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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'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 H. J. Heinen

To maximize productivity through improved minerals processing technology, the U.S. Department of the Interior, Bureau of Mines, is investigating particle agglomeration techniques as a means of increasing the percolation rates of leach solutions in heap leaching of clayey gold-silver ores. Simulated heap leach experiments were conducted on 50-pound charges of ore that were contained in 5.5-inch-diameter columns, 5 feet in height. Results indicated that the percolation rate of cyanide leach solution could be enhanced markedly by mixing the ore with controlled amounts of lime, flocculants, and water, and then aging the mixture prior to the column leach step. Experimental results obtained on 20-mesh silver tailings and gold ore crushed to 3/8 inch and to 1 inch showed that it was possible to increase percolation rates as much as 100-fold without sacrificing silver-gold extraction. Larger scale tests conducted in 24-inch-diameter, 16-foot-high columns closely paralleled bench-scale results. By improving percolation leaching, these techniques have the potential of helping to solve environmental problems associated with tailings disposal as well as making an important economic impact on gold-silver recovery operations. Investigations are continuing to develop binders superior to lime for particle agglomeration pretreatment.

Jan 1, 1979

By I. Liebman

Two triggered barrier systems and several extinguishing agents were tested against coal dust explosion propagating in the main entry of the Bureau of Mines Experimental Mine at Bruceton, Pa. One system used a high-pressure cylinder to propel the extinguishant; the second system used pressurized nitro-gas or Halon 1301 (CF3Br) in a low-pressure system to power the disperser. The relative efficiencies of the extinguishants were determined by compar¬ing calculated concentrations of the extinguishant clouds present in the mine during suppressing of the explosions. Results showed the following trend of increasing effectiveness: Purple-K (KHC03)<water<hybrids consisting of foam or water combined with Halon 1301<Halon alone. On a weight basis, water was two to three times as efficient as Purple-K, whereas the hybrids and Halon alone were only marginally superior to water. Maximum efficiency of an extinguishant is attained by high rates of discharge from the barrier and by minimizing the time interval between onset of discharge and flame arrival to that necessary for discharge. Both the high- and low-pressure barrier systems were demonstrated to be capable of suppressing coal dust explosions; however, because of the potential hazard of the former, the low-pressure system is considered to be the most attractive prototype.

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 C. B. Davison

One goal of the Bureau of Mines is to conserve the Nation&apos;s mineral resources by developing improved performance materials. Consistent with this goal, the Bureau conducted studies on the formation of undesirable cristobalite in seven different fire clays used as refractories. The studies employed scanning electron micrography, chemical and X-ray analyses, and pyrometric cone equivalent determinations to examine the sample clays and determine the effect of thermal history and stablilizing additives on the amount of cristobalite in various calcines. This research has indicated that as fire clay calcining temperatures increased from 1390° to 1,490° C there was a gradual decrease in the percent of cristobalite present in the calcines and a progressive development of mullite crystallization. No cristobalite was found in fire clays calcined above 1,550° C, but cristobalite reappeared when the calcines were reheated to temperatures between 1,400° and 1,500° C. The research also revealed that additions of lithium fluoride (LiF) prevented formation of cristobalite in fire clay calcines.

Jan 1, 1979

By Bruce D. Hanson

The Bureau of Mines conducted a series of experiments using four different coal types to determine the effect of attack angle and symmetric bit wear on airborne respirable dust (ARD) generated by point-attack bits and in energy consumption. Neither had a significant effect on ARD at the 95-pct confidence level, but bit wear had a significant effect (95 pct confidence) on specific energy (energy per gram of cut coal) for three coal types, Depth of cut was the most significant factor affecting ARD and specific energy.

Jan 1, 1979

By H. R. Beard

The Federal Bureau of Mines investigated the absorption of radium and thorium from waste uranium leach liquor by clays and other materials. This work was conducted in support of the Bureau&apos;s goal of minimizing the environ¬mental conflicts, impacts, and occupational hazards Associated with mining and mineral processing operations. Tailings and soil samples from Wyoming and Utah were contacted with tailings liquors to determine the degree of absorp¬tion. Absorption ranged from 0 to 99 percent for radium and from 0 to 31 per¬cent for thorium. Some samples, which readily absorbed radium, were contacted with various salt solutions that could be present in tailings solutions to determine their effectiveness as desorbents. The desorption of radium ranged from 0.06 to 100 percent. An alpha-spectrometric method was used to determine the radium and thorium, concentrations in the solutions and the solids.

