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By H. L. Miaw, A. M. Gaudin, D. W. Fuerstenau

A quantitative method for evaluating density of slime coatings has been developed and applied to formation of iron oxide slime coatings on quartz and on corundum. Slime coating density is related to flotation recovery and to properties of the electrical double layer at mineral surfaces. IN spite of considerable study, the nature of slime coatings in flotation is still not completely understood. However, phenomena that control floc-culation and dispersion of colloidal systems are now interpreted in terms of electrical double layers.",' Colloids will flocculate even though the particles carry the same charge, but when two dispersed colloids of opposite charge are mixed. flocculation ensues even more rapidly. Analogous phenomena seem responsible for slime coating on minerals in flotation systems. To shed new light on the issue it was considered desirable to devise a tool that would measure slime coatings. The usual method has been to examine photographs of presumably representative surfaces, after. an intervening washing in running water. But such an examination is non-quantitative, and the changes in chemical environment represented by the washing may have removed the slime coatings that existed during flotation. To provide the possibility for a correlation with electrical double layer phenomena, the experiments were made with quartz, corundum, and iron oxide, for which elec-trokinetic data are available.'-" Since the properties of the electrical double layers of these oxides depend on the pH of the solution, pH will be the most important variable. Furthermore, because the zero point of charge for silica, iron oxide, and alumina occurs at pH 3.7, 8, and 9.5, respectively, the relative charge on the slime and mineral can be changed over wide ranges. Because of its practical importance in quartz flotation, iron oxide powder was chosen as the slime. Also, its uniform composition, contrasting color, and ease of analysis make experimentation simple. In this investigation, correlation was sought between the effect on flotation recovery of slime addition and slime coating density. Materials and Methods Details are available in a thesis by Miaw." The quartz was selected from pure Brazilian crystalline quartz, crushed, sized (65/150 mesh) acid-cleaned, washed, and stored in conductivity water. The corundum (synthetic alumina of high purity prepared by Linde Co., Chicago) was crushed, sized (65/100 mesh) deslimed, boiled in nitric acid, washed, and stored in conductivity water. The iron oxide slime, reagent-grade ferric oxide (—400 mesh) from Allied Chemical & Dye Corp., was heated to 160°C, cooled, and stored in a vacuum desiccator. In the electron microscope the slime particles appeared to be about 0.3µ in size, but their large specific surface (87,900 cm per g, by gas-adsorption method, using krypton) suggests that the actual particles are smaller than 0.3r. Had they been perfect nonporous spheres, they would have had a diameter of 0.13µ.

Jan 1, 1959

By T. E. Leontis

The specific effect of various rare-earth metals on the room- and elevated-temperature properties of magnesium has been evaluated. Alloys containing didymium exhibit the highest tensile and compressive strengths at room and elevated temperatures. All the rare-earth metals increase the creep resistance of extruded magnesium at temperatures in the range of 400° to 600°F, but the degree of enhancement depends on the temperature and on the concentration of the added metal. THE effects of rare-earth metals on the properties of sand-cast magnesium were discussed in some detail in earlier paper by the author.' The present paper deals with the effect of the same alloying elements on the properties of extruded magnesium. This investigation also had as its aim the development of a wrought alloy having a better combination of room-temperature strength and ductility and elevated-temperature strength and creep resistance than is found in magnesium-Mischmetal-manganese alloys, which have been reported earlier.2-5 The only known attempt to study wrought magnesium alloys containing pure cerium instead of Mischmetal was made by Mellor and Ridley.6 They found that in the form of rolled bars there is a definite, optimum cerium content for creep resistance at 200 °C and that the creep resistance of these alloys at 200 °C is significantly Improved by heat treatment at 550" to 580"C. In the present investigation the compositional variation in mechanical properties of the following alloy systems is presented: I—magnesium-Misch-metal. 2—magnesium-cerium-free Mischmetal. 3— magnesium-didymium. 4—magnesium-cerium. 5— magnesium-lanthanum. Alloys containing predominately praseodymium are not included in this series because of the lack of this material. Experimental Procedures The alloying ingredients used in preparing the alloys described herein are the same as those reported in the earlier paper.' Cerium-free Mischmetal is the rare-earth mixture remaining when the cerium is removed from Mischmetal, which contains all the rare-earth metals as they occur naturally in mon-azite sand, the ore from which Mischmetal is produced. Removal of both cerium and lanthanum from Mischmetal leaves what is commonly called "didym-ium," consisting predominantly of neodymium and praseodymium. Although the composition of the particular batch of each metal used may differ somewhat from the analysis presented previously, these differences are not great enough to warrant repeat- ing the specific composition of each material. The electrolytic magnesium used as the starting material in these alloys has the same typical analysis as that given in the earlier paper.' The alloys were prepared in small laboratory melts applying all the necessary precautions for alloying rare-earth metals with magnesium described by Marande.' Most melts were large enough to cast one 3 in. diam billet 10 in. long. In a few cases, particularly the didymium-containing alloys, the lack of sufficient amounts of the rare-earth metal limited the size of the billet to 6 to 8 in. All billets were scalped to a diameter of 2 15/16 in. and faced to a length of 9 ¼ in. as limited by the size of the extrusion container. The alloys were extruded into ½ in. diam rod on a 500-ton direct-extrusion press using a 3 in. container. The details of the extrusion step are: billet preheat, 925°F (2 hr); container temperature, 900°F; die temperature, 900°F; extrusion speed, 10 ft per min; reduction ratio, 36:1; and percent reduction, 97.3. The lower melting point of alloys containing didymium' necessitated reduction of the extrusion speed to 5 ft per min in order to prevent hot shorting during extrusion. Adequate lengths were cropped from both ends of each extruded rod to assure that all the material used for tests was extruded under uniform conditions. Tensile and compressive properties at room temperature are reported in the several conditions of heat treatment. The ASTM designations are used to distinguish these conditions as follows: T5—Direct age at 400°F (16 hr) T4—Heat treat at 950°F (4 hr) for alloys containing didymium T4—Heat treat at 1050°F (4 hr) for all other alloys T6—T4 + age at 400 °F (16 hr) The lower heat-treating temperature for alloys containing didymium is necessitated by the lower melting point of these alloys. All heat treatments were conducted in electrically heated, circulating-air furnaces. A protective atmosphere containing 0.5 to 1.0 pct sulphur dioxide was used for the high temperature heat treatments. Tension and creep specimens 6 Yz in. long and compression specimens 1½ in. long were cut from the extruded rod. A reduced section of ? in. diam was machined on the tension specimens, whereas on the creep specimens a reduced section of 0.450 in. diam

