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By J. F. Abel, F. T. Lee

Subsidence is controlled by a complex com¬bination of mining and geologic factors. For example, a compilation of worldwide data shows that, as the percentage of shale in the overlying rock mass decreases and the amount of sandstone increases, the angle of draw (and the area affected by subsidence) decreases. Limestone in the over¬burden appears to cause a more than twofold decrease in the angle of draw compared to a like amount of sandstone. Increased amounts of sandstone were accompanied by a greater surface subsidence relative to the mining height. The total thickness of overburden did not appear to influence the subsidence magnitude above super-critical panels. The greater the thickness extracted, the smaller percentage of that thickness shows up at the surface as subsidence. The greater the percent of the seam extracted, the greater the subsidence reaching the surface. The maximum subsidence above room-and-pillar panels de¬pends on the pillar height and minimum width as well as the other factors listed.

Jan 1, 1984

By H. W. Mead, C. E. Birchenall

SELF-DIFFUSION of iron in austenite is a process which may play a significant role in some of the practically important reactions which occur in solid irons and steels. It also provides a system in which the interaction of vacancies on substitutional sites and atoms in interstitial positions may be investigated. For both purposes, accurate values of the diffusivities are required. Two sets of previous measurements exist, each containing features which require checking. In the course of an investigation to determine the rate of diffusion of iron in certain steels, Garwick and Rosenqvist' measured the self-diffusion coefficient of iron in a 0.10 pct* C steel and obtained a dicated that while at lower temperatures D increased with increasing carbon content, at the higher temperatures it first increased and then decreased. At the same time the activation energy decreased linearly from a value of 69,000 cal per g-atom for pure iron to 33,000 cal per g-atom at 1.06 pct C. This rapid decrease in activation energy implies that iron at higher temperatures within the austenite range would diffuse more slowly in high carbon steels than in steels of lower carbon content. Experimental Procedure The radioactive iron used in this work was obtained from Oak Ridge National Laboratory. The unit consisted of about 1 microcurie each of Fe7 and Fe It was allowed to decay for two years. At the end of this time most of the Fe with a half-life of 46.3 days, had decayed, while most of the original Fe(half-life 2.91 years) still remained. The iron as chloride was extracted into an ether layer, using the method of Ashley and M~rray. After evaporation of the ether the iron chloride was dissolved in 250 ml of aqueous solution containing 2.4 gpl Fe. The compositions of the steels used are listed in Table I. Disks of ¾ in. diam and about ¼ in. thick were machined from these steels for use in diffusion couples. The disks were surface ground on both sides to ensure parallel opposite faces. One face of each disk was polished through 000 emery paper. Half of the prepared disks were plated with radioactive iron. For this, 1 ml of the radioactive iron

Jan 1, 1957

By W. E. Horst

Flotation feed was hell constant for batch laboratory tests and continuous pilot and commercial plant tests on a spodumene ore to determine the relation.ship between flotation behavior and the size and type of flotation machine. Results. showed that additional retention time would be needed in the plant flotation circuit to duplicate laboratory or pilot plant performance when operating Dariables of the. plant flotation machines remained unchanged. During the past few years of operation at Kings Mountain, N. C., full-scale flotation has generally yielded poorer metallurgical results than those obtained in the laboratory or pilot plant. After 2 min in each size of Denver flotation machine in the spodumene rougher circuit, pilot recovery (41.7 pct) was almost three times that of the plant (13.6 pct) and about twice that of the laboratory (21.0 pct). Pilot and commercial plant data are based on continuous operation, and laboratory results on batch testing of rougher performance. The ore is a pegmatite containing spodumene, feldspar, quartz, mica, and amphibolite. Data were accumulated to evaluate the scale-up relationships between laboratory, pilot plant, and plant flotation cells. Flotation rate constants and dimensional analysis were used to define the relationship existing between flotation behavior and scale of operation. Measuring Flotation Rates: Efficiency of the rougher stage was measured by flotation rate, defined as the recovery that can be attained within a given time." • The problem of measuring flotation rates has been studied by many investigators, whose methods have varied. Published studies an flotation kinetics have been summarized recently by Gaudin.l When comparing flotation rates, it is more satisfactory to compare straight line relationships between recovery and flotation time than exponential curves resulting from plotting cumulative recovery vs cumulative flotation time. To convert the exponential curves into straight line relationships, rate equations were applied similar to those used in chemical kinetics to study the velocity of chemical reactions. Two rate equations have been used in this investigation to measure efficiency of the various cells: 1.5 order Rate Equation dR/dt=k (A-R)1.0 [Eq.1] Second Order Rate Equation dR ---- - K(A - R)2 [Eq. 2] dt Upon integration Eq. 1 becomes 1/(A-R)1/2=k/2 t+1/A1/2 [Eq. 3] and Eq 2 becomes: or fEq. 4] t/R=1/A2K+t/A [Eq. 4] where R = cumulative recovery [percent recovery of total value (spodumene) in flotation feed]. A = initial concentration, pct (100 pct of mineral to be separated). t = flotation time (minutes). k = flotation rate constant for 1.5 order rate equation [units: 1/(percent) 0.5 (min)1. K = flotation rate constant for second order rate equation [units: 1/(percent) (min) 1.

