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By E. R. Stover, J. Wulff

A tentative 870°C isothermal section, the solidus equilibria, and the solubility of Tic and graphite in the nickel solid solution have been determined with arc-cast specimens. Each of the Ni-Ti intermetallics forms two-phase fields with Tic; only Ti,Ni has a measurable solubility for carbon. A quasi-binary eutectic exists between Tic: and a titanium-rich nickel solid solution; ternary eutectics occur on either side, with TiNis or with graphite. Graphite is in equilibrium with a nickel solid solution containing a ratio of Ti/C which increases below the solidus. DURING the past decade, titanium-carbide cermets containing nickel or cobalt alloy binders have been widely studied for high-temperature and wear-resistant applications. Recent work has emphasized control of the carbide grain size and distribution2's and the thermal exparision match between the phases/ The present study was initiated to determine the phase compositions during the sintering or infiltration process, and during subsequent heating. Although the effects of additives and impurities in commercial compositions are important, it was necessary to consider first the pure ternary, Ni-Ti-C. Emphasis was placed on the nickel corner, since the nickel solid solution is the continuous phase in compositions having highest strength. Early metallographic work by Zarubin and Molkov- showed that solid solubility at either end of the section Ni-Tic is small. Edwards and Raine reported that nickel dissolves between 3 and 5 wt pct Tic at 1250° C, on the basis of microstructures of annealed, vacuum-melted powder mixtures. Although the solubility of nickel in Tic has not been measured, Tic formed by the menstruum process in liuid-iron solution contains as little as 0.06 wt pct Fe. BINARY SYSTEMS The most recent determinations of the three binary systems are summarized in Fig. 1. Titanium carbide (6) is predominant among the binary phases, and it melts above the boiling point of nickel. The Ni-C binary is based on separate liquid solubility' ) and solid solubilitylo measurements. The eutectic temperature, 1328OC, is taken from the solidus determination described below. However thermal analysis data by Morrogh and williams also show eutectic arrests in this vicinity in the absence of supercooling. The Ni-Ti binary is taken from the work of Poole

Jan 1, 1960

By K. R. Evans

The yield and fracture characteristics of a Ti-8 pct A1 alloy have been examined at room temperature as a function of exposure temperatures to 1700°F. Em-brittlenzent of the alloy is observed to occur following exposures below 1280°F, the critical temperature for formation of ordered Ti3Al particles. Presence of Ti3Al particles results in an increase in the yield and flout stresses which, for a given exposure time, are a maximum at the critical temperature. Embrittlement is attributed to the occurrence of plastically induced fracture controlled by the increase inflow stress. This interpretation is compatible with the decreasing ductility and increasing crack popagation rates observed with increasing exposure time below the critical temperature. Slip line observations and measurements of the gain size dependence of the yield stress indicate that the slip character of the alloy is not influenced by exposure treatments below the critical temperature. ThE potential usefulness of Ti-A1 alloys in structural applications has prompted considerable interest in studies of their microstructure and mechanical characteristics. The relatively recent surge of interest in the system and at the same time its complexities are indicated by the fact that despite numerous recent efforts14 there has not even been general agreement upon a phase diagram for the system. However, most of the Ti-A1 alloys of commercial interest range in aluminum content from 5.0 to 8.5 wt pct where most investigators achowledge the existence of the ordered Ti41 phase. Goldak and parrs confirmed the existence of Ti41 from X-ray diffraction analysis of the stoichiometric composition while Blackburn6 has determined its presence in commercial Ti-8 pct A1 alloys by electron diffraction analysis and dark field transmission microscopy. The embrittlement of Ti-8 pct A1 alloys was initially reported by Crossley and carew7 who showed that aging in the temperature range of 750" to 1110°F resulted in extreme brittleness. This behavior was later confirmed and correlated by Soltiss to the presence of long-range order in the commercial Ti-8 pct Al-1 pct Mo-1 pct V alloy (Ti-8-1-1) which exhibited anomalous creep and yield strength behavior at 950°F. This investigation was designed to study the mechanical characteristics of a binary Ti-8 pct A1 alloy in order to further examine the nature of the embrittlement behavior reported for the alloy system. EXPERIMENTAL PROCEDURE A Ti-8 pct A1 binary alloy was obtained from the Wah Chang Co. in the form of 0.050 in. sheet. The chemical composition of the alloy is given in Table I. Heat-treatment of the alloy was conducted in evacuated vycor capsules for the tensile sDecimens (1.25 bv 0.25 in. gage section) and in evacuated stainless steel jackets for the crack growth-rate panels. All specimens were annealed at 1700°F for 24 hr and water quenched before an exposure at elevated temperatures. Tensile testing was conducted at room temperature in an Instron testing machine equipped with a pushbutton control for instantaneous control of the cross-head motion. In this manner the change in stress, Aa, accompanying an increase in strain-rate by a factor of 10 was measured immediately after yielding. The crack growth-rate panels used were 3 by 18 in. with a precrack 0.33 in. long cut into the center of the panel. The panels were cycled at a maximum gross stress of 40,000 psi at a maximum to minimum tension stress ratio of 20. Cycling of the specimens was continued until the crack propagated the width of the panels. The crack length was intermittently measured during slow crack growth. EXPERIMENTAL RESULTS Correlation of Embrittlement to the Critical Temperature for Ordering. Blackburn6 has found that the critical temperature, T,, for the formation of Ti41 in a Ti-8 pct A1 alloy with an interstitial content on the order of that given in Table I is approximately 1245°F. The relationship between the ductility of the binary alloy used in this investigation and T, was estimated from tensile tests on specimens which were exposed for 24 hr at various temperatures followed

