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By M. E. Wadsworth, L. H. Raby, A. S. Peck

Infrared spec troscopy was used to study the adsorption of oleate collector on three varieties of hematite. Each of the minerals was found to react with either oleic acid or a solution of sodium oleate to form a mineral cation-collector anion chemisorbed layer at the solid-liquid interface. The chemisorption reaction displaced surface hydroxyls and was found to be pH dependent. The infrared band characteristic of the antisymmetrical C = 0 structural group of chemisorbed oleate appears between 1520 and 1540 cm-'. Evidence is presented which shows that molecular filming of the mineral surfaces with un-dissociated oleic acid precedes chemisorption. Infrared absorbance is correlated with the flotation behavior of the mineral. Adsorption processes are usually classified into two types which are distinguished and character- ized by the nature of the bond formed between the adsorbate and adsorbent. The process in which molecules chemically bond to solid surfaces is termed activated adsorption or chemisorption. If only weak van der Waals forces bind the molecules to the surface then the process is termed physical adsorption. Chemisorption is of primary interest in flotation systems since selectivity may be obtained if a single mineral is rendered air-avid by a specific collector mineral adsorption reaction. In previous studies infrared spectroscopy was used to define the mechanisms involved in the adsorption of oleic acid and sodium oleate on fluorite, barite, and calcite. Infrared techniques were particularly useful since adsorbed monolayers were identified in situ. Further, the infrared method permitted identification of reaction products in the solid, liquid, and vapor phases of the systems. The chemisorption reactions displaced F- from fluorite, SO4 from barite, and CO3 from calcite. This investigation was pursued in an effort to characterize and interpret the adsorption processes for synthetic hematite, compact red hematite, and specular hematite (crystalline hematite). Adsorption tests were performed using either oleic acid or

Jan 1, 1967

A contract for three 20 ft diameter vertically mounted axial flow fans of the same aerodynamic design, was placed by Mount ]sa Mines Limited in 1963. The hydraulic blade pitch changing mechanism, the method of blade fabrication, and the roll out centre casings are features of these fans. Protection devices and fan control are designed for unattended operation and remote control. The erection and commissioning of the fans during 1964-65 is described.

Jan 1, 1967

By P. Niessen, W. C. Winegard, C. J. Beingessner

DURING the last 10 years, several grain-growth studies have been made using zone-refined metals with controlled amounts of solute to elucidate the interaction of solute with moving boundaries. In all these studies, it was more or less implicitly assumed that the alloys used were, after recrystallization and grain growth, homogeneous within the grains with respect to solute and lattice defects. This note deals with observations made on microstructures originating from solidification of dilute alloys and from grain growth. Briefly, the experimental procedure used in these studies was the following: zone-refined cadmium and master alloys were melted and cast in Pyrex under vacuum to produce bars 14 mm in diam and about 150 mm long. These bars were cut into 8-mm-thick slices which were mechanically and chemically polished. The specimens were then deformed 30 pct in compression and given a 1-week anneal at 260°C in argon. After this anneal, a second deformation produced completely recrystallized samples 4 mm thick. The time-temperature controlled anneals were carried out in a bath of silicone oil. After the grain-growth anneal, the specimens were polished in Gil-man's' solution (33 g CrOs, 6 g NazSO, in 100 ml of water). Several etches were used depending on the alloy investigated, but mostly a mixture of concentrated HC1 and HNOj (98:2 vol) was employed. In all the alloys examined, the ease with which substructures could be revealed depended strongly on the crystallographic orientation of the surfaces of the grains. However, very frequently the microstructures to be discussed here etched up over broad areas comprising several grains. Fig. 1 is a micrograph of a Cd-0.05 at. pct Mg alloy annealed for 100 sec at 270°C. Different substructures are seen in this photograph. A denotes the now existing grain boundaries. The well-defined lines and points marked B are the remains of a solidification substructure. The lines are boundaries between cell colonies, and the points are nodes located on regular two-dimensional cells. This cellular structure has the same appearance as that found by weinberg2 for rapidly quenched Zn-Au alloys. The "ghost boundaries", marked C, are very similar in appearance to a grain boundary array in a polycrystalline sample. Repeated polishing and etching showed that all the substructures observed were three-dimensional. To date, the ghost boundaries have been clearly observed in all samples containing 0.005, 0.01, 0.05, and 1 at. pct Mg, and in samples containing 0.01 at. pct Zn. Attempts to outline these ghost boundaries in cadmium alloys containing 0.01 at. pct Ag and Au were only partially successful. In these alloys, parallel lines, having a resemblance to the ghost boundaries in the Cd-Mg and Cd-Zn alloys, were observed, but it was not possible to obtain complete arrays of ghost boundaries which extended over several grains. It is possible that a different etch than that presently employed would reveal the ghost boundaries in the Cd-Au and Cd-Ag alloys as clearly as in the Cd-Zn and Cd-Mg alloys. A close examination of the ghost structure showed that it consisted of linear etch-pit arrays, Fig. 2. The ghost boundaries were resolvable even in grains which showed over-all faceting due to the etching, as seen in the corner of Fig. 2. The general appearance of the ghost structure suggests that it originated during grain growth. This is supported by the observation that the mesh width in the ghost-boundary array generally increased with increasing final grain size. To test whether the ghost structure was formed during the long homogenizing anneal or during the grain-growth anneal, some as-cast samples were deformed and given a grain-growth anneal. This anneal was terminated by air cooling or