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 Richard C. Repsher

Intermittent mining in the slope section at Dutch Creek No. 1 mine, Carbondale, Colo., of the Mid-Continent Coal and Coke Co. has resulted in erratic and minimal rock noise data, which, in turn, has necessitated a change in the method used to plot daily mine noise in order to be useful to the researchers at the mine. Daily and weekly cumulative plots of rock noise under these conditions have not shown significant stress changes as clearly as bimonthly or longer noise rate plots. Hence, longer term cumulative rock noise plots, as described in this Bureau of Mines report, have been added to the data analysis at Dutch Creek No. 1 mine, and have been shown to delineate unique areas of rock noise activity more clearly than shorter term plots. The longer term plots should aid in the detection and delineation of potential failure areas, when used in conjunction with other proven forms of data analysis.

Jan 1, 1979

By Barbee J. Scheibner

This Bureau of Mines report describes the geology and physical properties of core samples at the Sunnyside coal mine No. 1, Sunnyside, Utah, and was written in conjunction with the Single-Entry Program conducted at the mine. The objective of this program was to test the hypothesis that the single-entry system in the Sunnyside mine, supported in the center by open cribs and divided by a fire-resistant partition, is equivalent to or better than a two-entry sys-tem. Drill cores, taken underground at 15 sites in the single-entry study area, facilitated the construction of geologic cross sections of the entries. Physical property data obtained from the drill cores was used in a three-dimensional finite element analysis program to evaluate the stability of the openings, the support requirements, and the de formation characteristics of the roof and floor material. Data on 10 physical property parameters for 5 rock types plus coal are also tabulated and discussed.

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 D. G. Puglio

This Bureau of Mines study covers 25 underground mines that were active in the Upper and Lower Freeport and Lower Kittanning coalbeds in 1976. The coal ranges from low to medium volatile in rank; its primary use is for steam generation. Seven mines emit more than 100,000 cfd of methane gas; those mines are the deepest and largest producers. The methane gas content of three core samples of the Lower Kittanning coalbed was estimated by the direct method. A sample from a depth of 320 feet contained 0.5 cu cm of gas per gram, at 620 feet there was 0.8 cu cm of gas per gram, and at 1,060 feet there was 11 cu cm of gas per gram. These results suggest that methane control problems will be encountered in the future as deeper coal is mined.

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. S. Dunning

A primary goal of the Federal Bureau of Mines is to minimize the requirements for scarce mineral commodities through conservation and substitution of more abundant elements, such as iron and molybdenum. One example of this is the research effort to devise substitute materials for specialty alloys, thereby conserving nickel and chromium in high-volume stainless steels. As a possible substitute for the solid solution strengthening of chromium and nickel, the precipitation hardening characteristics of a number of binary iron-based systems in which Laves phase precipitates, such as Fe2Mo, are formed were investigated. Several hardening responses were observed, but none were ideal. The Fe-Ta binary system had the highest magnitude of hardening, even with low alloy additions, and the Fe-Mo system had unique stability at temperature. Accordingly, the Fe-Mo-Ta system was selected for study to determine if a ternary Laves phase could combine high hardening with long-term stability at elevated temperature. Hardening and stability were reflected in excellent elevated temperature, tensile, and stress rupture strengths. Future research will study ternary systems based on more abundant resource materials, such as the Fe-Mo-Ti system, together with additions, such as aluminum and minimal chromium, to provide oxidation resistance.

