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By John L. Ellenberger

The Bureau of Mines investigated the occurrence of slickensides in mine roof in the Pittsburgh coalbed in a portion of the Valley Camp No.3 mine in southwestern Pennsylvania to improve the potential for prediction of slicken-sided zones and determine the orientations of the most prominent slickensided planes. Two distinct types of slickensides were identified; those which were associated with clay veins observed in the coalbed (genetic), and those which were unrelated to any visible structure (nongenetic). The study draws three conclusions: (1) Nongenetic slickensides are not the result of tectonic forces, (2) both genetic and nongenetic slickensides tend to dip at an angle of 30°, and (3) genetic slickensides tend to be alined parallel to the trend of the clay vein and usually dip toward the center of the clay vein. A schematic roof bolting plan is presented that may provide improved roof support where slickensides are present. Roof stability could be improved by supplemental bolting in the direction normal to the plane of slickensides.

Jan 1, 1979

By William J. Campbell

This Bureau of Mines report describes a study conducted to determine the relationship of mineral habit to particle size and shape characteristics for prismatic, acicular, fibrous, and asbestiform varieties of tremolite. Particle measurements were made with the petrographic microscope at X 1,250 and the scanning electron microscope at magnifications up to X 10,000. All of the varieties of tremolite, upon Wiley milling, produced a significant percentage of particles that meet the Federal regulatory criteria for counting as asbestos fibers. However, only the asbestiform variety gave milled particles that fell into a size range of >10 µm in length and <0.5 µm in width; some medical scientists consider this range significant for production of adverse health effects.

Jan 1, 1979

By C. D. Messelt

The Bureau of Mines investigated the application of a diffusion model to sintering rate data developed for lithium titanium ferrite. The data were obtained by sintering pressed pellets under identical conditions for various times up to 11 hours. Stereological measurements were made on polished sections, and sintering rates were calculated. A model for intermediate stage sintering was fitted to the stereological data. This procedure produced a method by which these type data could be used to study the relative importance of volume and grain-boundary diffusion under a variety of sintering conditions.

Jan 1, 1979

By G. R. Palmer

The Bureau of mines evaluated the elution of uranyl carbonate from a strong base resin with a mixed carbonate eluant in a fluidized system. The system consisted of a multiple-compartment ion-exchange (MCIX) elution column with a continuous flow of solution, except for short periods when the resin increments were withdrawn. The exchange of uranyl carbonate from the mill-loaded strong base resin with an eluant composed of 1.0 [M] NaaCOs plus 1.0 [M] NH4HCO3 was studied. The effects of solution flow rate, aqueous-to-resin flow ratio, column diameter, compartment height, initial resin concentration, and column length were examined. The experimental data indicate that for the eluant examined, a resin residence time of 240 minutes is necessary to attain 90-percent elution efficiency. Also provided is a technique for sizing an elution MCIX column form pilot plant experimental data.

Jan 1, 1979

By Richard G. Sandberg

The Bureau of Mins, U.S. Department of the Interior, is investigating a hydrometallurgical procedure to conserve cobalt, nickel, and copper by recovering the metals from the matte byproducts of smelting Missouri lead ores. For want of adequate processing technology the mattes are now either unmarketable or marginally so. The procedure involves leaching with manganese dioxide and sulfuric acid to obtain copper, nickel, cobalt, lead, and manganese sulfates, and elemental sulfur as expressed by the following reaction: MS + MnO2 + 2H2SO4 ? MSO4 + MnS04 + S° + 2H2O, where M = Cu, Ni, Co, and Pb. The leach solutions, containing near theoretical amounts of sulfuric acid and manganese dioxide at 85° to 100° C, convert up to 98 pct of the cobalt, nickel, and copper in the mattes to sulfates in less than 2 hr. As they are formed, the cobalt, nickel, and copper sulfates are dissolved leaving a residue of lead sulfate, lead, sulfur, and gangue. The soluble metals are recovered from the leach solutions by caustic and sulfide precipitation, and the residue returned to the smelter for lead recovery. The manganese can be reclaimed from the spent leach liquor as manganese oxide and recycled to leaching.

