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By P. A. Bloom

Bureau of Mines research was conducted to develop effective separation methods that might be used in exploiting substantial tonnages of complex barite-fluorspar ores in Arizona. The exploitable reserves now may be increased as recent batch and continuous flotation tests demonstrated that a complex barite?-fluorspar ore from the Red Chief deposit, Yuma County, Ariz., could be selectively treated to concurrently produce (1) fluorspar and (2) a barite byproduct of marketable grade. The sample contained 24.8 percent CaF2 and 24.3 percent BaS04. Processing comprised production of a fluorspar product containing 97 percent CaF2 with an 82 percent recovery, using a sodium fluoride-lignin sulfonate-fatty acid reagent combination. Concurrent retreatment of the fluorspar tailing, using sodium cetyl sulfate as a collector, yielded a barite product of 94 percent BaS04 grade with a 71-percent recovery. The products met specifications for acid-grade fluorspar and drilling mud-type barite.

Jan 1, 1963

By Robert V. Berryhill

Reconnaissance studies of beach deposits along approximately 220 miles of the shoreline of Bristol Bay, Alaska, were made to determine if more detailed investigations were warranted. In addition to preliminary mapping of the deposits, samples were obtained from auger borings spaced at 1-mile intervals in key areas; shovel samples were collected to supplement the borings. Most samples were roughly concentrated in the field; magnetic separation tests, petrographic analyses, and determinations for radiometric equivalent uranium, gold, platinum, iron, and titanium were made in the Bureau of Mines laboratory at Juneau, Alaska. Spot samples from some beaches along the shores of the Alaska Peninsula indicate small deposits containing up to 10 percent recoverable titaniferous magnetite; some larger deposits were indicated to contain from 1 to 2 percent total heavy metal, principally as titaniferous magnetite. Significant amounts of other commercial minerals were not detected.

Jan 1, 1963

By W. A. McKinney

Bureau of Mines Research has demonstrated that it is technically feasible to segregate oxidized copper ores by use of a direct-fired, refractory-lined rotary kiln. Previously, the segregation process had been effected only in much more complicated indirect-fired, stainless steel kilns, The method comprises heating crushed ore premixed with small quantities of salt and carbonaceous material, such as coke, to about 830° C to produce copper as fine flake and metallic films on the surface of the coke particles. After grinding of the cooled furnace calcines, the copper is recovered by conventional flotation. During direct-fired segregation it was necessary to closely control the air-gas mixture in the burner. Good copper recoveries were obtained only when adding air in the limited range of 1.15 to 1.2 times the theoretical amount required for combustion of the natural gas. Batch trials of the new technique on quartzite-, limestone-, sandstone-, and limonite-type oxidized copper ores containing from 1.4 to 6.2 percent copper yielded flotation concentrates containing from 3.7 to 45 percent copper, representing 84 to 95 percent recoveries. Analyses of the furnace gases showed that loss of copper by volatilization was negligible. The preliminary direct-firing segregation studies were complemented by continuous runs on the quartzite ore, containing 1.4 percent copper, in an integrated segregation-flotation pilot plant having a 60 pound-per-hour capacity. In a typical test, 84 percent of the copper was recovered in a cleaner flotation product containing 25 percent copper. The study will be continued to further delineate the conditions for good segregation as effective use of standard ceramic-lined kilns will render the process more attractive from a commercial standpoint.

Jan 1, 1963

By Scott W. Hazen

This Bureau of Mines report presents the results of a study and statistical analysis of part of the initial exploration churn-drill sampling and some of the subsequent underground diamond-drill-core sampling in the North are body at the San Manuel copper mine, Arizona. These data were derived from regular exploration and mine sampling, not from special samples obtained solely for statistical analysis. The study was conducted as part of the Bureau's continuing program on sampling-methods research. The major objective of the study was to investigate the feasibility of using the techniques of statistical analysis in evaluating sample and assay data and computing grade and tonnage of Ore from porphyry-type copper deposits. It was recognized that using existing data acquired over a period of several years by different methods would introduce problems and limitations for precise comparisons. However, it was expected that the study would provide some general conclusions and certainly a number of preliminary conclusions on the nature of the mineral characteristics and their effect on sampling procedures, the requirements for sampling deposits of this type, and the comparative results of churn-and diamond-drill sampling in the same area of the deposit. All of this information would be essential for future sampling-methods research for computing grade and tonnage of ore.

