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By Gary W. Kramer

The Bureau of Mines has developed a rapid analytical method for the determination of anions by ion chromatography (IC) in phosphate rock mining materials and cement kiln dust (CKD). The procedure employs an Na2C03 fusion of the sample, followed by a water extraction that allows direct injection of the sample into an ion chromatograph without separator column poisoning by the transition metal ions. Fluoride (F-) and phosphate (P043-) were determined in 24 phosphate rock processing and waste material samples by the IC method. The results were compared with a pyrohydrolytic distillation-titration method for F-and a colorimetric procedure for P043-. Excellent analytical agreement was obtained for F-and p043-values determined by IC and the comparable wet chemical methods. Fluoride values ranged from 0.3 wt-pct in the filter cake to 3.6 wt-pct in phosphate rock concentrate. Phosphate values ranged from 1.2 wt-pct in the filter cake to 33.8 wt-pct in the rock concentrate. Fluoride, chloride, phosphate, nitrate, and sulfate in several CKD samples were determined by the IC method and standard wet chemical techniques. Excellent agreement was obtained between the two methods for all anions. A total of 113 CKD samples from all areas of the United States was analyzed by the IC method. Fluoride values ranged from <0.01 to 0.36 wt-pct. Chloride values ranged from <0.01 to 12.5 wt-pct. Sulfate values ranged from 0.41 to 31.6 wt-pct. Phosphate and nitrate were detected in only about 25 pct of the samples at >0.02 wt-pct. Maximum phosphate and nitrate values were 1.0 and 1.6 wt-pct, respectively.

Jan 1, 1982

By David W. Houseknecht

Probabilities of encountering coalbed discontinuities during vertical or horizontal drilling in a specific coalbed can be estimated based on analysis of mined-out areas of the coalbed where the size, shape, orientation, and distribution of discontinuities are known. The result- ant probability estimates can be applied to cost-risk evaluations of drilling programs proposed for exploratory, developmental, or methane drainage purposes in undeveloped areas of that coalbed. Data compiled from mine maps of the Beckley Coalbed in southern West Virginia were used to estimate the probabilities that discontinuities would be encountered in two illustrative hypothetical drilling programs--one for drilling vertical boreholes and the other for drilling horizontal boreholes. Analysis based on a mined-out area of the Beckley Coalbed indicated that vertical methane drainage boreholes spaced 1,000 feet apart in a square grid pattern would each have a 29 percent probability of encountering a discontinuity in a geologically unexplored area of the coalbed. It was also determined that exploratory vertical drilling could locate most of the discontinuities if a borehole spacing of 2,500 feet were used. For horizontal drainage boreholes in the Beck- ley Coalbed, the analysis indicated a linear relationship between hole length and the probability of encountering a discontinuity.

Jan 1, 1982

By Leonard J. Prosser, Joseph Cervik, John H. Perry

The Bureau of Mines has developed several techniques for draining methane from coalbeds in advance of mining. Drilling long horizontal holes from an underground location is one such technique, which was successfully demonstrated in the Pittsburgh and Sunnyside Coalbeds. The same technique has now been applied in the Mary Lee Coalbed at Jim Walter Resources, Inc. &apos;s No. 4 Mine, Brookwood, Ala. , where two holes were drilled horizontally--one to a depth of 1,010 feet (308 m) and the other to 540 feet (165 m). The 1,010-foot (3083) hole proved successful in degasifying a portion of the Mary Lee Coalbed. The hole drained methane for 1 year, during which time the initial gas flow of 200,000 ft3/d (5,663 m3/d) declined to 65,000 ft3/d (1,840 m3/d). Total gas production was 40 x lo6 ft3 (1.1 x lo6 m3 ). The gas was of commercial quality, with 98 pct methane and a heat rating of 990 Btu/ft (36.89 Mj/m3). The methane emissions from the faces of the mine section advancing into the degasified zone were reduced by 60 pct. The 540-foot (165-m) hole was terminated prematurely when it became impossible to maintain an open hole. Because of caving, very little gas was drained through this hole.