Jan 1, 1979

By N. A. Gokcen

In this Bureau of Mines report, appropriate equations correlating the activity of water with the activities of electrolytes in binary and multicomponent solutions have been derived for computer calculation. It was found that the half-integer power series are far superior to the integer power series, for both types of series having the same number of terms. The pro-posed method of calculation is capable of accurately yielding the activities of all components from the measurements of the activity of a single component at various concentrations. This method replaces the cumbersome and objection-able method of graphical integration of the Gibbs-Duhem equation. Two novel methods are proposed for determination of activities of electrolyte solutions important in hydrometallurgy; (1) Water vapor pressure measurement by differential pressure transducers having an accuracy of 0.001 pet, and (2) transpiration method with an inert gas bubbled through concentrated solutions followed by the analysis of the evaporated and redissolved electrolytes with specific ion electrodes having a sensitivity of ±10-10 molal. The first method is suitable for nonvolatile electrolytes, and the second, for volatile electrolytes such as hydrogen halides, HN03, H2S03, etc. The existing methods of estimation of ionic activities have been surveyed, and the best method has been selected, discussed, and summarized.

Jan 1, 1979

By Yael Miron

Ammonium nitrate-fuel oil (AN-FO) mixtures are used as blasting agents in mining pyrite-bearing ores. The temperature of these ores can increase by the continuous, though at times slow, oxidation weathering of the pyrites. At elevated temperatures, AN-FO reacts exothermally with pyrite, and the reaction becomes self-sustained at 120° C ± 10° C. The Bureau of Mines has conducted an investigation to determine the reactivity of mixtures of AN-FO with pyrite containing ferrous sulfate. The results of tests in a heated vessel simulating a hot borehole demonstrate that small amounts of ferrous sulfate, a major product of pyrite weathering, initiate a self-sustained exothermic reaction with AN-FO at 80° C. Five pct by weight of urea was found sufficient to prevent a reaction among the three ingredients, at least within the limits of the test, which reached 180° C. Smaller amounts of urea and of potassium oxalate slowed down the reaction and delayed its onset to higher temperatures, but did not prevent it.

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.&apos;s Honey Run shaft is discussed.

Jan 1, 1979

By D. M. Soboroff

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 conducting research on a method for the economic inplant recycling of these waste etchants. Trivalent chromium, produced when the etchant reacts with a sub¬strate, 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 R. R. Brown

The solubility and the activity of aluminum chloride hexahydrate, A1C13?6H2O, in aqueous solutions were determined as a part of the Bureau of Mines, U.S. Department of the Interior, research to improve mineral processing technology for recovering alumina from low-grade domestic resources. The solubility of A1C13 in pure water was found to be 31.09 and 31.77 wt-pct at 25° and 85° C, respectively, and decreased drastically to 10 and 0.1 wt-pct when the respective amounts of 20.3 and 37 wt-pct hydrochloric acid (HCI) were added in solution. The equilibrium constant for the solubility of hexahydrate, activities, and activity coefficients of A1C13 and H2O were calculated and compared with the results from the available methods of estimation. The results were shown to be useful in leaching nonbauxitic ores for extraction of alumina by changing the solubilities of component salts upon addition of HC1. Simultaneous solubilities of A1C13, FeC13, KC1, and NaC1 in solutions of HC1-H2O were also determined and their effects on the purity of A1C13?6H20 crystallized from mixed salt solutions are briefly discussed.

Jan 1, 1979

By Philip Thompson

A part of the Bureau of Mines mission is to help improve the Nation&apos;s mineral posture by providing the technology for utilizing low-grade ores. In this regard, laboratory testing by the Bureau of Mines has shown that the removal of insoluble slimes using selective flocculation and flotation is a viable method for treating low-grade potash ores that have a high content of water-insoluble impurities. Results indicated that over 82 percent of the insoluble slimes could be removed from sylvinite ore containing 5 percent water insolubles and 13 percent K20 by using nonionic or cationic polyacrylamide flocculants and cationic, anionic, and/or nonionic collectors. Subsequent potash flotation recovered 87 percent of the potash in rougher concentrates containing 57 percent K2O. Sizing and cleaner flotation of the rougher concentrates upgraded the products to 60 percent K2O. Filtration of the water-leached insoluble-slimes flotation concentrates on a bed consisting of leached insoluble-slimes concentrate mixed with potash flotation tailings recovered 80 percent of the brine. Filtration rates using the mixed bed were nine times faster than filtration rates obtained when the insoluble-slimes flotation concentrates were filtered separately.

