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By A. F. Baker

Laboratory flotation of synthetic coal-pyrite mixtures and high-pyritic-sulfur coal indicated that ferric chloride (FeCl3), aluminum chloride (AIC13), chromium chloride (CrCl3), and cupric sulfate (CuSO4) are potential pyrite depressants. For each metal salt there appeared to be a range of pH values and optimum concentration for selectively depressing pyrite in coal flotation. Pyrite was depressed in the pH range from 4.5 to 7.0 with ferric chloride, from 5.8 to 7.0 with aluminum chloride, from 6.4 to 7.1 with chromium chloride, and from 6.4 to 7.4 with cupric sulfate. Best separation of pyrite from coal was achieved in flotation solutions containing from 2 X 10-5 to 5 x 10-5 mole/ liter of each salt. In solutions containing excess salt concentrations, coal was also depressed. These Bureau of Mines tests demonstrated on a laboratory scale that, in solutions containing 4 X 10-5 mole/liter ferric chloride and from 1 x 10-4 to 2 x 10-4 mole/liter sodium hydroxide, the pyritic sulfur content of a Lower Freeport bed coal sample could be reduced from about 2.51 percent to less than 0.60 percent with recoveries of over 83 percent. The depression of pyrite appears to be due to the adsorption of positively charged colloidal metal hydroxide at the pyrite-solution interface. This hypothesis is supported by zeta potential determinations which showed that suspended coal and pyrite particles in solutions containing metal salts are positively charged in the pH range where depression occurs.

Jan 1, 1971

By W. K. Sawyer

Resistivity, porosity, permeability, and saturation data were obtained on core samples from the Big Injun, Clinton, Gordon, Bradford Second and Third, and Venango Second oil sands and formation factor-porosity relationships were derived using the general form of Archie's equation F = aø-m, where F is the formation factor, ø is the porosity, and a and m are constants that depend on characteristics of the rock. It was found that a and m varied significantly between sands, as did the exponent in the Archie relation I = Sw-n, where I is the resistivity index and S, is the water saturation. The average exponent, n, determined from all data was 50 percent greater at residual oil saturation than at residual water saturation. Samples from each sand exhibited differences in directional resistivity and/or permeability. The Bradford Third sand data showed correlation between resistivity and permeability anisotropy.

Jan 1, 1971

By Robert Blickensderfer

Tungsten alloys with high-temperature strength properties, comparable to the best of alloys recently developed by others, were produced by a new process called here the oxyreaction process. The process involved additions of a powder of a reactive metal compound, ZrN, ZrW2, or HfW2, to a base metal powder, tungsten, which contained some oxygen. The powders were blended, compacted, sintered, and extruded. During sintering, diffusion and internal oxidation occurred to produce reactive-metal oxide particles and solid solutions. A dispersion of oxide particles could be precipitated by heat treating. The oxyreaction process circumvents many of the agglomerating and coarsening problems encountered in the current methods for dispersing a stable oxide in a metal. Oxyreaction strengthening results from solid-solution strengthening and from dispersion strengthening produced by the reactive metal and its oxides. At a test temperature of 1,650° C, the alloys prepared from WW, had tensile strengths up to 70,000 psi and stress-rupture lives up to 142 hr at 10,000 psi stress; the alloys prepared from ZrN powders had tensile strengths up to 80,000 psi and stress-rupture lives up to 27 hr at 10,000 psi stress. Tensile strengthening in the alloys was attributed to Zr in solid solution or to Zr-O-W structures too small to be observed in an electron microscope replica. Stress-rupture life was attributed to a dispersion of submicron Zr02 particles which precipitated and grew to 0.05-to 0.2-micron size during the test. Tensile strengthening and stress-rupture life were dependent upon both the zirconium and oxygen contents with the maximum occurring at roughly 0.9 atomic pot Zr and 0.9 atomic pot 0. Studies of the details of the oxyreaction process were made on the W-ZrW2 alloys and three general steps were determined: (1) The reaction of 0 in tungsten powder with ZrW2 to form relatively large Zr02 particles; (2) the dissolution of remaining ZrW2 into the W matrix and partial internal oxidation to form ultrafine but sparse zirconium oxide particles and possibly to establish Zr-O-W structures; (3) the development of ultrafine Zr02 particles during high-temperature aging.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated the properties and anisotropy in properties of rolled Zn-Ti and Zn-1.0 wt pct Cu-Ti alloys containing up to 0.36 wt pct Ti. Finish rolling was at varied temperatures to total reductions as high as 92 pct. Alloy properties are very sensitive to various combinations of composition, rolling temperature, and reduction. Properly rolled Zn-1.0 Cu-Ti alloys are superior in strength to Zn-Ti alloys. Conditions are described that lead to best tensile properties. Creep resistance for Zn-Ti alloys decreases with increased rolling temperature when finish rolled to 92-pct total reduction: but not when finish rolled to 33- or 67-pct reduction. Creep resistance for 7n-1.0 Cu-Ti alloys improves with increased rolling temperature to about 480° F. Heavily cold-rolled Zn-1.0 Cu-Ti alloys have fine grain sizes and poor hardness, tensile, and creep properties, but high ductility. Thermal expansivity is markedly affected by the copper addition. Data show the anisotropy of tensile, creep, and thermal expansivity properties. Large idiomorphic crystallites of TiZn15 appear in both Zn-Ti and Zn-Cu-Ti alloys when more than about 0.2 pct Ti is present. A new Zn-Cu-Ti intermediate phase was also identified. Empirical equations are presented relating creep rates with major process variables.

