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Jan 1, 1912

By E. A. G. Colls

Discusses corrosion in Trail chemical plants producing ammonia, sulphuric, nitric and phosphoric acids, ammonium phosphates, sulphate and nitrate, together with miscellaneous allied material problems and their solution using erosion or corrosion proof materials. Conclusion, that for work of this nature, most costly material may well be cheapest in the long run.

Jan 4, 1950

By R. T. Southin

Cast ingots of 99.99 pct purity A1 and aluminum/copper alloys containing up to 2 pct Cu have been found to contain four zones rather than the three previously accepted, i.e., chill, colummar, and equiaxed zones. The fourth zone consists of a coarse dendritic layer across the top surface of the ingot which is open to the atmosphere. It is also found that the grains in the equiaxed region have a "cornet" shape, with a head which is coarsely dendritic and a tail which grew with the same structure as the columnar grains. Experiments using mechanical barriers, and others involving the elimination of the surface dendrile layer, have indicated that nucleation of the equiaxed zone is caused by the showering of dendritic particles from this surface dendrite layer. These particles are the dendritic heads found in the comet grains. A mechanism of nucleation and growth of these comet grains is put forward. Experiments with a number of other metals and alloys suggests that these conclusions may apply generally to ingots cast without the addition of nucleating agents, and solidified under normal conditions. THE macrostructure of cast ingots may contain the following three zones: i) a peripheral zone of fine equiaxed grains, commonly called the chill zone; ii) a zone of columnar grains extending inwards from the chill zone; iii) a central zone of equiaxed grains; these are normally larger than the chill grains. All three zones are not necessarily present in any particular ingot since their existence and magnitude depend upon the casting conditions and composition of the cast material. The mode of formation of zones i and ii is fairly well understood. However, the cause of the central equiaxed zone remains a matter of conjecture. Previous theories put forward to explain the mechanism of nucleation in the equiaxed zone have been examined by Chalmers1 and Winegard.2 At the time when the present work was carried out the most re -cent hypothesis was that due to Chalmers,1 who recognized more fully than previous workers that conditions in this zone during solidification were not conducive to nucleation. In his hypothesis, he suggested that nuclei were formed near the mould wall during the very early stages of solidification, and that they can drift into the central zone by convective motion. This was supported by evidence from experiments using mechanical barriers to stop the drift of nuclei. A similar hypothesis had previously been put forward by Genders.3 More recently, Jackson et al. 4 have observed that dendrite arms in organic compounds can melt off during solidification. They have postulated that this occurs in metals and alloys, and that the dendrite arms which have been freed from the main dendrite act as nuclei for the equiaxed zone. In the present work, critical metallographic examination has shown that there is a fourth zone in the macrostructure of cast ingots which is a dendritic layer over the top surface of the ingot. It is also shown that there is a relationship between this zone and nucleation of the equiaxed zone. EXPERIMENTAL DETAILS The alloys examined were prepared from super -purity aluminum of 99.99 pct min purity (spectro-graphically detected impurities of Cu, Fe, Si, and Mg) and copper of 99.98 pct min purity (spectrographically detected impurities of Si, Zn, As, Fe, Pb, Bi, Ni, Sn, Mn, Ag, Cr, and Al). Three compositions of ingots were examined, containing 0.0, 0.1, and 2 pct Cu, respectively. The alloys were melted in an alumina-lined salamander crucible using a medium-frequency electric induction furnace; when the appropriate casting temperature was reached, the alloys were cast without degassing or fluxing treatment. The mould used was made of electrode graphite and had the following dimensions: external diameter 6 in., height 9 in., with a mould cavity 8 in. deep and a diameter tapering from 5 in. at the top to 4 in. at the bottom. Casting temperatures used were generally in the order of 70" to 90°C above the liquidus and the mould was at room temperature before casting. Inserts kere placed in the mould cavity in some experiments. These consisted of either an 18-g stainless-steel tube of 2 in. diam held axially in the mould i in. off the bottom and extending 1 in. out of the top of the mould or a "trap-door" barrier of stainless-steel gauze of 24-mesh held horizontally in the mould 31/2 in. down from the top. The construction of this insert is shown in Fig. 1. All inserts were preheated prior to casting to prevent chilling. RESULTS The macrostructures of ingots of the three compositions are described, in terms of the three generally recognized zones, in Table I, and illustrated in Figs. 2(a) to (c). The most interesting observation in this table is that relating to the shape of the equiaxed grains, which were not in fact equiaxed but of almost tear-drop shape. Closer examination of these grains showed that each consisted of a head which had a coarse dendritic structure and a tail which always grew in the opposite direction to heat flow, and which had the same structure as that of the columnar material of the ingot concerned; i.e., in the pure aluminum and 0.1 pct Cu alloy it was cellular and in the 2 pct Cu alloy it was cellular-dendritic. Identification of original cast grains was greatly hampered in the super-purity aluminum ingots, and to a lesser degree in the 0.1 pct Cu alloy,

