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By Martin Hertzberg

The concept of limit burning velocities, formulated in an earlier Bureau of Mines report (RI 8127), is applied to the problem of flame propagation through tubes of finite size. The limit burning velocity for conductive-convective wall-loss quenching (process b) is (Su)b = [aPe,] where the proper choice of critical Peclet constant, Pe, is determined mainly by the ratio of contact-perimeter loss area to flame-zone cross sectional area. This ratio of loss area to propagation area relates to the shape of the flame front and its control by buoyancy and by boundary conditions. The comparison of (Su)b with previously defined limit velocities for systems mixed by natural convection allows one to assess the influence of tube dimensions and boundary constraints on the "true" or earthly limits for the three directions of propagation. The flame quenching caused by inert powders is shown to be similarly described in terms of a limit burning velocity, (Su)?b. The tube's surface-to-volume ratio (~1/ro) is simply replaced by the powder's surface area per unit volume of the flammable mixture. Thermal loss quenching by these "internal walls" occurs at a critical Peclet constant somewhat higher than that observed for tubes, and the problem is complicated by the finite heat capacities of the powders and particle lag effects in the flame front.

Jan 1, 1980

By J. S. Dunning

One Federal Bureau of Mines research goal, to minimize requirements for domestically scarce mineral commodities through conservation and substitution, can be accomplished by utilizing more abundant elements such as iron, molybdenum, and titanium. An example of this research is the study of precipitation-hardening, iron-base alloys containing molybdenum and titanium, as substitutes for the high-tonnage stainless steels that are high in imported nickel and chromium. The precipitation hardened iron-base alloys are strengthened by a dispersion of the ternary Laves phase, Fe2 (Mo, Ti). Aluminum and chromium additions changed the solid solubility limits of molybdenum and titanium in a-iron and affected the composition of precipitating phases. A baseline composition of Fe-7Mo-2Ti was selected to study the effects of aluminum and chromium additions on the precipitation-hardening mechanism and microstructure and was also used in studies of mechanical properties and oxidation resistance. The study yielded workable, precipitation-hardening alloys, with elevated temperature strengths equivalent to or superior to types 304 and 316 stainless steels. Chromium and aluminum additions in combination were more effective in providing oxidation resistance than either addition was alone.

Jan 1, 1980

By H. O. McDonald

Solutions containing Cr6+ and sulfuric acid are used in a number of surface-finishing operations. Substantial quantities of chromium and copper are lost and pollution problems are created when the spent solutions are discarded. To minimize the undesirable environmental effects while improving secondary resource recovery technology, the Bureau of Mines is conducting research to detoxify and recover metals from these solutions. Spent etchants are treated to remove copper and reduce Cr6+ to Cr 3+ in an electrolytic cell. The anodes and cathodes are granulated coke. The spent solution is continuously pumped through the electrodes. Hexavalent chromium is reduced to trivalent chromium, and copper is recovered at the cathode. Reoxidation of Cr3+ at the anode was not observed. The removal and recovery of copper reduction of Cr6+ lessen chemical demand and increase efficiency in waste in treatment operations associated with the use of these solutions.

Jan 1, 1980

By J. M. Kuchta

The chemical and thermal criteria used for predicting the spontaneous combustion hazard are briefly reviewed and data are presented to characterize the gas desorptions and self-heating tendencies of 29 U.S. coals. Closed vessel desorption experiments showed that CO, CO2, and CH4 are the main gases evolved and that the CO, CO/?O2 index, and 02 absorption rate increase with decreasing rank and increasing oxygen content of the coal. In this Bureau of Mines report, the effects of temperature, moisture, and other variables are discussed together with the application of the data to the complex conditions encountered in a mining environment. An important finding is that the presence of CO alone in a mine is not necessarily an indication of a self-heating reaction of the coal. Based upon experiments conducted in an adiabatic-type calorimeter, the self-heating temperatures of lignite and subbituminous coals can be as low as 30° C, whereas the bituminous coals require a temperature of about 60° C or more. The self-heating hazard is greatest when the coals are dried and exposed to a high humidity condition, apparently as a result of the "heat-of-wetting." Generally, the hazard is greatest with the western coals of the United States.

