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By F. P. Haver

The Bureau of Mines has investigated the electrochemical reduction of lead chloride as a method for producing lead without the pollution problems associated with smelting. It was determined that high-purity metal (>99.9 pct Pb) could be obtained, using PbC12 prepared by ferric chloride leaching of galena concentrate: PbS + 2FeCl3?PbCl2 + 2FeC12 + S°. Optimum results in small-scale electrolytic tests were achieved with a bath consisting of 40 to 70 wt-pct PbCl2 dissolved in KC1-LiCl eutectic, an operating temperature of 450° C, a current density of 2.5 amp/in2, and an electrode spacing of 0.5 inch. In large-scale tests made to develop a cell design for commercial application, the optimum electrode arrangement proved to be a bipolar configuration with horizontal plates. This gave a current efficiency of 86 pct with an energy requirement of 0.52 kwhr/lb lead. To determine the effect of impurity buildup in the bath, 1,200 lb of PbC12 prepared by ferric chloride leaching of galena concentrate was electrolyzed over a period of 2 months. Little deterioration of the metal quality occurred in that time; all of the lead produced had a purity equal to or better than corroding grade (>99.94 pct Pb).

Jan 1, 1976

By R. Blickensderfer

Several thin film absorber stacks with spectrally selective characteristics were developed by the Bureau of Mines. The stacks consisted of a silicon thick film or a zirconium compound thin film on a reflective thin film of silver. The zirconium absorber films, with the general formula ZrCxOyNz, were prepared by reactively sputtering zirconium or zirconium carbide in argon with small amounts of oxygen, nitrogen, or both, or by oxidizing zirconium films in air. A few similar types of films were prepared from titanium. The short-wave absorptance over the solar spectrum, a(s), and thermal emittance at 600 K, e(600 K), of the solar absorber stacks were calculated from room-temperature reflectance data. The values of a(s) ranged from 0.47 to 0.93, e(600 K) from 0.49 to 0.034, and the ratio a(s)/e(600 K) from 1.7 to 34. The specimen with the best combination of properties, a ZrNx-Ag stack, had a solar absorptance a(s) of 0.85 and a ratio, a(s)/e(600 K), of 24. The effect of film thickness and composition on spectral selectivity was determined. An emissometer for measuring normal total emittance up to 800 K and a method for determining a (s), e(T) (hemispherical), and a(s)/e(T) using simulated solar radiation are described. A calorimetric method for measuring a(s) and e(T) (hemispherical) at elevated temperature is also described. Measurements made on several specimens agreed favorably with calculated values.

Jan 1, 1976

By David E. Siskind

The Bureau of Mines studied environmental blast effects in six occupied residential structures. Airblast, ground, and structure vibrations were measured both inside and outside residences for seven quarry production blasts. Walls and floors responded to the blast noise and vibration by shaking at their own natural frequencies, often with greater peak particle velocities than the ground outside the structures or their foundations. The vibrations of the houses generated noticeable internal noise, correlating with the arrival of the groundborne energy. The later arriving airblast wave was predominantly at low infrasonic frequencies (1.0 to 1.5 Hz) and had similar amplitude and frequency characteristics both inside and out-side the structures. Significant structural motions resulted from the air-blast overpressures for at least two of the seven blasts. The most severe airblast effect occurred at a house 1,800 feet from a 5,047-pound (200-lb/ delay) blast. This stucture was subjected to a peak 0.16-in/sec particle velocity and 130 dB(L) airblast. The wall of the second floor responded to the ground vibration and airblast by shaking at particle velocities of 0.15 and 0.28 in/sec, respectively. Analysis of these data and those from additional field studies will be used to identify appropriate, safe, and reasonable impulsive noise levels, measurement techniques, and factors of design applicable to minimizing the adverse environmental effects of blasting.

