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By M. D. Hassiallis

The claim is made in a number of patents1'2'3'4 that some compounds of the class known as aryl sulphides have collector properties. One of these patents generalizes the claim to include all aryl sulphides, whose generic formula is R-S2-R' (where x = 1,2, . . . ), with the restriction that if the aromatic radicals R, R' contain substituent groups these groups may not contain nitrogen or oxygen. Moses, Hess, and Perkins cite as evidence for their claims the results of flotation tests on Anaconda and Miami copper ores using diphenyl sulphide, ditolyl disulphide and dinapthyl disul-phide as collectors. The use of alkyl sulphides as collectors has also been reported5 with the conclusion that the alkyl sulphides are better collectors than the corresponding aryl sulphides. The experimental work cited appears to confirm this contention. In order to test these claims with respect to diphenyl sulphide, a sample, purchased from the Eastman Kodak Co., was tested against Anaconda ore. The procedure followed. was that of Moses, Hess, and Perkins. A sample of ore weighing 500 • grams was placed in a laboratory ball mill. To this was added 220 grams of water, 0.06 grams of commercial diphenyl sulphide (1/4 lb. per ton of ore), and 0.8 grams of lime (3 lb. per ton of ore). The material was ground until 93 per cent passed a 65-mesh screen. This pulp was diluted to 16 per cent solids. A sample of the diluted pulp was placed in a Minerals Separation type of laboratory flotation cell. After a a-min. agitation period, pine oil was added and the froth collected for a period of 15 min. This test recovered 68 per cent of the copper, with a ratio of concentration of 6.8:I. The tailing assay was 0.3 per cent Cu. Moses, Hess and Perkins attained a recovery of 75 per cent, with a ratio concentration of I2:I. Although these results do not compare too well with those of Moses, Hess and Perkins, subsequent tests showed an improvement, as judged by vanning of the tails. It is concluded, therefore, that the patent results are confirmed. Contact-angle Tests In order to study the response of the various minerals, found in Anaconda ore, to commercial diphenyl sulphide, some contact-angle tests were made. Polished particles of bornite, chalcodte, chalco-pyrite, pyrite and quartz were conditioned for 15 min. in a suspension of diphenyl sulphide in water. The concentration of this suspension was 0.284 grams per liter, this being the concentration of this reagent in the ball mill. The conditioned particles were rinsed with water (not rubbed with filter paper or boiled linen) and then tested against an air bubble in the bubble machine, with the following results: born-

Jan 1, 1943

By J. E. Ostberg, G. Phragmen, A. Hultgren, S. Wohlfahrt

Detailed study was made of a number of rimming ingots, both low and high carbon, and especially upon effects of superimposed air pressure. Requirement to suppress core bubbles is between 10 and 15 atm; at 6.5 atm freezing was in semikilled manner and at 3 atm, steel was of rising type. Probable mechanism of freezing under various conditions is discussed. AN earlier paper' reported an investigation made by a committee for studying rimming steel ingots appointed by Jernkontorets in Stockholm. The present paper is the outcome of some further work done by the same committee. Since the characteristics of ordinary rimming steel are connected closely .with the amount of gas liberated during freezing and since this amount of gas is governed by the pressure, it was considered of interest to ascertain in what manner and to what extent definite pressures applied to the top of the liquid steel in the mold would affect the solidification process and the consequent structure of a rimming steel of ordinary composition. The experiments were made at the Domnarfvets Steel Works. The steel was made according to normal practice in a 4-ton Rennerfelt electric furnace. Ferromanganese was added in the furnace; no aluminum was added, with one exception. Analyses of the four heats are given in Table I. The top-poured ingots measured about 12 in. sq x 48 in. and weighed about 1300 lb. One or two ingots of each heat were allowed to solidify under pressure, using a special device for admitting compressed air to the upper closed part of the mold, as shown in Fig. 1. A heavy plate sealed with asbestos was bolted to the top of the mold. The plate had a tapered aperture for pouring. Immediately after pouring the hole was closed by a wedged plug, and compressed air was admitted through a hole in the plug. Because of some delay in applying the plug, full pressure was not reached immediately. The pressure was adjusted to the desired value as indicated by a manometer. In order that the interior of the ingot might have the benefit of the pressure, the freezing of the top crust was delayed by a refractory lining applied to the top part of the mold, Fig. 1. Ingots were also cast from each heat without applied pressure, and with and without refractory lining at the top. Axial sections of ingots were cut either of the whole ingot or of some part of it of special interest; sections were polished and usually etched.' To facilitate description of structures the following terms may be used for different types of ingots solidified under gas evolution: 1. Box-hat or boot-leg ingot: Abundant gas evolution during casting and during rimming; no rim holes. 2. Normal rimming ingot: Lively gas evolution during rimming; usually rim holes in lowest part of