Jan 1, 1967

By R. W. Bartlett

DISILICIDE coatings, MeSi2, on refractory metals are usually grown by a solid-state diffusion reaction similar to the parabolic oxidation of metals. Two or more silicide compounds occur in each of the binary silicon-refractory metal systems. When an adequate source of silicon is available during the coating process, the lower silicide compounds are usually not formed.1 However, during service application of the coated refractory metal, continued heating causes further diffusion and growth of the lower silicides. A study of the growth kinetics of the lower silicides in the molybdenum and tungsten binary systems with silicon was previously reported.2 The present study is concerned with the growth kinetics of Ta5Si3 and Cb5Si3, formed as conjugate layers between TaSi2/Ta and CbSi2/Cb diffusion couples, respectively. Diffusion couples consisting of disilicide-coated tantalum and columbium sheet coupons were subjected to diffusion heat treatments, cross-sectioned, and scanned by an electron-microprobe analyzer to determine the relative X-ray intensity profiles. These profiles correspond closely to concentration profiles for the constituents, and were used to identify phases and locate phase boundaries. The analysis of a single specimen after a diffusion-anneal provides only one value for the Me5Si3 phase thickness, corresponding to the time and temperature of the diffusion treatment. Consequently, each isothermal curve showing the rate of accumulation or depletion of silicide phases required several samples with identical diffusion temperatures but different diffusion times. The disilicide coatings were prepared by pyrolizing commercially pure silane in a hydrogen carrier gas. The hydrogen was purified by passage through a palladium membrane. Commercially pure tantalum and columbium sheet metal coupons, 0.005 by $ by 2 in., were used. All of the coated specimens for each system were prepared together in a single group in order to minimize coating variations among individual specimens. During pyrolysis, the brightness temperature was maintained at 1200°C. With suitable flow rates at this temperature, only the disilicides of tantalum and columbium were formed in detectable amounts. Coated specimens were subjected to diffusion an-neals in a tube furnace with automatic proportional control within ±10°C. A H2-Ar mixture, deoxidized and dried over anhydrous magnesium perchlorate, was used to prevent oxidation during the diffusion anneal. Diffusion couples were cross-sectioned, polished and examined with an A.R.L. electron-microprobe X-ray analyzer. Both metal constituents in each specimen were simultaneously scanned using a 1-p beam spot size and either 1- or 2-µ steps. Analyses were performed using the Ka radiation of columbium and silicon, and the La, radiation of tantalum. For all specimens, an acceleration voltage of 30 kv was used, and integration was made against the specimen current. LiF and A DP monochrometers were used to isolate characteristic radiations. Three or more traverses were made on each specimen. The intensity scales were adjusted using the constituent metals and standard samples of the silicide compounds which had been verified by X-ray diffraction. The relative intensity profiles were used directly, in conjunction with the standard samples, to identify compounds and phase boundaries. The stoichiometries differ considerably between the silicide compounds in both systems, and the homogeneity range for these silicide compounds is narrow. These characteristics result in marked differences in relative intensities of the fluorescing elements—differences which permit ready identification of phases and phase boundaries. Projections of both electron back-scattered images and characteristic

