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By William C. McBee

Specialized sulfur concretes were developed by the Federal Bureau of Mines as a result of research for the beneficial utilization of sulfur in construction materials. Materials were developed for use in acid and salt corrosive environments where portland cement concrete has been found to deteriorate. Because the mineral aggregates also come into contact with the corrosive media, concretes were developed utilizing both limestone and quartz aggregates. The sulfur binder used with both aggregates was modified by reaction with 5 pct dicyclopentadiene to improve product durability. Sulfur quartz aggregate concrete was found to have moderately high strength characteristics (6,000 psi compressive) and was extremely resistant to chemical attack by both acid and salt solutions. Sulfur limestone aggregate concrete exhibited very high strength characteristics (9,000 psi compressive) and was extremely resistant to chemical attack of salt solutions. Both types of concretes maintained their strength and integrity after long-term testing in acid and salt solutions and exhibited considerable resistance to damage by the action of freezing and thawing. Potential uses include leach tanks, electrolytic cells, thickeners, bridge decking, industrial flooring, pipe, and tile.

Jan 1, 1979

By L. A. Stinnett

An investigation of hazardous surface openings of abandoned and inactive underground mines in the Black Hills area of South Dakota has revealed: (1) tracing legal ownership of mineral claims via county courthouses is confusing, complex, and oftentimes misleading, (2) in general, the selected mine openings in this investigation are to be considered relatively high in risks and hazard potential which poses a threat to the general public, (3) mine closure procedures and designs can generally be categorically implemented depending on the overall situation of the particular mine opening with subsequent unit costs estimates, (4) few preventive state or federal legal measures exist to date concerning mine closures, and (5) liability damages relating to mine opening accidents usually involve expensive and complex common law cases.

Jan 1, 1979

By Bruce T. Olenchuk, Wils L. Cooley

Electrical grounding is essential for the safe operation of power systems. A low-impedance path to ground is necessary to prevent the possibility of dangerously high potentials in human work areas. If for any reason this ground connection becomes faulty, a serious hazard may exist. One reason for faulty ground connections is ground bed corrosion. Corrosion of electrical ground rods has plagued the power industry and appeared in coal mine power systems. This paper will investigate ground rod corrosion, its cause, and possible solutions. Included is an evaluation of various ground rods for their ability to resist corrosion under stray current conditions. -The first known study of X-it3 Rod Corrosion is also presented.

Jan 1, 1979

By William H. Hamilton

This report describes the results and conclusions of the development and evaluation of a unique concept for a lightweight air powered drill tool for probe drilling in anthracite mines. A concept model of the lightweight air powered tool was constructed and evaluation testing conducted at the Kocher Coal Company Porter Tunnel Mine. The unique anchoring method proved to be extremely satisfactory and the overall light-weight air powered drill tool concept proved feasible. Based on the results of the concept model testing, two prototype production units were designed and manufactured. These prototype units proved to meet all of their design requirements of lightweight, portability, drilling controllability, structural integrity and miner acceptance. The need for a better bit and drill steel system, however, became evident during the testing program and recommendations are made for further investigation and development of a bit and drill steel system suitable for this application.

Jan 1, 1979

By Martin Hertzberg

A comprehensive study of the flammability behavior of air-dispersed coal dust was made using an 8-liter Bureau of Mines system which included the following: (1) An optical probe to continuously monitor the dust concentration; (2) measurements of ignition energy requirements; (3) the use of several narrow size distributions ranging from 3 to 65 µm in average diameter; (4) measurements of the extent of flame propagation based on pressure attained at constant volume, residual O2 content after combustion, and flame and dust surface temperatures. The measured lean limit for near-horizontal propagation of Pittsburgh coal dust was about 135 mg/l (milligrams per liter), virtually independent of particle size. Required ignition energies were hundreds of joules and measured limit flame temperatures were 1,450 to 1,600° K. Data on inerting? requirements with KHC03, rock dust, and NaC1 gave approximately the same results as full-scale explosion tests. The good agreement suggests that the cause of earlier discrepancies between small-scale laboratory data and full-scale mine experiments may not have been the difference in size, but were rather a problem of proper care in isolating and controlling the significant experimental variables and in consistently defining the extent of flame propagation at the limits.

