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By J. Hudy

An investigation has been made to determine the applicability of the Cendrex X-ray instrument for the measurement of the ash contents of washed bituminous coal products. The results obtained for selected products from five preparation plants in the northern Appalachian region are described. Emphasis of the study was placed on low-ash bituminous coals suit-able for utility or metallurgical markets. There was good agreement between the results obtained by conventional ash determination methods and by the Cendrex for all the products tested. A principal disadvantage of coal in competition with other fuels has been its inconsistent quality, especially with respect to ash content. Mine rnechanization and production from coalbeds of inferior quality have accentuated this failing. Present quality control methods in coal preparation plants are inadequate because (1) control samples taken over a production shift only serve to give the average quality of the product, (2) conventional sampling and analysis data are usually not available at the time a shipment is scheduled, and (3) the plant operator does not have the use of such data when the coal is being processed so that operating conditions may be adjusted for correcting variations in quality. Thus, the development and use of continuous-control monitoring instruments is of prime importance. The Federal Bureau of Mines arranged to investigate an instrument using x-rays for rapid continuous ash determinations. Developed by the Dutch State Mines and first described in 1958,' this instrument, which has found widespread acceptance in Europe, is designed to provide ash analysis of any desired coal feed or product stream with only a five-minute time lag between sample collection and analytical results. With limit controls, this unit could be used to feed back signals to preset the separating gravity of coal washers, control the ratio of various coals needed to produce an acceptable blend, and permit the sorting of a washed product into two qualities, one which is below and the other which is above a prescribed ash content. This unit can also be used discontinuously for rapid determination of coal samples taken in the usual manner. THEORY Di jkstra and Sieswerda of the Dutch State Mines studied the effect of chemical composition and ash content on the absorption coefficient of coal with the transmitted radiation method.' They found that with an X-ray wavelength of 1.79 A and values calculated for the absorption coefficients of ash and combustibles, the absorption coefficient of coal gave a linear relationship when plotted against the ash content. Thus, a method of measuring the absorption coefficient of coal could also be used to measure the ash content. However, practical attempts to measure the ash content of coal by comparing the intensities of the transmitted X-rays failed. The absorption coefficient of coal can also be obtained by irradiating a layer of coal with x-rays and measuring the intensity of the diffused reflection (backscatter method). The relationship between the diffused reflection and the ash content is actually hyperbolic but approximates a straight line over a narrow range. A measuring circuit that balanced the difference in intensity of the reflected radiation from a standard surface against that from a coal sample was used. By plotting this difference of reflected radiation against the ash content, a curve which approximated a straight line over a range of 8 percentage points of ash was obtained. DESCRIPTION OF EQUIPMENT The apparatus performs two distinct functions: (1) the preparation of the sample to a suitable size consist and moisture content for delivery to the x-ray element, and (2) the measurement of the ash content by the x-ray element. In a continuous operation the coal sample is delivered to a conditioner where it is dried to a maximum of 1% surface moisture and pulverized in a high speed mill to -48-mesh. This material is fed, at a rate of 250-300 gpm onto a rotating disk, shown in Fig. 1, where it is mixed with material already present. The mixture is rotated on the disk and

Jan 1, 1969

By Linda Lee, R. E. Reed-Hill, C. R. Smeal

Four fcc metal surfaces, etched to make them responsive to polarized light, have been studied with an electron microscope. Jones'prediction that these surfaces are grooved has been verified. Optical-goniometer measurements made on commercially pure nickel indicate that the groove walls are poorly defined (100) facets. Surface mientations close to either 4001 or {ill).- show no extinctions on the polam'zid-light microscope. An explanation is offered for this orientation dependence. It has also been deduced that polarized-light extinctions on a grooved cubic-metal surface should not be used directly in crystallographic-orientation determinations. The nature of the etching solutions that produce these surfaces is considered. A cubic-metal surface may be made responsive to polarized light in two basic ways."' In one, an anodic film, believed anisotropic, is formed on the surface. A plane-polarized-light beam, at normal incidence, should be reflected from this type of film with an ellipticity that varies with grain orientation. Under crossed polarizers of a polarized-light microscope, each grain may be distinguished from its neighbors by a difference in reflected-light intensity. An alternate treatment,' more generally applicable to cubic metals and of principal concern here, involves etching of grain surfaces. The characteristic features of this surface were first deduced by Jones3 from light-microscope observations. She concluded that, in general, grain surfaces were furrowed so that light was reflected from two parallel sets of etched facets. A grooved surface produces elliptical polarization of a plane-polarized beam because the beam does not strike groove walls at normal incidence. Jones also observed that the furrows must have faces inclined to each other by approximately 90 deg, since the light returns along the incident path, and that a grooved surface should show four maxima and minima of reflected-light intensity during a 360-deg stage rotation of the polarizing microscope. Positions of maximum extinction were predicted to occur when groove axes were parallel to either polarizer or analyzer vibration directions. Because of the limited resolving power of Jones' optical microscope, her deductions were primarily indirect. Proof of the correctness of her conclu-sions, as demonstrated by the electron microscope, will be given as well as evidence concerning the crystallographic nature of the etch furrows and the types of etching solutions that produce them. EXPERIMENTAL PROCEDURE During a comprehensive study of hot plastic deformation in nickel and nickel alloys, an etch was evolved that produced a surface with an excellent polarized-light response on Nickel 200 ("A" Nickel). The etching solution and associated metal-lographic procedures are given in Table I. In evaluating this etch, a study was made of the topological features of the etched surface and their relation to the underlying crystalline structure. As part of this investigation, large crystals (2 mm average diameter) were grown in a 1-cm-sq Nickel 200 specimen. After the surface was etched, the crystallographic orientations of ten grains were determined by the standard back-reflection Laue technique of Gren-inger.4 Maximum extinction positions during a microscope stage rotation were also measured for the ten grains. Groove-wall positions on the surfaces of the ten grains were measured with a two-circle optical goniometer. The technique was essentially that of Barrett and Levenson.5 Several grain surfaces were photographed with a Philips Model 100A electron microscope. All specimens were replicated with collodion, or collodion backed with formvar and chromium shadowed at 18 to 20 deg. The basic material was Nickel 200. However, an electron-micrographic study was also made of surfaces developed by polarized-light etches on other fcc metals (90-10 a brass, Monel 400, and lead). All etching procedures are given in Tables I and 11. EXPERIMENTAL RESULTS Fig. 1 shows typical electron micrographs of three different fcc metal specimens and an optical micrograph of a fourth. All photographs show a grooved structure corresponding closely to Jones'3 predictions. Also, as noted by Jones, extinctions were always observed when groove axes were either parallel or perpendicular to the microscopes' vertical cross hair. The symmetry of the grooves, with respect to the twin boundaries in Fig. 1, implies that furrows have a crystallographic basis. The coarse-grained Nickel 200 specimen was used to study this basis. Facet Orientation. The poles of the ten Nickel 200

Jan 1, 1964

By Peter Soo

Pvestrained Ferrovac E iron has been neutron-irradiated at approximately 90°C to an integrated flux of 1020 nut (E > 0.82 mev]. The irradiation was found to produce an incveased temperature dependence of the flow stress in addition to a greatly increased athemal stress. Measurements of the flow stress and stress relaxation, from which the activation volume and activation energy for slip were deduced, show that neutron irradiation changes the rate -controlling slip process to one based on dislocation interactions with tetragonal distortions which are Produced around submicroscopic interstitial loops in the lattice. The study indicates that without prestraining prior to irradiation the chances of detecting a change in the rate -controlling slip process are greatly reduced because in the initial stages of slip a substantial fraction of the radiation defects are swept out of the slip plane by gliding dislocations. Thus, activation parameters which are subsequently measured are representative of a greatly reduced defect density and would not differ appreciably from those for unirradi-ated material. The large increase in the athermal component of the flow stress is probably connected with the presence of depleted zones in the lattice which are introduced by irradiation. ALTHOUGH fast neutron-irradiation has not been observed to markedly alter the activation parameters for slip in bcc metals,' small but significant changes do occur. Most experimenters agree that irradiation predominantly increases the athermal component of the yield stress.'-= In addition to this, Laidler and smidt7 have shown that in iron irradiated to 5 X 10" nvt and molybdenum irradiated to 10" nvt, changes occur in the activation volumes for slip. A similar conclusion has been reached by Milasin and Malkin8 for irradiated iron. Work by Ohr et a1.5 shows that for Ferrovac E iron, irradiated to 1.2 X 1016 nvt, small increases in the activation energy for slip also occur. So far these changes in the activation parameters have not been explained on a firm theoretical basis. One important factor which would minimize the chances of detecting a change in the slip mechanism upon irradiation is the presence of "channeling" which has been observed in molybdenum,9 niobium,10 and iron.11These channels are formed by gliding dislocations which sweep irradiation defects out of the active slip planes and thereby create zones in which continued dislocation motion is encouraged. The activation parameters for the dislocations gliding in the defect-free channels would, therefore, be similar to those for unirradiated iron and a change in the rate-controlling slip process would be difficult to detect. In the present work, an attempt has been made to reduce the effect of uneven deformation on the measured activation parameters for slip in neutron-irradiated Ferrovac E iron polycrystals, so that a more realistic assessment of the effects of neutron-irradiation could be made. Primarily, the experiments involve the irradiation of specimens which had been prestrained to 9 pct elongation at room temperature prior to insertion into the reactor. It was hoped that the introduction of a large number of evenly distributed dislocations would substantially decrease any channeling effect which might otherwise occur. MATERIAL AND EXPERIMENTAL PROCEDURE The starting material was vacuum-melted Ferrovac E iron, an analysis of which is given in Table I. The standard tensile specimen had a gage length of 1.125 in., a cross-sectional diameter of 0.120 in., and a re-crystallized grain size of 1.2 x 10-3 in. All tensile tests were conducted on a floor model "Instron" tensile machine at a strain rate of 3 x 10-4 per sec. The irradiation of the prestrained specimens was performed in the Brookhaven High Flux Beam Reactor to an integrated flux of 1020 nvt (E > 0.82 mev) at a temperature of about 90°C. All specimens were excap-sulated in high-purity aluminum sheaths which were lightly swaged around the samples to ensure good thermal contact. Subsequent measurements on the irradiated specimens showed that within experimental accuracy the swaging had not deformed them. EXPERIMENTAL RESULTS Fig. 1 shows the flow stresses for a series of unirradiated control samples. In order to produce a comparable dislocation substructure throughout the test sm range, all specimens were prestrained