Jan 1, 1976

By Israel Liebman

The Bureau of Mines developed three types of passive water barriers for suppressing slow-moving coal dust explosions. One type is a modification of a conventional tub barrier and depends on the dynamic pressure generated ahead of an explosion to tilt the tub to release its water and suppress the explosion. The other two barriers operate in response to an increase in static pressure developed ahead of the explosion. Tests indicate the first barrier begins to release its water at air speeds as low as 50 ft/sec, and the second and third barriers will operate at a rise in static pressure as little as 0.5 psi. All three barriers were found to be effective in suppressing coal dust explosions propagating at speeds as low as 100 ft/sec. A plan is described for installing a water barrier in a working mine on a trial basis.

Jan 1, 1976

By Martin Hertzberg

This Bureau of Mines study concerns the use of the tube bundle method as a sensitive and reliable detector of mine fires. The method involves the pneumatic, sequential sampling of many points in a system through branching tube bundles that lead to a single analytic station of high sensitivity, good reliability, and convenient location. Two serious limitations inhibit its use: the relatively slow response times for long lengths of narrow sampling tubes and the wall-diffusion losses for submicrometer smoke particulates. These limitations were quantitatively evaluated by measuring tube transit times and smoke particulate transmissions as a function of tube length, diameter, and pressure drop. The comparison of the data with theory offered the challenge of extending the classical, incompressible flow solutions to the two compressible cases: isothermal and adiabatic. New equations were derived for these cases, and the measured transit time data gave reasonable agreement with calculated solutions in both the laminar and turbulent regimes. The measured transmission losses of smoke particulates from several combustion sources compared favorably with those expected from Brownian diffusion losses to the interior walls of the sampling tubes. Traveltime and smoke transmission graphs are provided and, pump power requirements are estimated.

Jan 1, 1976

By Seth C. Schaefer

The Federal Bureau of Mines studied the Gibbs free energies of formation of chromous fluoride (CrF2), chromic fluoride (CrF3), and chromium (II,III) fluorides (CrF2.40 and CrF2.45) with high-temperature galvanic cells employing calcium fluoride doped with 1 mole-pct yttrium fluoride as the electrolyte. Free-energy changes were obtained from open-circuit potential measurements for the following cells: Cr, CrF2 // CaF2 // NiF2, Ni (a) NiO, NiF2 // CaF2 // CrF3 , Cr203 (b) CrF2 , CrF2.40 // CaF2 // NiF2, Ni (c) and CrF2 ?45 , CrF3 // CaF2 // NiF2, Ni (d) with the following overall reactions Cr(s) + NiF2 (s) = Ni(s) + CrF2 (s) (1) 3NiO(s) + 2CrF3 (s) = 3NiF2 (s) + Cr203 (s) (2) 5CrF2 (s) + NiF2 (s) = 5CrF2.4O (s) + Ni(s) (3) and 3.64CrF2.45 + NiF2 (s) = 3.64CrF3 (s) + Ni (s) . (4) These results were combined with the best available literature values of ?Gf° of NiF2, NiO, and Cr203 to deduce Gibbs free energies of formation for the chromium fluorides expressed as follows: ?Gf°(CrF2) = -179.31 + 24.33 X 10-3T ± 0.43 kcal-mole. (5) (858.1 - 964.9 K) ?Gf° (CrF3) _ -226.16 + 1.82 X 10-3T ± 0.79 kcal/mole (6) (880.8 - 957.8 K) ?Gf°(CrF2.40) _ -213.65 + 32.14 X 10-3T ± 0.44 kcal/mole (7) (0053.9 - 936.8 K) and ?Gf°(CrF2.45) _ -176.17 - 12.67 X 10-3T ± 0.80 kcal/mole (8) (875.1 - 937.6 K). Free energies and equilibrium fluorine pressures for three univariant and one bivariant equilibria are illustrated.