Jan 1, 1970

By Maxwell Gensamer, Vsevolod N. Krivobok

It is generally recognized that "low temperatures" have a definite effect on the properties of metals and alloys. Furthermore, it is also generally understood that the effect is decidedly adverse. The possibility that the same low-temperature treatment might be employed for the purpose of improving certain properties of the alloys has received less attention until recently, and the experimental and theoretical knowledge consequently is meager. The effect of low temperatures may be studied in two ways: by studying such properties as tensile strength, hardpess, impact resistance, etc., at low temperature, and by studying the properties of alloys at room temperature after these alloys have been subjected to a low-temperature treatment. Even in the latter case, certain properties will differ materially from the same properties obtained on identical material but without cold treatment. In other words, subjecting alloys to cold treatment results in an irreversible change in mechanical properties. Changes of this character are usually indications of the appearance of a new phase or phases, and would be likely to occur in alloys which, either by virtue of their composition or by heat treatment, are retained at room temperature in a metastable condition. Consequently, studies of the effect of low temperatures logically should be conducted from the physicochemical point of view, since the results of such studies not only would furnish metallurgists with interesting theoretical data but would clearly indicate the classes of alloys that would hold promise of improvement, and, possibly, of new applications. As the present investmigation deals with chromium and chromium-nickel alloys of iron of the stainless variety, it has been thought desirable to present the data concerning low-temperature properties of these alloys, available from the most recent and most comprehensive work of H. S. Russell.l A summary of these data is given in Table 1. The data are confined to a limited number of alloys of the type dealt with in the present

Jan 1, 1931

By A. D. Rovig, D. W. McGlashan, Donald M. Podobnik

Crystal-chemical and stntctural properties of sulfide minerals are considered. The information gained is to be used to interpret (I ) freshly broken mineral surfaces, (2) modifications of the mineral surfaces, and (3) reactions at the mineral surfaces. From these basic disciplines, concepts with regard to the changes that surfaces undergo, reactions that might take place, the geometry of the interface, the state of different atoms and ions in the interface, and other physical and chemical properties of an interface must be developed, weighed and applied. The authors first deal with these conceptual considerations from which hypotheses are set forth to describe the environ men tal-interfacial relationships for several sulfide minerals. Qualitative and quantitative explanation of par-ticulate solid separations are unknown entities because of the lack of adequate models and mathematical relationships to explain the activity occurring between the solid and liquid phases. It is a transitional region in which it is difficult to ascertain the mechanisms of adsorption of ions, molecules, etc., on mineral surfaces, as well as other secondary reactions which occur in interfacial regions. Thus, in this paper the authors deal with conceptual considerations from which hypotheses are set forth to describe the environmental-interfacial relationships for sulfide minerals. GENERAL CONSIDERATIONS Interfacial Reactions:Interfacial reactions are the cruxes of flotation schemes as well as other processes such as thickening, filtration and hydrometallurgy. However, as noted by Klassen and Mokrousov: 1 "The problems concerning the surfaces of natural minerals, the laws governing simultaneous adsorption from aqueous solution on these surfaces of a whole series of reagents, the laws of the surface reactions and the properties of water layers separating the minerals, are all known to a first approximation only." An investigator has the privilege of postulating methods of solid-liquid interfacial reactions. REACTIONS WITH WATER - Water consists of hydronium (H3 O 4) and hydroxyl (OH-) ions in the ionized state. That this is so forms the basis for the postulated reaction of the hydrated hydrogen ion with net-negative mineral surfaces as depicted in Fig. 1. In this case water is bonded to mineral surfaces through hydrogen-bridge-type bonds - possibly hydrogen bonds. Although bonding of the van der Waal type may be responsible for this reaction, it is most likely that stronger bonds are involved. Once firmly bonded to the surface, the water layer is known to be quite tenacious. It is further speculated that a shear plane exists at some distance (see Fig. 1) away from the mineral surface. Exact location of this plane is not known, but in all probability it will be positioned across a weak bond of the hydrogen-bond type where the surface-attached water is coordinated to the original hydrated hydrogen ion. REACTION WITH METAL IONS - Klassen and Mokrousov ' state: "The presence of an ion in water leads to an immediate formation around that ion of a highly condensed atmosphere of water dipoles and thus to hydration of the ion." The fact is known that multivalent cations are strongly hydrated, usually by six or eight molecules of water, and that anions are not so strongly hydrated. Conceding the fact that thermodynamics, concentration, pH, and physical considerations are of utmost importance in truly explaining a mechanism of metal ions reaction with a hydrated mineral surface, it does seem logical that the mechanism illustrated in Fig. 2 is feasible. In this reaction, the metal ion (M) is coordinated in one dimension - to the mineral-surface hydration layer. Note also that explanation of this reaction requires that the shear plane move to a less stable bond configuration; that is, the shear plane has moved to a position between the metal ion and the other coordinated water molecules which are more free to dissociate. Reactions as depicted in Fig. 2 should cause the formation of an apparent mineral surface which is net-positive. Immediately, it must be noted that measurements of apparent-mineral surfaces serve - within limits - to indicate a degree of ion-surface reaction capability. The major limiting factor he re is one related