Jan 1, 1970

By E. R. Helderman, C. Y. Ang, C. C. Nealey

Beryllium-base alloys have been successfully p7.-epared by the liquid-phase sintering technique. Depending orz the composition and amount of the intended liquid please, microstructures either single -phase or duplex in feature with randomly oriented grains have been obtained. Qualitative and semi-qualitative determination of distribution of alloying elements md microsegregations in some experi)uzental alloys haue been made by electron-micro-probe analysis in conjunction with microliardness testing and standard metallography. Tensile tests reoealed that some conzpositions possess attractive elastic properties with Young's mot1uli greater than 40 X 10' psi. In powder metallurgy, liquid-phase sintering is a process or phenomenon that has proven to be of practical value. For example, the heavy metals such as tungsten-copper-nickel, high-strength heavy gyro alloys,' heavy-duty electrical contacts,' and tungsten carbide tool materials are all products of liquid-phase sintering. Mechanisms involved in liquid-phase sintering, however, are not completely understood. Questions regarding the exact roles played by rearrangement of particles, liquid/vapor surface energy, solution and precipitation, and so forth, have not been completely answered. Evidence has been cited3 that at least volume shrinkage in the densification process is diffusion-controlled. It is possible that the predominant mechanisms for the complete densification and grain growth in a liquid-phase sintered system depend primarily on the alloy systems involved, in addition to processing conditions. Despite the lack of sound understanding of the mechanisms of the process, liquid-phase sintering has been and is being used to advantage either to synthesize microstructures for their special properties or to prepare alloys which are difficult to form by fusion process. Liquid-phase sintering of beryllium alloys was first attempted by Jones and Williams.4 They first tried infiltrating beryllium with magnesium, and then succeeded in preparing the alloy by sintering Be-Mg powder compact in molten magnesium bath. This investigation resulted in the identification of some Mg-Be intermediate phases. Crossley et a1.5 also used liquid-phase sintering technique in an attempt to produce ductile beryllium alloys for structural applications. The major liquid-phase components investigated by Crossley et al. were aluminum and silver with minor additives of germanium, calcium, lanthanum, cerium, and yttrium. The lack of wetting and the bleeding out of liquid phase were the difficulties encountered during experimentation. According to Hodge,6 the two compositions investigated by Crossley, which showed some promise based on compression tests, involved large amounts (over 35 wt pct) of silver, thus making them too heavy to be of practical interest to the aerospace industry and military users. The present investigation was prompted by the search for light-weight (density less than aluminum) beryllium alloys exhibiting small anisotropy in physical properties for precision inertial navigation instrument applications. In addition to isotropy, good structural properties such as high elastic modulus or desirable combination of mechanical and physical properties are also objectives of this investigation. The technique of liquid-phase sintering was chosen for its versatility in producing either duplex or homogeneous microstructures. This report is concerned with the use of copper and aluminum, with or without silicon addition, as the intended liquid phase, and the resultant micro-structures and some physical properties of the beryllium alloys. Qualitative and semiquantitative electron-microprobe analyses of some of the alloys are presented to illustrate the usefulness of this microanalytical technique for the identification of microconstituents and their distribution. EXPERIMENTAL PROCEDURES The beryllium powder used was -200 mesh Brush Beryllium Co. QMV NP-50 grade. Typical chemical analysis of the powder is shown in Table I. Commercial high-purity copper, aluminum, and silicon powders all screened to —100 mesh were used as additions. Mixed powder compositions were ball-milled in ceramic jars for 1/2 hr to ensure thorough blending. Milled powder was loaded either in 3/4-in.-diam button die or in Metal Powder Association flat tensile specimen die and compacted under top and bottom pressure. No lubricant or organic binder was used. Sintering was carried out in a quartz tube under a vacuum of 50 to 100 µ pressure. Surface hardness and some microhardness readings were taken on sintered specimens. Sintered density was

Jan 1, 1965

By H. M. Otte, A. L. Esquivel

A new leasl-squares method is Presented for determining lattice parameters of hexagonal or tetragonul structures. The method is adapted for use on electronic computers and involves a reiterative procedure. The correction factor employed raries linearly with the lattice parameter, a (determined from the Brag, angle). In contrast, Cohen's method and recent modifications of it use a correction factor that varies incersely as the squure of the lattice paramneter, a. While the recent modifications attempt to improve the precision of the extrapolated lattice parameter, a, (or-cu). by stressing the importance of the weighting factor. the present approach emphasizes the need for choosing the correct extrapolation function. A comparison between the present method (the Linear method) and Cohen's method indicates that the Linear method may be more appropriale in certain cases. through a priori no critertion appears to he available for making a chorce between the methods. The size of hexagonal and tetragonal crystal lattices is determined by two parameters, a, and c,. Although in principle the two lattice parameters can be determined independently from reflections for which h - k = 0 and 1 = 0, respectively, in practice this may be inconvenient (because of the angular positions at which these reflections may occur) or not easily possible (because of low intensity). Furthermore, if a high precision or accuracy is required, the limited number of reflections of this type available, particularly in the high-angle region, is not sufficient for the necessary corrections (mainly due to absorption) to be determined with accuracy. Several methods1-7,11-13 have been proposed employing all reflections, to obtain the optimum values, a. and co, either by a trial and error procedure or a least-squares fit. Of the latter method, cohen's5 is the best known one since it provides explicit expressions for the optimum a. and c,. However, Cohen's method is only strictly valid if an extrapolation function is used that varies linearly with l/a2 or lie2 (see Section 3), a requirement that does not appear to be generally appreciated. On the other hand, all the better known and more widely used A recent trial and error method was proposed by Massalski and King8,7 who computed extensive auxiliary tables of axial ratios vs the functions A = [(4/3)(h2 + hk +k2) + l2+(a/c)2] and C = A(c/a)2 used in computing a and c values from the observed Bragg angles. These values of a and c were then plotted against a function which permitted linear extrapolation. As a criteria; for the "optimum" values, Massalski and King rely upon a visual fitting of the line through points representing reflections of low 1-index points to compute the extrapolated value of ao and high 1-index reflections to obtain CO. The successive computations and graphical plotting required to reach the "optimum" value are quite lengthy and tedious even on a desk calculator and no quantitative assurance is obtained of having in fact selected the optimum value.* If the method of Massalski and King is used on an electronic computer, then their published tables become redundant and a least-squares fit becomes a natural selection for the choice of optimum values. Such an approach will be called the Linear method. For work now in progress on the effect of certain physical variables on the lattice parameters of hexagonal crystals, it has become essential to determine the confidence limits of small changes in the lattice parameters. Since extrapolation functions that varied linearly with a and c actually also appeared to vary linearly with l/a2 or l/c2 when tested against published as well as our data, a comparison of Cohen's method and the Linear method was considered desirable (Sections 3 and 4). For the latter method an electronic computer was required since a reiterative procedure to obtain the optimum ao and co values had to be employed. The purpose of this paper is to describe the principles of the Linear method, illustrate its application, and compare it with Cohen's method. 1) THE LINEAR METHOD The standard practice in obtaining the lattice parameters in the Debye-Scherrer method is to