Jan 1, 1963

By J. P. Morris

An experimental blast furnace in normal operation was quenched by substituting cold nitrogen for the hot blast air. More than 2,200 samples from the stack, bosh, and hearth were taken; 500 of these were selected for detailed analysis. Deductions are made as to the patterns of burden movement and gas flow; the reduction of iron oxides, including a comparison of ore and sinter; and the behavior of sulfur above the smelting zone. Metal and slag beads from the bosh were analyzed, as were samples from the hearth metal and slag. A brief description of a petrographic examination of the quenched burden is included.

Jan 1, 1963

By John J. Mulligan

The Bureau of Mines investigated coal deposits at Mount Gran (latitude 76°59' S, longitude 161°07' E), Victoria Land, Antarctica, during the austral summer of 1959-60 as part of the continuing U.S. Antarctic Research Program, which is under the auspices of the National Science Foundation. The coals and associated rocks were measured, sampled, and analyzed. Five coalbeds, ranging in thickness from over 10 feet to scattered fragments of coaly material in sandstone, occur in a sandstone-coal series overlying a series of crossbedded red-buff sandstones. Both series are part of the Beacon group of sediments, and both show some evidence of pressure metamorphism. The sandstones are poorly cemented and are composed dominantly of rounded and often frosted quartz grains. The sediments have been broken and uplifted by a series of massive diabase sills. The broken nature of the sediments precluded an estimate of the amount of coal present. The Mount Gran coals are highly attrital banded anthracites and semianthracites that have most commonly a moderately dull luster but do include bright bands. Coal in contact with or near diabase intrusives is partly graphitic but shows no evidence of coking. Apparently the coal was beyond coking rank before emplacement of the adjacent intrusives. Fragments of the plant Glossopteris indica found with the coal suggest Permian age but do not prove it. The coals appear to be derived from plant remains that collected in shallow basins; individual coalbeds would tend to be lenticular bodies that formed in different places as the dominantly sandy sediments were deposited. The wide distribution of coal indicates that coal-forming conditions prevailed over much of the continent; the great thickness of Beacon sediments indicates that similar conditions may have persisted through a long period of geologic time. Generally similar coal deposits may occupy widely separated stratigraphic positions.

Jan 1, 1963

By R. S. McClain

Continuous-circuit flotation and batch-scale precipitation tests were made by the Bureau of Nines to determine rejection of carbon and recovery of fluorine and aluminum compounds from aluminum reduction plant residues, About 40 to 60 pounds each of aluminum fluoride and cryolite are lost for each ton of aluminum produced. Gasoline and turpentine were satisfactory for floating carbon from both fresh water and saturated solution systems. Soluble fluorine and aluminum compounds were recovered by precipitation with sodium aluminate and carbon dioxide. Over 99 percent of the carbon was removed by flotation. Fluorine and aluminum recoveries up to 77 and 63 percent, respectively, were obtained in a combined precipitate and nonfloat product, In the fresh water system the combined product was mostly cryolite with some gibbsite. In the saturated solution system the product was mostly sodium fluoride, some cryolite, and minor amounts of gibbsite.

