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By A. T. English

X-ray dif action techniques were used to investigate ordering and domain coalescence for the B2 (CsC1) superlattice in this alloy. Essentially complete disorder is obtainable by drastic quenching. isothertmal ordering occurs very rapidly at temperatures between 565° and 680°C, only a few seconds being required for development of substantial long-range order. A very fine antiphase dormain structure, found in samples annealed for short times, undergoes coalescence with further annealing. Domain "size" is found proportional to (t)1/2 . This Yate law can be derived by adapting the formalism of Hillert's analysis 01- metallurgical grain growth. For this Purpose the material is descvibed in terms of a "Swiss-cheese " structure, consisting of two multiply connected, mutually intertwined domain volumes. The observed activation enevgy for coalescence, 70 kcal per g-atom, agrees with an estit~lated value ,for volume diffusion in disordered rrzaterial. It is suggesled that the experimental value vejlects the substantially disordered environment of mobile vacancies located in the moving antiphase domain boundary. The alloy Fe-Co-2V is bcc below about 900'C and orders into a B2 (CsC1) superlattice below about 730c It has important applications in magnetic components, including many requiring extensive cold rolling.* example, Marcinkowski and Brown6 observed a re1atively small as-quenched domain size of about 250Å in B2 Fe3A1. Since there appear to be no published data on domain coalescence in B2 alloys, this process was studied in detail. MATERIALS AND EXPERIMENTAL TECHNIQUES A commercial high-purity alloy, nominally 49 Fe-49Co-2V, was obtained from the Arnold Engineering Co. in the form of cold-rolled sheet 0.004 in. thick. Samples were annealed for 1 hr at 800°C in dry H2 to produce disorder and quenched into iced brine. They were then annealed in a nitrate-nitrite salt bath for various times at temperatures between 525° and 625°C. Estimates of the LRO parameter S and the APD size D were made using established X-ray diffraction techniques. Superlattice peaks are best observed using CoKa radiation, for which the value of (fFe-fCo) is maximized. Peak-to-background intensity ratio was improved by filtering CoKß from the incident beam to eliminate sample fluorescence, and by using a pulse-height analyzer. The LRO parameter S was computed from the ratio of integrated intensities I 100/I 200- Owing presumably to systematic errors associated with the presence of crystallographic texture and X-ray extinction, only rough agreement was obtained between experimental and theoretical (absolute) intensity ratios. For this reason certain experimental refinements (e.g., use of balanced filters) were considered superfluous and were omitted. Emphasis was placed on maximizing intensity in order to reduce the time taken to accurately determine the contour of the very small (loo), peak. This was done by point counting 105 counts at appropriate intervals. Background intensity averaged about 1200 cps.

Jan 1, 1967

By Stanley A. Feitler

This Bureau of Mines report deals principally with the resources and economic aspects of feldspar in the United States east of the Mississippi River. Although in a strict sense, all phases of the feldspar industry affect its economic structure, emphasis in this study is on supply, demand, and marketing. Although feldspar was originally mined for use in the manufacture of pottery and other ceramics, the glass industry, which began to use feldspar in the mid-1920's, now consumes more than half of the annual output. Most mining is open cut, and the methods used are similar to those used in mining crushed b stone. Excess plant capacity has been chronic, and production is usually about 30 percent of capacity fur the industry as a whole. Since 1947, feldspar consumption has grown more slowly than the average for all U.S. industry. This has fostered intense competition, especially for the glass market. Prices have not kept pace with inflation, and profits are small. The trend of consumption through 1970 for glass feldspar is expected to be upward; less rapid in consumption of ceramic feldspar is anticipated.

Jan 1, 1967

By L. F. Heising

Ten composite samples of Mesabi Range nonmagnetic taconite from the Hibbing, Minn., area were evaluated by flotation and by reduction roasting-magnetic separation to determine their potential as a future source of iron are. Only one of the composites yielded concentrates that could be considered marketable, using as a criterion a 10-to-1 iron-to-silica ratio. Cursory petrographic examinations of all 10 composited samples and a detailed mineralogical study on 1 sample suggest that unfavorable mineralogical associations between iron and gangue minerals are responsible for their poor beneficiation characteristics.

