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By Thomas R. Bur

The strain and pressure gage methods for evaluating the relative performance of explosives in rock were compared. This comparison was based on a study of the responses of strain and pressure gages to explosion-generated seismic waves. Several explosives) representing a wide range of detonation pressures) were used. In general the relative performance of these explosives) as determined from amplitude) impulse parameter) and energy parameter measurements) is the same if the compressive portion of the strain pulse and the comparable portion of the pressure pulse are considered. Other similarities and differences of the two methods are also discussed.

Jan 1, 1967

By F. R. McDonald

This report presents a discussion of the spectra of 39 condensed thiophenes in which the structure includes at least 1 benzene ring. The vibrational bands present in three regions of the infrared spectra of these thiophenes were interpreted by comparing the similarities of the spectra of condensed thiophenes with the spectra of substituted benzenes. In the overtone-combination region 23 of the 39 condensed thiophenes had spectra which contained sufficient detail to be usable for correlating this region of the spectrum with the appropriate benzene spectrum. In the in-plane deformation region it was possible to make correlations for the vibrations of 18 of the 39 condensed thiophenes whose infrared spectra were studied. In the out-of-plane deformation region the C-H out-of-plane vibrations for hydrogen on benzene rings in the condensed thiophenes can be correlated using known data from substituted benzenes.

Jan 1, 1967

By L. B. Pankratz

The Bureau of Mines measured heat capacities of alpha and beta spodumene (LiAlSi2O5) and of beta eucryptite (LiAlSiO4) over the temperature range 51° to 298° K. The entropies at 298° K were found to be 30.9 ± 0.2 cal/deg mole for alpha spodumene, 36.9 ± 0.3 cal/deg mole for beta spodumene, and 24.8±0.2 cal/deg mole for beta eucryptite. High-temperature heat content measurements above 298° K were conducted for the same compounds. Measurements were made to 1,150° K for alpha spodumene, 1,600° K for beta spodumene, and 1,470° K for beta eucryptite. Tables of heats and free energies of formation are given from the elements and from the constituent oxides.

Jan 1, 1967

As part of its regular program to provide timely information on domestic mineral commodities, the Bureau of Mines conducted an engineering appraisal of more than 1,300 lode and placer gold deposits in the United States to deter-mine their gold production potential. While these deposits were estimated to contain over 400 million ounces of gold, only 9 million ounces, or slightly more than 2 percent, was found to be producible at $35 per ounce under prevailing mining and metallurgical technologies. The study revealed that any significant increase in available gold in the United States is most likely to come from the discovery of new sources, intensive exploration and development of the more promising known mineralized areas, and development of new or improved mining and metallurgical techniques.

Jan 1, 1967

By Karl-Heinz Frohne

This report presents the findings of a study of a portion of the Clover-Rush Run oilfield located in Roane County, W. Va. The study was made to investigate the possibilities of secondary oil recovery in the Big Injun sandstone underlying the William Kaufman lease. Reservoir properties, original reserves, and primary oil recovery are also presented. The investigation is based on a core analysis and related laboratory tests, well records, field production data, and subsurface information from the Kaufman property. A theoretical primary oil recovery of 9.7 percent of original oil in place is predicted for the reservoir. A waterflood performance prediction of a hypothetical pilot area was made by use of a computer. The prediction showed that, based on laboratory oil water relative permeability curves, the water-injection time needed to initiate oil production is excessive and that the stabilized water-injection and corresponding oil-production rates are very low. This precludes waterflooding the reservoir on an economic basis. A prediction for secondary oil recovery by gas injection was attempted but could not be completed because essential reservoir data were not available. In July 1965, the lease operator initiated, and is currently conducting, a gas-injection program, but there had been no increase in oil production up to November 1966.

