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By R. W. Freedman

The Bureau of Mines has developed a gas chromatographic method for the rapid and accurate determination of oxygen, nitrogen, carbon dioxide, methane, and, if present, carbon monoxide in mine air. This method replaces such presently used gas-reaction types as the Haldane or Orsat analysis, offering advantages in terms of precision, accuracy, speed, and convenience.

Jan 1, 1968

By Sabri Ergun

Previous studies of magnetic separation of pyrite from coals have been reviewed critically. Magnetic susceptibilities of United States coals of differing rank have been measured. The effects of crushing, magnetic mixing, drying, weathering, and heat treatment on the enhancement of the magnetism of pyrite have been analyzed. The importance of size distribution of pyrite in the coal and the necessity of crushing to liberate the pyrite has been discussed. It has been found that the inherent susceptibilities of the carbonaceous, mineral-free portions of coals (? -0.5 X 10-6 in cgs units) and of relatively pure pyrite isolated from coals (? -0.3 X 10-6) do not permit efficient separation of pyrite from coal; the average susceptibility of the magnetic fraction of coal must be raised to 3 X 10-6. Friction forces encountered in crushing sedimentary pyrite embedded in coal do not increase its susceptibility. Subsequent weathering or heat treatment below 400° C leads to the formation of iron sulfate and hence increases the effective paramagnetism of pyrite. Ferromagnetic compounds of iron are not formed in significant quantities at temperatures below 400° C. The degree of liberation and apparent susceptibility of pyrite are the most important parameters in its separation. It is concluded that effective beneficiation of coals can be achieved by magnetic separation. A sufficient increase in the susceptibility can be achieved by converting less than 0.1 percent of pyrite into ferromagnetic compounds of iron. Such conversions occur only at temperatures >500° C. An investigation of the dielectric properties of coals and pyrite in the frequency range 0.1 to 60 Mhz indicates that the imaginary dielectric constant of the pyrite is about 100 times larger than that of coal. Exploratory experiments indicate that pyrite can be selectively heated to temperatures above 500° C without appreciable rise in the temperature of coal. It appears that dielectric heating of coals in the Ghz frequency range is the most feasible method of enhancing the paramagnetism of pyrite.

Jan 1, 1968

By Karl C. Dean

The Bureau of Mines studied the precipitation of copper from dilute acidic sulfate solutions using shredded automobile scrap in a rotary drum. The tests established that the scrap in the rotary drum precipitated copper faster and more completely than shredded, detinned, tinplate scrap in a launder, with comparable iron consumption. Although power is required to rotate the drum, the faster precipitation and continuous recovery of cement copper are advantages of the tumbler method. Cost evaluation indicates that the rotary drum method, which uses relatively low-cost and readily available shredded automobile scrap, is competitive with the launder method, which uses relatively high-cost shredded tinplate scrap or detinned shredded cans.

Jan 1, 1968

By W. J. Wenger

Results of the analyses of 151 crude oils from 123 oilfields in the Williston basin are presented. Production statistics are compiled by geographical areas within the basin, by geological age of the producing zones, by States, and by field for the nine fields with the greatest production. Characteristics of the oils are tabulated, and correlations are included to show relationships between properties of the oils and some factors in the environment. Properties of the oils in some instances imply that there has been migration and mixing of the oils between productive formations of different geological time periods.

Jan 1, 1968

By R. F. Abernethy

A chemical method of determining microgram quantities of arsenic in coal was investigated by the Bureau of Mines to supplement a semiquantitative spectrographic method of determining arsenic in coal ash. In accordance with a method recommended by the International Organization for Standardization, 1-gram samples of coal are decomposed by wet oxidation with boiling sulfuric acid (H2S04) and nitric acid (HN03) to remove the organic matter. After heating to fumes of SO3 to remove HN03, the arsenic is separated as arsine by the action of zinc in H2S04 solution. The arsine is absorbed in dilute iodine solution in which the arsenic is determined colorimetrically by the molybdenum-blue reaction. Two modifications of the method for obtaining the arsenic in solution, in addition to the wet oxidation method, give satisfactory results. The modifications are (1) furnace ashing with MgO added to the coal, followed by treatment with H2S04, and (2) extraction of arsenic from the coal by dilute HNO3 without ashing. Float-and sink-tests show that arsenic is associated mainly with mineral matter in the three coals examined. High-temperature ashing tests show that very little arsenic is volatilized from coal ash below 1,000° C, but it is virtually all removed from the ash at 1,300° C.