Jan 1, 1965

By Donald B. Evans, Robert D. Pehlke

The solubility of nitrogen in liquid Fe-B alloys has been measured up to the solubility limit for the formation of boron nitride. The activity coefficient of nitrogen increases with increasing boron content in the range 0 to 7 wt pct B. From experimen -tal data, values have been calculated for the B-N interaction parameter e3 at temperatures in the range 1550" to 1750°C. A value of 0.038 has been estimated for the boron self-interaction parameter eg at 1550°C. The standard free energy of decomposition of boron nitride into the elements dissolved in liquid iron has been determined to be: ?F° = 45,900 -21.25T in the range from 1550° to 1750°C. The nitride is assumed to be of composition BN. BORON nitride has an unusual combination of properties which make it appear attractive in a wide range of engineering applications. Some of its more important and most recent applications are in the nuclear area, particularly in connection with the liquid-metal cooled reactor concept now receiving considerable emphasis. Boron nitride has a high degree of stability at elevated temperatures. It also has excellent ma-chinability and the ease with which its crystals deform suggests applications as a lubricant. These properties stem from a hexagonal layer-type structure similar to the structure of graphite. One of its primary uses to date has been for seals in liquid-metal pumping systems. It is also used in nuclear reactors as an insulating layer to separate two solid metals which are not themselves compatible under the conditions of temperature and atmosphere in which they are used. Its inertness to liquid metals has also suggested use as a mold-release agent in casting processes. In addition to its excellent machinability and reported inertness to liquid metals such as iron, silicon, aluminum, copper, and zinc, boron nitride has high thermal conductivity and excellent thermal shock resistance. This combination of properties would make it appear ideal as a refractory crucible material for refining of high-purity liquid metals, for example high-quality steels. However, since it is known that concentrations of boron as low as 50 ppm can have a marked effect on the physical properties of certain steels,' in particular on the creep and stress-rupture properties, an investigation was undertaken to define accurately the chemical equilibrium among boron, nitrogen, and liquid iron in the range of steelmaking temperatures. EXPERIMENTAL PROCEDURE Two experimental approaches to this problem were employed: a Sieverts' method and a quenching method. In the first method, the Sieverts' technique was used to measure the equilibrium nitrogen solubility in liquid Fe-B alloys of 0 to 7 pct B as a function of nitrogen gas pressure over the melt. The solubility limit of the boron nitride phase formed was determined by the point of departure of the nitrogen absorption from Sieverts' Law. This technique has been applied to liquid Fe-Ti alloys by Rao and parlee,' to liquid Fe-A1 alloys by Evans and Pehlke,3 and to solid Fe-V alloys by Fountain and Chipman.4 In the second method a melt of liquid iron was held in a crucible of boron nitride under a known partial pressure of nitrogen gas. After thermodynamic equilibrium was attained, the melt was quenched in a stream of helium and then analyzed by wet-chemical methods for boron and nitrogen. The Sieverts' apparatus used in the first method was essentially of the same design as the one described by Pehlke and Elliott.5 The charge materials were vacuum-melted high-purity iron (Ferro-vac E) supplied by the Crucible Steel Co. and -325 mesh boron powder supplied by Cooper Metallurgical Associates of Cleveland, Ohio. The boron contained less than 0.02 wt pct O, according to supplier's analysis. Recrystallized alumina crucibles were used to contain the melt. Examination of solidified melts showed these crucibles to be satisfactory with no evidence of any reaction or physical penetration of the crucible wall by the melt. The melt temperature was measured by a disappearing filament-type optical pyrometer sighted vertically downward on the melt surface through a 1/4-in.-diam sight hole in the crucible lid. The pyrometer was calibrated against the melting point of pure iron in the same apparatus, taking the emissivity of

Jan 1, 1964

By Robert E. Green, P. W. Kingman

Application of a constant geometry compression test to single crystals of aluminum of selected diameters from 1/4 to 1/64 in. showed the presence of a diameter-dependmt size effect. The most pronounced effects were found in those crystals oriented for single slip, while for specimens possessing orientations in the comers of the standard stereographic triangle virtually no size effect was exhibited. The yield stress of the crystals oriented for single slip was found to increase with decrease in specimen diameter, while the strain-hardening rate was found to be lower for the smaller specimens. The experimental results are in general agreement with those of other investigators obtained from lensile tests on copper and aluminum crystals. THE earliest systematic investigation of a possible size effect on the plasticity of metals was that of no,' who in 1926 performed tensile tests on cylindrical aluminum single crystals with diameters of 3 to 8 mm. Ono concluded that the gross stress-strain curve did not show a diameter dependence, but that the resistance to slip for strains of 0.1 pet and less appeared higher for 3-mm-diam crystals than for larger sizes. Later studies of aluminum by Maddin et al2 tentatively concluded that a size effect exists, but the conclusions were again open to question because of inconsistencies in the experimental data. Wu and Smoluchowski3 had previously shown that the slip system activated in a single-crystal sheet specimen of aluminum is a function of the specimen cross section in the slip direction, but no stress-strain data were obtained. Subsequently Fleischer and Chalmers4 studied the effect of the length of the slip direction of the primary-slip system on the stress-strain curve by testing aluminum crystals with geometrically dissimilar cross sections. In the course of this investigation a size effect was indicated in rather large crystals; however, the number of these tests was small. Other investigators have indicated that a size effect in aluminum is appreciable only for diameters of 0.5 mm or less.5, 6 Size-effect studies have also been carried out on copper crystals, the most detailed being that of Suzuki et a1.7 who performed tensile tests on specimens of many diameters ranging from 2 to 0.12 mm. Suzuki found a strong size dependence in the easy-glide region, both the extent of the easy glide and the hardening rate in easy glide were size-dependent, and the size effect was found to be orientation-dependent. Suzuki's results are in agreement with the less extensive observations of Pater-sonB and those of Garstone et al.9 A size effect was found by Rebstock using tubular copper crystals.'0 Size effects have also been noted in a brass,6, 11 in cadmium,12'19 and in hexagonal crystals.14 All the previously cited works have been entirely concerned with the variation of specimen cross section. The effects of specimen length and the change of specimen geometry which results from using progressively thinner specimens while maintaining the same specimen length have been largely ignored. A theoretical discussion of the effects of specimen length and geometry has been given by Hauser and Jackson,15 who predict a grip effect on easy glide as a function of specimen geometry provided that the specimen dimensions are large compared with the spacing between the slip bands, and by Fleischer and Chalmers,18 whose analysis of grip effects resulting from lattice rotation predicts an increase in easy glide with an increase in specimen length. A study of size and geometry effects in aluminum crystals by Kitajima and shimba17 indicated increasing amounts of easy glide in specimens of increasing length and identical cross section, and nearly identical stress-strain curves for specimens of different sizes having constant length-to-diameter ratios. Since the present study is primarily concerned with diameter dependence, the following factors were taken into account: specimen material, specimen geometry, testing method, range of sizes to be tested, and possible influence of surface and volume effects. Aluminum was chosen because of the present lack of conclusive results and the seeming possibility of size effects at relatively large diameters, the