Jan 1, 1968

D EC. 20-The spirit of Christmas and good will toward men has managed a few brief appearances on the front pages, welcome relief from man's usual ill-will toward man. A couple politicos did their best to brighten the scene by well-publicized romances. There was a general exodus to Florida to patch up nervous systems, and even the UNO quieted down as Mr. Vyshinsky departed for home via Eastern Germany. Before going he opened up a preliminary bombardment for the worldwide "communist peace offensive," and it is now the duty of the 600 million (according to the Cominform) ideological converts to press home the attack. In Washington, Mr. Lilienthal resigned as Chairman of the Atomic Energy Commission and demonstrated again the difficulty of government to retain the services of capable men. The President has yet to appoint another victim- possibly someone nicely noncontroversial and timid. So might the critics be appeased, but it would bode ill for the rapid exploitation of peaceful uses of atomic energy, the relaxation of excessive secrecy, wider sharing of developmental work with friendly nations and possible revision of the Acheson-Lilienthal proposals for inter- national control of the atomic bomb.

Jan 1, 1950

By J. J. Van Nouhuys

THE economics of aerial survey and the technical processes by the aid of which vertical and oblique aerial photographs are turned into line maps showing the most profuse topographical detail such as contours, rivers, roads, plantations, habitations and cultivated lands do not concern us here. They have been ably and exhaustively described in the publications of the British War Office, handbooks on surveying methods and on photogrammetry and in the South African mining, engineering and geological press. Suffice it to mention that for geological interpretation vertical photographs are used on such scales as 1/5000 to 1/10,000, overlapping each other by 55 to 60 per cent in the direction of flight and some 10 to 20 per cent sideways on to the next sequence or strip. Through this duplication in the overlap the stereoscopic examination becomes possible. The standards by which monochrome aerial photographs are interpreted can be grouped under the following headings: 1. Continuity.-The continuity of topographic relief not obtainable on the ground owing to the smallness of man relative to that relief. Here lies the greatest value of aerial survey with relation to geology. An immediate alignment can often be made of drainages running in different directions on each side of a hill; saddles and gorges in the mountainsides; abrupt termination of outcrop or indubitable signs of faulting. Most conclusive evidence is thus often obtained about faults which may be perfectly visible at one place on the ground but cannot elsewhere be identified because of decreased throw. Similarly, dikes can often be followed notwithstanding frequent interruption and disappearance under the soil. Scattered outcrop in scrub-covered or bush-covered country can be compared with field work. The same applies to geological contacts. Once these have been 3stablished at a few points on the ground, the intervening stretches can be drawn in.

Jan 1, 1937

By P. Ramakrishnan, Ramjilal

Fine powders of lead zirconate titanate have been prepared by three different methods such as ball milling, conventional coprecipitation and spray drying. Different powders have also been prepared by changing the process variables in each method. These powders were analysed for particle size chemical composition and reactivity. DTA, TGA and x-ray analysis have been carried out to study the lead zirconate titanate formation with reference to calcination temperatures. The calcined powders were then consolidated by compaction and sintering. An attempt has bean made to explain the consolidation behaviour of these powders on the basis of powder characteristics.

