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By Martin H. Stanczyk

Bench scale, laboratory batch attrition grinding tests were made of a coarse commercial kaolin in a stainless steel, 5-inch-diameter attrition grinding machine to study the effect of a number of basic operating variables on particle size reduction and electric energy consumption. The results of the investigation showed that the more important operating variables influencing the efficiency of kaolin comminution and energy consumption requirements were type, size, and shape of grinding media, grinding media to clay weight ratio, peripheral rotor speed, clay slip pulp density, degree of pulp dispersion, and the angular arrangement of the rotor and stator bars. The tests also indicated that variables having less influence on grinding efficiency and energy consumption were pulp temperature, design of rotor cage, rotor clearance, rotor-stator bar interval, addition agents, pulp level, degree of pulp aeration, and chamber liners. The research showed that grinding media had the greatest influence on abrasion of machine parts and that spherical-shaped grinding media were superior to sharp angular or long bladed media with respect to media degradation, machine abrasion as well as grinding efficiency.

Jan 1, 1968

Reports by researchers in government, industry, and universities of the United States are given for various projects on basic coal research concerning, the metamorphism, physical and chemical properties, and reactions of coal, and how many of these studies can lead to better utilization of coal.

Jan 1, 1968

During fiscal year 1966 the Bureau of Mines published 99 scientific and technical papers and engaged in 67 research projects on petroleum, natural gas, and oil shale. A basic appropriation of $3.4 million was supplemented by $1 million in cooperative funds from other Governmental agencies and industry groups. Petroleum conservation was advanced by development of scientific knowledge and improvement of technologic methods in both the extraction and utilization of petroleum, natural gas, and oil shale. Experimental work was carried out at research centers in Bartlesville, Okla., and Laramie, Wo., and in laboratories in Morgantown, W. Va., and San Francisco, Calif. ACHIEVEMENTS IN FISCAL YEAR 1966 Bureau of Mines--Petroleum Research in fiscal year 1966 (July 1, 1965- June 30, 1966) was involved in many public issues--air pollution, peaceful uses of nuclear explosives, utilization of oil-shale resources, computerization of recovery-stimulation techniques, and fuels for supersonic airplanes. Scientific contributions included compositional studies of petroleum and oil shale, determination of thermodynamic properties of petroleum compounds, development of analytical techniques, and correlations of petroleum properties with geologic occurrence. Technologic advances included rock-fracturing research, in situ combustion studies, waterflood techniques, use of radio-tracers to study stability of petroleum fuels, and hydrogenation as a tool to prepare shale-oil products.

Jan 1, 1968

By John J. Henn

An evaluation is presented for an ammonium sulfate leaching process designed to extract manganese from Cuyuna, Minn., and Aroostook, Maine, deposits. In this process the manganese and iron in the ore are reduced to MnO and Fe 3 0 4 in a shaft furnace; the reduced ore is then leached with ammonium sulfate solution forming soluble manganous sulfate while leaving most of the iron undissolved. After filtration, the manganese and some impurities are precipitated from solution as carbonates which are then pelletized and calcined to form a product composed mainly of Mn3O4. The plants are designed to produce 100 tons per day of manganese contained in a product that is suitable for the production of ferromanganese. A byproduct credit, together with the extra processing cost, is included for the Cuyuna ore processing plants because Fe2O3 may be recovered for use in blast furnaces. The estimated operating costs per ton of manganese, excluding income taxes and return on investment, are: [ ] The process with or without byproduct recovery, when treating Cuyuna or Aroostook ores, is not economically competitive with ores available at $71.43 per ton of contained manganese.

Jan 1, 1968

By John R. Hoskins

The Bureau of Mines conducted an investigation to more exactly define the influence of some end conditions on the laboratory-determined uniaxial compressive strength of rock samples. Limestone, marble, sandstone, and granite were used to provide a range of specimen modulus of elasticity from 2.7 X 106 psi to 10 x 106 psi. Four variables were studied: Nonparallelism and surface texture of specimen ends were the specimen variables investigated; the end platen size and the adjustable or spherical head friction were the machine variables studied. It was concluded that the loading ends of small laboratory models and samples should be prepared with surface irregularities that do not vary from a plane surface by more than 0.001 inch. It was also concluded that nonparallelism of the specimen ends should not exceed 8 minutes for a rigid head load or 15 minutes for an adjusting head load. The measured compressive strength of specimens prepared with these tolerances will be statistically the same with any diameter or thickness of platen and any degree of head friction if initial alinement of the specimen is assured.