Jan 1, 1980

By W. H. Eddy

The Bureau of Mines used several laboratory batch flotation schemes combined with magnetic separation to investigate the feasibility of recovering potash feldspar and glass sands from molybdenite tailings. Four molybdenite tailings or prospective tailings were used as test samples. Feldspar concentrates containing from 10.7 pct to 12.0 pct K2O were recovered from three of the four samples. The alkali content of the fourth sample met the grade for a mixed feldspar. All the feldspar concentrates contained iron in excess of the 0.10-pct-Fe203 specification for most uses. Electron-beam microprobe examination of the feldspar concentrates showed the presence of an iron-bearing potash feldspar in quantities that were excessive with respect to most iron specifications. However, a high-quality glass sand was produced from all of the samples.

Jan 1, 1980

By J. A. Eisele

The Bureau of Mines conducted bench-scale cyclic tests to determine the composition of recycled leach liquor in the Bureau?s proposed clay/HCl leach/ HCl sparge process for producing Al203 from clay. The data developed from these tests make it possible to synthesize leach liquors for predetermined steady-state operating conditions when conducting large-scale crystallization tests. The results of two sparge tests were compared. One was a 20-cycle test with a 36-pct-HCl concentration in the mother liquor; the other was a 10-cycle test with a 26-pct-HCl concentration in the mother liquor. The effect of impurity concentrations in the leach liquor on the purity of aluminum chloride (AlCl30?6H20) crystals was determined, but there was poor correlation between this data and results that have been obtained from miniplant-scale work.

Jan 1, 1980

By Robert F. Chaiken

A novel approach to eliminating environmental and public safety hazards that are associated with fires in abandoned coal mines and waste banks involves the use of in situ combustion technology developed by the Federal Bureau of Mines to accelerate the burning of the wasted coals in place. This technology would be used under exhaust ventilation control conditions that would allow for total management of the hot gases produced. Combustion stoichiometries would be optimized to minimize unburnt combustibles and to maximize the heat content of the gas products, which will be exhausted at one or more fan locations. When necessary, scrubber systems would be employed to remove air pollutants, such as sulfur dioxide; heat utilization systems (process heat, steam, and electricity) would also be employed to offset operational costs. Ultimately, complete burnout would solve the fire and acid water formation problems of the abandoned coal mine or waste bank. Pertinent technical data for burnout control are derived and discussed in terms of the important material and operational parameters. In general, it is believed feasible to operate a burnout system in an existing abandoned mine or waste bank fire at thermal power levels in the range of 10 to 100 Mw, and at exhaust gas temperatures of 1,000° C (1,830° F).

Jan 1, 1980

By R. F. Farrell

A goal of the U.S. Department of the Interior, Bureau of Mines, is the advancement of minerals technology through the development of improved metals and minerals processing. In support of this goal, the Bureau of Mines has developed a general method for preparing solutions from a wide range of metal and mineral samples for chemical analysis. The development of the method from current knowledge of vessel material, pressure dissolution techniques, and the fluoride-boric acid reaction is given. The method uses 7 ml of a mixture of HC1-HNO3-HF acids in a ratio of 3.5:2:1.5 sealed in plastic bottles that act as pressure vessels when heated in a boiling water bath. A final volume of 100 ml is obtained by the addition of 93 ml of a 1. 5-pct H3BO3 solution to the bottles, which are reheated; precipitated fluorides as well as sample residue are dissolved by the fluoride-boric acid reaction. A copper slag and a steelmaking slag treated using this method were analyzed by atomic absorption spectroscopy yielding values for Si, Mg, Ca, AI, Fe, Mn, Na, As, Pb, Sb, and Zn very close to certified values with an average relative standard deviation of 2.13 pct. The low cost, reduction in preparation time, ease and safety of sample handling, conservation of reagents, and ability to dissolve volatile materials without loss make this method superior to traditional wet digestion techniques for many materials, and ideal for use with atomic absorption, and optical emission or X-ray emission spectroscopy.