Jan 1, 1968

By F. P. Haver

The Bureau of Mines developed a process to extract about 90 percent of the sulfur from molybdenite flotation concentrate by compacting the concentrate with one-quarter of its weight of aluminum powder, heating it at 800° C for 30 minutes, and then allowing the product to react with water. This thermite reduction yields an impure molybdenum alloy plus aluminum sulfide. The latter readily hydrolyzes, to yield pure hydrogen sulfide which can be converted to elemental sulfur by the Claus process. At least 95 percent of the molybdenum can be subsequently recovered as 99.95-percent-pure molybdic oxide.

Jan 1, 1968

By J. E. Murphy

Field freezing was used by the Bureau of Mines to effect the redistribution of the components in a cerium-12.5-atomic-percent-iron alloy. The application of the electric field caused the iron to migrate toward the anode. A field intensity of 0.04 v/cm and a current density of 240 amp/cm2 were used. The conditions that yielded the greatest redistribution of alloy components were a small thermal gradient along the specimen (from 5° C/cm to 10° C/cm) and a very slow freezing rate (0.15 cm/hr). Under these conditions it was possible to process specimens of ½ -inch diameter as compared with the capillary-size specimens used by most previous investigators.

Jan 1, 1968

By D. R. Forshey

The recent occurrence of fatal accidents in copper mines, presumably due to premature ignition of loaded holes by the heat from reacting ammonium nitrate-fuel oil (AN-FO) and pyrite-bearing ores, has led to an examination of this reaction. The reactivity of prilled AN-FO mixtures with pyrite-bearing ores and the effects of water, dilute sulfuric acid, and potential inhibitors on reactivity of the mixtures were evaluated. Initiation of an exothermic reaction was observed as low as 150° F with acid in the absence of inhibitors. Low concentrations of urea, calcium carbonate, zinc oxide, and magnesium oxide were effective in inhibiting the reactivity of the mixtures. The temperatures produced during the reaction of mixtures of AN-FO and pyrite-bearing ores, in the absence of inhibitors, always exceeded the temperature at which electric blasting caps are thermally initiated.

Jan 1, 1968

By Andrew J. Fergus

The purpose of this study was to provide basic information to aid further research on beryllium mineral flotation. Contact-angle and microflotation (Hallimond tube) methods were used to study collector action and flotation response of beryllium minerals and associated gangue minerals with representative commercial surfactants. Chrysoberyl received prime attention. Results indicated that selective flotation of beryl and chrysoberyl from fluorite and quartz is possible with sodium isooctyl phosphate below pH 2, and fluorite and topaz are readily collected by both anionic and cationic surfactants. Several modifying reagents were studied at one pH and one level of collector concentration. Aluminum sulfate, starch, and sodium silicate proved to be depressants in chrysoberyl flotation.

Jan 1, 1968

By Andrew J. Fergus

A study of the flotation characteristics of columbium-tantalum minerals was made by contact-angle and microflotation methods, and the findings were confirmed by flotation of two natural ores. In the contact-angle study conditions for collection of columbite, pyrochlore, and tantalite were determined for (1) sodium oleate with a sulfonate; (2) sodium isooctyl phosphate; (3) a short-chain primary amine; (4) a long-chain primary amine; and (5) a quaternary amine. These conditions were confirmed in microflotation tests. Information about collector action on common gangue minerals was also obtained by these two methods. In batch flotation tests on a pyrochlore ore and a columbite ore, it was demonstrated that collectors selected on the basis of contact-angle and micro-flotation studies would float columbium minerals from a complex natural ore. However, multiple cleaner and scavenger flotation steps will be necessary to produce commercial concentrates. From a pyrochlore ore containing 0.54 percent Cb2O5, a 44.4 percent Cb2O5 concentrate was made containing 36.4 percent of the total Cb2O5. For a columbite are the corresponding values were: 4.35, 54.6, and 67.1 percent. During the batch flotation study, wetting agents were found to aid in the gangue-ore mineral separations.