Jan 1, 1980

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

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

Jan 1, 1968

By Nicholas J. Grant, William H. Ferguson, Bill C. Giessen

Ta-lr alloys have been examined over the complete range of compositions using metallographic and X-ray techniques. The terminal solid-solubility limits, solidus temperatures, and intermediate phases were determined. There are four inter-mediate phases: o, tetragonal, analogous to a (Fe-Cr); 0,. orthorhombic; az, tetragonal; and a TaZr,, cubic, AuCu, structure. Of these, o and a, melt peritecticaLly, a, decomposes peritectoidally, and a TaIrs has a congruent melting point. Three peri-tectic and one eutectic reactions occur. 1 HE Ta-Ir phase diagram has not been treated in the literature. Intermetallic phases and terminal solid solubilities have been described and estimated.'-4 The previous findings have been confirmed in this work. A complete diagram with additional phases and solidus curves is presented. EXPERIMENTAL METHODS Starting materials were tantalum powder of 99.8 pct purity, supplied by the National Research Corp., Cambridge, Mass., and iridium powder of 99.9 pct purity, supplied by the Bishop Co., Malvern, Pa. Both powders were -200 mesh. Table I lists the analyses as given by the suppliers. A standard procedure was employed in making the alloy buttons, which was described in detail in Refs. 5 and 6, and which included repeated arc-melting of powder compacts and determination of the composition by the weight-balance method. This is especially justifiable due to the similar vapor pressures of tantalum and iridium. In the critical parts of the diagram, a spacing of 1/2 at. pct was used, based on premelted master alloy material. The observed structures and X-ray spectra were consistent with the composition sequence of the alloys. Table II lists the final alloy atomic percentages with the calculated percent error of composition. Cross sections representative in grain size and composition were selected for the study, as described in Ref. 5. Based on prior experience, no contamination from the tungsten electrode was considered. Temperature measurements were obtained using a Leeds and Northrup optical pyrometer and have been described extensively in Refs. 5 and 6. All heat treatments were made in the high-vacuum tantalum tube furnace mentioned in Ref. 5. Samples annealed in tantalum containers cooled from 1800" to 1000"~ in 5 sec; those annealed in ceramic crucibles cooled over the same range in 15 to 30 sec. The thermal treatments are listed in Table 111. All specimens were homogenized at 1735°C for 24 hr. Tantalum-rich compositions were treated in tantalum buckets. Iridium-rich compositions were annealed in tantalum buckets below the eutectic temperature of 1950°C; up to 2200°C, tungsten-lined tantalum baskets were used; and above 2200°C thoria crucibles were used. It was found that refractory oxides (in early stages of the investigation alumina crucibles were used up to 1800°C and thoria crucibles were used to 2400"~) give off minute amounts of oxygen and thereby influence the microstructure considerably, or react directly with the alloys.

Jan 1, 1963

By L. H. Robinson

A proposed method of drilling utilizes sequential detonation of two types of explosive charges delivered to the hole by a conventional drilling fluid through pipe. A shaped charge first produces a long thin hole. A second charge, called a gauging charge, is pumped into the thin hole, explodes, and enlarges it to full gauge. In one suggested configuration, the explosives are contained in cylindrical capsules 4- to 5-ft long. A drilling head is positioned 2- to 3-ft off bottom. When a capsule is pumped to the bottom of the hole and stops, pressure inside the drill pipe increases and differential pressure detonates the explosive. Primacord along the length of the capsule disintegrates the capsule. The debris circulates out of the hole with the drilling fluid. The gauging-charge action was examined using 2-ft cubes of Berea sandstone. The sandstone (18 per cent porosity) was vacuum-saturated with water and surrounded by concrete. To prevent reflected tensile pulses, the acoustical impedance of the concrete matched that of the sandstone. A 750-psig pressure was applied to a drilling fluid within a shaped-charge-formed hole before detonating the gauging charge. In these tests, 190 gm of rock were removed for each gram of explosive detonated. A similar series of experiments on low-porosity (0.40 per cent) metamorphic limestone provided a more rigorous test. Extensive fracturing from the gauging-charge action prevented an estimate of the volume of the expanded hole. The diameter of the hole was irregular, ranging from about 2 to 4 in, or about fivefold larger than the hole created by the shaped charge. INTRODUCTION In the past, explosives have found a varied but somewhat limited use in the oil field. An early well stimulation technique, still in use today, in vo lves shooting ni troglycerin to en large the borehole and to increase matrix permeability near the wellbore. Bullets and jets are now the conventional method of perforating casing and tubing. Detonations are frequently used to "back off" or "shoot off" stuck pipe and, of course, seismo-graphic work has long depended on explosive-generated pulses to find attractive earth structures. Efforts to use explosives in drilling operations have received limited examinations1-3 which, in one respect, is surprising because explosives offer one way to transmit large amounts of energy directly to the bottom of the hole. Recently, Ostrovskii l described a Russian method of drilling with explosives that utilizes small capsules containing explosives which are pumped into the mud stream to the bottom of a borehole. As the capsules leave the end of the drill pipe, a detonation mechanism is armed. Impact detonates the explosive. In another configuration, two liquids (an oxidizing agent and fuel) in the capsule are separated by a frangible membrane. Separately, the liquids are nonexplosive. Near the bottom of the drill pipe, the capsule passes through a narrow constriction which ruptures the membrane. The mixing of the liquids produces an explosive. Impact is again used to detonate the explosive. About the time Ostrovskii was developing his method, Humble Oil & Refining Co. was independently doing research on another explosive drilling concept based on the sequential detonation of two types -of explosive charges. The proposed technique consisted of alternately pumping a shaped charge and then a "gauging charge" down a well. The shaped charge should drill a long, tapered hole, and the gauging charge should expand it to full gauge. This paper presents the visualized drilling concept and gives results of laboratory work which showed that sequential firing of charges can form hole at an attractive charge-to-rock removal ratio. An important finding was that increased environmental pressure, which is to be expected in wells, increases rock removal efficiency of the gauging charge.