Jan 1, 1952

By A. C. England, William F. Haney, Paul B. Crawford, Bobby L. Landrum

The creation of unsymmetrical vertical or horizontal fractures in a producing well will result in a unique distortion of the normal shut-in pressures existing at the four surrounding wells. An electrical model study has been made to show how the shut-in pressures at the wells surrounding the fractured producing well may he used to estimate the size and orientation of vertical or horizontal fractures. The pressure differences at the four surrounding wells are recorded during production from the fractured well. The resulting pressure dato are matched from a table of several hundred possible fracture combinations. The table refers to the figure showing the effective size and orientation of the commercially created fracture. INTRODUCTION The creation of commercial fractures about oil and gas wells has led to considerable speculation as to the size and shape of the fractures. It is important that the size and shape be known in certain instances, especially when pressure maintenance programs are to be initiated. It was shown that if knowledge of a vertical fracture could be found that such information may be utilized in planning a waterflooding or gas cycling program and that in some cases the fractures might be utilized very effectively.' Other work showed that it may be desirable to create "pancake" fractures in certain reservoirs but that they should exist in a desirable range.' If the fractures are too large, they should be plugged prior to initiating a pressure maintenance program. If an irregular shaped "pancake" fracture is created, it is desirable to know the orientation of this fracture because similar but unreported studies have shown that "pancake" fractures may or may not substantially affect the sweep efficiencies and performance of the flooding or cycling program. Consequently, it may be desirable in some instances to estimate the effective size and orientation of the fracture. ANALOG An electrical model was used in making this study. The electrical model consisted of a circular reservoir approximately 8 in. in diameter, 1 in. thick and was filled with a dilute salt solution. A copper band formed the periphery of the reservoir. A vertical fracture was simulated by a copper strip soldered to the wire well located in the center of the reservoir. Vertical copper strips of various lengths and orientation were soldered to the wire well to represent vertical fractures in the reservoir. In studies reported here on vertical fractures it was arbitrarily assumed that two fractures originated at the well and extended out into the reservoir. An electrical potential was imposed between the wire well and the periphery of the tank. Plots of the iso-potentials are shown in Figs. 1 through 9. This model provides the steady-state isopotentials existing in a uniform, homogeneous circular reservoir having a vertically fractured well at its center. The permeability of the fracture is much greater than the permeability of the matrix proper. The effects of gravity are neglected. In preparing Tables 1 and 2, four symmetrically located unfractured wells were assumed to exist around

Jan 1, 1956

By A. F. Bertuzzi, M. R. Tek, F. H. Poettmann

A method is presented for predicting pressure drop for two-phase fluid flow in horizontal pipes. A set of 267 experimental measurements randomly sampled from approximately 1,000 measurements from various literature sources was used. Pressure gradients calculated by the procedure developed and compared with the experimental values showed a bias of +0.82 per cent and a standard deviation of 20.8 per cent. The advantatges of this method over other available methods of predicting two-phase flow pressure drop are (a) its comparative simplicity of application, (b) its relative independence of flow patterns, (c) its accuracy, which on the basis of a statistical evaluation predicts pressure drop closer than other available methods, and, (d) its ability to satisfactorily correlate laboratory data from various sources while the correlations from these sources do not appear to agree with one another. The method has been reduced to a simplified graphical procedure, suitable for field use. A two-phase f factor is defined and correlated with parameters involving the flowing gas-liquid mass ratio, a Reynolds number for the gas phase, and a Reynolds number for the liquid phase. The choice of parameters allows the correlation to reduce to the usual f factor plot for the limiting conditions of (111 gas or all liquid. INTRODUCTION The mechanics and characteristics of two-phase flow systems have been of interest throughout the industry for some time. In numerous engineering installations such as pipe lines, chemical reactors, and heat exchangers, two-phase flow conditions are of every day occurrence. In oil production operations it has been desirable, in some cases, to consider transporting gas and oil together in a common pipe from oil field to process plant. The trend toward centrally located stock tank batteries in oil fields has resulted in longer gathering pipelines in which more than one fluid phase is flowing. The increase in the producing capacity of oil wells due to new production tech- niques has created the need for review and re-design of many surface gathering lines for properly handling the increased production. Optimum pipe size for the situations described above has become an important factor. The problem which is of interest here involves the ability to predict the relationship between pressure drop, fluid properties, fluid rates, pipe diameter, and pipe length. Although the literature1,5,10,13,18,19 contains various articles dealing with specific cases of the problem, Lock-hart and Martinelli17 proposed the most general solution. Their method has been later modified by Baker:1 Alves2 demonstrated that different flow patterns are possible for a flow mechanism defined by Martinelli such as gas turbulent, liquid turbulent. Baker explained deviations experienced with Martinelli's correlations on the basis that different flow patterns could exist for the same flow mechanism. Using Martinelli's method of correlatioil, Baker correlated data for each flow pattern for the turbulent-turbulent flow mechanism. Bergelin and Gazley6,7 presented a correlation for predicting gas phase