Jan 1, 1968

By Herman W. Sheffer

This report describes and discusses present-day leaching technology employed to recover copper from low-grade mine and dump materials derived from the exploitation of copper ore deposits in the Western United States. Illustrations of the integral parts of the leaching, precipitation, and recovery operations at several copper-producing companies are presented. Schematic drawings are included to present typical flowsheets of leaching and precipitation operations. Operational problems common to most copper leaching and precipitation plants are discussed. Areas of present and future research to improve leaching techniques are cited.

Jan 1, 1968

By M. M. Tilman

A series of alloys was laboratory prepared by adding up to 4 weight-percent cobalt to the basic composition of type AM 350 (AISI 633) stainless steel. Aging curves were established for each alloy at 750° F, 850° F, and 950° F for lengths of time up to 100 hours. A series of annealed steels containing as much as 1 weight-percent cobalt was cold-rolled 50 percent and aged for 3 hours at 850° F. No improvement in hardness due to cobalt was observed in the steels transformed by heat treatment. Slight improvements in hardness were observed in the steels transformed by cold working.

Jan 1, 1968

By Martin Berman

The Bureau of Mines has investigated the mineral matter content of 38 American coals using X-ray fluorescence. Measurements of the Ka intensity for magnesium, aluminum, silicon, sulfur, calcium, and iron permit the determination of those elements as well as an indirect determination of the ash con-tent of the coals. The percentage of each of the six elements was corrected for absorption by all six elements as well as by hydrogen, carbon, nitrogen, and oxygen. It made little difference whether the values used for hydrogen, carbon, and nitrogen were obtained from chemical analysis or whether average values for all coals were used. In all cases, oxygen was obtained by difference. The correction for absorption by all these elements involved the inversion of a 6 X 6 matrix and was performed by computer. Assuming that the elements magnesium, aluminum, silicon, calcium, and iron were present in the ash as oxides, the quantity of ash was determined. The results for the mineral elements as well as for ash and oxygen were in good agreement with chemical results. Particle size was found to have a significant effect on fluorescence intensities. A study of size effects was made for pyrite particles, since the sulfur content of coals is of particular interest. Theoretical equations were derived and verified relating the intensity to particle size. It was found that the coal samples must be ground to less than 2 microns. Sulfur appears in several forms in coal, and the effect of sulfur form on intensity was investigated. It was found that the Ka intensity was independent of sulfur form but the Kß intensity varied with the type of sulfur. Thus, the Ka intensity was used for determination of the quantity of sulfur present. Utilization of the sulfur KB intensity did not permit a determination of the proportions of sulfur forms present in coal. However, for synthetic mixtures of cystine and pyrite in carbon black, measurement of sulfur Ka and Kß permit determination of each constituents from measurements of sulfur intensities alone.

Jan 1, 1968

By A. F. Colombo

Bench-scale research was undertaken to determine if adding ammonia to cyanide leaching solutions would enhance the extraction of copper from an argillaceous Michigan copper ore. Two leaching techniques, (1) rolling using a tumbling bottle and (2) aerating using a modified Buchner funnel, and variations in pulp temperature; were employed in evaluating the effect of ammonia concentration on copper extraction. Under these experimental conditions, the extraction of copper was shown to be independent of ammonia concentration and entirely dependent on cyanide concentration.

Jan 1, 1968

By D. J. Bauer

A primary amine extraction system was investigated for fractionating a cerium-group, lanthanide sulfate mixture. Addition of diethylenetriaminepenta-acetic acid (DTPA) to the amine extraction system resulted in separation factors as high as 5.4 for lanthanum-cerium, 8.0 for cerium-praseodymium, 3.7 for praseodymium-neodymium, and 7.0 for neodymium-samarium. In multistage studies on a cerium-free lanthanide mixture, 96 percent of the lanthanum was recovered with a purity of 95 percent.