Jan 1, 1979

By Robert A. Speirer, Richard G. Burdick

Methods of detecting geologic faults and other linear features by means of processed LANDSAT satellite images have gained prominence during the past several years . There have been numerous programs written to pick these " lineaments , " but they have been almost universally tailored to large computers . This Bureau of Mines report describes a detection method developed for use with a minicomputer . The method comprises a suite of programs that scans an image for all " potential " lineaments . From this partially analyzed data , the final lineaments are picked by another routine . The method was field tested in an area of south- central Wyoming , and results indicated good agreement between computer- picked lineaments and ground features . Most of the known geologic faults in the area were picked by the method . Such features as roads and trails were also picked but were easily distinguished from faults during field inspection . The method is relatively new but promises to be a viable reconnaissance technique for the mining industry in geologic structural analysis .

Jan 1, 1965

By S. D. Cramer

Corrosion research is being conducted by the Federal Bureau of Mines to determine suitable construction materials for geothermal resource recovery plants. As part of this research, the corrosion resistance of 31 iron-nickel-, aluminum-, copper-, titanium-, and molybdenum-base alloys was characterized and evaluated in laboratory corrosion studies in low-and high-salinity geobrines representative of those found in the Imperial Valley, Calif. General, crevice, pitting, weld, and stress corrosion were measured at 105° and 232° C in deaerated brines and brines containing dissolved 02, C02, and CH4 General corrosion rates in deaerated brines at 105° and 232° C were usually below 5 mpy for the alloys tested except carbon steel, the low-alloy steels, Monel 400, 70-30 cupronickel, and the aluminum-base alloys. Dissolving carbon dioxide and methane in the brines at 2320 did not markedly alter these results. However, the introduction of oxygen, which can enter the brine during process operations, seriously degraded the corrosion resistance of many alloys by increasing the incidence of stress corrosion cracking, crevice corrosion and, except for the titanium-base alloys, pitting. In deaerated brine at 2320 C, the general corrosion rates for carbon steel and the low-alloy steels were relatively unaffected by pH in the range of 6.1 to 3.0. However, general corrosion rates increased sharply below pH 3.0. In deaerated brine at 232° C, welds in several iron-, nickel-, and titanium-base alloys corroded at rates comparable to the general corrosion rates of the alloys, but the addition of oxygen to the brine increased corrosion rates for welds in Inconel 625 and E-Brite 26-1. Alloys exhibiting good corrosion resistance in the deaerated Salton Sea KGRA-type brine at 232° C were E-Brite 26-1, Inconel 625, Hastelloy S, Hastelloy G, Hastelloy C-276, TiCode-12, Ti-0.2Pd, Ti-2Ni, Ti-1.7W, and TZM. The alloys most resistant to corrosion in oxygenated Salton Sea KGRA-type brine at 232° C were the titanium-base alloys. These alloys appear the most suitable for use in the construction of geothermal resource recovery plants. Carbon steel and the low-alloy steels are unsatisfactory for high-temperature, high-salinity brines and alternative low-cost materials with improved corrosion resistance should be sought.

Jan 1, 1980

By R. S. DeCesare

Operation of the Bureau of Mines raw refuse continuous separation pilot plant is described, including modifications made to plant equipment for improved performance. Products recovered from refuse, many of which have been evaluated by other laboratories and private firms, are discussed. Sampling procedures used in the pilot plant and detailed data obtained from processing refuse from 13 municipalities are presented in appendixes. Fuel evaluations made on combustible fractions of refuse from the various municipalities are also presented. Information and data obtained at the pilot plant have been used to assist many municipalities in solving their urban refuse problems.

Jan 1, 1980

By B. S. Covino

The Bureau of Mines, U.S. Department of the Interior, is conducting research to devise substitute corrosion-resistant materials by using ion implantation to form alloyed regions near the surfaces of metals. These alloys were prepared by implanting 25-kev Cr+ and/or Ni+ ions into iron. Their resistance to corrosive attack was evaluated by determining their anodic polarization behavior under potentiodynamic conditions in a solution containing sodium chloride, boric acid, and sodium borate. These electrochemical studies have shown that the general corrosion resistance of ion-implanted alloys was comparable to nominally equivalent bulk alloys. The pitting-corrosion resistance of the ion-implanted alloys was superior to that of iron, although not as good as that of most of the bulk alloys tested.

Jan 1, 1980