Jan 1, 1968

By E. A. Mihok

A pilot plant for treating mine drainage by neutralization with limestone was designed, fabricated, and operated by the Bureau of Mines. The process consists of (1) producing a very fine (minus 400-mesh) limestone slurry, (2) mixing the slurry with the mine water, (3) aerating the resulting mixture to remove carbon dioxide and precipitate iron, and (4) separating the solids from the liquid by sedimentation. A mine discharge of pH 2.8, containing 1,700 ppm total acidity, 36 ppm ferrous iron, and 360 ppm total iron, was treated at rates from 300 to 400 gpm. The treated water ultimately reached a pH of 7.4 and contained no detectable iron. The resulting sludge compacted to approximately one-third the volume of sludge from mine water neutralized with lime. The advantages of the limestone process, compared with the conventional lime process are as follows: Widespread distribution and lower cost of run-of-mine, indigenous limestone; simplicity of plant design; reduced hazards and plant operating and maintenance costs accruing from the use of a less reactive chemical agent; higher solids concentration of the precipitated sludge; and no deleterious effect caused by accidental overtreatment. While total process costs could not be determined, it is conservatively estimated that the cost of treating mine water by the limestone process is one-third to one-half the cost of the lime process, depending on the characteristics of the water to be treated and the availability and quality of limestone used.

Jan 1, 1968

By E. J. Kloos

Two self-contained breathing apparatus of the closed-circuit compressed-oxygen type were evaluated for performance at 32° to -25° F. Low-temperature effects of oxygen and carbon dioxide concentration, visual properties of the facepiece, and mechanical operation of the apparatus were studied. Although operation varied with the wearer, his breathing rate, the apparatus precooling time, and the temperature, results suggest that general use of currently approved compressed-oxygen closed-circuit breathing apparatus be limited to temperatures above 32° F.

Jan 1, 1968

By Joseph W. Martin

The Bureau of Mines investigated the backscattering of low-energy gamma rays as a method for rapidly determining the incombustible content of coal mine dust. In this method, 60-kev gamma rays from americium-24l penetrate the dust and are reflected by elements in the dust to a thin crystal scintillation detector. The number of backscattered gamma rays is proportional to the incombustible content. Tests of 40 dry, mine-dust samples containing 50 to 100 percent inert material show an average error of 2 percent. Calibration of the apparatus is necessary for each rock dust to account for variable composition. Results for samples containing more than 6 percent moisture are subject to error, but the values are lower than values obtained by chemical analysis, and thus fall on the safe side. Development of a small portable meter based on the backscatter principle appears feasible. Such a meter would find application within coal mines to check the effectiveness of rock dusting procedures.

Jan 1, 1968

By Robert L. de Beauchamp

The Bureau of Mines designed a chlorination apparatus to prepare CrCl2 free of CrCl3 by the direct reaction of chlorine and chromium. Equipment and procedures were developed for routine preparation of 25-pound batch quantities of anhydrous CrCl2. Calcium, iron, nickel, and silicon impurities were in the 0.01 to 0.05 percent range, and all other impurities were below 0.01 percent.

Jan 1, 1968

By R. W. Van Dolah

The feasibility of formulating cap-sensitive slurry explosives for use in underground mines with potentially flammable gas atmospheres was examined. Formulations containing aluminum metal as sensitizer and sodium chloride to reduce incendivity were prepared; some were cap-sensitive and had adequate air-gap. Flaked aluminum metal rather than the atomized type proved to be the more effective sensitizing agent of the formulations tested for incendivity in the large gallery of the Bureau of Mines, some were found to be suitably nonincendive.

Jan 1, 1968

By D. S. Burgess

The characteristics of gas-phase detonations were observed in 20 instrumented firings within earthen tunnels, in 100 such detonations in a 24-in-diam by l63-ft-long steel pipe, and in about 200 smaller scale firings. Most of the fuels studied were representative hydrocarbons--acetylene, propane, gasoline, and a roughly equimolar mixture of methylacetylene, propadiene, and propane. In a pipe with two closed ends, the detonable limits were demonstrated to be very nearly the same as reported limits of flammability. The side-on impulses (pressures integrated over 200-msec intervals) were shown to be the same function of concentration regardless of whether deflagration or detonation had occurred. In a pipe with only the initiation end closed, the impulses of all fuel-air systems tended toward the same level when averaged over comparable ranges of fuel concentration; the lower pressures with saturated hydrocarbons were nearly compensated by longer durations of pressure transient. In all fuel-air systems, unexpectedly high impulses were obtained with slightly lean mixtures. In earthen confining structures, the impulse, of the explosion was efficiently converted into momentum of the failing wall. In the configurations studied, an earth velocity of about 20 fps was critical to overcome the soil's resistance to shear. The destructive effect was determined by gas pressure rather than by total energy release. The assignment of a "TNT equivalent" to an explosive gas mixture is discussed in terms of the confinement of the mixture.