Jan 1, 1968

By Floyd G. Anderson

Bureau of Mines studies show than an electronic counter can be used for determining just concentrations from midget impinger samples collected in bituminous coal mines. A sample correlation coefficient of 0.91 for data obtained using the electronic counter and the Bureau of Mines microprojector procedures indicates a significant linear relationship between the methods. The electronic counter provides better counting precision and reduces analytical time.

Jan 1, 1968

By Henry C. Meeve

This report describes work done in the Creede Mining district, Mineral County, Colo., in 1965-66 as a part of a Bureau of Mines study of the silver production potential of the United States. The ruining history of the district is briefly covered, and representative former and current mining operations are described. Mining and milling costs of the Emperius Mining Company's operation are given in some detail as being representative of the cost of mining typical Creede ore bodies under current technology. An estimate of the silver reserves and resources of the district is presented, subject to many uncertainties stemming from inaccessibility of old workings, lack of mining records, and low level exploration activity, all of which limit the opportunity to accurately evaluate ore potential. The report concludes with an analysis of future silver production trends in the Creede district. An increase of silver production to as much as I million ounces yearly is projected, possibly starting in 1969. As long as ore bodies in the zone of enrichment, in which silver is a major constituent, contribute a substantial part of Creede production, silver price will affect overall production rates appreciably. As the richer are bodies become depleted, an increasing portion of production again will be coming from primary sulfide ores in which silver is a byproduct of lead and zinc. When this occurs, the level of silver production will be governed chiefly by lead and zinc production and prices and can be expected to decline to the 1960-66 level, which amounts to an average of 240,000 ounces per year.

Jan 1, 1968

By E. L. Singleton

The electrochemical reduction of aluminum chloride to aluminum was investigated in a closed, two-compartment cell utilizing a molten chloride electrolyte. The externally heated cell was divided into a reduction compartment and a combination AICl3 feed and metal removal compartment. Aluminum was deposited at 700° C on a molten aluminum catbode from a KCI-NaCI-AICI3 electrolyte. The AICl3 content of the electrolyte was replenished by either vapor or solid additions. The chlorine evolved was collected and measured to give a quantitative evaluation of AICl3 reduction. The effects of anode and cathode current densities and AIC13 concentration on anode current efficiencies were studiedo A range of 64 to 84 percent anode current efficiency was obtained with the 25-pound electrolyte capacity cell and related auxiliary equipment.

Jan 1, 1968

By J. Hudy

The performance of six dense-medium washers was evaluated in five preparation plants. Three of the plants were making a two-product separation that produced a clean coal and a refuse; one plant employed dense-medium vessels in series to effect a primary and a secondary separation; and one plant was equipped with a two-compartment washer effecting two separations in one vessel. The separate secondary drum-type washer produced a low-ash metallurgical coal and an intermediate-ash product suitable for plant fuel or steam generation. The two-compartment washer produced a premium anthracite product and a middlings product. The sharpness-of-separation values ranged from good to excellent for the five primary separations and for the secondary separation.

Jan 1, 1968

By W. S. Landers

This bulletin is a detailed study of low-temperature, entrained-bed carbonization of a Texas lignite. The lignite studied was from the Sandow strip mine and is representative of the Rockdale formation of the Wilcox formational group. Carbonization was conducted in a continuous entrained-bed reactor at several temperatures in the 8801 to 1,52°C F range, and at air-coal ratios it the 0 to 10.30 scf/lb range (moisture- and ash-free basis). Carbonization rates ranged from 97.1 to 410.0 lb/hr (as-received basis), At the higher air-to-coal ratios employed, all or most of the carbonization heat was provided by internal combustion with air in the reactor. At the lower air-to-coal ratios, parts of the heat for carbonization was supplied externally. It was demonstrated that the entrained-bed carbonization of lignite is a complex reaction and that several variables, of which carbonization temperature, air-to-lignite ratio, and the average size of lignite are important, act together to influence both the carbonization yields and the properties of the resultant products, Process variables established by pant tests were used to design the industrial scale carbonizer operated at Rockdale, Texas, by the Texas Power & Light Company as agents for the Aluminum Company of America. Properties of the carbonization product obtained from the industrial scale reactor were essentially the same as those obtained from the pilot plant reactor operated under the same conditions.