Jan 1, 1970

By A. U. Seybolt, J. L. Walter

The effects of the addition of 0.5 pct ThO2 (by volume) on the grain structure and texture of heavily rolled tungsten sheet were studied. Powder metallurgy ingots were rolled to sheet, 0.001 in. thick, and samples were annealed at temperatures from 1200" to 2500°C. The heating rate to the anneal temperature was varied from 3°C per min to 6500°C per min. The orientations of the largest grains were determined by X-ray diffraction. The disposition and loss of the ThO2 particles were determined by electron transmission microscopy and the activation energy for remozlal of the thorium was measured by mass spec-troscopy. Heating rates below about 800 C per min produced large, highly elongated grains. Higher heating rates produced much smaller, less elongated grains. The grain structure and texture of the slowly heated samples were identical to the structures and textures of heavily rolled tungsten foil conventionally doped with aluminum, silicon, and potassium but the recrystallization temperature was about 200°C lower. There was stringer-like dispersion of larger ThO2, particles superimposed on a uniform dispersion of fine particles. The particles increased in size and decreased in number with time at temperature. The loss of particles was accompanied by formation of grain boundary voids and surface pits. The activation energy for removal of the ThO2 was about 40 kcal per mole. THE addition of small amounts of aluminum, silicon, and potassium to tungsten has a profound effect on the grain structure of heavily rolled sheet1 or drawn wire."4 Thus, "doped" tungsten sheet, rolled to 0.001 in. and recrystallized, develops a structure consisting of large, highly elongated grains of a specific preferred orientation.' It has been shown that the elongated grain structure was caused by a dispersion of particles, identified as mullite (Al6si2O13),1,4 in strings parallel to the rolling direction in sheet or to the wire axis. Identical results were obtained for iron which was doped with glass and rolled to 99 pct reduction of thickness and recrystallized.5 Again, the glass particles were disposed in strings parallel to the rolling direction. The strings retarded boundary migration in the lateral direction but grain growth was able to proceed relatively unhindered along the direction parallel to the strings.1,5 In both the doped tungsten and the glass-doped iron, the particles were highly plastic during the high-temperature deformation. Since mullite melts at about 1800°C and the glass employed melts at about 810ºC, the particles were probably molten during the recrystallization anneals (above 1800°C for the doped tungsten and 850°C for the glass-doped iron). There are indications in the literature that particles not plastic at hot-working temperatures (up to about 1550°C for tungsten) may also impart elongated grain structures by primary recrystallization of worked alloys. Examples are dispersions of tantalum carbide in chromium,6 and ThO2 in nickel where elongation ratios of recrystallization grains of up to 20:l were obtained.7 Strings of ThO2 particles in W-ThO2 wire have been seen by Rieck.8 In view of the available evidence, it was of interest to extend the previous studies of doped tungsten and glass-doped iron to include W-ThO2 sheet materials. Of specific interest was the grain structure, preferred orientation, recrystallization temperature, and disposition of the thoria particles. EXPERIMENTAL PROCEDURE A) Material Preparation. About 380 g of blue tungsten oxide (approximate composition WO3) was wet with a sufficient amount of aqueous solution of Th(N03)4 to provide 0.5 vol pct ThO2. The wet mixture was stirred to distribute the doping material uniformly throughout the powder. Stirring was continued while the mixture was heated until it was completely dry. The dried, doped mixture was then reduced to tungsten powder by heating at 850°C for 2 hr in a stream of dry hydrogen. The doped tungsten powder was hydropressed in a rubber sack at pressures of 50,000 psi to produce an ingot approximately 2 cm diam by about 5 cm long. Next, the pressed cylinder was heated in hydrogen for 2 hr at 1350°C to render it strong enough for machining. The cylinder was machined to a square cross section of 1.6 by 1.6 cm with rounded corners. Finally, the bar was heated for 2 hr at 2150°C in hydrogen to provide a sufficiently dense mate rial to withstand the hot-rolling operation. Prior to rolling, the ingot was reduced in thickness by about 20 pct by forging at 1550°C. This served to increase the density of the material and to widen it slightly for better rolling characteristics. The forged ingot was then rolled at 1550°C to a reduction of 45 pct of thickness, following which the rolling temperature was reduced to 1300°C and the slab rolled, with several reheats, to 0.050 in. Further reduction was accomplished at 800°C in tungsten sheet packs to a total reduction of about 99.85 pct. B) Annealing Treatment and Observation of Structure. Small samples of the rolled foil were annealed in one of two ways. Some of the samples were suspended in a covered tungsten can and annealed at temperatures from 1200" to 2200°C for various times in vacuum of l0-7 to 10-6 mm Hg. The can was heated by induction and temperatures were determined by optical pyrometry

