time. In 1921, a number of laboratory tests were made at Midvale on other ores, among them ore from the Sunnyside mine at Eureka, Colo. Both sodium and calcium sulfites were used with success on this ore. Early in 1923, further tests were made at Eureka, shortly after the Sunnyside company had resumed operations after a two-year shutdown. As a consequence sodium sulfite was given a trial in the mill. The results showed sufficient improvement over previous work as to warrant continuous use of this reagent in the lead circuit. Except for a week or so in 1926 and for several weeks in April, 1927, when sodium cyanide and zinc sulfate were given trial runs in this mill, sodium sulfite has been used ever since. Sodium sulfite was chosen rather than the calcium sulfite because of its greater solubility, making it possible to introduce the reagent as a solution. This solution is introduced into the Marcy ball mills along with the original feed of ore. The consumption of sodium sulfite in the Sunnyside mill varies from ¼ to ½ lb. per ton of ore, the smaller amount probably being nearer the average. In February, 1924, laboratory work at Midvale demonstrated conclusively that good results could be obtained on the company's Bingham ore and on most of the custom ores tested by using sodium sulfite as the zinc depressant, xanthate as the lead enhancer in the lead circuit, followed by copper sulfate and additional xanthate to float the zinc. Sodium sulfide was used to float the iron pyrite after the lead and

Jan 1, 1928

By C. R. Johnson, R. A. Greenkorn, G. W. Widner

This paper describes a short, simple well-testing procedure evolved from unsteady-state concepts to appraise wellbore damage in water-input wells. Input rates are changed at specific intervals over a 30-minute period and the wellhead pressure recorded at the end of each interval. From these data, the pressure drop due to the "skin" can be computed. This pressure drop in terms of psi/B/D of input rate is referred to as the "skin factor". Two of these variable-rate tests are required to determine change of wellbore damage and to evaluate well-treatment techniques. There are several advantages to the variable-rate procedure. The necessary data can be obtained with wellhead gauges and meters. There is little interference with normal operations. The short testing period eliminates many interpretative difficulties that come from interference from adjacent wells. The shut-in period required for standard tests before the plot of pressure vs log of time attains a straight line is often 12 hours or more. Such a time period is incronvenient, especially when a well must be tested repeatedly to evaluate change in wellbore characteristics. This variable-rate procedure has been successfully npplied to water-input wells in three fields. For some of the wells, skin factors were calculated from both the standard and the variable-rate tests. These results show good agreement. THEORY OF THE VARIABLE-RATE PROCEDURE In many waterflood input wells, the pressure in the wellbore differs from the pressure in the reservoir immediately adjacent to the well because of the restriction of flow through the skin of the well. If the true pressure of the reservoir at the well, p,, is that pressure which would exist in the well if no skin were present, and p,' is the actual pressure as measured in the well, this difference, is the skin effect. Fig. 1 shows the change in skin effect with change in flow rate. As the flow is reduced, the skin effect is reduced by an amount equal to the change in wellbore pressure minus the change in reservoir pressure. The equation of pressure change without skin using the point-source solution of the diffusivity equation is (after van Everdingen')

By Ionel I. Gardescu

In connection with some of the experiments carried out by the writer on the behavior of gas and oil in a sand reservoir,' an interesting phenomenon was observed which may throw some new light on the problem of recovery of oil from a natural reservoir. The experiments are intended to show the effect of the surface area of the occluded gas masses, originally present in a reservoir, on the further evolution of gas from the oil and its consequent effect upon the rate of production of oil. The apparatus used in the experimental work is shown in Fig. 1. It consists primarily of a sand reservoir R and a displacement chamber D, which is used to induce small variations in volume. The reservoir and displacement chamber form a unit, and a lowering of the plunger D is equivalent to increasing the volume occupied by the oil and gas in the reservoir. The reservoir was first filled with dead oil and maintained under pressure until it was ascertained that most of the free gas had gone into solution. The volume of free gas present in the reservoir was computed from the coefficient of compressibility of the fluids by means of the displacement chamber D, reading to 0.005 c.c. and a special gage J reading to 0.02 lb. per sq. in. The oil was saturated with gas under pressure in reservoir S by circulating the oil for a long period of time through the gear pump B. Subsequently, the saturated oil was circulated through the sand reservoir following the circuit S6, B, S6, R4, the sand reservoir R, R1, R², F4, F1, back to reservoir S. In the following experiments the sand reservoir R was filled with gas-saturated oil at a pressure of 415Ib. per sq. in. with no free gas present. This was ascertained by closing off all the outlet valves and determining the coefficient of compressibility of the system by means of the displacement chamber D. Much difficulty was encountered in eliminating all of the free gas masses from the oil reservoir. The dead oil originally present in the

Jan 1, 1932