Jan 1, 1968

By Robert M. Becker

A multistage probability model for assessing the reliability of mineral samples following any number of stages of sample reduction is presented. Sample reduction is the process of alternately crushing or grinding and sampling mineral particles prior to assaying. The final multistage model developed accurately describes the ideal sample reduction practice. This model is based on previously developed and experimentally tested models for a single stage of sampling. The problem is approached through the probability distributions for the various stages of sampling. The probability distribution, moments, and moment relationships for a single stage of sampling are first reviewed, and the useful concept of unit moments is defined. In presenting the models for two stages of sampling, emphasis is placed on the physical description of the sample reduction process which leads quite naturally to its mathematical representation. In this representation, crushing or particle-size reduction between the stages of sampling is viewed as a random process with respect to the number and proportion of particles of the various kinds produced. The physical and mathematical description is extended to more than two stages of sample reduction, and the first three moments for any number of stages are developed. In common sample reduction practice the effects of a finite population (finite amount of material) at each stage of sampling appear to be important in describing the variance contribution of each stage. This is also true for the third moment about the mean. An example is cited in which the skewness increases by more than an order of magnitude when several stages of sampling are considered. This is largely due to the dependence of the multistage third moment about the mean on the variance. In general the model and results should be useful in helping to understand, control, and reduce the random errors that arise in the sample reduction process.

Jan 1, 1968

By R. V. Higgins

This paper describes a method and a computer program for calculating shape factors and areas of channels that turn more than 90° and conduct fluids into the backs of wells. The program represents an improvement over a previous Bureau of Mines investigation by using a 4-point Lagrange interpolation equation instead of a 3-point and by summing areas of trapezoids with either x altitudes or y altitudes. Some of the techniques reported in this paper can also be used to compute the areas between contours and the lengths of lines that turn more than 90°.

Jan 1, 1968

By J. O. Winget

Amino acids were investigated in conjunction with rare-earth separation by ion exchange to determine whether they can be utilized effectively as retaining agents for metals separation using ethylenediaminetetraacetic acid (EDTA) eluant at 85° to 90° C. Hydroxyethylethylenediaminetriacetic acid (REDTA) and diethylenetriamine pentaacetic acid (DTPA) were the most effective amino acids investigated. Elements of atomic numbers 39 and 57 through 68 were effectively retained, whereas elements of atomic numbers 69 through 71 passed through the retaining-agent band. Utilization of REDTA or DTPA retaining agents allows an increase of 75 percent in the EDTA eluant concentration over that possible with hydrogen-or copper-retaining ions without precipitation occurring. Eighty-five percent recovery of the EDTA eluant collected before rare-earth breakthrough and during elution of lutetium, ytterbium, and thulium, and essentially complete recovery of the REDTA or DTPA retaining agents, are possible without extensive processing.

Jan 1, 1968

By H. E. Powell

The magnetic susceptibility, the geographical source, and associated minerals are given for 44 copper-, 26 lead-, and 19 zinc-bearing minerals. Of the 44 copper minerals/ all had a susceptibility of less than 15 X 10-6 cgs, and about 20 percent of them were diamagnetic. Of the 26 lead minerals, all had a susceptibility of less than 11 X 10-5 cgs, and almost half of them were diamagnetic. And, of the 19 zinc minerals, all except four had a susceptibility of less than 9 X 10-6 cgs, and about one-fourth of them were diamagnetic.

Jan 1, 1968

By John Ward Smith

Oil-yield data are presented for core samples from Colorado Corehole No.1, drilled by the Bureau of Mines and the Atomic Energy Commission in a previously untested oil-shale area near the northern edge of Colorado's Piceance Creek Basin. Continuous oil shale 2068 feet thick, averaging 18.41 gallons of oil per ton of shale and representing 1.8 billion barrels of oil per square mile, occurs at the core site.

Jan 1, 1968