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Unfortunate occurrences resulting in injuries, loss of life, and destruction of property by explosion, fire, and other mishaps during shaft sinking focused the attention of the Bureau of Mines on the need for safety standards For such operations. Information Circular 7810 was published to meet that need. The current revision updates and replaces IC 7810. Several States have some rules and regulations applicable to local conditions, and several Bureau publications (including some now out of print) cover the hazards that may be encountered in shaft sinking. Certain requirements of the Federal Mine Safety Code and Federal Coal Mine Safety Act may be applied, but there are no definite, uniform standards that will guide those desiring to sink a shaft safely and bring about uniform safety inspections.

Jan 1, 1968

By O. B. Bucklen, P. G. Meikle

INTRODUCTION The trend in the coal industry for many years has been to make every- thing "bigger and faster." This also held true for loading and storage facilities. Where once a million ton per year mine was rare, three to five million ton per year mines are not uncommon today in the bituminous industry. This greatly increased production, made possible through mechanization, required greatly improved loading facilities just to get the coal away from the mine. Also, there is a trend toward combining production from more than one mine and cleaning it in a single preparation plant. In addition to increased loading capacity, this frequently necessitates raw coal storage and blending facilities. The development of the unit train with its attendant economics, more than any other factor, has contributed to the widespread construction of storage and high-speed loading facilities. In the export market, the construction of ever larger coal colliers has contributed to a need for faster and larger loading facilities. In this climate of rapidly changing technology, any written account is faced with the possibility of obsolescence before its appearance. Thus, this chapter seeks to define the common and current practice in coal loading and storage facilities with the full knowledge that this practice is an ever-moving target. FUNDAMENTALS OF COAL STORAGE Storage of coal is becoming an increasingly important part of coal handling systems at mines, particularly since the advent of the unit train concept in transportation. In order to take advantage of reduced transportation rates on trainload shipments of coal offered by unit train movement, operators have found that storage is an economic necessity. In unit train practice large predetermined quantities must be loaded in relatively short periods of time as opposed to conventional practice where coal is loaded at a speed dependent on the production capacity of the mine and/or the cleaning capacity of the preparation plant. Two surveys of storage practices at mines reveal several objectives for storage.1, 2 Raw and/or clean coal storage is generally practiced in order to accomplish one, or a combination, of the following objectives: 1. To improve plant efficiency by distributing plant feed over the entire operating time, or to allow a preparation rate different from the production rate. 2. To limit interruptions of supply, ie, allow mine and plant to function independently with delays in one not affecting the operation of the other.

Jan 1, 1968

By Frederick C. Moore

This paper describes the original planning which actually resulted in the opening of a new aggregate plant located in central New York State. This plant, which is now named the Skaneateles Plant of The General Crushed Stone Company is unique in that the plant itself is a departure not only in design but in concept of operation from the normal aggregate plant the company has operated in the past. Whether or not the concepts which resulted in the Skaneateles Plant are economically feasible remain to be proven by the next few years of operation. By way of background data about our company which will help set the stage for this presentation, we currently operate seventeen stone quarries in the states of New York, Pennsylvania and Virginia. These quarries range in size from 200,000 tons per year to 1,500,000 tons per year with a total annual stone production of approximately 7,500,000 tons. We also produce about 1,250,000 tons of sand and gravel at six sand and gravel plants, 300,000 cubic yards of ready mix concrete, 1,500,000 tons of bituminous concrete, aglime and other minor construction materials. In many cases we are our own best customer consuming a large percentage of the total production of our own aggregates in our various ready mix and blacktop plants. Up to the concept of the Skaneateles Plant our operating facilities have been of the permanent type as opposed to the moveable or portable type plant. The steps involved in the case history of Skaneateles will begin with the basic economic requirements, market research, geologic surveys, land acquisition, zoning and financing and carry through to the final design and construction. We will attempt to show what some of the problems were, how we interpretted them and how we proceeded to solve them. The current results are apparent and can be analysed. The success of the total concepts of the Skaneateles Plant remains for future analysis.