Jan 1, 1971

By J. D. Dixon

The Bureau of Mines investigated the principles of support-rock interaction, based on structural matrix methods which permit mathematical formulation of the problem and computer solution. The principles are given under two main sections: the first discusses the idealization of the tunnel support structural system for matrix analysis; the latter discusses the analysis procedures necessary for carrying out the solution. A general frame matrix computer program and a medium-size computer should be sufficient for carrying out the procedures involved. The example problem consists of a circular tunnel support which is subjected to a uniformly distributed vertical load, Three wall thickness-radius ratios are studied in combination with four support-rock modulus ratios. This problem illustrates the main procedures of the support-rock interaction analysis involved, and examination of the results reveals the influence of the relative rigidities of the support and the rock.

Jan 1, 1971

By B. Dimitriades

Data on smog-forming reactivities of exhaust aldehydes are scarce. Such data were obtained by irradiating in a smog chamber typical exhaust aldehydes, individually and in exhaustlike mixtures. Observed reactivity manifestations were rate of nitrogen dioxide formation (RNO2) and yields of oxidant, peroxyacetyl nitrate, and formaldehyde. Results showed that exhaust aldehydes vary widely in reactivity. Formaldehyde showed high RNO2 reactivity but low oxidant yield; benzaldehyde, [m]-, and [p]-tolualdehyde were totally unreactive when irradiated individually; [o]-tolualdehyde was reactive. In mixtures, benzaldehyde manifested reactivity in terms of peroxybenzoyl nitrate yield. Exhaust aldehydes as a group are judged to be as reactive as the exhaust olefin group. The importance of the aldehyde contribution to exhaust reactivity and methods for assessing such contribution are discussed.

Jan 1, 1971

By R. E. Meaker

Electrical conductivities and densities of molten fluoride systems were measured as functions of the melt temperature and composition. For any given mixture, the two properties change linearly with temperature. Three alkali metal fluorides were selected as solvents for melts of the type LiF-, NaF-, and KF-MFx, where M is a metal selected from the alkali metal or alkaline earth groups, or from the lanthanide or actinide series of elements, and x = 1-4. Heats of activation for conductance were calculated from the experimental data and varied from 2.3 to 9.2 kcal/mole at 1,000° C. Some relation between position in the phase diagram and the conductivity changes was suggested.

Jan 1, 1971

By W. F. Marshall

This report describes exhaust-emission data from 10 diesel engines: six 4-cycle, direct-injection, naturally aspirated engines; two 4-cycle, direct-injection, turbocharged engines; one 4-cycle, precombustion-chamber, turbo-charged engine; and one 2-cycle, direct-injection engine. These engines were tested over a 3-year period (1968-70). Lowest emissions were obtained with a precombustion-chamber engine. Emissions from the 2-cycle, direct-injection engine fell within the range of emission rates for the 4-cycle, naturally aspirated, direct-injection engines. Excluding the precombustion-chamber engine and excepting one of the 4-cycle, naturally aspirated engines, carbon monoxide emission rates were about the same for all engines tested. Test data on smoke, odor, and emissions of hydrocarbons, oxides of nitro-gen, carbon monoxide, and aldehydes are given.