Jan 1, 1964

By J. W. Downey, S. T. Zegler

A study has been made of the occurrence of Phases having the Cr30-type structure in ternary alloys having the general composition where B cept for iron and copper all the B components are known to form binary compounds having the type structure. The occurrence of the struc-ture type in the ternary alloys was investigated using optical and X-ray metallography. The results indicate that iron can replace virtually none of the cobalt in at 900°C, but substitutes for nickel in up to the approximate composition tually insoluble in V3Ni and 2) and exhibit complete solubility. At 100 nickel can be substituted for cobalt in VSCo up to the composition solubility; and 3) in the system , two solid solutions having the type structure occur. At the same temperature, 1000°C, V3Si exhibits limited solubility for V3Co but is completely mis-cible with V3Ga. Lattice parameters have been determined for all the binary and ternary phases. The solid solutions are discussed in terms of the atomic size and electronic factors which are thought to influence the occurrence of Cr30-type phases. The binary compounds V3Co and V3Ni were found to form peritectoidally from o phases and a vanadium, the former compound at a temperature between 1000" and 1050°C, the latter between 800°and 900°C. The substitutions of nickel and rhodium for cobalt in V3Co were determined not to raise the superconducting transition of VSCo to a temperature as high as 2°K. The occurrence and stability of binary intermediate phases having the Cr30- or A15-type structure (space group o;, Pm3n) have been discussed in several recent papers . Vanadium forms the struc -ture at or near V3B stoichiometry with all the mem -bers of the cobalt and nickel groups in the periodic table and also with Au, Ga, Si, Ge, Sn, P, As, and Sb. This paper describes a survey of the occurrence of the CrsO-type structure in ternary alloys having the general composition V3(B, B') where B and B' are Fe, Co, Ni, Cu, Rh, Ir, Si, and Ga. The purpose of the survey was to clarify the connection between the position of the B partner in the periodic table and its CrsO-type phase-forming tenden~y.~,~ The survey is part of a broader program concerned with the influence of B-partner substitutions on the superconducting transition temperatures of CrsO-type compounds. The transition temperatures, Tc, of some of the ternary Cr,O-type phases found in the survey are also discussed in this paper. EXPERIMENTAL PROCEDURE The alloys were prepared by arc-melting in an A-He atmosphere and were in the form of buttons, weighing approximately 3 g. The metals used in their preparation were received from commercial sources and were in all cases 99.9+ pct pure. The vanadium was spectrochemically pure except for 800 ppm of Si, 200 ppm of Fe, and 200 ppm of Al. For study of each pseudobinary system at least seven alloys were prepared having the general compositions case of alloys containing gallium, melting losses were small, usually less than 0.3 pct of the total weight of the metals charged for melting. Melting losses were somewhat greater for gallium alloys, ranging in general from 0.9 to 5.0 pct. Ternary V-Si-Ga alloys were chemically analyzed and the results are given in Table I. The analyses show most alloys to be within 2 at. pct of the intended composition. Throughout the balance of the paper the intended compositions are used in discussing the alloys. The cast buttons were annealed within evacuated quartz capsules for times ranging from 3 to 6 weeks at temperatures between 800" and 1000°C and water-quenched. The phases present in the annealed and quenched alloys were identified by optical and X-ray metallography. X-ray diffraction photograms were made with powders prepared from the bulk specimens, by the use of a 114.6-mm-diam powder camera with copper irradiation. The lattice parameter of CrsO-type phases and their standard errors

Jan 1, 1963

By J. W. Goss, M. J. Coolbaugh

Most grouting has been done to stop water flaw in mines and for stabilizing foundations of various man-made structures, a survey of the U.S. literature reveals. Apparently Sun Manuel is one of the first mines in this country to use grout extensively underground for strengthening and stabilizing ground in drifts, shafts, and stations. A comparison with other procedures as well as details of the Sun Manuel program are covered. The employment of pressure grouting as a ground stabilizer at the San Manuel Copper Corp. mine reduces delays in both development and production, lowers costs, and makes possible safer working conditions. It specifically reduces delays in haulage operations and permits the maintenance of normal ventilation. In development work this grouting allows faster excavation by cementing together highly fractured or broken ground that otherwise would require extensive cribbing or spiling. In drift repair, it consolidates the loose or fractured rock over the timber or steel drift supports, thus decreasing the frequency of repair, lessening the hazards from falling rock, and curtailing delays due to blockage of drifts by muckpiles and repair operations. Pressure grouting is the process of pumping an accurately controlled mixture of cement and water into loose, fractured, or porous rock. The ratio of water to cement varies according to the nature of the rock encountered, from the thinnest mixture of 30 gal of water per sack of cement, used to fill very fine fissures, to very thick grout of 5 gal of water per sack of cement, used to fill large fissures or extensive areas of loose, broken rock. The pumping pressures at San Manuel vary from about 100 to 1000 psi, depending upon the compactness of the rock, while at other mines the pressures sometimes go as high as 5000 psi. In order to grout an area in which ground water is encountered, the pumping pressure of the grout must be increased by an amount equal to the pressure of the ground water. GROUTING IN DEVELOPMENT WORK The areas under development at San Manuel include many sections of loose, highly fractured rock. Prior to the advent of the grouting program, drifts, shafts, and stations in these areas could not be excavated without utilizing extensive support such as cribbing, spiling, and breast boarding. This slowed down the development work and increased the costs considerably over that required for excavating in more competent ground. Now, when a particularly bad area is contacted, the mining is temporarily stopped while the bad portion of drift or shaft is grouted. After the grouting is completed, the excavating is resumed with an approximate decrease of 50 pct in lost time and costs. Grouting in Drifts and Turnouts: The grouting procedures and patterns used in drifts and turnouts are very similar. The standard procedure for grouting such a turnout is shown in Fig. 1. After the ground is supported as well as possible with cribbing or lagging, the gaps between the back lagging and side lagging are plugged with empty cement sacks or additional timber, if necessary. The ground surrounding the proposed turnout is then grouted in two stages. In the first stage, the broken and caved rock is drilled and grouted to a depth of 5 to 10 ft, depending on the depth of the broken rock. This stage forms a grouted seal that allows higher pressures to be used at depths beyond 10 ft without developing excessive leaks at the face. After a grout hole is drilled, a 10-ft long pipe is wedged tightly into it with empty cement sacks. Grout is then pumped into the hole until the pressure reaches 200 to 300 psi, and the pipe is subsequently removed if it hasn't become cemented in. No more than one hole at a time is drilled and grouted because the grout has a tendency to go from one hole into another, plugging up the latter. Five or six holes are usually adequate for the first 10 ft of grouting. Experience has shown bentonite to be a useful admixture to the grout, particularly when it is indicated that the grout is being lost into large fissures or voids. Bentonite increases the plasticity of the grout enabling it to remain in place more easily until it has begun to set. In the second stage, the longer holes are drilled through the previously grouted rock, after which the

Jan 1, 1961

By John M. Tinsley, Calvin D. Saunders, H. K. van Poollen

In the past few years much con-sideration has been given to the evaluation of the effect of hydraulic fracturing on the productivity of wells. Generally, these studies included the evaluation of fracturing materials, fracture extension and formation damage due to the use of various fracturing fluids. Only little consideration has been given to the characteristics, and in particular the flow capacity, of the fracture itself and its effect on well productivity. This paper presents the results of laboratory investigations pointed toward fie evaluation of the efficiency of various fracrures with special emphasis on the flow capacity of these fractures. Data presented in this paper are the results of both an electrical model study and physical testing. Under consideration are (I) effect of overflush, (2) premature production of well after treatment, (3) "tailing-in" with coarse sand near the end of the treatment, (4) effect of propping agent size and concentration, (5) reduction in effective frac-ture permeability caused by formation caused by formation fines, silt and clays, and (6) effect of various fluids on formation strength and competency. The results of this investigation indicate that the flow capacity of a fracture is affected by any or all of the various parameters mentioned above. The authors believe that a better understanding arid utilization of these factors should result in more efficient formation fracturing. INTRODUCTION Hydraulic fracturing has become almost a standard practice of many companies for stimulating production from old and new wells. Although most companies utilize this service, techniques of application vary widely between companies and areas. Probably too often when a well in an area responds favorably to a particular technique all future wells in the same area are treated in a similar manner. Possibly a modification of the technique would result in a further production increase. Variables, of which many are extremely difficult to evaluate from field results, hamper the selection of procedure changes. Attempts are being made by a number of organizations to analyze statistically treating techniques from production data. This is a very worthy and necessary approach but very possibly laboratory investigations may aid in evaluating some of the variables which tend to affect the results of a fracturing treatment. Some of the factors cannot be studied from practical field experience and only laboratory tests can show the possibilities which might exist. One of the factors which appears to be of major concern today is the flow capacity of the created fracture and how it can be changed. Papers on this general subject have been primarily concerned with the size of propping agent and the extent of fracture. Papers have also been written on the possible permeability damage to formations by fracturing fluids. In addition, it might be possible that another type of flow restriction is prevalent. This would be a restriction of flow through a sand-packed frac- ture caused by foreign materials integrating within the propping agent. This paper presents preliminary data obtained in an attempt to evaluate the effect of some factors affecting flow through sand-packed fractures. No attempt is being made to offer a fracturing technique adaptable to all areas and conditions, but to furnish data tending to show the possible effects which might be caused by variations in procedures and materials. PROPPING AGENT PERMEABLLITIES A hydraulically induced fracture containing sand as a propping agent may theoretically be classified as a packed-sand system. The flow of fluids through such packed systems has been the subject of much research. Although there have been numerous methods proposed for the evaluation of such systems, most writers agree on the general properties affecting their flow capacity or permeability. These properties include porosity, particle size, sphericity and the roughness of the particle. In some methods of evaluation . the particle size and sphericity terms are combined to produce an equation which is a function of the surface area of the particles. In this study the permeability of various fracturing sands was both measured and calculated. The apparatus for the permeability measurements consisted of a 52-in. Lucite tube with a 2.5-in. ID. A screen and drain plug were fitted in the bottom of this tube to retain and hold the sand in place while allowing fluid flow. Two pressure taps consisting of thin, highly perforated