Jan 1, 1959

By Clarence Wright

THE average lead and zinc content of the ores mined and milled in the Joplin district is low as compared with that of other lead and zinc deposits throughout the United States. Because of this fact and of the high grade of the concentrates, the ratio of concentration is unusually high. Most of the operating companies have aimed to produce as high a grade of concentrate as possible in order to obtain the highest price for their product. They have done this at the sacrifice of the percentage of zinc recovered. The average percentage of zinc recovery is from 60 to 70 per cent. For percentage of recoveries from actual mill tests, see tables. The concentration is commonly effected by crushing the ore to h-in. (12.7 mm.) size and subjecting it to a roughing and cleaning over two or more large Cooley jigs, of the Harz type, the finer sands being treated on the usual types of sand and slime tables. The treatment of slimes by flotation is being tested at several of the larger mills. COARSE CONCENTRATION When the ore. has been hoisted from the mine it is dumped onto a chute leading to a grizzly made of iron bars, usually heavy rails, spaced 4 to -5 in. (101 to 127 mm.) apart. The oversize is caught on the grizzly, the mineralized pieces are broken with sledge hammers so as to pass through, and the boulders that are practically barren are sorted out by hand and trammed to the waste-rock pile. The proportion of waste rock thus sorted out varies from a fraction of 1 per cent to 15 per cent., depending on the nature of the rock.

Jan 10, 1917

By Norman Ketzlach

Manganese Products, Inc. has developed a chemical process for the recovery of high-grade manganese oxides from low-grade manganese ores. Ammonium sulphate is also produced. Manganese ore is leached with sulphurous-sulphuric acids. The impurities are removed with ammonia, heat, and air. Manganese oxides are produced by addition of more ammonia and air under pressure. Ammonium sulphate is recovered from the remaining solution.

Jan 3, 1950

By G. R. Speich, R. A. Oriani

The rate of coarsening (Ostwald ripening) of copper precipitate Particles in an a-iron matrix has been studied in three Fe-Cu alloys containing 2.3, 4.0, and 5.4 wt pct Cu in the temperature range 730° to 830°C. The kinetics of Ostwald ripening ohevs the law as deduced by Lifshitz and Wagner so that matrix diffusion controls the process. The equilibrium shape of the particles is that of rods with hemispherical caps, and is due to the BOTH Lifshitz and slyozov and wagner3 have recently solved the complex problem of determining the rate of coarsening of an assembly of precipitate particles. Both workers, although using somewhat different mathematical approaches, arrive at the same equation for the relation between the mean radius 7 of a distribution of spherical particles and the bulk solubility co, diffusivity D in the matrix, large anisotropy in the copper/a iron interfacial free energy (y,/y, = 4). A Lifshitz -Wagner equation, modified for both the nonsphericity of the diffusion field and the reformulation of the Gibbs-Thomson equation for the case of nonsphencal particles, is derived. Using the modified equation, the calculated values of the mean radius are smaller than those observed by a factor of about one -half. absolute temperature T, gas constant R, surface free energy y of the precipitate/matrix interface, and the time t of aging: where V, is the molar volume of the precipitate and v is a stoichiometric factor. Wagner's treatment is restricted to the case of spherical particles growing in a liquid matrix where strain energy is not a factor. Lifshitz and slyozov have discussed the effect of anisotropic particle shapes and internal strains on the rate of coarsening. Oriani4

Jan 1, 1965

P. Herasymenko (New York University, New York) —The authors' experiments on equilibria between water vapor and liquid synthetic slags represent a valuable contribution to our knowledge of the nature of liquid slags. They can be regarded as a proof of ionic splitting of water molecules dissolved in slags. The assumption that water dissolved in slag was com- pletely ionized was made in my report on hydrogen equilibria in steelmaking as early as 194010. In that paper, the first systematic data were given on the content of ionized hydrogen in acid and basic open-hearth slags. The paper probably escaped the notice of the authors, although they mention the articles published later by other investigators who reported erratic and