Jan 1, 1968

By C. D. Thurmond

Jan 1, 1968

By M. J. Blackburn

The ordering reaction and its effect on dislocation awangements in alloys based on Mg3Cd has been studied by transmission electron microscopy. Ordering occurs by the growth of ordered domains until they impinge, thus producing an antiphase domain boundary (APB) network. In the disordered alloy, slip is confined to the basal plane while in the ordered condition slip occurs on the basal, prism, and pyramidal planes. Superdislocations have been identuied on these planes and their origin and expected spacings are discussed and compared with the observations. The APBs between the dislocation pairs have been resolved and have proved useful in the identification of superdislocations. Observed slip structures are related to the changes in mechanical properties produced by ordering. At high temperatures magnesium and cadmium form a continuous series of disordered hexagonal solid solutions. At lower temperatures three ordering reactions occur; two based on the compositions Mg3Cd and MgCd3 are transformations to DO19-type superlattices while alloys based on the composition MgCd transform to a B19 lattice. The ordering process in alloys near the composition Mg3Cd has been studied by several workers'-4 and it has been shown to be a first-order type transformation. The variation of mechanical properties with the degree of order and temperature have been reported in some detail by Stoloff and Davies.5 It was shown that the disordered alloy was stronger and less ductile than the ordered alloy, the differences being attributed to changes in the number of active slip planes and to the presence of short-range order in the disordered alloy. In this investigation the ordering reaction has been qualitatively followed by transmission electron microscopy. The effect of this ordering transformation on the dislocation arrangements in deformed specimens has been studied in some detail. EXPERIMENTAL Alloys were melted in a stainless-steel crucible under a flux and chill cast; both melting and casting were performed in an argon atmosphere. The ingots were hot-rolled and tensile specimens cut from the resultant strips. Some large-grained specimens were grown by the strain-anneal method. Heat treatment was carried out in inert atmosphere furnaces and in oil baths at the lower temperatures. Thin foils for transmission electron microscopy were produced by electropolishing in a cooled solution (temp = -40°C) containing 50 cu cm of nitric acid and 180 cu cm of methanol at a potential of 10 v. The ordering reaction was followed by transmission electron microscopy, X-ray, and electrical resistivity measurements but this paper will be concerned chiefly with the electron-microscopy results. Much of the work described in this paper was performed on an alloy containing 26.10 at. pct Cd although two of the micrographs are taken from work on a 25.55 at. pct Cd alloy. RESULTS i) The Quenched Solid Solution. Specimens which were quenched from above the critical temperature showed diffuse superlattice reflections. sark-field analysis on these reflections failed to reveal the presence of ordered domains and thus the superlattice reflections were assumed to arise from regions of short-range order. Quenching from temperatures of 400" to 450°C results in the formation of dislocation loops and helical dislocations. Such defects have been observed and analyzed in detail in several hexagonal metals6-' and as the crystallography and interactions of such loops appear similar in this alloy they will not be reported in detail. Fig. 1 shows a high density of loops

Jan 1, 1968

By John A. Emery

The Pea Ridge iron ore deposit near Sullivan, Missouri, is a dike-like mass of magnetite enclosed in Precambrian porphyries. The ore body tops at the Precambrian surface at a depth of 1300 feet below the present surface and extends to an unknown depth. It dips nearly vertically, intersecting the dip and strike of the enclosing porphyries at an extremely sharp angle. Faulting, both pre- and post-ore, appears to be of minor consequence, and present knowledge indicates that no preferred structural conditions existed prior to emplacement. The ore body is composed of magnetite with specular hematite, quartz, apatite, and pyrite occurring as accessory primary minerals. Specular hematite in appreciable quantities occurs on parts of the cap and the footwall of the ore body. Fresh porphyry breccia is enclosed in the magnetite along the hanging wall and in the western portion of the ore body. Hanging-wall quartz-amphibole and footwall quartz-hematite occur as replacements of certain porphyries. Further alteration has caused sericitization of parts of these zones. The ore deposit is interpreted as having been formed essentially by a single injection of a magmatic differentiate with hydrothermal end phases forming the quartz-amphibole and quartz-hematite portions of the deposit.