Jan 1, 1952

By L. S. McNickle

Commonly accepted maintenance methods are being outdated by the rapid acceptance and use of more complicated hydraulic circuitry on modern mining equipment. It is no longer adequate to use the maintenance program to merely repair or sustain equipment operation. Ever increasing operating costs place a huge premium on lost production time. It has, therefore, placed the maintenance programs in the position of being required to alleviate equipment malfunctions on production shifts and still attain the maximum unit life from each component part. Ireland mine of Hanna Coal Co., which operates two production shifts and one maintenance shift per day, performs hydraulic maintenance with a plan that is geared to assure the bulk of work being handled on the midnight or maintenance shift. Production is thus allowed to continue without interruption from major hydraulic component malfunction. The plan is called selective maintenance because the specific part to be worked on and the time the work is to be accomplished are selected according to a definite plan.

Jan 10, 1961

By S. E. Haszko

Fused alumina or silica crucibles were used as the containing vessel. X-ray powder photographs were taken with CrKa radiation and the use of Straumanis type Norelco cameras of 114.6 mm diam. Crystallographic data for these compounds are shown in Table I. These results are in agreement with others of this series reported previousiy by Wernick and Geller.l The abnormally large atomic volume of Eu and Yb metal3 is manifested in EuA12 and YbAl2, when one compares them with the compounds reported in Ref. 1. However, the behavior of Yb in the Ni compound is the same as that observed in Ni5Yb having the Cu5Ca structure.4 Thus, it appears that Yb has a valence closer to 3 only in the Ni compounds; i.e.. the 2s and Id electrons are lost to the conduction band. 1,4 Europium in EuAl2, appears to have a valence closer to 2. In previous work.' X-ray patterns of ingots of NdCo2 indicated a multiphase material with faint indication of the presence of a phase having the MgCu2 structure. It was thought that NdCo2 formed peri-tectically from the melt, resulting in a multiphase system when cooled under nonequilibrium conditions. An X-ray pattern of a sample from a melt cooled more slowly than in past work showed that the major phase was NdCo2. The lattice constant, Table 1, is in excellent agreement with the value one can predict from the data of Ref 1. One of the other phases was identified as Co,Nd. The author wishes to thank J. H. Wernick for his guidance in this work, and D. Dorsi for the preparation of these compounds. 'J. H. Wernick and S. Geller: AIME Trans., in press. 'J. H. Wernick and S. E. Haszko: to be published. 'F. H. Spedding and A. II. Daane: Progress in Nuclear Energy, Series 5, Eds.: H. M. Finniston and J. P. Howe, McGraw-Hill Book Co., 1956. 'S. E. Haszko: to be published. 'J. H. Wernick and S. Geller: unpublished work. 6J. 11. Wernick and S. Geller: Acla Cryst., 1959, vol. 12, p. '162. The Influence of Hydrogen on the Lattice Parameters of Ti-Sn Alloys A. Coucoulas and H. Margolin A reinvestigation of the lattice parameters of Ti-Sn alloys by the present authors has revealed consistently higher c and a values than those obtained by Worrier. The difference is most pronounced in the c-parameters which are, therefore, used as a basis of comparison. This discrepancy was not due to air contamination, since precautions were taken to exclude this possibility. Specimens for Debye-Scherrer photograms were prepared by arc-melting 15-g buttons of Bureau of Mines titanium and 99.99 pct Sn, with compositions of 6, 8, 10, and 12 at. pct Sn. These buttons were forged under an oxygen-acetylene torch to 1/8-in. sq rods to produce relatively fine grained material. Scale and some surface were ground off, and the rods, after wrapping in molybdenum and titanium sheet, were vacuum annealed 15 min at 800 °C to remove hydrogen. Heat treatment of one of the samples at 875°C to produce ß and reveal a at the surface showed no surface contamination. Following the vacuum treatment, the specimens were wrapped in molybdenum and annealed for 1week at 800°C under two atmospheres of argon. After water-quenching, the rods were ground so that the thickness tapered to 0.1 mm at the tips. The ground specimens were then recapsuled as previously and reannealed 1 hr at 800°C to remove cold work. The