Jan 1, 1958

By E. Douglas Sethness

The uranium industry is booming. In Texas alone, there are about 22 different companies with active exploration programs. Twelve solution mines have been permitted; three surface mines have been authorized; and two mills are currently in operation. However, the industry also has a problem, and that is the disposal of radioactive wastes. Over the past several years, stories concerning nuclear wastes have appeared frequently in the news. One of the most frequently cited cases occurred in Grand Junction, Colorado. In 1966, after ten years of investigations, the U. S. Public Health Service (PHS) discovered that tailings from a uranium mill were being used as fill material and aggregate for local construction purposes. It was estimated that between 150,000 and 200,000 tons of material had been removed and used under streets, driveways, swimming pools, and sewer lines. In addition, tailings had been used under concrete slabs and around foundations of occupiable structures. Further studies prompted the Surgeon General to warn that the risk of leukemia and lung cancer could be doubled at the measured radiation levels. More recently, the L. B. Foster Company discovered that its building site in Washington, West Virginia, was radioactive. While digging a foundation, the ground erupted and a ball of fire 30 feet high shot out. Evidently, the dirt was laced with radioactive thorium and zirconium, a potentially explosive mixture contained in a Nigerian sand which had been used by the previous site owners in the manufacture of nuclear fuel rods. Just this month we have read about legal suits to stop exploration for a nuclear waste disposal site in Randall County, Texas. The U. S. Department of Energy is trying to locate a deep underground nuclear waste depository for final burial of over 76 million gallons of high-level wastes. The problem is acute, the wastes are accumulating at a rate of about 300,000 gallons per year. Nor do these numbers include the spent fuel elements from nuclear power plants that are in temporary storage facilities. Fortunately, public awareness of these and other related issues is high. Unfortunately, the differences in the waste products from the nuclear fuel cycle are not always apparent to the general public. There are two distinct types of radioactive wastes: "high-level", which consist of spent fuel or wastes from the reprocessing of spent fuel; and "low-level", which, in general, are by-product wastes. There are numerous non-technical definitions that can be applied to help the layman differentiate between high-level and low-level wastes. For this latter purpose, it is best to think of them in terms of what we can see and feel. In general, high-level wastes are physically hot and can cause acute radiation sickness in a short period of time. Low-level wastes are not hot, but may cause chronic health effects after long exposure. The wastes which we are concerned with in the uranium mining and milling industry are low-level wastes. As recently as ten years ago, there were very few controls or regulations governing tailings disposal methods. At the same time, mine reclamation was not enforced through either state or Federal laws and the long-term viability of abandoned tailings ponds was not assured. The regulatory climate has changed significantly in the last decade, however. The low-level radioactive wastes generated by uranium mining and milling are generally contained in a tailings pond. Approximately 85-97% of the total radioactivity contained in uranium ore is present in the mill waste that goes to such tailings ponds. The isotope Radium-226 is probably the most potentially harmful radioactive parameter in the ponds. Radium emits gamma radiation and is also an alpha particle emitter. Because gamma radiation is very penetrating, it presents a potential health problem when a source is located external to the body. Gamma radiation will go through the body, causing damage to each cell encountered on the way. Although alpha particles have very little penetration capability, they can cause extensive cell damage. For this reason, alpha particles are a problem after inhalation or ingestion. Radium creates a health hazard by both of these mechanisms. Radium decays to radon gas which can be inhaled and serve as an alpha particle emitter. Additionally, radium is very soluble and readily enters the natural hydrologic cycle if allowed to leach from a tailings pond. With a half-life of 1620 years, radium has plenty of time to be taken into the food chain and end up in our bodies, emitting alpha particles. Because the potential health problems are better understood today than ten years ago, and because the Nuclear Regulatory Commission (NRC) has developed increasingly stringent government regulations, the uranium mining industry applies a high level of technology to the disposal of nuclear wastes. In most cases, low-level radioactive wastes are disposed of at or near the site where they are produced. There are six commercial burial grounds for low-level wastes, but it would not be economical to ship all mine or milling wastes to these sites. The on-site disposal methods most often used are ponding

Jan 1, 1979

By E. H. Rennhack, J. F. Libsch

Definite transition behavior was found in unalloyed titanium at 0.13 pct 0 equivalent. The addition of 0.5 Sn, 1.0 Al, 0.5 Al, and 1.0 Sn lowers the tvansition temperature of titanium at oxygen equivalents exceeding 0.22, 0.29, 0.40, and 0.51, respectively. Metallographic evidence indicates that progressive amounts of oxygen restrict deformation at low temperatures resulting eventually in brittle fracture. The presence of tin or aluminum is thought to alter the atomic distribution of oxygen within the titanium lattice in such a manner as to facilitate some degree of slip and twinning. 1 ITANIUM-like iron and zinc experiences a transition from ductile to brittle fracture with decreasing temperature. The presence of sufficient quantities of the interstitial elements, carbon, oxygen, and nitrogen in solid solution, has been shown to progressively lower the room-temperature impact resistance of titanium with increasing interstitial content.1"1 Ogden,et al,2 reported finding no transition from ductile to brittle fracture with decreasing temperature in iodide titanium. However, a definite transition was found to occur at 0.36 pct 0 equivalent in an alloy containing 0.47 pct carbon in solid solution. The oxygen equivalent in this case was obtained by assuming the effects of carbon, oxygen, and nitrogen in combination on the impact properties of titanium to be additive on the same basis as their separate effects on tensile strength, namely: Oe = 2/3 (pct C) + pet 0 + 2 (pet N) They concluded that the tendency toward transition behavior is dependent on the total interstitial content in solid solution and not on any one particular interstitial element. Rennhack,4 however, recently found transition behavior in iodide titanium at an oxygen equivalent of 0.17 pct. Ogden, etal3, reported that the strengthening effects of carbon, oxygen, and nitrogen in titanium decrease with the addition of tin. They showed that tin additions increase the tolerance of titanium for the interstitials, that is, 10 pct Sn permitted individual additions of up to 0.4 wt pct of the interstitial elements without any significant loss in ductility. Aluminum tends to decrease ductility and impact strength of titanium for a given interstitial ~ontent.3 Van Thyne and Kessler5 found that the solid solubility of carbon in titanium doubled in the presence of 10 pct Al. The precise effects of tin and aluminum in the nrespncp of rorvfen nn the impact properties of titanium had previously not been determined. The high oxygen tolerance of titanium containing tin may provide a suitable means for improving the impact properties of titanium containing the interstitial elements, particularly oxygen. Unlike tin, however, aluminum has a high affinity for oxygen and will reduce rutile titanium dioxide (TiO2)by a thermit-type reaction.6 Thus, the atomic distribution of oxygen in titanium might be different in the presence of aluminum. The present work was undertaken to: 1) Determine the effect of oxygen on the transition behavior of unalloyed iodide titanium. 2) Determine the effect of small amounts of tin and aluminum on the transition behavior of iodide titanium in the presence of oxygen and other interstitial~. EXPERIMENTAL Three different lots of iodide titanium were employed to prepare the alloys studied in the present work. Their chemical composition is presented in Table I. The compositions of the tin and aluminum used for alloying are shown in Table 11. Oxygen additions were made using calcined rutile titanium dioxide (TiO2)of 99.7 pct purity. Alloy Preparation—Four titanium-base alloys containing separate additions of 0.5 and 1.0 pct each