Jan 1, 1968

By R. K. Ham, M. L. Wayman

TD-Nickel has been broken in tension and in fatigue at voom temperature. Rod specimens failed in tension by necking, with axial cracks attributed to voids elongated in the extrusion direction. Fatigue specimens failed in shear. Thin-film electron microscopy showed that the subgrain structure of TD-Nickel was very stable, and that particle-matrix detachment was very difficult, in tension and fatigue. TD-Nickel softened slightly during fatigue but had a high fatigue ratio (0.5at 10' cycles). Fractography suggested that Stage I fatigue crack propagation is greatly extended in TD-Nickel. Td-NICKEL* is a dispersion of 2 pct by volume of thoria (ThO2) in nickel, produced by powder-metallurgical methods including compaction, sintering, and extrusion. The spherical thoria particles, which may have a mean diameter of a few hundred angstroms, are dispersed with a mean planar spacing of a few thousand angstroms. By a combination of cold working and annealing, a subgrain or cell structure of dislocations intimately associated with the dispersion can be produced.' This gives the material useful tensile properties which are extremely resistant to exposure to high temperatures.'-= At the same time, the material shows considerable ductility.3'4 At the beginning of the present work, it was considered of great interest to investigate the mechanical stability of TD-Nickel under conditions of fatigue. On the one hand, materials which derive strength from a cold-worked structure are unstable in that they are susceptible to fatigue softening: in addition, the presence of discontinuities such as the particle-matrix interfaces might be expected to assist in the initiation and propagation of fatigue cracks, in that they may provide local concentrations of internal stress and sites for the initiation of voids." On the other hand, the substantial ductility of TD-Nickel suggests that if it obeys Coffin's relation8 (or the more refined form proposed by Manson9) it should have good fatigue resistance. The initial purpose of this investigation was to assess the importance of these factors. Also, relatively little fundamental work has been done on the mechanism of fatigue in dispersion-strengthened materials. Work on overaged A1-4 pct CU10-12 revealed a very large Bauschinger effect indicative of internal stresses at the particles, and very great fatigue hardening1' presumably due to the multiple slip stimulated by these internal stresses, followed by softening which was initially due to softening in the matrix, but later might have arisen from cracking at the particle-matrix interfaces. The study of overaged Al-4 pct Cu could not settle this latter point by the electron microscopy of thin films, since the dispersion is too coarse. A previous study of the fatigue of internally oxidized copper13 was complicated by inter granular failure, attributed to oxide particles at grain bouhdaries; internal oxidation of single crystals, however, improved their fatigue properties.'3 Investigations of SAP (sintered aluminum powder) are complicated by the complex particle shapes, and the possibility of continuous internal oxide films.14 It was hoped to avoid these difficulties with TD-Nickel, which had the further advantages that it was commercially available and suitable for study by the thin-film technique. 1) MATERIALS AND EXPERIMENTAL PROCEDURE TD-Nickel was purchased from the Driver-Harris Co. as 3/9-in.-diam rod which had been extruded, swaged, and "stress-relieved" (normally at 1010°C for 1 hr). Continuous-radius fatigue specimens with a minimum diameter of -0.1 in. were ground to shape and electropolished in 40 pct phosphoric, 35 pct sul-furic, 25 pct water at 25oC, with a stainless-steel cathode, at -6 v. Fatigue tests were carried out at room temperature with a Sonntag SF-1-U machine operating in push-pull at 1800 cycles per min, and in an Instron TT-C-L modified for reversed stressing at 26 cycles per min as described elsewhere.10 Round tensile specimens were ground with 0.85-in. gage lengths of 0.135 in, diam, electropolished, and tested in a Tinius Olsen hydraulic machine. The surfaces of fatigue specimens were examined with a Reichert metallograph. Discs for electron microscopy with a Siemens Elmiskop I were spark-cut 0.01 in. thick with a modified Servomet 11 employing a tool of moving molybdenum wire, cleaned in 50 pct acetic, 30 pct nitric, 10 pct phosphoric, and 10pctsul-furic at 85oC, and thinned by the window method in the electropolishing solution at -20°C and -6 v. Two-stage replicas (parlodion, then Pt-50 pct C self-shadowed at 40 deg) were taken from fatigue fracture surfaces for electron microscopy. Plane sections parallel to the specimen axis and containing the direction of fatigue crack propagation were polished, etched with Carapella's reagent, and examined optically. Transmission Laue X-ray photographs of as-received material electropolished to a point were used to determine preferred orientation. 2) RESULTS 2.1) The Structure of As-Received Material. Grains -1 µ diam and elongated 20 to 30 u in the direction of the rod axis were observed, With' elongated "intergran-ular" voids (-4 p diam and -90 µ long and identified as such using longitudinal and transverse sections and