Jan 1, 1971

By W. J. Wenger

Analytical, geographical, and geological data on 67 samples of crude oils from Utah are presented, along with some correlations and interpretations. Most of the, geologic formations that produce oil in other areas are also productive in Utah; and as in many other locations, the Permian, Pennsylvanian, and Mississippian formations account for the major amount of the total oil produced in the State. Some anomalies and unusual phenomena are noted. Although most Utah oils are low in sulfur, a sample containing the highest percentage of sulfur ever recorded by the Bureau of Mines is among the oils discussed in this paper. Most of the oil from the major producing formations in Utah is low in sulfur; the same formations produce high-sulfur oils in adjoining Rocky Mountain States. Some Utah oils are both waxy and asphaltic, an unusual combination of characteristics. Correlation index curves for some oils are shown suggesting compositional differences in oils from different producing formations. Production statistics trace the rapid rise of oil production in the State after the first commercial discovery in 1947 and indicate a decline in amounts produced since 1959, the year of peak production in Utah.

Jan 1, 1971

In 1962 and 1963, two in situ combustion pilot tests were conducted in the shallow Second Venango sand near Reno, Pa. Because of poor oxygen utilization and lack of production response, both tests were considered failures and were terminated. The area was then relatively inactive until late 1966, when a development well drilled near the 1963 test site had surprisingly good production in what was considered to be a pressure-depleted reservoir. Other wells drilled in and around the old thermal pilot areas also came in as good oil producers. This report presents a study of the increased oil production from the Second Venango sand in the Reno area, and the apparent connection of the present production response and the old thermal pilot tests. Apparently combustion occurred in the Second Venango sand after the 1962 and 1963 experiments were terminated and, supported by large volumes of air left in the reservoir after the 1963 test, generated carbon dioxide which helped repressure the formation. This field evidence of combustion warrants another pilot experiment to further explore the use of properly designed in situ combustion techniques in increasing production from the Second Venango sand.

Jan 1, 1971

By P. G. Pigott

This Bureau of Mines laboratory research demonstrated that building bricks meeting ASTM specification C62-66 for grades SW and MW of FBS-type bricks can be produced from waste copper mill tailings. Waste tailings from accumulations at Magna, Utah, Anaconda, Mont., and Hayden, Miami, and San Manuel, Ariz., were dry-pressed into bricks, and the products were tested in accordance with ASTM Designation C67-66 on sampling, and testing of brick. An evaluation derived from pilot-plant production of similar brick at the Coal Research Bureau of West Virginia University indicated the production cost to be about $34 per 1,000 bricks. Utilization of such mill tailings on a commercial scale would eliminate the need for digging new pits for brick raw material production, conserve natural resources, and simultaneously remove potential sources of air pollution.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated creep and other properties of extruded Zn-30 pct-AI alloys containing 0 to 0.7 pct Mg. The alloys were extruded both above and below the Zn-Al eutectoid temperature of 275° C. Creep behavior is defined for the alloys as extruded and after various heat treatments. Tensile properties, hardness, thermal expansivity, impact resistance, and microstructures are given. The alloys, either with or without magnesium, required substantially less pressure for extrusion near 275° C than at higher or lower temperatures. The alloys containing magnesium exhibited significantly greater hardness, tensile strength, and creep resistance, but much lower ductility than the 2n-30 pct Al alloy. The properties were very sensitive to the processing conditions.