Jan 1, 1979

By R. H. Nafziger

Bureau of Mines research has shown that very low-sulfur pressure vessel steels with improved mechanical properties can be prepared by two melting processes. Four pressure vessel steels having sulfur contents ranging from 0.0008 to 0.0040 wt-pct, were produced by the electric-arc furnace or by the electroslag processes. Calcium carbide was used as a desulfurizer in the electricarc furnace. Fluxes containing at least 40 wt-pct CaO provided sufficient desulfurization during electroslag remelting. Element recoveries were higher for electroslag remelting than for metal melted in the electric-arc furnace. Bar rolled from electroslag-remelted ingots generally possessed higher tensile strengths and ductility than bar rolled from it t melted in the electric-arc furnace. Charpy V-Notch upper shelf energies were also improved as a result of electroslag remelting. The primary failure mode during impact testing was was microvoid coalescence. Sulfide inclusions were minimal, especially in the electroslag-remelted material.

Jan 1, 1979

By A. B. Campbell

The Bureau of Mines is developing alloys using ion implantation as an alternative to bulk alloys that consume large quantities of strategic materials such as chromium and nickel. These alloys are formed at the outer layer of relatively common materials. To more fully understand the corrosion characteristics and physical properties of this outer layer, it was necessary to deter-mine the alloy concentration as a function of depth into the substrate material. Also, since many of the ion-implanted alloys would be utilized at elevated temperatures, it was necessary to determine the diffusion behavior of the implanted element. Proton-induced X-ray emission and inert gas ion sputtering have been utilized to generate composition depth profiles for Fe-Cr, Fe-Ni, and Fe-AI ion implanted alloys fabricated by implanting 25-kev Cr+, Ni+, or AI+ into iron substrates. The data were fitted (utilizing a computer program) with symmetrical Gaussian profiles yielding values for the range and range straggle of the ions. These parameters were then compared with those calculated from theory. Changes in the profiles due to annealing were investigated and values for the diffusion coefficient were obtained assuming diffusion according to Fick&apos;s Law. For the Cr+ and Ni+ implantation, the profiles as-implanted agree reason-ably well with theory and exhibit ?norrmal" diffusion characteristics at 500° C. For the Al+ implantation, the profile as-implanted is much broader than predicted and exhibits substantial enhanced diffusion at temperatures up to 500° C.

Jan 1, 1979

By Robert C. Gabler

Evaluation of incinerated sewage sludge as a secondary resource for aluminum, phosphorus, and minor constituents such as copper and zinc was initiated as part of the Bureau of Mines secondary resource program. The elemental composition of sludge ash for 14 plants in 11 U.S. cities was determined. Comparing industrialized cities with cities where most of the sewage is domestic, significant differences in heavy metal content were noted. Various parameters were investigated affecting the extraction of metals and phosphorus from a typical industrial city sludge ash and from a Palo Alto, Calif., sludge ash with a high precious metal content. Three extraction-recovery procedures for metals and phosphorus using sulfuric acid leaching, ion exchange, and various precipitation techniques were investigated. The last procedure developed was a combination approach using a three-stage countercurrent sulfuric acid leach that recovered most of the economic values from the sludge ash and also removed the leachable fraction of elements of environmental concern.

Jan 1, 1979

By Harold L. Rhodes

The Bureau of Mines has developed a method for determining the H2S content in natural gas samples. A gas chromatograph with a flame photometric detector was used to analyze samples with H2S concentrations ranging from 5,000 ppm to a minimum detectable limit of 0.01 ppm. A mass spectrometer was used to analyze samples containing H2S in amounts greater than 5,000 ppm. Methods are presented for preparing containers for H2S samples and for preparing standards using partial pressure and weighed standard methods, Sample collection techniques are discussed, as are analytical results which illustrate the loss of H2S while in the sample container and provide a basis for evaluating containers used for sampling and standard preparation.

