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By Gerald W. Elger

A new process under development by the U.S. Bureau of Mines for producing synthetic rutile from ilmenite is described. Rutile formation is based on oxidation and fluxing of titania slag produced by electric furnacing of ilmenite. Laboratory tests show that phosphorus pentoxide flux additions to oxidized slag enhance conversion to rutile by forming a phosphate-based glass matrix. This matrix contains most of the major impurities, including the oxides of iron, aluminum, magnesium, manganese, and silicon. Rutile crystals of 5 to 150 microns in size were formed in slags heated to temperatures of 800° to 1,550° C. The synthetic rutile crystals were liberated from ground slag by treating with phosphoric acid to weaken the glass matrix, followed by attrition scrubbing. Rutile fractions analyzed as high as 94 percent titania content. In several instances, more than 90 percent of the titanium in the shag was recovered to yield combined rutile fractions containing 90.2 to 92.6 percent titania.

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 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 V. E. Edlund

Laboratory batch flotation tests were conducted on copper converter slags to evaluate the relative merits of recovering copper from slow-cooled versus water-quenched slags. Three slags containing 1.6, 5.0, and 6.6 percent copper were used. More than 90 percent of the copper was recovered in a rougher concentrate leaving a 0.2- to 0.3-percent copper tailings when treating slow-cooled slag. Lower recoveries and higher copper tailings ranging from 0,5 to 0.6 percent copper were obtained from quenched slag. Grindability studies were made on the respective heat-treated slags. Quenched slags proved more difficult to grind than slow-cooled slags. Cost studies showed that (1) the cost of slow cooling and crushing off-sets any advantages of higher copper recoveries from slow-cooled slag, and (2) water-quenched slag, which requires no crushing preparatory to grinding, could be treated more economically. Costs based on processing 1,000 tons of slag per day would be $1.85 per ton for quenched slag versus $2.37 per ton for slow-cooled slag.

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 Jack C. White

Studies were made to determine the character and distribution of the copper lost in copper mill tailings. Acid soluble (oxide) and acid insoluble (sulfide) copper were determined for heavy-liquid sink and float products of screen-sized fractions from 12 copper mill tailings. In most of the tailings studied, the coarse-size fractions are higher in copper grade than the respective bulk tailings, high in sulfide copper, and low in oxide copper. Oxide copper occurs predominantly in the minus 325-mesh "slimes." Microscopic examination of heavy-liquid sink products indicated that recovery of liberated copper sulfide minerals is complete in most mills, and that copper minerals not being recovered are locked with gangue particles. Additional copper could probably be recovered from most tailings by size classification, scavenger froth flotation of the coarse fraction, and regrinding of the concentrate to achieve liberation of the locked sulfides.

Jan 1, 1971

By L. A. Haas

The feasibility of removing sulfur dioxide by carbon monoxide reduction in a fixed-bed catalytic reactor was investigated by the Bureau of Mines. The reduction rate of sulfur dioxide with carbon monoxide was significantly dependent upon the iron and alumina content of the mixed catalyst. Maximum catalytic activity was obtained with about 40 percent iron-alumina mixture with a nominal gas mixture of 10 percent carbon monoxide, 5 percent sulfur dioxide, and the balance nitrogen. The synergistic effect of this catalyst mixture was explained by a dual reaction site mechanism, with both iron and alumina augmenting their specific sites at their interparticle contacts. The catalytic activity also increased with decreasing catalyst pellet size. With O.7-mm pellets, the entire pellet appeared to be catalytically active in a 2-gram catalyst bed. The apparent activation energy of the reaction was 18.3 kcal per mole in the temperature range of 350° to 600° C. Carbonyl sulfide (COS) was produced by the interaction of carbon monoxide and sulfur. The amount decreased with decreasing CO concentration. The ratio of COS formed per SO2 removed reached a maximum at about 400° C. The reaction rate appeared to be independent of S02 concentration in the range of 0.2 to 16 percent. The rate, however, increased directly with the CO concentration in the range of 5 to 20 percent. The presence of CO2 (<15 percent) had no appreciable effect on the rate. However, not over 0.5 percent oxygen could be tolerated. This method appears feasible for removing S02 from waste gas if the oxygen is removed prior to the catalytic S02 reduction process.

Jan 1, 1971

By J. G. Walters

The method for predicting coke strength developed at Steinkohlenberg-bauverein, Germany, in which experimental parameters are readily determined by small-scale laboratory tests, was found to be applicable to cokes produced from industrially used blends of American coals. Predicted 1-inch ASTM tumbler indices for four industrial blends were found to be in excellent agreement with the experimentally determined values. The laboratory determined prediction parameters include the proximate analysis of the coal the size consist of the coal, and Ruhr dilatometer test data.

Jan 1, 1971

By James H. Russell

Several solid sorbents were compared for their effectiveness in removing sulfur dioxide from flue gases. The materials were tested for the rate of sorption and capacity at about 300° C, and rate of regeneration around 700° C in thin beds and in 4-inch-diameter fluidized beds. Rates of material loss were also estimated. The sorbents tested included three samples of alkalized alumina, two samples of sodium carbonate-impregnated alumina, and one proprietary sample of porous silica impregnated with copper and iron compounds. The results showed that all the alkalized aluminas had good sorption capacities and rates, required high temperature regeneration, and suffered excessive material loss; the sodium carbonate-impregnated aluminas (1) had high sorption rates but barely adequate capacities, (2) required high temperature regeneration, and (3) suffered excessive material losses; and the copper-iron impregnated silica suffered only slight material loss and could be regenerated at a relatively low temperature, but the sorption rate and capacity were too small. None of the sorbents met all the arbitrary performance criteria that follow: sorption rate constant of 1 min-1, sorption capacity of 0.1 g sulfur per g sorbent, regeneration rate constant of about 0.075 min-1 at a reasonable temperature, less than 0.07 pct per hour material loss during operation, and a chemical life of 500 cycles.