Jan 1, 1967

By Harry L. Brown, James M. Dickinson, Philip E. Armstrong

The elastic stiffness coefficients of niobium have been rneaslrred from -150°C to over 650 C and ave in accord with the anomalous temperature dependence previously observed for Young's modulus. This unusual behavior has been shown to be the result of changes in the relative values of the shear elastic coefficients. The bulk modulus remained essentially constant over the temperature range studied, while changes in the shear coefficients produced a more nearly isotropic behavior as the temperature increased. A number of investigators have reported data on the temperature dependence of Young's modulus of polycrystalline niobium. The values cited for the room-temperature modulus ranged from 0.71 to 1.17 x 10" dynes-cm-' (10.3 to 17.0 x lo6 psi) and in each case the modulus was observed to decrease with increasing temperature. In our recent study,8 both polycrystalline and single-crystal samples of essentially strain-free high-purity niobium showed a Young's modulus whose temperature dependence as well as magnitude was strongly dependent on specimen orientation. This was shown to be the result of changes in the relative magnitude of the two shear moduli, C and C'. Young's modulus of polycrystalline samples with strong [110] textures and Young's modulus of single crystals whose orientations were away from the [loo] actually increased as much as 12 pct between room temperature and 1000°C. While studies on the residual effects of previous fabrication, thermal treatments, and impurity contents will probably resolve the problem of the widely differing Young's modulus values observed in polycrystalline niobium, a more complete description of the elastic properties requires an evaluation of the single-crystal elastic constants. A knowledge of these constants can provide a clearer picture of the nature of the temperature dependence, as well as establish a basis for predicting the modulus behavior of polycrystalline niobium, both in the randomly oriented condition and with various fabrication textures. The effects of residual strains on the elastic behavior then can be separated from orientation effects. EXPERIMENTAL METHOD Thin rod-resonance techniques were used to obtain both the Young's modulus and shear modulus of single-crystal specimens. The determination of these moduli as functions of the crystallographic orientation of the specimen axis provided sufficient information to permit calculation of the single-crystal elastic constants. The necessity for torsional as well as longitudinal measurements led to the design and assembly of a vertical-tube vacuum furnace incorporating probes for the simultaneous determination of both longitudinal

Jan 1, 1967

By R. A. Friedel

THE IMPORTANCE of infrared and ultraviolet-visible spectrometry in studies of the structure of coal and similar substances is described. Special experimental techniques have been developed for these studies. Thin sections of coal are preferred, but halide pellets are easier to prepare. Information obtained from infrared spectra on chemical functional groups has been discussed; the importance of both intensities and wavelengths of absorption bands has been emphasized. Functional groups assigned include aliphatic and aromatic CH, methylene and methyl groups, hydrogen-bonded hydroxyls, hydrogen-bonded and chelated carbonyls, phenolic structures, minerals, and aromatic structures that are benzenoid or polynuclear. Infrared studies of structures of coal extracts, distillates, and reaction products of various processes, both chemical and physical, are discussed. Coallike infrared spectra of chars of model compounds have been utilized extensively in studies of coal structure. Ultraviolet-visible absorption spectra of coals show a lack of fine structure and low spectral intensities. These results have been applied to the questions of the chemical and physical structure of coal, particularly the question of polynuclear aromaticity of coals. The color of coal is also treated. The physical-chemical origin of the color of coal may be due to free radicals, as interesting correlations of ultraviolet-visible spectra with electron paramagnetic resonance have been obtained. The optical color of coal has been explained and simulation of the color changes observed in thin sections has been carried out, The spectra and structure of coal derivatives and other carbonaceous materials are also discussed. Possible sources of error in absorption spectral measurements are pointed out. Limited measurements of the ultraviolet-visible reflectance spectra of coal are described.

Jan 1, 1967

By David E. Nicholson

In a Bureau of Mines investigation of the dynamic compaction of mine hydraulic backfills, two basic forms of mechanical vibration inducers were used and compared for effectiveness of compaction. Internal compaction, using concrete probe vibrators of various sizes, and external compaction, using plate vibrators} were studied and evaluated for use in underground stopes. An aluminum plate, which was light and displaced sufficient volume to remain afloat in fluid fill, and a steel plate were both used in the external compaction tests. Efficiency of compaction was better in studies conducted with internal probe vibrators. Tests were conducted in an underground backfilled stope with three different-sized probe vibrators (2-, 4-, and 6-inch-diameter) to determine an approximate area of influence. Results showed the areas of influence to be approximately 3, 4, and 5 feet in diameter, respectively, for the three different probes. Physical properties of hydraulic slurries were determined; preferred grain-size distributions, water exudation properties, and water contents of hydraulic slurries are reported. The best compaction results were obtained with moderately well-graded, fully saturated backfills, with slow rates of water exudation, which were capable of remaining in a semifluid state during the compaction process.