Jan 1, 1968

By Frank G. Schwartz

The Bureau of Mines developed a rapid test method for predicting the stability of motor gasoline during long-term storage. The amounts of gum and inorganic residue formed in 13 gasolines during a l6-hour oven test at 200° F were compared with the amounts formed in the same gasolines stored at 110° F, and analyzed following 8-, 16-, 32-, 44-, and 52-week storage periods. Satisfactory methods were developed for predicting gum and inorganic residue formation during fuel storage periods as long as 32 weeks at 110° F, the approximate equivalent of 5.7 years at 80° F. The only data required to apply the methods are the amount of gum and inorganic residue formed, and the amount of oxygen that reacted, during a l6-hour oven test. A direct relationship existed between inorganic residue formed during the oven test and during 110° F storage. Statistical treatment of the data showed predicted values were as reliable as determined values. By use of a modified Arrhenius equation, the 110° F storage time can be extrapolated to equivalent time at any temperature below 110° F. Thus by combining the stability prediction method with the mathematical extrapolation, the storage performance of motor gasoline for extended periods can be estimated at any temperature up to 110° F.

Jan 1, 1968

By David E. Nicholson

The Bureau of Mines has constructed a special compression chamber for developing stress-strain relationships of mine backfill and simulating the high compressive ground pressures encountered in underground mines. A one-dimensional, or Earth-Pressure-at-Rest model is proposed for backfills subjected to these pressures. Results of the compression tests performed in the chamber indicate that reliable stress-strain relationships can be developed from these tests. The primary objective of the test series was to evaluate the effectiveness of compaction of common backfills in retarding ground closure. Analysis of the stress-strain data shows an eightfold reduction in relative strain in optimum well-graded, compacted backfills over poorly graded, loose backfill material. Analysis of the one-dimensional compression test data also indicates a significant retardation of transmitted stress in dense compacted samples of backfill and natural sands. Although not fully understood, a deformation mechanism is thought to occur at the intergranular contacts in cyclic fashion causing frictional heat loss and a reduction in transmitted stresses in the densely packed materials. The experimental values of transmitted stress are compared with theoretical values of effective stress calculated from the one-dimensional compression relationships developed by Hendron (4).3 These experimental values of transmitted stress compare very closely with the theoretical values of effective stress.

Jan 1, 1968

By H. V. Makar

Laboratory tests were performed to obtain a quantitative description of the effectiveness of sodium sulfate (Na2SO4) for removing copper from molten iron and to determine the effectiveness of Na2SO4 on actual auto scrap. The tests were conducted on induction melted heats of iron averaging 0.58 and 1.50 percent initial copper and on cupola-melted auto scrap containing 0.45 percent initial copper. The Na2SO4 was added in powder form in amounts ranging from 2.9 to 43.8 percent of the weight of iron being treated. The data showed that copper removal for the various Na2SO4 treatments followed a similar trend, regardless of the iron composition that was tested. The equation Y = 1 - e-3.23x approximately reflects the relationship between copper removal and amount of Na2SO4 added, where Y is the fraction of copper removed and x is the ratio of the weight of Na2SO4 added to the weight of metal treated. Copper removals ranged from 3.3 to 74.5 percent and reductions down to less than 0.10 percent final copper were achieved in the auto scrap. Copper removals were generally accompanied by sulfur removal, and initial sulfur contents ranging from 0.10 to 0.20 percent were reduced to as low as 0.02 percent. High temperatures and long slag reaction times tended to induce copper and sulfur reversion from the slag, but, generally, the Na2SO4 treat¬ments were effective up to approximately 2,820° F with reaction times not exceeding 7 minutes.

Jan 1, 1968

By Wilbur I. Duvall

The Bureau of Mines presents a theoretical solution for the stresses and displacements in an infinite elastic plate containing a circular hole whose boundary is subjected to applied shear loads over four separated arcs. The results for the applied shear loads can be superimposed on the results for applied radial loads, given in a previous publication, to obtain a complete two-dimensional approximation of the stresses and displacements induced in the rock by tunnel boring machines anchored in a circular tunnel by means of four props. Analysis of the various solutions shows that the tangential tensile stresses induced on the boundary of the circular tunnel by applied radial loads can be minimized in the roof and floor of the tunnel by the application of appropriate shear loads to each of the four props. Thus when planning tunnel boring operations, consideration should be given to the in situ stress field in the rock and the induced stresses in the rock resulting from the applied radial and shear loads produced by the props of the boring machine.

Jan 1, 1968