Jan 1, 1967

By Frank J. Klima

Explosives are probably the most widely used and most mysterious large scale' mining tools of modern times. The post black powder explosives were primarily nitroglycerin-based straight dynamites, ammonia dynamites, blasting gelatin, gelatin dynamites, ammonia gelatin dynamites, etc. Of these, the strongest and highest velocity explosive used in industrial operations is blasting gelatin, which is nitroglycerin colloided with a nitrocellulose of medium nitrogen content in proportions which give the product a plastic character, or about 93 to 7. Many variations of the basic groups above were developed by substituting ammonium nitrate and/or sodium nitrate for some of the nitroglycerin. The nitrates being insensitive to caps required a certain percentage of nitroglycerin to sustain detonation in smaller quantities or diameters. Paralleling the development of industrial dynamites was the development of more expensive, highly sophisticated explosives which were developed for specific military purposes. Such explosives as Amatol, RDX, Composition A, Composition B, Composition C, Lead Azide, PETN (Pentaerythritol Tetranitrate), Tetryl, Pentolite, TNT, etc., were primarily military explosives. Amatol, which is a cast mixture of ammonium nitrate and TNT (Trinitrotoluene), and identified by percentage of AN versus TNT as 50-50 Amatol, 80-20 Amatol, etc., was a favorite World War I explosive. RDX, or Cyclonite, was widely used in World War II. Also used during WW II were compositions A. B, and C, which were mixtures of RDX (Cyclotrimethylene trinitramine), TNT, and other nitrotoluenes. These high explosives, along with nitroglycerine, are exact chemical compositions or mixtures of exact chemical compositions which are individually explosive, or in other words, individually capable of explosive chemical decomposition when properly initiated. These chemical decompositions result in the formation of simpler compounds and/or large quantities of common combustion gases, and large amounts of energy in the form of heat. Of these, the most powerful is RDX which, based on the ballistic mortor test, is 1.5 times as powerful as TNT. Chemically, the decomposition of TNT releases about as much energy as the reaction of ammonium nitrate and fuel oil.

Jan 1, 1967

By R. C. Hickman

Preliminary evidence indicated that the Chattanooga Shale might constitute a potential vast low-grade source of uranium. Investigation by core drilling indicated that while the Chattanooga Shale may constitute a resource for the future, the very low (0.006 percent) average uranium content is not economic when compared with the relatively higher grade western ores. A total of approximately 12,000 feet of test drilling was done in 72 drillholes, and large samples were mined for extractive and metallurgical testing. An experimental mine site was selected on the basis of the drilling project.

Jan 1, 1967

By Robert W. Ageton

The Bureau of Mines investigated the in situ vertical component of the rock stress in the rib of the haulage drift on the 6100-level of the Star mine, Burke, Idaho, using the flatjack and borehole deformation methods. The estimate of the vertical component of stress about 2 feet into the rib at a station along the haulage drift on the 6100-level of the Star mine by the flatjack method is approximately 5,875 psi, whereas the borehole deformation procedure at this station yielded a value of 5,500 psi for the same depth into the rib. The test zone is approximately 5,625 feet below the surface.No attempt was made to extrapolate stress estimates beyond the depth of the flatjack installation.

Jan 1, 1967

By Wilson Blake

The Bureau of Mines used a mathematical model based on the finite element method of stress analysis to calculate stresses and displacements surrounding an open pit mine in a gravity-loaded rock mass. Comparison of the finite element solution for a semicircular notch in a gravity-loaded plate with the theoretical solution for a semicircular notch in a plate under uniform compression parallel to the free boundary demonstrates the inapplicability of the latter method to openings at the free surface of a gravity-loaded medium. High stress concentrations are formed at irregularities along the boundary of an open pit in a gravity-loaded continuous competent rock; however, for this type of rock the magnitudes of the stresses are too low to be considered a major factor in open pit slope stability. High stress magnitudes will occur if, in addition to the gravity stress field, a large horizontal stress field exists.