Jan 1, 1980

By H. D. Jacobs

The Bureau of Mines undertook a research program to insure an adequate supply of iron raw materials for future iron and steel making needs. A sample was obtained of oxidized taconite from the western Mesabi Range in Minnesota, and the metallurgical response of the taconite to beneficiation by a process that included selective flocculation-desliming-cationic flotation was evaluated. The sample contained 35.3 pct iron and represented approximately 2 billion tons of crude material. Selective flocculation and flotation were evaluated in a pilot plant with a feed rate of 900 Ib/hr. Concentrates averaging 61.7 pet iron and 5.1 pet silica were obtained, with an accompanying iron recovery of 67.2 pet. About 83 pct of the process water requirements were reclaimed from the slime and froth tailing and then recycled.

Jan 1, 1980

By J. E. Schiller

The Bureau of Mines has investigated the surface charge of amphibole asbestos fibers and nonasbestiform cleavage fragments, as part of the Bureau's fundamental studies to provide new knowledge on the physical and chemical properties of the amphibole minerals. Microelectrophoresis was used to measure the electrophoretic mobilities, in water, of particles from six asbesti-from amphiboles and seven nonasbestiform amphiboles over the pH range of 5 through 9. The particles generally ranged in size from 2 to 5 µm wide by 10 to 30 µm long. The isoelectric point was determined for four of the minerals, and values were found to be between pH 3.5 and pH 5. The minerals studied had zeta potentials that generally ranged from -25 to -so mv in neutral solution. Attachment of colloidal positively charged AgI was also studied as a means of determining surface charge. Scanning electron microscopy of amphibole particles that had been in contact with aqueous AgI showed equal attachment of AgI to asbestos fibers and to cleavage fragments; the extent of AgI coating was the same for both. The electrophoretic mobilities of asbestos fibers were essentially the same as those of elongated cleavage fragments of the same aspect ratio (particle length divided by width). Blocky particles from both asbestiform and nonasbestiform specimens had lower mobilities.

Jan 1, 1980

By S. A. Matthes

This Bureau of Mines report describes analysis of a copper slag for 13 elements from a single sample solution by flame atomic absorption spectroscopy. Samples are dissolved with 7 ml of an HC1-HF-HN03 (3:1.5:2) mixture in heated plastic pressure vessels. A 1.5-pct boric acid solution is added to dissolve precipitated fluorides and to reduce matrix effects that interfere with atomic absorption analysis. Preparation time is less than 1 hour per batch of 10 samples. Total analysis time is less than 6 person-hours for 130 determinations with an average relative standard deviation of 1.83 pct for the 13 elements. Simple acid standards were used for all determinations. Values obtained by this method are in excellent agreement with values obtained by slower, more costly procedures.

Jan 1, 1980

By G. R. Palmer

Using a fluidized, countercurrent multiple-compartment ion-exchange (MCIX) column previously developed by the Bureau of Mines, Bureau researchers have successfully extracted uranium from a simulated acidic in situ leach liquor that contained 150 ppm U30s? This successful demonstration of the MCIX system is reported, and the effects of varying the operating conditions on the performance of the system are also examined. Operating the MCIX system with a flow rate of 15 gpm/ft2 and an aqueous-to-resin flow ratio of 200:1, more than 90 percent of the uranium Has extracted, and a resin containing approximately 28 grams U308 per liter was produced. The absorption column used to investigate the operating variables was approximately 18 feet long with a 2-inch ID and was divided into compartments that were 1 foot long.