Jan 1, 1961

By H. Margolin, A. Coucoulas

Fused alumina or silica crucibles were used as the containing vessel. X-ray powder photographs were taken with CrKcll radiation and the use of Straumanis type Norelco cameras of 114.6 mm diam. Crystallographic data for these compounds are shown in Table I. These results are in agreement with others of this series reported previousiy by Wernick and Geller.l The abnormally large atomic volume of Eu and Yb metal3 is manifested in EuAl2, and YbAl2, when one compares them with the compounds reported in Ref. 1. However, the behavior of Yb in the Ni compound is the same as that observed in Ni5Yb having the Cu5Ca structure.4 Thus, it appears that Yb has a valence closer to 3 only in the Ni compounds; i.e.. the 2s and Id electrons are lost to the conduction band.1,4 Europium in EuAl2 appears to have a valence closer to 2. In previous work.' X-ray patterns of ingots of NdCo2 indicated a multiphase material with faint indication of the presence of a phase having the MgCu2 structure. It was thought that NdCo2 formed peri-tectically from the melt, resulting in a multiphase system when cooled under nonequilibrium conditions. An X-ray pattern of a sample from a melt cooled more slowly than in past work showed that the major phase was NdCo2. The lattice constant, Table 1, is in excellent agreement with the value one can predict from the data of Ref. 1. One of the other phases was identified as Co5Nd. The author wishes to thank J. H. Wernick for his guidance in this work, and D. Dorsi for the preparation of these compounds. 'J. H. Wernick and S. Geller: AIME Trans., in press. 'J. H. Wernick and S. E. Haszko: to be published. 'F. H. Spedding and A. II. Daane: Progress in Nuclear Energy, Series 5, Eds.: H. M. Finniston and J. P. Howe, McGraw-Hill Book Co., 1956. 'S. E. Haszko: to be published. 'J. H. Wernick and S. Geller: unpublished work. 6J. 11. Wernick and S. Geller: Acia Cryst., 1959, vol. 12, p. '162. A reinvestigation of the lattice parameters of Ti-Sn alloys by the present authors has revealed consistently hiher c and a values than those obtained by Worrier. The difference is most pronounced in the c-parameters which are, therefore, used as a basis of comparison. This discrepancy was not due to air contamination, since precautions were taken to exclude this possibility. Specimens for Debye-Scherrer photograms were prepared by arc-melting 15-g buttons of Bureau of Mines titanium and 99.99 pct Sn, with compositions of 6, 8, 10, and 12 at. pct Sn. These buttons were forged under an oxygen-acetylene torch to 1/8-in. sq rods to produce relatively fine grained material. Scale and some surface were ground off, and the rods, after wrapping in molybdenum and titanium sheet, were vacuum annealed 15 min at 800 °C to remove hydrogen. Heat treatment of one of the samples at 875°C to produce ß and reveal a at the surface showed no surface contamination. Following the vacuum treatment, the specimens were wrapped in molybdenum and annealed for 1 week at 800°C under two atmospheres of argon. After water-quenching, the rods were ground so that the thickness tapered to 0.1 mm at the tips. The ground specimens were then recapsuled as previously and reannealed 1 hr at 800°C to remove cold work. The

Jan 1, 1961

By S. K. Mitra

A refinement of the Seeger model for intersection process is investigated which is in better agreement with experimental observations than the original. It is shown that, in single crystals, the strain hardening in Stage II is mainly due to the short-mnge interactions when intersection is the rate-controlling process. It is also demonstrated that the creep curves, as predicted by this theory, are in good agreement with the experimental observations. MOTT: Cottrell? and Seeger have developed an approximate theory for plastic deformation of single crystals over the range of variables where the strain rate is controlled by the rate of intersection of dislocations. Although it is now generally agreed that the low temperature deformation of many pure metals is controlled by the intersection mechanism, various dictates of the over-simplified Seeger model are not in good agreement with all the experimental facts. It is the purpose of this paper to reveal that by appropriate extensions of the Seeger model, particularly those suggested by Basinski: a much more reliable theory results. The refined model to be presented here will be shown to account, in a satisfactory way, for the effect of stress, temperature, and strain on the creep rate under constant stress and for the effect of temperature and strain on the flow stress in constant strain-rate tests. EXPERIMENTAL METHOD To Check the theoretical deductions, both creep and tension tests were conducted on single crystals of high-purity Al (99.994 pct Al) so oriented that both the active slip plane and the Burger's vector of the operative dislocations on that plane made angles of about 45 deg to the tension axis. Single crystals of aluminum (5/8 in. by 1/10 in. by 8 in.) were grown in a graphite mold under an inert atmosphere using the Bridgman method. The chemical composition of the aluminum is given in Table I. A common seed was used for all crystals and their orientation is shown in Fig 3. The extensometry consisted of two differential transformers with matched outputs mounted so as to measure the extension in a 2 in. gage length. The amplified difference in output of the two transformers was recorded by a potentiometer. The amplification was calibrated before each run so that one chart division of the recording potentiometer indicated a 105 shear strain on the specimen. Stresses were measured to the nearest 1 x l04 dynes per sq cm. ACTIVATION VOLUME The concept of Basinski that the activation volume is not constant but is a function of the force that aids thermal fluctuation in effecting the cutting of dislocations will be adopted in this section. The force acting due to an applied shear stress on the dislocation being intersected is where L is the mean spacing between the forest dislocations, is the Burger's vector and T is the back stress. A detailed discussion about the origin of back stress will be taken up later in this report. As shown by Basinski, the activation energy, U, that must be supplied by a thermal fluctuation in order to effect intersection, is equal to where x is the distance through which the dislocation must be translated for complete intersection, and Fm is the maximum force encountered in intersection. When the applied stress is decreased abrupt ly F also decreases and the activation energy increases correspondingly as documented in Eqs. [ 1 ] and [2]. The Seeger equation for the strain rate when the deformation is controlled by rate of intersection of where the shear strain rate (per sec) N = the number of points per unit vol at which intersection can take place