Jan 1, 1957

By R. S. Goodrich, G. S. Ansell

The microstructure of three Al-Al2O3 SAP-Type alloys (containing 2.0, 3.0, and 5.7 wt pct alumina, respectively) was studied utilizing transmission electron microscopy. These alloys were fabricated from aluminum powders by powder-metallurgical techniques, cold-rolled into thin strips, and recrys -tallized. Thin foils suitable for an electron-transmission study were then prepared from the strip material by electropolishing. The microstructure of these alloys is shown to consist of small (0.1 mean diameter) plate -shaped alumina particles finely distributed in an aluminum matrix. In the higher-oxide content alloys the platelets are somewhat larger and more irregular in shape. The distribution of oxide particles is not uniform and there is an increasing tendency toward clumping SINCE the discovery by Irmann1 that aluminum alloys produced by compacting, hot pressing, and extruding fine aluminum powders possess remarkable high-temperature mechanical properties, the Al-A12O3 SAP-Type alloys have been utilized extensively as model dispersion-strengthened alloys in both experimental and theoretical invest igations.2-8 The use of the SAP-Type alloys as model dispersion-strengthened alloys implicitly assumes that their microstructure has been completely delineated. This is, however, not the case. with increasing oxide content. In all the alloys studied, the mean center-to-center spacing of particles was quite small (0.2 u) due to the very fine oxide debris present. Selected-area diffraction of the specimen identified the oxide as either y Al2O3 or y' Al2o3. The re crystallized MD-5100 alloy exhibited a mean grain diameter of only 0.7u, while the grain size of the other alloys was several hundred microns. Severe pinning of the grain boundaries by oxide particles was rarely observed, and the grain boundary triple points in the small-grained MD-5100 alloy were often particle -free. Diffraction contrasts visible around the particles are attributed to elastic strain fields set up by differential thermal contraction during cooling from the recrystallization anneal. Early investigation demonstrated that optical metallography did not possess sufficient resolution to observe the microstructure of the SAP-Type alloys.' Later, extensive use was made of replication techniques to study the microstructure by means of electron microscopy.7-9 These studies indicated that the SAP-Type alloys consist of a dispertion of irregular Al2O3 platelets, approximately 150A thick 9 and a micron or so on edge,9 distributed in a matrix of commercial-purity aluminum. These oxide platelets tend to be oriented in the aluminum matrix, with their largest dimension parallel to the extrusion direction. 8,9 A study employing polarized-light techniques1' indicated that the grain size of a series of as-extruded SAP-Type alloys was several microns in diameter, while the grain size after re-crystallization was several millimeters in diameter. A more recent study 12 utilizing surface-replication techniques examined the particle morphology,

Jan 1, 1964

By H. C. Chao, Y. E. Smith, L. H. Van Vlack

ThE phase relationships for the MnO-MnS system have been investigated only in the eutectic region. wentrupl reported a eutectic at 1280°C (2345°F) with approximately 50 wt pct of each component, as based on the earlier work of Andrew, Maddocks, and Fowler.2 More recently silverman3 corrected these figures to 2275° ±10°F (1246°C) with 63 wt pct MnS and 37 pct MnO. Neither Wentrup nor Silverman investigated the solid-solution limits in this system. However, Wentrup did suggest with his phase diagram sketch that the maximum solubility of MnS in MnO is 10 wt pct, and the solubility of MnO in MnS is nearer 20 wt pct, Fig. 1. These figures have been utilized in subsequent publications without further verification.4 There had been evidence found in this laboratory that the above solid-solution figures were high. An investigation was therefore conducted using the following procedure. Samples containing MnO and MnS were contained in platinum foil, heated just above the eutectic temperature in a purified nitrogen at- mosphere, and quenched into distilled water. The MnO had been prepared by calcining reagent grade MnCO3 in nitrogen at 1400°C. Only MnO was detected in subsequent X-ray diffraction analyses. The MnS had been prepared by sulfur deoxidation of reagent grade MnSO4 according to the reaction: MnSO4 + S2 ? MnS + 2SO2 The details of the sulfide preparation procedure, which utilized atmospheric sulfur pressures at 950°C, are discussed elsewhere.5 The sulfur content of the sulfide was determined to be 36.8 * 0.2 pct, which matches the stoichiometric value of 36.9 pct. No evidence of either MnO or MnSO4 was detected microscopically or by X-ray diffraction. The single-phase combinations of MnO and MnS at the eutectic temperature indicate the limit of solid solution as shown in Fig. 2(a) and (c), and the revised phase diagram is shown in Fig. 2(d). The melting temperature for MnO is that provided by Glasser.6 The eutectic temperature of 1232° ± 5°C and eutectic composition of 64 wt pct MnS are in close agreement with Silverman's correction of Wentrup's work. The maximum solubility of MnO in MnS was determined to be 1.7 ± 0.2 wt pct. The maximum solubility of MnS in MnO was determined to be 1.8 ± 0.2 wt pct. These figures represent the lower limit for the presence of liquid at 1260°C and are significantly lower than the earlier estimated solid-solution figures. The authors wish to acknowledge the support of U.S. Steel's Edgar C. Bain Laboratory for Fundamental Research. The comments and critical suggestions of Drs. A. S. Keh, R. Rickett, and R. B. Snow are appreciated.

Jan 1, 1963

By J. W. Marx

A method is given for predicting the complete gravity drainage characteristics of arbitrarily long columns from centrifuge drainage measurements on reconstituted core samples. Oil residuals corresponding to hundreds of years of normal gravity depletion can be obtained in a few hours on the centrifuge. The gravity flow rate at any stage of the depletion process may be determined from the time correlation derived, and experimentally checked, in this study. INTRODUCTION Apart from the original observations of Muskat et al1, research publications2,3,4 on the subject of gravity drainage have been largely concerned with establishing in detail the saturation, S as a function of the height, z, in a draining column at any given time, t. Some form of numerical integration must be employed to obtain production rates and cumulative production even when S(z, t) is known. Furthermore, the relevant experimental work has been concentrated on drainage of a single wetting liquid from unconsolidated media. Since oil production usually concerns the drainage of a partially wetting liquid from consolidated media, in the presence of connate water, and since it is unlikely that sufficient information exists to establish S(z, t) in detail for any natural reservoir, the published research work appears to be, at best, only qualitatively applicable to production problems. With this in mind, the present study was undertaken by the writer. Experiments were planned whose results would have two advantages over existing measurements: 1. Observations were to be made on specific reservoir rock, reconstituted with formation water and formation oil. This would reduce their generality, from the research viewpoint, but increase their utility for production purposes. 2. The measurements were to be self-integrating, i.e., the phenomena were to be described and interpreted in terms of cumulative results. THEORETICAL DEVELOPMENT It was commonly known that centrifuging a liquid bearing porous medium increases the drainage rates and minimizes capillary end effects. The specific problem lay in selecting an acceleration, a, such that the mean residual saturation of a model cylinder was equal to the residual saturation of an arbitrarily long prototype column when the latter was drained by earth gravity alone. The physical conditions required to permit a valid scaling of model drainage time, tm with prototype drainage time, t, may be stated as follows: (a) At t = tm = O, So = Smo; (b) At t = tm? 8 Sr. = Smr.; (c) For all intermediate values of t and dS/dt=dsm/dtm whenever S = Sm; (d) S(z) = Sm(z) = a constant when t = tm = 0. 1 Here S = T I S(z)dz, where h is the length of the « Jo cylindrical column being drained and the subscripts S,Sm, and refer to model, initial, and residual systems, respectively. The first three conditions mean, simply, that an 3 vs t plot will be numerically identical with an S, vs t, plot,

