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By A. S. Peck

This report presents the results of a cooperative study between the Bureau of Mines and the University of Utah to define the mechanism involved in the adsorption of oleic acid and sodium oleate on fluorite, calcite, and barite, using an infrared spectrophotometer for identifying and measuring the adsorbed reagents and reaction products. Fluorite, calcite, and barite react with oleic acid and sodium oleate in a water system, forming chemisorbed and solution products. The chemisorbed species is a surface mineral cation-collector anion salt, Chemical analysis of solution resulting from the adsorption reaction indicates that the adsorption process causes displacement of mineral anions, namely, fluoride, carbon ate, and sulfate from the surface of these minerals.

Jan 1, 1963

By C. M. Mason

Bureau of Mines studies were made on the sensitivity of several ammonium nitrate-fuel oil (AN-FO) mixtures to bullet impact. The experimental work was done with one military rifle and two high-velocity sporting rifles with a variety of ammunition. For the three rifles used, the order of efficiency in initiating detonation in AN-FO mixtures was 220 Swift >300 Weatherby Magnum >30-&apos;06. The velocity of the bullet was found to be a decisive factor in the initiation. The sensitivity of various materials studied increased as follows: Clay-coated prills with 4 percent oil <fresh surfactant-coated prills with 4 or 6 percent oil <surfactant-coated prills with 4 or 6 percent oil and aged 270 days <crushed prills with 6 percent oil <very low-density, surfactant-coated prills (micronized), with 4 percent oil.

Jan 1, 1963

By George H. Johnson

This report describes the procedures and summarizes the results of an investigation of surface subsidence above caving blocks at the San Manuel mine, San Manuel, Ariz., in order to obtain quantitative information on subsidence and ground movement caused by mining large volumes of ore. This investigation is one part of an overall study of rock mechanics being undertaken by the Bureau of Mines. Attention was given to the improvement of a rapid and precise method of surveying a large number of subsidence pins and cracks in the surface terrain. Photogrammetric methods were used as an adjunct to the triangulation subsidence surveying as well as in ordinary topographic work Maps of various kinds were prepared to show the results obtained. The computation of the survey notes was programed for an electronic digital computer at a saving of time and expense over the use of a desk calculator and trigonometric tables.

Jan 1, 1963

By A. C. Rice

Aminopolyacetic acid chelating agents were added to separatory-funnel-scale solvent-extraction systems to determine the effect on separating rare-earth elements. Average values for separation factors between adjacent elements obtained with Primene JM-T2 increase 36 percent when EDTA is added to the aqueous phase. Adding HEDTA or DCTA also improves separation factors for certain rare-earth elements. Percentage of extraction and the separation factors exhibit marked sensitivity to concentrations of amine, chelating agent, and hydrogen ion. The chelating agents improved separation in Primene JM-T, BHDA, and Primene 81-R extraction systems.

Jan 1, 1963

By W. T. Benson

The nickel-bearing laterite deposits in the Pine Flat and Diamond Flat areas, Del Norte County, Calif., were investigated by the Bureau of Mines to determine the extent and nickel content of the two deposits and the amenability of the ores to metallurgical treatment. The work was based on drill-hole sampling and metallurgical tests in which attrition scrubbing and sizing, reduction roasting, and magnetic separation were used. Results of the sampling indicated that the deposits are comparatively small and are marginal or submarginal in grade. Metallurgical tests showed that no separation of cobalt from nickel and iron was made by sizing; however, a large portion of the chromium was separated. Reduction roasting and magnetic separation did result in upgrading the iron, nickel, and cobalt, and the simultaneous rejection of chromium.

Jan 1, 1963

By F. C. Gibson

An electrical method for the continuous determination of propagation velocities in opaque, confined explosives, and propellants is described. A resistance element imbedded in the reactive material generates electrical signals that are displayed oscillographically and indicate the position and progress of a reactive zone associated with progress of a reactive zone associated with burning or detonation. The method is applicable to both solids and liquids.