Jan 1, 1982

By John H. Perry

The Bureau of Mines has developed several techniques for draining methane from coalbeds in advance of mining. Drilling long horizontal holes from an underground location is one such technique, which was successfully demonstrated in the Pittsburgh and Sunnyside Coalbeds. The same technique has now been applied in the Mary Lee Coal bed at Jim Walter Resources, Inc.&apos;s No. 4 Mine, Brookwood, Ala., where two holes were drilled horizontally--one to a depth of 1,010 feet (308 m) and the other to 540 feet (165 m). The 1,010-foot (308-m) hole proved successful in degasifying a portion of the Mary Lee Coalbed. The hole drained methane for 1 year, during which time the initial gas flow of 200,000 ft3/d (5,663 m3/d) declined to 65,000 ft3/d (1,840 m3/d). Total gas production was 40 x 106 ft3 (1.1 x 106 m3). The gas was of commercial quality, with 98 pct methane and a heat rating of 990 Btu/ft3 (36.89 Mj/m3). The methane emissions from the faces of the mine section advancing into the degasified zone were reduced by 60 pet. The 540-foot (165-m) hole was terminated prematurely when it became impossible to maintain an open hole. Because of caving, very little gas was drained through this hole.

Jan 1, 1982

By A. D. Mah

Thermodynamic data on compounds of arsenic and sulfur were critically evaluated by the Bureau of Mines. Changes of standard enthalpy and Gibbs energy, and logarithms of the equilibrium constants were tabulated as a function of temperature for reactions involving these compounds.

Jan 1, 1982

By Tobias W. Goodman, George N. Aul, Joseph Cervik

The Bureau of Mines conducted research to degasify a virgin block of coal in the Beckley Coalbed using long horizontal holes drilled in an array from the bottom of a ventilation air shaft. Eight horizontal holes and an in situ pressure hole were drilled in a radial pattern to depths ranging from 418 to 910 ft (127 to 277 m) and 205 ft (62 m), respectively. The investigation showed the shaft was in a basin saturated with water, which resulted in low gas flows from holes. The in situ pressure at 200 ft (61 m) into the coalbed was 79 psig (544.6 KN/m2). The aver- age gas and water flows for the eight holes were 94,100 ft3/day (2,665 m3/day) and 13 gal/min (49.3 l/min) . After 514 days of degasification, 18.7 million ft3 (0.53 million m3) of gas had been drained. Methane face emissions, which were measured as a section advanced toward the shaft, were reduced about 77 pct, emphasizing the value of drainage by this technique. All holes were grouted before the area around the shaft was mined.

Jan 1, 1982

By L. E. Schultze

The Bureau of Mines operated a mineral recovery unit to recover metal values from post-flash geothermal brines from the Salton Sea known geothermal resource area as part of its research into the use of plentiful resources. The brine was available for metals recovery after its heat content had been used to generate electricity. The brine source was treated with lime to precipitate the contained iron, manganese, lead, and zinc before injection of the heat-depleted brine into the underground reservoir. Data are presented on the effects of process variables, such as rate and method of lime addition and air oxidation versus air exclusion. Variations in precipitation of metal values, composition of precipitates, effectiveness of slurry thickeners, and methods of treating the precipitates to recover metal values are discussed.

Jan 1, 1982

By Arthur V. Petty

In Bureau of Mines research on recycling chrome-containing refractory wastes, used refractories from argon-oxygen decarburization and electric steelmaking furnaces were beneficiated. By means of dry magnetic separation on minus 6-mesh crushed wastes, a concentrate was produced. After minor adjustments to the particle size distribution, full-size refractory brick were dry-pressed by a commercial producer and fired to 1,450° and 1,730° C. Standard testing procedures were used to determine the cold-crushing strength, modulus of rupture at 25°, 1,300°, and 1,500° C, hot load, thermal shock resistance, thermal expansion, and slag resistance. Optical and electron microscopy were used to determine grain-bonding mechanisms, and energy-dispersive analysis of X-rays was used to determine elemental distribution. The test results indicate that the beneficiated material could be used to produce a refractory product suitable for moderate-temperature applications.

Jan 1, 1982

By R. O. Dannenberg

The Bureau of Mines conducted laboratory batch and small-scale continuous tests to remove traces of dissolved molybdenum from water simulating waste discharged from a molybdenum concentrator, Molybdenum concentrations, initially ranging from 2 to 10 ppm, were decreased to 0.5 ppm or less by coprecipitation of the molybdenum with freshly precipitated ferric hydroxide" The precipitate was separated as a froth by dissolved-air flotation for subsequent disposal. Although the treated water met current environmental standards for contained molybdenum, contained particulate iron might have to be removed by filtration for the water to be acceptable. Estimated costs for treating concentrator effluent water were 55 cents, 57 cents, and 64 cents per 1,000 gal at initial molybdenum concentrations of 2, 4, and 10 ppm, respectively.

Jan 1, 1982

By H. C. Ko

As part of the Bureau of Mines effort to provide thermodynamic data for the advancement of mineral technology, the standard enthalpies of formation for ZnO?2ZnSO4 and COS04-6H20 were determined by HC1 acid solution calorimetry. The values are -550.31 ±0.28 and -641.33 ±0.15 kcal/mot, respectively.