Jan 1, 1967

By F. A. Skirvin

Purification techniques were investigated for removing low-level metallic impurities from tungsten hexachloride. These techniques included distillation) fused-salt scrubbing) zone refining) and adsorption. Fractional distillation of tungsten hexachloride was found to be an effective purification method. The impurity levels of molybdenum) iron) nickel) copper) magnesium) and manganese were reduced to provide a tungsten halide sample which contained a total of less than 10 ppm detectable metallic impurities. Purification by fused-salt scrubbing of tungsten hexachloride in a lithium chloride-potassium chloride eutectic produced a hexachloride product which was of approximately the same quality as that obtained by distillation. Zone refining and adsorption did not appear to be as effective as distillation or fused-salt scrubbing.

Jan 1, 1967

By V. Taylor

"THE petroleum industry in Canada has been experiencing considerable difficulty in filling its manpower requirements during the last few years, and because of the rapidly expanding nature of the industry it is concerned about the supply that will be available to fill the needs of the future. As the oil industry is one of the more technically oriented industries, the most acute problem exists primarily in the field of profession-al/technical personnel. This is particularly true in the production and exploration side of the business, because it employs the highest percentage of this type of personnel. Let me illustrate this by giving you some figures reported by the Alberta Bureau of Statistics as of December, 1965 -out of a total of 9,641 male employees engaged in oil producing and geological and geophysical operations in Alberta, 3,021, or 31 per cent, were classified as engineers, geologists, geophysicists, managers and other professional personnel. No figures are available for 1946 to make a direct comparison of the expansion of the industry over the past twenty 466 years, but it is doubtful whether more than 100 professional/technical people were engaged in producing in Alberta at that time"

Jan 1, 1967

By Erle C. Donaldson

The pendant drop interfacial tensiometer is being used to study interfacial phenomena that influence the production of crude oil. A description of the instrument showing the modification of the cell and cell holder is presented. The modified cell and cell holder allow formation of a precise and reproducible drop size, and the image of the drop is easily alined and focused. Interfacial tension measurements and observations of film formation can be conducted at various temperatures with the jacketed cell.

Jan 1, 1967

By Murray Weintraub

In an investigation of the incineration of combustible wastes, the Bureau of Mines studied the effect of dimensional parameters, process variables, and fuel properties on the operation of an incinerator that consisted of a single cylindrical combustion chamber in which all combustion air was supplied tangentially above the fuel. Construction and operation of three designs of such a device proved that the tangential overfire air design is effective in providing efficient combustion and low concentration of particulate matter in the effluent gas. A correlation was found that related burning rate with air rate, chamber diameter, and inlet port diameter. In one of the incinerator models, ignition was by radiation from a preheated surface. The temperature of this surface was required to be 1,400° to 1,600° F to insure ignition of moist refuse; however, this had little effect on combustion rates. In the combustion of moist refuse, evaporation of the water proceeded through the fuel bed as a wave, with an ignition wave following the evaporation.

Jan 1, 1967

By Henry M. Harris

A study was made by the Bureau of Mines to determine if shapes of oxide-glass compositions could be roll-formed at high temperatures, and to find the conditions required for adequate formability. A unit with directly connect' furnaces and heated rolls that allowed forming of most of the compositions developed. Glasses of the feldspar type were chemically unreactive with the alumina grains, and allowed the best roll forming. Optimum forming was attained at temperatures of 1,400° to 1,530° C, with compositions containing 30 or 40 percent feldspar and 60 or 70 percent alumina. Formability was better when compositions contained minus 325-mesh materials, rather than coarser or finer powders. In many cases, roll-formed shapes had physical properties equal to or better than the normally sintered shapes of the same composition.