Jan 1, 1968

By A. J. Ardell, O. D. Sherby

The elevated-temperature steady-state creep behavior of polycrystalline a Zr was studied in vacuo under constant tensile stress. The experiments were conducted from 660° to 845°C over the stress range 870 to 5400 psi. The steady-state creep rate, is, of a Zr was found to be related to the applied stress, a, and temperature, T, by the equation where C is a constant. Two interpretations of the data are considered, each requiring different values of the parameters ß, Q, and . It is shown that this formula can be derived using Gilman's phenomeno logical equation relating dislocation velocity to the shear stress for the case where dislocation mobility is limited by the nucleation of kink motion. From the fundamental dependence of strain rate on dislocation velocity and the density of mobile dislocations, the factor exp(ßo) can be related to the stress dependence of the dislocation density, and Q to the energy of kink formation. The two interpretations considered are as follows: Case I—the parameters are adjusted so that the equation above describes the data over the entire range of stress and temperature, implying that creep is controlled exclusively by dislocation glide; Case IIthe parameters are adjusted to allow for the possibility that creep is diffusion-controlled at high stresses but glide-controlled at low stresses. For both cases the values of the parameters are within the spread permitted by the data. Factors favorable to the observation of the unusual stress -dependence of i, for a Zr are discussed and it is shown that the anomalously rapid rates of self-diffusion and the low modulus on the principal glide system are primarily responsible for the anomalous creep behavior. Metal-lograflhic observations are presented and discussed with reference to the overall creep behavior. PREVIOUS investigations of the creep behavior of a Zr have been conducted from room temperature to about 500C The results of these investigations are primarily of engineering significance because of the variety of conditions under which they were carried out, and the low testing temperatures employed. Little information is available concerning the fundamental nature of the elevated-temperature creep behavior of a Zr. This investigation of the creep behavior of a Zr above half the melting temperature (the melting temperature, T,, of a Zr is estimated to be about 1860"K was initiated because there are two significant anomalies of the physical properties of a Zr: a) the rate of self-diffusion in polycrystalline a Zr is anomalously rapid: b) both Young's modulus for polycrystalline a Zr and the shear modylus as-sociated with the prismatic slip system { 1010)( 1120) (the principal slip system in a Zr 7) have anomalously large temperature variations The importance of these quantities to the understanding of creep behavior has been demonstrated, and it was hoped that this investigation would provide a critical test of the predictions based upon the analysis of creep data for other pure metals. However, as the investigation progressed it became increasingly clear that the unusual creep behavior of a Zr could not be analyzed in a conventional manner. 1) EXPERIMENTAL EQUIPMENT AND PROCEDURES Two grades of zirconium, designated A and B, were used in this investigation. The analyses, as supplied by the vendors, are presented in Table I. Material A, with a nominal purity of 99.84 pct, was supplied by the Wah Chang Corp. in the form of cold-rolled sheet from which specimens were machined without further fabrication. Material B, with a nominal purity of 99.95 pct, was purchased from the Nuclear Materials and Equipment Corp. in the form of iodide crystal bar.