Jan 1, 1967

By C. G. Dunn

James, Jones, and Leak (JJL) conclude that growth-rate and orientation-distribution data obtained in a steep thermal gradient should be used with caution to account for isothermally produced recrystallization textures. I agree. However, it is not clear whether they conclude a) that the orientation dependence of rate of growth of secondaries in (commercial) silicon iron depends on both temperature and a temperature gradient or b) that, in applying rate data obtained in a steep thermal gradient, the isothermal annealing temperature must be close to the temperature for which the rate data apply. Also, it is not clear what tem-

Jan 1, 1967

By R. W. Snyder, W. H. Guilinger, B. S. Gottfried

Two numerical methods are presented JOT solving the equations Jor one-dimensional, multiphase /low in porous media. The case oF variable physical properties is included in the Formulation, although gravity and capillarity are ignored. Both methods are analyzed mathematically, resulting in upper and lower bounds for the ratio of time step to mesh spacing. The methods are applied to two- and three-phase waterflooding problems in laboratory-size cores, and resulting saturation and pressure distributions and production histories are presented graphically. Results oJ the tuo-phase flow problem are in agreement with the predictions of the Buckley-Leuerett theory. Several three-phase flow problems are presented which consider variations in the water injection rate and changes in the initial oil-and ujater-saturation distributions. The results are different physically from the two- phase case; however, it is shown that the Buckley-Lez~erett theory can accurately predict fluid interlace velocities and displacing-fluid frontal snturations for three-phase flow, providing the correct assumptions are made. The above solutions are used as a basis JOT et~aluuting the numerical methods with respect to machine time requirements and allowable time step for a fixed mesh spacing. INTRODUCTION Considerable progress has been made in recent years in obtaining numerical solutions of the equations for two-phase flow in porous media. Douglas, Blair and Wagner2and McEwenll present different methods for solving the one-dimensional case for incompressible fluids with capillarity (the former using finite differences, the latter with an approach based upon characteristics). Fayers and Sheldon4 and Hovanesian and Fayers8 have extended these studies to include the effects of gravity. West, Garvin and Sheldon, l4 in a pioneer paper, treat linear and radial systems with both capillarity and gravity and they also include the effects of compressibility. Douglas, Peaceman and Rachford3 consider two-dimensional, two-phase, in compressible flow with gravity and capillarity and Blair and Peaceman1 have extended this method to allow for compressible fluids. No one, however, has examined the case of three-phase flow, even for the relatively simple case of one-dimensional flow of incompressible fluids in the absence of gravity and capillarity. In obtaining a numerical technique for simulating forward in situ combustion laboratory experiments, Gottfried5 has developed a method for solving the one-dimensional, compressible flow equations with any number of flowing phases. Gravity and capillarity are not included in the formulation. The method has been used successfully, however, for two- and three-phase problems in a variable-temperature field with sources and sinks. This paper examines the algorithm of Gottfried more critically. Two numerical methods are presented for solving the one-dimensional, multi-phase flow equations with variable physical properties. Both methods are analyzed mathematically, and are used to simulate two- and three-phase waterflooding problems. The numerical solutions are then taken as a basis for comparing the utility of the methods.

Jan 1, 1967

Jan 1, 1967

By F. Haessner, M. Wilkens, U. Jakubowski

ThOUGH at present there is a wide range of possibilities for the quantitative determination of preferred orientations, pole figures of identical specimen material have not been determined by different methods as yet.''' In this paper a comparison of (Ill), (200), and (220) pole figures is presented which were obtained from a 95 pct cold-rolled high-purity cop- per sheet (99.9998 pct Cu), by three different methods. The three methods are: a) The combined X-ray reflection-transmission technique of plane samples by schulz3 and Decker, Asp, and Harker. 4 A Siemens texture goniometer was used. The experimental details are described elsewhere. 6 b) The X-ray reflection technique of spherical samples by Jetter and Boric.' A Siemens texture goniometer with some modifications was used. The samples were prepared by sticking 140 polished sheets together with an adhesive and machining a sphere (20 mm diam).* Additional

Jan 1, 1967

By Ronald P. Hollenbeck

The value of mineral production in Alabama increased 1 percent above the record high set in 1965. Alabama ranked second among the States in the production of bauxite, third in the production of masonry cement, native asphalt, and scrap mica, sixth in the production of portland cement, ninth in the production of iron ore, and tenth in the production of lime. The mineral industry of Alabama was dominated by the mining and processing of coal and stone, the manufacturing of cement, and the production of crude petroleum. These industries accounted for 87 percent of the State's total value of mineral production, compared with 85 percent in 1965.