Jan 1, 1960

By L. Adler

The author recently proposed a technique for handling the effect of planes of weakness on failure in geologic material.1 The technique employed an "extended" Mohr's rupture envelope, on which was superimposed a generalized three dimensional stress representation. Subsequently, the method was applied to so-called two-dimensional stress states" which were in reality degenerate three-dimensional ones. Since a two-dimensional stress solution usually refers to a plane stress condition, the terminology was confusing. The distinction between a plane stress state and a degenerate three-dimensional one is shown in Fig. 1. The solution of problems involving a generalized three-dimensional stress state is greatly aided by continual reference to the basic principle that no stress components can act on a plane, oriented as is the weakness plane, which lies outside of the weakness plane's rupture enVelope.2 This is shown in Fig. 2; and if it is also remembered that the radii of the Mohr's Circles give the orientation of such a plane, solutions are easier to follow, and perform. Sample Problem 1: Site Location (generalized three-dimensional case).' Given: 1) Both rupture envelope for the solid and plane of weakness. 2) Existing principal stresses and orientations in space (?12, ?13) obtained from a stress analysis of the proposed structure. Find: Permissible orientations of the weakness plane in order to select a suitable site.

Jan 1, 1963

By Peter J. Conroy, Julianne H. Gyarmaty

INTRODUCTION The current study is part of the U.S. Department of Energy's (DOE) on-going subsidence research program. The long-term objective of the DOE program is to develop analytical methods of subsidence prediction applicable over a broad range of geologic and mining conditions encountered in the United States. The DOE currently has several contracts in progress to develop a sound data base that can be used in the development of predictive models. Dames & Moore is currently under contract to DOE to collect and analyze detailed subsidence and hydrologic data from a coal mine employing longwall mining methods in the Eastern Coal Province. Work under Contract No. DE-AC22-80PC 30335 began in October of 1980 and will continue through September of 1984. The contract includes monitoring of two adjacent longwall panels. This paper summarizes the surface monitoring work that was performed through February of 1982. Mining of the first of the two panels (3 off 3 north) was completed on February 3, 1982. Results of the surface monitoring through completion of this panel are presented and discussed. SITE DESCRIPTION The mine being studied is located in eastern Ohio. The site is west of the Ohio River, approximately 56 km (35 miles) south of Wheeling, West Virginia. The topography of the unglaciated region