Jan 1, 1962

By N. H. Mannakee

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

Nov 1, 1909

By Phillip E. Deering, Robert M. Cox

A model pillar study was conducted in which the engineering principles of dimensional analysis were applied to the problem of coal mine pillar design. The paper reviews the theory of similitude as applied to the model pillar study conducted in the investigation. An example solution of a design problem is included to indicate how the results of the study may be used as a first approximation in the design of coal mine pillars. The design of mine pillars for adequate support with minimum loss of valuable raw materials has always presented a problem to the mining engineer. Most often, for lack of a better method, past practice has influenced the design of new mine pillars. This process has always left doubt as to the safety factor of the pillars. The work presented in this paper is an initial attempt toward adapting the engineering principles of dimensional analysis to the problem of pillar design in underground mines. The use of the dimensional analysis technique is advantageous because all the variables associated with the problem are considered, and by systematic analysis the relative influence of each variable is determined. The model material utilized in this study was taken from the Helena seam of the Cahaba coal field located in central Alabama. The research study was sponsored by The Southern Electric Generating Co. as part of an over-all rock mechanics investigation of the Helena seam area. THEORY OF SIMILITUDE Model analysis is used extensively in engineering today, particularly in the solution of design problems that defy the classical methods of analysis. Such problems arise when materials with a nonlinear stress-strain relationship are involved, when geo- metric boundaries are difficult to define in simple form, when strains become large, or when partial failure occurs. All of these difficulties usually exist in pillar design problems. Those principles which underlie proper design and construction of models, and the interpretation of test results, comprise the theory of similitude. That is, the theory of similitude includes a consideration of the conditions under which the behavior of two separate entities or systems will be similar, and the techniques of accurately predicting behavior of one from observation of the other. The theory of similitude may be developed by dimensional analysis. Dimensional analysis, as a powerful analytical tool, is developed from a consideration of the dimensions in which each of the important quantities involved in a phenomenon is expressed. It is based on two axioms: 1) Absolute numerical equality of quantities may exist only when the quantities are similar qualitatively. 2) The ratio of the magnitudes of two like quantities are dependent on the units used in their measurement, provided that the same units are used for evaluating each. Dimensional analysis, developed from these two axioms, differs from other types of analysis in that it is based solely on the relationships that must exist among the pertinent variables because of their dimensions, rather than on the relationship of natural laws. In itself, dimensional analysis ~rovides qualitative, rather than quantitative relationships, but when it is combined with experimental procedures, it may be made to supply quantitative results and accurate prediction equations. APPLICATION OF THEORY The design of an adequate mine pillar requires the determination of a design equation and the selection of a dimensional system with which to work. Since force plays an important part in the design of mine support, the FLT (force, length, time) system has been used. The factors involved in the dimensional analysis of mine pillars and their dimensions are: A = cross-sectional area L Cp = design strength FL- E, = tangent modulus of elasticity FL

Jan 1, 1969

By Wolfgang Pietsch

Direct Reduced Iron is a product obtained during solid state reduction of iron oxides into metallic iron. General chemical and physical characteristics of all direct reduced iron materials result in a noticeable reoxidation tendency and a relatively low ignition temperature. As most of the chemical reactions are exothermic, normally heating occurs and if water is present hydrogen evolves. Dry direct reduced iron deactivates quickly in air but is still reactive if it comes into contact with moisture. Because of these characteristics, special requirements are necessary for safe storage, shipment, and handling. In an effort to improve this situation passivation techniques were and still are being developed. The paper discusses the properties of direct reduced iron, presents past experience with storage, shipment, and handling of MIDREX® Iron, a direct reduced iron material produced in the MIDREX® Direct Reduction Process, and evaluates benefits derived from different passivation techniques.