Jan 1, 1971

By F. D. Sutterfield

This study was conducted to provide experimental evidence on the effect of modifications of gasoline front-end composition on the photochemical specific reactivities of automotive emissions. Evaporative and evaporative-plus-exhaust emissions from an automobile operated with four fuels of different volatility and varying levels of C.-C5 olefins were irradiated in a 10040 environmental chamber at three sets of initial hydrocarbon-nitrogen oxides concentrations. Reactivity was measured and expressed in terms of rate-of-NO2 formation and dosages of oxidant, peroxyacetyl nitrate, and formaldehyde. The compositional changes that were necessary in reducing fuel volatility were found to have no significant effect on the reactivity of the emissions. However, replacing C4-C5 olefins with saturated components resulted in sharp decreases in all reactivity manifestations observed for the evaporative emission samples. A lesser influence (of C4-C5 olefin replacement) was found with the composite exhaust-plus-evaporative samples; the effect that was observed could be attributed to the evaporative emission portion of the sample. The data therefore suggest that saturation of front-end fuel olefins had no large effect on exhaust emission reactivity.

Jan 1, 1971

By J. R. Ruark

This report presents results of the research and development work and operations performed during stage II of the gas combustion retorting research program conducted by the Colorado School of Mines Research Foundation and six major oil companies at the Bureau of Mines Anvil Points Research Facilities. The experimental program, including retort modification and air-gas distributor development, effects of shale quality and particle-size distribution, and other variables on the process, is discussed. Although operating problems are not fully resolved, it appears that the gas combustion retorting process can be successfully applied to achieve oil yields in excess of 85 percent of Fischer assay at mass shale feed rates of 500 pounds per hour per square foot of cross-sectional bed area, approximately twice the rate previously demonstrated to be reasonably practicable.

Jan 1, 1971

By Robert E. Wood

[The temperature dependency of the low-density thermal conductivity coefficients, ?°T, of nitrogen, 100° to 1,200° K, is correlated with the Keyes' equation, ?T ½ -1 -12/T) WT = aT+ bT 10 The equation ?T,P = ?°T +a[ ]ß represented 509 experimental higher V pressure thermal conductivities in the temperature range 131.2° to 973.15° K for pressures to 500 atmospheres, with a mean absolute deviation of 2.35 percent. This equation was used to compute thermal conductivities of gaseous nitrogen for 47 pressures, 1 to 240 atmospheres, and 110 temperatures, 133° to 740° K, which are common to conditions encountered in Bureau of Mines helium purification processes. Isobaric heat capacities, CP, and viscosities, ?T,P, from previous work were combined with the present thermal conductivities, ?T,P, to compute Prandl1 numbers, C?T P / ?T ,P, of nitrogen. Tabular values of Prandtl num¬bers are presented for 49 pressures, 1 to 240 atmospheres, and 75 temperatures, 133° to 740° K. Estimated uncertainties are ±5 percent in the tabulated thermal conductivities and ±15 percent for the computed Prandtl numbers. However, the uncertainty may rise to ±10 percent for thermal conductivities and to ±30 percent for Prandtl numbers as the critical conditions of nitrogen are approached.]

Jan 1, 1971

By Lester J. Crow

A preliminary survey was performed to investigate the impregnation of relatively weak, porous volcanic tuff and a relatively strong, dense sandstone with five different monomers. Increases in compressive strengths by factors of 2 to 5, and elastic moduli by factors of 2 to 3.5, are reported for natural rocks (tuff., sandstone, dacite), which were impregnated with five monomers (methyl methacrylate; chlorostyrene; 40 percent TMPTMA-60 percent styrene; 40 percent TMPTMA-60 percent chlorostyrene; 60 percent polyester-40 percent styrene); polymerization took place after monomers were forced into the rock. Impregnation was performed (1) by pressurizing rock specimens from one end, or (2) by a vacuum-soak operation. Polymerization was accomplished by either radiation or chemical initiation techniques. Strength improvement is dependent on (1) the type of monomer used, (2) the amount of polymer incorporated into the rock, and (3) the degree of water saturation of the rock. Water saturation strongly reduced the effectiveness of the method for the polymer systems tested. The more viscous monomers (for example, 60 percent polyester-40 percent styrene) were more effective in displacing the water from the rock, and compressive strengths of wet rock were doubled with these systems. Water saturations ranging from 25 to 100 percent of maximum saturation gave essentially identical results. Further tests on other types of mine rock; including shale and coal, are planned. Water-compatible polymer systems should be developed, or present systems should be suitably modified. For application to tunnel stabilization, design studies evaluating the improvement in rock strength and its influence on the support system are also recommended.

