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By Klaus Schwerdtfeger

Activities of lead in Pt-Pb and Pd-Pb melts in the temperature range of 800° to 1200°C have been detev-mined from electromotive-. force measurements 202th the cells Both systems display strong negative deviations from Raoult's law. The data obtained with cell [1] were combined with available data on the activity of PbO in silica-satuvaterl PbO-SbO2 melts to calculate the standard free cnergy of formation 01- liquid PbO. FREE energies of formation of oxides and activities of components in metal and oxide melts can be determined with galvanic cells consisting of a metal phase, an electrolyte containing the oxide of one of the components of the metal phase, and an oxygen electrode. This technique has been used previously to measure the standard free energy of formation of solid sio2, 1 and activities in Fe-si, CO-si,2 Ni-Si,2 and CaO-P2O5 3 melts. The present paper reports activities in Pt-Pb and Pd-Pb melts as measured with the same experimental technique. EXPERIMENTAL METHOD General Considerations. The following cells were used: Pbl (PbO-SiO2)liquid, SiO2 Pt-Pb 1 (PbO-SiOz)liquid, SiO2solidO2 [2] Pd-Pb (PbO-SiOz)liquid, SiO2solid O2 [3] Liquid alloy and' oxide melt were contained together in a silica glass crucible of essentially the same design as described previously.1'2 The PbO-SiO2 melts are ionic conductors.' During the experiment, the silica glass crystalizes in a layer adjacent to the electrolyte. The electrolyte equilibrates with solid silica and hence attains the composition of the Si02-liquidus curve in the system PbO-SiO2 at any particular temperature. Molybdenum wires were used to establish contact with the liquid metal. The oxygen electrode, which reaches the surface of the PbO-SiO, electrolyte from above, consists of a platinum wire inserted into a ceramic tube and provided with a 2-mm-diam platinum bead at its end. Gas of known oxygen partial pressure (pure oxygen of 1 atm: air, or N2 with 1.04 pct 0,) is blown through the ceramic tube onto the surface of the electrolyte. The cell reaction is Pb (metal) + 1/2O2 (gas) = PbO (electrolyte) [4] No oxidation of platinum or palladium ("displacement reaction") occurs. This is to be expected from the noble character of platinum and palladium, but was also shown experimentally, as described in the next section. The galvanic electromotive force of the cell is given by where AG is the change in free energy for Reaction [4], E(=2) is the number of electrical equivalents necessary to form 1 mole of PbO, and F is the Faraday constant. Formula [5] is valid only if no junction potential exists within the electrolyte. Junction potentials occur only when the compositions of the electrolyte are markedly different at the electrodes. Such differences are negligible in the PbO-SiO, electrolyte, as shown in the next section. Since molybdenum contact leads are used, appropriate corrections were made on the measured electromotive forces to account for the thermoelectric effect of the Mo-Pt couple. The thermoelec-tromotive forces were measured separately with a Mo-Pt couple, and were found to vary linearly from 19 mv at 740°C to 40 mv at 1310°C with molybdenum being positive and platinum negative (cold junction at 25°C). Extrapolation of these values to higher temperatures yields values which are in satisfactory agreement with those obtained previously in the temperature range 1440° to 1630°c.1,2 The change in free energy for Reaction [4] is expressed as where chemical potentials of the species. The value of constant for a given temperature because the slag composition is fixed. Inserting [6] into [5] and using appropriate expressions for upb and uO2 the relation

Jan 1, 1967

By Robin O. Williams

The increase in internal energy as the result of deformation has been measured for lead, aluminum, silver, nickel, iron, and zirconium by using rapid, adiabatic compression. The stored energy increase is roughly Proportional to the strain; the propor-tionality constant increases rapidly with increasing melting point. The fraction of the mechanical energy which is stored increases more slowly, since the strength of the metals also increases with melting point. The values of the stored energy are considered accurate to about 10 pet. The present values appear about 50 pet larger than the more reliable published results where comparisons are possible. It is possible that this difference is due to the high strain rate used in this investigation. Immediately after deformation all these metals release energy at a rate roughly proportional to (time)-'. This release is considered to be associated with dislocation motion but in aluminum (and copper) some additional process seems to be present. This release can represent 20 pet or more of the stored energy. WHEN pure metals are plastically deformed, most of the mechanical energy is converted into heat. The energy remaining within the metal is significant in that it is the energy of the disorder produced and thus detailed knowledge of this energy is a powerful tool in understanding the nature of deformational disorder. While much effort has been expended on this problem, the amount of information available is limited. The situation as of 1958 has been carefully reviewed by Titchener and ever.' The present results have been obtained by a new experimental approach to this problem. The method necessitates high-strain rates which make comparisons with published results less certain, but a high-strain rate is an advantage in that the energy release immediately after deformation can be followed. EXPERIMENTAL PROCEDURE In the experimental method used, the internal (stored) energy is given as the difference between the mechanical work used in deforming the sample and the heat which is released (the first law of thermodynamics). The work is supplied by two identical hammers swinging freely from a fixed height, the available energy being the product of the mass, the gravitational constant, and the distance through which the center of gravity moves. The initial temperature rise of the sample represents the heat produced by the deformation. The sample temperature is determined by a small thermocouple embedded in and supporting the sample. This process can be repeated over and over to produce increased strains. Most samples are run through about five cycles to a total strain of around 0.7. Further details are covered elsewhere. The determination of the heat is dependent upon the sample weight, its specific heat, the rise in temperature, and any gains or losses to the surroundings. One is dependent on published results for specific heals (the values were taken from a collection).3 The values must be accurate to about 0.1 pet in order that they not affect the results. The best values thus do not contribute to the uncertainty, but this is probably not always the case. The accuracy of the temperature rise is limited primarily by knowledge of the thermocouple characteristics over short temperature intervals, but careful calibration eliminates this as an important factor. One can calculate readily the heat flow between the sample and hammers if the time of contact and the sample temperature are known and if there were no oil at the interface. Assuming the maximum temperature difference, upper values for this interchange have been calculated (the time of contact is determined from the decrease in sample length) and it may or may not be significant. However, no correction is colnsidered necessary because of the presence of a thin oil film which has a thermal conductivity much less than the metals. Except for the possible uncertainty in specific heat, the heat is considered to be adequately known. The mechitnical losses which are recognized as important are: 1) friction between the sample and the hammer:;, 2) the kinetic energy in the hammer suspension system which may not be entirely usable, 3) the rebound energy of the hammers, and 4) the vibration of the hammer heads. All these have been covered in detail elsewhere2 and only the more significant points are made here. The friction turns out to be small except for soft materials (lead)

Jan 1, 1962

By R. Bruce Tippin

Background Iron ore is the No. 1 metal mining industry in the U.S. with dollar value of $2.3 billion in 1984 (U.S.B.M Mineral Commodity Sunnnaries , 1985). However, during the past decade this nation's iron ore industry has been subjected to a major market depression and a correspondingly downward adjustment in output. The recent trend in the curtailment of iron ore production traces a slow-down of the country's steel industry. Both pig iron and steel production have decreased significantly over the past several years. These trends are shown in Figure 1 from data collected by the federal Bureau of Mines (U.S.B.M. Mineral Commodity Summaries, 1985; U.S.B.M. Mineral Industry Surveys 1986). The industry is presently operating at less than 60% of its annual capacity. The domestic steel industry has been forced by reduced profits or losses to close facilities, curtail operations and restructure the financial status of several corporations. Companies have been sold or are trying to sell selected properties to improve their financial circumstances. Even with such actions, many of the steel companies are in very serious straits, including the seventh largest steel company, LTV, which has filed for bankruptcy. Many of the major steel companies have financial interests in iron ore mining and thus their adverse economic conditions directly reflect those operations. Several iron ore producers have been shut down including Reserve Mining Company in May, 1986 and Butler Taconite in June, 1985. The latter recently filed for bankruptcy under Chapter 11. A1 so in mid-1986, U.S. Steel Corporation, owner of the Minntac mine and iron ore processing plant, underwent corporate restructuring. The effect on their Minnesota plant is not known at this time. An excellent summary of the interrelationship of the iron ore companies and the steel producers has been provided by Skillings (1986), and an analysis of the iron ore situation was given by Robert F. Anderson, CEO of M. A. Hanna Company, in his keynote address at the 1986 University of Minnesota Mining Symposium (Anderson, 1986). Steel imports to the United States decreased slightly in 1985 because of import restrictions, but the long-term import situation remains dim and uncertain. As shown in Figure 2, the imports averaged about 25% in 1985, and the preliminary indications are that this figure could be as high as 30% when the final 1986 information is collected by the U.S. Bureau of Mines. At best, the industry can only hope for imports to stabilize at a constant level in the near future. Although the tonnage is small, the quantity of U.S. export steel has fallen over 50%. With many other materials replacing steel , the projected demand through 1990 is expected to increase only about 1% per year. Consequently, 1986 U.S. iron ore production will probably be 15% lower than in 1985. The 41 mil lion tons of iron ore production expected in 1986 represents only 53% of the industrial capacity, which is about 74.5 mil lion tons. Over 95% of this iron ore is in the form of beneficiated pellets. Today there is not an iron ore producer west of the Mississippi River, nor is there any production in the South. The Birmingham (Alabama) iron ore industry has been shut down since 1971. The western producers ceased operations in the early 1980's. Only the taconite operations in Minnesota and the plants in the Upper Peninsula of Michigan remain as our major domestic iron ore source. The economic situation for both the iron ore producers and the steel industry can be described as confused and in turmoil. Such a condition directly impacts the iron ore processing plants' operations and plans for the future. Plant Practice At present the nation's eight major operating iron ore mines, listed below, are concentrated in northern Minnesota (Mesabi Range) and the Upper Peninsula of Michigan (Marquette Range). The only exception to the Minnesota/Michigan location is the Pea Ridge Iron Ore plant in Missouri, which is a subsidiary of St. Joe Mineral s.