Jan 1, 1957

By Ronald C. Koo

THE effect of grain size on the mechanical properties of the bcc metals has been a subject of intensive theoretical and experimental study.'-l5 Quantitative relationships have been established experimentally between yield stress and grain size and between the ductile-brittle transition temperature and grain size in a number of metals.6"15 Much significance has therefore been attached theoretically to the grain size dependence. In all these experiments, different grain sizes were always achieved by annealing specimens at various temperatures. The implicit assumption was that any change in the dislocation substructure or in the distribution of impurities which might occur simultaneously with the production of various grain sizes had only a negligible effect on the mechanical properties. The validity of this assumption, however, is questionable. transformation in iron-nickel alloys is actually an extraneous phenomenon due to inadvertent compositional changes in the martensite if the heating rate is not sufficiently rapid. This complication can be avoided by up-quenching for the reversal treatment,5 and then the stabilization does not appear. Clearly, the lattice imperfections and strengthening produced by the reverse transformation are not responsible for the marked stabilization which has been observed by other investigators in these alloys. Data will be presented in this note to show that, at least in recrystallized tungsten of commercial purity, the difference in the ductile-brittle transition temperature of specimens annealed at various temperatures is more a result of a variation in the distribution of impurities rather than of the difference in grain size produced by the anneal. Ductile-brittle transition temperatures in tension were determined on powder-metallurgy tungsten specimens recrystallized at various temperatures. Tensile specimens having a gage length of 1.50 in. and gage diam of 0.18 in. were recrystallized at 1450°, 2000°, 2350°, 2550°, 2750°, or 2800" for 30 min in a vacuum furnace at a pressure of 1 x 10"5 mm of Hg and then tested at a constant extension rate of 8 x 10 per sec in an argon atmosphere from 100" to 800". Typical quantitative analyses of impurities are given in the Table. These results show that, within the precision of the analyses, see Table, annealing did not result in any detectable change in the impurity contents of the specimens, nor was there any detectable difference in purity between specimens having large differences in grain size annealed at the same temperatures . The results of the tensile tests yielded three distinct ductile-brittle transition curves approximately 225' apart. As shown in Fig. 1, data of specimens annealed at 1450°C and those of specimens annealed at 2000°C (O) fell on Curve A. Data of specimens annealed at 2350" and 2550°C fell on Curve B, and those of specimens annealed at 2750" and 2800°C fell on Curve C. The decrease in ductility with increase in annealing temperature became so pronounced that one third of the specimens annealed at 2750" and two thirds of the specimens

Jan 1, 1963

By R. J. Walter, W. T. Chandler

The Ch-H phase diagram was determined for by-drogen concentrations up to ChHo.9 at temperatures below 400°P'. The phase diagram includes a mis-cibility gap and a eutectoid transformation. A peri-tectoid transformation is postulated at the hydrogen-rich end of the diagram, Phase diagrams were determined for two levels oj purity, of the columbium. A single solid solution exists in the Cb-H system above 400°F. There has been considcrable disagreement among investigators concerning the system at temperatures below 400°F. Albrecht, Goode, and ~allett' proposed a miscibility gap containing two bcc phases with the two lattice parameters converging at about 140°C (285-F), and Brauer and ~erman' found a two-phase room-temperature region between 10 and 41 at. pct H. At sufficiently high hydrogen concentrations in the one-phase region, the hydrogen-rich phase was found to be face-centered orthorhombic. Wainwright, Cook, and Hopkills3 recently reported that the face centered orthorhombic hydride phase is derived from a unit cell which is slightly tetragonal with a small departure from 90 deg of the angle (y) opposite the r axis. The orthorhombic hydride phase was observed for hydrogen concentrations between 0.2 and 0.8 H/Cb atom ratio. Paxton and coworkers4 found that needlelike hydride plates formed in a hydrogen-charged columbium single crystal and suggested that this transformation possessed the characteristics of a diffusionless phase transformation. On the basis of room-temperature, X-ray diffraction data, komjathy' suggested that an order-disorder or martensitic transformation occurs. In the present study, the Cb-H system was investigated to resolve the discrepancies found in the literature for this system. PROCEDURE The columbium specimens were prepared from two heats of wrought 1/2-in.-diameter electron-beam melted columbium rod and from two columbium powders of -80 mesh size of different impurity contents. The columbium bar stock was pur chased from Urah Chmg Corp.; the 99 and 99.5 pct purity colulnbium powders were obtained from Fansteel Metallurgical Corp. and Kern Chemical Co.. respectively. The chemical analyses of the columbium bar and powders are listed in Table I. Hydrogen charging was performed by exposing the columbium specimens to hydrogen at 1 atm pressure at various temperatures. After exposure the specimens were quenched to prevent the hydrogen pickup which would take place if cooled in hydrogen, or the hydrogen loss that would occur if cooled in an inert gas. Adequate hydrogen purity was achieved by passing high-purity tank hydrogen (maximum 5 ppm total impurities) through an Engelhard catalytic Deoxo unit, magnesium per chlorate desiccant, and finally through activated charcoal at the temperature of boiling nitrogen. Activated charcoal at -321°F has been reported6 to remove impurities from hydrogen to a nondetectable level. A schematic representation of the heat-treating apparatus is shown in Fig. 1. A metal-sheathed thermocouple embedded in the colun~bium specimen was used to control the temperature during heat treatment and to pull the specimen boat into

