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By B. J. Scheiner

The Federal Bureau of Mines investigated an electrolytic oxidation procedure for extracting lead, zinc, copper, and silver from lead-zinc concentrates. Concentrates slurried in brine were pumped through the anode compartment of electrolytic cells equipped with selective ion diaphragms. Hydrochloric and hypochlorous acids generated in the anode compartment converted the metal sulfides in the concentrates to soluble metal chlorides, sulfate ion, and elemental sulfur. Metal extractions of 92 to 100 pct were obtained from lead-zinc concentrates at an energy consumption ranging from 1.5 to 5.0 kW-hr/lb metal extracted. Sodium hydroxide was formed in the cathode compartment at a current efficiency of >99 pet. Silver and copper were extracted from refractory tetrahedrite minerals, but the process entailed a relatively high energy consumption. Sealing the top of the diaphragm cell utilized the chlorine more effectively, thereby reducing energy consumption 10 to 50 pct.

Jan 1, 1975

By Seth C. Schaefer

The Bureau of Mines studied the standard free energies2 of formation of ferrous fluoride (FeF2) and ferric fluoride (FeF3) with high-temperature galvanic cells employing calcium fluoride doped with 1 mole-pet yttrium fluoride as the electrolyte. A free-energy change for the cell reaction Fe (s) + NiF2 (S) = FeF2 (S) + Ni (s) together with the standard free energy of formation of nickel fluoride yields a standard free energy of formation of ferrous fluoride from the elements of ?GF° = -168.74 + 30.63 x 10-3T ± 0.41 kcal/mole (897-1,098 K). (2) Combining the standard free energies of formation of magnesium fluoride, ferric oxide, and magnesium oxide with the free-energy change for the overall cell reaction 3MgO(s) + 2FeF3 (s) = 3MgF2 (S) + Fe2 03 (S) (3) gives a standard free energy of formation of ferric fluoride from the elements as ?Gf° = -281.45 + 90.46 X 10-3T ± 0,67 kcal/mole (880-935 K). (4) Free energies and equilibrium fluorine pressures for the two univariant equilibria of the Fe-F system are tabulated and illustrated.

Jan 1, 1975

By S. R. Borrowman

Mill tailings from conventional uranium extraction processes contain nearly all of the radium originally in the ore. Such tailings require controlled storage in perpetuity to safeguard the surrounding environment from radioactive contamination. Alternatives to controlled storage of the tailings are (1) removal of the radium from the tailings for separate storage or use or (2) removal of the radium when processing the uranium ore. In laboratory tests conducted by the Federal Bureau of Mines, radium was leached from tailings using either hydrochloric acid or ethylenediamine tetraacetic acid. A hydrochloric acid leaching method was used to extract both radium and uranium from the ore to yield tailings containing less radium than those produced by either conventional sulfuric acid or alkaline leaching processes. From 77 to 94 percent of the radium in mill tailings was concentrated by sedimentation in slime fractions representing nearly 25 weight-percent of the original sample.

Jan 1, 1975

By R. L. Stein

For the past several years, the Bureau of Mines has been actively engaged in developing two new oxygen self-rescuers through research contracts with private industry. These new oxygen self-rescuers are designed to be carried by a miner while he is at work and are used during emergency escape, supplying high-purity oxygen to the user and, at the same time, absorbing carbon dioxide (C02), The first of the two new self-rescue breathing devices is a 10-minute, self-contained apparatus developed by the Mine Safety Appliance Co, Size and weight of the unit are comparable to the currently used self-rescue devices. The second device, designed and developed by Lockheed Missiles and Space Corp., is 8. 4.5-lb package which supplies 1 hour of oxygen to the miner. Both devices have a canister which contains the oxygen-producing and CO2-absorbing potassium superoxide chemical, a breathing bag, a bite-type mouthpiece, noseclip, goggles, and hoses connecting the canister and mouthpiece. When needed in an emergency, the miner removes the outer protective cover and dons the unit. For both devices oxygen is immediately available once the mouthpiece is placed in the mouth. These two new units have received prototype approval from the National Institute for Occupation and Safety Health (NIOSH) and the Mining Enforcement and Safety Administration (MESA).

Jan 1, 1976

By R. A. Guidotti

The Federal Bureau of Mines studied the thermal decomposition of the nitrides of the Group V A metals (CbN, Ta3N5, and VN) with the goal of preparing high-purity metals. Solid-state purification and arc and electron-beam melting were examined. Electron-beam melting proved to be the most efficient means of nitrogen and oxygen removal. Columbium and tantalum of 99.9-pct purity were prepared by this technique; in the case of vanadium, however, nitrogen could not be reduced below the solid-solution level.