Jan 1, 1986

By H. E. Cline, E. F. Koch, J. L. Walter

It has been postulated and, in a few instances shown, that some kind of dislocation structure will be present at semicoherent interfaces to accommodate small lattice mismatches. In the present study of the NiAl-Cr eutectic, regular arrays of interface dislocations are observed at the boundary between the chromium-rich rods and the NiAl-rich matrix. The networks were examined by transmission electron microscopy and selected area diffraction. The rods and the matrix have a crystallographic relationship in which all directions and planes of the two phases are parallel. The dislocation networks are cmposed of a<100> dislocations lying on the intersections of the cylinders with (100) planes. Dislocations forming hexagonal rather than square arrays are also observed at certain areas of the network. The morphology of the network is consistent with the interpretation of mismatch being accommodated by interface dislocations in the cylindrical geometry. The measured spacing between dislocations was used to calculate an apparent lattice mismatch between the phases (˜0.35 PCt)interface network energy (-140 ergs per sq cm), and network strengthening (-10,000 psi). It has been proposed by Frank and Van der Merwe1 that dislocations should be present at the boundary between two semicoherent crystallographically related phases. The role of the interface dislocations would be to reduce the internal stresses, caused by the mismatch in atomic spacing across the interface. Such dislocations have been observed at the interface between expitaxially grown films and Substrates.2-4 Interfacial dislocations have also been observed at precipitate-matrix interfaces.&apos;-&apos; Directionally solidified eutectics have been shown to have semicoherent phases1&apos; and would, therefore, be expected to have interfacial dislocations as found by Weatherly at a lamellar fault in A1-A12Cu.11 The NiAl-Cr eutectic appeared to be a promising system to examine because both phases are cubic, the lattice mismatch is small, and the phases are crys-tallographically related. Furthermore, the eutectic is easily thinned for transmission microscopy. Indeed, interfacial dislocations were observed and this report describes the nature of the dislocation networks in the boundary between the NiAl-rich ma-trix-phase and the fine chromium-rich rods.21 I) EXPERIMENTAL PROCEDURE Ingots, 3/4 in. in diam and 6 in. long were made by melting in vacuum and casting under argon using 99.9 pct pure material. The composition, in at. pct, was 33 pct Ni, 33 pct Al, and 34 pct Cr. The ingots were then placed in A1203 crucibles on a water-cooled base, melted by means of induction, and withdrawn from the hot zone at the rate of 1 in per hr under argon.* * T his material was first directionally solidified in this laboratory by E. R. Stover Slices were taken perpendicular to the growth direction of the directionally solidified ingot for metallography and for transmission electron microscopy. The electron transmission samples were thinned mechanically, then thinned electrolytically in A-2 electrolyte* *A-2 electrolyte: 62 ml perchloric acid, 700 ml ethanol, 100 ml butylcellosolve, 137 ml distilled H20. until a hole appeared in the foil. 11) EXPERIMENTAL RESULTS A) Optical Microscopy. The microstructure, viewed on a plane perpendicular to the growth direction, is shown in Fig. 1. The structure consists of cells or colonies of parallel chromium-rich rods in the NiAl matrix. The cells occur when there are impurities present12 or, in a ternary eutectic, if the composition is slightly off the eutectic composition. The axis of the chromium-rich rods is parallel to the growth direction except near the cell boundaries. Here the rods may assume angles to the growth direction; however, examination shows that the crystallographic relationship between the rod and the matrix remains the same. Fig. 1 includes cell boundaries where the rods formed at a large angle to the growth direction. The variation of rod position across the cells made it possible to Fig. 1-Structure on plane perpendicular to growth direction. Rods near cell walls are at large angle to growth direction. Magnification 315 times.

Jan 1, 1970

By D. O. Hobson, P. L. Rittenhouse

We have recently found that many lots of Zircaloy-2 and -4 tubing tested in tension deform to cross section shapes that are "polyhedral" rather than circular. The noncircular cross sections seem to result from a circumferential variation in plastic proper -ties and, therefore, in texture. We examined the diffracted X-ray intensity from (OOOl), {1010), {ll20}, and {1011} planes parallel to the tubing surface around the entire circumference. Tubing that deformed to a circular cross section showed <5 pct variation in diffraction intensity around the circumference from any of these planes. Greater intensity variations were found for all the tubing materials that developed non-circular cross sections during deformation. In each instance the number of intensity maxima and minima was consistent with the number of sides of the &apos;polyhedral" cross section. THE effects of crystallographic texture on the mechanical properties of zirconium, zirconium alloys, and other anisotropic hexagonal materials such as titanium and hafnium have been intensively studied. If the natural crystallographic anisotropy of these materials could be controlled by selected fabrication operations, a material could be produced with a texture, or preferred orientation, in which the maximum strength directions are in the stress directions of the structure. The permissible stress levels of the structure could then be increased. Rittenhouse and Pickle-simerl have shown that highly textured Zircaloy-2 plate can vary from 52,000 to 70,000 psi in tensile yield and from 62,700 to 122,000 psi in compressive yield strengths as a function of specimen orientation. Similar texture effects have been observed in Zircaloy tubing, whose mechanical properties differ depending upon whether the tubing has basal poles predominantly radial or tangential and upon the mode of testing. These same texture effects might be troublesome if the texture in the tubing is not uniform around the tube walls. This paper is concerned with the effects of nonuniform texture on the strain behavior of commercial Zircaloy tubing. BACKGROUND Previously, various lots of commercial Zircaloy tubing were tested under selected stress conditions as part of a program to determine the four quadrants of the yield locus. One of the testing procedures was uniaxial tension and it is the influence of texture variations on the tensile deformation behavior of the tubing that is of interest here. The effect of texture on the strain behavior in tubing is very apparent from a uni-axial tensile test.2 This behavior is illustrated schematically in Fig. 1 for three different tubing textures: 1) basal poles predominantly in the radial direction; 2) basal poles predominantly in the tangential direction, and 3) basal poles equally distributed between the radial and tangential directions. In the first example most of the grains are oriented for prism slip to operate to allow axial lengthening and diametral reduction of the tube. Reduction in wall thickness requires {1122} twinning, a more difficult operation than slip.* In the second example, the texture is such that *The singleCrystal analogy will be used quite often in this paper when strong texturesare being discussed. The textured material is assumed to react as if it were a single crystal aligned in the same orientation and under the same stress system as the predominant texture._____________________________________________ prism slip operates to give axial lengthening and wall thinning. Diametral reduction requires twinning and again should be more difficult to accomplish. A specimen with basal poles equally distributed between the radial and tangential directions should exhibit about equal diametral and wall strains.* Table I shows the *Diametral strain is accomplished by a combination of circumferential and longitudinal strains. But, for the purposes of this paper, it will be considered as a strain causing a change in the length of a specified diameter.__________ strain behavior of two lots of tubing with different textures. The first tube has a texture with basal poles equally distributed between the radial and the tangential directions. The ratio of true thickness strain to true diametral strain is almost unity. The second tube has a predominantly radial basal pole texture and it is apparent that most of the total strain has occurred by diameter reduction, just as one would predict. There is over three times as much diametral strain as thickness strain. RESULTS We found that specimens from certain lots of commercially fabricated tubing did not retain round cross sections during uniaxial testing. Instead, the speci-

