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By P. W. Bennett, E. M. Elkin

A new technique for the recovery of palladium and platinum and sludge from go12 electrolyte eliminates many of the drawbacks of the zinc-dust cementation process. In the electrolytic refining of gold by the Wohwill method, the electrolyte contains about 100 gpl gold as AuCl, and 100 gpl free hydrochloric acid. Any palladium and platinum contained in impure gold dissolve and accumulate in the electrolyte. When their concentration approaches that of gold, it becomes desirable to discard the electrolyte and to recover the gold and the palladium and platinum. As practiced at Canadian Copper Refiners until recently, discarded electrolyte was treated with sulfur dioxide to precipitate the gold. 2AuCl3 + 6H2O + 3SO2 —2Au + 6HC1 + 3H2SO4 The gold precipitate was filtered off, washed with water, and melted with scrap anodes. The wash water was added to the gold-free filtrate and treated with zinc dust to cement the palladium and platinum. PdCl2 + Zn — Pd + ZnCl2 PtCl4 + 2Zn—Pt + 2ZnCl2 The precipitate was separated and sold as Pd-Pt concentrate, and the barren filtrate and wash water were discarded. The receipts of palladium and platinum at this company were too small to warrant their refining. The process suffered from a number of disadvantages. Handling the gold-free solution was disagreeable, as it was laden with sulfur dioxide even after blowing with air overnight. Subsequent treatment with zinc dust was also troublesome. A large excess of zinc dust was required. Spray, acid mist, and vigorous evolution of hydrogen accompanied the reaction. The Pd-Pt precipitate was grossly contaminated with occluded unreacted zinc and with yellow granules of sulfur, thought to be formed by the reduction of sulfur dioxide and its derivatives. Repeated boiling of the precipitate with hydrochloric acid and washing with water decreased somewhat, but did not eliminate, the zinc. After drying overnight, the precipitate hardened to a clinkerlike mass that was difficult to grind. Grinding, handling, and packing created heavy dusting. Even weighing in an analytical balance generated dust, indicating that the powder was easily charged with static electricity. The total palladium and platinum content of the powder varied from 56 to 72 pct, with an average of 65 pct. The powder dissolved in aqua regia with difficulty, leaving a small amount of insoluble residue. However, the main drawback of the process was the strongly hygroscopic Pd-Pt product. The powder showed a marked though erratic increase in weight and a corresponding decrease in assay on exposure to air, even during the course of laboratory analysis. Such changes were the source of disagreement between Canadian Copper Refiners and the buyers of concentrate. The cause of the change in weight is believed to be hydrogen, liberated by the action of zinc dust on hydrochloric acid. Some of this hydrogen was adsorbed so strongly by the precipitate that it could not be driven off during the drying. On exposure to air it oxidized catalytically, forming water. Experiments soon showed that the entire process of treatment of discarded electrolyte then in use would have to be changed. A small quantity of apparatus was moved into the gold room, and experimentation was held to a minimum compatible with the development of a new process. PALLADIUM AND PLATINUM PRECIPITATION It was thought that zinc could be replaced with a reagent other than a hydrogen-evolving metal. Semiquantitative experiments showed that platinum and palladium could be precipitated completely from the gold-free solutions with such well-known reagents as sodium formate, formic acid, formaldehyde, and paraformaldehyde. Sodium formate was the preferred reagent, since the other three are volatile and somewhat toxic. The gold-free solutions used were those saturated with sulfur dioxide, partly freed of sulfur dioxide by aerating overnight, completely freed by boiling, as well as strongly and weakly acidic, neutral, and alkaline solutions. The reactions are complex and can be represented by these over-all equations: PdC1, + HCOONa — Pd + NaCl + HC1 + Co2 PtCl4 + 2HCOONa — Pt + 2NaCl + 2HC1 + 2CCX, Strongly acidic solutions required as much as five times the theoretical amount of sodium formate as did solutions neutralized to pH 4.5. Increasing the pH decreased the consumption of