Jan 1, 1976

By Carl F. Wingquist

Electrical resistance heating to effect thermal fragmentation of semiconductive rock was examined by the Bureau of Mines. Tests were carried out on copper-bearing ores of the Nonesuch Shale Formation in the laboratory and in the the field at White Pine, Mich. Fieldwork included primary and secondary breakage tests. Heating tests on in situ rock failed to produce thermal dam-age to an extent considered useful; however, boulders up to 30 ft3 were effectively broken by the method. Power input to the test rock was taken from a 50-kV, 5-amp dc power supply.

Jan 1, 1976

By Arthur M. Hartstein

The Federal Bureau of Mines, under a contract with Ultrasystems, Inc., investigated the thermal oxidative degradation characteristics of conveyor belts used in underground mines. This included the determination of smoke evolution, glow characteristics, char yields, and the identification and quantification of all volatile decomposition products in the form of gram of specific product formed per gram of belt sample tested. In addition to these investigations, degradation studies were conducted on some pure ingredients used in conveyor-belt formulations. Three basic classes of belts were investigated: neoprene, polyvinyl chloride, and styrene-butadiene rubber compositions. The studies indicate that styrene-butadiene-based belts exhibit good flame resistance and are the least hazardous in regard to overall formation of toxic decomposition products. Under this program, thermogravimetric analysis was definitely established as a method of material differentiation.

Jan 1, 1976

By Joan T. May

The Bureau of Mines conducted laboratory tests to evaluate the production of high-purity H3P04 by HCl digestion and solvent extraction. Both batch and bench-scale continuous tests were made. Western phosphate rock concentrates were acidulated with HCI, and the digestion liquors were processed by solvent extraction. Phosphoric acid was extracted with isoamyl alcohol and recovered from the organic extract by contact with an NH4F solution. This solution was fractionally distilled to yield high-purity H3P04. The raffinate from solvent extraction was treated with lime to precipitate CaF2, which was subjected to steam pyrolysis to generate HF. This method was successful in recovering 95 pet of the phosphate and 80 pct of the fluoride contained in the concentrates.

Jan 1, 1976

By Philip E. Sanker

The Bureau of Mines conducted small-scale batch and semicontinuous tests on the reduction of zinc sulfide with iron according to the reaction ZnS + Fe ? FeS + Zn to determine reaction kinetics in the temperature range 1,000° to 1,400° C and to investigate the potential use of a scrap iron reductant. Batch tests indicated that a temperature of at least 1,300° C with a 1:1 mole ratio of Fe to ZnS is needed for good zinc recovery. Semicontinuous tests were conducted, using four zinc concentrate samples, containing various percentages of copper, cadmium, and lead, which were reacted with iron and iron contaminated with iron oxide and tin in an externally heated graphite furnace. Analysis of the zinc metal and FeS matte reaction products showed cadmium to be entirely in the zinc metal, copper to be in the FeS matte, and lead to be about 60 pct in the zinc metal and 40 pct in the matte. Tin reported to the matte, and none was detected above the O.OS-pct level in the zinc. Sulfur dioxide was not detected in the offgas when up to 20 pct of the iron was replaced by Fe203.

Jan 1, 1976

By J. B. Janus

This report, the 25th in a series, lists analytical data of coal samples collected by the Bureau of Mines in connection with the purchase of several million tons of coal for various Government agencies during fiscal year 1975. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. Ultimate analyses are given for these coalbeds only. The delivered coal was sampled at destination in accordance with instructions furnished by the Bureau of Mines, and all samples were analyzed in the Bureau laboratory at Pittsburgh.

Jan 1, 1976

By J. R. White, S. W. Lambert, C. M. McCulloch

Examination of several coalbeds in Walker County, Ala., Cambria, Greene, and Fayette Counties, Pa., and Raleigh and Wyoming Counties, W. Va., indicates that cleat orientations are similar throughout a vertical sequence of strata. Studies of cleat orientation were carried out in underground mines that are operating in separate coalbeds vertically above one another. The data show that over a vertical separation of 100 to 400 feet, the average difference in coal cleat orientation between mines is 04° for the face and 08" for the butt cleat. Variations of coal cleat direction between coalbeds examined in strip-mined areas show similar values. Cleat orientations measured at outcrops agree well with the directions measured underground, suggesting that the amount of vertical separation between coalbeds has little effect on the resulting differences in cleat directions. The largest variation of cleat directions between adjacent coalbeds occurs where a large horizontal distance separates two sample locations. Cleat orientations for deeper coalbeds are most reliable where the data are taken from directly above.