Jan 1, 1970

[The following notations will be used: O an ore body. z a point in O. z&apos; another point in O. w0 (z) a point support of infinitely small dimensions w0 centred in z. w (z) a sample (or block) of finite dimensions kv centred in z. W (z) a block of size W greater than or equal to w. W&apos;(z) a block of size W&apos; greater than or equal to W. W" (z) a block of size W" greater than or equal to W&apos;. x (z) value of the regionalized variable x with support wO at point z. p (z) average value of x in w (z). pw WZ) = E[x(z&apos;)l zt in w(z) pw (z) average value of x in W (z). pwl (z) average value of x in W&apos; (z). pwU (z) average value of x in W" (z). Note that pW (z), pw (z), pwf (z) and pw,, (z) are (regular- ized) regionalized variables with support w, W, W&apos; and W" respectively. The relative sizes of wO, w, W&apos;, W" and O are represented schematically in Fig. 7.1. The variance of pw (z) when w (z) takes all possible positions in O is known as the dispersion variance of w in O and is denoted by a? (w in O) or a\: 0; = a2(w in a = Ew,z, inn {[p~ (z) - p121. (7.1) For convenience, the following simpler notation will be used: a> Ew in n [(p w - pl21. Consider now a large block W (z) in O with average value p~(z), and all the possible smaller blocks (or samples) w (z&apos;) of size w in W (z). We can calculate the variance of the blocks w (z&apos;) in the block W(z), which is the dispersion vaciance of w in W (z), from the relationship a2 [w in W(z)l = Ewcz,, in W(Z) {[PW (z&apos;) -pw (z)l21. (7.2) Provided the intrinsic hypothesis is satisfied (§3.4.4), this variance is a function only of the dimensions of the supports w and W, and is independent of the position z of the block W (z). We can therefore define the dispersion variance of w in W, as follows: u2 (win W) = Ew in w [(ptti - PW)~]. (7.3) In cases where the intrinsic hypothesis is not satisfied, the variance of samples w in blocks W may vary only slightly from block to block, so that the average dispersion variance of w in W (z) for all possible W (z) in O can be used: ayw in W) = Ew(,, ~n n {a2 [W in W (z)]}. (7.4) The following example will help to illustrate the importance of the variance of dispersion. Assume that we plan to develop a bedded coal deposit Q. We consider mining the ore body with only one giant dragline, which will extract each day a block of coal of size W&apos;. The total area mined in a year will have a size W". We want to know whether this scheme is acceptable, given that the daily variation in ash content must not exceed a given percentage specified in the sales contract, which is renewable on a yearly basis. On a given day, if we mine the block W&apos; (z), the ash content will average pwT (z). In a period of one year, the expected daily variation in ash content is measured by the expected variance of pwf (z) in W", i.e. by a2 (W&apos;in W"). An alternative mining method might be to use two smaller draglines, each one mining W&apos;/2 of ore per day, and Wn/2 per year. If the draglines are used to mine two distinct sections of the deposit, the expected daily variation in ash content will be u2 (W&apos;/2 in Wj1/2)/2 Other situations, where economic decisions cannot be made without knowledge of the dispersion variance, are illustrated in § 7.4 and 7.5 below. Remark: The notation a2 (w in W) is used in this publication because of its clarity. An alternative notation, which is increasingly accepted in the literature, is s2w/W. ]

Jan 1, 1978

By R. H. McLean

Jet impingement produces two mechanisms to clean the bottom of a borehole during jet-bit drilling operations. One is an impact-pressure wave in the immediate area of jet impingement. The other is crossflow, which spreads across the bottom away from the pressure wave. Measurements of the vertical distribution of the cross-flow at several positions beneath a 4 3/4-in. tricone jet bit in a laboratory model show that the maximum velocity in the crossflow is directly proportional to the square root of the product of the rate of flow and the velocity of the jets through the nozzles (QV). Other measurements in the laboratory model show that gradients in the impact-pressure wave are directly proportional to the jet QV if the diameters of the nozzles are held constant. Consistency of the basic relationships through changes in the Reynolds numbers of the jets from 31,000 to 93,000 suggests that the laboratory results should be representative of typical flow in field operations having higher Reynolds numbers. Estimates of the impact-pressure waves under conditions other than those in the jet-bit model may be made by comparison with a less complex model—impingement of a jet against an unrestricted flat surface normal to the jet. Equations derived from current jet technology describe the wave in this simple system for a wide range of conditions. INTRODUCTION The efficiency of rotary drilling operations is strongly linked to the efficiency with which cuttings are removed. Cuttings remaining on the bottom of the borehole will impede further penetration by the bit until they are removed. Wasteful regrinding is prevented if the fluid circulated past the bit removes cuttings as rapidly as they are made. Most investigations of bottom-hole cleaning under bits have been concerned with the rate-of-penetration effects of bit type, nozzle configuration, fluid properties, pressure gradients and utilization of hydraulic horsepower. These investigations have shown that drilling muds, weighted to keep the pressure in the borehole greater than in adjacent formations and carrying material which forms a filter cake, apparently plaster cuttings against the bottom, making them difficult to remove. In addition to a demonstration of the factors causing poor cleaning, the most significant result of these previous investigations has been the increased use of jet bits accompanied by better hydraulic programs and better selection of drilling fluids. Undoubtedly, these practices have improved bottom-hole cleaning, but rates of penetration when drilling with muds are still often lower than would be expected with perfect cleaning." Although there is general agreement with the concept that increasing hydraulic energy at a jet bit often increases the rate of penetration by improving cleaning, research workers have differed as to the best criterion for evalyating hydraulics. Some lean toward maximizing the product of the rate of flow and the velocity through the nozzles (QV) others prefer to maximize the hydraulic horsepower at the bit;&apos;"-&apos; "till another says that neither criterion is universally suitable."&apos; This controversy shows that conclusive field evidence has not established the superiority of either of these criteria. Analysis of the fluid flow which cleans the bottom should contribute to resolving the controversy. Impinging jets clean the bottom by creating two mechanisms capable of dislodging cuttings. One is the impact from the momentum of the jet and the other is the flaw parallel to the bottom away from the area of impingement. The impact force appears in the form of a pressure wave on the bottom and, in this paper, is called the impact-pressure wave. The flow parallel to the bottom is called crossflow. Fig. 1 illustrates these two mechanisms. This paper describes crossflow and the impact-pressure wave beneath jet bits and relates them to controllable parameters. Through these relations, criteria for use in designing hydraulics to achieve maximum use of the mechanisms of cleaning are derived. PROPERTIES OF CROSSFLOW CONCEPTS DEVELOPED IN PREVIOUS INVESTIGATIONS Concepts of scavenging the bottom by crossflow have been well discussed by Bobo, et al." They examine the means by which crossflow may create forces on cuttings and conclude that the cleaning action of crossflow can be increased by increasing the velocity of the flow stream close to the bottom. Using boundary layer theory, they indicate that a reduction in the viscosity of the drilling