Jan 1, 1970

By R. E. Delavault, H. V. Warren

In normal soils there are usually 10 to 50 parts of copper in every million parts of .soil. Only 0.2 to .5 pct of this copper can be found by any simple cold chemical attack. Now, with rubeanic mid reagent paper, a prospector or field geologist can detect as little us 4 ppm of readily available copper ill soil. This degree, of sensiticity is enough to determine the presence. of copper anamalous an as and, ecentually, to discouer copper mineralization. Circumstances determine whether it is better to make analyses in the field or in a permanent laboratory. The rubeanic acid test described in this article has been designed primarily for field use: it is simple and virtually foolproof, and it requires a minimum of field kit." It is sensitive, easily de- • Ed. Note: Persons Interested in purchasing kits suitable for rubeanic acid prospecting can obtain information by writing Eldrico Geophysical Sales Ltd., 633 Hornby Street. Vancouver 1, B.C. The University of British Columbia does not produce these kits for sale and has no financial interest in their production tecting 4 ppm of readily extractable copper in a soil. This is by no means a quantitative test, but it is accurate enough to provide a valuable indicator of copper anomalous areas for both prospectors and field geologists. The easiest method for detecting metal deposits that do not produce visible float or stains is to make a simple chemical test for the metal in overlying soil, or in the silt of a stream that may have picked up metal farther upstream. In Brief: Testing for copper may be done easily by shaking a soil sample with strong acetic solution in a small test tube and pouring the mud into a small filter, the tip of which rests upon a strip of reagent paper impregnated with rubeanic acid (di-thio-oxamide). When copper is present—and only when it is—a blue spot develops. The more copper, the darker the spot. If the copper content is merely the small amount present everywhere, there is a pale blue or hardly visible spot; if it is abnormally high, the spot will be dark. There are, of course, intermediate cases where the experienced geochemist cannot tell offhand whether a medium-strength spot represents rich agricultural soil, weak copper mineralization, or distant rich copper mineralization. Reagents and material are inexpensive; the test may be readily done on the spot with a simple kit easy to pack and handle. Anyone interested in general problems of soil sampling as applied to prospecting may refer to an article recently presented to the AIME. In exploration work it is the contrast between the metal content of anomalous and background areas that is important; absolute values become of greater interest when an anomalous area is being investigated in detail. With specific reference to copper, it has been the authors' experience that the amounts of metal extracted from anomalous and normal soils with buffer solutions of decreasing pH show better contrast if an acid reagent is used. This contrast tends to increase with increasing acidity until 3 to 4 pH is reached. Using a short cold attack on unheated soil, it has been found that further increases in acidity do not produce better results, and only increase the hazards involved in carrying strong acids. An acidity of about pH 4 is satisfactory for direct determination of copper by dithizone. But dithizone itself introduces some problems: it must be made up fresh at frequent intervals, and with some soils, notably those with much ferric iron, oxidation mag take place before all the copper has reacted with the dithizone. Rubeanic acid keeps its strength unimpaired for long periods, is unaffected by oxidation, and is practically specific for copper at pH 4. Consequently it seems an ideal reagent to use in prospecting for copper. History and Background: Rubeanic acid (systematic name: dithio-oxamide (SC-NH2) has long been known as a spot test reagent for some heavy metals with which it gives a number of compounds. Only copper and some metals of the platinum family are believed capable of providing any ru-beanate compounds under conditions of moderate

Jan 1, 1959

By E. T. Turkdogan

This is a compilation and a critical review of the data on the Fe-Ca-0 ternary system. Using the results on the reductiorz-equilibria, an oxygen potential diagram is drawn for the greater part of the system. A number of univariant systems and invariant points, not determined experimentally, are evaluated by making use of the theorem on univariant curves intersecting at an invariant point. The formation of solid solutions and ternary compounds and the crystal structures of some of the phases in the composition-diagram are given for a feu! temperatures. DURING the past thirty years there has been a continued interest in the study of the Fe-Ca-0 system. A detailed literature survey made by white1 in 1943 indicated that further work was required to clarify the phase relationships; in fact, the work carried out in the subsequent years, reviewed by Burdese2 in 1954, made a valuable contribution to a better understanding of this subject. Most of the data were obtained by the step-wise reduction of mixtures of iron oxides and calcium ferrites. However, there is some uncertainty about the phase relationships in this system, arising mainly from insufficient use of thermodynamic concepts in the construction of phase diagrams. In this paper an attempt is made to establish the invariant points from the available data. OXYGEN POTENTIAL DIAGRAM Schenck and coworkers3,4 were the early investigators who studied part of this system by the step- wise reduction method and suggested the formation of two ternary compounds, CaO.FeO.Fe2O3 and 2Ca0.5Fe0.2Fez03, the latter being referred to as point X. They also deduced from their results that the phases Y (8.74Ca0.32.5Fe0.8.74Fe2O3 and Z (2.02CaO-97.98FeO) were formed near the w?stite corner of the system. Martin and voge15 postulated the existence of the compounds CaO.9FeO and 4Ca0.3Fe3O4; the former is very close to the composition of point Z and the latter to that of CaO.FeO-Fe2O3. The most valuable contribution to the presen knowledge on this system was made by Cirilli and Burdese6-8 who showed by X-ray and chemical anal yses that there were two ternary compounds, CaO-Fe0.Fe2O3 and CaO.3FeO-FezO3; the former is the same as that suggested by Schenck et al. and the latter is close to their point X. The results of Cirilli and Burdese show that the phases Y and Z postulated by Schenk et al. are solid solutions of calcium oxide in w?stite. In most of the above-mentioned reduction-equilibria measurements carbon monoxide-carbon dioxide mixtures were used and in a few cases hydrogen-water vapor mixtures were employed. Using the

Jan 1, 1962

By R. E. Steiner, A. F. Weinberg, R. J. Van Thyne

Uranium solubility in molten bismuth was determined in the temperature range 350" to 600°C, varying from 0.09 wt pct to near 2 wl pct, respectively. Zirconium and magnesium, simulated fission products, and sodium were found to increase or decrease uranium solubility in bismuth in the temperature range 370° to 420°C, depending upon the addition or temperature. Data were obtained by both chemical analysis of samples obtained by filtration from saturated melts and by measurement of the variation of electrical resistance with temperature. IN a study for the United States Atomic Energy Commission, a Liquid Metal Fuel Reactor Experiment (LMFRE) was proposed in which a solution of uranium dissolved in molten bismuth served as both the fuel solution and the primary coolant. It was proven necessary to add other elements to this solution for certain desirable properties: 1) zirconium acts to prevent reaction of the fuel solution with the graphite core (which would result in the formation of uranium carbide) and also to inhibit mass transfer of iron and chromium from the walls of the reactor tubing to cold spots resulting in blockage; and 2) magnesium acts as a deoxidant and prevents loss of uranium. In addition to these intentional additives, other elements entering the solution are: 1) fission products which are a by-productof reactor operation, 2) sodium (the secondary coolant) through possible small leaks in the heat exchange system, and 3) iron and chromium from the container walls. Each of these elements may affect the solubility of uranium in the fuel solution. Since the concept of this reactor is based upon a liquid solution, the relatively low solubility of uranium in bismuth will dictate the minimum temperature at which the reactor heat exchanger can be operated. The solubility of uranium in liquid bismuth and the effect of some additives on this solubility have pre- viously been investigated1-' (more recent results6" became avaliable after initiation of this investigation). However, some discrepancies between the various results have been noted, and also the cumulative effect of the several additions or impurities was not known. This investigation was commenced to obtain definitive results. MATERIALS Analyses of the materials used are presented in Table I. Although ostensibly of extreme purity (99.999 wt pct), the bismuth was found to contain a significant amount of impurities, probably oxides. Except for determination of the binary system, Bi-U, prior to use all bismuth was hydrogen-refined and