Jan 1, 1979

By W. I. Nissen

This Bureau of Mines report presents the design for a commercial-sized flue gas desulfurization (FGD) demonstration plant that uses the citrate process. The goal of the Bureau's citrate process is to minimize the undesirable environmental impacts of industrial plants emitting SO2-bearing gas. The FGD plant is located at the George F. Weaton powerplant, Monaca, Pa. Construction was completed in April 1979 and will be followed by preliminary testing and a 1-year testing and evaluation program. Design capacity of the FGD plant is 156,000 scfm of 0.2-volume-percent-SO2 flue gas yielding about 16 tons of sulfur per day. The plant is intended to (1) clean fly ash, SO2, and Cl- from the gas while cooling the gas in a venturi scrubber, (2) absorb SO2 from the gas using 1,200 gpm of a countercurrent-flowing citric acid-sodium citrate-sodium thiosulfate solution, (3) react the absorbed SO2 in two 13,000-gal stirred closed vessels with added H2S, thus precipitating elemental sulfur and regenerating the citrate solution for recycle, and (4) recover the sulfur from the slurry by air flotation, followed by melting in a heat exchanger and separation from the occluded citrate solution in a sulfur decanter at 35 psi and 135° C.

Jan 1, 1979

By Anthony T. Iannacchione

The Bureau of Mines developed data on the methane content of the Hartshorne coalbed, Haskell and Le Flore Counties, Okla. The methane content is calculated to be between 1.1 and 1.5 trillion cubic feet, based on an estimate of total coal in place of 2.4 to 3.2 billion short tons. Methane increases with depth, but the rate of increase decreases with greater depths. Degasification in advance of mining is recommended for all mines operating at depths greater than 500 feet to reduce hazards and methane explosions, decrease mine ventilation costs, and conserve the natural gas that would be otherwise wasted.

Jan 1, 1979

By J. B. Stephenson

The Bureau of Mines, under an interagency agreement with the Department of Energy (DOE), investigated the feasibility of hardfacing the critical surfaces of valves and similar devices by chemical vapor deposition. The purpose of this research was to increase the wear resistance of these components for use in the abrasive and erosive environment of coal gasification units. Tungsten and molybdenum coatings were produced on nickel-plated carbon steels and stain-less steels by hydrogen reduction of the metal hexafluoride at 325° to 600° C. Titanium nitride coatings were produced on low-carbon steels by the reaction of titanium tetrachloride, hydrogen, and nitrogen at 1,000° C. Titanium carbonitride coatings were produced on low-carbon steels by the reaction of nitrogen, hydrogen, and methane at 900° C. Tungsten, molybdenum and titanium nitride coatings were formed on 6-, 10-, and l2-inch (0.15-, 0.25-, and 0.30-meter) ball valve seats for evaluation in the low-Btu coal gasification pilot plant at the Morgantown Energy Research Center, Morgantown, W. Va.

Jan 1, 1979

By A. E. Raddatz

The Federal Bureau of Mines, as part of its goal to minimize undesirable environmental impacts associated with mineral processing, has investigated a soda-smelting technique for processing ilmenite into pig iron and a titanium slag that is suitable for a feed to a sulfate-process titania pigment plant. By this procedure, the generation of ferrous sulfate waste and its associated disposal problem is obviated. Molten titania slag was quenched, water leached, and filtered to yield a sodium titanate intermediate product containing about 70 wt-pct Ti02, 1 wt-pct Fe, and 20 wt-pct Na20. This intermediate product, high-soda titanate (HST), was mixed with H2S04, calcined, quenched, and water leached to produce a low-soda titanate (LST) product that contained only 2 wt-pct Na20. Both the HST and LST were evaluated as feed materials for preparing titania by the sulfate process. About 95 pct of the Ti02 was extracted from HST and LST by digestion in concentrated or 50-wt-pct-H2S204 solutions. About 95 pct of the solubilized Ti02 was subsequently recovered from the titanyl sulfate solutions by hydrolysis. Barren solutions from hydrolysis, containing about 26-wt-pct H2S04, were upgraded by vacuum-thermal evaporation or electrodialysis. The regenerated acid solutions were used to digest additional HST and LST.

Jan 1, 1979

By Gerald L. Finfinger

The Bureau of Mines conducted an experimental degasification project in Island Creek Coal Co.'s Virginia Pocahontas No. S mine. Methane from the overlying Pocahontas No. 4 coalbed was entering mine workings in the Pocahontas No. 3 coalbed through fractures in the roof rock. Small-diameter (l-S/B-inch) holes were drilled into the overlying coalbed to reduce the gas pressure and intercept methane flows, which were piped to the surface through an underground 6-inch-diam steel pipeline. The total methane flow rate from the vertical holes averaged 150,000 ft3/day for the first month. Methane flows into the mine were reduced by 47 pet, thereby demonstrating the effectiveness of this form of degasification in reducing ventilation requirements and providing a safer working environment.