Jan 1, 1976

By H. H. Fields

The Bureau of Mines conducted research to determine the effectiveness of long holes drilled in solid virgin coal in degasifying an area of the Pittsburgh coalbed showing that horizontal holes drilled into a virgin coalbed from the bottom of any shaft will effectively remove methane gas in commercial quantities from the Pittsburgh coalbed. The in situ pressure at a depth of 214 feet into the coalbed and the average gas and water flows from the five degasification holes were 3 lb/in2 gage and 860,000 ft3/d and 1.7 gal/min, respectively. On June 19, 1975, after 593 days of degasification, a compressor was installed and pipeline quality gas was introduced into a commercial pipeline. As of June 1, 1976, after 1,022 days of degasification, over 753 million cubic feet of gas had been drained and 117 million cubic feet of gas had been purchased by the gas company for use in the local community of Wadestown, W. Va. The gas drained to date is six times the gas estimated to be in the area subtended by the holes. Methane emissions at the working face of 1 West mains, Federal No.2 mine has been reduced by 50 pct, proving the value of methane drainage by horizontal degasification holes drilled from shaft bottoms ahead of mining.

Jan 1, 1976

By Joan T. May

The Federal Bureau of Mines investigated the potential for recovering aluminum from copper-dump leach liquors by use of single-contact ion-exchange technology. A strongly acidic ion-exchange resin was used to extract aluminum from a typical dump leach liquor and from synthetic leach liquors. Aluminum was stripped from resin with a HS04 or NaCl solution. Bench-scale experiments indicate that a single-contact ion exchange is technically feasible, but that the process is limited by the relatively low loading capacity of the resin and the excessive amount of stripping agent required. A further limitation is that significant amounts of magnesium and iron are loaded and stripped along with the aluminum.

Jan 1, 1976

By Robert W. Freedman

Vacutainers are used by the Bureau of Mines and the Mining Enforcement and Safety Administration (MESA) for sampling mine air and products of combustion. Tests were conducted on both 10-ml and 30-ml sizes to study shelf life stability during storage, pretreatment of stoppers, and handling of a wider range of compounds. A chamber was constructed to provide convenient, efficient evacuation of the Vacutainers shortly prior to use. Fixed gases and C1 ?C5 hydrocarbons could be stored for 1 week or more after sampling. Where decreases occurred (C02 and C3-C5 hydrocarbons), they were predictable as a function of storage time. An unexplained phenomenon, slow accumulation of CO in evacuated Vacutainers, occurred after a few weeks of storage. The levels were low and time dependent. Attempts to eliminate this behavior by pretreating the stoppers were unsuccessful.

Jan 1, 1976

By M. J. Sapko

The pressure and flame development of the methane-air-nitrogen system was investigated in the Bureau's l2-foot-diameter sphere to define buoyancy effects and to develop relationships for predicting venting requirements. Pressure rise (?P) is defined as a function of time (t) and nitrogen dilution and is shown to deviate noticeably from the cubic law (?P = kt3), depending upon the period of combustion and the mixture composition. Corresponding flame speed (Sf) and burning velocity (Su) data are given which show that Sf is time dependent and that Na dilution has a greater effect than air dilution in inhibiting the flame propagation. The Su data agree with "accepted" values and are unique in that they are based on much larger flames than those used in other investigations. Downward propagation limits are shown to depend mainly upon buoyant forces, which can affect the burning of even stoichiometric CH4-air systems. Theoretical expressions, based on the mixture burning velocity and expansion ratio, are given for predicting the venting requirements for ignitions of hydrocarbon-air-nitrogen mixtures in spherical or cubical enclosures.

Jan 1, 1976

By Raymond M. Stateham

The Bureau of Mines evaluated temperature increases on the heads of resin-grouted bolts as indicators of the integrity of the anchoring of the bolt. Expected increases were calculated by the finite difference method; the calculations were checked by bolthead temperature measurements, both in the laboratory and in the field. The accuracy of the calculations varies with the validity of assumptions necessary to the process. Measurements in the laboratory produced a temperature rise of about 4.00 F on the head of a 4-foot bolt when installed with a full column of resin. This increase remained for about 30 minutes. Similar increases were noted on bolts installed at the White Pine mine, White Pine, Mich., but bolthead temperature increases in the mine lasted only about 10 to 15 minutes. When partial columns (reduced amounts) were used, the temperature increases were smaller.