Jan 1, 1965

The Palabora ore consists of two types, a carbonatite containing a low titanium magnetite, and a foskorite containing high titanium magnetite. The latter type also contains substantial quantities of phosphate. These two ore types are separately crushed and are kept separate through copper flotation and magnetic separation, for recovery of magnetite, with the low Ti magnetite being shipped as iron ore. High phosphate tailings are pumped to Foskor, a government-owned phosphate plant nearby. The Palabora plant was originally designed in 1966 for 33, 000 tpd using two 54 in. by 74 in. Allis -Chalmers gyratories; two 7 ft (2. 13 m) standards; four 7 ft shortheads; and six grinding lines, each using one 1,200 hp rod mill and two 1,200 hp ball mills. A fifth short- head and one more grinding line were added later; and with flowsheet improvements, the capacity of the plant was increased to 59, 500 stpd. A further plant expansion involving a third 54 in. primary and two 32 ft by 15 ft (9.75 by 4.6 m) 9,000 hp autogenous mills and another flotation section will bring its capacity to 87,500 stpd in 1977. These two fully autogenous mills are constructed entirely out of doors near the primary crusher, and the ground ore will be pumped a mile to the concentrator by a five-stage pumping system. The Palabora ore is mined with 6, 10, and 12 7d (4.6, 7.6, and 9. 2 cu m) shovels and hauled to the crushers in 110 and 165 st trucks. Sixty-five ton trucks were originally used, but the crusher dump pockets were designed for larger units. Dump pockets, crushers, feeders, and take- away belts are offset in order to keep the two ore types separate. Centerlines of the crushers are only 43 ft (13. 1 m) apart; but, because of their being offset, maintenance room is ample. Initially, more carbonatite ore than foskorite was mined; but as the pit has deepened, this ratio has been reversed. The Palabora ore breaks in the pit with a large amount of oversize boulders; and, with the use of larger trucks, a splitter has been installed on one side of each dump pocket to protect the crusher spider. Smaller trucks dump on the opposite side. To accomodate the splitter, the pocket edge has been raised one meter and moved back one meter. Dust is collected through a special vent shaft between the crushers and the mantle relining area; but even so, two high-pressure water spray headers with nozzles are installed under the edge of the pocket at each dumping position. While only one truck dumps at a time, sprays from all four headers are used to suppress dust. Any leakage of water through the seal around the upper bowl of the crusher is caught by a circular trough under the seal and directed to a sump pump. At this point, there

Jan 1, 1978

By Emma Smith, R. W. Guard

INVESTIGATION of the nickel-rich end of the Ni-Zr system has been prompted by an interest in the effect of small amounts of zirconium in high temperature alloys. Hansenl presents a hypothetical diagram based on the work of Allibone and Sykes,2 who investigated the system up to 44 atomic pct (55 wt pct) Zr by metallographic means. Since the alloys they used were melted in Alundum crucibles they were probably contaminated with appreciable amounts of aluminum. They found two compounds which they called Ni3Zr and Ni4Zr. Hayes, Roberson, and Paasche3 identified a compound NiZr (50 atomic pct Zr) with a melting point of 1470°C. Such a high melting compound is not compatible with the observation of Allibone and Sykes2 hat a eutectic is formed near 50 atomic pct. The alloys containing up to 60 atomic pct Zr were melted in an inert atmosphere in a noncon-sumable electrode arc furnace. Analysis of most of the alloys indicated negligible loss of zirconium. The alloys were examined in the as-cast condition and also after annealing for 6 hr at 1175°C (or 1000°C for the alloys between 25 atomic pct and 45 atomic pct). Metallographic specimens were etched using mixtures of HF-HNO3-H2O or acetic acid- HN0,-H,O. The specimens for the solidus determinations were wrapped in molybdenum foil and sealed in evacuated quartz tubes. Specimens to be heated above 1300°C were enclosed in zirconia tubes inside the quartz to prevent reaction with molybdenum. The solidus determinations were carried out by heating the specimens at various temperatures for a few minutes and then examining the interior structure metallographically to determine at what temperature melting began. The 150 mesh powders for X-ray analysis were annealed in an evacuated quartz tube for 2 hr at 540 °C to remove cold work. Alloys with 22.5 atomic pct Zr and 44.4 atomic pct Zr required annealing at 700 °C for complete recovery. The grains of both of these alloys were soft and rather ductile. Both Debye-Scherrer film patterns and spectrometer traces were made for each alloy using filtered copper radiation. Results and Discussion The presence of a substantial amount of second phase in an alloy with 1.1 atomic pct Zr indicated that the solid solubility of zirconium in nickel is somewhat less than 1 atomic pct. The a0 value for the face-centered-cubic matrix in the same alloy was equal to that of pure nickel, so that the solubility must be very small. This observation is as expected from the large atom size difference. Annealed specimens of alloys with 15.0, 16.7, 22.5, 28.6, 44.4, and 59.4 atomic pct Zr showed. micro-structures that were essentially single phase. When