Jan 1, 1978

By M. E. Glicksman, G. S. Ansel

It has been shown by Walton and Chalmers,&apos; that the mechanism of the development of solidification textures in castings involves the preferential growth of dendrites along certain crystallographic directions as determined by the influence of prevailing heat-transfer conditions. Specifically, this growth is parallel to the direction of heat flow. The purpose of the present investigation was to determine the applicability of this mechanism to: 1) commercially pure aluminum (99.75 pct) solidified to coarse columnar crystals, 2) an aluminum-silicon casting alloy (5.25 Si, 0.38 Fe, 0.02 Cu, 0.10 Ti, 0.002 S) cast to a fine-grained structure under complex and reproducible heat transfer conditions. PROCEDURE AND RESULTS 1) Specimen Preparation—Using a technique similar to that employed by Northcott and Thomas,2 samples were melted in the directional solidification mold, Fig. 1, by heating the entire assembly to 670° C. The mold was then end cooled using a water jet. From considerations of harmonic analysis, the likely distribution of isotherm normals encountered by the growing crystals is shown in Fig. 1. 2) Orientation Analysis—The pure aluminum sample froze to large columnar crystals, nucleated close to the metal diaphragm, with the growth direction parallel to the mold axis. Using the back-reflection Laue technique, the growth direction of these crystals was determined to be a <100>, which coincided within 53 deg to the mold axis. Metallographic examination of the relatively fine-grained aluminum-silicon sample revealed a dendritic mode of growth having its primary dendrite arms along isotherm normals. Back-reflection Debye-Scherrer patterns, taken with the specimen rotating about its cylinder axis, yielded rings displaying symmetrical arcing, thus proving that the sample did, indeed, possess the solidification texture inferred from the preliminary metallographic examination. To determine the extent and orientation of the texture in the aluminum-silicon alloy, a density distribution of the (111) poles of the sample was plotted using the transmission Debge-Scherrer

Jan 1, 1960

Jan 1, 1901

By Irving Cadoff, Kurt Komarek, Edward Miller

Barium can be purified by equilibration with titanium. The melting point of barium was found to be 726.2° i 0.5 °C. The room-temperature lattice parameters of BaTe and Bask are 7.004 * 0.002A and 6.600 * 0.002A. Melting points for BaTe and Base were found to be 1510° * 30°C and 1830° ± 50°C, respectively. HIGH-purity barium and its compounds are difficult to prepare because of the reactivity of barium with the atmosphere and the large heats of formation of the compounds. Purification of barium by vacuum distillation,&apos; and the preparation and properties of barium oxide2 and barium sulfide3 have been reported. However, little has been done on the homologous compounds barium selenide and telluride. PURIFICATION OF BARIUM Distilled barium obtained from King Laboratories was used as the starting material. The analysis supplied with the metal showed the presence of: 0.4 wt pct Sr, 0.001 pct Mg, 0.02 pct F, 0.003 pct Cu, 0.005 pct Na and less than 5 x 10-3 wt pct of any other metallic impurity. Analyses for oxygen and nitrogen were not available. Since there is evidence4 that any barium nitride present in the starting material may decompose on distillation producing nitrogen which can contaminate the distillate, further purification was performed. At elevated temperatures, any nitrogen and oxygen present in barium should be removed by reaction with titanium. Assuming that the solubility of oxygen in liquid barium is negligible near the melting point of barium, any oxygen present will be in the form of BaO. Removal of oxygen from molten barium is expressed by the equation: BaO(S)+ TixOy(S) = Ba(l)+ TixO(y+1)(s) where Ti,Oy and TixO(y+1) are solid solutions of oxygen in titanium. At 1000°C, the change in free energy for this reaction is negative for (y+1)/x +y+1) x (100) 17.5 at. pct O.5 Since reaction with commercially pure titanium (containing 0.07 wt pct oxygen) results in a free energy change for the reaction of -19 kcal per g-atom, slight solubility of oxygen in barium would not hinder the oxygen removal. Since comparable thermodynamic data are not available to permit calculation of the partition of nitrogen between liquid barium and titanium, a similar quantitative relationship cannot be obtained. However, on the basis of work by Kubaschewski and Dench,5 complete removal of nitrogen from liquid barium can be expected. Since the melting point of barium is depressed markedly by small additions of nitrogen,&apos; the change in melting point during reaction of barium with titanium was used to follow the purification reaction. MELTING POINT OF BARIUM A 50-g sample of barium was sealed by arc welding under argon into an all titanium crucible provided with a thermocouple well. The melting point of the sample was determined by thermal analysis, using a Pt/Pt-10 pct Rh thermocouple which was calibrated according to National Bureau of Standards specification6. The crucible was then heated for 48 hr at 950°C in vacuum and the melting point redetermined. This procedure was repeated until three successive thermal analyses agreed within ±0.5oC, the limits of error of the analysis. The melting point increased from an initial value of 720.0°C to a final value of 726.2°C. Analysis on samples quenched from 950°C gave a solubility value of 0.004 wt. pct Ti. Assuming that the titanium-barium phase diagram is similar to those of titanium-magnesium7 and titanium-calcium,8 the solubility of titanium in liquid barium decreases with decreasing temperature. Therefore, the solubility of titanium in liquid barium should be less than 0.004 wt. pctat the melting point (726oC), and the effect of dissolved titanium on the melting point would be negligible. Addition of up to 3 wt pct Sr does not significantly change the melting point of barium,7 so that the effect of the 0.4 wt pct Sr in the starting material will also be negligible. The value of 726.2" ± 0.5C obtained for the melting point of barium can be compared .with a determination carried out by Keller and coworkers in low-carbon steel crucibles,&apos; who obtained a value of 725± 1C, using barium purified by fractional distillation. The higher value obtained in the present investigation is indicative of the effectiveness of titanium in removing traces of nitrogen. PREPARATION OF BaTe AND Base The compounds were prepared by direct reaction