Jan 1, 1965

By Hsun Hu, R. S. Cline

The formation of annealing textures during the course of recrystallization in 2 pct Al-Fe crystals rolled in the (111) [112], (112) [111], and (112) [Till orientations has hem studied in detail. When the rolling texture is composed of both (111) [121] and (001)[110] components, the annealing texture consists of mainly (110) [001] and (113) [332] components. As the (001) [110] component diminishes from the surface to the interior of the rolled crystal, the relative concentration of the (113) [332] component in the annealing texture decreases accordingly, whereas that of the (110)[001] component increases with the (111)[112] component in the rolling texture. Such dependence of the annealing texture on the composition of the rolling texture is in accmdance with the oriented growth mechanism. Grain-growth characteristics during recrystallization, hence the annealing texture, can he considerablv different in (112) [111]-type crystals depending sensitively on the initial orientation of the crystal. In a previous publication,&apos; the formation of rolling textures in 2 pct A1-Fe single crystals with initial orientations of approximately (1ll)[112], (112)[111], and (112)[111] was studied in detail. The deformation texture of these crystals consisted of either a single (111)[112] or a combination of (111)[112] and (001)[110] components in various concentrations. For the (lll)[112] crystal, the deformation texture was a single (lll)[112] up to 70 pct rolling reduction, but it became (lll)[112] plus (001)[110] after -90 pct reduction. For the (112)[113.]-type crystals, the relative concentration of the (111)[ 112] and (001)[110] components varied with the depth below the surface of the crystal, as well as with the amount of deformation. These series of specimens, having deformation textures with a range of concentration of the (111)[112] and (001)[110] components, could therefore be used for a thorough investigation of the effect of deformation-texture components on the formation of annealing textures. In a study of rolling and annealing textures in Si-Fe crystals, Dunn and Koh3 noted that the addition of a (001)[110] component to the (111)[112]-type deformation texture had practically no effect on the recrystallization texture.* According to the ori- ented growth mechanism for the formation of annealing textures, nuclei related to the deformation texture by approximately 30-deg rotation around a common [110] axis have the highest rate of growth and the resulting annealing textures generally have such an orientation relationship with respect to the deformation textures.314 It was reasoned by Dunn and Koh3 that if the oriented growth mechanism operated the recrystallization texture developed from a deformation texture containing both (111)[112] and (001)[110] components should be strongly centered around (113)[332], because (113)[332] is approximately midway between the (111)[112] and (001)[110], and is related to both of these two orientations by [110] rotations of 25 to 30 deg. Hence, nuclei of (113)[332] orientation should have a high rate of growth in the deformed matrix. However, their results were not in accord with this prediction. It was felt by the writers that a detailed study was needed to clarify the effect of deformation-texture components on annealing-texture formation. For this reason, the present investigation was conducted. EXPERIMENTAL PROCEDURE Specimens used for the present investigation were taken from the crystals rolled previously for deformation-texture studies.&apos; In order to follow the progress of annealing-texture formation during the course of recrystallization, a single specimen was taken from each rolled crystal and its textural changes examined after successive anneals until recrystallization was complete. The specimen was carefully cut from the rolled strip with a jeweler&apos;s saw. Prior to annealing, the sawed edges were etched to remove distorted metal, while both faces of the specimen were protected from the etching solution by acid-proof plastic tape. After annealing, the specimen was etched from the "bottom" face only (the reference or "top" face of the specimen was protected by plastic tape) to one half of its original thickness, so that the texture at the surface and at the central section of the strip could be determined by the reflection technique. The

Jan 1, 1965

By Kenric C. Owen

INTRODUCTION Situated 23 miles east of Pretoria the Premier Mine started diamond production in 1903. Two years later it produced the largest diamond yet discovered, the 3 106 carat Cullinan stone. For the period to 1932 when the mine was closed down due to economic circumstances, open cast mining was practised using inclined rope haulage traction and by this time had produced 48.5 million carats of predominantly industrial quality diamonds from 148 million tons of ore. In 1945 it was decided to re-open the mine using underground mining methods. A system using long hole benching was devised (Hodgson and Sewel 1960). This system was later modified but still forms the basis for approximately fifty percent of production. Following the successful introduction of block caving on associated diamond mines in the Kimberley area (Gallagher and Loftus 1960) this mining method was introduced to the Premier Mine in the late 60&apos;s and now accounts for nearly 50% of production. This paper will discuss block caving at Premier Mine in the light of our experience and discussion will be directed to the main geological and structural features of the orebody and host rocks and the related constraints imposed on the mining methods. Reference is made to the long hole benching mining method for comparative purposes. GENERAL DESCRIPTION OF OPERATIONS The ore from the block caving and bench mining areas gravitates via ore passes to a twin haulage, 500m below surface. Electric 13 tonne locomotives, each hauling a train of 10 Granby type cars, deliver the ore to two 42" x 48" (1.06m x 1.22m) jaw crushers. The ore is reduced in size to minus 0.15m before being hoisted to the treatment plant on surface. Hoisting is done with 12.5 tonne bottom discharge skips in a five compartment rectangular shaft using two 3 240 H.P. semi automatic Ward Leonard winders. A small single drum service winder operates in the other compartment. Men and materials travel in a separate shaft in a 5,4m x 2,8m cage operated by a Koepi winder. These two shafts are also the main intake airways to the mine. The two main extraction fans capable of 250 m3/s at 3,2 kPa are situated on surface and are connected to the underground workings by an incline and a network of air passes and return airways. GEOLOGY Although there are numerous occurrences of kimberlite bodies in the district, the Premier Mine kimberlite pipe is the only economic orebody. It is roughly oval in shape with surface dimensions of 900m on the long axis and 450monthe short axis. The surface area is 320 000 m2. The kimberlite has intruded a massive body of felsite and norite which is intersected by a number of faults. The contact between the kimberlite and host rock is clear cut and dips inward at an average angle of 80°. Cutting across the pipe and the country rock is a 75 metre thick gabbro sill, the top of which intersects the pipe below the 347m level and dips at 15&apos; to the north west. The kimberlite has been metamorphosed a distance of some 20m both above and below the sill contacts. Age measurements on biotite from the gabbro date the sill as 1 115 million years, thereby providing a minimum age of the pipe. (Pre Cambrian). All other pipes in South Africa are of Cretaceous age (60 million years). A simplified geological plan and section of the Premier Mine orebody is shown in Figure 1. It is thought that the kimberlite intruded in at least three distinct phases. The kimberlites of these different phases can be distinguished most easily by their characteristic colour. BROWN KIMBERLITE. This is the oldest kimberlite and forms a crescent shape in plan on the south eastern side of the pipe. In depth it increases in relative area. Although the brown kimberlite carries the highest diamond grade in terms of carats per ton all the various kimberlites in the Premier pipe are economic to mine.

Jan 1, 1981

By Leslie W. Austen

ROTARY kiln operators will agree that some of the most severe conditions a refractory must stand occur in the hot zone of a kiln burning Portland cement, dead burn dolomite, magnesite, peri-clase, and similar materials. Frequently the operator is faced with factors beyond his control which drastically shorten the life of refractories. Shutdown due to mechanical failure can be serious if the period is of sufficiently long duration to cause the dropping of coating or the loosening of the lining. A change in slurry can affect the coating and cause ring buildup. A change in type of fuel and its effect upon the flame can cause a shift in location of the hottest zone. Weekend shutdowns or any other interruption can cause the operator trouble and may damage the refractories, since stopping and starting a rotary kiln is certainly more difficult than stopping and starting a motor. Some operators have tried to set an estimate of damage for each shutdown in equivalent days of running time. Conditions affecting the refractory may be roughly grouped in four classes: chemical attack, mechanical stress, thermal shock, and abrasion. Chemical Attack: The drive to obtain maximum production through a kiln demands maximum operating temperatures, temperatures which are limited more by the ringing up or melting of the clinker. This can cause interface temperatures at the junction of coating and refractory which require the use of a basic kiln block to withstand the chemical attack. Chemical changes take place within the refractory itself, especially in chemically bonded or unburned kiln blocks. These changes cause the formation of the ceramic or burned bond. Migrating liquids or fluxes from the kiln charge have an effect within the refractory and lead to mineral or glass formation. The alkalies, sodium and potassium, migrate into the refractory as silicates, chlorides, sulphates or other salts. They may move under capillary action or may be caused to move by volatilization with condensation in the cooler portion. Mechanical Stress: Concentrated stress may be caused by several factors or combinations thereof. I—The rings of refractories must be kept tight and rigid within the kiln, and this alone demands considerable force to hold the blocks in place. So that the force will not be concentrated, the blocks should fit the circle as perfectly as possible, with the faces in contact overall. 2—As the kiln is heated, thermal expansion takes place at the hot end of the kiln block. Since this disturbs the plane face it too can cause a concentrated stress at the two ends of the block, and shearing stress can be set up within the brick itself because of the difference in expansion between the two ends. 3—If a lining becomes loose and moves in the shell very severe stress can be set up, and as the kiln rotates this load changes and gives the effect of repeated loading. Permanent expansion of the refractory can also cause severe loading. 4—Not least important, flexing of the kiln is frequently the cause of concentrated stresses. Thermal Shock: Thermal shock, the result of heating and cooling too rapidly, occurs on starting and stopping or when a large patch of coating drops, exposing the bricks. Again, its destructive effect is often the result of phase change, liquid to solid or the reverse; dense refractories loaded with glass-forming impurities are particularly susceptible. Thermal shock is a. problem with refractories set in the wall or roof of a stationary furnace, and becomes even more serious in a rotary kiln, the tendency to spa11 being magnified with movement and concentration of stress. Uniform rate of feed and loading insures both better coating and a more uniform stress. Abrasion: If the refractories do not take a coating, abrasion can become a most destructive factor. Movement of the lining in shell or movement of loose blocks causes abrasion, which is also most destructive if the refractories do not take a coating. An analysis of the problem of basic lining for the hot zone reveals, therefore, a number of desirable characteristics: high refractoriness, basic chemical reaction, resistance to spalling, good strength at all stages, ability to take coating, true sizing, volume stability, and abrasion resistance. Increased demand