By C. P. Miller

In order to determine the usefulness of geochemical and biogeochemical prospecting for nickel, ten localities representing several types of nickel occurrences were selected as sites from which to collect plant and soil samples. This report covers the investigations in two of the areas. After a brief geologic description of the areas, the author presents details of the experimental tests and resulting data. Conclusions drawn from the studies led to several general guides for further prospecting. In a study of the usefulness of geochemical and biogeochemical prospecting for nickel made about three years ago, approximately ten localities, representing several different types of nickel occurrences, were sampled and about 1500 samples of plant and soil were collected. This report will cover briefly the data and results for two areas, and a summary of guides for prospecting. DESCRIPTION OF AREAS SAMPLED One locality is the Red Flats nickel prospect in Curry County, Ore., about six miles southeast of Goldbeach, and the other is the Little Rocky Creek prospect in Stillwater County, southcentral Montana, just southeast of the Benbow chromite mine. The Oregon area is a lateritic-type nickel deposit formed on a nickel-rich serpentinite peridotite complex, similar to the Josephine intrusion in southwestern Oregon. The Montana area is a nickel prospect in norite, peridotite, and related rocks of the Stillwater igneous complex. The Stillwater complex is a series of layered basic and ultrabasic rocks, with a layer of norite-gabbro at the base and a series of peridotites and gabbros above. The nickel in the Oregon deposit occurs in both the peridotite and the overlying soil. A deep lateritic soil is developed locally on the peridotite and serpentinite and constitutes the ore. The average nickel content of the lateritic soil is less than 1 pct, whereas the nickel content of the weathered peridotite is about 1 to 1.5 pct. The nickel occurs as garnierite (Mg, Fe, Ni, Mn)3 (OH)4 (SiA1)2O5 in the soil and in the olivine and pyroxene in the peridotite where it probably substitutes for Fe2+ or Mg2+ in the silicate lattices. Nickel is found in three distinct ways in the Still-water rocks: 1) it is in the olivine and pyroxene minerals in norite, harzburgite, etc.; 2) it occurs as widely disseminated grains of pentlandite-pyr-rhotite, which tend to be concentrated in the lower norite band; and 3) it occurs as discrete bodies of pentlandite-pyrrhotite and chalcopyrite which are localized in the norite zone, close to the contact with the underlying rocks. The nickel content of the norite is probably less than 1 pct, and the nickel content of the pods and lenses within the norite is about 1 pct. PROSPECTING APPROACH Although the areas are different geologically, the approach in prospecting them is fundamentally the same. The procedure is twofold: 1) a rapid reconnaissance survey to outline an area of high nickel content, and 2) a more detailed survey to outline zones of possible ore grade within the area of high nickel. The possible ore at Red Flats is concentrated in the lateritic soil, whereas at Little Rocky Creek it is in the sulfide pods. Both types are surrounded by an area of relatively high nickel content. CHEMICAL ANALYSIS Chemical analyses of nickel were made by a di-methylglyoxime colorimetric test, similar to the standard test for nickel, utilizing concentrated sul-furic acid for extraction. The lower limit of detection for nickel in soil by the method used was about 10 ppm and for nickel in plants about 5 ppm. The relative deviation was about 25 pct. SOIL PROSPECTING General Statements: A summary of the approximate average parts per million of nickel in soil, as compiled from the literature and from my study, is given in Table I. Selected references are given at the end of the paper. Few of the investigators reported the type of extraction or analysis, so the data given may not be strictly comparable to mine, which were made with a sulfuric acid extraction. Any nickel concentration greater than these average values might be considered anomalous, although each area must be studied in relation to the surrounding rocks. Method of Soil Sampling: The soil samples were taken in a zone from 1 in. to 1 ft below the humus layer, and within a 15-ft radius around a station.

Jan 1, 1961

By G. W. Tracy, R. D. Carter

Numerical calculations were made to determine the behavior of reservoirs with high-pressure drawdown and wide well spacing where the initial productivity is low and the wells are completed by hydraulic fracturing. The two-phase flow equations were solved for the flow into a single well. This well was assumed to be producing from a reservoir with hydraulically created horizontal fractures (four different systems with fractures were studied). For comparison purposes, additional two-phase flow calculations were made assuming a reservoir with uniform rock properties. The two-phase flow results were also compared with the conventional calculation methods, which do not include the effect of saturation gradients resulting from a simultaneous flow of oil and gas which are normal to this type reservoir. It was found that the conventional methods predict (1) a high and too optimistic value of ultimate recovery, (2) a high producing rate and a high reservoir pressure at a given oil recovery and (3) a low trend of gas-oil ratio with oil recovery. Included in the two-phase flow calculations were provisions to control the oil production rate by an allowable rate and, also, by a gas-oil ratio penalty rule. For the systems with hydraulic fractures, the producing rate was controlled by the gas-oil ratio penalty rule for most of the life. This is in contrast to the system with uniform rock properties which went "on decline" almost immediately. An unexpected characteristic of the systems which included fractures was the early rise in producing gas-oil ratio from 730 cu ft/bbl to approximately 1,200 cu ft/bbl, followed by a "leveling off" before the normally expected gas-oil ratio rise began. Additional features which are a result of hydraulic fracturing are (I) greater ultimate recovery, (2) higher average producing rates and (3) a lower average reservoir pressure at a given oil recovery. INTRODUCTION Some oil fields discovered during the past few years are producing from certain volumetric ally controlled reservoirs (often referred to as solution or internal gas- drive reservoirs) which are characterized by high-pressure drawdown at the wells. Since the available pressure drawdown at a well is limited by the static reservoir pressure and the producing rate is controlled by the available drawdown, wells completed in this type of reservoir usually produce at a rate less than the allowable from the time of completion. Because of this, this type of reservoir is referred to as a low productivity reservoir. Economic considerations require the use of wide well spacing and well stimulation by hydraulic fracturing to make commercial wells in this type of reservoir. Performance predictions for volumetrically controlled reservoirs have been made using a combination of two standard equations. 1. The "Schilthuis" or "Muskat" type material balance equation is used to relate the average reservoir pressure and the cumulative oil recovery. 2. The results from the material balance equation and the productivity factor as described by Pirson' are used to relate the cumulative recovery with producing rate and time. The material balance equation assumed uniform pressure and liquid saturation conditions throughout a reservoir. The steady-state radial flow formula allows for a pressure gradient toward a well but assumes uniform liquid saturation. These calculation methods are adequate for application to reservoirs wherein the drawdown at the well to realize satisfactory producing rates is small compared to the total pressure. In low productivity, volumetrically controlled reservoirs, the pressure drawdown at the well is large cornpared to the total pressure. Although a precise number cannot be given for the magnitude of a large pressure drawdown, values in excess of 1,000 psi would definitely be included. For practical considerations, this usually occurs when the formation flow capacity is less than about 100 md-ft. However, this limit of formation flow capacity will vary with the well producing rate. The low pressure in the neighborhood of the well which results from a high drawdown causes evolution of large volumes of gas. This causes the gas saturation to be higher near the well than at a greater distance—-hence, a non-uniform gas saturation. Also, the relationship between the relative permeability to oil (K/K) and gas saturation is nonlinear but decreases approximately in an exponential way with increases in gas saturation. Because of this, the following chain reaction is established.

By S. P. Hansen

Gravity sedimentation is one of the most widely used processes for separating solids from liquids whether it be for ore and mineral processing or for treating municipal sewage or industrial wastes. Investment in sedimentation equipment can represent a significant portion of the total capital costs associated with a processing or treatment facility. In spite of the importance of sedimentation, little attention has been devoted in recent years to improving this equipment by applying the basic principles involved in sedimentation. In the water and waste treatment field, design criteria established one half-century ago is still the accepted standard and in reflection of this lack of progress, sedimentation and thickening equipment has remained virtually unchanged. The primary purpose of this paper is to present and describe a new innovation in gravity sedimentation which has been applied to water and wastewater treatment and could definitely have application in the field of ore and mineral classification. A secondary object is to introduce the mixed media filter which has been widely used to treat municipal drinking supplies, industrial process water and to provide tertiary treatment of sewage and industrial wastes. The tube-type clarifier was developed primarily to be applied in the field of water and waste treatment where it was found that it could be used to considerably reduce the size and cost of clarification facilities. A logical extension of the tube clarifier would be to the area of minerals classification, ore separation, and for treating waste water associated with these activities. In water treatment practice, most clarification processes are followed by a filtration step to provide further polishing of the water prior to use. This paper will also discuss the mixed media filter which is graded from coarse to fine in the direction of filtration and is capable of operating at high filtration rates and with greater applied suspended solids loading than other filter designs while providing a high qualify filtrate.