Jan 1, 1961

By Edward Martinez

The reactions occurring in the copper segregation process were studied by heating mixtures of chryso-colla, salt, and a reducing agent. The techniques used in this investigation were differential thermal analysis (DTA) and thermal gravimetric analysis (TGA). The initial chloridizing of the oxide copper occurs below 500°C and cupric chloride may be the compound formed. Volatilization and reduction of the copper chloride take place above 550°C, although these reactions do occur to some extent below 550°C. A difference in the distribution of the metallic copper in the reducing agent was found when sodium chloride was used compared to magnesium or calcium chloride. Segregation was obtained with mixtures of cupric oxide, salt, and charcoal with no quartz or silicate present. Preliminary tests indicate that segregation may occur even in the absence of water vapor. The DTA and TGA techniques were found to be of great value in studying these reactions. The copper segregation process is a method for treating oxide copper ores. The ore is heated, most commonly in a kiln, with a reducing agent and a halide salt, generally sodium chloride, to approximately 700°-750°C and held for 30 to 60 min. The addition of the salt results in the migration and reduction of the oxide copper to metallic copper on the surface of the reducing agent rather than in the original mineral structure. The metallic copper can then be recovered by a subsequent leaching or flotation step.1-4 Experimental work in 1923 on oxide copper ores from the Sagasca mines in Chile led to the discovery of the reduction process. It was found that during the reduction of the copper mineral with coal, at about 700°C, the copper migrated to the surface of the coal instead of remaining disseminated in the ore. The unusual behavior of the copper, which caused it to migrate from the ore particles to the coal, was traced to the presence of a small quantity of sodium chloride occurring in the ore. Further experiments with oxide copper ores proved that the presence of a halide, either occurring naturally or admixed with the ore, caused the copper to migrate from the ore particles and to segregate in the charge. The ratio of salt to reducing agent may vary somewhat, but in general 0.5% to 1.5% sodium chloride and 0.5% to 1.0% coal or coke have been mixed with the ore. Less than stoichiometric amounts of salt are required to convert all the oxide copper to a chloride, so that a cycle of reactions appears to be occurring. Several investigations reported in the literature have proposed reactions to explain the mechanism of the process.5-10 There appears to be general agreement that water is necessary for the reactions to occur; that once the sodium chloride reacts with silica or silicates in the ore, the hydrochloric acid formed will convert the cupric oxide in the mineral structure to cuprous chloride. However, there appears to be a conflict of opinion on the reactions involved in the reduction of the cuprous chloride to metallic copper on the surface of the carbon. Rey has indicated that salt, water vapor, and

Jan 1, 1968

By A. E. Nash

This title is somewhat of a misnomer, because it does not accurately describe the phase of heat generation and application coming within the scope of this discussion. This paper is concerned primarily with that particular phase of radiant-heat transfer sometimes erroneously referred to as "shielded" radiant heat, to differentiate it from the open radiant heat of either flame or settings, in which the actual source of the radiant heat is a small incandescent furnace composed of a highly conductive superrefractory, within whose walls the combustion of the fuel is completed. This small furnace is usually located directly in the furnace proper, and although its refractory walls do shield the heat-absorbing surfaces from contact with the gases of combustion, there is no interference with the radiant heat given off by the furnace itself. We do not believe it either necessary or advisable to shield or screen radiant heat when properly controlled and applied. We do believe it essential to prevent the excessively hot gases of combustion from coming in contact with those parts of the heat-absorbing structure that are already receiving heat at high rates by radiation. In connection with any process for the refining of oil with which we are familiar, we are convinced that it is most advantageous to transfer the maximum of the heat generated in the form of radiant heat, applied directly to the heat-absorbing surfaces without the interposition of any form of shield or screen to prevent or reduce the radiant-heat transfer. While the term radiant heat is broadly used to cover all heat energy transferred from one body to another by radiation, in contradistinction to heat given up by gases in direct contact with the heat-absorbing structure (convection) or transmitted simply by conduction, in furnace work it is perhaps more often limited to the heat rays given off either by