Jan 1, 1965

By Colin Baker, G. C. Smith

Investigation of the initiation and propagation of ductile failure in OFHC copper was undertaken to determine the role of nonmetallic inclusions. The effect of inclusion initiated voids on the formation of the internal cavity and the final shear separation was studied by metallographic eranzination of strained test pieces. A strain anneal technique was used to enlarge the voids under uniaxial stress conditions to elinzinate triaxial stress effects. Measurements of void size us stress and strain were made to show the point at which void im'tiation begins and becomes an important factor in the deformation process. The work of separation of copper-cuprous oxide was determined to attempt to correlate the breakdown of the matrix inclusion interface with void initiation and propagation. The zloid shape and position relative to the tensile axis suggested an interface breakdown mechanisnz of initiation. Evidence is presented that shows a basic similarity between the central cavity propagation and the 45-deg shear portions of the failure. DUCTILE fracture has been studied by a number of workers1-lo and attention drawn to the importance of hard second phase particles in the initiation of the failure. Holes formed at the matrix-particle interface can elongate by plastic deformation and then subsequently expand sideways to link up and produce a major crack. This is usually observed first in the center of the macroscopically necked region of a test-piece where the hydrostatic stresses are at a maximum. As the crack spreads sideways towards the free surface of the specimen, well defined shear zones develop from the crack tip and the final separation is along a direction at approximately 45 deg to the stress axis. This shear failure may also be associated with voids formed adjacent to second phase particles. In this way a cup and cone type fracture is produced. The stage at which separation takes place between particles and the surrounding matrix has not been clearly identified. In addition, although researchers have dealt with anisotropy of tensile behavior" as a result of material fabrication variables, not much is known about the microstructural features of aniso-tropic behavior. In the present work evidence on these points is presented in relation to the behavior of copper containing second phase particles of cuprous oxide. I. MATERIALS AND PROCEDURES EMPLOYED The material used was +-in. diam or 2-in. sq cold-drawn OFHC copper bar which contained 0.6 pct by volume of cuprous oxide inclusions. These ranged in COLIN BAKER, Junior Member AIME, formerly at -mnF of Metallurgy, University of Cambridge, Cambridge, England, is presently Research Scientist Reynolds Metals Co., Richrnand, Va. G. C. SMITH, Member AIME, is Senior Lecturer, Department of Metallurgy, University of Cambridge. Manuscript submitted June 20, 1967. IMD size from approximately 1 to 6 p in length and 1 to 4 p in width. The shape was generally slightly ovoid. Tensile tests were made on specimens having a gage length of 2.5 cm and diameter of 0.643 cm. Metallographic examination was carried out by sectioning deformed and fractured specimens; in addition fracture surfaces were examined optically and with a scanning electron microscope. Some measurements of the work of separation between copper and cuprous oxide were made, using a sessile drop technique which was a modification of that used by Kingery and umenick." The best metallographic results were obtained by using a vibratory polisher, which minimized smearing of the surface. 11. RESULTS A) Initial Experiments. Specimens from the +-in. diam rod were annealed for 2 hr at 650°C in uacuo, at which temperature complete recrystallization occurred without any change in the form of the inclusion. They were then fractured at temperatures from -190" to 600°C. Cup and cone fractures were obtained at all temperatures from -196" to 400°C. With increase in temperature there was, however, a continuous increase in the extent of the central transverse area and a corresponding decrease in the shear portion of the fracture. Above 400°C, the fractures became intergranular. Sections of specimens tested below 400°C revealed extensive small voids which were always associated with inclusions. However, the voids only reached dimensions greater than the inclusion size in the region of the macroscopic neck, where they were many times longer. Lateral expansion was found only near the fracture surface of the test pieces. As observed by Puttick, the voids were either (a) triangular holes initiated in the direction of the tensile axis and elon-

Jan 1, 1969

By C. D. Williams, C. E. Ells

The susceptibility of quenched and aged Zr-2.5 wt pct Nb alloy to embritt2ement during irradiation has been examined for a number of solution temperatures and aging times. Material quenched from temperatures approximately 40°C below the transus has high tensile ductility, and this ductility is insensitive to aging at 500°C or to irradiation. If, however, the material is quenched from temperatures above the transus it becomes highly susceptible to loss of ductility either from aging at 500 or from irradiation. Inter granular failure is characteristic of the materials having low ductility. The distribution of the equilibrium phase is found to control the susceptibility to embrittlement by restricting 6 grain growth during heat treatment and thus influencing crack propagation. IN zirconium, as in titanium, -stabilizing alloy additions are used to obtain high strengths via quench and age heat treatments, and the Zr-2.5 pct Nb alloy has been developed1 because of its strength advantage over the Zircaloys. Early in the development of the Zr-2.5 pct Nb alloy the problem of 13 embrittlement was appreciated, and for this reason the solution temperature was chosen below the p transus.' In the course of irradiation studies on quenched and aged Zr-2.5 wt pct Nb alloy it was found' that irradiation introduced an important aspect of p embrittlement, riz., material quenched from the phase and aged 24 hr at 500°C was severely embrittled by moderate doses of neutron irradiation. This effect had not been studied in titanium alloys. In titanium the metallurgical features leading to 0 ernbrittlement were found to be structures with: a) coarse a platelets at the grain bondaries, b) finely dispersed a uniformly distributed throughout the (0) matrix,6 c) Widmanstatten a-13 with more than 50 pct P, d) the presence of some metastable p transformation products,3 and e) large prior -phase grain size.5 Alternatively, the presence of a uniform distribution of coarse a was conducive to high ductility and a structure largely of equiaxed a was very dctile. The detailed mechanisms of the embrittlement have not been worked out for all of these conditions, although weakness at either a-matrix boundaries or prior p grain boundaries have been prominent in the eculation. It was proposed that acicular a might act as a mild notch, and low ductility has been associated with easy fracture along its boundary.' There have been two opposing suggestions for the source of the high ductility associated with equiaxed a phase. JaffeeB proposed that this a would accept a large por- tion of the oxygen, thus increasing the ductility of the matrix, whereas after study of a Zr-Nb-Cu alloy Weinstein and oltz proposed that the a phase, softer than the martensitic matrix, acted to blunt cracks formed in the matrix. In the present work we have studied the effect of neutron irradiation on the ductility, particularly the P embrittlement, of the Zr-2.5 wt pct Nb alloy. By a variation of solution temperature and aging time a variety of metallurgical conditions have been examined, and a range of resultant ductilities obtained. The ductility has been related to the material microstructure and mode of fracture. EXPERIMENTAL The alloy used in the present work came from two separate ingots fabricated into rod of 3/8 or i in. diam, Table I. For both batches the P transus temperature was approximately 890° C. Most of the heat treatments were done directly on lengths of the j} in. diam rod, after which the tensile test specimens were machined. Quenching was achieved by dropping rods from a dynamic vacuum into water, the cooling rate estimated to be 2 100°C per sec. For aging the rods were encapsulated in evacuated silica tubes. Round tensile test specimens, with gage diam and length 0.160 and 1.0 in., respectively, were used throughout and pulled at room temperature or 300°C on Instron tensile machines, at a crosshead speed of 0.05 ipm. Specimens were irradiated in the NRX and NRU reactors, in facilities described in previous publications.'0 The metallurgical conditions examined have been: All tensile test specimens were machined with axes in the axial direction of the swaged rod. Although the specimen had a degree of preferred crystallo-graphic orientation with basal plane normals both parallel with and perpendicular to the tensile axis, the material was comparatively isotropic." The techniques of thin foil examination in the electron micro-