Jan 1, 1982

By E. Morrice

As part of its efforts to maximize process efficiency and decrease energy requirements in mineral processes, the Federal Bureau of Mines has investigated methods for beneficiating bastnäsite ores from Mountain Pass, Calif. The results of a bench-scale study on the flotation of bastnäsite ore are presented. Flotation at a pulp temperature of 40° to 45°C yielded a cleaner concentrate containing 58.7 pct RE203 at a rare-earth recovery of 67 pct. These results are comparable to those reported for the commercial beneficiation method in which the pulp is heated to boiling before flotation. An attempt was also made to recover a barite flotation concentrate from the bastnäsite rougher tailing. Concentrates containing only 70 pct barite were obtained.

Jan 1, 1982

By H. H. Dewing

The Bureau of Mines constructed a process research unit (PRU) to demonstrate new technology for extracting zinc from sphalerite concentrates. Up to 9 kg/hr of sphalerite (ZnS) concentrate was reacted at ambient pressure in the PRU with 80 pct sulfuric acid at 160° to 180° C to produce zinc sulfate and elemental sulfur. The PRU consisted of a three-stage glass reactor system: a 4-liter premix stage in which feed was slurried with 78 to 82 pct H2S04, a 40-liter stirred reactor, and a ISO-liter settling stage in which high reaction conversions were effected and excess H2S04 for recycle was separated from insoluble ZnS04 and sulfur. Evolution of sulfur-containing gases was minimized by sub-surface addition of acid feed slurry to the stirred reactor and by exclusion of air from the reactor to prevent the oxidation of elemental sulfur. Conversion of zinc to zinc sulfate averaged over 99 pct at the optimum acid concentration of 80 pct. Total sulfur losses (primarily S02) were less than 2 pct of the sulfur in the sphalerite. Elemental sulfur remained in the insoluble portion of the settled reactor product after leaching with simulated spent zinc electrolyte containing sulfuric acid. The sulfur residue contained 75 to 89 pct sulfur. Neutral zinc sulfate, required for zinc electrowinning processes, was separated from the sulfuric acid leach solution by crystallization at -15° C as zinc sulfate heptahydrate (ZnS04?7H20). The crystallization operation simultaneously effected a partial concentration of the recycled electrolyte solution by removing water.

Jan 1, 1982

By John P. Coughlin

Software techniques developed by the Bureau of Mines Denver Research Center for real-time microseismic data analysis are presented. These techniques focus on the simple acquisition of P-wave arrival times and their use in event location. The paper discusses in detail software techniques to separate microseismic events from mining noise such as drilling and from very large events such as rock bursts. Incorporation of these techniques has enhanced the reliability and accuracy of computer-based monitoring of microseismic activity in ongoing research by the Bureau.

Jan 1, 1982

By William H. Pomroy

The Bureau of Mines, through a 4-year program of combined in-house and contract research, has developed the necessary hardware and software technology to provide rugged, reliable automatic fire protection for surface mining mobile equipment. One element of this program was a continuing effort to help foster rapid mining industry acceptance of the technology by keeping end user costs reasonable. This report is an analysis of the economic impact of surface mining mobile equipment fires and the cost benefit of utilizing automatic fire protection systems to abate these losses.

Jan 1, 1982

By Victor R. Spironello

The Bureau of Mines has conducted studies of the slags related to ferrous technology to evaluate experimentally acceptable substitutes for the auxiliary flux, mineral fluorspar, in steelmaking operations. Comparative heats were made in a 1/4-ton, pilot-scale, basic oxygen furnace (BOF) to evaluate a waste material known as "used potlining." Used pot lining is recovered from alumina reduction cells after its useful life and contains significant levels of fluorine and sodium in various compounds. This material in both lump and pelletized form provided adequately fluid slags, based on observations made during BOF operation. No adverse effects were found on furnace performance, metal and slag chemsitry, the strength of the steel produced, or the environment. Fluorine recovery in the slag was about the same as that obtained when using fluorspar, as were the losses to the scrubber water and solids. No difference was observed in furnace-refractory attack, as determined by the level of magnesia in the slag. The sodium recovered in the slag apparently also contributed to fluidity, since the fluorine input was at about two-thirds that of the fluorspar. Used potlining was determined experimentally to be a satisfactory substitute for fluorspar in basic oxygen steelmaking.