Jan 1, 1979

By M. L. Fenger, S. F. Mauser

This 1s a report on an Investigation performed during Contract No. H0166069 "High and Medium Voltage Trailing Cable Splices and Connections," which presents a summary of the requirements formulated. The requirements are presented in the form of considerations for medium-voltage splices, and medium- and high-voltage couplers used in underground coal mines.

Jan 1, 1979

By H. V. Makar

Ferrous fractions recovered from urban refuse were tested by the U.S. Bureau of Mines, U.S. Department of the Interior, to assess their character, composition, and response to detinning. This research was conducted as part of the Bureau's efforts to conserve mineral resources through recycling. Results from laboratory and pilot tests established the technical feasibility of detinning scrap recovered from household refuse. Detinned products containing less than 0.03 percent residual tin were produced. Concentrations of other residual elements were determined and compared with those in existing commercial scrap and with proposed specifications. Studies were extended to include evaluations under commercial conditions. Preliminary tests on 5-1/2 short tons of ferrous fractions revealed the need for adequate shredding to assure optimum metal-caustic contact and minimize retention of tin-bearing rinse solution in the final baled product. The washed metal product contained 0.06 percent residual tin. Subsequent melt tests showed a yield of 91.4 percent. Based on these studies, full-scale commercial demonstrations showed that detinned bales equivalent to No. 1 bundle quality could be produced in carload quantities. Up to 5 pounds of tin per gross ton of scrap is con-currently recovered during the detinning process.

Jan 1, 1979

By L. E. Schultze

As part of the Bureau of Mines research program on recovering alumina from domestic resources, methods for extracting iron from aluminum sulfate solutions (obtained by leaching kaolinitic clay with dilute sulfuric ,acid) were investigated. In countercurrent extraction experiments at a l-gal/hr flow rate of aluminum sulfate leach liquor, the iron concentration 'was decreased from 1.4 g/l to 0.01 g/l after four stages of using a primary amine extractant. The iron-loaded amine solution was regenerated in five stages using 3[N] sulfuric acid or in four stages using 6[N] sulfuric acid. The aluminum sulfate solution obtained was suitable for the preparation of alumina meeting cell-grade standards of less than 0.01 pct iron.

Jan 1, 1979

By M. M. Tilman

Etchants containing hexavalent chromium and sulfuric acid are used in a variety of surface-finishing operations. When the resultant spent solutions are discarded, substantial quantities of chromium are lost and pollution prob¬lems are created. To minimize the undesirable environmental effects while improving metal and minerals recycling technology, the Bureau of Mines is con¬ducting research on a method for the economic inplant recycling of these waste etchants. Trivalent chromium, produced when the etchant reacts with a substrate, is oxidized in the anode chamber of a diaphragm cell; other metals, dissolved during the etching operation, are transferred to the catholyte. When waste brass etchants are treated in this manner, all of the trivalent chromium is oxidized and more than 40 percent of the copper and zinc is removed. Similar copper removal and chromium oxidation are achieved with waste printed circuit board etchants and rinse waters from plastic etching operations. The electrical energy needed to regenerate 1 kg sodium dichromate is less than 9 kwhr. Regenerated brass etchants evaluated by two companies equaled or exceeded the performance of fresh etchants.

Jan 1, 1979

By T. G. Carnahan

The Bureau of Mines investigated a flotation-nitric acid leach procedure as part of the goal to maximize minerals and metals recovered from primary and secondary domestic resources. Studies were conducted on an ore that contained carbon-bearing and sulfide mineralization that rendered a portion of the ore refractory (resistant) to conventional leaching technology. The procedure investigated for treating the ore consisted of the following: (1) separation by flotation of the carbonaceous and sulfidic components from the ore, (2) leaching the flotation concentrate with nitric acid at 100° to 110° C, (3) leaching the flotation tailings with sulfuric acid, and (4) processing the combined leached slurries in a conventional manner to recover yellow cake. In step 2, HN03 is converted to gaseous products from which it is regenerated by reacting these products with air and water for further leaching. An overall uranium extraction of 96 pct was achieved by this procedure.

