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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 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 David E. Siskind

The Bureau of Mines studied airblast from surface mining to assess its damage and annoyance potential, and to determine safe levels and appropriate measurement techniques. Research results obtained from direct measurements of airblast-produced structure responses, damage, and analysis of instrument characteristics were combined with studies of sonic booms and human response to transient overpressures. Safe levels of airblast were found to be 134 dBL (0.1 Hz), 133 dBL (2 Hz), 129 dBL (6 Hz), and 105 dB C-slow. These four air-blast levels and measurement methods are equivalent in terms of structure response, and anyone could be used as a safe-level criterion. Of the four methods, only the 0.1-Hz high-pass linear method accurately measures the total airblast energy present; however, the other three were found to adequately quantify the structure response and also represent techniques that are readily available to industry. Where a single airblast measuring system must he used, the 2-Hz linear peak response is the best overall compromise. The human response and annoyance problem from airblast is probably caused primarily by wall rattling and the resulting secondary noises. Although these will not entirely be precluded by the recommended levels, they are low enough to preclude damage to residential structures and any possible human injury over the long term.

Jan 1, 1980

By Seth C. Schaefer

[As part of the Bureau of Mines effort to provide thermodynamic data for advancement of mineral resources technology, the standard Gibbs energies of formation (?G°f) of MnS (manganese sulfide) and Fe0.9 S (pyrrhotite) were investigated with a high-temperature galvanic cell employing stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, MnS, MnO, S02 (g, 1 atm)//Zr02//02(g, 0.0114 atm), Pt with the overall cell reaction MnS (s) + 1.5 02 (g, 0.0114 atm) = MnO (s) + S02 (g) . (1) These results give the standard Gibbs energy of formation of MnS for the reaction Mn (s) + 0.552 (g) = MnS (s) (2) ?G°f = -66.487 + 15.19 x 10-3T±0.207 kcal/mole (896.4 - 1,208.1 K) (3) where temperature (T) is expressed in kelvins. Similar measurements were obtained for the cell Pt, FeO .9S, Fe304 , S02 (g, 1 atm) //Zr02//02 (g, 0.0114 atm) , Pt with the overall cell reaction 10/3 FeO .9 S (s) + 16/3 02 (g, 0.0114 atm) = Fe.,04 (s) +10/3 S02 (g). (4) These results yield the standard Gibbs energy of formation for the reaction 0.9 Fe (s) + 0.5 S2 (g) = Fe0.9 S (s) (5) ?G°f = -35.229 + 12.67 x 1073T+-0.104 kcal/mole (839.5 - 1,086.6 K). (6) A third-law analysis of MnS data yields a standard enthalpy of formation (AH°f) for the reaction Mn (s) + S (rh) = MnS (s) (7) ?H°f298 = -51.16±0.21 kcal/mole (8) A similar third-law analysis for Fe0.9S data yields a ?29°f298 for the reaction 0.9 Fe(s) + S(rh) = FeO .9S(s) (9) ?HO\°f298 = -24.01±_0.15 kcal/mole. (10) ]

Jan 1, 1980

By V. R. Spironello

The Bureau of Mines is involved in research directed toward the conserva¬tion of important raw materials and the utilization of solid waste. Two of the objectives are to conserve high-quality coking coals used for foundry coke and to utilize waste materials of marginal quality but of high calorific value. These objectives are consistent with Bureau goals. Pilot plant cupola trials were made to evaluate the adequacy of various alternative fuels, and to determine to what extent they could replace the foundry coke in cupola charges. Information was obtained on furnace performance, metal and slag chemistry, environmental questions, and the properties of castings. It was shown that anthracite or bituminous coals can partially replace charge coke up to the 40 pet level. Briquetted materials prepared from fuel fines, and waste prod¬ucts or byproducts of high calorific value, all tend to break down on heating in a cupola so that their use must be restricted to below 20 pet replacement. In cases where pitch-bonded coal fines or petroleum coke were used, carbon pickup by the iron was inadequate for gray iron specifications. Although emphasis during this work was placed on basic slag practice, some acid practice results are included.

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 R. E. Simpson

Beginning in 1972, fully grouted resin bolts were used in underground mines. An estimated 20 million resin bolts will be installed in 1980 owing to their apparent support improvement in most roof-bolt applications. Inorganic cements were tested to replace the resin at a lower cost while retaining the advantages of a grouted bolt. Although other inorganic materials were considered, all but portland and gypsum cements were rejected for reasons of availability, performance, or cost. Portland and gypsum-type cements were tested by the Bureau of Mines to select a fast-hardening, low-cost material that would anchor a roof bolt adequately to meet safety standards. An alpha-gypsum cement, accelerated with potassium sulfate, was selected as the best material because it had adequate pull strength at a desired set time of less than 5 minutes and was readily available.

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

As part of the Bureau of Mines subactivity in secondary resource recovery and to expand the Nation's mineral base, the Tuscaloosa Research Center made characterization and preliminary beneficiation studies of the waste residues from various coal-conversion processes: from pilot plant tests of the Synthane process for coal gasification, the Synthoil process for coal liquefaction, and the solvent-refined coal (SRC) process for sulfur removal from coal. Those coal conversion processes selected for this study were based on the availability of pilot plant samples. Physical, chemical, and mineralogical examinations of the wastes made to determine the mineral content prior to physical beneficiation tests indicated that in addition to significant quantities of carbon, some trace elements offer potential for concentration.

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 H. D. Jacobs

The Federal Bureau of Mines, as part of a program to insure future raw material needs for the iron and steel industry, undertook research to beneficiate the oxidized taconites from the western Mesabi range in Minnesota. The data presented were obtained by applying the Bureau-developed selective-flocculation/cationic-flotation process to the second of three oxidized taconite samples. These three samples are representative of an estimated 10 billion tons of ore analyzing 30 to 40 pct iron. The experimental work was performed in a 900-lb/hr pilot plant. Treating the ore sample (36.1 pct Fe) with the Bureau's process produced commercially acceptable concentrates averaging 63.5 pct Fe and 4.3 pct SiO2, with an average iron recovery of 84.6 pct.

Jan 1, 1980

By K. R. Farley

A simplified method for the atomic absorption determination of antimony is described. Samples are dissolved in hydrobromic acid and diluted to volume with water. Solutions can be ready for analysis in about 10 minutes and are stable for at least 24 hours. The spectral line at 231 nanometers is used, and there is no effect on absorption resulting .from the presence of any concentration of HBr. Absorbance is linear with antimony concentrations up to 120 micrograms per milliliter. Sensitivity is 1.48 micrograms per milliliter per 0.0044 absorbance. Relative errors on National Bureau of Standards Standard Reference Materials were 3 percent or less, and relative standard deviations on 12 determinations of each of three flue dust samples were 4 percent or less (95-percent confidence limit).

Jan 1, 1980