Jan 1, 1976

By C. M. McCulloch

Examination of several coalbeds in Walker County, Ala., Cambria, Greene, and Fayette Counties, Pa., and Raleigh and Wyoming Counties, W. Va., indicates that cleat orientations are similar throughout a vertical sequence of strata. Studies of cleat orientation were carried out in underground mines that are operating in separate coalbeds vertically above one another. The data show that over a vertical separation of 100 to 400 feet, the average difference in coal cleat orientation between mines is 04° for the face and 08° for the butt cleat. Variations of coal cleat direction between coalbeds examined in strip-mined areas show similar values. Cleat orientations measured at outcrops agree well with the directions measured underground, suggesting that the amount of vertical separation between coalbeds has little effect on the resulting differences in cleat directions. The largest variation of cleat directions between adjacent coalbeds occurs where a large horizontal distance separates two sample locations. Cleat orientations for deeper coalbeds are most reliable where the data are taken from directly above.

Jan 1, 1976

By Cavallaro. J. A.

This report presents the results of a washability study of 455 raw coal channel samples with special emphasis on sulfur reduction. These raw coals contained on the average 14.0 percent ash, 1.91 percent pyritic sulfur, and 3.02 percent total sulfur. The complete washability data are presented for each sample processed. A statistical evaluation is included for the coalbeds from which more than 10 samples were collected and for the geographical coal producing regions. A graphical summation is presented for the coal producing regions and selected coalbeds. Finally a similar statistical evaluation is included showing composited data interpolated at Btu recovery levels of 50, 60, 70, 80, 90, and 100 percent. Graphical summations are presented for the various coal producing regions. Generally, significant sulfur reduction is achieved if the coals are crushed to a finer size and the higher specific gravity increments are removed. If a 50-percent Btu recovery was acceptable, then 32 percent of the samples tested could be upgraded to meet the current Environmental Protection Agency (EPA) standard of 1.2 pounds of S02 emission per million (MM) Btu when crushed to 14-mesh top size and separated gravimetrically.

Jan 1, 1976

By David E. Emerson

The Bureau of Mines has developed a mass spectrometer method for deter-mining the helium-3 content of high-purity helium. The work was performed to evaluate experimental methods for removing helium-3 from high-purity helium and to better determine the composition of pure helium used in research. This was accomplished by increasing the inlet sample pressure, ionizing current, and amplification of the current produced by the ions collected on a conventional mass spectrometer that had been modified. With these modifications, the helium-3 content was determined in the parts-per-million and parts-per-billion range in helium-4.

Jan 1, 1976

By W. P. Diamond, B. M. Bench, C. M. McCulloch

Coalbeds exhibit a directional permeability, with the maximum permeability oriented parallel to the face cleat. Thus, the most efficient pattern of vertical degasification holes for a coalbed is dependent upon cleat orientation. Surface joints, infrared photolinears, and Ronchi grating photolinears were investigated as potential estimators of subsurface cleat orientation. Cleat orientations were masured in 18 mines, in the Pittsburgh coalbed in southwestern Pennsylvania and northern West Virginia to be used as a standard against which prediction techniques would be evaluated. Two cleat systems with a strong geographic segregation were measured in the study area: N 67° W - N 28° E (95° separation) for the north, and N 76° W - N 17° E (93° separation) for the south. Directional data obtained from the three techniques investigated yielded satisfactory regional predictions of cleat orientation. Analysis of surface joints was the only technique considered sufficiently reliable on a local basis. Prediction of cleat orientation is based on the pairing of the principal directional sets into all reasonable combinations of fundamental systems. The system or systems composed of the most dominant sets nearest to 90° separation are likely to be a reliable prediction of cleat orientation. The most dominant set of the system selected is likely to be the face cleat.