Jan 1, 1967

By Richard W. Knostman

A study was made of the factors affecting lead and zinc production in the Pacific Northwest. Costs, ore reserves and potential resources, and domestic demand were analyzed. It was concluded that a projected 3.1-percent average annual increase in U.S. demand for zinc through 1975 and a corresponding 2.5-percent rise for lead will be supplied mainly from mines in the Eastern and Central States. Annual Pacific Northwest mine production of lead is estimated to fluctuate around 82,000 tons, while zinc output may average 135,000 tons through 1975. Measured, indicated, and inferred reserves in the Pacific Northwest, containing 1.56 million tons of lead and 2.59 million tons of zinc, are more than sufficient to maintain this level of production. Annual production from Pacific Northwest electrolytic zinc plants is expected to increase to over 300,000 tons of slab zinc by 1975. Lead smelters may experience difficulty in maintaining output at 1964 levels.

Jan 1, 1967

By Gordon W. Hines

This paper, dealing with network planning in an industrial complex, discusses the type and size of project that can be handled on a manual basis. After a review of the fundamentals of network planning, and specifically of the Critical Path Method, the author analyses several different types of projects, each with its own characteristics. Some can be handled in conjunction with a computer, but others can be dealt with equally well without one. Among the projects discussed are a blast furnace reline, the installation of a billet mill flying shear, and routine maintenance-type operations.

Jan 1, 1967

By G. J. Biefer

"Fatigue and corrosion fatigue measurements were carried out on five commercially available metals -four steels and an aluminum alloy -which are used as structural materials in mine shaft conveyances. In the corrosion fatigue measurements, drain waters collected in the shafts of three different Canadian mines were used as corrodents. The mine waters had been selected on the basis of their relatively large differences in acidity and/ or composition.It was found that the corrosion fatigue strengths of the four steels were similar, despite their differences in tensile properties, and that the type of water used in the tests had little effect on the results. Mild steel showed the highest and most consistent values of the damage ratio (ratio between the corrosion fatigue and the plain fatigue strengths at 107 cycles). The corrosion fatigue behaviour of the aluminum alloy (ASTM Type 6061-T6) was found to differ markedly in the three mine waters. A high damage ratio (i.e., superior performance) was shown in a mine water in which the corrosion attack was uniform; much lower damage ratios were shown in waters which produced localized corrosion attack. Corrosion rates were too low to be deter-mined conveniently by conventional weight-loss methods, but calculations from polarization curves provided a rapid demonstration that corrosion rates were distinctly lower in the mine water which produced high damage ratios."

Jan 1, 1967

By Robert E. Barieau

This report describes a method for treating pressure-volume-temperature (PVT) data obtained with a Burnett compressibility apparatus. The method makes use of a general nonlinear least-squares technique developed at the Bureau of Mines Helium Research Center. It is assumed that an adequate functional form is available for the expression of the compressibility factor as a function of either the molal density or the pressure. The functional form of the compressibility factor can be either linear or nonlinear in the parameters to be evaluated. Formulas are given for calculating variances and covariances of all parameters evaluated and for calculating the variance of calculated quantities of interest.