Jan 1, 1970

By Sheldon P. Wimpfen

EVER since the Phoenicians roamed the known world in quest of metals to harden their helmets and precious metals and gems to adorn their ladies, many other nations have sought metals in the far corners of the earth. During the past 75 years American engineers have been among the foremost in seeking for and developing ore deposits. They have been responsible for many of the principal discoveries and for the application of modern methods to mines in the far comers of the earth. American mining engineers with a zest for travel and an insatiable appetite for metals have also introduced throughout the world many articles made of metal which we consider essential to everyday life. Production and consumption of these metals in many foreign countries has brought to these countries an increased standard of living and added tax revenue to their governments. But unfortunately engineers from this country are no longer given ready access to all the countries of the world. This is not only unfortunate for American engineers but also for the countries that have adopted the exclusion policies and especially so since time has proved that in countries where the American engineers have gradually been excluded there has been a significant decline in the progress of the mining industry. Removal of these barriers to professional men would aid immensely in the world-wide development of the mineral industries. New areas brought into production under the guidance of American engineers with their exceptional know-how would provide more jobs for nationals of the countries involved and a better standard of living for the nations as a whole.

Jan 1, 1946

By J. O. Scott

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

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

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

Jan 1, 1954

Edward Halse, Puerto Berrio, Colombia, S. A. (communication to the Secretary): I have read with much pleasure the interesting and valuable paper by Mr. Kunz, and hope that the following brief notes, gathered a few years ago, while a resident in Mexico City, may help to elucidate the subjcct: Turquoise.—This was known to the Aztecs as Xihuitl. Santiago Ramirez states that they found it in the Cerro Xicohtzonc, close to Atzcapatzalco, a suburb of the City of Mexico (compare page 59). Opal.—This was known to the ancient Mexicans, for they named it mezcuitlatt (compare page 63). Jade.—Under this was iucluded a third mineral, prehnite, not mentioned by Mr. Kunz. According to James D. Dana, part of the "jade " of China is prehnite; and Humboldt informs us, in his work on New Spain, that the same species of jade is known in some parts of Mexico as mahagua (majagua ?). The same writer says, in his Views of the Cordilleras, that the Aztec name Tecpatl included flint, hornstone, and green jade; and finally, in his Travels in South America," he discusses the nature of the ancient amazon-stones, and declares them to have been made out of a jade resembling " compact feldspar," one of the constituents of the gabbro verde di Corsica. IIence those stones were probably composed of nephrite. According to Humboldt, the form given to them most frequently is that of the Babylomian cylinder, longitudinally perforated, and loaded with inscriptions and figures. They were also cut by the natives into very thin plates, perforated at the center, suspended by a thread, and worn as amulets. According to the historian Clavijero, the specific name given by the Aztecs to the nephritic stone (jadeite) was Quitzalitztli,