Jan 1, 1968

By J. M. Woodall

GuAs crystals which have been grown in quartz boats by the horizontal Bridgman method in the pvesence of Ga20 vapov have beetz found to have carrier and donor distributions which do not correspound to those expected from simple dopant seg-vegation during directional freezing; Instead, the carrier distribution is determined by the heat-trentnzent history of the crystal, while the donor distribution, zohiclz is principally due to silicon, is fixed by the pozuth rate, the geo)tlet.ry of the crystal growth vessel, and tlze initial Ga20 pressure. WHEN semiconducting materials are made into doped crystals by the normal freezing method,&apos; they usually exhibit doping variations along the growth axis. If a) there is no dopant diffusion in the solid, b) the dopant is distributed uniformly in the melt, and c) the distribution coefficient, k, does not vary with composition, then the doping variation along the growth axis is represented by the equation: where C is the doping level in the solid at a point where a fraction g of the original liquid has frozen, and Co is the mean concentration. When the dopant is either a singly ionized shallow donor or shallow acceptor, C also represents the carrier concentration. Even though this equation accurately describes the dcping profiles of a large number of normal freeze systems, there are several special systems for which Eq. [I] does not apply. One such system is the horizontal Bridgman method for preparing oxygen-grown GaAs crystals using quartz vessels. Several workers2"* have shown that GaAs crystals grown by the horizontal Bridglnan method using quartz vessels are generally contaminated with silicon in concentrations in excess of 5 < 10lG atoms per cu cm. This contamination is ascribed to a reaction: occurring at the walls of the crystal-growth vessel which liberates silicon into the melt and Ga2O vapor. It has been shown4 that this reaction, and, hence, the silicon contamination, can be suppressed by the addition of oxygen to the crystal-growth apparatus. It is the purpose of this paper to describe a special apparatus capable of yielding single crystals of GaAs grown in the presence of oxygen and to describe both the kinetics of silicon suppression in this system and the relationship between the carrier concentration profile and the silicon concentration profile. EXPERIMENTAL-CRYSTAL GROWTH A schematic diagram of the apparatus used in the oxygen addition experiments is shown in Fig. 1. The most important features of this apparatus are: a) the use of a sand blasted quartz boat, h) a quartz rod of length 1, with a hole of cross section A, that is placed near the boat to limit the free space volume V, over the melt during the growth, and c) the temperature gradient at and near the solid-liquid interface. Sand blasting the boat is necessary to prevent wetting of the melt. The quartz rod retards the diffusion of the GazO vapor away from the melt to the colder portions of the ampoule. A crystal is prepared by first loading a 5.5-in. boat, which has been cleaned in aqua regia, with 40 g of 99.9999 pct Ga along with 1 to 8 mg of Ga203 powder. GazO3 is a convenient source of oxygen since it reacts with gallium at the melt temperature to form Ga20 vapor, the species which apparently controls the suppression of silicon contamination. The loaded boat, the quartz rod, and the 99.9999 pct As are placed in the ampoule as shown in Fig. 1. Generally, GaAs seeds were not used since most of the unseeded growths resulted in monocrys-tals. The ampoule is evacuated to 10-5 Torr and sealed off. The GaAs melt is synthesized by placing the ampoule into a two-zone horizontal Bridgman furnace. The two zones are separated by several sandwiched layers of -in. Fibre-Fax board drilled with holes slightly larger than the OD of the ampoule. This causes a very large temperature gradient between the two zones, which is necessary for single-crystal growth. The two-zone furnace is mounted on a stand fitted with a roller bearing which allows uniform motion of the furnace in a horizontal direction. A uniform velocity of the stand is achieved by the use of a windlass device which winds up a wire attached to the stand. Movement of the solid-liquid interface is accomplished by fixing the position of the ampoule and moving the stand. Growth rates investigated in this experiment were between 0.4 and 1.2 in. per hr. The composition of the melt is fixed by maintaining an arsenic reservoir at 618°C. The stand is moved away

Jan 1, 1968

By H. E. Cline

Solidification of Pb-Sn alloys ranging in composition from 1.2 to 56 at. pct Pb ws observed with polarized light. Lamellar structures were observed over a larger range of compositions in alloys containing excess tin than excess lead, as expected from constitutional supercooling. The occurrence of pools of supercooled liquid surrounded by lead is explained by the difficulty in nucleating tin. Cells and dendrites weve observed in tin-rich alloys. Evidence was found that the degenerate structure formed at low growth rates, the formation of faults, and abrupt changes in composition and structure can be attributed to non-steady-state growth. The apparent interface shape was observed to have deep grooves at the interphase boundaries. HUNT and Jackson have observed the shape of the interface during growth of organic eutectics. They observed the formation of lamellar faults and shape instabilities upon changes in growth rate. The lamellar structure in these organic eutectics was not restricted to the eutectic composition. Recent work by Mollard and Flemings2 indicated that Pb-Sn alloys from 12 to 26 at. pct Pb could be solidified with a lamellar or rodlike structure if a sufficiently steep temperature gradient was used at a slow growth rate. Observations of the solid liquid interface of the Pb-Sn eutectic were made by Davies3 using polarized light. Photographs were at too low a magnification to determine the interface shape, but he has concluded that tin was the leading phase. In the following experiments, solidification of a range of Pb-Sn alloys from 1.2 to 56 at. pct Pb was observed using polarized light, to determine the factors controlling stability of the lamellar structure. EXPERIMENTAL Procedure. One hundred-gram ingots of alloys prepared from 99.999 pct pure Pb and Sn were cast into graphite molds under argon. The compositions of the alloys were 1.2, 6, 12, 26, 36, 46, and 56 at. pct Pb. Two-gram pieces were melted between two cover glass slides which were squeezed into a 1-mm separation. Samples were then observed under polarized light in a hot stage shown in Fig. 1. A long working distance objective designed for viewing at 500 times was used. Photography was made difficult by the lack of illumination and contrast at these high magnifications. By using an elliptical polarization compensator, as suggested by A. Holik, the contrast and illumination could be optimized. Photographs could be taken only at slow growth rates to avoid excessive interface motion during the 15-sec exposure used. The solidification rate was varied by increasing or decreasing the power to the heater. It was found that insulation was necessary to avoid undesired growth rate fluctuations. The temperature gradient, as measured with two thermocouples 1 cm apart, was 80" ± 20°C per cm during all the experiments reported here. The advantage of this procedure is in being able to observe solidification while it is occurring. However, the observations are restricted to the glass-metal surface and may be influenced by this surface. Also, one has no knowledge of the interior of the sample, in contrast to studies of the freezing of transparent organic eutectics.&apos; Observations. The alloy near the eutectic composition (26 at. pct Pb) solidified in a lamellar structure when the growth rate was uniform. If the growth