Jan 1, 1979

By Edward D. Thimons

Because of the high number of accidental methane gas ignitions in metal and nonmetal mines, the Bureau of Mines searched for a simple guideline that would allow mine personnel to evaluate the methane hazard in a given mine. Air samples were collected by the Bureau in 53 metal and nonmetal mines and analyzed for trace evidence of methane gas. Samples were collected in the returns and at the working faces. Those mines classified as gassy by the Mine Safety and Health Administration had a significantly higher average methane concentration than those classified as nongassy. Of the 9 gassy mines sampled, 7 had methane concentrations above 100 ppm, whereas only 1 of the 44 nongassy mines had a concentration above 100 ppm. The 100-ppm concentration may be used as a simple and convenient guideline for forecasting the methane hazard in a mine, whether or not the mine is classified as gassy. There was no consistent correlation between commodity mined and methane concentration, nor was there a correlation between mine depth and methane concentration. Neither of these factors can be considered a guideline for predicting methane hazards.

Jan 1, 1979

By G. R. Smith

This report describes research carried out by the Bureau of Mines to develop new technology for electrorefining metals at much higher current densities than those normally used in commercial practice, preliminary studies using rotating-ring and cylinder electrodes to increase the mass transport of copper are discussed. Following this work, single- and multichannel cells were developed that utilized a high electrolyte flow in the channels formed by the anode-cathode pairs. Using these cells, copper was successfully refined at current densities in the range of 70 to 300 amp/ft2. The effects of flow rate, electrolyte composition, and grain-refining and leveling agents on the morphology and purity of electrodeposited copper were determined.

Jan 1, 1979

By Seth C. Scharfer

"As part of the Bureau of Mines effort to provide thermodynamic data for the advancement of mineral technology, the Gibbs energies of formation of MoS2 (molybdenite) and WS2 (tungsten disulfide) were determined with high-temperature galvanic cells employing stabilized Zr02 (zirconia) as the electro¬lyte. In the temperature range from 867 to 1,209 K, potential measurements were obtained for the cellPt, MoS2 , Mo02 , SO2 = 1 atm // Zr02 // 02 = 0.0112 atm, Pt, with the overall cell reactionMoS2(c) + 3 02(g, 0.0112 atm) = Mo02 (c) + 2 S02(g). (1)These results, combined with the best available values for Gibbs energies of formation (?G°f) of Mo02 (molybdenum dioxide) and SO2 (sulfur dioxide) from the literature, give the standard Gibbs energy of formation of MoS2, ?G°f, for the reactionMo(c) + S2(g) = MoS2(c) (2)?G°f = -96.681 + 43.76 x 10-3T±0.538 kcal/mole, (3)where temperature (T) is expressed in Kelvins.Similar measurements in the temperature range from 872 to 1,210 K were obtained for the cellPt, WS2 , W03 , SO2 = 1 atm // Zr02 // 02 = 0.0114 atm, Pt, with the overall cell reactionWS2(c) + 3.5 02(g, 0.0114 atm) = W03 (c)+ 2 S02(g). (4) Combination of these results with the best available data of ?G°f for W03 (tungsten trioxide) and SO2 from the literature gives the Gibbs energy of formation of WS2 in the temperature range from 872 to 1,210 K for the reactionW(c) + S2(g) = WS2 (c)(5)?G°f = -92.429 + 43.88 x 10-3T ± 0.280 kcal/mole. (6)A third-law analysis yields a standard enthalpy (?H°f) for the reaction298Mo(c) + 2 S(rh) = MoS2(c), (7)?H°f = -67.36±0.60 kcal/mole, (8)298where the standard states are pure crystalline MoS2 / and rhombic sulfur."

Jan 1, 1980

By H. C. Ko

As part of the Federal Bureau of Mines effort to provide thermodynamic data for the advancement of minerals technology, energy conservation, and environmental preservation, the standard enthalpies of formation of a-magnesium sulfate, a-magnesium sulfate, and magnesium sulfate monohydrate were determined by hydrochloric acid solution calorimetry. The values of the standard enthalpies of formation in kcal per mole at 298.15 K are -307.95 ± 0.13 for a-MgS04, -307.03 ± 0.13 for ß-MgS04, and -384.72 ± 0.13 for MgS04 .H2O.

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