Jan 1, 1970

By Peter N. Holtham, Mary M. Ng

"Resistivity measurements of minerals in the laboratory are commonly made with a low DC voltage source. Common test voltages specified in the ASTM Standard D257 are 100, 250, 500, 1000, 2500, 5000, 10000 and 15000 V, however 100 and 500 V are the most frequently used. Resistivity results obtained in the laboratory have been used to infer the electrical behaviour of minerals undergoing electrostatic separation. However because the voltages employed in electrostatic separation in the plant are of the order of thousands of volts, typically greater than 15000 V, whether the laboratory results are applicable as a predictor of plant performance is a critical question. It is unclear whether resistivity values taken at a low voltage are characteristic of those seen in electrostatic separation, in which the minerals are exposed to a much higher voltage. No definitive answer could be found in the literature.In this work, the resistivities of zircon, rutile and ilmenite were measured in a corona field for the first time. The measurement principle was based on a technique developed to measure fly ash resistivity in electrostatic precipitators, however the test apparatus and findings are novel.Resistivities of rutile and zircon were found to be easy to measure. The values measured in a corona field were several orders of magnitude less than those obtained with a dc voltage of 100 V. Evidence of back corona was observed with zircon. When the voltage drop was greater than the sample layer could withstand a localised electrical stress developed, resulting in a voltage breakdown, at which point a sudden surge of corona current (back corona) was detected in the sample layer. Rutile, on the other hand, exposed to the same conditions as that of zircon (i.e. same temperature and applied voltage) did not exhibit any sign of back corona. Its resistivity across the range of test voltages (14 to 33 kV) remained fairly constant."

Jan 1, 2003

By Tell Ertl

TODAY'S mining industry is witnessing a transition in labor utilization. The drill-jumbo operator, the mucking-machine operator, the blasting crew, the scaling and timbering crew are all specialists. The all-around miner is rapidly disappearing. As mechanization has resulted in a higher order of underground skills; specialization of labor has been a natural consequence, as has the need for more supervision and engineering. Mines now are cleaner, neater, safer, and have a greater productivity per man-shift than ever before. Nothing spectacular like the continuous miner has yet come to the underground metal mines, but t a gradual improvement in methods, equipment, and technical knowledge is achieving the increased efficiency. With the exhaustion of the rich ores and large profits and who-cares-about-the-costs, mining has become a business; that of producing low value ores at costs below selling price. Charles A. Chase, patriarch of Colorado mountain mining men, manager of the Shenandoah-Dives, was one of the first to preach and prove his preachings that mining is a business. He has been mining a lead-copper-zinc-gold-silver ore, much from elevations above 1.3,000 ft, for a quarter century without a shutdown.-The ore is of such low value that most engineers and investors still would consider it foolhardy. Yet he has kept Silverton, Colo., alive, has paid wages without a lapse, has produced $25 million of new wealth and maintained a steady return to the investors. This type of responsibility is increasingly apparent in the mining business and is one feather that can be worn proudly. .Much emphasis is being placed on improving, the productive mining operations-breaking, loading and transportation. Breaking in underground metal mining is done by drilling and blasting. To the writer's knowledge, no chain or rotary-type machine has been developed for mining strong, abrasive rock. Drilling Percussion drills are still the standard drilling machines underground. Diamond drills, that: were the rage a decade ago for drilling long holes, are being superseded by the rock drill. The development of the hard abrasion-resistant carbide bit permits full-gage long holes to be drilled by percussion drills at a lower cost than diamonds. The change in the use of percussion drills is chiefly in the method of mounting. The column and arm are disappearing and the jackleg and rubber-tired or track-layer jumbo mountings are taking its place. At the Homestake mine .lightweight jackhammers mounted• on pneumatic legs using 7/8-in. hexagonal drill. rods and 1 1/2-in, tungsten-carbide detachable bits have been found more portable and maneuverable. They have less air consumption, lowered, dynamite consumption, and more footage and tonnage per man-shift than with 3 1/2-in. drifters on a column mounting. Drills now are mounted on longer feed carriages, drilling up to 20 ft without changing steel. These mountings result in great savings because the driller can set up quickly, drill the entire depth of the hole without changing the drill rod or bit using carbide and one-use bits, and can move his machine quickly to the next hole. One man to the machine is becoming general practice. The result is longer rounds rounds drilled at a lower cost than the previously used short rounds. A jumbo developed in the Tri-State can be extended to mine ore left in the roof up to 65 ft above the floor. Drill-rod life was formerly considered to be about 250 min of actual use. The increase in the drilling time per rod per day has gone up considerably with the development of the jumbo and the long-feed carriage, resulting in which is apparently more rod breakage., Consequently, a great deal of research is being done in the attempt to develop an alloy-steel rod with longer service life to offset the greater cost. Some reports indicate that alloy steel or Swedish steel results in cheaper drilling than conventional drill rod. However, several tests have shown only slightly increased life for alloy drill rod. Undoubtedly, the blow of the rock drill, the length of the drill rod, and the resiliency of the rock being drilled are important factors in the life of drill rod, so it follows that alloy steel might work well in some mines and result in no savings in others. The bit forged on the drill rod is seldom encountered and steel detachable bits are not as common as in the recent past. The one-use bit is gaining popularity because of. the difficulty in rehardening reconditioned steel bits satisfactorily. It is thought that the, carbie-insert bit is most applicable to drilling hard 'rock' where the steel bit is unable to drill out a full change, for instance, in extremely abrasive

Jan 1, 1952

By Richard E. Ray

INTRODUCTION Main mine fan installations at underground coal mines must be designed to comply with the requirements outlined in 30 CFR (Code of Federal Regulations) Part 75. However, very little emphasis is typically placed on the aerodynamic optimization of shaft collar designs, ductwork configurations, and the selection of a fan isolation, or "closing door," system. Field testing has shown that poorly designed systems may produce large pressure losses between the shaft and fan inlet, as well as air turbulence problems which adversely impact fan efficiency and sometimes fan structural integrity. This paper analyzes each component of a surface exhaust fan system for an underground coal mine: • The shaft collar arrangement, • The 45 or 90-degree turning duct that isolates the fan motor from the return airstream, • Alternative ductwork arrangements for parallel fan installations, • The self-closing doors or dampers that are required for multiple fans, and • Horizontal and vertical evas6 arrangements on the discharge side of the fan. While discussion is limited to axial fan installations at shaft mines, most of the recommendations would also apply to centrifugal fan installations and to main mine fans for drift mines. FEDERAL REGULATIONS The mandatory safety standards for underground coal mines that apply to the installation of main mine fans are listed in 30 CFR Part 75.310. Stipulations which impact the design of the fan sys- tem arrangement are contained in paragraphs (a)(l), (a)(5), (a)(6),(d), and (1) of 75.31 0: • Each main mine fan shall be installed on the surface in an incombustible housing; • Each main mine fan shall be protected by weak walls or explosion doors in direct line with possible explosive forces; • Explosion doors or weak walls shall have a cross-sectional area at least equal to the area of the return air shaft or drift opening through which the pressure from an underground explosion would be relieved; • Each main mine fan shall be offset by at least 4.57 m (15 feet) from the nearest side of the mine or shaft opening; • Automatic closing doors shall be provided to prevent possible air reversals through the fans in mines ventilated by multiple main mine fans. The installation of main mine fans underground is prohibited by 30 CFR Part 75.310, (a)(l). Providing explosion doors or weak walls in line with a possible underground explosion and offsetting the fan 4.57 m (1 5 feet) from the edge of the shaft preclude the installation of the fan directly over the shaft. In addition, 30 CFR Part 75.507-1 specifies that all electrical equipment used in return air courses be permissible, which requires locating the fan motor outside of the airstream exhausted through the fan. To comply with the Part 75.310 regulations, explosion doors are typically located directly over the shaft as part of the shaft cover or 'bonnet." A sufficiently long section of ductwork placed between the shaft enclosure and fan, equipped with a 45 or 90- degree turn, enables the fan to be offset at least 4.57 m (1 5 feet) from the shaft and the motor to be isolated from the airstream. The need for the turn in the ductwork can be eliminated by driving the fan from the discharge side, instead of from the inlet side, and providing for a 90-degree bend in the evas6. For multiple main mine fan systems, self-closing doors can be located on the inlet or discharge side of the fan. FAN SYSTEM COMPONENTS A poorly designed exhaust fan arrangement will produce turbulent conditions at the fan inlet and significant pressure losses between the shaft and fan. Field tests have shown that pressure losses through inlet ductwork at some installations may constitute as much as 30 percent of the total mine head. Unfavorable flow conditions may cause a change in the operating point on the fan performance curve, resulting in reduced fan efficiency and pres- sure generation capability. In some instances, poor airflow distribution through the fan may create mechanical stresses that lead to fan blade or fan housing fatigue failures. The objective in designing an air duct arrangement for a fan system is to provide a low cost duct that will move the air from the shaft to the fan in a uniform air distribution and with minimum energy requirements. The optimum solution is a compromise between technical and economic factors. Aerodynamic design considerations for the shaft collar and cover, fan inlet ductwork for both single and parallel fans, self-closing doors, and evas6 are discussed in the sections below. Shaft Collar/Cover To prevent excessive turbulence and non-uniform air distribution through the fan, a smooth transition for the change in direction of airflow at the top of the shaft must be provided. However, the concrete lining of the shaft is abruptly terminated at the surface at many coal mine installations (see Figure I), creating a sharp 90-degree bend. The airflow exiting the shaft becomes heavily concentrated in the upper portion of the horizontal fan in-