Jan 1, 1953

By H. L. Hartman

The drop tester has proved an invaluable tool for the investigation of percussion drilling in the laboratory in "slow motion". It has allowed the process of rock penetration by impact to be studied a single blow at a time. In the present work, the relation of cratering to indexing has been determined under conditions simulating those in the bottom of the hole at atmospheric pressure. Indexed blows form craters which are influenced by others adjacent to them. Two unique effects are involved: (1) the provision of additional free faces in proximity to the point of impact and (2) the creation of subsurface damage by the previous blow(s). Both have a pronounced influence on the volume of rock removed per blow, which governs the rate of penetration in actual drilling. The emphasis in this study was placed on determining effects of index distance and impact energy on crater volume when blows were struck on a previorusly "drilled" or damaged surface, a situation most representative of down-hole conditions. The results indicated that (I) the optimum index distance on a damaged surface is greater than on a fresh, undamaged rock surface; (2) the volume of rock broken at optimum index distance is about the same for both surface conditions with die-shaped chisels but tends to be greater on a cratered surface with wedges; (3) the optimum index distance and maximum crater volume are proportional to the energy level; (4) at a given energy level, the volume of rock broken by dies generally exceeds that by wedges; and (5) maximum crater volume varies, approximately, inversely with width of die but is nearly independent of included angle of wedge. INTRODUCTION This is the third of a series l,2 of papers reporting on one phase of a continuing program of drilling research being conducted in the Rock Mechanics Laboratory at The Pennsylvania State U. The phase under consideration is crater geometry — blow energy relations in percussion drilling. While the previous papers have discussed mainly craters produced by single blows, indexed-blow studies are the subject of this paper. The basic mechanism of drilling under study here — that of penetration of a chisel-shaped bit subjected to impact — is the one employed in probably 90 per cent of all rock drilling in mining, percussion drilling. It also forms the fundamental action in nearly all oil well drilling with the so-called rotary (roller-bit) method. Here, the action is more complex, however, and may in actuality comprise rotary-percussion drilling. Certainly, the down-hole air and mud hammer drills, which superimpose percussion on rotation, belong in this latter category. In any event, impact blows constitute one of the principal mechanisms in the vast majority of drilling, mining or petroleum, and it is essential in drilling research to study percussion in all its basic aspects. Percussion drilling can be simulated in the laboratory by means of an impact drop tester. Striking one blow at a time with chisel-shaped bits, the drop tester permits study of most of the parameters in the drilling process except blow frequency and the interrelationship of certain variables. Single-blow craters, the simplest to produce, allow the determination of basic relationships, such as volume vs blow energy; while indexed craters most closely resemble the action in real drilling and provide data for the establishment of optimum operating criteria. Indexed-blow craters are those which are influenced by others in proximity. The simplest case to visualize, and the one studied in detail here, is that in which a given crater is formed adjacent and parallel to a previous crater, such that the second crater breaks into the first. A more complex situation usually exists downhole, where indexing is achieved by rotation of a radial-winged or rolling-cutter bit. But, admittedly, the phenomenon of indexing is more likely to be understood eventually if it is first studied in its simplest form, that related to parallel craters. Limited research has been conducted on indexed blows. The most complete study was that by Simon, 3,4 who proposed universal indexing curves to relate the important variables. His work, however, was conducted entirely with rows of craters formed on a

By E. J. Dulis, R. M. Fisher, K. G. Carroll

IT is well known that ferritic steels containing more than 15 pct Cr when subjected to temperatures in the range of 700" to 1000°F exhibit increasing hardness and decreasing ductility. The phenomenon has been widely termed the "885 °F embrittlement," after the temperature of most marked effect.&apos;.&apos; In view of the excellent review articles available in the literature3-6 only a brief account of experimentally established facts need be given here. The extent of changes in physical characteristics during embrittlement depends on chromium concentration and time at temperature, higher alloy content and longer time both promoting more rapid and extensive changes. In a 27 pct Cr steel, changes in impact strength and in angle of fracture in bending can be detected after only a 1 hr exposure at 885°F; after 50 hr this steel becomes quite brittle. Hardness increases slowly with time during thousands of hours exposure and may attain a maximum hardness number twice as large as that of the unexposed steel. Microstructural changes accompanying embrittlement have been described as an initial widening of grain boundaries followed by eventual darkening of ferrite grains. Embrittled steels etch more readily, e.g., the weight loss of a 27 pct Cr steel in acid solution may occur at a rate one hundred fold greater following exposure at 885 OF. Marked changes which accompany embrittlement have been observed in electrical resistivity, specific gravity, and magnetic coercive force. Changes in physical properties may be readily removed by heating at temperatures above the embrittling range, such as a treatment at 1100°F for 1 hr. It has frequently been noted that the 885 °F embrittlement suggests precipitation on a submicro-scopic scale of a chromium-rich constituent, the nature of which has not been revealed by X-ray diffraction. Progressive broadening of the body-centered cubic diffraction lines during embrittlement has been observed," and recent observations by Lena and Hawkes&apos; upon single crystals have shown early asterism in X-ray photographs, disappearing within an hour at 900 °F. Many workers have ascribed8-13 the phenomenon to a precipitation of a phase (FeCr), which is known to cause embrittling effects at temperatures much higher than 885°F. Two general observations, however. suggest that a precipitation cannot be responsible for the 885°F phenomenon: 1—prior cold work greatly enhances a formation, whereas it scarcely affects the 885 °F embrittlement, and 2—the presence of an alloying element such as nickel or manganese may have an effect on the 885 °F embrittlement which is opposed to its effect upon a formation. The slight enhancement of a formation and 885°F embrittlement observed in the presence of elements with strong carbide and nitride forming tendencies&apos; is probably a consequence of lessened chromium depletion of the matrix. The bar graph in Fig. 1 shows a typical example, taken from two 27 pct Cr steels used in this work, of the hardness after exposure for 10,000 hr at 900°, 1050°, and 1200°F. Steel A (0.03 pct C, 3.13 pct Mn) showed marked hardening at 900" and 1200°F, whereas steel B (0.12 pct C, 0.63 pct Mn) exhibited only the 900°F hardening. The cr phase was found in steel A at the higher temperatures but not in steel B. Presumably a formation is enhanced by the low-carbon and high-manganese concentrations in A," Thus there are two distinctly different hardening phenomena present which cannot both be ascribed to v precipitation without invoking a transition phase possessing remarkable properties. Materials A number of chromium steels exposed for long periods (5000 to 34,000 hr) at 900°F, as well as unexposed samples of one of the steels, were available for this investigation. Table I gives the chemical compositions and aging treatments of these steels. In addition to these steels exposed in the elevated temperature test furnaces of the National Tube Division, a number of high-chromium steels were heated for short periods in small laboratory air furnaces and lead baths. Supplementing these commercial steels, a sample of high-purity (0.018 pct C, 0.002 pct N) 28 pct Cr iron, exposed 1000 hr at 887°F. was furnished by the Union Carbide and Carbon Corp. In addition, an alloy of iron and chromium of high purity containing 46 pct Cr was used. This