Jan 1, 1966

By Archer E. Wheeler, Milo W. Krejci

The Boston & Montana Reduction Works at Great Falls, Mont., was formerly the reduction works of the Boston & Montana Consolidated Copper & Silver Mining Co., and continued as the reduction plant for the independent company until June 1, 1910, when the consolidation of a large number of the operating companies of Butte was effected. It then became merged in the Anaconda Copper Mining Co. as the Boston & Montana Reduction Department of the Anaconda Copper Mining Co. The history of copper converting at this plant, while not covering the entire period of the commercial use of the process in this country, does cover by far the larger part of it, and as the operation of and appliances for the process have undergone many changes during the time, it may, perhaps, be of some interest to put the record of these changes into permanent form. The plan followed in the preparation of this paper has been to give first a brief chronological record of the principal events and changes and then, even at the risk of some repetitions, to give more detaild accounts of some of these changes under separate headings. The headings for the complete paper are as follows: 1. General. Chronological Review. 10. Development of Different Classes 2. Mechanical Manipulation. of Converters After Class I. 3. Casting of Finished Copper. 11. Basic Lining. 4. Tamping of Linings. 12. Number and Size of Tuyeres. 5. Early Acid Linings. 13. Cast Copper Tuyeres. 6. Acid Linings With the Use of Ore. 14. Efficiency of Air. 7. Introduction of Flux Through the 15. Size of Converter Mouth. Tuyeres. 16. Height of Converter. 8. Bottom Blast. 17. Summary. 9. Disposal of Converter Slag, General Chronological Review. Ground was broken for the general concentrating and smelting plant in the spring of 1,891. The first departments to start operations were the concentrator in March, 1892, and the Brückner roasting and reverbera-tory smelting departments in April, 1892. The converter department