Jan 1, 1997

By W. Jacobi

INTRODUCTION The radon problem concerns the radiation exposure from inhaled short-lived radon daughters and the associated risk for the induction or promotion of lung cancer. In several groups of miners which were exposed in the past to relative high radon levels during their underground work, an excess lung cancer frequency has been observed. On the basis of these findings it has to be stated that the inhalation of radon daughters is the most important radiation hazard in mining. Involved in this radon problem in mines are the difficulties to measure the individual radon daughter exposure of miners and to estimate the dose to critical cells and target tissues in the lung from inhaled radon daughters. And finally the reduction of radon levels in mines confronts us with special technical problems which are difficult to solve. Thus the setting of annual limits for the radon daughter exposure of miners alone is not sufficient to guarantee an appropriate standard of radiation safety. Of same importance are the improvement of air monitoring and the optimization of technical protection measures in mines. This has to be kept in mind for the following considerations on exposure limits. The ICRP has recommended in 1959 for the first time a maximum permissible concentration (MPC) for the occupational exposure to radon and its short-lived daughters (ICRP, 1959). This MPC in air was derived from a maximum permissible dose equivalent of 0.15 Sv (15 rem) per year to the epithelium of the large bronchi which was regarded as the "critical tissue". This old MPC-value was derived using a simplified lung model which paid main attention to the dose contribution from the inhalation of unattached 218Po(RaA) atoms. Since this time more realistic dosimetric models for radon daughters have been developed; some of these models will be presented in special papers on this conference. Furthermore in the last 10 - 20 years substantial epidemiological information on the lung cancer risk among several groups of Rn-exposed miners has become available. Taking into account these epidemiological and new dosimetric findings the ICRP has adopted in March this year new recommendations on occupational limits for inhalation of 222Rn, 22ORn and theirshort-lived daughters. This report will be published this year as ICRP Publication 32 (ICRP 1981). The recommended limits for radon daughters were derived from the basic dose and risk limits as they were proposed by ICRP in its new basic recommendations (ICRP Publ. 26, 1977). In the following this basic system of dose limitation is shortly outlined before the special recommendations for radon daughters are described. [BASIC CONCEPTS AND LIMITS] The new basic recommendation of ICRP (Publ. 26, 1977) proceed from the assumption that in the dose range which is relevant for radiation protection, the risk RT of so-called stochastic radiation effects (carcinogenic and genetic effects) in a target tissue T increases proportionally with the mean dose equivalent HT in this tissue: RT = aT HT. If several target tissues are irradiated the total individual (stochastic) risk is given by the sum of risks in these tissues: [R = ?TRT = ? T aT HT]. Thus this concept of individual health detriment takes into account the risk contribution from each relevant tissue. It replaces the old concept of the critical tissue, which neglected the exposure of other tissues. Applying this new concept a dose quantity can be defined which is proportional to the total individual radiation risk from stochastic effects. This so-called "effective dose equivalent (HE)" is given by the sum of the weighted dose equivalents in the relevant tissues: [HE = E wT HT with E wT = 1 T '1] The weighting factor wT of each tissues follows to wT = aT/awB, where awB is the total stochastic risk coefficient for a uniform irradiation of the whole body. For the lung as a single organ comprising several target tissues, the ICRP recommends a total weighting factor w = 0.12 (ICRP 1977/79). This concept of risk or detriment, respectively, has important consequences. To meet the objectives of radiation protection the new ICRP-system of dose limitation is based on the following three principles: 1) The justification of practices involving radiation exposures; no pratice shall be adopted unless it produces a net benefit. 2) The ALARA-principle that all exposures shall be kept as low as reasonably achievable; this requires the optimization of the level of protection. 3) The limitation of individual exposure (annual dose limits). It is important to note that the dose limits for individuals are only one part of this system of dose limitation. Furthermore, these limits cannot be regarded as a boundary between safe and unsafe. They have to be interpreted as the lower boundary of an unacceptable exposure region. This means that in addition to the observance of these basic dose limits it is demanded to optimize the level of protection. Consequently the optimized exposure levels or the corresponding operational limits will be normally lower than

Jan 1, 1981

By H. B. Probst

Mechanical twins were produced in zone-refined tungsten single crystals by explosive working at room temperature. These twins are parallel to (112) planes and have irregular boundaries rather than the classical plane twin boundaries. These boundaries aye grooved surfaces in which the grooves themselves are parallel to a <111> direction and the sides of the grooves appear to be par-allel to (110) planes. TWINS were produced in tungsten single crystals by explosive working at room temperature. These twins differ in character from any previously reported for tungsten; however, they are similar to those found in molybdenum after compression at -196°C.1 Deformation twins "resembling Neumann bands in ingot iron" have been observed in tungsten by Bech-told and Shewmon.2 This observation was made with sintered polycrystalline tungsten pulled in tension to fracture at 100°C and using a strain rate of 2.8 x 10-4 sec-1. More recently Schadler3 found deformation twins in zone-refined tungsten single crystals pulled in tension at -196"&apos; and -253°C. These tests were conducted using a strain rate of 3.3 x l0-4 sec-1, and the twin bands were found to be parallel to a (112) plane. Deformation twins in tungsten&apos;s sister metal, molybdenum, were observed by Cahn.4 These twins were produced by compressing small (0.7 mm) vapor-deproducedposited molybdenum single crystals at -183°C. The compression was performed &apos;by impact." By the use of precession X-ray techniques, Cahn was able to identify the twin plane as {112} and the shear direction as <1ll>. Mueller and Parker1 produced deformation twins in polycrystalline electron-beam-melted molybdenum by compression at -196°C. Their "loading rate" was 5000 psi per min which, judging from their stress-strain curve, corresponds to a strain rate of approximately 0.3 x 10-4 sec-1. These twin bands were found to be parallel to (1 12) planes; however, they differed in appearance from previously observed twins. In place of straight and parallel twin boundaries they were found to be irregular, jagged, and sawtoothed. The sides of the saw teeth were identified as (110) planes and irrational planes of a (111) zone. The twins observed in the present work in tungsten single crystals are similar in appearance to those of Mueller and Parker in polycrystalline molybdenum. The starting material used in this investigation was 3/16-in. diam commercial tungsten rod produced by powder-metallurgy techniques. This material was converted to a single crystal by the electron-bombardment floating-zone technique.= The process was carried out in a vacuum of 10-5 mm of Hg using a traversing speed of 4 mm per min. Segments (=2 in. long and 3/16 in. in diam) of two crystals (A and B) produced in this manner were studied. Crystal A received one zoning pass, while crystal B received two passes. The two crystals were explosively worked at Bat-telle Memorial Institute in the following manner. A 1/2-in.-thick layer of plastic was applied to the crystals to serve as a buffer in an attempt to prevent cracking. The composite, crystal and buffer, was then wrapped with 1/8-in.-thick DuPont sheet explosive EL506A2 and detonated in water at room temperature. Metallographic samples of the worked crystals were prepared, and back-reflection Laue X-ray patterns were obtained using unfiltered molybdenum radiation. RESULTS AND DISCUSSION Blasting the crystals as described above failed to prevent cracking. The crystals fractured into several fragments about 3/16 to 1/2 in. long; however, the fragments were of sufficient size to be useful for the subsequent study. The diamond pyramid hardness of the crystals after blasting was in the range 430 to 450 as compared with 340 for the as-melted material, which shows a definite hardening resulting from plastic deformation. These hardness values were obtained using a 1000-g load and taking readings only in sound portions of the crystals free of cracks. The crystals exhibited profuse twinning as shown in Fig. 1. No such structure is present in the as-melted condition. Most of these twins have jagged twin boundaries and are similar in appearance to those found in molybdenum by Mueller and Parker. The twins in both crystals were found to be parallel to {112} planes. This identification was made by using the conventional two-trace method. Subsequent efforts to describe these twins more fully were carried out on crystal A. If the longitudinal axis of crystal A is placed in the (001)-(011)-(Il l) basic triangle of the standard cubic stereographic projection, as in Fig. 2, then the two sets of twins shown in Fig. 1 are parallel to the (112) and (121) planes. Fig. 3 shows a schematic representation of a twin with jagged boundaries. This type of twin with a <111>