Jan 1, 1967

By Frank A. Peters

An evaluation is made of a lime-soda sinter process for extracting alumina from clay. In this process, alumina is extracted by sintering clay with soda ash and limestone and then leaching the sinter with a dilute sodium carbonate solution. The sodium aluminate solution formed during leaching is separated from the residue and treated with lime in autoclaves to remove dissolved silica before alumina trihydrate is precipitated with carbon dioxide. The tri-hydrate is then calcined to a-alumina. Two options, dry grinding and wet grinding, are used in the sintering step. The fixed capital costs for plants producing 1,000 tons of alumina per day are $72 million for the dry grinding option and $66 million for the wet grinding option on a Marshall and Stevens chemical equipment index basis of 240.0. Specific geographic locations of plant and raw material sources are not assigned, but, since this process requires large quantities of both lime-stone and clay, the plant site is considered as variable with relation to the clay mine and limestone quarry. A nomograph is given to find operating costs at various delivered costs of clay and limestone. If the plant is located nearer the limestone quarry so that the delivered cost of clay is $2 per ton and the delivered cost of limestone is $1 per ton, the operating costs are $76.47 and $71.61 per ton of alumina for the dry grinding and wet grinding options, respectively. On the other hand, if the plant is located nearer the clay mine so that the delivered cost of clay is $1 per ton and the delivered cost of limestone is $2 per ton, the operating costs are $80.15 for dry grinding and $75.34 for wet grinding.

Jan 1, 1967

By J. B. F. Champlin

The continuing development of the nuclear industry in the United States requires a program of waste disposal that insures against the release of large amounts of radioactivity to the environment. This paper describes research on one proposed means of disposal of this waste, that of injection into geologic formations at depth. Nuclear production plant wastes were simulated and injected into samples of sedimentary rock obtained from outcrops, quarries, and deep wells. Changes in the chemical and physical characteristics of the rocks caused by the interaction of ions and suspended particles in the waste solutions with the cementing material and claylike particles in the rock are discussed. Laboratory tests show that nuclear wastes can be injected into many natural porous, permeable geologic formations. Injectivity can be maintained over a longer period by monitoring the ionic balance and particle-size distribution of waste streams. The combination of permeability and porosity with low cation-retention capacity, as exhibited by most sandstones, would satisfy the engineering requirements for the subsurface disposal of nuclear waste. Shales and clays with their low permeability and high cation-retention capacity would make excellent confining formations. The amount of cation retained by sedimentary rocks increases with increasing valence or concentration of the cation or decreasing brine concentration. The use of rock cores as model reservoirs had proved successful in determining some of the parameters that need to be considered in full-scale field disposal of wastes.

Jan 1, 1967

By C. M. Sellars, F. Maak

Electvomotie -force measurements hazle been made on ten Au-Ni alloys at temperatures 7754 825O, 900O, and 935°C using galvanic cells with solid electrolyte. Partial and ivtegral thermodynamic functions are derived from the determined activities. which show la9,ge positive deviations jvom Raoult's law. The enthalpies of mixing- are in close accord with calorinletric data and are of comparable accuracy. The results are used to determine the miscibility gap and the spinoidal curL1e, and are qlalitaticely interpreted in terms of the large size difference and electvonic interactions between gold and nickel. Tabulated nalues of the actielities and partial and inteqal free energies, entropies , and enthalpies of mixing are given in the appendix. The Au-Ni binary alloys are of particular interest thermodynamically as despite the large size difference between gold and nickel atoms they have a simple phase diagram.' This shows complete solid solubility above a miscibility gap with a maximum at about 71 at. pct Ni and 810°C. Activity measurements (over a range of temperature) have been made previously on this system using an electrolytic-cell method with a liquid chloride eletrolyte. The accuracy of this data has, however, been queried3'4 as it leads to values for the enthalpy of mixing which are too high when compared with calorimetric measurements.46 Also, the entropy of mixing is too high when compared with the values derived from specific-heat measrements. It was therefore considered worthwhile redetermining the activity data using a galvanic cell with a solid electrolyte (0.85 ZrO, 0.15 CaO). This method is based on a technique introduced by Kiukkola and aner'' and has been used to determine the thermodynamic data for Cu-Ni alloys.' THE ELECTROLYTIC CELL The cell used to determine the activity of nickel in Au-Ni alloys was: The cell reaction, which is discussed for a similar cell by Rapp and Maak, gives a direct measurement of the activity of nickel in the alloys as where aNi(alloy) is the activity of nickel in the alloy, 3 is Faraday's constant, E is the measured electromotive force, R is the gas constant, and T is absolute temperature. For the valid application of this type of cell the arrangement must be ther modynamic ally stable, which means that: 1) The free energies of formation of the oxides fulfill the relation 2) The vapor pressures or dissociation pressures of each component must be so small that during the time of the experiment the amount of any material transported by the gas is negligible. 3) Side reactions which change the alloy composition must be negligible. These reactions are possible both with the surrounding gas atmosphere and with neighboring solid material. The first two conditions are fulfilled by the above cell.' The third condition is approached by care in the experimental technique. The factors which control the attainment of equilibrium in this type of cell have been considered by Rapp and aak, who conclude that metallic diffusion in the alloy is the rate-control ling step. A lower temperature limit for the practical application of this cell is therefore set by the condition that equilibrium must be attained in reasonable times. EXPERIMENTAL MATERIALS AND TECHNIQUE The starting materials were mint gold (99.99 pct Au) and Mond nickel (99.9 pct Ni). Alloys, nominally 5 at. pct Ni and then each 10 at. pct across the system, were produced by vacuum-levitation melting compacts of mixed drillings of the pure metals. The nickel used for the reference tablets in the cells was melted in a similar manner. The alloy ingots, cast in boron nitride molds, were cold-forged and