Jan 1, 1968

By Wesley T. Holmes

This report describes the first phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected slag compositions in the titania-alumina-silica-calcia-magnesia system. Both the melting-holding-quenching method and the hot-stage microscope method were used in the tests. Liquidus temperatures of slags studied ranged from 1,217° to 1,667° C. The lowest liquidus temperature of the slags occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. Liquidus temperatures were also lowered when Si02 was substituted for Ti02 plus Al2O3 when CaO and MgO levels were held constant. Improved methods for the measurement of liquidus temperatures on very small samples are described.

Jan 1, 1968

By John T. Eastlick

The Banner mining district is about 70 miles northeast of Tucson in the southern part of Gila County, Arizona. Production from the district, valued at about $26 million, is chiefly from copper-silver-lead zinc ores. The stratigraphic section consists of Precambrian conglomerates, quartzites, dolomites, and limestones, Cambrian quartzites; Devonian limestones; dolomites, and shales; Mississippian limestones; Pennsylvanian limestones and shales; and Cretaceous volcanic and sedimentary rocks. Deformation of these rocks presumably started near the end of the Cretaceous, and extended into the late Tertiary. The sedimentary rocks were folded, faulted, and intruded by fine grained diorite, quartz mica diorite, and dacite porphyry. At least four distinct stages of mineralization are recognized. In the first stage of contact metamorphism and the second stage of hydrothermal alteration, favorable zones were prepared for ore deposition. Metallization occurred in three of the mineralizing stages. Magnetite, pyrite, and hematite were deposited near the end of the second stage of hydrothermal alteration. The third stage included the main deposition of sphalerite, chalcopyrite, bornite, and galena. In the fourth and final stage, minor amounts of sulfide minerals were deposited with a late anhydrite and quartz gangue. The ore deposits in the form of veins and veinlets, pipes, irregular massive replacements, and bedded replacements are localized by the extent and distribution of metamorphic and hydrothermal alteration, by the proximity to the intrusive contacts, and by the effects of structural development. Oxidized ores of copper, lead, and zinc constituted the principal production of the district prior to 1940, but, for the most part, supergene enrichment was of minor economic importance. The ore bodies of the district are in the mesothermal class of deposits, occurring as normal metasomatic replacement and vein types.

Jan 1, 1968

By I. H. Warren, F. A. Forward, A. Vizsolyi

"Observations are reported on the pressure leaching of material produced by subjecting chalcopyrite to two types of heat treatment. Calcination of the mineral at 825°C, in the absence of oxygen, induces some sulphur loss by volatization, producing a material from which copper can be leached more rapidly than from chalcopyrite. Treatment of the mineral with elemental sulphur at 475°C leads to sulphur uptake accompanied by a change in mineralogical structure of the chalcopyrite. Copper is prefer-entially and rapidly leached from the sulphur-treated material. A tentative explanation of the sulphur-chalcopyrite re-action is presented."