Jan 1, 1962

By C. P. Proctor, J. B. Morrow

With numerous plans under consideration for coal classification, and with the advent of the Bituminous Coal Code, the intelligent sampling of coal has become increasingly important. To us it is rather significant that there have been very few fundamental studies of coal sampling in American technical literature since those of E. G. Bailey, which appeared in the Journal of Industrial and Engineering Chemistry in March, 1909. He covered the subject up to that time so thoroughly and in such an excellent manner that perhaps many other later students have felt that they could add very little to his findings. The recent studies of the British Engineering Standards Association have indicated the possibility of a somewhat different interpretation of Bailey's results, permitting the taking of smaller samples, and perhaps it will now be helpful to reopen this question. C. W. H. Holmes, in an informative series of articles on coal sampling recently published in Colliery Engineering, makes two rather interesting statements, as follows: It is scarcely surprising to find a lack of interest and knowledge regarding the sampling of coal not only in the mining industry itself but also among consumers of industrial fuel: at its best coal sampling is a dirty business, regarded as a nuisance and an expense by the commercial man, and usually as a nuisance and nothing else by the chemist. The writer can conceive only two classes of people who have never experienced any difficulty in obtaining representative samples of coal from wagons; those who have never tried to, and those who have never had the necessity or desire to check the accuracy of their work. The primary purpose of this paper is to present some tabulated data of the more significant results of a sampling investigation undertaken during the last four years to obtain certain fundamental data on the variables connected with coal sampling and to point out that often assumptions have been made that are not in accordance with the facts. One of the standard sampling methods states:

Jan 1, 1936

By C. P. Proctor, J. B. Morrow

With numerous plans under consideration for coal classification, and with the advent of the Bituminous Coal Code, the intelligent sampling of coal has become increasingly important. To us it is rather significant that there have been very few fundamental studies of coal sampling in American technical literature since those of E. G. Bailey, which appeared in the Journal of Industrial and Engineering Chemistry in March, 1909. He covered the subject up to that time so thoroughly and in such an excellent manner that perhaps many other later students have felt that they could add very little to his findings. The recent studies of the British Engineering Standards Association have indicated the possibility of a somewhat different interpretation of Bailey's results, permitting the taking of smaller samples, and perhaps it will now be helpful to reopen this question. C. W. H. Holmes, in an informative series of articles on coal sampling recently published in Colliery Engineering, makes two rather interesting statements, as follows: It is scarcely surprising to find a lack of interest and knowledge regarding the sampling of coal not only in the mining industry itself but also among consumers of industrial fuel: at its best coal sampling is a dirty business, regarded as a nuisance and an expense by the commercial man, and usually as a nuisance and nothing else by the chemist. The writer can conceive only two classes of people who have never experienced any difficulty in obtaining representative samples of coal from wagons; those who have never tried to, and those who have never had the necessity or desire to check the accuracy of their work. The primary purpose of this paper is to present some tabulated data of the more significant results of a sampling investigation undertaken during the last four years to obtain certain fundamental data on the variables connected with coal sampling and to point out that often assumptions have been made that are not in accordance with the facts. One of the standard sampling methods states:

Jan 1, 1936

By F. W. Maclennan

PAPERS by D. B. Scott, E. G. Deane, and J. H. Hensley, Jr.1 describe the succession of mining methods used in the Miami mine—squarelset system, shrinkage stoping, top-slicing method, and the undercut caving system which was then being used, and which embraced the use of finger raises. The last-named system worked well but when the rich ore was exhausted it became necessary to reduce costs so as to make available a low-grade ore containing an average of less than 0.9 per cent. total copper with less than 0.8 per cent. in sulfide form and with no precious-metal values. There was then developed for this low-grade ore the system of separate large block-caving stopes, in lateral dimensions 150 by 300 ft., or 150 by 150 ft., with intervals between stopes of the same size so that subsequently these pillars may be similarly mined. The results have been most favorable. Under the previous system the production of ore per man-shift for all underground labor was 8 tons. The present production per man-shift underground is 28 tons. In starting this work the problems were: 1. How the ground would cave above the stopes. 2. Whether in the first stopes caving would encroach on the pillars as laid out. 3. Whether in subsequent mining of the pillars waste filling would be drawn from the previously caved adjacent stopes. Fig. 1 is a small key plan for showing the location of cross-sections as well as of ore mined and the limit of the escarpment and limit of cracking on the surface caused by the caving of the capping overlying the ore