Jan 1, 1982

By M. D. Banus, M. B. Bever, A. K. Jena

Measurements of the heat effects on addition of various solid phases of InSb to a solution calorimeter have confirmed the existence of a new high-pressure plzase InSbQII), which was jormed at 37 kbar and 623°K. The heats of formation of InSbQ), InSbfl), and InSb(111) have been measured and the heats of transjormation of InSb(1) to InSb(1l) and InSb(Iii) and of 'InSb(ll) to InSb(iiI) at atmospheric pressure and 78°K have been determined independently. Other thermodynamic properties of these phases, the phase boundary InSb(i)/InSb(ll), and the relative positions of the triple points are calculated. The pressure-Dolume term is shown to be more critical than the internal energy difference in making the phase InSbQ) less stable than InSb(II) at high pressures. Observations on partially transformed specimens suggest that the transformation of' metastable InSb (III) takes place in the two steps InSb(lll) — InSbQI) and InSbQI) — InSb(l). The compound InSb can exist as several phases depending on the temperature and pressure. The phase InSb(I), which is a semiconductor having the zinc-blende structure, transforms into the phase InSb(11) at a pressure of about 23 kbar and room temperature.'-3 The phase InSb(II) has the 6 tin structure,4-6 is metallic, and becomes a superconductor below 2.lok7 An orthorhombic phase of InSb has been reported to occur above a pressure of approximately 30 kbar at room temperature.' This phase is also a superconductor below about 3.4k9 The phase InSb(I1) is retained at atmospheric pressure if it is quenched to 78°K under pressure,6,7 but tends to transform at higher temperatures and does so explosively above approximately 210ok,7 A value of the heat of transformation of InSb(1) to InSb(II) at 210°K and atmospheric pressure has been reported.' A concurrent publication'0 reports evidence for a new solid phase InSb(III), which was formed by annealing InSb above 58 1°K at 37 kbar, above 560°K at 52 kbar, and above 473°K at 65 kbar. Specimens of InSb(II1) had a superconducting transition temperature of 4.lo ± 0.1oK. X-ray diffraction patterns also indicated the presence of a new phase. In this communication, thermodynamic properties of the phases InSb(I), InSb(II), and InSb(II1) are reported and discussed. The phase boundary InSb(I)/InSb(II) and the relative positions of the triple points are calculated. 1) EXPERIMENTAL 1.1) Preparation of Specimens. Specimens of the high-pressure phases of InSb were prepared in a belt-type high-pressure chamber by a tichnique described in detail elsewhere.'' Charges of 0.6 to 0.8 g of Cominco semiconductor grade InSb were used. The temperatures were measured with a chromel-alumel thermocouple, the hot junction of which was within 0.5 mm of the specimen. The specimens were heated under a pressure of 37 kbar for 1 hr at 723°K (which is well above the liquidus) and quenched to room temperature. One set was annealed at 523°K and another set at 623°K for 20 to 24 hr. These annealing temperatures were chosen because 523°K was below and 623°K was above the temperature of the transformation of InSb(II) to InSb(1Tl) at 37 kbar.10 The specimens were then cooled to 125°K by passing liquid nitrogen through the jacket of the belt die before the

Jan 1, 1968

US 4,135,913-Extraction of nickel values from iron-containing nickel sulfide ore, particularly pentlandite or nickeliferous pyrrhotite A mixture of raw ore, roasted ore, or iron powder, and coal as a reductant is heated to a temperature of 800- 1000° C in a nonoxidizing atmosphere to convert the bulk of the iron content to metallic iron while diffusing into the iron the bulk of the nickel, the mixture cooled, and the cool material separated into a magnetic fraction containing most of the nickel and a non-magnetic gangue fraction A Illis arid L S Renzoni, assigned to International Nickel Co, Inc Jan 23, 1979 7 pp (75-21) Filed 10-10-75 (621,343) Priority Canada, 10-27-72 (155,032) Same Canadian 981,910, dated Jan 20, 1976 Same British 1,389,145, dated Apr 3, 1975 US 4,135,917-In the recovery of gallium from a solution obtained by the digestion of bauxite or nepheline in an alkali solution for the production of alumina, the digestion solution is neutralized, the neutralized solution evaporated to an op¬timum caustic alkali concentration and adjusted to a ratio of alkali metal oxide to alumina of above 2, the corrected solu¬tion contacted with a gallium-aluminum alloy, arid high-purity gallium recovered from the solution by electrolysis or cemen¬tation K A Badaliants, et al Jan 23, 1979 6 pp (75-109) Filed 12-19-77 (862,201) Priority USSR, 12-22-76 (2,428,¬006) US 4,135,918-Extraction of copper from copper sulfide ore containing also one or more of the metals iron, nickel, arid cobalt Ore is roasted at a temperature of 750-800° C to expel sulfur, the sulfur-free calcine slurried in water containing a sufficient amount of sulfuric acid to supplement any sulfuric acid formed in situ, the slurry heated at 150-165° C in the presence of a reducing gas to form soluble sulfates of metals other than copper while reducing copper to elemental form, arid the slurry filtered to recover copper solids Any precious metals present in the ore will report with the copper solids V A Ettel, A P Devuyst, R Sridhar, arid C. E O'Neill, as¬signed to International Nickel Co, Inc Jan 23, 1979 5 pp (75-117) Filed 3-2-78 (882,610) Priority Canada, 5-13-77 (278,360)

Jan 1, 1980

By Leon W. Dupuy

SUPPLEMENT THESE tables should accompany Figs 6, 7, 8, 9 and 10, respectively. To follow Fig 6: TABLE 2[a]-Drill Rod [ ] To follow Fig 7: TABLE 3-Rod Coupling [ ]