Jan 1, 1976

By Roy E. Peterson

The Bureau of Mines conducted an investigation to produce metallized pellets from domestic iron ore superconcentrates using lignite and subbituminous coal as reductants. Feed materials for the metallizing process consisted of commercially indurated iron oxide pellets and green pellets prepared from upgraded domestic concentrates with graphite or limestone as internal additives. Durability of the green pellets during metallization was investigated in tests conducted in a 7-inch-ID rotating drum furnace. Test results indicated that the major cause of pellet disintegration with the concentrates used was the tumbling action during reduction rather than forces generated within the pellets. In larger scale tests made in a 34-inch-ID by 35-foot-long kiln, the previously indurated pellets were metallized with lignite at 1,030° C with little disintegration. A 96-percent level of metallization was obtained in pellets having an average compressive strength of 420 lb. In subsequent, similar tests using green pellets containing graphite or limestone, pellet disintegration was more severe, with 10 to 40 percent of the feed being lost as dust. The surviving pellets had metallizations ranging from 88.3 to 94.4 percent and compressive strengths ranging from 60 to 68 lb.

Jan 1, 1976

By A. F. Colombo

The western Mesabi range nonmagnetic taconites containing about 34 percent Fe were evaluated by the Bureau of Mines in a 900-pound-per-hour pilot plant employing a selective flocculation-desliming-cationic flotation technique. The flotation step was a reverse flotation process and involved the flotation of the gangue minerals. The objective of the research was to increase the availability of domestic raw materials for the iron and steel industry. The beneficiated ores yielded concentrates containing 62 to 64 percent Fe and less than 5.5 percent Si02 with accompanying iron recoveries that averaged about 75 percent. Comparable flotation results were obtained with either fresh or 80 to 90 percent reclaimed water. Recycled waters having turbidities as high as 5,000 ppm Si02 did not affect the flotation process. Reclaimed waters containing residual calcium contents of less than 10 ppm gave better flotation concentrates than those containing 15 ppm.

Jan 1, 1976

By Philip C. Tully

This Bureau of Mines report contains experimentally determined vapor-liquid equilibria data for a helium-nitrogen-methane mixture with a nominal composition of 15, 60, and 25 mole-percent, respectively. Measurements of the equilibrium phase compositions were obtained by means of a windowed cell, in conjunction with an automated chromatograph and a special analyzer for low helium concentrations. The data presented include a comprehensive table and eight graphs depicting phase compositions, vaporization ratios, and correlations with a previous study of two helium-nitrogen-methane mixtures of different compositions.

Jan 1, 1976

By Stephen A. Hare, O&apos

Powder metallurgy processing of commercial Raney nickel powders was examined. The typical angular particle shape, in conjuction with aluminum present in a eutectic phase, facilitated interlocking leading to excellent green strength after compaction. Density and porosity as influenced by the compacting pressure were studied over the range of 37.5 to 207 meganewton per square meter (MN/m2). Sintering in an inert atmosphere from 575° to 850° C caused a volume increase which is attributed to a solid state reaction between Al and Ni2Al3 phases. The reaction is 3Al + Ni2Al3 ? 2NiA13. A thermal pretreatment of 70 hours at 700° C was required to prevent this reaction from occurring during sintering. Density and porosity as a function of compacting pressure and sintering temperature were determined after a thermal pretreatment of the powder.

Jan 1, 1976

By Mark I. Copeland

Bureau of Mines researchers investigated the combined effect of copper and tin additions on the mechanical properties of hot-rolled steels. Wrought steels containing 0.2 wt-pct C and up to 0.2 and 1.0 wt-pct Sn and Cu, respectively, were made and evaluated by conducting tensile and impact tests and electron-beam microprobe and electron microscopy examination. Tin additions did not significantly affect the tensile properties of steel at different copper contents in the hot-rolled condition. Tin lowered the copper content at which strengthening by copper precipitation normally starts, 0.8 wt-pct, and decreased the strength of steel aged at 1,022° F (550° C). The most adverse effect of tin was lowering the notch toughness of steels at most copper contents.