Jan 1, 1968

Jan 1, 1968

By A. F. Giamei, E. J. Freise

A discussion of the various factors affecting the accuracy of volume fraction determination by the direct comparison X-ray diffraction method is presented. To minimize errors introduced by nonrandomization effects such as preferred orientation and large grain size, as well as errors introduced by statistical effects, an iterative mathematical analysis is introduced. This analysis is applied to all observable diffractio~ spectra from a given specimen by means of computer techniques and is statistically superior to the standard direct comparison technique which utilizes only one or tm sets of intensity spectra. The computer program also presents a graphical interpretation of- the results which enables the investigator to visualize and readily assess the scatter in volume fraction estimates caused by deviations from randomness. Finally, the iterative analysis is applied to experimental data collected from a series of plain carbon steels in both the as-received and spheroidized conditions to determine the volume fraction of cemen-tite present in each case. The results show markedly good agreement with chemical analyses for all spheroidized specimens. In theory, quantitative X-ray diffraction is a power-ful analytical technique for precise determination of the volume fractions of various phases present in a multiphase poly crystalline aggregate. There are two generally used methods; both utilize the fact that the intensity of a diffraction line of a particular phase is a function of volume fraction of that phase present in the aggregate. The more common method is the so-called internal standard technique where a known amount of standard substance is mixed with the aggregate containing the unknown. The resulting ratio of the intensity of a particular diffraction line of the unknown to the intensity of a diffraction line from the standard is used to find the weight fraction of unknown material by reference to the intensity data obtained from a previously prepared set of standards containing the same amount of standard material. The details of this technique are outlined in standard works on X-ray diffraction.&apos; The disadvantages of the technique are that it requires the use of powder specimens and that the powder mixture must be homogeneous near the surface to the maximum effective beam depth. The alternative technique is the direct comparison method in which the ratio of the intensity of a diffraction line of a phase in the aggregate to the intensity of a second-phase diffraction line yields the ratio of the volume fractions of each phase present. This method has been applied most extensively to the determination of the percentage of retained austenite in martensitic steels and to determining the amounts of hcp and fcc allotropic modifications in pure cobalt5 and the amounts of hexagonal and rhombohedra1 modifications in graphite.8 This method is applicable to bulk as well as powder aggregates and is the technique which will be considered in the following text. It is the purpose of the present communication to show that by combining the results of X-ray diffrac-tometry with the use of high-speed digital computers the results of the direct comparison quantitative X-ray analysis technique can be optimized by using all of the data available on a diffraction pattern. THEORETICAL DISCUSSION In optimizing any quantitative X-ray diffraction experiment, the problem of accuracy vs time to collect and analyze the experimental data arises. For any method to be practical, it is required that both experimental and analytical procedures are reasonably short. In most of the previous work performed by the direct comparison method, intensity data from only one or two sets of peaks were used to calculate the volume fraction of phases present in the aggregate. Consequently, rather long-time experimental measurements are required to assure that the intensity data are sufficiently accurate to justify the use of one or two sets of data. By using computer techniques to analyze the experimental data it becomes feasible to use all of the available data on a diffraction pattern. By so doing, the time spent in measuring any one diffraction maxima can be appreciably reduced. Although this results in poor counting statistics for any one maxima, the number of data points available for analysis is greatly increased. Based on the above discussion, it will be assumed that a continuous scanning counter-diffractometer technique will be used to collect intensity data from a two-phase mixture. The integrated intensity of the ith diffraction line from the a phase in the aggregate is given by:&apos;" where is the volume fraction of the a phase, The various quantities in Eq. [la] are angular independent while those in [lb] depend on the hkl spectrum of a particular phase. The meaning of the individual quantities in Eqs. [la] and [lb] are given in Appendix 1. It is convenient at this point to outline briefly the factors which will affect the measured intensity of any one hkl spectrum. a) Extinction effects arise from two independent experimental conditions. Primary extinction arises from a high degree of crystal perfection and results in spectra having lower intensity than predicted by Eq. [I]. Any treatment, such as powdering, which reduces

Jan 1, 1968

By Marvin P. Barnes, John G. Simos

The Park City District, Utah, is situated in the Wasatch Range at the intersection of the westward extension of the axis of the Uinta Range. Ore has been mined almost continuously from the first discovery in 1869 to the present day, with a total production of over 14 million tons. Sediments of Carboniferous to Triassic age have been folded into the northerly plunging Park City anticline and subsequently modified by thrust faulting, diorite and diorite porphyry intrusions, and strong east-west normal faulting during the Laramide orogeny. Younger andesitic volcanics partially cover the eastern edge of the district. The ore bodies occur as both lode and bedded replacement deposits over widely scattered localities. Near surface, high-grade silver "bonanza" ores were mined in early days from the Ontario and Daly Lodes, which occur along the east-west zone of faulting near the center of the district. Other lode or fissure deposits were found along the Mayflower and Hawkeye faults to the east and southeast. Large bedded replacement silver-lead-zinc ore bodies associated with east-west zones of fissuring, have been mined from favorable horizons in the Park City Formation in the Daly West and Judge mines. A series of long, narrow, high-grade, replacement ore bodies occur in the Silver King mine at a single horizon in the Park City Formation. Ore is currently being mined from strong bedded replacements in the Humbug Formation near the apex of the Park City anticline. Factors controlling ore deposition are: magmatic source, structural feeder systems, and favorable host rocks. Ore deposition along favorable beds is primarily a function of physical conditioning and secondarily of chemical composition.