Jan 1, 1967

By Forrest T. Moyer

The overall disabling work injury experience, excluding office- workers, at nometal mines and mills during the period 1961-63, as reported to the Bureau of Mines by operators, was 77 fatal and 7,201 nonfatal injuries during an aggregate worktime of 335,029,685 man- hours. These injuries, fatal and nonfatal combined, occurred at a frequency rate of 21.72 per million man-hours, comprising 0.23 for the fatal and 21.49 for the nonfatal injuries. The combined severity rate of the disabilities was 2,312 days lost or charged per million man-hours, consisting of 1,379 for the fatal and 933 of the nonfatal injuries, The average severity of all disabilities during 1961-63, was 106 days per injury, The number of days lost or charged, excluding officeworkers, at nonmetal mines and mills during 1961-63, was 462,000 days charged to fatal injuries and 312,461 days lost from nonfatal injuries. The outstanding causes for fatal injuries were explosions (18 fatalities occurred in a major mine-explosion disaster in a potash mine in Utah in 1963) and falls of rock or ore from back or side, while most nonfatal injuries were caused by handling materials, slips or falls of persons, haulage, and machinery. The parts of the body most frequently injured during the period 1961-63 were the trunk, hand and finger, and foot and toe, An average of 52,810 men were at work daily, There were 20 nonfatal disabling injuries reported for office- workers at nonmetal mines and mills during the period 1961-63 during an aggregate worktime of 23,088,496 man-hours, These injuries occur- red at a frequency rate of 0.87 per million man-hours, There were no fatal injuries reported.

Jan 1, 1967

By F. D. Everett

This report summarizes the results of a nationwide investigation completed in 1964 to determine the nonferrous base metal ore reserves and potential sources of ore and to evaluate criteria for their ultimate exploitation. Engineers of the Bureau of Mines contacted mining company officials, reviewed reports and Government records, and where necessary made personal appraisals in arriving at the results. The estimates are presented by metals in ores in geographic regions and include some of the problems affecting the reserves and potential sources. The recoverable metal in the measured ore category and in the total ore reserves was estimated as follows: [ ] At the 1963 rate of domestic mine production these total reserves would be adequate to provide copper for 62 years, lead for 121 years, and zinc for 42 years. Data also are given for gold, silver, and other coproducts. Reserve estimates greatly exceed those of previous investigations; some prior estimates of copper reserves are included for comparison (table 23). Projections of requirements for base metals indicated the United States will need approximately 45 percent more copper in 1970 and 110 percent more by 1980 than was consumed in 1960; similar projections for lead indicate increases of 20 percent by 1970 and 45 percent by 1980; zinc projections are 40 percent more by 1970 and 90 percent by 1980. Much of the production of gold and silver is a coproduct of base metals recovery and the projected need for the precious metals exceeds all the United States can produce. Some problems of the industry are mentioned. A graphic evaluation of the economic availability of the reserve and potential sources is shown.

Jan 1, 1967

Devitrification of a glassy volcanic ash equivalent to an alkaline trachyte in composition has resulted in the formation of an interstratified illite-montmorillonite with an 1:1\1 content of 1:4 as the principal clay mineral.A high concentration of potassium ions and a deficiency of magnesium ions favoured the formation of the potassium-bentonite.A poorly ordered mica mineral, equivalent to illite, was produced by weathering of potassic feldspar. Subsequent degradation of the illite through the loss of potassium was responsible for the formation of several interstratified minerals with very approximate 1:1\1 contents of 4: I as minor components.Other authigenic minerals present in small amounts were u-cristobalite, sepiolite, and the zeolite clinopitolite.The non-swelling character of the potassium-bentonite makes it economically unattractive...