Jan 1, 1963

By John K. Alley

Fibrous silicon carbide was produced by thermal decomposition of certain silicates contained in graphite crucibles. Induction heating was used to produce the necessary temperature and thermal gradients. Both green and white fibers were mainly the beta modification even though each color grew within a different temperature zone. Alpha silicon carbide, present in insufficient amounts for X-ray detection, was identified by electron diffraction. The white fibers formed in a zone between 1,365° and 1,634° C (±50° C). The green fibers (less contaminated) formed in a much more narrow zone between 1,650° and 1,672° C (±50° C). The average lengths and widths of microscopic fibers grown by this method were 1.5 mm/0.002 mm (white) and 1.2 mm/0.0035 mm (green); however, same fibers observed by electron microscope had cross-sectional measurements of 150 to 300 A. Both differential thermal analysis and thermogravimetric analysis showed that silicon carbide fibers oxidized in air at temperatures above 500° C. Fibrous silicon carbide was indexed as a cubic cell with the dimensions a = 4.358 A. The density calculated from X-ray data was 3.217 g/cm3.

Jan 1, 1963

By Allan F. Smith

The influence of hydraulic fluids on spontaneous heating in bituminous coals is determined by measurement of the temperature increases produced in coal-fluid mixtures heated to a temperature sufficient for the initiation of self-heating. Similar tests on as-received coal samples and water-coal mixtures are compared with the results obtained for the various hydraulic fluids. Three of the four coals were sampled from coalbeds known to have a history of spontaneous heating. The data provide a basis for predicting the possible effects in gob or carbonaceous refuse of coal mines.

Jan 1, 1963

By John S. Berber

Bureau of Mines research on the production of phthalic anhydride by vapor phase oxidation of hydrocarbons began at Morgantown, W. Va., in October 1960. For these preliminary studies, a known solution containing naphthalene and 1-methylnaphthalene was used. In another series of tests, pure naphthalene was dissolved in different solvents. A series of investigations was conducted with the neutral oil fraction (210° to 270° C) of a low-temperature tar obtained from the Texas Power and Light Company's low-temperature carbonization unit. The neutral oil fraction was first dealkylated, and then the product was distilled into 210° to 250° C and 250° to 270° C fractions. These two fractions were then subjected to catalytic vapor phase oxidation. Although a number of catalysts was tested, most of the experiments were made using 9 percent vanadium pentoxide on inert alumina. The activity of this catalyst did not decrease after 162 hours at 1,030° F. Studies were conducted over a temperature range from 610° to 1,180° F. An operating temperature of 1,030° F yielded 47.50 percent of phthalic anhydride from a synthetic mixture of naphthalene and 1-methylnaphthalene. The highest yield (84.40 percent phthalic anhydride) was obtained with naphthalene dissolved in toluene and also with naphthalene dissolved in methyl ethyl ketone. With a 210° to 250° C fraction the highest yield of phthalic anhydride obtained was 12.32 percent at a temperature of 900° F, and, with a 250° to 270° C fraction, it was 15.80 percent at a temperature of 875° F.

Jan 1, 1963

By James S. Browning

Recovery of fine mica from a sample of impounded tailing from the Dixie Mines, Inc., crushing and screening operations, Heflin, Ala., was investigated to determine if plant losses of mica could be reduced while econmically producing a commercially acceptable mica concentrate. Conventional wet-tabling and agglomerate-tabling methods yielded concentrates assaying about 95 percent mica from the tailing that contained 17 percent mica. Products containing about 98 percent mica and accounting for mica recoveries of 86 percent were obtained by flotation, using as reagents sulfuric acid, kerosene, and coco amine acetate (a mixture consisting chiefly of dodecyl and tetradecyl amine acetates). The results of the batch flotation tests were verified by tests in a small continuous flotation pilot plant.

Jan 1, 1963

By H. E. Powell

A laboratory investigation was conducted by the Bureau of Mines to study the magnetic characteristics and to measure the magnetic susceptibility of the mineral siderite. All susceptibility measurements were made by the method of Gouy on powdered samples and at room temperature. Specific susceptibilities of samples from 15 different locations, domestic and foreign, were determined. Values ranged from 66 to 103 (10-6) cgs electromagnetic units. The relation of susceptibility to mineral composition is discussed in this report. The specific susceptibilities of 76 minerals are tabulated in an appendix.