Jan 1, 1958

By M. P. Sidorova, D. A. Fridrikhsherg

The surface charge, electrokinetic potential and surface conductance were studied for silica, alumina and rutile as the functions of PH and concentration of 1-1 electrolyte solutions. The adsorption potentials of potential-determining and specifically adsorbed ions were calculated from isoelectric and zero charge points on the basis of Stern equation and thermodynamic description. From surface conductance and charge data the mean ionic mobilities in double layer were estimated. The results give some information about the real structure of oxide-electrolyte interface and gel-layer concept.

Jan 1, 1980

By D. H. Davis

HAND picking was the earliest form of coal preparation, first practiced to improve the outward appearance of the coal being loaded and to remove any pieces that might appear objection- able to the buyer. It is still extensively practiced on the plus 1-in. sizes and particularly on the plus 4-in. and larger sizes. The percentage of ash reduction that can be obtained by hand picking depends entirely upon the amount of free impurity occurring in the coal. In a particularly dirty seam, where a considerable quantity of rock occurs with the coal as mined, hand picking produces sizable reductions in ash. If the coal is prepared clean at the working face hand picking is a final check; in some cases, on the smaller sizes, it is practiced only to show that an effort is being made to prepare a clean product. Because of the variety and different methods of handling coal, the early plants were not always adapted for efficient hand picking. At most mines an attempt is made to remove the visual impurities at one or more of the following places in the surface plant? (1) in the tipple during screening; (a) on picking band, belt, or shaking conveyors;*(3) during the loading of the coal as it goes into the railroad car. Whatever the physical arrangements of the plant may be, the usual practice is to run the coal over the screen, picking table or boom at such a rate that each piece of impurity is exposed to the view of the picker. Coal should be uniformly sized and spread out on the table so as not to exceed one particle in depth. The flow should be even in tonnage and the speed of travel should be from 30 to 60 ft. per minute and not exceed 80 ft. per minute. The dirtier the coal, the slower the speed required for a fixed number of pickers. Actually, picking capacity depends on the number of particles per minute that can be picked out and rejected. The percentage of impurity removed is determined by this and the average weight of piece rejected. Handling a mixture of sizes from nut to the largest lump over the same picking table or conveyor is not conducive to efficient separation by hand picking because the lump hides the smaller

Jan 1, 1943

By D. V. Doane, G. A. Timmons, W. G. Scholz

Molybdenum of high purity can be produced by direct dissociatiott of commercial molyhdenm disulfide in vacuo at 1600° to 1700°C (2910° to 3090°F). The Product is lower in oxygen than commercially available molybdenzdm powder. Analyses of ingots arc-cast from commercial molybdenum powder, hydrogen-re-cluced from animonium molybdate, and from thermally dissociated molybdenum disulfide indicate that the levels of chemical impurities in these ingots are similar. Equipment now in operation will produce 100-lb hatches of powder product. The paper describes development of processing equipment, control of processing varzahles, handling of the product, and evaluatiotl of the melal produced. MOLYBDENITE (molybdenum disulfide) can be decomposed by heat in the absence of oxygen to produce elemental molybdenum and sulfur, which is evolved as a gas. The temperatures required for the dissociation are above 1370°C (2500°F); the sulfur must be continuously withdrawn to permit the reaction to proceed to completion. This is accomplished by continuous evacuation of the thermal dissociation chamber and condensation of the gaseous sulfur in another part of the system. Cognizance of the fact that the dissociation takes place in two steps is important in controlling the process. Basically, the molybdenite dissociation process has two potential advantages as a method of produc- ing pure molybdenum: 1) The materials entering into the process contain little or no oxygen. Since the process is carried out in vacuum at high temperature, the quantities of interstitial oxygen, nitrogen, and hydrogen in the product should be very low. 2) The process is more direct than the commercia1 method of producing high-purity molybdenum. In the conventional process, molybdenite is roasted to molybdic oxide, the oxide is purified first by sublimation, then by conversion to ammonium molybdate, and finally, the molybdate is reduced in a hydrogen atmosphere (usually in two steps) to the metal lic molybdenum powder. This paper presents a description of the stages in scaling-up of the dissociation equipment and an account of attempts to evaluate the molybdenum produced by thermal dissociation, rather than a report of a fundamental study of the dissociation reaction. Since little has been written on the subject, it is appropriate, before detailing the development of the process, to review briefly the research that has been conducted over quite a period of years. LITERATURE SURVEY The first accounts of the possibility of thermal dissociation of the mineral molybdenite were re-