Jan 1, 1982

By Seth C. Schaefer

The Bureau of Mines investigated thermodynamic properties of Mn304 (manganomanganic oxide) and Mn203 (manganese sesquioxide). The standard Gibbs energies of formation (?Gf°) of Mn304 and Mn203 from their lower oxides were determined with high-temperature galvanic cells using stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, MnO, Mn304//Zr0 2//02(g, 0.0112 atm), Pt, with the overall cell reaction 6Mn0(c) + 02(g, 0.0112 atm) = 2Mn304(c), where- 02 refers to indicated partial pressure of oxygen at the reference electrode. Similar measurements were obtained for the cell Pt, Mn304, Mn203//ZrO2//02(g, 0.0115 atm), Pt, with the overall cell reaction 4Mn304(c) + 02(g, 0.0115 atm) = 6Mn203(c). Equilibrium oxygen pressures for the Mn0-Mn304-02 and Mn304-Mn203-02 systems were measured and may be expressed for the respective systems as [23,400 109 P02 T + 11.91 (764.9 - 1,208.6 K) and log p02 = - 11,957 + 9.66 T (968.6 - 1,208.2 K),] where pressure (p02) is in atmospheres and temperature (T) is in kelvins. Standard thermodynamic properties of Mn304 and Mn203 were derived from these measurements and auxiliary thermodynamic data from the literature.

Jan 1, 1982

By J. M. Stuve

A novel calorimetric solution technique, recently developed at the Bureau of Mines, was tested using synthetic samples of chalcocite (CU2S) and covellite (CuS). The solution of these refractory sulfides was accomplished by oxidation with bromine in a moderately acidic, aqueous solution. The resulting values for the standard enthalpies of formation (?Hf°, 298.15) for CU2S(c) and CuS(c) were -18.1 ±1.1 kcal/mol and -13.3 ±1.1 kcal/mol, respectively. These values are in good agreement with published formation values derived from other methods of physicochemical measurement.

Jan 1, 1982

By V. E. Edlund

As part of a research program for recovering alumina from domestic nonbauxitic resources, the Bureau of Mines investigated a lime-sinter, caustic leach technology for anorthosite. This report discusses the unit operations--feed preparation, sintering, and leaching. Acceptable pellets for the bench-scale sintering studies were prepared from mixtures of minus 200-mesh anorthosite and limestone using water alone as the pelletizing agent. Heating pellets at 1,270° to 1,360° C for periods of 0.5 to 2 hr, followed by a 15-min soaking period at 700° C and cooling to room temperature, produced a sinter that dusted to more than 90 pct minus 65 mesh. The weight ratio of limestone to anorthnsite was critical in producing sinter exhibiting good dusting and leaching characteristics. A ratio of 2.0 was optimum for the bulk samples of anorthosite and limestone used in this research. Leach solutions from lower ratio sinters were unstable; gelation became progressively more severe with higher ratio sinters. Leaching the dusted sinter with 10-pct Na2CO3 at 60° C extracted 85 to 90 pct of the alumina in a product solution containing about 50 g/l A1203. Leach residue in contact with pregnant solution tended to set up as a rigid gel as a result of cementation, comp action, and gelation. The presence of a calcium-sodium zeolite [(Cn,Na2)6?(Al2Si04)12?27-3OH20] in the ungelled residues seemed to be the main difference between gelled and ungelled residues.

Jan 1, 1982

By R. Emmett Hughlett

The Bureau of Mines has developed a statistical approach to the laboratory evaluation of response bias and precision in gas detectors. The techniques described employ a computerized analysis and a new method of data presentation called composite graphing. The underlying theory, its practical application to the data, and the experimental equipment and procedure are described.

Jan 1, 1982

By L. W. Higley

It is estimated that well over 20 million lb of chromium and 8 million lb of nickel, plus other metal values, are diverted annually to furnace dusts, mill scale, and contaminated swarfs in the domestic stainless and other specialty steelmaking industry. Little inroad has been made toward the in-plant recycling of these wastes to reclaim the metal values. The Bureau of Mines has devised a process for recovering about 90 pct of the chromium and molybdenum and well over 90 pct of the nickel and iron from stainless steelmaking furnace dusts, swarf, and mill scale. Other metals such as manganese are also recovered. Initial laboratory results were confirmed and expanded to include a wide variation of stainless steelmaking waste mixtures. Later experiments have included specialty steelmaking wastes other than from stainless steelmaking. Significantly, the ease of technology transfer has been demonstrated by a number of industrial-sized (19-ton) commercial electric furnace heats, in which the pelletized wastes represented some 10 to 20 pct of the furnace charge, replacing part of the normal scrap charge. Results of these successful large-scale trials are presented. Some information is also presented on incorporation into the pellets of chromium-bearing particulate wastes originating from other than steelmaking production. Cost evaluation indicates the process is economically attractive.

Jan 1, 1982