Jan 1, 1963

By F. B. Petermann

Two-stage electric smelting tests, using small submerged arc furnaces, were made on high-iron manganiferous materials from the Pioche District, Nev., and the Cuyuna Range, Minn. The object was to reduce sufficient iron in the first stage to give a slag with a favorable Mn to Fe ratio for smelting to ferromanganese in the second stage. The nodulized flotation concentrate from the Pioche District contained 29.2 percent Mn and had a Mn to Fe ratio of 2.3:l. When smelted with coke and silica or alumina as flux, more than 90 percent of the manganese was recovered in slags with Mn to Fe ratios of 10: :24:1. The Pioche slag was smelted to ferromanganese using coke and lime- stone or dolomite as flux. The ferromanganese was high in silicon but other- wise met specifications. Recovery of manganese to ferromanganese in this step was 73 to 78 percent. Overall recovery of manganese was about 70 percent. The sintered flotation concentrate from the Cuyuna Range material contained 12.9 percent Mn and had a Mn to Fe ratio of 0.3:1. When smelted with limestone as flux, about 83 percent of the manganese was recovered in a slag with a Mn to Fe ratio of about 6:1. The Cuyuna slag was smelted to ferromanganese with coke and limestone for flux. Recovery in this step was 61 percent of the manganese in a high silicon ferromanganese. Overall recovery of manganese was about 50 percent.

Jan 1, 1963

By D. G. Kesterke

The electrolytic reduction of uranium dioxide to molten uranium in fluoride baths at approximately 1,200° C was demonstrated. Electrolyte constituents were BaF2, UF4, and either MgF2 or LiF. Preliminary laboratory-scale experiments were made in which the uranium oxide was added continuously for 3 to 5 hours to the cell during electrolysis. Over 1,000 grams of metal of 99-8 percent purity was made in some tests, Major impurities were aluminum, barium, iron, silicon, carbon, and oxygen. The effects of cell design, geometry, and bath composition were investigated. Electrode arrangement was the most important factor in cell performance.

Jan 1, 1963

By Albert W. Deurbrouck

This report describes the preparation characteristics of the significant, presently producing coalbeds in Mercer County, W. Va. Approximately 650,000 tons of coal was produced in Mercer County, W. Va., in 1960, of which over 630,000 tons was cleaned in four preparation plants. In 1960 the Pocahontas Nos. 3, 6, and 11 coalbeds supplied 99.5 percent of the total coal mined in the county. Because the number of working mines In this county was small, only six samples were collected; four of which were of metallurgical quality as mined. The remaining two samples could be upgraded by washing at suitable specific gravities. Many of the samples taken were of metallurgical quality as mined; however, the float-and-sink analysis on these coals has been included to point out their amenability to the production of premium quality, special purpose coals. In general the coals were low-volatile bituminous in rank with low ash and sulfur contents.

Jan 1, 1963

By John L. Miller

The synthetic fluormicas may be divided on the basis of silicon content into tetrasilicic, trisilicic, and disilicic. Properties of lead and barium disilicic fluormicas were determined to characterize these two representative members of the disilicic group. Properties described include unit-cell parameters from X-ray diffraction, optical data, chemical composition, density, melting point, and mechanical and dielectric properties. Both the lead and the barium micas were typically monoclinic; neither was sufficiently cleavable to yield usable mica splittings. Both yielded polycrystalline, machinable ceramics with excellent mechanical and dielectric properties.