Jan 1, 1971

By David E. Nicholson

This report investigates the mechanical behavior of fine soils in a lunar environment in engineering gravity-flow bins. The ultrahigh vacuum, absence of moisture, and a lunar gravity one-sixth that of earth gravity represents a unique environment, both advantageous and detrimental to these systems. On earth, moisture and gases contained in powder masses can be responsible for complex descriptions of gravity flow. Their absence appear to simplify the lunar soil behavior. However, simulation of the lunar gravity and vacuum complicates the development of experimental data for designing bins. The properties of a dry soil powder, its behavior under one-dimensional compression, and its torsional and direct shearing strength under earth atmosphere are described in part 1 of this paper. These properties provide the parameters for a finite-element analysis to optimize the design of bins, to be described by Dr. William Pariseau in part 2. Shear tests assess the failure criteria for the material. Compression tests provide modulus and (Ko) stress-ratio values from the loading portion of the compression cycle, duplicating the condition of a bin at rest with the discharge closed. During the unloading portion of the compression cycle (soil overconsolidated), the residual Ko values rise. It is postulated that this phenomenon creates a high-lateral stress in bins when they approach incipient flow. Assessment of the Ko value, overconsolidation ratio, and the void ratio state is proposed as a criterion to determine the flowability of powder.

Jan 1, 1971

By J. A. Lamonica

The Bureau of Mines studied a pulsation damping device designed to smooth pulsating flow in personal respirable dust samplers. The effect on the pulsation dampener efficiency of six parameters was investigated, as follows: Volume, diaphragm elasticity, diaphragm area, center orifice area, inlet-outlet orifice area, and geometry (LID ratio). The results indicate that volume pre-dominates in determining snubber efficiency, while the other parameters become important at small volumes. Geometry has no effect on snubber efficiency. Criteria for an efficient pulsation dampener construction were obtained.

Jan 1, 1971

By R. V. Higgins

The results of two separate but related studies are given. In the first study, four equations were tested; the object was to determine which would produce a curve that would best fit data points that represent a trend of declining oil production in 90 California fields. Two conventional equations (the Arps and semilog) and two novel equations (extreme-c and double semilog) were tested. The curves were first fitted to the initial 9 years of the 15-year production data and then extrapolated for 6 years to determine how well the extrapolated curve would fit the data points. The generated curves were also extrapolated beyond the last data point to predict rates of future production. The results of the first study showed that no equation was clearly superior to the others in all respects. The semilog equation resulted in the best fit to production data for the first 9 years, but the Arps and extreme-c equations produced a better fit for the extrapolated data for the period of 9 to 15 years. The Arps and extreme-c also gave more realistic production rates when extended to the point where cumulative production equaled reserves. A second study was made to determine if the least-squares technique applied to the Arps equation would result in more accurate extrapolations. The merits of the logarithmic and the nonlogarithmic forms of the Arps hyperbolic equation were also tested. For the logarithmic expression, it was found that one of the constants of the Arps equation reached a value so small or so large that the equation was not applicable to the data of 40 of the 90 California fields. The nonlogarithmic form of the Arps equation was applicable to neither the same 40 fields nor to a few additional ones. When the data and the Arps equation were compatible, the use of the least-squares technique as compared with other methods improved the extrapolation accuracy somewhat.

Jan 1, 1971

By R. D. Groves

Techniques were developed for preparing metallurgical-grade copper powder from industrially produced cement copper. Flotation was used for rejecting discrete gangue particles, acid leaching to remove residual iron and aluminum, hydrogen reduction to eliminate oxygen, sintering to consolidate the fine-sized copper, and grinding to obtain copper powder. Powders prepared from six different cement copper samples contained, in percent, 98.5 to 99.0 Cu, 0.10 to 0.05 Fe, 0.10 to 0.08 insoluble material and the remaining individual impurities less than 0.15 percent. The apparent density, flow characteristics, and other physical properties were suitable for powder metallurgy applications. An economic evaluation showed that this process was economically feasible. Processing costs appeared modest when considering that copper powder commands a price normally about 17.5 cents per pound over that of electrolytic copper.

Jan 1, 1971