Jan 1, 1947

By C. W. Mason

TIN has long been cited as offering a classic example of polymorphism, second in repute only to the allotropy of sulphur. The notorious "tin disease," which Cohen1 has studied so exhaustively in terms of the enantiotropic transformation of tetragonal white 0 tin to cubic gray a tin, has apparently encouraged the expectation that one or more addi-tional polymorphic modifications might exist. The search for confirma-tion of this idea has, as might be anticipated, led to the accumulation of a body of miscellaneous evidence, much of which would probably never have been sought, or taken seriously even by its discoverers, but for previous assumptions. The ball apparently was started rolling in 1880 by Trechmann,' who reported a new modification of tin (y tin), which was brittle and found in "hard head," a highly arsenical, slaggy material produced in a certain stage of tin smelting. A mixture of two kinds of crystals was obtained from a Cornish tin furnace, and those thought to be y tin were studied crystallographically. The results indicated that these crystals were rhombic and of different density from the tetragonal tin prepared electrolytically by Miller.3 Their analysis was given as 98.7 per cent Sn, 1.3 per cent Fe, and traces of As, Sb, Bi and S. In 1881 von Foullon4 obtained similar crystals from a Bohemian tin furnace. Headden5 examined crystals similar to those of Trechmann and von Foullon and reported them to be monoclinic, but of analysis corresponding to stannous sulphide. Later, Stevanovic,6 by goniometric measurements, proved that these crystals of SnS were really rhombic. Groth7 pictures and describes both "rhombic tin" (Fig. 9, vol. 1) and stannous sulphide (Fig. 84, vol. 1); their faces and angles correspond within the accuracy of measurement. Spencer3 in 1921 examined the above evidence critically; he found similar crystals from Cornish tin furnaces, proved them to be SnS, and even was able to analyze some of Trechmann's original specimens, finding high sulphur content. (Apparently Trechmann's analysis had been based on a second lot of crystals, not described crystallographically.)

Jan 1, 1939

By H. Biloni, R. Morando

The surface structure and substructure of Al-Cu alloys solidified as conventional ingots and under particular conditions such as those used by Bower and Flemings are studied. The influence of lampblack coating on the mold walls is especially considered and the results compared with those obtained in copper and graphite molds where no coatings exist. When high heat extraction conditions exist the observations show that mechanism of copious nucleation is responsible for most of the chill zone. When the heat extraction through the mold walls is low, a coarse grain structure with dendritic morphology arises, with a size that depends on the degree of convection present, analogous to that analyzed by Bower and Flemings. In both cases the effect of the convection on the macroscopic and microscopic appearance is discussed. The ingot macrostructure consists of one or more of three zones: "chill zone", "columnar zone", and central "equiaxed zone". The mechanism of the columnar-equiaxed transition has been subject of considerable interest and at present at least three theories exist about the formation of the equiaxed region: 1) the constitutional supercooling theory1 maintains that the equiaxed crystals nucleate after the columnar zone has formed, as a result of the constitutional supercooling of the remaining liquid; 2) chalmers2 pointed out, however, that there were several objections to this proposal, and that consideration should be given to the possibility that all the crystals, equiaxed as well as columnar, originated during the initial chilling of the liquid layer in contact with the mold; 3) Jackson et aL3 and O'Hara and ~iller~ suggested that a remelting mechanism of the dendrite arms is responsible for the formation of the equiaxed region. After the work of Cole and Bolling and other authors6 it became evident that convection (natural, reduced, or forced) plays a very important role in the transition from columnar to equiaxed and on the size of the resultant equiaxed structure. Until recently the accepted explanation of the chill zone was that it occurs as a result of copious nucleation in the liquid layer in contact with the mold walls.798 The columnar region is a subsequent result of the growth of favorably oriented grains and, as a result of a selection mechanism studied by Walton and Chalmers,9 elongated grains with marked texture are formed. Recently, however, Bower and Flemings" using an ingenious laboratory experiment introduced the idea that the "copious nucleation" mechanism is not responsible for the formation of the chill zone and that the presence of convection, introducing some form of "crystal multiplication", plays a decisive role in the formation of the chill zone. Unfortunately, it is important to consider that for their conclusions Bower and Flemings extrapolated the results obtained in their special experiments to the case of conventional ingots, and that these authors only analyzed the macrostructures of the specimens. Let us consider the work by Biloni and chalmers" concerning predendritic solidification. These authors were able to show that a study of the segregation substructure of A1-Cu gives information about the nucleation and growth of crystals formed in contact with a cold surface. A spherical predendritic region characterizes the first part of every grain nucleated in contact with the surface as a result of the chill effect. The aim of this paper is to elucidate through the observation of the segregation substructure the conditions under which (in the Bower and Flemings type of experiments and in conventional ingots) either the nucleation or the multiplication mechanism gives rise to the structure in contact with the mold walls. I) EXPERIMENTAL TECHNIQUES The experiments were performed on two alloys: Al-1 wt pct Cu and A1-5 wt pct Cu. The purity of the aluminum was 99.99 pct and the copper 99.999 pct. The results obtained with both alloys were similar. In the Bower and Flemings type of experiments the apparatus employed to obtain rapid solidification against a surface was similar to that used by those authors. The liquid was drawn by partial vacuum into the thin section mold cavity. Plate casts were 5 cm wide and usually 7.5 cm high. The thicknesses of the cast were 0.1 and 0.3 cm. Two different materials were used for the mold, copper and nuclear-grade graphite. The internal mold surfaces were polished and left uncoated for some experiments. In other experiments, the copper or graphite surface was coated with a thin film of lampblack material. In some of these particular experiments one of the mold walls was left with an uncoated region (usually in the form of a cross). The conventional ingots were cast in graphite or copper molds. In different experiments the mold walls were sometimes uncoated or coated with lampblack material. The results obtained in conventional and Bower and Flemings copper molds were compared with those obtained with copper molds coated with a very thin film of graphite; the results obtained were essentially similar. The size of the conventional ingots was 5 cm diam and 7 cm high in all cases. The cast surfaces produced by the Bower and Flemings type of experiments and conventional methods were observed macroscopically and microscopically without any metallographic preparation. As Biloni and Chalmers showed," the observation of the chill surface can give considerable information about the structure and segregation substructure.