Jan 1, 1914

By J. N. Maycock, P. W. M. Jacobs

Previous measurements of the thermoelectric power of ionic crystals are reviewed briefly. It is concluded that, while extensive measurerements are available on systems in which the electrode M has a cation in cornon with the sall MX, there is as yet little modern work on systems in which the metal electrode M' does not haue a calion in common with the salt. We haue now measured the thermoelectric power of- single cryslals of KC1 and of KC1 + SrCl2 between plati.nu?n electrodes over a much wider range of temperature than before. individual ionic heats of transport, which, while probably not very accurate, are of a reasonable order of magnitude, are obtained from this data on the basis of an assumption that charge carriers do not cross the electrode/salt interface. RELATIVELY little work has been done on thermal diffusion in ionic crystals. Reinhold and coworkers1-I measured the thermoelectric power and Soret effect in silver and cuprous salts and their mixed crystals. One electrode was kept at constant temperature and electromotive force was measured as a function of the temperature gradient. This is not a satisfactory technique if the results are to be compared with theory; rather should the electromotive force be measured for small temperature differences as a function of the mean temperature of the two electrodes. They used electrodes having the same cation as the salt. Patrick and Lawsons measured the thermoelectric power of AgBr and of AgBr containing 0.25 mole pct CdBr2 using silver electrodes and temperature gradients of 10°C in the temperature range 100° to 400°C. The results were analyzed using the Teltow9 values of the ratio of the mobility of the two types of charge carrier (cation vacancies and interstitials) found from conductance measurements and the wagnerlo estimate of the heterogeneous contribution to the thermopower, Ohet They obtained values of qi = 0.017 ev and q$ = -0.385 ev for the heats of transport of interstitial Ag ions and cation vacancies, respectively. Their data has been reanalyzed by Haga using the corrections to the Wagner formula for ehet given by Howard andLidiard; Haga found ev. Christy et a1.14 have measured the thermopower of AgBr containing 0.01 to 1.0 mole pct CdBr,. They analyzed their results in terms of the theory of Howard and Lidiard and found that excellent agreement with the theory was obtained if q5 + : + hF was set equal to 0.70 ev at 175°C and equal to 0.58 ev at 250°C. Since Teltow's value for hF, the enthalpy of formation of a Frenkel defect pair, is 1.27 ev, this means that qt + q: increases in magnitude from -0.57 ev at 175°C to -0.69 ev at 250°C. This result is in poor agreement with Patrick and Lawson's value of -0.37 ev for pure AgBr (for which the corrections to the Wagner estimate for ehet are very small). christy1' has also reported thermopower measurements for pure silver halides and for the systems he finds that qr + qt for AgBr increases in magnitude from about -0.55 ev at 150°C to about -1.1 ev at 400°C. The temperature dependence of the sum of the heats of transport in AgCl is very similar in magnitude. The sum qi + q cannot be decomposed into the individual interstitial and vacancy heats of transport without a knowledge of the entropy contribution from the change in the lattice vibrational frequencies around the interstitial and vacancy. Despite this it seems an inescapable conclusion from Christy's analysis that and -6 = Q Ag are quite strongly temperature-de pendent and that -q: is much greater in magnitude than the corresponding activation energy for vacancy migration, +0.37 ev. It remains a mystery as to why the data for pure AgBr are fitted so well by the assumption of temperature-independent heats of transport if association of impurity ions and vacancies is neglected.l The values for q$ and q: so obtained are also much more in line with those expected from a simple kinetic interpretation of the heats of transport due to wirtz.17 Christy and Hsueh have also measured the thermopower of CuCl between copper electrodes; 0 for pure CuCl is comparable with that for the silver halides but, owing to the limited solubility of divalent cation impurities it was not found possible to deduce values for the heats of transport. In contrast to these extensive measurements on cells of the type M MX 1 M, there have been relatively few attempts to measure the thermoelectric power of cells of the form M' 1 MX I M'. (We specifically exclude from discussion cells of this type in which the metal electrodes M' are in contact with gas containing a controlled partial pressure of either M or X,, since in these cells the electrochemical reactions are analogous to those of the first type.) The thermoelectric power of Pb12, PbC12, TlC1, TlBr, TlI, NaNO3, and KNO 3 between platinum electrodes was measured by Thie1e.l3 In discussing these measurements Holtan20 asserts that the thermopotential initially fluctuated wildly and even changed sign before approaching a steady value. A high degree of irreproducibility is also evident in the work of Nikitinskaya and Murin21 who first studied the thermopower of NaCl and KC1 between platinum electrodes. Much better reproduci-bility was achieved in our earlier measurements on KC1;22 these were, however, confined to a relatively narrow temperature range and one of the objects of the work reported in this paper was to extend the temperature range of the measurements of the thermoelectric power 8 of KC1. The only other published