Jan 1, 1967

By Howard N. Egan

EASTERN COAL CORPORATION is located in the heart of the Appalachian Mountain area of extreme Eastern Kentucky, The mountains are of sedimentary origin, and have been deeply eroded by streams as the area has been thrust up during geologic time. There are many seams of coal interspersed between beds of shale and sandstone. While some of the seams are thin, there are a number that can be economically mined. We are mining the Pond Creek, or No. 2 Gas Seam, at a rate in excess of 6,000 tons per day. Our central preparation plant utilizes tromp baths for the plus 3/8" size and Rheolaveur for the minus 3/8" portion. No provision was made to recover the fine coal, which was included with the plant effluent pumped to a 12 acre refuse pond. The pond is impounded behind the coarse refuse dump. This pond rose 15 feet last year. Obviously, no pond could stand many years at this rate. Limited pond space in this rugged area of steep hills and narrow valleys dictated a revised disposal method. Our first thought was that it would be necessary to dry the fine refuse sufficiently to permit inclusion with the coarse refuse, which is hauled uphill by monitor and then trucked to final disposal.

Jan 1, 1967

By B. S. Gottfried

This paper is concerned with possible transport mechanisms which occur during segregated burning (i.e., burning in an oil reservoir in which the oil-bearing formation is overlain by a "clean" porous zone containing only gas). ,Two analytical models are presented. In the first, burning is assumed to occur at the gas-oil interface, and the dominant mechanism is taken to be the rate at which oxygen diffuses to the interface. The second model assumes that combustion occurs within the clean zone, with the dominant mechanism being the mechanism of fuel deposition from the oil-bearing formation to the clean zone. ,Comparison of the results of the analyses with limited experimental data indicates that the latter mechanism is much more plausible. Both models are idealized representations of the actual process and are somewhat conjectural, however, owing to the lack of more definitive laboratory or field data. INTRODUCTION In recent years there has been considerable theoretical and experimental research directed toward understanding the recovery of crude oil by underground combustion. Although two different recovery schemes have been proposed, known as forward and reverse combustion, it is only forward combustion that shows promise of becoming a practical recovery technique.17 Most of the analyses of the forward combustion process have considered it to be pistonlike; i.e., oil is displaced by a vertical combustion zone which, with its ensuing gases, pushes die oil forward as the flame front is propagated through the reservoir.l-8,ll,l2,14-16 However, information gained in field pilot studies indicates that, at least to a certain extent, forward combustion proceeds in a segregated manner in oil reservoirs.10 An ideal segregated system is one in which the oil-bearing formation is overlain by a "clean" porous zone containing only gas. The location of the combustion zone in such a system is not immediately evident, although combustion is believed to occur either at the gas-oil interface or within the clean zone. In either case, the combustion zone may be horizontal and it moves in parallel rather than in series with the produced oil. The purpose of this paper is to explore the likely mechanisms by which segregated burning can occur, and to determine the sensitivity of the resulting models to changes in various physical parameters. Two governing mechanisms are considered: the case of a horizontal combustion zone at the gas-oil interface with the rate of combustion governed by the rate at which oxygen diffuses to the interface, and the case of combustion within the clean zone with the combustion process controlled by the transport of fuel from the oil-bearing formation to the clean zone. Both models are somewhat hypothetical and involve considerable simplification of the actual process. However, the results allow some preliminary understanding of segregated burning which is useful in the absence of more definitive laboratory or field pilot data.

Jan 1, 1967

By Ronald P. Hollenbeck

The value of mineral production in Alabama reached a new high of more than $246 million. 4 percent above the previous record established in 1964. New high values were reported for bentonite, portland cement, fire day, kaolin, miscellaneous clay, lime, crushed limestone, crushed marble, mica. salt, and sand and gravel. Among the States, Alabama ranked second in the production of bauxite and scrap mica and third in the production of native asphalt. The mineral industry of Alabama was dominated by the mining and processing of coal and Slone, the manufacturing of cement, and the production of crude petroleum, which together comprised 85 percent of the total value of mineral output, compared with 84 percent in 1964. The iron ore industry continued to decline. Coal production continued to increase, resulting in the State's coal-mining best year since 1948.