Jan 1, 1963

By Frank A. Peters

A series of evaluations is being made to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. These evaluations include the estimated operating and capital costs as well as recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The three processes considered in this evaluation are designed to leach alumina as aluminum sulfate from calcined clay with sulfuric acid and to remove the silica residue by filtration. The filtrate from leaching is then purified by one of the following methods: Removal of iron in electrolytic cells using mercury cathodes; removal of iron by chemical precipitation through the formation of an iron-manganese complex; or precipitation of the alumina from an aqueous-ethanol solution, leaving iron in solution. Both the operating and capital costs for these processes are higher than those for the Bayer process. For plants producing 1,000 tons of alumina a day, the estimated operating costs per ton of alumina are: Electrolytic iron-removal process........... $81.35 Chemical iron-.removal process............... 82.08 Ethanol purification process............... 86.17 The investment in mercury is not part of the operating cost since this cost is considered equivalent to catalyst cost which would not be shown. The estimated capital investments for 1,000- ton-per- day plants on a Marshall and Stevens chemical equipment index basis of 240.0 are: Electrolytic iron-removal process...... $116,775,500 Chemical iron-removal process............... 99,418,900 Ethanol purification process................ 94,210,200 These investments include the working capital but not the land for each of the processes. Included in the electrolytic iron-removal process is an investment of $4,859,400 for mercury. Investigation of other methods for removing iron, of the decomposition operation, and of the leaching operation could reduce these costs.

Jan 1, 1963

By L. W. Higley

Procedures were developed for reclaiming high-temperature alloy scrap in the form of standard cobalt-base alloy. A cobalt-base, multicomponent, high- temperature alloy, such as S-816, can be successfully melted from scrap, and its specified chemical composition can be retained. Induction furnace melting in a controlled atmosphere was used to obtain ingots that were subsequently fabricated by impact forging to provide specimens for heat treatment and testing. Of the numerous metal elements in S-816 alloy, only small quantities of molybdenum were lost in the melting operation as finally developed. Test results indicated that the scrap material, after melting, forging, and heat treatment, was equivalent in room-temperature tensile strength, in high-temperature creep and stress-rupture properties, and in chemical composition to commercially produced S-816 alloy made from virgin material.

Jan 1, 1963

By Robert M. Doerr

Isothermal oxidation kinetics were determined for three grades of Ni and for 99.99 percent Co in Ca and in air from 800° to 1,200° C. The oxidation reactions followed approximately the parabolic rate law. For 99.99 percent Ni in 02 at 1,200° C, the parabolic rate constant was 2 mg cm-2 hr-2. For 99.99 percent Co in dry air, the constant ranged from 1 mg cm-2 hr-2 at 800° C to 18 mg cm-2 hr-2 at 1,200° C; for 99.99 percent Co in 02 the constant was 2 mg cm -2 hr-2 at 800° C and 10 mg cm-2 hr-2 at 1,000° C. For 99 percent Ni in dry air, the constant ranged from 0.2 mg cm 2 hr-2 at 800° C to 3 mg cm 2 hr-2 at 1,200° C. By X-ray diffraction measurements, only divalent oxides were found in the scales. Volumetric and quartz-helix gravimetric methods were used. The volumetric apparatus was designed to permit less stringent restrictions on the corrosion specimens; it was also more convenient to use. The agreement between the weight gain determined gravimetrically and the 02 consumption determined volumetrically was not good enough for direct comparison of gravimetric and volumetric results.

Jan 1, 1963

By S. J. Hussey

This Bureau of Mines report presents a discussion of the statistical approach to the design of experiments and indicates, by concrete examples, how and when statistical design is essential for obtaining meaningful data with a minimum number of experiments. Every research worker plans his work and designs his experiments in a manner which, based on his experience, seems most rational to him and which he believes will produce the information essential for resolving the problems. If the results obtained are open to multiple interpretations and are not of definitive reliability, the failure of the experiment design to produce the desired information may be due to several causes, These include faulty judgment in selecting the factors to be tested, ignoring the importance of interaction between factors, failure to adequately control test variables, and assuming that meaningful trends in the results can be identified without comparison to a predetermined experimental error. An experienced researcher probably will deduce from the nature of the data obtained that the design is faulty and may by trial and error ultimately arrive at the correct solution to the problem. Statistical methods of planning research minimize the chance of faulty experiment design, embody concrete procedures for testing the validity and reliability of the test data and for indicating mandatory changes in the design, and enable the researcher to obtain meaningful information with the least number of tests.

Jan 1, 1963