Jan 1, 1967

By N. Mungan, F. W. Smith, J. L. Thompson

Adsorption of polymers and transport, rheology and oil recovery efficiency of their solutions were studied in the laboratory to evaluate the use of polymers in waterflood-ing. While a tenfold mobility reduction was obtained with polymer concentrations as low as 0.05 per cent by weight, the mobility reduction depended on the type of polymer, molecular weight, salinity and pH of water, crude oil and capillary properties of the porous media. Choice of a suitable polymer and a workable concentration will have to be tailored for each application. Little reduction in the residual oil saturation can be expected from polymer flooding. Improvement in the volumetric sweep efficiency is possible hut the extent of the improvement can best be evaluated by properly designed field testing. Some aspects of the field use of polymer floods are discussed. INTRODUCTION Waterflooding is a simple, inexpensive secondary recovery method and is being used widely. Innumerable laboratory studies have been made to unravel the fundamentals of the displacement of oil by water and to find the ways of most efficient oil recovery. These studies and a great many field case histories have revealed that the prime cause of poor oil recovery is the inefficient and incomplete sweep of reservoir volume by the injected water. Sweep efficiency is affected by many factors of which the mobility ratio is an important one. Mobility ratio M is defined here as the ratio of water to oil mobilities: M = (k»/y,r)/(k,JJJJ........(1) In Eq. I, the permeabilities are the effective permeabilities and depend on fluid saturations and, hence, change during the different depletion stages in a flood. A wide practice is to use the effective water permeability at residual oil saturation and the effective oil permeability at interstitial water saturation in Eq. 1. If the mobility ratio is greater than one, the mobility ratio is unfavorable and water, being more mobile than oil, would finger through the oil zone resulting in poor oil recovery efficiency. If the mobility ratio is favorable (one or less) the displacement of oil by water occurs more or less in a pistonlike fashion. In some waterfloods. the mobility ratio is unfavorable and any additives by which the mobility of water can be decreased would favor more efficient oil recovery. The thing to bear in mind, however, is whether or not the improvement in oil recovery is sufficient to more than pay out the cost of the additives needed. For example, materials like sugars, alcohols and glycerine reduce water mobility by thickening the water, but the cost of material requirement precludes any field application. For an additive to be useful in water-flooding, it must bring about a large reduction in water mobility at low concentrations; it must be adsorbed only negligibly; and it must not completely plug up the formation. Some synthetic organic polymers have shown promise of meeting these requirements and have been used in the field.'-W owever, no in-depth studies of the rheological, adsorption and oil displacement characteristics of polymer solutions have been reported. The present work is a study of these properties. EXPERIMENTAL In this work, concentrations are given on a weight per volume basis; 0.5 per cent concentration means 0.5 gm of polymer is dissolved in enough water (or NaCl solution) to make 100 ml. A bactericide, usually 0.1 to 0.2 per cent by volume of 38 per cent formaldehyde solution, was used in the polymer solutions. The NaCl solution was 30,000 ppm. Some properties of the polymers studied are given in Table I. Physical properties of all cores used are in Table 2. Flow behavior of polymer solutions was studied by three consecutive flow tests in cores. First, water (or brine) was injected at constant rate of about 1 ft/D to obtain the water mobility. Then, filtered polymer solution (prepared in water or brine) was flowed through the core. Since the rate was constant, increase in the pressure drop across the core reflects decrease in the mobility. Finally, the core was flooded with water (or brine) to study recovery of mobility. The Alundum cores which were used in

Jan 1, 1967

By the use of flotation tests it was confirmed that there are two functions of oxygen in sulphide mineral flotation. Sized samples of galena and chalcopyrite were sulphidized, washed free of excess sulphide ion, and then contacted with air-saturated water for certain lengths of time. The mineral was then transferred to a sealed laboratory flotation cell containing water with a known concentration of dissolved oxygen. Xanthate and frother were added and flotation continued for 1 min.Both the extent of mineral oxidation and the concentration of dissolved oxygen markedly affected the flotation of galena and chalcopyrite. The response to a change in either variable is dependent on the level of the other, but generally best flotation occurs with the maximum degree of air saturation of the pulp. Galena flotation is hindered by oxidation of the mineral beyond a small threshold amount but a similar effect for chalcopyrite was not observed...

Jan 1, 1967

By Jr. Hill

Laboratory metallurgical treatments of three high-iron bauxite ores from Arkansas were conducted to determine the relative effectiveness of experimental methods for recovering alumina and a commercially acceptable iron concentrate. The standard for evaluating recoveries from experimental processes was the Al2O3 recovery from Bayer digests of the crude ores; recoveries from digestion of the three ores were 74.1, 87.4, and 88.7 percent. Flotation, magnetic separation, or various combinations of digestion, calcination, and reduction-sintering, leaching, and magnetic separation of leach residues failed to produce Al2O3 recoveries as high as the standard. A high-iron-bearing fraction, containing between 68 and 78 percent of the total iron, was produced in a three-phase treatment involving a caustic, lime reduction-sinter of the crude ore, water extraction of Al2O3 from the sinter, and magnetic separation of the leach residue.