Jan 1, 1954

By J. F. Pierce, S. M. Enterline

Since January 1959 a zinc refiner of novel design has been in operation at Blackwell, Okla., producing 99.995+ zinc from the output of the Blackwell horizontal retort smelter. The refiner is a continuously operated, pyro-metallurgical unit with principal dimensions horizonhl permitting one floor operation. It is very ruggedly constructed. Furthermore it is not subjected to deterioration from high concentrations of iron in the feed metal because the boiling units are separate from the rectification columns and constructed with silicon carbide brick arches through which the heat is transferred radiantly to the zinc. A zinc refiner of novel design has been in operation since January 1959 at the Blackwell, Okla. plant of the Blackwell Zinc Co., Inc., a wholly owned subsidiary of American Metal Climax, Inc. Developed by the company&apos;s technical and operating staffs, the new refiner produces special high-grade zinc (nominally 99.995+ pct Zn) from the prime western1 slab output of the Blackwell horizontal retort smelter. The refiner is a continuously operated, pyromet-allurgical, high-capacity unit employing fractional distillation to separate zinc from its impurities, consisting principally of lead, cadmium, and iron. In prime western slab, these elements may vary in concentration from 0.005 to 1.6 pct. Table I shows the impurities usually encountered in the Blackwell prime western metal fed to the refiner together with their boiling points and vapor pressures at 907oC. The commercial pyrometallurgical smelting processes for extracting zinc from ore include distillation from retorts and a limited degree of refining can be accomplished by redistillation in similar retorts. To achieve special high-grade purity, an impractical number of batch redistillations would be required, however, with an accompanying loss of much metal. A continuously operated and integrated unit is required in which fractional vaporization and condensation can take place in a large number of stages. The first commercial continuously operated unit was developed by the New Jersey Zinc Co.4 In the separation of any two substances the degree of separation is limited if a mixture exists having a constant boiling point. The Zn-cd5 and Zn-pb6 systems contain no constant boiling points and hence these metals may be separated to any degree of purity. Basically, the pyrometallurgical refining of zinc involves three steps: a) iron, copper, and other metals having no appreciable vapor pressures at 907ºC concentrate in the bath when the impure zinc is boiled, b) lead, bismuth, antimony, and other metals having boiling points above but closer to that of zinc are selectively condensed from the vapor boiled from the bath, and c) cadmium and other metals having lower boiling points than zinc are fractionally distilled by reboiling and subsequent condensation of the zinc from the vapor. The boiling and condensation of zinc must be conducted in vessels constructed of materials which are refractory at the temperature involved (907 ºC) and it is highly desirable that they also be resistant to attack by the various metals. This requirement dictates construction from relatively small, simply shaped pieces which limits the pressures which may be employed to avoid leakage through the numerous joints. Stresses induced must be limited essentially to compressive ones and suitable provision must be made to permit thermal expansion of the components in order to minimize these stresses. Where heat is to be added for boiling or removed for condensation, refractory material through which the heat flows must have a high thermal conductivity. Silicon carbide is highly conductive but is subject to attack by iron and is expensive compared to other commonly employed refractories. A hard, dense aluminous fireclay is well suited to contain these metals where high thermal conductivity is not required. Zinc will penetrate the pores of fireclay brick but only to a limited depth in an exterior wall and has little effect other than an increase in weight and conductivity. The design objectives of the Amax refiner were: a) to achieve a long life by heavy, rugged construction and by employing silicon carbide refractories only where required for heat conductivity and not in contact with liquids of high iron concentrations, b) to simplify operation, manning and control by essentially horizontal construction, and c) to obtain high capacity in a single unit. DESCRIPTION Flow of metal through the Amax refiner is shown diagrammatically in Fig. 1 and schematically in Fig. 2.

Jan 1, 1963

By U. N. Bhrany, J. H. Brown

The specifications of particle size and the size analyses of fine particulate materials are commonly presented without reference to the method of analysis. A review of the various sizing methods showed that not only numerous sources of error but also different definitions of size are inherent in the different methods of analysis. To demonstrate the magnitude of the differences, the size distribution of finely crushed quartz was determined by several methods and a critical comparison of the data was made. The experimental results show that appreciably different sizes may be indicated for one material depending on the method of analysis used. However, because the shape of the size-distribution curves determined by almost all methods was constant, a simple method of correlating the data can be adopted. Conversion factors, by which size measurements obtained by the various methods can be expressed in terms of screen sizes, are presented as one method of correlating the results. The size analysis and size specification for lump rock and particulate materials are commonly determined with sieves. With this technique, a readily reproducible measure of size can be obtained merely by duplicating the sieve and the method of sizing. For coarse materials, such as lumps of rock, this technique is simple and effective; and the effects of properties of the material such as shape can be readily understood. When very small particles are measured, however, problems arise. Small sieves are difficult to construct and maintain, and size separations become sensitive to the analytical procedure. For these difficult sieve sizes and for still smaller particles, other sizing techniques employing, for example, sedimentation, light extinction, and microscopy are available. Because these various techniques employ different size-dependent responses to establish size, it is appropriate to examine them and the results they yield to determine their relationships and their limitations. The &apos;size&apos; of a lump of rock is not an absolute quantity, but rather a defined one. With sieves, for example, the size is defined by the screen aperture and no reference is made to the actual shape of the particle, yet only in the case of a regular body, such as a sphere, can the sieve size be related to the shape. With sieves only two dimensions of a particle can be suggested, for the sieve makes no allowance for the length of the particle passing through an aperture. Similarly, the size of a particle as measured by a microscopic technique need bear no relationship to the size as measured by sieves, although the two measurements may be related statistically. In fact, all size measurements are not only defined quantities, but the measurement actually used is an average that is controlled by the technique employed and, hopefully, reflects the property in question of the material of interest. Many papers have been presented that illustrate the accuracy of the various sizing methods, present the advantages of certain methods for certain applications, and describe the principles and technical backgrounds of the various methods. No attempt will be made in the present paper to review this work in detail. The purpose of the present paper is to examine the limitations of the various sizing methods, and to demonstrate experimentally the relationships between the sizes as determined by the various methods of analysis. It is hoped that by recognition of these limitations and relationships, errors in size specification and size interpretation will be avoided. REVIEW OF SIZING METHODS In specifying the size of a material, not only the data but also the method of measurement must be stated. For example, the size of the lump might be specified as its total volume, as its weight, as its maximum dimension, or as its minimum cross section; any one definition might be completely satisfactory for one problem, but not for another. In practice, size analyses follow four basic approaches and fortunately, the conditions that restrict each approach are known. These major methods include: 1) screen analysis, 2) direct measurement of particle dimensions, 3) determination of equivalent spherical size in response to fluid flow, and 4) specific surface determination. Each of these techniques has several variations and some new techniques are also available, but the limitations of the basic techniques are sufficient to permit at least a preliminary

Jan 1, 1962

By C. K. Dumbauld, B. E. Morgan

The need for a low-strength cementing composition for use in well cementing is reviewed and results are presented of laboratory and experimental field tests of a modified cement having a controlled ultimate tensile strength of approximately 200 psi. The modified cementing composition may he prepared from either high early strength or normal portland cements by the addition of bentonite clay and a suitable agent for dispersing and controlling the set of the slurry. Substitution of the modified cement for conventional slow-set cements may give better completion results in many wells because the modified cementing composition has lower set strength, lower slurry density, and greater slurry stability than conventional cement slurrieh. The lower ultimate strength allows greater penetration with less shattering of the set cement when perforating casing and cement. The lower elurry density allows the placement of longer columns of cement slurry, and the greater slurry stability reduces the possibility of having an uncemented section caused by the settling of cement particles before the cement set.. INTRODUCTION High strength lias always been one of the accepted criteria of a good cement. During the early use of portland cement in well cementing. emphasis was placed upon securing cements with higher strengths. In 1931, Barkis&apos; reported that, "Normal oil well cements have been improved to develop greater strengths and uniformity of product, which has aided in producing successful jobs in cementing the deeper strings." As long as most wells were completed by the open-hole method. the use of cements having high strengths seemed desirable, and there was no objection raised against high-strength cementing compositions. For a number of years. how-ever, the industry has been completing a large numher of wells by setting and cementing casing through productive horizons and then obtaining production by gun-perforating the section of casing opposite the desired interval. Although this method has been generally successful, difficulties have been experienced in some cases in completing or recompleting wells because of apparent lack of adequate penetration by the bullets through the casing and surrounding sheath of cement and into producing formation. In addition to the penetration trouble: there have been indications that fracturing and shattering of the set cement by perforating might he a contributing factor in causing the failure of some jobs to exclude water or gas from oil producing zones. The possibility that cements having high set strengths were contributing to til difficully ill obtaining satihfartory perforating results has re. ceived attention during recent years. Gun perforating tests conducted in 1944 showed that the depth of bullet penetration into set cement varied with the hardness of the cement, the greater the strength of the cement the less being the penetration. In 1946, Farris2 pointed out that high strength cements were not needed in well cementing, and in 1947, data published by Oliphant and Farris3 showed that set cement was perforated without shattering at approximately 150 psi tensile strength. whereas at approximately 300 psi tensile strength severe cracking and shattering occurred. Oliphant and Farris suggested that wells be perforated at the proper time interval after placement of the cement so that the set cement would have the desired strength. Several difficulties may he encountered in trying to perforate a cement job at the correct time to catch the tensile strength near 150 psi. The rate of strength development of different cements varies considerably. This fact is illustrated by results of tensile strength measurements presented in Fig. 1. These data show that at 175°F the tensile strengths of three conventional slow-set cements varied from 75 to 235 psi at the end of 12 hours. After 24 hours, the tensile strengths varied from 200 to 455 psi. The rate of strength development is affected. also. by the temperature of the forniation, and this adds to the uncertainty of perforating at the rorrect time, since accurate well cementing temperatures may not he known in many cases. Furthermore, in the recomple-tion of wells it is sometimes necessary to perforate cement which has set for a long period and has developed maximum or final strength. In view of the apparent need for a cementing composition having a controlled ultimate strength, an investigation was