Jan 1, 1967

By Manuel Gomez

Low-temperature carbonization product yields for 129 coals representative of 12 Utah coalfields were estimated, using regression equations developed from heating value and proximate and ultimate analysis data. It was shown that yields of char, tar plus light oil, water of decomposition, and gas, as well as the gas volume and the heating value of the gas, could be predicted with reasonable accuracy. Published and experimental results from eight Utah coals carbonized at selected temperatures in the 4500 to 1,000° C range were used to determine the effect of temperature on product yields. Carbonization temperature, heating value) oxygen, and volatile matter of coal appear to be the principal variables influencing carbonization product yields. Data presented show that the heating value and the residual volatile matter in low-temperature char may be predicted using relationships developed from proximate analysis data for 220 coals.

Jan 1, 1967

By Clyde M. Pearce

This paper describes the facilities at Pointe Noire, Quebec that Wabush Mines utilizes for the receipt, distribution, stockpiling and shipping of iron ore concentrate and pellets. The main topics to be covered will be: 1. - General description 2. - Concentrate receiving facilities 3. - Conveying circuits 4. - Stockpiling 5. - Vessel loading GENERAL DESCRIPTION The map of the eastern Quebec - western Labrador area as shown in Appendix #1 shows the location of Wabush Mines properties. You will note the Scully Mine located at Wabush Lake, Labrador, 235 miles north of the town of Sept-Iles, Quebec. Our neighbors, the Iron Ore Company of Canada have their properties further north at Shefferville, near by at Carol Lake and at Sept-Iles. To the Southwest, our other neighbors, Quebec Cartier Mining, have their iron ore processing facilities and their terminus on the St-Lawrence at Port Cartier. Concentrates are prepared at the scully Mine by mining, crushing, grinding, concentrating, drying and high tension separation for shipment by rail to Pointe Noire, Quebec. Pointe Noire is situated across the bay from the town of Sept-Iles, Quebec on the North Shore of the St-Lawrence River. The concentrate consists of 66% iron, 2 ¼ percent silica and practically no moisture, permitting the use of specially constructed railroad cars and handling facilities to convert the concentrate into pellets, the final product.