Jan 1, 1929

By Robert Linton

Tats paper deals with work that has been carried on for over three years by the management and staff of the North Butte Mining Co. in an effort to standardize mining methods, to eliminate lost motion in the operating organization, and to improve the efficiency of the individual workman. Naturally, much of this work is an adaptation of ideas suggested by other mining operations or by practice in manufacturing and other productive industries. The studies, however, have developed some features that it is believed are new. Both new and adapted features are given in detail. The normal capacity of the North Butte mines is about 2000 tons per. day. Hoisting is done principally through the Granite Mountain shaft, which is 3740 ft. (1140 m.) deep and equipped with an electric hoist capable of hoisting 200 tons per hour from a depth of 4000 ft. (1219 m.). The lowest stoping level is the 3400-ft. The Granite Mountain shaft is connected with the Speculator shaft, about 850 ft. (259 m.) south, and with the Gem, about 1150 ft. (350 m.) east, which are 3000 (914.4 m.) and 2000 ft. (609.6 m.). deep, respectively. These two shafts are equipped with reversible fans for ventilation. The Speculator has a; steam hoist with a capacity of 150 tons per hour from the 3000-ft. level. The Granite Mountain shaft is concrete lined from the 1600-ft. to below the 3000-ft. level and gunited with cement from the 1600-ft. level to the surface. Sections of the Speculator shaft with a total combined length of 500 ft. (152.4 m.) are also concreted. There are approximately 36 miles (58 km.) of drifts and crosscuts in the mine, in which there are 15.2 miles (24.5 km.) of track. At normal capacity, about 75 stoping faces, 20 raises, and 30 sill development faces are working. Stoping is usually by the standard square-set method. Where the size of the oreshoot and character of. the walls permit, the rill (or cut-and-fill) system is employed.

Jan 8, 1920

By Rossiter W. Raymond

(Read at the Amenia Meeting, October, 1877.) IN the case of The Eureka Consolidated Mining Company v. The Richmond Mining Company of Nevada, recently tried at San Francisco, California, the real defendant was the Richmond Consolidated Mining Company, of London; but this being a foreign corporation, holds its mining property in Nevada through the Nevada corporation of similar name, in which the London Company owns all the stock, except the few shares necessary to "qualify" the American directors. The trial would naturally have taken place in the Circuit Court at Carson City, Nevada, and before a jury. But by stipulation of the parties, the case was tried in San Francisco, before Hon. Stephen J. Field, Justice of the Supreme Court of the United States, Hon. Lorenzo Sawyer, United States Circuit Judge of the Ninth Circuit, and Hon. E. W. Hillyer, United States District Judge, for the District of Nevada. The hearing began July 23d, 1877. The witnesses occupied two weeks, and the argument of. counsel three days. Very eminent lawyers were. engaged on both sides ; for the plaintiff, Messrs. Solomon Heydenfeldt, R. S. Mesick, John Garber, and H. J. Thornton ; for the defendant, Messrs. S. M. Wilson, Thomas Wren, and J. J. Williams. The court held the case under advisement until August 22d, when Mr. Justice Field delivered its unanimous opinion in favor of the plaintiff. The action was a complaint in ejectment, and an appeal was taken to the United States Supreme Court. The questions at issue between the Eureka and the Richmond Company in this suit, comprised several points in the construction of the mining law of the United States, and its relation to the customs and regulations of the mining districts, which possess an importance and an applicability far beyond the limits of the case in which they arose. It is my purpose to state these points, the arguments

Jan 1, 1878

By M. B. Mirza, F. D. Wright

Models of photoelastic material were made to simulate a mine roof that had cracked over the edge of the pillars and at the center of the span. Models were restrained from moving laterally outward so they acted as flat arches. Uniform loading was approximated by loading the models along the bottom at eight points spaced equally along the span. It was found that for models with depth to span ratios of 1:3 to 1:6, the maximum stress at the top of the center crack could be calculated directly by the following formula: Elastic stresses in mine roofs composed of sedimentary beds are usually computed by assuming that the immediate roof bed acts as a fully restrained beam uniformly loaded by its own weight and by overlying strata. Very little work has been done to analyze stresses in roof beds or beams which contain vertical (normal to the span) or nearly vertical cracks. Yet every mining engineer has walked safely under roofs that show such cracks. As far back as 1933, Bucky' made model studies of the effect of vertical cracks on the behavior of horizontal strata. He did not make any analysis of the stresses but did show that a cracked beam will stand safely under certain conditions, and also showed that a beam restrained at the ends can crack over the supports and in the middle without collapsing as long as the ends of the beam are not free to move laterally outward. The beam, or rather, part of the beam, acts like a flat arch and supports itself by pushing outward at its supports. In 1941 Evans2 treated analytically the problem of a beam cracked along so many planes perpendicular to the axis of the beam that no tensile stress can operate. He named this type of beam a "voussoir-beam" by analogy to the voussoir-arch. In 1962 ~a~cocks~ modified Evans's solution by including the effect of the shear stress component of the resultant force at the abutment. This paper gives the results of a photoelastic study of the stresses in a beam containing vertical cracks in the center of the span and over the supports. A

Jan 1, 1963

By Cyril Stanley Smith, Earl W. Palmer

A complete discussion of the literature on the subject of the influence of copper on iron and steel will be published elsewhere.' The present paper is concerned especially with the precipitation-hardening of copper steels, and brief mention will be made here only of the work of Kin-near,2,3 Nehl4 and Buchholtz and Koster,5 who alone have studied this phase of the subject. Kinnear found that normalized low-carbon steel castings containing about 1.0 per cent copper on drawing at temperatures in the neighborhood of 530" C. (1000" F.) increased in tensile strength and yield point, with little decrease in ductility. The maximum effect was obtained with about 0.9 to 1.0 per cent copper, and when the copper exceeded 3 per cent no improvement occurred on reheating. Kinnear did not study the effect of time of reheating—an all important factor where precipitation is concerned. Neh1,6 who apparently was unaware of Kinnear's work, recognized the change as due to precipitation and studied the interdependence of time and temperature of reheating, the temperature of the initial solution heat treatment, and the speed of cooling necessary to retain the bulk of the copper in supersaturated solution and to give an increase in hardness and tensile strength on reheating. Nehl found that if the final rolling or forging temperatures exceeded 700" C. (1300" F.) it was not necessary even to normalize the steel, but full precipitation occurred on merely reheating the forged or rolled shapes at 500" C. (930" F.). Buchholtz and Koster7 studied in detail the precipitation-hardening of a mild steel containing 1.0 per cent copper and 0.5 per cent chromium. From data on the electrical and magnetic properties of copper steels, they drew the portion of the equilibrium diagram in Fig. 1, assuming the