Jan 1, 1963

By E. C. Pattee

A mobile spectroscopic laboratory was completed by the Bureau of Mines in 195 to provide a rapid, inexpensive means of field testing samples for beryl¬lium and other associated metals of possible commercial importance. Spectro-copes have been used in laboratories for many years in various types of research and routine analyses, but this spectroscope is probably the first mobile unit. The laboratory provides for spectroscopic, radioactivity, fluorescent, and limited chemical tests of samples. The unit has been a valuable reconnaissance tool. It has been used to search for beryllium, cesium, columbium, tantalum, rubidium, and lithium in Idaho, Washington, and Montana. Several very low grade deposits of these elements were found, and occurrences of other important elements were identified; however, none are of economic importance. The spectroscope permits the detection of elements by analysis of visible light produced when elements in a small powdered sample are volatilized in an electric arc., A total of 70 elements can be detected; 29 can be detected at or below 0.01 percent, Electric power for the arc is supplied by a gasoline motor-driven generator, Equipment is housed in an aluminum van, mounted on a 4-wheel-drive vehicle for easy maneuverability on mountain roads, A trailer with crushing, pulverizing, and splitting equipment permits the reduction of samples to a small representative pulp.

Jan 1, 1963

By B. K. Shibler

A highly flexible laboratory-scale fluidized-bed reactor was designed, constructed, and successfully operated continuously at temperatures up to 1,300° C during an investigation of thermal methods for decomposing gypsum. This report discusses briefly the many problems encountered in developing the 10-inch-diameter reactor and describes its design and construction in sufficient detail to enable other research organizations to build a comparable unit. The reactor consists of a 10-inch-inside-diameter vertical tube which can be varied from 6 to 10 feet high; it is formed from 2-and 3-foot sections of silicon carbide pipe. The tube is surrounded by a 3-inch heating space formed by an outer 4.5-inch-thick circular wall of insulating firebrick. A cone-shaped fluidizing chamber is bolted to the bottom of the reactor. Fluidizing gas enters through the bottom of the cone, and ore is introduced by means of a screw feeder connected to an inlet located just above the gas port. A silicon carbide overflow tube of 1.25-inch inside diameter extends upward into the reactor. The depth of the bed is controlled by substituting different lengths of overflow tube. Twin dust-recovery systems, each composed of a cyclone and Fiberglas filter, are attached to two gas outlets at the top of the reactor tube. The reactor is designed for research on both exothermic and highly endothermic reactions. It can be fired externally by means of four natural gas burners that jet tangentially into the annular space at the base of the reactor. Alternatively, it can be fired internally, using a mixture of air or oxygen and natural gas as the fluidizing medium. A separate instrument panel contains flowmeters, manometers, an automatic program controller, and a multiple-point recorder for printing a record of the temperatures measured by thermocouples located at critical points in the reactor.

Jan 1, 1963

By Hal J. Kelly

A number of problems that developed in processing the halloysitic clays of eastern Washington and northern Idaho were investigated by the Bureau of Mines. The deflocculating effect of tetra sodium pyrophosphate is compared with several other compounds, and on the basis of current theory, the advantage of sodium pyrophosphate as a deflocculating agent is explained. The adsorption of the sodium ion by clay in a clay"-water system was established by a radioactive tracer technique, and the deflocculating action of sodium pyro- phosphate was postulated. The effective dispersion of the halloysitic clays was limited by the occurrence of tightly bound aggregates of small, individual crystals. Disaggregation of the agglomerates was investigated by liquid extrusion and ball milling of dilute slurries and by extrusion of the clay in a plastic state. The greatest increase in the production of small particles was by high? pressure liquid extrusion.

Jan 1, 1963

By F. D. Stevenson

A metal diaphragm pressure relay system was constructed to measure vapor pressures of the metal halides, oxyhalides, and other substances at temperatures up to 700° or 800° C. The vapor pressure of arsenic (III) oxide (As2O3) was determined to verify the reliability of the apparatus for such measurements. The data for the liquid AS2 Os (2820 to 4830 C) are represented by the equation, log Pmm = 6.875 - 2,929/T, from which the normal boiling point was calculated to be 461° C. The heat of vaporization calculated from this equation was 13.40 ±0.09 kcal/g mole As4OS and is essentially constant over the interval studied. The melting point of the octahedral arsenic (III) oxide was determined to be 278° C from the inter-section of the solid and liquid vapor pressure curves, A thermal analysis apparatus is also described by which melting and transition temperatures could be checked by a method independent of vapor pressure data. The melting points of the monoclinic and octahedral forms were determined to be 314.4 ±1.4° C and 278 ±5° C, respectively.

Jan 1, 1963

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 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&apos;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 John J. Mulligan

The Bureau of Mines investigated coal deposits at Mount Gran (latitude 76°59&apos; S, longitude 161°07&apos; 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 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