Jan 1, 1902

By Ronald W. Klusman, Erik B. Nelson

The Front Range portion of the Colorado Mineral Belt is an extensive area of mineralization with mining activity dating from 1859 with the discovery of large gold deposits. After an initial boom period and gradual diminishing production, present activity is restricted to molybdenum in Clear Creek County, uranium in Jefferson County, and several small operations extracting gold and silver in Clear Creek and Gilpin Counties. Gold and silver have dominated the production in the Front Range, though the complex mineralization created milling and smelting problems and it is postulated that considerable amounts of precious metals remain in the mine dumps. This area is plagued by a severe mine drainage problem, with Clear Creek most impacted by many draining mines and tailings in the basin. Boyles et al. Moran and Wentz, Wentz, Wildeman et al., have examined various aspects of the impact of mine drain¬age in the Clear Creek basin. The primary objective of this study was to collect data on the tailings, drainages, and leaching experiments in order to make preliminary suggestions for reducing the impact while recovering metal values to offset treatment costs. A variety of leaching experiments were performed on tailings from the Nevada Gulch area in the Central City mining district. Leachings were performed in vertical tubes indoors and wooden boxes exposed to the outside environment. In the leaching experiments, the leaching solution, grain size, and residence times were varied, while forced aeration was used in some experiments. Bacterial nutrient 9K° and mine drainage were used in some of the experiments. A total of 14 additional tailings samples were analyzed for base and precious metals. The composition of the mine drainage and tailings used in the leaching experiments, as well as data on the additional samples are shown in [Table 1]. Leachate samples were taken periodically for analysis until compositions leveled off. Results and Discussion Leaching with distilled water was used as a control and best illustrates the basic behavior of the leaching process for zinc in a vertical tube [(Fig. 1)]. More acidic leachings increased concentrations of metals as did smaller grain sizes, though the time required increased significantly. Mine drainage with its high concentration of dissolved iron sometimes decreased the heavy-metal concentration in the leachate due to oxidation of Fe 2 and precipitation of Fe(OH)9 which absorbs some of the dissolved heavy metals. In the larger scale experiment carried out in the simulated leaching pad, substantial concentrations of metals were attained in the final leachate after one month. In this experiment the leachate was not recycled, but allowed to saturate the tailings continually with evaporation loss made up by additions of Quartz Hill drainage and nutrient 9K. The concentration of the metals in the leachate and the increase over the input solution are given in [Table 2]. Heap leaching of low-grade copper and uranium ores is successfully carried out in many districts, enhanced by the metabolism of autotrophic bacteria of the Thiobacillus-Ferrobacillus group. These ubiquitous organisms enhance metal leaching, and general aspects of heap leaching are discussed by Malouf, Trudinger, Pings, and Duncan et al. Conclusions and Recommendations Returning to the primary objective, how to reduce the mine drainage impact and recover metal values, we need to consider how the data may suggest avenues toward this objective. Boyles, et al., considered various

Jan 1, 1977

By John V. Morgan

Although the Lansing-Kansas City groups One one of the more important producing horizons of Central Kansas, exploitation has been hindered by inability to consistently identify and correlate the various productive intervals. A study of gamma ray-neutron logs and core data indicates that definite zones exist which are related to production and which may be generally correlated over an appreciable portion of Central Kansas. A suggested system of zoning and nomenclature is developed and illustrated, along with examples of its specific application in overall evaluation and in development of zonal production characteristics. General adoption of the suggested system should aid appreciably in the future development of commercial Lansing-Kansas City production in Central Kansas. It is probable that similar systems might be developed for other regions where production is obtained from various uncorrelated and unnamed zones in thick pay intervals. GENERALIZED GEOLOGY OF CENTRAL KANSAS The most important large subsurface feature in Central Kansas regarding oil production is the Barton Arch, which is part of the Central Kansas uplift. The Barton Arch is a buried ridge of Pre-Cambrian granite running northwest-southeast, near which the majority of Central Kansas oil fields have been found. To the northeast of this arch, the granite dips sharply into the Salina Basin and similar basin areas to the west and south are termed the Hugoton Embayment and Anadarko Basin, respectively. This report deals Primarily with the region of the Central Kansas Uplift and its southwestern flank. Fig. 1 indicates the general location of subsurface structural features along with the oil and gas fields of central Kansas. Above basal granite lies the Cambro-Ordovician Arbuckle Dolomite which is the principal oil producing zone in Central Kansas. This formation, as well as those higher in the section, reflects the general underlying granite structure; however, the Arbuckle top is an erosional surface and most oil producing structures are probably topographic hills. Formations above the Arbuckle in ascending order may include those of the Ordovician, Silurian, Devonian, Mississippian, Pennsylvanian, and Permian periods as well as certain recent sediments. As the Barton Arch is approached, those formations below the Pennsylvanian and above the Arbuckle tend to pinch out until Pennsylvanian rocks, which include the Lansing-Kansas City groups, rest directly upon the Arbuckle. The Arbuckle itself is also completely eroded away at points on the Arch, but is up to 600 ft thick only 20 to 30 miles down dip. Formations of the Pennsylvanian system vary considerably in thickness but probably average about 1,000 ft as an overall total. The more commonly known oil productive zones are the Tarkio, Topeka, Toronto (Dodge), Lansing-Kansas City and Marmaton. Of these, the Lansing-Kansas City, which varies from about 200 ft to 400 ft in thickness, is the most important, since its areal frequency of oil production is exceeded only by that of the Arbuckle. Most Pennsylvanian rocks in Central Kansas were deposited in shallow seas which alternately covered, then retreated from the land. This resulted in recurring cycles of thin beds which cover relatively large areas. Small surface deformations during the period of deposition also caused variations in the type material deposited and its thickness. The local structures of Pennsylvanian time probahlv influenced the accumulation of