Jan 1, 1928

By Joseph Chalmers, J. S. Desmond, R. Van A. Mills

[Because of the limited space in this volume and the fact that a description covering the oil recovery buildings and equipment (see page 4, Technical Publication No. 144) will be given in a forthcomnig U. S. Bureau of Mines publication, and because the paper was published in detail as Technical Publication No. 144, and is available as a separate at the Institute, it is impossible to include here more than the following brief extract.] Problems Being Studied The selection of the first problems to be studied was based largely upon the following very practical questions asked by several of the largest operators in the Mid-Continent field. 1. What are the causes for the formation of excessive amounts of bad thick oil on properties that are being repressured with compressed air and how can this trouble be prevented? 2. Why, in some areas, does the oxygen in the air injected into an oil sand during repressuring operations apparently change to carbon dioxide? Is carbon dioxide formed by the oxidation of some of the oil in the sand&apos;? How can the formation of inert or low B.t.u. casinghead gas, loaded with nitrogen, carbon dioxide and oxygen, be prevented? 3. What percentage of the oil originally present in an oil sand can be recovered by the ordinary methods of operation when the gas originally dissolved in the oil is the main propulsive agent? 4. What percentage of the amount of oil produced by ordinary methods can be recovered under average conditions by repressuring a so-called depleted oil sand? 5. What are the relative propulsive efficiencies of compressed air and natural gas in repressuring operations? 6. What are the practical advantages of pressure maintenance and early repressuring as compared with late repressuring?

Jan 1, 1929

By A. B. Hildebrandt

P. B. Baxendell is to be complimented for an exccllent piece of work. To our knowledge there has been no previous publication of field data on the flow of oil and gas through the annulus of a well. It is certainly gratifying to see this work on annular flow confirm the previous published correlation procedure on tubing flow. It extends considerably the range under which reliable gas-lift calculations can be made. Baxendell discussed this work with us about a year ago and was kind enough to send a large scale plot of his correlation. We had been designing gas-lift installations on flow through the annulus, assuming that the original correlation of the f factor based on tubing flow&apos; was valid as long as we stayed within the same mass velocity range on which the correlation was based. Doing this work necessitated the use of an equivalent diameter for the annular flow. The equivalent diameter is defined as area&apos; of stream cross section wetted perimeter and for the case of an annulus is D, — D,. Substituting this in the basic equation correlating energy loss along with the area to flow required to convert the velocity, to volumetric flow rate, D (Baxendell&apos;s Eq. 7) becomes dell&apos;s expression, D,). Similarly, the D in 1.4737 X 10 (M&/D) becomes (D, + D;) for annular flow. On receipt of Baxendell&apos;s data, we. of course, recalculated it to put it into the form we were using, and to see how well it agreed with the correlation based on tubing flow. Fig. 1 shows the results, which were certainly gratifying. For low values of (D, - D,) pv, the data coincide with the data on flow through tubing, whereas at high values the data on flow through the annuli appear to be leveling off to a constant value. For very high rates of flow where the turbulence is very high, one might expect the value f to level out and become constant. A bulletin published in 1914 by the U. of Wisconsin presented results of a large number of laboratory teats in air lifting water through short lengths of 1.25-in. tubing. It was possible to correlate a random sampling of

By Carl F. Cline, Richard R. Vandervoort, Willis L. Barmore

THE objective of this investigation was to determine the high-temperature plastic deformation behavior of stoichiometric uranium mononitride as a function of stress and temperature. Interest in the properties of this material stems from its potential use in high-temperature nuclear reactor systems. The creep of other refractory compounds containing uranium (e.g., U02, UC) has been studied by various investigators.1"4 Fassler et al.4 have studied the creep of UN in vacuum from 1100° to 1350°C at stresses of 6000 and 8000 psi. In the present work, the creep of stoichiometric UN was investigated from 1500° to 1800°C at stresses from 2000 to 5000 psi in a partial pressure of 200 mm of nitrogen. The specimens were prepared by hot isostatic pressing of UN powder into cylinders of $ in. diam by about 1 in. high. After pressing, the specimens were heat-treated in nitrogen at 1900°C for 50 hr. The densities of individual specimens were determined by the water displacement method. All specimens were theoretically dense, based on a value of 14.32 g per cu cm.5 Principal metallic impurities in ppm by weight were: Ca, 50; Cu, 5; Fe, 30; Mg, 5; Ni, 10; and Si, 20. Oxygen content was 400 ± 50 pprn and carbon content was 100 i25 ppm. The nitrogen content was 5.56 ±0.05 wt pct. The average grain size for five specimens, as determined by the intercept method, was 0.14 i 0.01 mm. One specimen had a grain size of 2.0 mm. This large grain size is an anomaly, since all specimens had the same chemical and thermal histories. Specimens of 1/4 in. diam by 1/2 in. high were creep-tested in compression in a clam shell furnace heated by W-25 pct Re sheet elements. Temperature was measured to ilODC by an optical pyrometer which had been calibrated by a standard source. The distance between fiducial marks on the specimen was measured before placement into the furnace. The furnace chamber was evacuated to 10-5 Torr and back-filled to 200 mm N2. After heating rapidly to temperature, the load was applied and controlled to ±2 pct by an Instron testing machine. Upon initial loading, the specimen was deformed until a constant crosshead rate was obtained, then quenched to room temperature, remeasured, and replaced in the furnace. Upon subsequent reloading at temperature, the crosshead rate was constant for the selected condition indicating steady-state creep.