Jan 1, 1980

By Arne Landsberg

Accessory metals, although valuable resources, present possible environmental concern in the smelting of base metals. The Bureau of Mines, U.S. Department of the Interior, has undertaken research to define the chemistry involving these metals. Arsenic in copper smelting is the first to be investigated. Roasting, the first step in many copper smelters, was chosen for initial investigation because of the potential for arsenic removal in this primary process. Simple, static-bed, vaporization experiments were devised to obtain the data in this study. Ancillary transpiration and mass spectrometry were also used to delineate conditions necessary for arsenic volatilization from a roaster feed. For nearly complete arsenic removal, a temperature of 650°-700° C, a reducing atmosphere including carbon monoxide, and a source of sulfur were found to be essential.

Jan 1, 1980

By Robert Blickensderfer

Equipment and procedure for the continuous roll bonding of metal strips are described. The reels, mill rolls, and furnace were located within a vacuum chamber capable of operation at a residual gas pressure of 1 x 10-4 to 1 x 10-5 torr. Several metals were successfully clad at rolling temperatures of 930° to 1,050° C in lengths up to 120 ft. The bimetals that were clad included stainless steel to carbon steel, molybdenum and nickel to stainless steel and carbon steel, and titanium to carbon steel. Bend tests of bond integrity are described, and microstructures of the interfaces are presented. The amounts of brittle intermetallic phases formed at the interface are minimized by this cladding method.

Jan 1, 1980

By Anthony W. Sparks

The Bureau of Mines conducted tests designed to compare its breathing metabolic simulator (BMS) with other methods that are currently used to evaluate the performance of respiratory protective equipment. The BMS is a commercially developed device that uses a piston cylinder to simulate breath movement. Using a propane furnace that consumes oxygen and forms CO2, the BMS also simulates the respiratory metabolism of humans. The breathing and metabolic subsystems of the BMS are described in detail in this report. Results are compared from tests that used the BMS to evaluate respiratory equipment and from tests that used human subjects for the same purpose. The BMS was also tested against a pulsatile breathing machine (PBM) previously designed by the Bureau. Both machines were used to test respiratory equipment, and the test results are compared in this report. To illustrate typical applications of the BMS, the report briefly describes how the BMS was used to test two different types of closed-circuit respiratory apparatus, and the test results are presented. This research showed that BMS test results compared more closely to the results of tests that used human subjects than did results obtained using the PBM.

Jan 1, 1980

By G. W. Elger

The Bureau of Mines conducted laboratory and larger scale studies on samples of domestic perovskite and ilmenite ore concentrates to devise a procedure for recovering TiC from these ores. From the concentrates, mixtures of titanium and calcium carbides were produced. The carbides were then ground and reacted with water. This reaction decomposed the CaC2 to acetylene and hydrated lime and simultaneously liberated the TiC. Using a combination of elutriation and gravity-separation techniques to separate the hydrated lime, approximately 93 pct of the titanium was subsequently recovered as purified carbide containing 54 to 70 pct titanium with CaO content as low as 0,6 pct. This combination of techniques can be used to separate more than 90 pct of the CaO from the TiC. Therefore, this carbiding procedure is a viable method for treating titaniferous materials, including perovskite, that contain more than 20 pct CaO. Tests made in a static-bed reactor showed that for the reaction of TiC with elemental chlorine to produce titanium tetrachloride (TiCI4), a temperature of at least 940° F is desirable to achieve a suitable extraction of titanium in a laboratory chlorination reactor. In fluidized-bed tests at 840° F, 98 pct of the titanium contained in TiC was extracted.

Jan 1, 1980

The Bureau of Mines, U.S. Department of the Interior, devised a flotation technique for upgrading chromite in chromium ores and gravity concentrates. The technique consisted of cationic flotation of chromite from a slime-free pulp acidified to pH 2.5 or lower using H2S04 modifier. Flotation results showed that ore containing serpentine as the primary gangue mineral was more amenable to concentration by this technique than ore containing the readily floatable olivine as the primary gangue mineral. Rougher flotation of a chromite ore containing abundant serpertine increased the grade form 19 to 41 percent Cra03 at a chromite recovery of 89.6 percent. Rougher flotation of ore containing abundant olivine upgraded the chromite from 23.4 to 29.6 percent Cr203 at a recovery of 89.4 percent. The technique was also applied to chromite gravity concentrates to further upgrade chromite and to reject silicates. Flotation of a gravity concentrate containing 40.9 percent Cr203 and 4.4 percent SiO2 recovered 90 percent of the chromite in cleaner products containing 44.9 percent Cr203 and 0.63 percent Si02. The combined recovery by gravity and flotation was 87 percent. An economic evaluation of this technique will be undertaken to deter-mine its feasibility for commercial use.