Jan 1, 1969

By Ben. B. Cox

The principal events during the year consisted in the exploitation of the Kirkuk field, the regular operation of the four-million-ton pipe line to the Mediterranean, and the discovery of low-gravity oil on three other structures in the West Tigris (Shergat) area. The Iraq Petroleum Co., Ltd. continued the systematic exploitation and exploration of its Kirkuk field, maintaining a carefully unitized operation. Bottom-hole pressure differentials and low gas-oil ratios were maintained. All crude was produced by flowing The cleaning up following the construction of the Mediterranean pipe line, which began deliveries in August, 1934, was completed during the first quarter of 1935. The line easily maintained its rated capacity for the remainder of the year. The Mosul Oilfields, Ltd., through its operating subsidiary, the B.O.D., Ltd., expanded its exploratory organization from 9 to 16 drilling rigs and discovercd 20" A.P.I. crude on the Sadid, Hibbarah and Qasab anticlines. Whether these discoveries will be commercial pools remains to be proved. The Qaiyarah-Najmah-Jawan field, which was discovered by the I.P.C. in 1928, was extended arid production was found in the Eo-Cretaceous as well as the "Main Limestone" (Eocene, Oligocene and Lower Miocene). Gas caps were found under each of the crests of the West Tigris structures. Negotiations are in progress between the Mosul Oilfields, Ltd. and the Iraq Government for the extension of the Anatolian Railway from the Turkish border to Mosul, with a view to tanking the heavy West Tigris crude to the Mediterranean. The subsidiary of the Anglo-Iranian Oil Co., Ltd.', the Khanaqin Oil Co., Ltd., continued to operate its Naft Khaneh field near the Iranian (Persian) border to supply the local Iraq market through the Rafidain Oil Co., Ltd. Somewhat more than 28 million barrels of crude was produced in Iraq during 1935. Crude delivcred to the pipe line for export during the years 1934 and 1935 was: Year BaRrels 1934................................................. 7,096,669 1935................................................. 27,014,904 Total as at Dec. 31, 193.5.............................. 34,111,573 ° Converted at an avcrage of 7.0 bbl. per ton.

Jan 1, 1936

The principal events during the year consisted in the exploitation of the Kirkuk field, the regular operation of the four-million-ton pipe line to the Mediterranean, and the discovery of low-gravity oil on three other structures in the West Tigris (Shergat) area. The Iraq Petroleum Co., Ltd. continued the systematic exploitation and exploration of its Kirkuk field, maintaining a carefully unitized operation. Bottom-hole pressure differentials and low gas-oil ratios were maintained. All crude was produced by flowing The cleaning up following the construction of the Mediterranean pipe line, which began deliveries in August, 1934, was completed during the first quarter of 1935. The line easily maintained its rated capacity for the remainder of the year. The Mosul Oilfields, Ltd., through its operating subsidiary, the B.O.D., Ltd., expanded its exploratory organization from 9 to 16 drilling rigs and discovercd 20" A.P.I. crude on the Sadid, Hibbarah and Qasab anticlines. Whether these discoveries will be commercial pools remains to be proved. The Qaiyarah-Najmah-Jawan field, which was discovered by the I.P.C. in 1928, was extended arid production was found in the Eo-Cretaceous as well as the "Main Limestone" (Eocene, Oligocene and Lower Miocene). Gas caps were found under each of the crests of the West Tigris structures. Negotiations are in progress between the Mosul Oilfields, Ltd. and the Iraq Government for the extension of the Anatolian Railway from the Turkish border to Mosul, with a view to tanking the heavy West Tigris crude to the Mediterranean. The subsidiary of the Anglo-Iranian Oil Co., Ltd.', the Khanaqin Oil Co., Ltd., continued to operate its Naft Khaneh field near the Iranian (Persian) border to supply the local Iraq market through the Rafidain Oil Co., Ltd. Somewhat more than 28 million barrels of crude was produced in Iraq during 1935. Crude delivcred to the pipe line for export during the years 1934 and 1935 was: Year BaRrels 1934................................................. 7,096,669 1935................................................. 27,014,904 Total as at Dec. 31, 193.5.............................. 34,111,573 ° Converted at an avcrage of 7.0 bbl. per ton.