Jan 1, 1962

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The microhardness of single crystals of tungsten disilicide has been investigated by the Knoop method. The average random room-temperature hardness of the WSi, matrix was 1350 kg per sq mm. Hardness crnisotropy was noted with respect to plane and indenter orientation as determined by single-crq.stal X-rny studies. Annealing at 1600" and 1800°C decreased the average hardness to 1310 and 1230 kg per sq tnm, respectively, and produced a second phase identified by X-ray diffraction and electron-microprobe analysis to be wSio.7. Ball-impact experiwzents produced rosettes at 850°C. Optical and electron microscopy showed evidence of slip and cross slip and twinning produced by microhardness indentations. Prismatic (100), [001] slip was found and cor~elated with hardness data. THE present study was undertaken to investigate the hardness anisotropy of as-grown and annealed single crystals of tungsten disilicide. The existence of the silicide WSiz in the W-Si system has been well-established and its structure thoroughly investigated zachariasen2 found WSi, to have a tetragonal C type of structure, similar to that of MoSi, with lattice parameters a = 3.212A, Kieffer et al. studied the W-Si system and measured the density and microhardness (at a 100-g load) of both polycrystalline WSi, and WSi,.,. The values found were 9.25 g per cu cm and 1090 kg per sq mm for WSi,, and 12.21 per cu cm and 770 kg per sq mm for WSi0.7, respectively. According to Samsonov et a1.5 the microhardness of polycrystalline WSi2 is 1430 kg per sq mm (at a 120-g load). EXPERIMENTAL The WSi, single-crystal boules investigated in this paper were grown by a Verneuil-type process using an electric arc by the Linde Division of the Union Carbide Corp.6 The largest specimens were 8 mm in diameter by 16 mm long. The crystals had an average density of 9.01 g per cu cm with a tungsten • silicon content of 99.9 wt pct. The major impurities were: 87 ppm O, 41 ppm N. 54 pprn C, 500 ppm Zr, 50 ppm Na, and 50 ppm Mn. The crystals were silicon-poor, the average silicon content being 22.20 pct (stoichiometric value is 23.40 pct), and tungsten-rich, the average tungsten content being 77.70 pct (stoichiometric value is 76.60 pct). As-received single crystals were ground and analyzed by powder X-ray diffraction technique using Cu Ka radiation. Laue and layer line rotation patterns were obtained on cleaved sections of WSi, single crystals. Electron-microprobe traverses of representative crystals were done using a Phillips-AMR electron microanalyzer. Carbon replicas were used to prepare electron micrographs. This work was done with a JEM-6A electron microscope. Prior to the metallographic examination, the specimens were mounted in Lucite and then polished for short times on polishing wheels using 9-, 3-, and 1-p diamond-grade pastes. Finally they were fine-polished with Linde A powder for 24 hr on a Syntron vibratory polisher. The samples were etched with 4H 2 O:1HF:2HNO3, which is a medium fast-acting etchant. The combination 1HF:2HNO3:5 lactic acid is also a satisfactory etchant. Annealing runs for selected specimens were made at 1600" and 1800°C for 3 hr at 1.0 to 3.0 x 10-5 mm Hg. A Brew tantalum resistance furnace with WSi2 powder for setters was used. The WSi2 powder was the same as that used for the crystal growth. Temperatures were measured with a calibrated W, W-26 pct Re thermocouple and a microoptical pyrometer. Powder X-ray diffraction, emission spectrographic, and electron-microprobe analyses were done after the annealing runs. For microhardness measurements a Tukon Microhardness Tester Type FB with a Knoop indenter was used. Although measurements were taken at loads ranging from 25 to 1000 g, the 100-g load was chosen as the standard load. All measurements were taken at room temperature. Only indentations of cracking classes 1 and 2 were considered.&apos; DISCUSSION OF RESULTS Powder X-ray diffraction analysis showed the as-received crystals to be single-phase WSi2. Laue and layer line rotation patterns obtained on cleaved sections of WSi2 single crystals proved them to be tetragonal WS 2 2 The results also indicated that the c axis of the crystal was oriented parallel to the boule or growth axis. Electron-microprobe traverses across the matrix of the as-grown crystals showed them to be homogeneous WSi,. Optical and electron microscopy of etched crystals, however, revealed that they contained minute amounts of the "golden" and the "blue" second phases as opposed to the "white" or WSi2 phase. These two second phases were concentrated in inclusion and etch-pit

Jan 1, 1965

By B. H. Johnston, B. N. Doyle

Introduction In 1983-84 Kidd Creek Mines Ltd. in Timmins, Ontario, started up the second commercial zinc pressure leaching plant based on the Sherritt Gordon Mines Ltd. direct pressure leach process. The first plant using this process was that of Cominco Ltd. at Trail, B.C. (Parker, 1981; Martin and Jankola, 1985). The Kidd Creek plant was constructed to take advantage of the extra capacity that the existing purification, cell house, and casting sections had in comparison to the roasters and acid plant. In addition, pressure leaching offered flexibility in other areas such as treatment of low grade concentrates. The process design package and the detailed design of the autoclave system was carried out by Sherritt. The detailed design for the rest of the plant was done by Cambrian Engineering Ltd. under the direction of Kidd Creek. The construction and commissioning of the plant has been described earlier (Johnston, 1983). This paper describes, briefly, the application of the direct pressure leaching process for zinc concentrates and the integration of the pressure leaching plant into the main zinc plant at Timmins. It discusses some of the startup problems and changes made to the plant. The damage following a fire inside the autoclave is also described. The subsequent repair and recommissioning of the autoclave has enabled Kidd Creek to demonstrate the originally sought advantages of pressure leaching and to take advantage of their extra cell house and casting capacity to produce more zinc. Process principles The development of the direct pressure sulphuric acid leach of zinc sulphide concentrate at temperatures above the melting point of sulphur and at elevated oxygen pressure has been described in detail in a number of papers (Martin and Jankola, 1985; Johnston, 1983; Veltman and Bolton, 1980; Kawulka et al., 1975; Veltman et al., 1977). The most significant aspect of the process is that sulphidic sulphur is converted to elemental sulphur in reactions that can be simply described as follows. ZnS + H2SO4 + 1/2 O2 ZnSO4 + S° + H2O (1) FeS + H2SO4 + 1/2 O2 FeSO4 + S° + H2O (2) The rates of these reactions increase with temperature. However, at temperatures above the melting point of sulphur, 12°C, the presence of a surface active agent is necessary to prevent the occlusion of the sulphide particles by elemental sulphur and the consequent termination of the leach. The zinc that is dissolved according to reaction (1), after purification of the zinc sulphate solution, is recovered by electrowinning. The iron that is put into solution according to reaction (2) is further oxidized to the ferric state and subsequently, as the acidity decreases, precipitates as hematite or as complex basic sulphates. MINERALS AND METALLURGICAL PROCESSING Examples of this are shown below. 2FeSO4 + H2SO4 +1/2O2 - Fe2(SO4)3 + H2O (3) Fe2(SO4)3 + 6H2O - Fe2O3.3H2O + 3H2SO4 (4) 3Fe2(SO4)3 + 14H2O - 2(H3O)Fe3(SO4)2(OH)6 + 5H2SO4 (5) (hydronium jarosite) The conventional zinc process involves concentrate roasting to produce zinc oxide and sulphur dioxide. The zinc oxide is leached in spent electrolyte and the sulphur dioxide is converted to sulphuric acid. The pressure leaching process can, therefore, be used to replace conventional concentrate roasting, sulphuric acid manufacture, and atmospheric leaching with one unit operation. Integration of pressure leaching into the Kidd Creek flowsheet A block flowsheet of the Kidd Creek zinc plant, with the new pressure leach plant integrated, is shown in Fig. 1. The original plant, which was constructed in 1972, is based on standard electrolytic zinc plant technology. Concentrates are dead roasted to remove sulphur. Sulphur dioxide is treated to produce sulphuric acid. Calcine is leached in two stages using cell-house electrolyte. Iron is precipitated as jarosite and solutions are purified to remove copper, cobalt, nickel, and cadmium to provide feed for a partially mechanized cell house. Zinc is plated from solution, and the resulting cathode is melted, cast, and sold (Johnston, 1983). The integration of the pressure leaching plant into the main zinc plant is relatively simple. As shown in Fig. 1, a fraction of the zinc concentrate and spent electrolyte are fed to the pressure leach autoclave, while part of the calcine from the roaster is used as a neutralizing agent in the oxidation step along with. the jarosite leach solution. The main exit stream from the pressure leaching plant is the slurry discharged from the oxidation step, consisting of neutral zinc sulphate solution, unreacted calcine, and precipitated iron oxides. This slurry is transferred to the neutral leach step in the main zinc plant. The leach residue from the pressure leaching step, consisting of basic iron sulphate and elemental sulphur, is washed and impounded along with the jarosite residue produced in the main plant.

Jan 1, 1987