Jan 1, 1980

By J. P. Hansen

In order to help assure an adequate domestic supply of minerals essential to the Nation's economy and and security by developing more efficient minerals extraction technologies, the Bureau of Mines Tuscaloosa Research Center examined the application of autogenous microgrinding to calcium carbonate minerals. Treatment of minus 8-mesh Alabama marble resulted in a product 80 pct minus 5 micrometers (µm) at a power consumption of 70 to 80 kwhr/ton, This study shows that coarse particles of calcium carbonate minerals are effective as the grinding media for the autogenous attrition grinding of these minerals. The minus 8- plus 30-mesh fraction is an effective grinding medium (sand) for particles smaller than 30 mesh. A 40-pct-solids slurry and a sand: marble ratio of 2.5 appeared to be near optimum. For residence times above 13 minutes, products were greater than 80 pet minus 5 µm and greater than 54 pct minus 2 µm. Power consumption was uniformly low, ranging from 50 to 100 kwhr/ton of product depending upon the feed rate. One marble sample from Georgia was shown to be the most persistent grinding medium, with losses of less than half those of the other materials tested.

Jan 1, 1980

By F. X. McCawley

The Bureau of Mines, in pursuing its goal of extending the life span of strategic materials, conducted field corrosion studies at the East Mesa Known Geothermal Resources Area (KGRA) in the Imperial Valley, Calif., to determine the optimum materials of construction for use in geothermal mineral energy resource recovery plants. These studies included characterization of geothermal environments and in situ corrosion testing. The corrosion resistance of 10 alloys exposed to 5 brine and steam process environments was evaluated using the low-salinity, high-temperature brine from geothermal well Mesa 6-1. Of these alloys, Hastelloy C-276, Hastelloy S, Incone1 625, titanium-2nickel, and 316 L stainless steel had excellent resistance to corrosion in all of the process environments; E-Brite 26-1 and 430 stainless steel had fair resistance. Although general corrosion rates for 4130 steel and 1020 carbon steel were substantially higher than those of the other iron-base alloys, these two alloys could prove useful in low-salinity process environments because of their low cost. Aluminum alloy 5005 was the least corrosion resistant alloy and pitted severely. Scales formed on all of the alloys in every process environment. Calcite, aragonite, and an amorphous silicate were the major components of the scales.

Jan 1, 1980

By Mark S. Stagg

Blast-induced ground vibrations from surface coal mine, quarry, and construction blasting were measured and analyzed for frequency content and duration characteristics. Eighteen commercially available ground vibration measurement systems were evaluated in the field and laboratory for linearity, accuracy, and crosstalk. Buried, surface, and sandbagged transducer placement methods were compared, along with peak and vector-sum measurements. The recommended minimum frequency ranges for ground vibration instrumentation are 2 to 150 Hz for coal mine and quarry blasting, and 5 to 200 Hz for construction and excavation blasting. When higher or lower frequency vibrations are possible, as in construction blasting or for a quarry shot close to a residence, care should be taken to insure proper choices of instrumentation and vibration criteria. Several instruments operating in these ranges are available, and all but one of the seismographs tested fell within ±3-dB accuracy limits (+41 pct, -29 pct). Waveform recordings of all three ground vibration components are recommended as the peak amplitude and frequency may vary among the three. Peak or vector-sum readings are adequate if only amplitude levels are desired. The soil density matched box should be anchored or buried, particularly for high-frequency, high-amplitude construction blasting.

Jan 1, 1980