Jan 1, 1962

By G. P. Walters, W. C. Fuller

THE production of thin films of beryllium became essential early in the irradiation program at Harwell in order to study the fundamentals of irradiation damage in this metal. In common with other metals, electron-microacope specimens of beryllium can be produced by different techniques. The techniques used to produce thin-film specimens varied according to the starting material. Most of the starting material was -0.060 in. thick. Large-area specimens (1 in. long by 0.5 in. wide) were chemically thinned to -0.005 in. thick in a solution containing 85 pct orthophosphoric acid, 10 pct chromium trioxide, and 5 pct sulfuric acid at 70°C prior to electropolishing. Small-area specimens, Fig. 1, had to be mechanically thinned prior to electropolishing because chemical thinning considerably reduces the area as well as the thickness. Mechanical thinning tends to produce a worked layer about 0.002 in. deep and hence this method cannot be used to thin bulk specimens below about 0.005 in. thick. Mechanical thinning is carried out by mounting the specimen on perspex then carefully polishing on wet grinding papers. Polishing is continued until about half the initial thickness is removed; the reverse side is then polished in a similar manner. After the bulk specimens have been mechanically or chemically thinned to -0.005 in. they are elec-tropolished in the solution shown in able I at 50" to 80°C. This solution should be prepared by adding the chromium trioxide to the orthophosphoric acid and then the glycerol last. The glycerol should be added slowly because a vigorous effervescence can occur. Electropolishing is carried out by holding the specimen in stainless-steel tweezers and gently agitating in the solution. Masking or "window" techniques are not required for beryllium, good microscope specimens being obtained from the edges of elec-tropolished foils. A stainless-steel beaker should be used, acting as the cathode and solution container. A closed circuit voltage of 30 v is used for polishing. Too low a voltage produces a matt surface and pitting occurs when it is too high. The solution temperature is important. If it is too low, the solution is viscous and bad polishing results and, if too high, etching of the specimen occurs. After electropolishing, the foils are thoroughly

Jan 1, 1963

By Thomas A. Simpson

THE Birmingham red iron ore district in Jeffer-son County, north central Alabama, Fig. 1, is bounded on the northwest by the Warrior and Plateau coal fields and on the southeast by the Cahaba and Coosa coal fields. The area of study includes the ridge and valley between Red Mountain and Shades Mountain, Fig. 2, approximately 70 square miles extending from Homewood in the northeast to Greenwood in the southwest. The district is one of the most important producers of hematite in the United States, with an annual production of about 7 million tons.' The amount of hematite mined between 1870 and 1950 ranged from 6 to 16 pct of the nation's total annual production,' and the iron and steel products from blast furnaces in the Birmingham district supply the entire southeastern section of the country. Most of the mining in the Birmingham district is from slope mines along the outcrop of the ore on Red Mountain, such as Red Ore, Muscoda, Spaul- ding, and Sloss. The Pyne and the Shannon are the shaft mines of the area. The Shannon mine of Republic Steel Corp., in the central part of the area under study, is in Shades Valley at the foot of Shades Mountain. The Pyne mine of Woodward Iron Co. is 2 miles east of Readers Gap in Shades Valley. The hydrology problem has become more prevalent as mining in the area has progressed downdip. An extensive exploratory diamond drilling program is necessary to determine areas where water pressures and abnormal flows are excessive. This operation, added to higher pumpage rates, has greatly increased the costs of ore extraction. In November 1952 the U. S. Geological Survey began a detailed study of occurrence and movement of ground water in the iron mining areas of the Birmingham district. The study is a part of a small-scale but nationwide program to develop data that will be of help to the mining industry in solving mine water problems. The area of the study, in the Ridge and Valley province of the Appalachian system, Fig. 1, is a series of alternate ridges and valleys trending northeast. The principal ridges are Red Mountain, altitude about 1000 ft, and Shades Mountain, about 1100 ft. Shades Valley is between these two ridges, and its lowest point is about 480 ft. Shades Moun-

Jan 1, 1956

By Foster Bain

MOST of us householders in the East burn anthra-cite, so the problem that interests us most is the distribution and supply of the domestic sizes of anthracite. That, however, is only a small part of the coal problem and has its own peculiarities. Whether anthracite prices are high or low is largely a matter of relativity, depending on the size of the transaction, the available supply, and other things. As an isolated example which I hesitate to quote because it is not entirely representative, you may be interested to know that the Government fuel yard has been delivering to the Government buildings in the District of Columbia, white-ash stove coal at 16 c. a ton less during January, 1923, than during the same month of 1922. The reason is that the Government deals only with large companies who have been wise enough not to boost their prices and the small increase at the mine has been more than offset by the decrease in railroad rates. The total cost is $12.50 per ton, but I want to make it perfectly clear that it does not follow that this would be a just price for a retail dealer to charge the domestic consumer. For example, in the Government business there is no such thing as a bad debt, and certain other fixed or general charges are charged to other departments. The Bureau of Effi-ciency made an effort to determine what would be a. legitimate handling charge for a retail dealer, in Washington, and concluded that if the Government's cost of handling was $1.00, then $1.88 would be the corresponding fair charge to pay a retail dealer carrying the same volume of business, allowing for bad debts, complete depletion and depreciation of his equipment, and 10- per cent. profit. Assuming that this is the correct differential for Washington, it does not' follow that it would be equally just for Pittsburgh, New York, or elsewhere; nor does it by any means follow that it is a fair differential this year, because the dealer, after being unable to use his equipment in the summer months, now has to deliver an unusually large quantity of coal. I merely cite this instance to show that on the basis of primary cost of coal plus railway charges the retail price is not necessarily higher this-year than last.