Jan 1, 1969

By E. S. Rowland, J. Welchner, R. H Marshall

This paper presents results on an extension into the realm of high-carbon steels of some work recently published1 on the effects of time at temperature, quenching temperature and prior structure on the hardenability of one 0.20 and four 0.40 per cent carbon alloy steels. It was shown at that time that unless the conditions of time, temperature and prior structure are substantially the same in performing the hardenability test as in conducting hardening of parts in production, the correlation of hardenability information with the hardness and properties of production parts is often not of satisfactory accuracy. The general effects of these variables on the austenitic grain size, distribution of excess carbides and critical cooling rate have been known for many years and one or more have been investigated by Shepherd,2,3 Davenport and Bain,4 Digges,5,6 Digges and Jordan,&apos; Post and associates8 and Roberts and Mehl,9 to mention only a few. There has been no systematic investigation, however, into the quantitative variations produced on the hardenability of commercial high-carbon steels by changes in these factors of time, temperature and prior structure. Procedure A plain carbon hypereutectoid steel, S.A.E. 52100 and Graph-Mo, a molybdenum-bearing high-carbon steel containing some graphite, were chosen for this investigation. The chemical analyses of these electric-furnace steels are given in Table I. The procedure used was exactly that reported previously,&apos; hence the details will not be repeated here. Normalized (165o°F.) and spheroidized prior structures were utilized on all steels with hot-rolled and quenched (I600°F. oil) prior conditions added for the plain carbon steel. The end-quench test developed by Jominy10 was sclected for use in this investigation and, with the noted exceptions, the American Society for Testing Materials standard procedure was followed. The effect of time at temperature was examined at intervals of o, 10 and 40 min. and 4 hr., and a few 16-hr. tests were run. Salt-bath heating of the specimens was employed to control and minimize the

Jan 1, 1944

By R. H. Marshall, J. Welchner, E. S. Rowland

This paper presents results on an extension into the realm of high-carbon steels of some work recently published1 on the effects of time at temperature, quenching temperature and prior structure on the hardenability of one 0.20 and four 0.40 per cent carbon alloy steels. It was shown at that time that unless the conditions of time, temperature and prior structure are substantially the same in performing the hardenability test as in conducting hardening of parts in production, the correlation of hardenability information with the hardness and properties of production parts is often not of satisfactory accuracy. The general effects of these variables on the austenitic grain size, distribution of excess carbides and critical cooling rate have been known for many years and one or more have been investigated by Shepherd,2,3 Davenport and Bain,4 Digges,5,6 Digges and Jordan,&apos; Post and associates8 and Roberts and Mehl,9 to mention only a few. There has been no systematic investigation, however, into the quantitative variations produced on the hardenability of commercial high-carbon steels by changes in these factors of time, temperature and prior structure. Procedure A plain carbon hypereutectoid steel, S.A.E. 52100 and Graph-Mo, a molybdenum-bearing high-carbon steel containing some graphite, were chosen for this investigation. The chemical analyses of these electric-furnace steels are given in Table I. The procedure used was exactly that reported previously,&apos; hence the details will not be repeated here. Normalized (165o°F.) and spheroidized prior structures were utilized on all steels with hot-rolled and quenched (I600°F. oil) prior conditions added for the plain carbon steel. The end-quench test developed by Jominy10 was sclected for use in this investigation and, with the noted exceptions, the American Society for Testing Materials standard procedure was followed. The effect of time at temperature was examined at intervals of o, 10 and 40 min. and 4 hr., and a few 16-hr. tests were run. Salt-bath heating of the specimens was employed to control and minimize the

Jan 1, 1944

By R. H. Marshall, J. Welchner, E. S. Rowland

THIS paper presents results on an exten¬sion into the realm of high-carbon steels of some work recently published&apos; on the effects -of time at temperature, quenching temperature and prior structure on the hardenability of one 0.20 and four 0.40 per cent carbon alloy steels. It was shown at that time that unless the conditions of time, temperature and prior structure are substantially the same in performing the hardenability test as in conducting harden¬ing of parts in production, the correlation of hardenability information with the [ ] hardness and properties of production parts is often not of satisfactory accuracy. The general effects of these variables on the austenitic grain size, distribution of excess carbides and critical cooling rate have been known for many years and one or more have been investigated by Shepherd ,2 3 Davenport and Bain,4 Digges,5,6 Digges and Jordan,7 Post and associates&apos; and Roberts and Mehl,9 to mention only a few. There has been no systematic investigation, however,&apos; into the quantitative variations produced on the hardenability of commercial high¬carbon steels by changes in these factors of time, temperature and prior structure. PROCEDURE A plain carbon hypereutectoid steel, S.A.E. 52100 and Graph-Mo, a molyb¬denum-bearing high-carbon steel contain¬ing some graphite, were chosen for this investigation. The chemical analyses of these electric-furnace steels are given in Table I. [ ] The procedure used was exactly that reported previously,&apos; hence the details will not be repeated here. Normalized (1650°F.) and spheroidized prior structures were utilized on all steels with hot-rolled and quenched (1600°F. oil) prior conditions added for the plain carbon steel. The end-quench test developed by Jominy10 was selected for use in this investigation and, with the noted exceptions, the American Society for Testing Materials standard. procedure was followed. The effect of time at temperature was examined at intervals of 0, 10 and 40 min. and 4 hr., and a few i6-hr. tests were run. Salt-bath heating of the specimens was employed to control and minimize the

Jan 1, 1944