Jan 1, 1967

By H. I. Aaronson, H. A. Domian, G. M. Pound

The thernodyna,nics of I the Proeutectoid ferrite re-action ha1.e been investigated on the bases of three diifevent descviptions of the statistical thernzodynamics of interstitzal solid solutions. Especially at low ternperatures, substantial dijeretzces are found in the valltes of the extrapolated y/y + a and cr/a + y equilibriurn curls, and in the To- co7nposilion metastable eqliilibriunz curl-es thus co,npited. Although neither actiztity nor phase-diagram date are able to distingrish udeqiutely among the various descviptions, the statustics of Lacher, Fouller, and Guggenheinz provide the ?nost conplete epresentation az3ailable of the single carbon-ctrbon interaction energy (w) nzodel of an intevstitiril solid solution, and the relationships deduced frojrl then2 are accordingly pre.ferred. The findings tlzut w in austenite 'aries significu?ztly uith tenpevntrue and that phase-diagawr data arc not accurately con?palible usith eqcrctions deduced on the basis of actility infoation indicate, hou'e13er, that a wzore cornplex nlodel of the uustenite , und pvobably of the .feyrite, solirl solutions will have to forn the basis of f4tuve statistical t1.eat1nents. Some suggestions for such a ruodel arc advanced. Althoug11 w represents a vepltlsio energy in austozite, it was found to corvcsporzd in ferrite to a binding energy, in qualitatit.e accord zc,itlz the internal-friclion results of Keefer and wert. ThE transformation of austenite to proeutectoid fer-rite is becoming recognized as an exceptionally useful vehicle for quantitative studies of the kinetics of phase transformations.'" Reasons for this popularity include well-characterized microstructures which develop on a convenient scale with acceptable kinetics within a considerable temperature-composition region, the absence of great sensitivity to common impurities, and, especially. the availability of a unique wealth of the ancillary information indispensable for the quantitative interpretation of kinetic measurements, including phase diagram,3 crystallographies diffusivity,5 inter-facial energy,=17 elastiit," specific vlume, ''' and ativity'-' data. Development of considerable amounts of additional thermodynamic information from activity data is of particular importance with respect to kinetic studies, since much of this information is needed in temperature-composition regions not directly accessible to presently available techniques for the measurement of equilibrium properties. A generally useful approach to the thermodynamics of solid solutions, which is of especial value in this situation, is based upon the formulation of the free energy of such solutions as a function of temperature and composition. The free energy of solid solutions has been resolved into many components. Particularly in the case of interstitial solutions, with which we shall be concerned in the present study, however, only the positional entropy component has been intensively studied. The other components are conventionally taken into account by fitting equations for the activity of the interstitial species or the temperature-composition path of phase boundaries, derived principally from positional entropy considerations, to experimental information on these quantities through adjustment of one or more constants in the equations. A number of studies of the thermodynamics of interstitial solid solutions have been made primarily on this basis,'"25 but only Kaufman, Radcliffe, and cohenZ2 (hereafter KRC) and ener''% ave applied the results of such studies to develop relationships for the thermodynamic quantities of interest in the austenite —- proeutectoid ferrite transformation. KRC made use of a model developed by cheil'' (on the basis of a previous study by ohansson'), and subsequently rede-rived correctly by Speiser and retnak,' in which a carbon atom is considered to inhibit occupancy of a certain number of its nearest-neighboring interstitial sites. schei120 determined the number of sites in austenite thus excluded by matching calculated and experimentally measured curves for the variation of carbon activity with the mole fraction of carbon. zener17 used a different approach. He assumed that the positional entropy of carbon is ideal both in austenite and in ferrite (i.e., no excluded interstitial sites), and included all other contributions of carbon in a temperature-independent "free-energy change" accompanying the transfer of 1 mole of carbon between the two phases. This quantity was determined by "pinning" an equation derived for the boundaries of the a + y region to experimental data on the compositions of these boundaries at a single temperature. In the present investigation, three different approaches to the thermodynamics of the proeutectoid ferrite reaction are examined comparatively: I) the method of Zener; 2) the model employed by KRC and predecessors; and 3) the more detailed statistical thermodynamic treatment of the same model developed by acher and Fowler and uenheim, ' in which the problem of overlapping regions of influence of individual interstitial atoms is resolved. In order to make these comparisons, it is necessary to undertake an extension of one aspect of Zener's method; since the Lacher- Fowler -Guggenheim (LFG) treatment has not been previously used in the present context, the necessary thermodynamic "superstructure" for this treatment will be developed in parallel

Jan 1, 1967

By J. J. Shields

The Bureau of Mines observed two different types of longwall mining; the advancing longwall method and the retreating longwall method at seven bituminous coal mines located in five of the coal producing states. In two mines using the advancing face method, the coal faces were abandoned because of roof failures and poor production. In the other five mines using the retreating method, roof control was good as was production. The success of longwall mining depends on good roof control and good production. The use of self-advancing hydraulic roof supports, such as Westfalia, Dowty, and Wanheim props along with Westfalia coal planers and the Anderton and Eickhoff shearer-loaders have been a factor in recent successes.

Jan 1, 1967