Jan 1, 1952

By E. J. Efsic, C. M. Wayman

The fcc to bcc y to a transformation in an Fe-24.5 at. pct Pt alloy was studied and found to be martensitic. Large martensite plates are formed in this alloy which are ideal for crystallographic studies; the Ms temperature is about -5°C. Ordering of the parent phase prior to transformation to martensite causes a pronounced lowering of the Ms temperature. For the first time in the case of alloys of iron, measurements of the habit plune, orientation relationship, and magnitude and direction of the shape stvain have been obtained on preselected martensite plates. It is shown that by measuring the initial and displaced (as a result of the shape strain) positions of three or more non-parallel fiducial scratches on one reference surfice the maguitude and direction of the shape strain and the state of distovtion at the parent-mavtensite interface can be determined with a reasonable degree of accuvacy. The agreement between the phenomenolog-cal crystallographic theory of martensitic transformations and the experimental results habit plune, orientation relationship, and nlagnitude and direction of the shape strain) is essentially perfect, and is thought to be the best reported to date for iron alloys. THE comparatively few investigations on binary Fe-Pt alloys have been concerned with magnetic properties, ordered phases, and the equilibrium diagram itself. Various investigations have shown that the equilibrium diagram is of the open y field type; in addition there is a peritectic transformation, a minimum melting point, and three ordered phases: Fe3Pt, FePt, and FePt3. The results of a number of investigators1-6 have shown that the temperature dependence of the y to a (and reverse) transformation in iron-rich alloys is reasonably well-established. The Fe3Pt phase was first noted by Kussman and Rittberg,7 and its existence was later confirmed by Franklin et al,8 Steijn and Donahoe,9 and Berkowitz et al.10 The FePt phase was reported by Isaac and amman' and later confirmed by a host of others.3,6,7,12,13 Kussman and Rittberg7 noted the existence of the superlattice FePt3. Prior to 1956, the 1 to a transformation in iron-rich Fe-Pt alloys was termed "irreversible". In 1957 Klokholm and Donahoe" termed this transformation martensitic, presumably because of its occurrence at temperatures well below those where diffusion normally takes place. This observation served as a point of departure for the present investigation, and in the very early stages of the work to be discussed it was readily verified that the y to a transformation in iron-rich Fe-Pt alloys is indeed martensitic. Quite large martensite plates exhibiting the well-known surface tilt were observed. These plates are ideal in the sense that the boundaries between the parent and product phases were usually very straight. It thus appeared that Fe-Pt martensites would be ideal for crystallographic studies, and this was the purpose of the present investigation. Details of the crystallography of martensitic transformations (particularly for iron alloys) and the phe-nomenological crystallographic theories15-l7 have been discussed many times and thus will require very little elaboration here. The end result of these theories, given in matrix form, is

Jan 1, 1968

By Robert Bosworth

THE liability for damages to the surface caused by subsidence is an ever present threat in all underground mining. In ordinary lode mining, this threat rarely materializes into an action, due to the method of mining metaliferous ores, the dip of the veins, and the nature of the ground itself. In the mining of coal, however, this threat is very real. The coal frequently lies close to the surface, in beds underlying large areas of land the surface of which is suitable for agricultural or urban development. Furthermore, the coal is generally mined by the "room and pillar " method and when the pillars of coal are removed, the subjacent support is destroyed. This question of the duty of surface support has now become a very live one in Colorado. What was waste prairie land a few years .ago, has become valuable agricultural land dotted here and there with growing towns. Frequent references will be made here to Colorado conditions and adjudicated cases, but those conditions and cases and the conclusions to be drawn therefrom are equally applicable to all coal-mining states. Briefly stated, the question is "Does the owner of the substrata or underlying mineral, owe any duty of surface support to the owner of the superjacent strata or surface?" There is no absolute duty of support owed by the mineral owner and this assertion is made with full knowledge of numerous expressions to the contrary by courts of Pennsylvania, Illinois, Colorado and other coal-mining states. Whether or not any duty exists depends upon the circumstances surrounding each case, and since in the nature of things those circumstances are rarely identical, there can be no absolute rule.

Jan 1, 1927

By Robert Bosworth

THE liability for damages to the surface caused by subsidence is an ever present threat in all underground mining. In ordinary lode mining, this threat rarely materializes into an action, due to the method of mining metalliferous ores, the dip of the veins, and the nature of the ground itself. In the mining of coal, however, this threat is very real. The coal frequently lies close to the surface, in beds underlying large areas of land of which the surface is suitable for agricultural or urban development. Furthermore, the coal is generally mined by the "room and pillar" method and when the pillars of coal are removed, the subjacent support is destroyed. This question of the duty of surface support has now become a very live one in Colorado. What was waste prairie land a few years ago has become valuable agricultural land dotted here and there with growing towns. Frequent references will be made here to Colorado conditions and adjudicated cases, but those conditions and cases and the conclusions to be drawn therefrom are applicable to all coal-mining states. Briefly stated, the question is "Does the owner of the substrata or underlying mineral owe any duty of surface support to the owner of the superjacent strata or surface?" There is -no absolute duty of support owed by the mineral owner and this assertion is made with full knowledge of numerous expressions to the contrary by courts of Pennsylvania, Illinois, Colorado and other coal-mining states. Whether or not any duty exists depends upon the circumstances surrounding each case, and since in the nature of things those circumstances are rarely identical, there can be no absolute rule.

