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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, T. W. Goodman, Joseph Cervik

The Bureau of Mines conducted research to determine the effectiveness of long holes drilled in solid virgin coal in degasifying an area of the Pitts- burgh 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 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 Edward D. Thimons

Several types of inflatable stoppings, developed under Bureau of Mines contract for use as mine air barriers during underground production, have been tested by the Bureau. All of the stoppings tested showed significant internal leakage initially but, in all but one stopping, the leaks were sealed with limited effort The stoppings were tested underground in two western noncoal mines under production conditions. The results from the Colorado molybdenum mine showed the stoppings to be generally unsatisfactory for daily mine usage if they are deployed near blasting areas or in locations where near-perfect air seals are required. They were very susceptible to blast damage and seldom were better than 90 percent efficient as air barriers. However, stoppings tested in the New Mexico uranium mine were located substantially distant from any blasting. Because slight leakage past the stoppings was acceptable, they proved very satisfactory in that application.

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 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

By J. A. Eisele

The Federal Bureau of Mines is engaged in a continuing program on the recovery of alumina from domestic source materials. Of the six processes being studied, current efforts focus on HCl leach of clays. A key step in the HCI process is the removal of iron from the aluminum chloride leach liquor. This was accomplished .by solvent extracting the iron with a tertiary amine in kerosine to which decanol was added as a phase modifier. In a mixer-settler operation, iron in the raffinate was reduced to <10 ppm in two extraction stages from a feed containing 1.4 gil Fe. Iron was stripped from the organic phase in three stages with dilute HCl.

Jan 1, 1976

By G. W. Murrie, W. P. Diamond, S. W. Lambert

A geologic study of the Mary Lee Group of coalbeds in the Black Warrior coal basin was undertaken to examine coal stratigraphy and determine regional trends and extent of the coalbeds. The area investigated encompasses 835 square miles in Jefferson, Walker, and Tuscaloosa Counties, Ala. More than 700 core logs were used to construct a structure map, coal, interval, and overburden isopachs, and cross sections. There is evidence that structure affected sedimentation. Coalbed isopachs indicate the Mary Lee Group was deposited in fluvial-deltaic and low-lying coastal plain environments. The Mary Lee coalbed is the only coalbed which is continuous throughout the area, commonly with two benches which have a combined thickness of 2 to 12 feet. The Mary Lee coalbed changes rank in the basin from high- through medium- to low-volatile coal. The methane gas potential of the Mary Lee Group coals is estimated to be greater than 1 trillion cubic feet. There is an excellent correlation between the orientation of surface cleats with those measured underground in the Mary Lee coalbed. The face cleats roughly parallel the axes of the area&apos;s folds and trend northeast-southwest.

Jan 1, 1976

By G. W. Murrie

A geologic study of the Mary Lee Group of coalbeds in the Black Warrior coal basin was undertaken to examine coal stratigraphy and determine regional trends and extent of the coalbeds. The area investigated encompasses 835 square miles in Jefferson, Walker, and Tuscaloosa Counties, Ala. More than 700 core logs were used to construct a structure map, coal, interval, and overburden isopachs, and cross sections. There is evidence that structure affected sedimentation. Coalbed isopachs indicate the Mary Lee Group was deposited in fluvial-deltaic and low-lying coastal plain environments. The Mary Lee coalbed is the only coalbed which is continuous throughout the area, commonly with two benches which have a combined thickness of 2 to 12 feet. The Mary Lee coalbed changes rank in the basin from high-through medium-to low-volatile coal. The methane gas potential of the Mary Lee Group coals is estimated to be greater than 1 trillion cubic feet. There is an excellent correlation between the orientation of surface cleats with those measured underground in the Mary Lee coalbed. The face cleats roughly parallel the axes of the area&apos;s folds and trend northeast-southwest.

Jan 1, 1976