Jan 1, 1936

By T. R. Ingraham

When aluminum sulfate was decomposed in an evacuated apparatus and the sample cooled, Q alumina was found. The thermodynamics of the decomposition reaction were resolved by measurements of the total pressure of SO3, SO2, and O2 generated over the sample at various temperatures. The results were correlated with other published data to calculate the rmges of thermodynamic stability of the various compounds involved. The thermal decomposition of aluminum sulfate was studied by Wijhler, Pluddeman, and Wöhler1 and by Warner and Ingraham.2 The results of both studies were critically reviewed by Kellogg,3 who observed that "each set of data shows considerable scatter and strong curvature on a plot of log pso3 vs 1/T".3 He agreed with Warner and Ingraham2 that both the discrepancy in the two sets of results and their curvature may arise from the indefinite properties of the particular form of A12O3 which is formed during the decomposition. While studying the thermal stability of other sulfate systems, we had noted the presence of nonequilibrium oxide properties in both the cobalt4 and manganese5 systems, but neither had shown any appreciable curvature on a logPSO, vs 1/T relationship, and the data from both systems agreed reasonably well with prior work. It therefore seemed reasonable to reexamine the technique which had been used in our earlier work on aluminum sulfate.2 The principal difference was that a tightly compacted pellet had been used for the earlier aluminum sulfate work, whereas a loose powder, contained in a platinum boat, was used for our work on other sulfate systems. In addition, a better technique had been developed for dehydrating the samples. From work done on the nickel system,6 we had become aware of the highly protective nature of some sulfate layers on their oxjdes, and hence of the necessity of providing a large surface area of P3e sample when equilibrium was to be attained in a reasonable time. That observation suggested that perhaps a steady state, rather than equilibrium, had been reached in the earlier work on aluminum sulfate. This paper reports a repetition of the experimental work with large, finely divided samples of anhydrous aluminum sulfate. APPARATUS AND PROCEDURE The apparatus used in the experimental work was described in earlier papers.2,7 The source material was Anachemia reagent-grade Al2(sO4)3 - 18H2O which was first partly dehydrated by heating at 400°C for 48 hr and then completely dehydrated by repeated baking of an aluminum sulfate-oleum slush to dryness at 450°C. ? Alas was prepared by decomposing some of the sulfate in a muffle furnace at 800° C overnight. Approximately equal amounts of the 7) alumina and aluminum sulfate were used in the experiments. The finely divided samples were handled under dry box conditions, and in addition some of the aluminum sulfate was decomposed in the apparatus while it was under vacuum, to ensure its complete dehydration prior to sealing the apparatus. The samples were heated to a series of constant temperatures on both increasing- and decreasing-tem-perature programs. Two to three days were required to obtain steady readings of the total decomposition pressure on an increasing-temperature program, and 5 to 6 days on a decreasing-temperature program. Three samples were examined on both programs. Within experimental error, the results for each sample and each program could not be distinguished.

Jan 1, 1969

By M. R. J. Wyllie, P. F. Southwick

The importance of the so-called "dirty sand" or "conductive solids" problem in electric log interpretation was first stressed in a paper presented in 1949. Since that time the problem has been generally recognized as a most serious one. Several research papers bearing on the theory of the effects of clay contaminants on reservoir rock resistivities have appeared. These papers, while contributing to the theory of the problem, have not offered any practical solution. In the present paper an experimental investigation has been made of the effects of ion-exchange materials on the electrical properties of natural and synthetic porous media. The method used to make synthetic dirty sands is entirely novel and has proved a valuable guide to a better understanding of the properties of dirty sands generally. The effects of ion-exchange materials on both the resistivity and self potential (S.P.) logs have been examined. From the data obtained it has been possible to formulate a simple, practical method whereby electrical logs of dirty sands can be qualitatively interpreted. The method is in all essentials identical to that presently in use for interpreting clean sands. New light has also been thrown on the significance of the term formation factor when it is applied to dirty sands. In 1949 a paper was presented1 which showed that the presence of so-called "conductive solids" introduced considerable complexities into the analysis of the resistivities of dirty sands, i.e., permeable formations containing clay. The reduction of the self potential (S.P.) resulting from the presence of interlaminated shale or interstitial clay in permeable formations has been discussed by Doll.2,3 Noteworthy papers which dilate further upon the effects of shale and clay on the resistivity of permeable formations are those of deWitte,4,5 Berg,6 Wyllie,7 and most recently, Winsauer and McCardell.8 The last authors have endeavored to elucidate the chemistry of the resistivity phenomena in dirty sands in terms of an adsorption hypothesis. Specifically, they attribute the electrolytic conductivity of shales and clays within a permeable formation to an ionic double-layer effect and, for this reason, regard the term "conductive solids" as a misleading one. Some consideration has been given to the effect of dirty sands on the S.P. by Wyllie7 and by McCardell, Winsauer and Williams." Published work to date has cast light only on certain theoretical aspects of the problems created by the presence of clays and shales within permeable formations. One object of this paper is to describe experiments which serve to elucidate further the theory of the dirty sand problem and particularly the significance of the term "formation factor" as applied to dirty

Jan 1, 1955