Jan 1, 1971

By I. L. Nichols

The inplace cyanidation leaching of gold from placer deposits is a potential method for treating gravels too deeply buried and too low in gold content to be processed economically by conventional dredging methods. Laboratory experiments were made to evaluate those placer cyanidation factors adaptable to small-scale studies. The variables investigated included gold particle size and location in sand beds, cyanide solution flow rate, and cyanide solution strength as factors affecting gold solubility rates. The solution flow rate, in turn, was influenced by variables such as bed slope, solution head pressure, and sand size, and the effects of these factors were studied. Free gold, minus 150-mesh and finer in size, is rapidly dissolved by dilute cyanide solutions from mixtures of gold and silica sand prepared to simulate placer deposits. About 94 percent of minus 325-mesh free gold was extracted in 5 hours from silica sand mixtures, and 94 percent extraction of minus 150-mesh gold was obtained in 21 hours with 0.1 percent NaCN solutions. Moving solutions were almost twice as effective in leaching free gold from silica sand mixtures than stagnant solutions.

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 N. S. Petersen

As part of the Demand Evaluation Program of the Bureau of Mines to determine future needs for minerals, a study was instituted to develop and describe a methodology for approaching the problem of substitution between mineral commodities and between mineral commodities and other materials. The report comprises three sections: A review of general factors relative to substitution, a case study of the effect of substitution on zinc die-casting markets in recent years, and a general methodology for reviewing materials substitution with specific emphasis derived from reviewing substitution in the domestic zinc die-casting markets.

Jan 1, 1971

By John Nagy

Data from experiments and literature on gas and dust explosions in closed vessels are presented to show the effects of the vessel size and shape; the initial pressure, temperature, and turbulence; and the fuel-air ratio and the strength of ignition source on pressure and rate of pressure rise. An attempt is made to correlate some of these parameters with an elementary mathematical model. Analyses of data on 17 vessels--spherical, cubical, cylindrical, and rectilinear in shape--ranging from 0,018 to 905 cubic feet in volume were made. Although the study was initiated to provide information primarily on dust-explosion phenomena, some data were obtained for gas explosions so that the factor of initial turbulence caused by the pneumatic blast used to disperse dust could be evaluated. The mathematical interpretation of the explosion phenomena was in general accord with the experimental data, and correlation was obtained for several factors affecting explosion development. Neither vessel size nor shape affected maximum pressure (when heat loss was neglected). The rate of pres-sure rise decreased as vessel size increased, and the rate was proportional to the ratio of the surface area of the vessel to its volume. Induced initial turbulence markedly increased the rate of pressure rise and slightly increased the maximum pressure. Changes in initial pressure produced proportional changes in maximum pressure and rate of pressure rise. Initial temperature and maximum pressure were inversely related, but initial temperature had little effect on the maximum rate of pressure rise. Comparative experiments showed no appreciable difference in explosion development of gas and dust fuels. The vessels and experimental work are described, and all data are given in tables. The mathematical model will facilitate extrapolation from laboratory to industrial conditions and will allow comparison of results obtained in different laboratories.

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

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 Thomas O. Llewellyn

Laboratory semicontinuous and continuous heavy liquid cyclone separation pilot plant tests were made to determine the feasibility of producing a high-grade kyanite concentrate from a kyanite-quartz rock sample from Graves Mountain, Ga. Use of a three-stage heavy liquid cyclone circuit demonstrated that a 96.4-to 99.0-percent kyanite concentrate could be obtained with recoveries of 95.5 to 96.7 percent. The test work showed that by steam stripping with 6.9 tons of steam per ton of ore and two stages of detergent scrubbing the residual TBE content of kyanite cyclone products was 0.22 pound per ton of ore.

Jan 1, 1971

By C. Kenneth Eilerts

A method is described for controlling instability in finite-difference computations of liquid saturation near the borehole of a recovery well. Differences of pressure-and saturation-dependent variables are indexed offcenter, upstream and downstream alternately, to provide a stabilizing average. It was found that size of the time step could be increased by a factor of 4 without loss of numerical stability. Finite differences of the variables occur in a variety of relative numerical sizes and combinations. Those relationships of the differences that contribute to instability may be identified by the computing program in which they occur and modified to assist convergence of the computations and execution of the partial differential equations of liquid and gas flow.

Jan 1, 1971

By David P. Lindroth

The heat content above 25.0° C up to 1,000° C was measured for six rock types: St. Cloud Gray Granodiorite, Holston Limestone, Sioux Quartzite, Rockville Quartz Monzonite, Salem Limestone, and the basalt at Dresser, Wis. The calorimetric data were obtained with an isothermal jacket-copper block calorimeter. The experimental heat content data for each rock type are presented, along with specific heat data obtained from the temperature derivative of the heat content. For the six rock types the maximum deviations of the specific heats at a given temperature were within 10 percent below 575° C and within 34 percent above 5750°C. The increase in the values of specific heat range from a minimum of 13 percent for the basalt at Dresser, Wis. (temperature range, 100° to 1,000° C) to a maximum of 46 percent for Holston Limestone (temperature range, 100° to 870° C).

Jan 1, 1971

By Donald P. Schlick

This Information Circular presents a brief historical digest of the early attempts of the Bureau of Nines and the U.S. Public Health Service to establish coal mine dust exposure standards. It reviews current, accepted standards of the United States as well as available standards of other countries.

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