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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 D. J. Bauer

Solvent extraction separation of light group rare-earth elements in a quaternary ammonium compound-chelating agent system was demonstrated in single-stage studies, Typical separation factor values obtained were 93 for lanthanum-praseodymium, 5.4 for praseodymium-neodymium, and 11.6 for neodymium-samarium. These values are significantly higher than those obtained using organophosphate extractants. Further studies in a 20-stage countercurrent mixer-settler resulted in the production of 99 percent lanthanum (oxide basis) at 96-percent recovery. Subsequently, 88 percent of the neodymium with a purity of 92 percent was recovered in the raffinate.

Jan 1, 1971

By A. W. Deurbrouck

This Bureau of Mines report describes the washability characteristics of 14 coalbed samples collected in Wyoming. Such data is needed to evaluate the quality of the coals of the West where most of our low-sulfur-content coal reserves are found. Of the 14 samples included in this report 13 had a total sulfur content of 1.1 percent or less. All of the samples contained low per¬centages of ash or could be readily washed to a desirable ash level with minimal loss of yield. The coals ranged in rank from high-volatile B bituminous to subbituminous C, although 10 of the samples were high-volatile C bituminous. The coalbeds varied in thickness from 4.5 to an unknown thickness greater than 67.5 feet.

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 Irven A. Jacobson

The thermal reactions of l-methylindole were studied in the temperature range of 525° to 627° C in a flow reactor. The major products consisted of 2-methylindole, 3-methylindole, indole, quinoline, hydrogen, and methane. 2-Methylindole is formed from 1-methylindole by an irreversible isomerization reaction. The 2-methylindole isomerizes in a reversible manner to 3-methyl-indole, the equilibrium favoring the 3-methyl isomer. Indole is formed directly from 1-methylindole. Quinoline is formed from l-methylindole, 2-methylindole, and 3-methylindole.

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 Richard J. Kline

This publication comprises tables listing friction loss for a flexible, spiral-reinforced circular ventilation tubing system. The tables were constructed with the following parameters: a friction factor of 62 X 10-10, 10-foot sections of tubing ranging in total length from 100 to 550 feet, air quantities ranging from 1,000 to 15,000 cfm, and one to four 90° bends in the tubing. The aim of this publication is to improve ventilation tubing analysis and to provide a method of proper fan selection.

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

By R. F. Waters

The Bureau of Mines developed laboratory-scale processes to recover sodium phosphates and metal values from waste sludges generated by the phosphate treatment of automobile and appliance components. After treatment of the sludge with NaOH, followed by coke or hydrogen reduction and sintering, zinc and lead were recovered as fume; the sinter was separated by leaching into a metallic product, chiefly iron and nickel, and high-purity disodium or trisodium phosphate.

Jan 1, 1971

By R. F. Abernethy

A small-scale method was developed for determining the free-swelling index of coal samples of limited quantity, especially the macerals. Results of a series of tests using a 0.3-gram sample correlated well with those by the standard method using a 1-gram sample. The standard and small-scale methods are modified to give unrestricted swelling for those coals having swelling index numbers above 7.

Jan 1, 1971

By J. M. Stuve

Calorimetric determinations of the low-temperature heat capacities, standard enthalpy of formation, and high-temperature enthalpies were made of (Na20)4 ?Fe20,(c). The resulting values of entropy (S°), enthalpy of formation (?Hf°), and free energy of formation (?Gf°) at 298.15° K are 104.676 cal/deg mole, -656.2 ±.kcal/mole, and -603.4 A kcal/mole, respectively. Tabulations of Cp°, S°, - (G°-H°298)/T, H°-H°298, ?Hf°, ?Gf°, and log Kf are given to 1,200° K.

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