Jan 1, 1967

By J. Buchwald, R. W. Heckel

THE DeHoff method' of analysis of ellipsoids of constant shape provides a quantitative metallo-graphic technique whereby the actual size distribution of the ellipsoids may be determined from polished and etched random planar sections. This method provides a useful metallographic tool since it appears to be the only method available for determining the size distribution of nonequiaxed second-phase particles. This method, however, assumes that the type of particle being studied is known to be either oblate or prolate of a fixed minor to major axis ratio, q. This, in general, means that one assumes either oblate or prolate ellipsoids of a given q and checks the total volume and surface area of the second phase as determined from the particle size distribution to values of these quantities determined by other techniques. Suitable check methods may be point counting, lineal fraction, and areal fraction methods for obtaining the total volume and the Smith and Guttman2 method of intercepts for obtaining the total surface area. If the initial guess at particle shape and q were incorrect, i.c., the volume and surface information obtained from the particle size distribution data does not agree with those values obtained by other techniques, another assumption must be made and the particle size dist distribution must be recalculated. A current study in this laboratory has involved a large number of these calculations. To facilitate the handling of the calculations, the DeHoff method was programmed in the FORTRAN language for an IBM 1620 computer. The purpose of this note is to briefly describe this program. The complete program along with a list of variable names, a sample input, and a sample output may be obtained from the senior author. Basically, the program provides for the calculation of particle size distributions for a series of q values for both oblate and prolate ellipsoids for each set of input data. The total volume of second-phase particles per unit volume are calculated for each calculated particle size distribution. The output of the program is arranged to allow a rapid comparison of the calculated volume and surface values to data obtained by independent check measurements. A condensed flow chart of the program in the notation of DeHoff1 is given in Fig. 1 The calculation of the number of particles per unit volume in the jth size class, Ni, according to the DeHoff method' is: where k(q) is the shape-correction factor given by DeHoff as a function of q for both oblate and prolate ellipsoids, A is the size-class increment, k is the number of size classes, ni is the number of particles in the ith class on the planar measurement surface, and B(j,i) are the saltykov3 coefficients which correct for measurement surfaces which do not pass through the major and minor axes of the particles. The values of /3(j,i) are included as a two-dimensional array in the program. Particular values of k(q) are included in the program in increments of q of 0.05. The first calculation is carried out for q = 1 (spheres), the second for q = 0.95 oblate, the third for q = 0.95 prolate, and so forth. The number of q values chosen for the calculation is determined by a control card in the input for each set of data.

Jan 1, 1965

By Larry Kaufman, Joan B. Berkowitz-Mattuck, Edward V. Claugherty

The oxidation characteristics of hafnium and zirconiunr diboride were measured between 1200 and 2200'K by a thermal- conductivity method which continuously ttzeasures the rate of reaction of oxygen with the diboride and by a metallographic air oridation method zuhich provides a measure of the total arr7ount of bovide conuerted to oxide for a given time interval. The oxidized specimens obtained from the tl~eritaal-coi~ductitrity method were also examined by quantitatire metal-lographic procedares. The significant results obtained in this investigation reveal that metal-rich compositions of lzafi~iutil diboride proride the most oxidation-resistatzt material up to 2000°K; hafnium diboride is tmre oxidation- resistant titan zirconium diboride at all tempevatures examined; the morphology of the oxide formed on H/B2 and Llie temperature coefficient qi. the oxidation rate constants change at the temperature of ttze monoclinic to tetragonal phase transition] in HfO2; the oxidation of neither HfB2 nor ZrB2, results iN catastrophic Jazlure at lorc. oxygen pressures; and pvefevetztial gvaLti boundary oxidation was not obsevued for either HfBi or ZYB, A comprehensive study of the high-temperature characteristics of refractory transition-metal di-borides is currently in progress. This program has included investigation of the physical, thermal, and thermodynamic properties of TiB2, ZrB2, HfB2, NbB2, and TaB2. In addition, aspects of the synthesis and fabrication of such materials have been studied. In view of the diverse nature of this research, a number of other laboratories have actively participated and contributed specific capabilities for analysis and characterization of these materials. As a consequence, an extensive description of the relevant properties of these compounds has emerged which is central in evaluating their high-temperature (1200" to 2500°K) performance. To date, information on thermodynamic stability, specific heat, and vaporization characteristics,1 hot hardness and electrical resistivity,1, 3 therma1 expansion:'4 and thermal conductivity 1, 5 has been presented. This information has been generated on materials of the highest purity (98.5 to 99.9 wt pct Me + B) and density currently available. Samples fabricated by zone melting6 and high-pressure hot pressing"3'7 techniques have been used to generate suitable specimens for all of the aforementioned studies. dation characteristics of the most oxidation-resistant of these materials, hafnium and zirconium diboride, is presented and a description of the synthesis and the experimental procedures used to prepare and characterize specimens is given. The high-temperature range under consideration (1200" to 2200°K) and the known dependence of oxidation characteristics on sample chemistry, density, and oxidation conditions required a close coupling of the synthesis, fabrication, and evaluation procedures.8 This was accomplished by continual surveillance of chemical composition of starting materials before and after specimen fabrication and by evaluation of density, phase constitution, and microstructural features prior to and after oxidation exposure. I) PROCUREMENT AND CHARACTERIZATION OF STARTING MATERIALS In view of the current state of the art in fabricating refractory boride materials, the methods used in preparing samples for the present study are given in detail as follows: starting materials were purchased in high-purity powder form and fabricated by high-pressure hot pressing into 0.40 by 1.00 in. bars from which oxidation specimens were obtained. The hafnium diboride used in this study was purchased from Wah Chang Corp.; the zirconium diboride from U.S. Borax and Chemical Co. These powders were routinely characterized by quantitative chemical analyses for metal, boron, carbon, oxygen, nitrogen, and iron, by qualitative emission-spectrographic analysis for trace impurities, by X-ray procedures for extraneous phase identification, and by powder densitometry for comparison with X-ray (theoretical) density. Hafnium and zirconium metal and elemental boron were also purchased as high-purity powders and characterized for impurities by emission-spectrographic analyses. The hafnium diboride was procured in three shipments which were designated as HfBl.g7(1), HfB1.88(2A), and HfB2.12(2). The indicated stoichiometry is based on the atomic ratio of total boron to total hafnium; the number in parentheses identifies the shipment number. Shipment 1 was 5 1b, shipment 2A, 1 1b, and shipment 2, 8 1b. The zirconium diboride was procured as a 20-1b shipment and designated as ZrB1.89(1). A small quantity of purified zirconium diboride was also supplied and designated ZrB1, 9(P). The averaged results for chemical analyses which were generally performed according to the procedures set forth in the compilation by KrieGe9 are presented in Table I. Qualitative spectrographic analyses indicated that Ca, Cr, Ti, Si, Zr (in H~B~), and A1 were present at levels between 0.01 and 0.10 wt pct. Other metallic elements were found to be less than 0.01 wt pct. Since it is virtually impossible to purchase these materials in the desired quantities (5 to 20 lb) as single-phase compounds it is necessary to obtain