Jan 1, 1967

By Heinz W. Sternberg

A method for the electrochemical reduction of the benzene ring was developed and applied to the electrochemical reduction of coal. Successive electrochemical reductions of a vitrain from low-volatile bituminous coal in ethylenediamine saturated with lithium chloride resulted in the addition of 53 hydrogens per 100 carbon atoms. Ultimate analyses and pyridine solubility of the vitrain recovered after each reduction showed that hydrogen added at the beginning has a much greater effect on solubility than hydrogen added at a later stage. Surprisingly, the removal of sulfur from the vitrain takes place only after the more reactive aromatic rings are reduced. Nuclear magnetic resonance analysis and average molecular weight determination of the extracts of the reduced vitrain samples, representing about 18 percent of the vitrain, showed that these fractions had 95 percent of their hydrogen content on saturated carbon atoms and an average molecular weight of 800 to 900. A study of the effect of operating variables on current efficiency showed that current efficiency is highest with aluminum as cathode material and with lithium chloride as electrolyte. A substantial increase in current efficiency of difficulty reducible olefinic double bonds was achieved by adding a proton donor. This result is significant in connection with the electrochemical reduction of coal which proceeds from readily reducible aromatic double bonds to difficultly reducible isolated double bonds. It is proposed that reduction is achieved by electrolytically generated and subsequently solvated electrons and hence does not require prior adsorption of the substrate at the electrode surface. This offers a distinct advantage for electrolytic reduction of sparingly or insoluble substrates such as coal.

Jan 1, 1967

By D. A. Elkins

This report is the second of a series of three that will evaluate, in order, the metallothermic, carbothermic, and electrolytic methods of magnesium production. The historical development of the carbothermic process is outlined. Production costs varying from 38.9 to 21.8 cents per pound of magnesium are estimated for different versions of the process. Additional suggested process modifications are listed. The technical and economic potential of the different versions are compared. Areas deemed most promising for future research on the process are delineated.

Jan 1, 1967

By H. G. Iverson

Solid state reactions of manganese with silica were investigated in high-temperature tests. Reactions of 0.5 to 4.0 moles manganese (Mn) with 1 mole silica (SiO2) at 1,100° C and of 2.0 Mn:SiO2 mole-ratio mixtures at 1,000° to 1,150° C yielded products consisting of a slag phase and a metallic phase. At 1,100° C, the slag phase from reactions of the low Mn:SiO2 mole-ratio mixtures was composed of SiO2 and rhodonite (MnSiO3), and the slag phase from the high Mn:SiO2 mixtures was composed of MnSiOs and tephroite (Mn2SiO4). The metallic phase from the corresponding low Mn:SiO2 mole-ratio reactants consisted of two manganese silicides, Mn5Si3 and Mn3Si; from the high Mn:SiOg mixtures, it was Mn and the manganese silicide (Mn5Si). For the higher mole ratios of MnSiO2 the manganese content in the metallic phase increased, while the manganese and silica contents of the slag phase remained nearly constant. The slags did not contain free or uncombined manganese oxide (MuO). For the 2.5 to 4.0 Mn:SiO2 mole-ratio mixtures reacted at 1,100° C, the maximum quantities of silica reduced and of the manganese in the slag appeared to become asymptotical at about 41 and 48 percent, respectively. A brominating procedure was developed that was highly selective in removing the metallic constituents from the reaction product, leaving the slag phase as residue. X-ray diffraction patterns were obtained on prepared silicides Mn5Si, Mn3Si, and MnSi.

Jan 1, 1967

By L. C. George

The Bureau of Mines measured vapor pressures of selected mixtures in the binary system SnCla-ZnC12 by the static pressure method. Equations expressing the vapor pressure) and the heat and free energy of vaporization) as functions of temperature were developed by numerical analysis based on the sigma-plot method. It was found that the vapor pressure of any SnCl2-ZnCl2 mixture) at any temperature within the range of this investigation) could be accurately calculated from the derived values for the heat and free energy of vaporization for the mixture, with a probable error of 0.01 cm Hg or less.