Jan 1, 1979

By T. E. Bernard

The CO2-absorbent canisters used in four approved rescue breathing apparatus were investigated. A breathing machine was used to simulate human expiration with gas flow rates of 26, 37, and 48 1/min of 3.5% CO2 in air. The exit gas CO2 concentration, the pressure drop across the canister, and the exit-gas temperature were monitored. The absorbent capacities of the packed-bed canister designs were found to be dependent on flow rate within the range studied, while the capacities of the other designs were less affected. The radial canister had the least resistance to breathing while the complex bed design proved to be the most effective in utilization of the chemical. The overall results indicated that LiOH (lithium hydroxide) has the highest capacity for CO2 absorption among the absorbents tested. It can be used in a simple packed-bed design while maintaining acceptable levels of resistance and exit-gas temperature. Examination of oxygen supply with respect to CO2-absorption capacity suggested that it is desirable to closely match CO2-absorption capacity with the avail-able O2 supply to minimize the size and weight of rescue breathing apparatus.

Jan 1, 1979

By David R. Flinn

This Bureau of Mines report describes methods to electrodeposit erosion-resistant titanium diboride coatings from molten alkali metal borate baths at 900° C. These coatings have been shown to be highly resistant to material loss during impingement with high-velocity alumina and silicon carbide powders, and they show promise as protective coatings to reduce metal loss in erosive chemical environments, such as coal gasification systems. The most erosion-resistant coatings were prepared on nickel, Inconel, and molybdenum from an electrolyte containing LiBO2, NaBO2, Na2Ti03, and TiO2. The best coatings were deposited at current densities of [~]20 ma/cm2, using titanium or titanium diboride anodes. Erosion-resistant coatings were shown to exhibit (1) a high degree of crystallographic orientation along the (100) or (110) planes, (2) a chromium impurity level of less than 3 pct, and (3) a uniform, smooth, consolidated surface appearance when viewed under a microscope or by scanning electron microscopy. Optical spectroscopic studies of the molten electrolyte suggest that the lower valent (+3) titanium ion predominates in the baths.

Jan 1, 1979

By H. -F. Krausse

Roof failures in underground coal mines are related to the lithology and geologic structure of the roof. There are two distinct suites of roof rock above the Herrin (No. 6) Coal in Illinois, and each has distinctive patterns of structure and roof failure. In black shale-limestone roof areas, roof instability is correlated with thinning of limestone beds and presence of faults and clay dikes. In gray shale roof regions, the prime roof hazards are posed by rolls, shear bodies, and presence of coal or carbonaceous partings in the roof. Most structural features examined are believed to have formed during early stages of sediment diagenesis and compaction. Structural trends and lithologic patterns are strongly interdependent for this reason. In many cases geologic patterns are so complex and locally variable that prediction of roof stability far in advance of mining is difficult. The need for greater flexibility in roof control planning is apparent.

Jan 1, 1979

By George N. Aul

This report describes a method developed by the Bureau of Mines for sealing horizontal degasification holes so that they do not create a gas explosion hazard when intercepted by mining. A cement slurry is pumped into the hole through an injection pipe that extends to the back of the hole. Pumping continues until the slurry returns through the annulus to the hole collar. The hole is then shut in and the grout allowed to harden. Application of the procedure to six horizontal degasification holes at Eastern Associated Coal Corp.'s Honey Run shaft is discussed.

Jan 1, 1979

By R. P. Beyer

[The Bureau of Mines has measured the low-temperature heat capacities and high-temperature enthalpies of crystalline K2Si2O5 as part of a program for advancing mineral resources technology with energy economy. High-temperature enthalpies of glassy and liquid K2Si2O5 and crystalline K2SiO3 were also mea¬sured. An adiabatic calorimeter operating over the range 5 to 308 K was used for the heat capacity measurements for K2Si2O5 from which the standard entropy at 298.15 K, S°298 = 45.55 ±0.05 cal/deg-mole, was calculated. Tabulated values of Cp°, S°, -(G° -HO°)/T, and H°-HO° from 5 to 300 K are given for K2Si2O5. A copper-block drop calorimeter was used in the enthalpy measurements, operating from 298.15 to 1,198 K for K2SiO3 and from 298.15 to 1,453.8 K for K2Si2O5. No transitions were found for K2SiO3. The KI2Si2O5 showed two reversible first order transitions, one at 510 K with a heat of transition of 0.29 kcal/mole and one at 867 K with a heat of transition of 0.38 kcal/mole. The heat of fusion for K2Si2O5 20 5 was calculated to be 8.42 kcal/mole. Relative enthalpies are given in equation form, and high-temperature values are tabulated for Cp°, S°, - (G°-H°298 )/T, and H°-H°298 . Also tabulated are ?H°, ?G°, and log K for formation of K2SiO3 and K2Si2O5 from both the elements and the oxides.]

Jan 1, 1979