Jan 1, 1967

By L. Nahai

Overall mineral industry productive activity in Europe increased in 1965, following general upward trends in gross national product and total industrial production4 recorded. The gross national product of non-Communist Europe in market prices in 1965 was estimated at $572 billion and that of Communist Europe at $409 billion. However, the extractive sectors of the mineral industries generally did not fare as well as the processing sectors. In fact, a number of countries recorded lower production levels in this sector in 1965 than in 1964 and most countries had a lower growth rate in extractive industry output than in overall industrial output. Among the non-Communist nations of Europe, a general decline in coal production and lower levels of iron ore output in France, West Germany, and Luxembourg contributed significantly to the smaller growth rates or declines in extractive indexes. Where higher indexes were registered, this generally resulted from the performance of the petroleum and natural gas industry; exceptions were Greece, Norway, and Sweden. The decline recorded for Czechoslovakia was attributable entirely to poorer performance by that nation's coal industry.

Jan 1, 1967

THIS bulletin presents all analytical and lest methods regularly used by Bureau of Mines laboratories for characterizing coal and coke. To provide better service to coal producers and consumers, the scope of this bulletin has been expanded to include important test methods used to evaluate coal properties for commercial processing. The methods described will prove valuable to all persons interested in analyzing and testing coal and coke.

Jan 1, 1967

By Forrest T. Moyer

To keep the mineral and allied industries informed of trends in the causes of accidents and to point out the need for corrective measures, the Bureau of Mines collects, analyzes, and periodically published health and safety statistics. This report includes data for 1964 on injury experience, with related employment statistics, at coal mines in the United States. These data are presented in tabular form under the following headings: General Injury Experience Tables 1 to 6: Current data on number of injuries, degree of injury, frequency and severity rates, average severity, and related employment and production data by work location.

Jan 1, 1967

By J. M. West

Expanded war in Viet-Nam overshadowed activities in the Far East in 1965, diverting capital and materials from potential regional development projects. Japan with-stood a period of business recession that was particularly felt by its coal mining and iron and steel industries. Toward yearend signs of improvement began to show. Despite the recession with attendant credit restrictions and forced cutbacks in areas of overproduction, Japan's overall industrial output rose nearly 5 percent during the year. Foreign trade, liberalized in 1964, was a strong point in the Japanese economy and took the place of lagging domestic demand. Japan maintained its third place in world production of iron and steel ahead of West Germany and in 1965 was the world's fore-most exporter of iron and steel in primary and semimanufactured forms. Economic setbacks in mainland China caused by its "Great Leap" failures and subsequent withdrawal of Soviet technical assistance were difficulties relegated to the past. However, a newly formed "Red Guard" political group, part of a so-called cultural revolution, was due to cause new disruptions in 1966. Nevertheless, significant gains were claimed in Chinese industry, and the country approached self-sufficiency in petroleum in 1965 by virtue of its Tach'ing oilfield. Restoration of friendly relations was achieved between South Korea and Japan accompanied by Japanese offers of industrial aid and increased trade. Indonesia's economy was deteriorating; the country withdrew from regional development organizations and continued its stubborn confrontation policy against Malaysia throughout 1965. Late in the year after a Communist uprising had been quelled, there was a period of political retrenchme t and it was hoped that economic improvements would follow. Petroleum remained a strong area in Indonesia's varied resources, and its production was increasing. Tin output declined, however, because of operating difficulties.

Jan 1, 1967

By Clarence Karr

AN EXTENSIVE characterization was conducted on the neutral oil components in a low-temperature bituminous coal tar. A total of tai individual compounds identified with respect to individual isomers, and at least 55 other compounds were indicated to be present. The amounts were determined in all instances. A comparison of isomeric distribution in the tar with thermo-dynamic equilibrium distribution, and kinetic distributions indicated that the composition of the tar largely reflected the structure of the coal from which it was formed. Detailed descriptions are presented for the separatory and qualitative and quantitative procedures for the characterization of the neutral oil component. These include micro fractional vacuum distillation, displacement liquid chromatography, gas-liquid chromatography, countercurrent distribution, and infrared and ultraviolet spectrophotometry. Descriptions are given for the synthesis of authentic specimens of alkylindenes, The ultraviolet and infrared spectra of 134 polycyclic compounds, ranging from alkylindenes to alkylphenanthrenes, either found in the distillable neutral oil, or thought likely to be present, are also given.

Jan 1, 1967