Jan 1, 1968

By J. L. Schroeder, W. G. Talman

EXPERIENCE has shown that certain known natural conditions and other indefinite characteristics combine to make a mining area vulnerable to mountain bumps. Some of the known conditions are heavy overburden, an overlying stratum of strong non-elastic rock, a structurally strong coal seam that does not crush easily and yet is the weakest stratum in the series, and a floor stratum of more than ordinary firmness. The indefinite characteristics could include resistance of top or bottom of a coal seam to lateral flow, effect of immediate top and bottom strata, nature of the coal seam, and other factors about which very little is known. It is in this area that exhaustive study is needed to achieve positive control of the dreaded mountain bump hazard. In the Gary district, West Virginia, two of the five operating mines have areas known to be vulnerable to mountain bumps.These are the No. 2 and 6 mines, which are working the Pocahontas No. 4 coal seam. In this area the seam is overlain at a zero to 10-ft interval by the massive Eckman sandstone, which is about 100 ft thick in the vulnerable areas. Total overburden, consisting of shale, coal seams, and sandstones, ranges from 700 to 1400 ft where bumps have occurred (Fig. 1). The coal seam is 4 to 8 ft thick and has a weak columnar structure of very soft and spongy or woody coal. The immediate top is either the Eckman sandstone or hard shale, both of which provide generally good roof conditions for mining operations. The bottom ranges from medium to hard gray shale. The incidence of bumps in the Gary district dates from about 1930 and can be correlated to some degree with the increased rate of extraction attained with mechanical mining. During early years of operation at the No. 2 and 6 mines, most of the work was development and under comparatively light cover. As overburden became heavier, together with an increasing percentage of coal coming from pillar extraction, mountain bumps began to occur. Before 1945 they were much less severe than in later years, and because there were no injuries or fatalities, no records were kept. But by 1951 the incidence of bumps had increased to such extent that it became evident a mining system would have to be designed to eliminate or at least minimize these occurrences. Drawing on experience with modified versions of old systems and certain characteristics peculiar to the Pocahontas No. 4 coal seam, the district mining engineer, Martin Hayduk, outlined the essential factors for bump control in the Gary district. These control factors indicated: 1) The highly stressed area, which lies within the limits of convergence effects, moves at approximately the same rate as the retreating pillar line. 2) There is a decided softening of the periphery of blocks which is greatest and deepest on the gob side. 3) Blocks less than 45 ft wide never have been known to bump in the Pocahontas seams. Fig. 2 shows the mining plan based on these observations—a thin-pillar system with a minimum of secondary development. It was recognized from the start that the Hayduk system had certain limitations. When pillar work backed up to an inevitable surrounded block it was no longer applicable; also, burnt bottom and/or unknown factors reduced the system's effectiveness in certain headings. Since there was no way to eliminate the loaded block, it was decided to experiment with auger drilling to attain controlled release of this stored-up energy. The decision to auger was made after consideration of three separate plants, which were: 1) To cut the solid block into pillars of maximum size by driving away from the fracture line and at such a distance outby that development