Jan 1, 1951

By A. Kenneth Schellinger

THE terms surface tension .and surface energy are well known when applied to liquids and are generally described by referring to the excess energy of the air: liquid interface as a result of unsaturated molecular forces surrounding the surface molecules of the liquid due to the presence of the air phase on one side. Such unbalanced forces produce the familiar water droplet of spherical form and are generally summed up as a surface tension measured in dynes per centimeter which can be shown mathematically to be equal numerically to a corresponding surface energy expressed in ergs per square centimeter. A specific surface energy, however, is best thought of as the energy necessary to produce one unit of new surface on a substance. Hence, in producing a bubble in a flotation cell the impeller must supply surface energy corresponding to the air: liquid interfacial area on the interior of the bubble. Inasmuch as it is relatively easy to extend or contract the surface of a liquid, there are a number of successful methods for liquid surface tension, or energy, measurement based upon surface deformation. This happy state of affairs does not, however, extend to solids, which are considered to possess surface energies for the same reasons as do liquids, i.e. because of unsaturated ionic bonds at the solid gas interface. As in the case of the flotation cell producing surface on liquids as new bubbles, it takes energy to produce new surface on solids as new particles. As every mill man knows, this surface is produced on mineral solids in a grinding mill by the action of a tumbling mass of iron balls. But here so much energy usually is wasted by the inefficient action of these balls that a large amount of heat is generated, and the surface energy production may be easily confused with the energy necessary to produce this ineffective heat. The tumbling balls and fracturing minerals ultimately take their energy from a rather large electric motor. It has been variously estimated that from 10 to 20 pct" only of this energy from the motor does not appear as heat and may be presumed to appear as surface energy on the minerals present.. Such a production of new surface on the mineral phases is accompanied, of course, by a size reduction that is inevitable as more and more mineral interior molecules become surface molecules by the fracture exposure. This size reduction of mineral particles, although the most obvious feature and perhaps the sole object of the milling operation, is from this energy viewpoint the outward manifestation of the production of surface energy only. Measurement of the characteristic surface energies of pure minerals and their various mixtures in ores would be a step towards understanding of the energetics of the commercial grinding operation. In addition, the characteristic surface energy of a mineral is probably a physical property specific for that mineral, and therefore, from a scientific standpoint, should be measured. It is interesting to note that, in contrast to the large body of work on the surface tensions of liquid systems and biological systems, the field of solid surface energies has been neglected. Prior to. 1920 it is difficult to find more than one or two references to work on solid surface energies in Chemical Abstracts. Since 1920 such references number somewhat less than 100, while those on liquid systems are numbered in the thousands. Much of this apparent neglect of the field of solid surface energies (the term is intended to be somewhat inclusive at this point and refers both to the solid: gas, and the solid: liquid interface) is because of the lack of a reliable method of measurement rather than any lack of scientific curiosity. It was, and still is, difficult to produce new surface on a solid without the simultaneous production of interior changes in the same solid which may consume part of the energy used. The extension in the surface area can be measured, but the interior crystal-

Jan 1, 1952

By A. Stanley, J. C. Mead

The MacIntyre Development of the National Lead Co. is located at Tahawus, N. Y. The operations involve the mining and concentrating of a titaniferous iron ore to produce an ilmenite concentrate and a magnetite concentrate. Construction of the MacIntyre plant was commenced during the summer of 1941,when world conditions threatened to cut off the supply of Indian ilmenite. An open pit mining operation was developed and the crushing and milling equipment put in operation in July 1942. A general description of the operation was given in the Adirondack Issue of Mining and Metallurgy for November 1943. The metallurgy of the mill operation was described by Mr. Frank R. Milliken,* Plant Manager, National Lead Company, MacIntyre Development, and presented at the AIME New York Meeting, February 1948. The magnetite concentrate produced in the milling operation was too fine (minus 20 mesh) to be used directly in iron blast furnace operation, and most of the magnetite had to be stockpiled in 1942 and 1943. In 1943, the Defense Plant Corp. built a Greenawalt sintering plant at Tahawus, N. Y., to put the magnetite concentrate in a more suitable form for use in the iron blast furnace. The Greenawalt sintering plant consists of three 10 by 25 ft sintering pans designed to produce 1800 gross tons of sinter per 24 hr. The vacuum to each pan is produced by two Greenawalt fans in series, pulling approximately 30,000 cu ft of air per minute at 50 in. water gauge vacuum. The plant started operation in August 1944. The present plant production averages 25 tons per operating pan hour (approximately 224 lb per operating hour per square foot of grate area) of plus 1 in. sinter. Raw feed to the plant consists of 61 pct magnetite, 4 pct anthracite coal culm, and 35 pct minus 1 in. return fines which are conveyed to a pug mill where the materials are mixed thoroughly and water added to give the mixture 5.5 to 6 pct moisture. The mixed prepared feed is conveyed to two 4 by 10 ft vibrating screens where the minus 1 in. plus 5/8 in. return fines are screened out and discharged into a surge bin for use as a hearth layer. The minus % in. prepared feed is discharged into another surge bin for use as prepared feed. A charge car, electrically operated, having a capacity of one charge of prepared feed and several charges of hearth layer, lays a thin layer of plus 5/8 in. return fines and 9 1/2 in. depth of prepared feed into the pans. A fluffing roll and a vibrator on the car fluffs and spreads the prepared feed into the pans. An ignition car, electrically operated, ignites the top of the bed with a 30 sec flash burn. The 9 1/2 in. bed sinters in approximately 13 min. Dumping the pan, and recharging and igniting the bed requires 2 min. To improve the quality of the ilmenite concentrate produced in the mill and to reduce the amount of titanium dioxide lost in the mill tailings and in the magnetite product, extensive research work and pilot plant operations have been done on grinding the crude ore to minus 65 mesh size (rather than to minus 20 mesh) and concentrating it by a combination of magnetic separation (for magnetite recovery) and flotation (for ilmenite recovery). These tests have proved successful in increasing ilmenite recovery and grade. With the development of the ilmenite flotation process to a stage where a full scale flotation plant was in the design stage, the problem arose of handling the 65 mesh magnetite concentrate that would be produced. In order to study and solve the problems of handling and sintering the 65 mesh magnetite in the sinter plant, a pilot sinter plant was plus from John E. Greenawalt. The effect of using 65 mesh magnetite in the sintering operations was then studied on the 2.4 sq ft test pan, operating under conditions as similar to the large plant as could be set up in the laboratory. A series of tests were run in the test pan on present sinter plant feed that had been mixed in the plant pug mill. An average production and an average quality of sinter produced in this series

Jan 1, 1950

By C. A. Doh, R. Q. Fields, M. Lebourg

A formation tester run on logging cable is now available to the oil industry. It offers a method of safely and rapidly testing possible producing formations in uncased holes. These tests can be made up the hole after running the electric log. Reservoir pressure data is continuously recorded at the surface as the fluid sample is extracted. The tester may be assembled with a reservoir of 1-, 2.75-, or 5.5-gal capacity. A retaining pad on the body of the tool is expanded against the wall of the hole at the exact depth desired; this depth is determined by electrical log control. Two bullets are then fired through the center of the retaining pad which create a connection between the formation and a flow line to the sample chamber. When the chamber is filled, a valve is closed and the fluid sample sealed at maximum pressure. The tool is retracted to minimum diameter and brought out of the hole. Electrical circuits permit a complete recording at the surface of the mechanical operations of the tool as well as the formation pressure build-up and the hydrostatic mud pressure. The tool was introduced commercially during the latter part of 1955 in the Gulf Coasts of Louisiana and Texas. Over 1,000 operations have been made to date (Sept. 1, 1956); 50 per cent of which resulted in successful tests. Failures have been due mostly to ineffective sealing in unconsolidated sands. One major company had 41 successful tests out of 80 attempts with 23 ineffective pad seals. Results for this company were very gratifying as to pinpointing gas-oil ratios, indicating productive permeabilities and aiding in determination of fluid content where electrical log and side-wall coring information were inconclusive. Eight typical pressure curves are discussed (including misruns). Six types of fluid recoveries are interpreted. Eight actual field examples of electric logs, showing the problems solved by the formation tester, are illustrated. The present applications of the tool are discussed: 1. Determination of productive fluid—varticularlv differentiating between gas and oil. 2. Determination of reservoir pressure as an aid to: (a) safety in completion technique, (b) reduction in drilling costs, and (c) reservoir analysis. 3. Determination of minimum gas-oil ratios. 4. Location of gas-oil or oil-water contacts. 5. Recovery of samples for examination and analysis: oil (gravity); gas (hydrocarbon content); water (salinity). Additional applications envisioned for the future are also given: (I) subsurface exploration based on accurate pressure, (2) recovery of fluid samples from the undisturbed reservoir for PVT work, and (3) possible quantitative study of permeabilities or productivity index. Running the formation tester requires no special pre-cautionary measures. Because full hydrostatic mud pressure is maintained at all times, well depth is no problem. Thus, the method allows safe, economical testing in wells which heretofore could only be tested by setting casing. INTRODUCTION A new method of safely and rapidly testing possible producing formations in uncased holes is achieving considerable success. The method offers promise of further advances in reservoir study. Called the formation tester, the new instrument is unique in that it operates on logging cable. It thus offers all the advantages of wire-line operations and becomes an important adjunct to present logging and side-wall coring services. The tester is operated against the wall of the hole at any depth desired. Zones to be tested are usually determined by a study of the electrical and the micro-caliper surveys. Reservoir data, as well as the operating cycle of the tool in the hole, are continuously recorded at the surface during the operation. The tester, as it was originally designed, was capable of recovering a 1-gal sample of reservoir fluid per trip in the hole. Tools with reservoirs of 2.75- and 5.5-gal capacity are now available. The 5.5-gal reservoir is equipped with a segregating system, set before going in the hole, so that the last portion of the recovery (usually 1 gal) is automatically separated from the first portion. This makes it possible