Jan 1, 1976

By W. P. Diamond

Coalbeds exhibit a directional permeability, with the maximum permeability oriented parallel to the face cleat. Thus, the most efficient pattern of vertical degasification holes for a coalbed is dependent upon cleat orientation. Surface joints, infrared photolinears, and Ronchi grating photolinears were investigated as potential estimators of subsurface cleat orientation. Cleat orientations were measured in 18 mines, in the Pittsburgh coalbed in southwestern Pennsylvania and northern West Virginia to be used as a standard against which prediction techniques would be evaluated. Two cleat systems with a strong geographic segregation were measured in the study area: N 670 W -N 280 E (950 separation) for the north, and N 76° W -N 17° E (930 separation) for the south. Directional data obtained from the three techniques investigated yielded satisfactory regional predictions of cleat orientation. Analysis of surface joints was the only technique considered sufficiently reliable on a local basis. Prediction of cleat orientation is based on the pairing of the principal directional sets into all reasonable combinations of fundamental systems. The system or systems composed of the most dominant sets nearest to 90° separation are likely to be a reliable prediction of cleat orientation. The most dominant set of the system selected is likely to be the face cleat.

Jan 1, 1976

By D. A. Wilson

A laboratory method for processing lead battery scrap has been developed that eliminates virtually all of the S02 emission that normally is produced when a reverberatory or blast furnace is used. The method employs a hydrometallurgical step to convert the PbS04 to PbO and CaS04 by mixing the battery scrap with a slurry of Ca(OH)2. The reaction is exothermic and goes to completion in 2 to 5 minutes at room temperature. The dried product is mixed with a KC1-NaC1 flux and carbon and reduced at 6500 C. A minimum charge ratio of 3 parts of carbon to 100 parts of battery scrap is required for reduction. The process produces lead reductions and recoveries as high as 97.0 and 94.9 percent, respectively. The KCI-NaCl flux is recovered using a standard counter-current water leach followed by evaporation.

Jan 1, 1976

By G. M. Martinez

A cell concept adaptable to large-scale electrowinning of zirconium metal from zirconium tetrachloride was investigated by the Federal Bureau of Mines. Tests were made in twin cells, each 12 inches in diameter by 33 inches long. Electrowinning was performed in one chamber from which the electrolyte was transferred after electrolysis to the other chamber where it was renewed by the introduction of ZrC14 by direct sublimation. The formation of a salt plug in the connecting pipe provided a seal between the chambers. Optimum electrolyte composition, with respect to quality of the metal product (91 pct meeting ASTM standards except for the oxygen content) and current-carrying capability (about 350 amp) was determined to be 16.7 wt-pct NaF-83.3 wt-pct NaCl mixture plus ZrC14 equal to about 3 wt-pct zirconium. A twin-cell design incorporating the unit operations covered by this investigation is proposed.

Jan 1, 1976

By Martin Hertzberg

The concept of limit burning velocities is used to formulate a quantitative theory of flammability limits. Competing processes dissipate power from a combustion wave and quench propagation at some characteristically low limit velocity. There are four competing processes and one complication: (a) Free, buoyant convection, (b) conductive-convective wall losses, (c) radiation, (d) selective, diffusional demixing (the complication), and (e) flow gradient effects (flame stretch). These complexities are unraveled by creating an idealization that is initially freed from these competing processes. The ideal serves as a standard, and its burning velocity (Su), ideal is a unique function of the initial thermodynamic variables of state. By adding each process individually, it is possible to evaluate their significance, quantitatively, in terms of a limit velocity (Su)a , b , c , or e , and to explore the nature of their cooperative interactions. The larger the limit velocity, the more significant the process. The apparently diverse observations of flammability behavior are readily unified within this simple, conceptual framework.

Jan 1, 1976

By M. J. Ferrante

The standard enthalpy of formation, low-temperature heat capacities, and enthalpy increments above 298 K were determined by the Federal Bureau of Mines for synthetic dawsonite [NaA1C03(OH)21. The enthalpy of formation was determined by hydrochloric acid solution calorimetry, with the result ?Hf°298 = -469.4±0.7 kcal/mole. The low-temperature heat capacities were determined from 6 to 307 K by adiabatic calorimetry. Tabulated are low-temperature values of Cp°, S°, and H.-Ho° from 3 to 298 K. The derived entropy at 298 K is S298 = 31.55±0.3 cal/deg mole. Enthalpy increments above 298 K were obtained by copper-block drop calorimetry. Tabular data of Cp°, S°, H°-H°298, -(G°-H°298)/T, ?Hf°, ?Gf°, and log Kf are given from 298 to 477 K. Enthalpies and Gibbs energies of decomposition are also reported.

Jan 1, 1976