Jan 1, 1928

By Robert Bosworth

THE liability for damages to the surface caused by subsidence is an ever present threat in all underground mining. In ordinary lode mining, this threat rarely materializes into an action, due to the method of mining metalliferous ores, the dip of the veins, and the nature of the ground itself. In the mining of coal, however, this threat is very real. The coal frequently lies close to the surface, in beds underlying large areas of land of which the surface is suitable for: agricultural or urban development. Furthermore, the coal is generally mined by the "room and pillar" method and when the pillars of coal are removed, the subjacent support is destroyed. This question of the duty of surface support has now become a very live one in Colorado. What was waste prairie land a few years ago has become valuable agricultural land dotted here and there with growing towns. Frequent references will' be made here to Colorado conditions and adjudicated cases, but those conditions and cases and the conclusions to be drawn therefrom are applicable to all coal-mining states. Briefly stated, the question is "Does the owner of the substrata or underlying mineral owe any duty of surface support to the owner of the superjacent strata or surface?" There is no absolute duty of support owed by the mineral owner and this assertion is made with full knowledge of numerous expressions to the contrary by courts of Pennsylvania, Illinois, Colorado and other coal-mining states. Whether or not any duty exists depends upon the circumstances surrounding each case, and since in the nature of things those circumstances are rarely identical, there can be no absolute rule.

Jan 1, 1928

By Robert Bosworth

THE liability for damages to the surface caused by subsidence is an ever present threat in all underground mining. In ordinary lode mining, this threat rarely materializes into an action, due to the method of mining metalliferous ores, the dip of the veins, and the nature of the ground itself. In the mining of coal, however, this threat is very real. The coal frequently lies close to the surface, in beds underlying large areas of land of which the surface is suitable for agricultural or urban development. Furthermore, the coal is generally mined by the "room and pillar " method and when the pillars of coal are removed, the subjacent support is destroyed. This question of the duty of surface support has now become a very live one in Colorado. What was waste prairie land a few years ago has become valuable agricultural land dotted here and there with growing towns. Frequent references will be made here to Colorado conditions and adjudicated cases, but those conditions and cases and the conclusions to be drawn therefrom are applicable to all coal-mining states. Briefly stated, the question is "Does the owner of the substrata or underlying mineral owe any duty of surface support to the owner of the superjacent strata or surface?" There is no absolute duty of support owed by the mineral owner and this assertion is made with full knowledge of numerous expressions to the contrary by courts of Pennsylvania, Illinois, Colorado and other coal-mining states. Whether or not any duty exists depends upon the circumstances surrounding each case, and since in the nature of things those circumstances are rarely identical, there can be no absolute rule.

Jan 1, 1928

By John Parker

During 1965, a new stoping method was developed at the Bunker Hill Mine at Kellogg, Idaho to enable the profitable mining of a large low-grade zinc orebody. This method, called the Bunker Hill pillar system, incorporates the use of the air-powered Atlas Copco T2GH or CAVO 310 as the prime production component. The method and equipment proved highly successful and was the first step in mechanizing what had been a classic example of a square-set and horizontal cut-and-fill operation. Since that time there has been a realization that the small rubber-tired type of loader could be effectively used to advantage in increasing productivity and decreasing costs in many different stoping and development applications throughout the mine. The net result since 1967 has been that a large and increasing portion of the mine production and an increasing share of the development is being done with small rubber-tired loaders. Presently, ten Atlas Copco T2GH and six CAVO 310 air-operated loaders are in use, having replaced the time-honored slusher which was first introduced into the Bunker Hill Mine in about 1898 in the form of a slip scraper. The recent advent of diesel powered loaders in the one yard size range has in 1970 further accelerated the trend toward rubber-tired mobile equipment at the Bunker Hill Mine. Although The Bunker Hill Company is using small diesel loaders of several different types and manufactures for inclines, declines and level development and will undoubtedly find stoping applications for this equipment, .the bulk of this paper will be confined to the use of the air-operated loader, leaving the diesel equipment to a future presentation. It is sufficient to say that we feel at this time that the Autoloader type air-powered equipment and the small diesel front end-loader

Jan 1, 1970

Discussion of the paper of GEORGE S. RICE and H. H. CLARK, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin No. 94, October, 1914, pp. 2563 to 2571. NORMAN V. BRETH,* Pittsburgh, Pa.-It was my privilege to visit in the last two months on behalf of the U. S. Bureau of Mines 10 mines where electric shot-firing systems controlled from outside the mine are installed. I will describe briefly what I saw in some of these mines, which are located in Utah, New. Mexico, Oklahoma, Alabama, and Kansas. At a mine in Utah, 230-volt alternating current is used to fire the shots, which is taken from a small transformer in the substation. The shot-iring circuit is independent of all other wires and is tested for grounds every day. There are no lightning arresters on the firing circuit. Porcelain insulators are used inside of the mine, and glass outside. The switches are situated as follows: One in the substation, one in, the shot-firer's cabin, two at each cross entry; where the shot-firing circuit crosses the trolley wire a switch is placed on either side of the entry in series with the shot-firing circuit. The miners are checked in and out of the mine. The coal is undercut and is shot down with permissible explosive, the shots being connected in multiple. There are 75 to 110 shots fired each day. A great many times there are no missed shots. If not more than two or three are missed they are left until next day. The fan is kept running at full speed when the shots are fired. The shot-firing switch is closed only once and the whole mine is shot at once. At another mine in Utah, power wires are used for shot-firing circuits; 500-volt, direct current is used to fire the shots. The only sizes of wire used outside of the power wires are Nos. 8 and 14 B. & S. gauge. The return is connected to the pipe lines and track. Porcelain insulators are. used inside of the mine.