Jan 1, 1958

By Leslie W. Austin

ROTARY kiln operators will agree that some of the most severe conditions a refractory must stand occur in the hot zone of a kiln burning Portland cement, dead burn dolomite, magnesite, periclase, and similar materials. Frequently the operator is faced with factors beyond his control which drastically shorten the life of refractories. Shutdown due to mechanical failure can be serious if the period is of sufficiently long duration to cause the dropping of coating or the loosening of the lining. A change in slurry can affect the coating and cause ring buildup. A change in type of fuel and its effect upon the flame can cause a shift in location of the hottest zone. Weekend shutdowns or any other interruption can cause the operator trouble and may damage the refractories, since stopping and starting a rotary kiln is certainly more difficult than stopping and starting a motor. Some operators have tried to set an estimate of damage for each shutdown in equivalent days of running time. Conditions affecting the refractory may be roughly grouped in four classes: chemical attack, mechanical stress, thermal shock, and abrasion. Chemical Attack: The drive to obtain maximum production through a kiln demands maximum operating temperatures, temperatures which are limited more by the ringing up or melting of the clinker. This can cause interface temperatures at the junction of coating and refractory which require the use of a basic kiln block to withstand the chemical attack. Chemical changes take place within the refractory itself, especially in chemically bonded or unburned kiln blocks: These changes cause the formation of the ceramic or burned bond. Migrating liquids or fluxes from the kiln charge have an effect within the refractory and lead to mineral or glass formation. The alkalies, sodium and potassium, migrate into the refractory as silicates, chlorides, sulphates or other salts. They may move under capillary action or may be caused to move by volatilization with condensation in the cooler portion. Mechanical Stress: Concentrated stress may be caused by several factors or combinations thereof. 1-The rings of refractories must be kept tight and rigid within the kiln, and this alone demands considerable force to hold the blocks in place. So that the force will not be concentrated, the blocks should fit the circle as perfectly as possible, with the faces in contact overall. 2-As the kiln is heated, thermal expansion takes place at the hot end of the kiln block. Since this disturbs the plane face it too can cause a concentrated stress at the two ends of the block, and shearing stress can be set up within the brick itself because of the difference in expansion between the two ends. 3-If a lining becomes loose and moves in the shell very severe stress can be set up, and as the kiln rotates this load changes and gives the effect of repeated loading. Permanent expansion of the refractory can also cause severe loading. 4-Not least important, flexing of the kiln is frequently the cause of concentrated stresses. Thermal Shock: Thermal shock, the result of heating and cooling too rapidly, occurs on starting and stopping or when a large patch of coating drops, exposing the bricks. Again, its destructive effect is often the result of phase change, liquid to solid or the reverse; dense refractories loaded with glass-forming impurities are particularly susceptible. Thermal shock is a problem with refractories set in the wall or roof of a stationary furnace, and becomes even more serious in a rotary kiln, the tendency to spall being magnified with movement and concentration of stress. Uniform rate of feed and loading insures both better coating and a more uniform stress. Abrasion: If the refractories do not take a coating, abrasion can become a most destructive factor. Movement of the lining in shell or movement of loose blocks causes abrasion, which is also most destructive if the refractories do not take a coating. An analysis of the problem of basic lining for the hot zone reveals, therefore, a number of desirable characteristics: high refractoriness, basic chemical reaction, resistance to spalling, good strength at all stages, ability to take coating, true sizing, volume stability, and abrasion resistance. Increased demand

Jan 1, 1952

By N. Piret, B. Shoukry, S. Buntenbach

Traditional or artisanal goldmining, also known as small scale goldmining, has a strong and probably a negative environmental impact. The processing methods applied are very frequently a source of severe pollution due to the emissions of mercury by the extraction of gold by means of amalgamation as well as the emissions of cyanide through cyanide leaching of gold bearing ores. The emissions find their way into the environment and contaminate soils, sediments, water and atmosphere. Abnormal concentrations of mercury and cyanides in waterways are known to occur year after year destroying irreplaceable regions of the world. Mercury and cyanide compounds are highly toxic and may directly create permanent damage to the whole ecosystem. Existing methods for recycling of mercury and for decontamination of mercury and cyanide contaminated tailings are not customary applied in small scale mining and are ineffective as well. Based on investigations of traditional and small size goldmining, this paper presents: -processing methods of gold and discarded tailings under consideration of environmental protection; -figures on actual situation; -recommendations for equipment; -some decontamination methods for mercury and residual cyanide. Mineral Processing methods in traditional gold mining Gold is usually existing in its ores as the metal alloyed with metallic silver and perhaps copper. The element may occur in the form of: -native gold -inclusions also of microns or submicroscopic size metal sulfides (auriferous) such as pyrite, pyrrhotite, stibnite, arsenopyrite and galena -combined as telluride or sulphotelluride. The separation process selected depends on whether the gold can be freed from its unfavorable associations (e.g. gangue) at a sufficiently coarse grain-size, or whether it is carried in a heavy sulfide which can be freed similarly. The usual practice is to concentrate the goldbearing mineral at a relatively coarse grain-size and to regrind the ore if necessary. The gold content is concentrated by secondary or tertiary gravital methods or is extracted by chemical methods (amalgamation, cyanidation etc.) Gold, even when of fine grain-size, settle readily due to its high specific gravity from pulps in which the main gangue mineral is quartz or silicates. Amalgamation is the process of separating gold and silver from their associated minerals by binding (entrapping) them into a mixture with mercury. The cyanide process is applied to separate gold or gold-bearing compounds by dissolution from the finely ground ore (CIP, CIL, RIP), or as heap leaching. The dissolved gold is separated from the solids and the metal-rich or pregnant solution is then treated to recover its gold. Gold is also recovered by flotation methods. This process is widely used in treating base metal ores and in separating various sulfide components of ores, as well as in removing the barren gangue. The gold usually associates with a specific product in a sequence of flotation operations and is recovered subsequently in the smelting of the sulfide concentrates and refining of the metallic products, or by cyanidation of the roasted concentrates. Froth-flotation can be applied to separate gold and sulfide minerals from a finely ground pulp. The Amalgamation Process Amalgamation is the main method for the recovery of gold in traditional mining and is applied for the extraction of gold from placers as well as primary ores. The mineral technology used depends on the nature of ore deposits. In winning gold from solid ore, the matrix of minerals and rocks must be crushed and ground to sufficient fineness to liberate the gold. The liberated gold could be treated similar as free gold from placers. Gold is mainly separated from the valueless gangue (barren rock) by utilizing the difference between the density of the impure native metal (density about 16-19) and the gangue (density about 2.5). In simple operations the material is carried by a stream of water down a sluice generally equipped with small transverse barriers (riffles) against which the gold collects. The riffled sluice is the principal device used by artisanal gold miners. Nowadays, spirals as well as centrifuges, such as Knelson separator or Falcon separator, are occasionally applied for gold recovery. Gold may also be recovered from the pulp, by passing it over corduroycovered tables that catch the heavier particles - a method maybe as ancient as gold mining itself. In history, sheep skins were used to catch gold particles in this manner. Furtheron, gravity separation of gold is practiced on jigs, hydraulic traps, shaking tables and

Jan 1, 1995