Jan 1, 1933

By N. R. Tipman, G. E. Agar, L. Paré

The flotation chemistry of the commercial INCO matte separation process was investigated. The slow cooling of Bessemer converter matte forms discrete phases of Cu2S and Ni3S2 and a Cu-Ni alloy. After magnetically removing the alloy, the Cu2S and Ni3S2 are separated by flotation at pH 12.4 (saturated lime) using diphenyl guanidine (DPG) as both collector and frother. DPG has been used exclusively in this flotation process because of its unusual selectivity for copper minerals. The surface product resulting from chemisorption of DPG onto theCu2S was identified as the double salt CU(DPG)2SO4.CU(DPG)2(OH)2. The adsorption followed Langmuir behaviour up to a monolayer coverage. In the absence of DPG, the rapid adsorption of oxygen by Cu2S in flotation pulps was observed. The surface product was identified as the insoluble basic copper sulfate CuS04.3Cu(0H)2 with the production of sulfate ion. In the presence of DPG, the oxidation reaction appears to be suppressed. The frothing properties of DPG and commercial frothers were compared. DPG is not a powerful frother. Batch flotation tests confirmed that DPG is a highly selective collector when compared to most sulfhydryl collectors.

Jan 1, 1976

By D. Cox, M. J. Duggin, L. Zwell

The carbides of approximate composition and Mn have been studied using X-ray diffraction techniques. Those carbides of the type (Fe,Aln)zC ave isostructural with cementite. The cell pararmeters a and c have minimum values at approximately 10 at. pd substitution of manganese for iron; no satisfactory explanation has yet been found for this phenomenon. The carbide fFeMn4)C has a monoclinic unit cell whose dimensions are close to those of ,11,15Cz A neu-troip-dij~ractiot~ study of (F'eAlrz4)C~ reveals that, like MnsCZ, it is isostructural with Pd5Bz. The iron and manganese atoms occupy the palladium atom sites, while the carbon atoms were found to have the same atomic coordinates as the hovon atoms. A neutrorr-diffraction study of indicates that the carbon-atom positions are very close to those occupied in (Fez.,ll/lr~,.3)C. In both carbides studied, tlre iron and manganese atomzs were found to be essentially randomly distributed, although, in the case of (Fe,.811fn1.2)C, it is possible that there may be a slight preference of manganese atoms for- the general (d) positions and a corresponding slight preference of iron atoms for the special (c) positions. It has been found that a complete range of solid solution exists between Fe3C and Mn3C at 1050°C,I although Mn3C becomes unstable when the temperature is reduced to 95O0C,' and can only be retained by rapid quenching. It is also known that a complete range of solid solution exists from Fe5Cz to M~SC~,~ although the stability range of carbides of the type (Fe,Mn)sCz as a function of the relative proportions of iron and manganese is not known. X-ray examinations of Oh-man's carbide3 and Spiegeleisenkristall,~ which have the approximate compositions (Fe3.67Mnl.33)C2 and (Fe3-,Mn,)C, where x lies between 0.4 and 1, respectively, have been made. The following carbides have also been studied: ] The lattice parameters determined during these investigations are listed in Table I. It is seen that carbides of the type (Fe,Mn)sCz have a monoclinic unit cell while carbides of the type (Fe,Mn)3C have an orthorhombic unit cell. It is evident that the variation of lattice parameters with manganese content is not linear for carbides of the type (Fe,Mn)3C. The coordinates of the atoms in (Fe2.7Mno.3)C have recently been determined by single-crystal analysis., The fractional atomic coordinates have been shown by Fasiska and jeffrey to be in good agreement withj those deduced from an earlier analysis of Fe3C by Lipson and etch.' However, it was impossible to determine whether iron and manganese atoms occupied ordered positions because of the small difference between the atomic scattering factors of iron and manganese. The atomic positions in Mn5Cz (Refs. 8 and 9) and Fe5C2 (Refs. 7 and 8) have been obtained only by comparisons made with the isostructural compounds P~SB~.' Since X-ray diffraction techniques were used in these investigations, accurate positioning of the carbon atoms, which have a low atomic scattering factor, was difficult. No attempt has been made to determine the atomic positions in the other carbides previously studied. It was felt that an investigation of the lattice parameters of a number of intermediate carbides of the types (Fe,Mn)sCZ and (Fe,Mn)& would be of interest. It seemed likely that a neutron-diffract ion study of such carbides would indicate whether ordering occurred between the iron and manganese atoms because of the large difference between the neutron-scattering cross sections of iron and manganese. It also seemed probable that such an investigation would provide a determination of the atomic coordinates of the carbon atoms. I) EXPERIMENTAL DETAILS Specimens, each weighing approximately 20 g, were carefully prepared according to the following proportions: The components were 500-mesh powders of 99.995 pct purity iron and spectroscopically pure carbon and a 200-mesh powder of 99.995 pct purity manganese. The component powders were intimately mixed by prolonged shaking, then each specimen was inserted into a spot-welded cylindrical container of tantalum foil, whose end was closed but not sealed. Each specimen in its envelope was then sintered at 1050° C for 24 hr in a thin-walled evacuated quartz capsule, such a time having been previously found sufficient for equilibrium to be attained.' Each specimen was then quenched in order to attempt to retain the high-temperature phase, as the literature indicates that transformations may occur on cooling. Debye-Scherrer X-ray photographs were taken of each specimen using a 114.6-mm-diam camera, Fig. 1, patterns 2 to 6. The exposure time was 6 hr using filtered iron radiation at a tube voltage of 40 kv and a tube current of 12 ma.