Jan 1, 1968

By R. S. Fowkes

Jetstream pressure distributions and coal cutting rates were determined for a number of nozzles and under different operating conditions. The jetstrearn pressure distribution data were fitted to an assumed curvilinear equation by the utilization of a numerical least-squares technique with the aid of a digital computer. Subsequent manipulation of the approximation equation showed that the total force of the jetstream, rather than its maximum pressure or total kinetic energy per unit Lime, was the most significant quantity affecting the coal cutting rate. A shorter method for assessing the ability of a nozzle to cut coal was found.

Jan 1, 1968

By W. L. Acherman

The Bureau of Mines found the chemical and galvanic corrosion behavior of the TZM and molybdenum-30 tungsten alloys to be generally equal or superior to that of unalloyed molybdenum in many aqueous solutions of acids, bases, and salts. Notable exceptions occurred in 1 [N] nitric acid, where both alloys corroded appreciably faster than molybdenum. In mercuric chloride solutions, the TZM alloy was susceptible to a type of crevice corrosion which was not due to differential aeration. The alloys were usually not adversely affected by con-tact with dissimilar metals in galvanic couple experiments, but the dissimilar metals sometimes corroded galvanically. Both alloys were resistant to substitute ocean water spray at 60° C.

Jan 1, 1968

By P. Shibley, P. R. Clarke

Since this was an interim report of the initial operation of a long term project it is not available for publication. It is expected when the project is completed a full report of the work will be published.

Jan 1, 1968

By M. C. Fuerstenau, J. D. Miller

The response of calcite to flotation with saturated fatty acids and alkyl sulfonates of various chain lengths is presented. The amount of collector re-quired for flotation is shown to decrease systemati-cally with increasing carbon content from 8 to 12-carbon atoms per molecule. This systematic flotation response is correlated with the solubilities of the calcium-collector salts, which were established with a nephelometer. The 14-carbon collectors deviate from this systematic behavior, and no flotation is possible with the 16-carbon homologs. As determined by infrared analysis, the mechanism of collector adsorption involves a specific chemical reaction be-tween the collector and the surface. A reaction of the form CaCO3(s)+ 2 RCOO"=*=Ca(RCOO)2(s) + C03= is suggested. The pH of the system is also shown to be a most important parameter as it controls the carbonate, calcium, and collector ion concentrations in solution and thus controls flotation response. The importance of hydrocarbon chain length of collectors was recognized early, and various studies have been made on this aspect of flotation. Wilkinson, &apos; for example, noted that as the chain length of alkyl xanthates is increased, the amount of collector required for flotation of sphalerite is decreased. The same effect has been shown in the flotation of galena.2 Similar results were obtained when malachite3 and calcite4 were floated with various fatty acids. DeBruyn5 has shown that a similar phenomenon occurs when quartz is floated with amines at constant pH. Recently, Fuerstenau, Healy, and Somasundaran6 correlated this phenomenon with the van der Waals cohesive free energy of association of the hydrocarbon chains. It seems unlikely, however, that chain association could be involved in the sulfide and carbonate systems with the collector additions employed, especially with the short-chain xanthates. Rather, it would seem that the decrease in collector concentration with increase in chain length noted for flotation is related to the solubility of the metal-collector salt. The purpose of this investigation is to verify this premise and also quantify this phenomenon if possible. Calcite was selected for study with both alkyl sulfonates and saturated fatty acids as collectors. EXPERIMENTAL MATERIALS AND METHODS The collectors used in this investigation ranged from 8 through 14 carbon atoms per molecule. The fatty acids had a reported purity of greater than 99%. The sodium alkyl sulfonates were provided by the Marathon Oil Cot, Littleton, Colorado, and had the

Jan 1, 1968