Jan 4, 1915

By F. R. Hutto Jr., F. L. Kady Jr., L. E. Weymouth

The behavior of particulate non-metallic materials in moving contact with smooth surfaces is of interest and concern to manufacturers and users of abrasives, of fillers, and of pigments alike. The theoretical aspects of the subject have been treated to considerable extent in the literature, and correlatic,ns are available that attempt to relate various methods of hardness determination." 2 The particle size and friability are characteristics of the abrasive that are not related to the smooth surface. The hardness, on the other hand, may be visualized as relative to that of the smooth surface. In a study of abrasive action, the role that hardness, per se, plays is a complicated one. For it is necessary to compare the "hardness" of the abrasive, usually a non-metallic, with that of the smooth surface, generally a metal. Hardness of non-metallics is defined as resistance to scratch and is almost universally described with respect to the Mohs scale.3 Minerals have been rated by Mohs numerically from the softest (talc = 1) to the hardest (diamond = 10). By definition, a mineral has a designated hardness when it is scratched by the standard that is numerically just above it on the scale; and conversely, when it scratches the standard that is just below it. Hardness of metals. however.. implies resistance to indentation, a property that has been measured by a number of methods. In fact, the indentation hardnesses of the standard minerals on the hlohs scale have been determined by the Rockwell tester. Reproduced below are two versions of this correlation. 'A conversion chart, prepared by Wilson Mechanical Instruments Division of American Chain and Cable Co., merely gives the conversion from Rockwell to Knoop hardness. The relation between Knoop indentation hardness and Mohs scale has been reported by G. S. Smith — A New Scale of Hardness, The Engineer, Aug. 26. 1949. G. F. Kinney in Engineerin Properties and Aplications of Plastics reports the Rockwell hardness of the minerals directly in the Mohs scale. The question immediately arises as to whether this relation is valid when applied in reverse; namely,

Jan 1, 1961

By R. P. Abendroth

This study is concerned with the kinetics of selective oxidation of chromium in a commercial Fe-Cr-Ni alloy. Selective oxidation of chromium in this alloy, by use of a low oxygen-potential atmosphere, leads to the formation of a compact, protective layer of Cr2O3. This layer serves to protect this alloy from gross scaling when it is subsequently exposed to severe oxidizing conditions at high temperature. The interaction of low oxygen-potential atmospheres close to equilibrium with Fe-Cr and Ni-Cr alloys has been studied by others."' These studies werk concerned with the surface-structure variations under slightly oxidizing conditions. NO detailed study was made of the oxide scale formation kinetics, however. The alloy samples were cut from 0.012-in.-thick sheet, with an apparent surface area of 7.1 sq cm. These sheet samples were abraded through 4/0 metallographic paper, and washed in alcohol and acetone. The analysis of the sheet alloy is (in weight percent): 42 pct Ni, 5.5 pct Cr, 0.09 pct C, 0.18 pct Al, 0.36 pct Si, 0.26 pct Mn, balance Fe. The weight gain vs time data were obtained with a 2-g capacity fused-silica spring—cathetometer system. The spring deflection was optically magnified ten times before being read by the cathetometer. A sensitivity of about 0.01 mg was attainable. The spring was enclosed in a water jacket maintained at 60°C to minimize the effect of temperature changes. The sample was suspended from the spring with a fused-silica hangdown and was positioned in the thermal center of a mullite furnace tube. Sample temperature was read with the aid of a thermocouple placed outside the mullite tube and an inside vs outside temperature calibration. Temperature change during the course of a run was ±0.25°C, with a temperature gradient of less than l.O°C over the length of the sample. Total temperature uncertainty was no more than ±3.0°C. Alignment difficulties between the hangdown and radiation shields in the furnace tube required that the sample be positioned in the furnace when cold, and heated with the furnace until the temperature stabilized at the desired point. This required 5 to 6 hr, and was carried out in Matheson ultrahigh-purity hydrogen. Oxidation was started, after evacuation, by introducing a hydrogen-water vapor mixture, obtained by saturating hydrogen with water vapor at 31.00o ± 0.02oC. Oxidation was continued for 90 min. Gas flow was 300 ml per min during heat up and oxidation. Since only several milligrams of oxide are formed on each sample, chemical analysis of the oxide is difficult. A representative analysis is: 80 pct Cr2O3, 5 pct Fe2O3, 3 pct Al2O3, 4 pct MnO, 7 pct SiO2, 1 pct or less NiO. X-ray diffraction analysis of the oxide as formed on the alloy gives rhombohedra1 Cr2O3, and barely distinguishable amounts of a cubic spinel phase, and possibly AlZOs and SO2. The identification of these latter two compounds is by no means certain. The spinel phase could be based on iron or manganese as these elements are present in significant amounts in the oxide. The results of the kinetic studies using 31°C dew-point hydrogen-water vapor mixtures were found to conform to a parabolic rate law. In many cases the parabolic plot consisted of two intersecting straight lines, defining an early and a late rate for a particular run, and in the other cases the parabolic plot consisted of one straight line for the entire run. The slopes of the various straight lines were determined by the method of least squares. Reproducibility of the data was good enough for multiple runs at the same temperature such that the value given for the rate constant is the average for two or more closely similar values, rather than widely varying values of the rate, where more than one determination is indicated in Table I. The exhibition of only one or of two rate constants during a run can happen at the same temperature. Thus, Table I shows that at 11'74°C a single rate constant was obtained from one sample, while other samples oxidized at the same temperature gave an early and a late rate constant. It should be noted that the single rate constant corresponds very closely with the early rate constant. This is also true at 1153°C. The time at which the late rate started to appear was variable, usually occurring 20 to 40 min after oxidation had started.