Jan 1, 1959

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

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

Jan 1, 1970

By H. O. Hofman

(Canal Zone Meeting, November, 19]0.) THE sudden decease, April 1, 1910, in Chicago, of Dr. Franklin R. Carpenter was a shock to his- many friends. He died in his sixty-second year, of heart paralysis. To most fellow-members of the Institute who have followed the progress of the. last twenty-five years in the mining and treatment of non-ferrous ores, the work of Dr. Carpenter in that line is familiar ; but very few, even of those who knew him well in the later years, are acquainted with his earlier struggles to satisfy an inborn hunger for knowledge. The story of his life resembles that of the pioneer who opens up new country; overcoming hardships with indomitable courage, meeting doubts and difficulties with an alert and open mind, and exercising in the face of reverses an unconquerable perseverance. It seems appropriate to place on record in the Transactions a brief outline of the life and work of this eminent engineer. During the past 15 years of his life Dr. Carpenter was much interested in genealogy. In the pursuit of this study as an avocation, he traced his own ancestry to the time when ?Hugh," called "le Charpentier" on account of the dexterity with which he had swung his battle-axe as a crusader, settled in Sussex on lands received from William the Conqueror. The Carpenters came to this country with William Penn. A prominent member of the family was Joshua Carpenter, the founder of Christ Church, Philadelphia. Dr. Carpenter's branch of -the family moved from Pennsylvania into that part of Virginia which is now West Virginia, where his grandfather settled in Harrison county, while the grand-uncle went further west, and built the first iron-furnace at Hanging Rock, Lawrence county, Ohio. In fact, since early times, the Carpenters appear to have been iron-masters. Franklin R.. Carpenter was born, Nov. 5, 1848, in Parkers-

Aug 1, 1910

By E. Horton Jones

CONTENTS I Page Introduction ....:......................... 3 Chapter I. Unit Costs. . ...................... 4 Chapter II. Comparative Costs ..................... 20 Chapter III. Composite Costs..................... 32 Chapter IV. Wage Scale....................... 36 Chapter V. Raw Material Prices................. 37 Chapter VI. Description oF Costs ................... 64 Introduction We have endeavored in the following "sheets" to give the unit construction costs derived from 'the building of the Arizona Copper Co.'s new smelter, Clifton, Ariz., starting in February, 1912, and completing February, 1914.l In Chapter I—Unit Costs—are to be found the most elementary total unit costs which the accounts provide for. They are usable in the Clifton district. Here too are found the percentages to be added to an estimate for Engineering and General Expense. In Chapter II—Comparative Costs—these elementary costs have been classified, averaged and reported as labor and material unit costs. In such form the labor unit costs, when properly applied to similar conditions as these under which they were derived, are usable anywhere. The material unit costs are better disregarded for more accurate estimates and replaced by a newly priced bill of material. In Chapter III Composite Costs are given. They are unit costs built up from several elementary units, and likewise units of larger dimensions and simpler application, valuable for

Jan 1, 1915

By H. F. A. Hergt, K. L. Sutherland, J. Rogers

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By J. Rogers, H. F. A. Hergt, K. L. Sutherland

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

Executive Committee Board of Directors L F Reinartz, Chairman, H DeWitt Smith, Vice-Chairman, T B Counselman, M L Haider, Philip Kraft Finance Committee Board of Directors Andrew Fletcher, Chairman, A B Kinzel, D Wilson Endowment Fund "X" G F Moulton, Chairman, Erle V Daveler, '55, Philip Kraft, '56, I Brigden, '57 Honorary Memberships W M Peirce, Chairman, '56, M L Haider, ex officio, Andrew Fletcher, ex officio, John M Lovejoy, '55, D H McLaughlin, '57, Henry Krumb, '58, L F Reinartz, ex officio Investments Erle V Daveler, '57, Chairman, W M Peirce, '55, Henry Krumb, '56, G F Moulton, ex officio as Treasurer, Andrew Fletcher, ex officio as Chairman Finance Committee Local Section Appropriations A B Kinzel, Chairman, M L Haider, W S. Cumings, Fred J Meek

Jan 1, 1954