Jan 4, 1923

By Jerome Alexander

It is an outstanding fact of Nature that many of the practical properties of substances are dependent, not on their ultimate chemical composition, but on the kind and degree of aggregation of their constituent particles. Thus, a granite boulder is unmoved by wind or water, but if reduced to a fine dust it will be blown about by the wind and washed away by the rain. Carbon in one crystalline state of aggregation (diamond) is the hardest known substance, whereas in another crystalline state (graphite) it is so soft that it is used as a lubricant. Laying too much stress on the mere chemical analysis of substances is apt to obscure the fact that the nature of the aggregation of their particles is always a factor of importance, and sometimes the most important factor. Colloid chemistry deals with matter in a very fine state of subdivision; its sphere begins with particles just a little smaller than a wave length of light and extends down until they blend into molecular dimensions. With particles of this size, such phenomena as surface tension and adsorption, which depend on the development of free surface, become enormously magnified. Thus a cube of 1 cm. edge has a surface of only 6 sq. cm.; but if it is reduced to colloidal dimensions by being cut up into cubes each having an edge of 0.01 µ (0.00003 mm.), it will yield one million, million, million (1,000,000,000,000,000,O~) such cubes, having a combined area of 600 sq. m., or 21,274 sq. ft. The tiny force with which a drop of rain clings to the window pane becomes a factor to be reckoned with, if the surface involved is increased millions of times. From the colloid-chemical viewpoint, metals and alloys may be regarded as jellies or sponge-like structures,. the viscosity or stiffness of which at ordinary temperatures is exceedingly great; and like all jellies their properties are dependent on the composition and degree of dispersion of their constituent phases. These, in turn, depend on chemical composition, mutual solubility, speed of chilling, subsequent mechanical and heat treatment, etc. In fact, in preparing metals and alloys for practical use, we remove undesirable constituents (as in the conversion of pig iron into steel), add desirable constituents (as in

Jan 1, 1919

By James A. Beck

Phosphorus is essential to all life processes and therefore to the existence of man. In this role, there are no substitutes for phosphorus. In a commercial sense, phosphorus and its compounds are important to our entire economy, both in agricultural and in nonagricultural applications. The world's phosphate requirements are met by mining phosphate rock. Two general types of phosphate ore deposits are commercially important-igneous and sedimentary. Igneous deposits generally are more difficult and more expensive to mine than sedimentary deposits and are of importance mainly in the USSR, North Vietnam, and South Africa. Approximately 15% of current world production comes from these deposits. Over 80% of world production is from the pellet sedimentary deposits of Florida, North Africa, and elsewhere. Guano, the second type of sedimentary deposit, is produced in South America but is declining in world importance. Production Production of phosphate rock was reported in 31 countries during 1972. However, about 80% of world output is produced in three countries: the United States, the USSR, and Morocco (Table 15.2A.1). Throughout the past 20 years, between 75% and 80% of world output has been produced by these three leading countries. Between 1948 and 1972 world production increased at an average rate of 10% per year, from 21.5 to 103.9 million tons. Growth was quite steady at 6% per year through 1963, but in the 5 years from 1963 to 1968 production increased 11 1/2% per year. Since 1968 production has increased about 91/2 % annually. Since 1948 several new phosphate mining ventures have been developed in Senegal, Togo, Israel, and North Vietnam. In the same period, only one important phosphate deposit, on Makatea Island, has been mined out and closed. A number of other phosphate mining ventures are in various stages of planning and development. The most important new venture in phosphate mining is in the Spanish Sahara. New mining capacity is expected also in Syria, and serious investigation is in progress in Peru, India, Turkey, and Australia. Major expansion of existing operations is expected in Morocco, Russia, Tunisia, Israel, and Jordan. Consumption Historical data on world consumption of phosphate rock are not available in detail, but world consumption of phosphate has closely paralleled world production in the past two decades. The United States is the world's largest user of phosphate rock, accounting for 30%

Jan 1, 1976

By Francis Foley

WITH the possible exception of high-speed tool steel, the service demanded of rock-drill steel is probably more precarious than that of any other tool steel. Unaided by the helpful influence of alloys and dependent solely on the efficiency of the heat treatment applied for its ability to stand up under the abuse to which it is necessarily subjected, rock-drill steel is worthy of intensive study. For its heat treatment the smith has his fire, an oil fire perhaps, and a quenching bath; he judges' the temperature by his eye. There are shops where excellent drills are produced by this method, but there are more where the product varies between very good and very bad. Pyrometers with specially designed equipment are used in but few cases. But the responsibility for rock-drill failures does not rest entirely on the smith. Little has been published concerning the efficiency of drill steel, though the Canadian Mining Journal' published the breakage record of a large number of hollow drill steels. This record indicates that most of the breaks occur during the early life of the steel and that as a given batch of steel is used, its percentage of breakage decreases. This fact, the article points out, is at variance with the much-talked-f theory concerning failure from crystallization and fatigue. It seems to point to the fact that the greater part of drill-steel failure from breakage is traceable to faulty manufacture, resulting in defects in the bore of the hollow steel from inclusions of slag or oxides, etc. As this defective material meets with early failure, it is weeded out. In addition, some breakage may be caused by a lack of proper condition with respect to heat treatment of the steel as furnished by the manufacturer. In the article mentioned, the breakage of 1 ¼ -in. (3.17 cm.) hollow steel is given as 4.62 per cent. for the early period of use, with a decrease to 3.35 per cent. and 2.67 per cent. With time in use. For 1-in. (2.5 cm.) hexagonal hollow steel, the figures for breakage are 0.18 per cent. and 0.06 per cent.; attention is called to the "enormous decrease in breakage by the use of smaller diameter drills." The figures are given as so many "drills sharpened," but there is no way of determining the percentage of

Jan 6, 1921