Jan 1, 1967

By M. W. Dumais, E. P. Abrahamson

In a paper by Abrahamson and Alexander concerning a series of correlations between electronic structure and property changes, it was hypothesized that each solute atom in a dilute solution had a characteristic volume of solvent atoms over which some form of electronic interaction occurred. From this description it is possible to picture the solute atoms as occurring in an ordered array for the most efficient arrangement. A recent review article2 has shown that some form of anomaly exists for a whole series of properties when dilute additions of tungsten are made to iron, of. Fig. 1. Any mechanism to fit one property must also be amenable to mechanisms for the other properties. The possibility of some structural change in this region appears to offer the best hope. The system chosen for investigation was the iron tungsten system. Zone-refined iron with zone-leveled tungsten additions were supplied by Materials Research Corp. as 3/8-in.-diam bars. Transmission electron microscopy was used to study the structure. One-quarter inch specimens of each alloy were cold-rolled to 10-mil sheets, cleaned, punched to electron-microscope specimen-holder size, and annealed in vacuum for 2 hr at 800°C and 2 hr at 700°C followed by a furnace cool. The specimens were attached to a platinum wire and the specimen edge and wire were painted prior to thinning in a solution of 10 pct perchloric acid in glacial acetic acid. It was believed that if ordering were present due to electronic interactions the polishing procedure chosen would provide a simultaneous combination of chemical attack and electropolishing to exhibit the ordered structure. The chemical attack would be expected to penetrate those areas equidistant from the tungsten atoms, while the electropolishing would serve to "plane off" the volumes where the chemical attack had taken place. If one of the ordered tungsten planes were parallel to the specimen face at the edge of the thinned hole, a plate or micalike structure would be expected. A typical result of this polishing is shown in Fig. 2. Here a series of plates can be seen lying one upon the other. In several other specimens the plates parallel to the electron beam have been observed, behaving like slices of bread in a loaf. These edge views coupled with moire patterns indicate that the minimum plate thickness is 37 to 42A. This is equivalent to a concentration of 455 at. ppm of W if a simple cubic superlat-tice exists, or one tungsten atom every twelve iron atoms on the ordered plane. It was further noted that the base iron exhibited no signs of platelike structure. As the concentrations increased above 100 at. ppm W the amount of plate material increased. Among the specimens investigated was that shown

Jan 1, 1967

By E. P. Williams

"Prince Edward Island, Canada's smallest Maritime Province, is located in the southwestern part of the Gulf of St. Lawrence. The Province is more or less centrally located in the Maritimes Basin, a large intermontane basin within the Appalachian orogenic belt. The Maritimes Basin is subdivided into sub-basins and uplifts which exhibit two dominant structural trends: east and northeast. The Basin is known to be petroliferous because of the seeps, shows, oil shales and albertite found in southern New Brunswick and northern Nova Scotia and the gas and oil produced from the Stony Creek field near Moncton, New Brunswick.Permian beds are exposed on the Island, mostly along sea-cliffs. A maximum thickness of about 5,000 feet of red beds -shales, sandstones and conglomerates -make up the sequence. Over most of the Island, the Permian section is much thinner. Four key wells (Mississippian tests) and several shallower tests have been drilled. The Pennsylvanian-Mississippian section thickens rapidly off the Port Hill Uplift at the northwest, where it is less than 4,600 feet thick, and continues to thicken to about 20,000 feet in the Cumberland Basin at the southeast. Geological and geophysical data combine to give us the structural picture of the deeper beds.Prospective reservoir rocks are primarily in the Missis-sippian Horton and Windsor groups. Prospects are:-1. on or over structural highs in the basement; 2. on anticlines or fault highs; 3. over or peripheral to salt domes or salt-core anticlines; 4. at truncation pinchouts of Mississippian prospective beds; 5. in basal sandstone or granite wash on the pre-Carboni-ferous basement; and 6. in facies traps at changes from sandstone to shale or porous to tight carbonate rocks."

Jan 1, 1967