Jan 1, 1967

By Henry C. Freeman

During the early period of the construction of the Illinois and Michigan Canal, about 1838, in excavating for the canal, where the present town of Utica stands, hydraulic limestone was discovered, and its value was recognized. A kiln for calcining and a mill for grinding were erected, and the cement was used in the construction of the locks of the canal. This property was subsequently bought by the present owner, Mr. James Clark, and the work has been continued to the present time in much the same primitive manner as it was begun. The bed is exposed in the Illinois River valley by stripping off a few feet of the covering rock. It is from 4 feet to 6 feet 9 inches thick, and nearly level, dipping gently to the northeast. The Utica Cement Company's establishment, which is two miles west of Utica and two miles east of La Salle, was an outgrowth of the Illinois geological survey. The writer was in charge of the district which included La Salle county, and, in working out the details of the geology of that county, discovered, below the Utica bed, another workable hydraulic limestone, which makes its appearance in the northern bluff of the Illinois River valley, rising above the water level at the point where the company's works are established. This cement group, of which there are several thin beds, lies just below the St. Peter's sandstone, with a few feet intermediate of transition-rock, which appears to represent the Calciferous, and is exhibited in place, in concretionary form, at the top of the bluff. The hydraulic beds are very regular, and the one worked by the company is 10 feet thick; or, speaking more definitely, there are two beds, separated by 18 inches of sandstone, lying about two feet above the bottom, and the two beds are worked as one, the sandstone being first cut out and removed, to prevent mixture. In 1869 I was invited to join with a company, and to take charge

Jan 1, 1885

By Richard Hunt

BINGHAM has produced 6 per cent. of this country's copper. In total production, it ranks fourth among the copper camps of North America, the order being Butte, Michigan, Bisbee, and Bingham. In its annual production, it held that same rank until 1919, when its production was exceeded by the combined production of the Globe-Miami district of Arizona. Bingham has also been a lead camp of the first order. Utah ranks third among the lead-producing states, and its production comes largely from three camps which, in the order of their productivity, are: Bingham, Tintic, Park City. Bingham's silver production is important, but it does not rank high as a silver producer. Utah owes its rank as first among the silver-producing states to Tintic, a camp 40 miles due south of Bingham. The United States Mineral Resources reports a total production from Bingham for the period 1865-1920 having a gross value of $528,043,432. Bingham is on the eastern flank of the Oquirrh range 30 miles south-west of Salt Lake City, from which it can be reached in an hour by auto, or by the Denver & Rio Grande or the Bingham & Garfield railroads.. The automobile route is a paved road across the floor of Great Salt Lake Valley, through farming country. The Bingham & Garfield railway leaves the level of Great Salt Lake at the northern end of the Oquirrh range, and in 20 miles it climbs 2100 ft., and deposits the traveler upon a shelf cut in the side of Bingham Canyon below most of the mines, which are farther up Bingham Canyon and its tributary Carr Fork. Below lies the town, a narrow ribbon running for a couple of miles along the bottom of a canyon 2000 ft. deep-an almost impossible site for a community numbering, in prosperous times, 5000 to 7000 inhabitants drawn from all quarters of the globe. Up the canyon and down, and beneath the steep slopes nearby, and beneath the town itself, are the mining operations of over half a century.

Jan 3, 1924

R. F. McELVENNY.- The next item is: "Center and other methods, vs. side charging." That was all discussed in the Carson case, and I do not know but what many of the plants are still using center charging. Some are using side charging. Did I understand that where you use the wet charge it is all side charging on the wet ore? B.-G. C. HONEYMAN.- We were on center charging for about a year with wet ore. R. F. McELVENNY.- Then you went to side charging. Has anyone any remarks to make on side versus center charging? E. A. BARNARD.- We have one side and one center, both on deep bath. It is an experimental proposition so far, but the side charge looks very favorable.. R. F. McELVENNY.- This is with calcine? E. A. BARNARD.- This is with calcine on a floating charge proposition.. They are both water jacket. The charge acts very similar on both center and side charging. The calcine spreads much the same as it does on the center charge. It will run down 75 ft. on the furnace side as well as the center. The advantage is in taking care of secondaries and things of that nature. C. BARDWELL.- Do you get any side wall protection from it? E. A. BARNARD.- No. R. F. McKENZIE.- Do you not project the side wall up to protect the skewback? E. A. BARNARD.- There is a slot projection down around the top of the bath; but the repairs on the side wall have been practically the same; that is, they, have been practically the same as they have on the center charge. A. H. RICHARDS.- A point I would like to make is that if you have any doubt about the center charging, we feel that we get better tonnages and lower fuel ratios and better slags with center charging than we ever got with side. Different kinds of charges would, of course, vary, and I could readily see that if you had the same advantage with deep bath smelting that you mention you would probably get just as good a slag and as good fuel ratios. E. A. BARNARD.- In fact, I think the calcine charge spreads more on the side than on the center charge. A. H. RICHARDS.- If you maintain a deep bath. E. A. BARNARD.- That is one thing we have to be careful about, to hold the charge back.

Jan 1, 1930