Jan 1, 1976

By L. L. Oden

The Bureau of Mines is conducting research to develop methanation catalysts for converting synthesis gas derived from coal to synthetic natural gas. This report describes a method to prepare supported Raney nickel coatings by dipping screen-covered nickel sheet in molten aluminum-nickel alloy. Coatings were formed at 1,050° C that were comparable in thickness, composition, microstructure, and catalytic properties to flame-sprayed commercially pre-pared Raney nickel. A molten salt comprising cryolite-8 wt-pct LiF was employed over the molten metal bath to clean and preheat the substrates, to protect the metal bath from oxidation, and to heattreat the coated specimens. Immediately following heat treatment, specimens were quenched to 700° C in a molten salt bath containing CaC12-34.5 wt-pct NaCl, which also functioned to remove the insoluble occluded fluoride salt.

Jan 1, 1976

By Wallace W. Roepke

The Bureau of Mines studied the cutting characteristics of point-attack bits to reduce airborne respirable dust and energy during cutting. Linear cutting of two coal types using four bit types at three depths of cut with three space-depth ratios was performed with a modified horizontal milling machine using an optical particle-size monitor for respirable dust sampling. The cutting action of one bit on a rotary hardhead mining machine was mathematically analyzed and compared with the results of the linear cutting test. Airborne respirable dust per unit mass cut (specific dust) was found to be a monotonically increasing function of specific energy. Specific dust and energy decrease with increasing depth of cut. The amount of nonairborne respirable dust was 100 to 1,000 times greater than the airborne dust. The plumb-bob bit produced the most airborne respirable dust and the highest specific energy of the four bits tested. Rotary cutting was a greater dust producer and energy consumer than linear cutting because of the constantly changing depth of cut, space-depth ratio, and attack angle of the bit relative to the horizontal bedding planes. A new cutting technique is proposed to minimize the existing problems of the rotary cutting machines by providing greater production, reduced dust, and minimized methane ignition potential at the face.

Jan 1, 1976

By Daryl R. Tweeton

The Bureau of Mines compared the effects of surface-active chemicals with those of pure water on core-drilling rock and quartz and on fracturing quartz. The objectives were to determine if these chemicals assist drilling and fracturing rock and if zeta potential control was worth pursuing as an aid to full-scale drilling. All tests were performed in the laboratory. No significant increases in drilling rates were observed for 1 to 10,000 ppm Al (as AlC13) in flushing water when drilling microcline or serpentine, nor for 1 to 10,000 ppm Mg (as MgC12) when drilling microcline or marble. Concentrations near those giving a zero zeta potential were used with microcline and marble. A 50-pct rate increase was observed for drilling quartz in 0.7 ppm oleylammonium acetate, which gave a zero zeta potential. No other concentrations were used. No effect on the tensile strength of quartz thread in 0.05 ppm Al (as AlC13), which gave a zero zeta potential, was observed. Heptanol, reported to give a zero zeta potential on quartz, did not reduce the bending strength of small quartz bars below that in water. These generally negative findings raise doubt about the usefulness of zeta potential control in full-scale drilling. The results, combined with previous studies, suggest that controlling physical properties of drilling fluids, such as viscosity, is more useful than altering chemical properties.

Jan 1, 1976

By K. O. Bennington

Thermodynamic properties were determined by the Federal Bureau of Mines for lithium metasilicate (Li2Si03) and lithium disilicate (Li2Si205). Their enthalpies of formation were investigated by hydrofluoric acid solution calorimetry. The standard values are ?Hf°298 -393.8 ± 0.8 kcal/mole for Li2Si03, and ?Hf°298 -611.8 ± 1.0 kcal/mole for LiSi205. Enthalpy increments above 298 K were measured by copper-block drop calorimetry from 298 to 1,404 K for Li2Si03, and from 298 to 1,281 K for Li2Si205. Low-temperature heat capacities were determined adiabatically from 6 to 305 K for Li2Si205 only. The derived standard entropy is S°298 = 29.20 ± 0.10 cal/deg-mole. The various experimental data were combined with other data from the literature, and resulting properties of ?Hf°, ?Gf°, and log Kf were tabulated as a function of temperature.

Jan 1, 1976