Jan 1, 1964

By F. L. Sizer

The mining regulations of British Columbia and Mexico present some features which might well be copied in the United States, if we are to have a complete revision of the laws governing mining titles. 1. First and foremost is the "squarc" location, which would mean the abolition of extralateral rights. This is a condition in both of the countries above named which has seemed to work no hardship upon any one, and certainly the limitation of underground rights by vertical planes through all lines makes a locator's rights clear. In view of the long and costly litigation which has involved so seriously many of our most important mining districts, it would seem to be the part of wisdom to avoid a repetition of similar trouble on titles of lode mining claims, by the enactment' of a law similar to that in force in British Columbia. Objections have been raised by .representatives of English companies to the investment of large amounts of money in mining operations in the United States, because of the insecurity of title under the 'present apex law; and the statement has been made to me personally by one of the largest English operators, that he would .never again consent to the purchase of mines in the United States, preferring Mexico with all its revolutionary troubles to the danger of encroachment upon his underground rights by an unscrupulous neighbor. Without going into further argument as to the desirability of the I(square location," it should be sufficient to say to those who are inclined to "let well enough alone" and still stick to the "law of the apex" that there have never been any serious objections raised to this feature of the square location in either British Columbia or Mexico. There are well founded and logical reasons for abandoning the doctrine of extra-lateral rights since it is so difficult of interpretation; the most natural substitute being a law similar to that of British Columbia, giving to each locator an area 1,500 ft. square. I would advocate the right to locate adjoining claims of equal extent on either side of the discovery claim, on the strike of the lode, subject to a seasonable requirement in the matter of work upon them; and in the case of a vein dipping flatter than 45' from the horizon, or in case of a

Jan 1, 1915

By C. W. Spencer, F. G. Hochgraf, R. F. Cheney

Columnar grained specimens of nickel, containing 0.25 pct Si and 0.22 pct Mn, have been exposed to liquid bismuth in the temperature range 670° to 1050°C. Under isothermal conditions the liquid penetration rate is constant. The activation energy for the process is 22,000 cal per g-atom. Small amounts of plastic deformation, introduced into specimens prior to exposure, increase the penetration rate. The slou. step in liquid film penetration is associated with a reaction which occurs at or near the leading edge of the film. Either transfer of nickel across the liquid-solid inteqace or diffusion in the grain boundary ahead of the liquid film is suggested. Aliquid metal, if brought into contact with the surface of an unstrained solid metal, will usually penetrate to some extent into the grain boundaries of the solid. Under isothermal conditions the extent of penetration after any particular time of exposure is related to the relative magnitudes of the interfacial tensions concerned.1,2 If the liquid-solid interfacial tension is less than one-half the grain boundary tension the liquid may penetrate at a relatively rapid rate for an indefinite distance into the grain boundary surfaces. If the liquid-solid interfacial tension is greater than one-half the grain boundary energy, liquid penetration occurs at a continually decreasing rate so that after the liquid has penetrated to a relatively short distance below the surface the process essentially ceases.3 Many observations of a qualitative nature concerning inter crystalline attack by liquid metals have been reported, for example, liquid bismuth upon copper,' liquid mercury upon brass,4 and liquid mercury upon nickel.' Scheil and Schessl determined the rate of penetration of liquid bismuth into the grain boundaries of hot rolled copper rod? At constant temperature, penetration rate was found to be independent of the depth penetrated, the rate in- creasing with increasing temperature corresponding to an activation energy of 20,000 cal per g-atom for the process. It was suggested that at lower temperatures the liquid travelled mainly along lines of three grain intersections while at temperatures greater than 1000°C essentially all grain boundary surfaces were covered. Recently, in a study of copper bicrystals having a common [loo] axis it was found that at 649°C bismuth penetrated 22, 25, and 63 deg boundaries while it did not penetrate 2, 12, 15, and 72 deg boundaries.' Elbaum reported that liquid gallium penetrates aluminum grain boundaries to a depth of 0.6 cm after 11 hr at 27°c.8 Assuming that the rate controlling step in the process was diffusion down the liquid film to the specimen surface, a diffusion coefficient of 10-5 cm2 per sec was calculated. This paper reports a study of the penetration of bismuth-nickel liquids into the grain boundaries of a nickel alloy, containing 0.25 pct Si and 0.22 pct Mn as principal alloying elements. The phase diagram

Jan 1, 1962