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By A. Gene Collins

During recent years the interest in trace and minor constituents of oil-field water, petroleum, and their associated reservoir rocks has increased. The metals copper, nickel, lead, manganese, iron, zinc, and cadmium are not determined routinely in oilfield brine analyses. Determination of these metals and subsequent correlation of these data should yield information to aid 1n the interpretation of the origin of different waters. The methods of analyzing oilfield waters have several potential applications: (1) Aiding in the search for petroleum; (2) identifying sources of intrusive brines; (3) controlling corrosion; (4) controlling produced water; increasing knowledge of the geology of subsurface formations; (5) identifying incompatible waters in waterflooding operations; (6) increasing the knowledge of the flow of oil, gas, and water in underground formations; and (7) aiding in the identification and location of valuable mineral reserves. Some brines contain enough valuable minerals to be recovered commercially.

Jan 1, 1962

By F. P. Haver

A procedure is described for recovering both lead and sulfur from galena flotation concentrate, comprising the following steps: (1) Aqueous oxidation of the concentrate, using ferric sulfate to convert lead sulfide to sulfate and to give elemental sulfur; (2) regeneration of the ferric sulfate by electrolysis in a diaphragm cell; (3) treatment of the leach residue with ammonium carbonate solution to change the lead to an acid-soluble form and to produce ammonium sulfate as a byproduct; (4) solution of the lead carbonate in hydro-fluosilicic acid followed by electrolysis to recover the lead as metal and regenerate the acid; and (5) extraction of the elemental sulfur from the final residue with an organic solvent. About 90 percent of the lead can be recovered by the above method as 99.9-percent-pure metal, together with two-thirds of the sulfur--half in the elemental form and half as ammonium sulfate.

Jan 1, 1970

By M. M. Jones

A procedure for the spectrophotometric determination of uranium has been developed in support of minerals research being conducted by the Bureau of Mines. Uranium is separated from the sample by tributylphosphate extraction from acid solution containing added aluminum nitrate and (ethylene dinitrilo)-tetraacetic acid solutions. The colored uranium-dibenzoy1methane complex is developed in the organic phase by adding an ethanol solution of dibenzoylmethane buffered with triethanolamine. Absorbance is measured at 410 nanometers, and the response is linear up to at least 100 micrograms U30S in the aqueous aliquot taken for analysis. Aliquots containing as little as 8 micrograms U30S may be analyzed with relative errors no greater than ±5 percent. For aliquots containing at least 35 micrograms U308, relative standard deviation at the 95-percent confidence level is about ±2.2 percent. Appropriate procedures are given for analyzing a wide variety of samples.

Jan 1, 1980

By James P. Ulery

A Bureau of Mines geologic study of Pennsylvanian and Permian coalbeds in southwestern Pennsylvania was undertaken to determine the effects of coalbed geology and petrology on in situ coalbed gas contents. Data were obtained from 18 coreholes from parts of four 7.5 ' quadrangles in southwestern Washington and northwestern Greene Counties, and from a single corehole in Westmoreland County. A total of 88 samples from 24 coalbeds were collected for direct-method testing to determine gas content. The samples were also analyzed for petrographic composition, chemical composition, and vitrinite reflectance values. Corehole information was used to generate isopach maps and geologic cross sections useful in data interpretation. Results of the investigation show that coalbed gas content is related to vitrinite reflectance, but not to petrographic composition. Gas contents are also influenced by other geologic factors such as roof rock lithology and competency, and location with respect to local fold structure.

Jan 1, 1989

By J. Grumer

Nine dust and gaseous inhibitors of propagating coal dust-air flames (lean, stoichiometric, and rich) were evaluated in a newly developed 15-cm-id, 3.6-meter-long instrumented flame duct, under conditions such that wall quenching was virtually absent and the dust concentration was temporally and spacially uniform to within about t5 percent. Listed roughly in order of increasing efficiency, the inhibitors evaluated were rock dust (calcium carbonate), powdered oyster shells (calcium carbonate), Halon 1301 (trifluorobromomethane), Halon 1211 (difluorochlorobromomethane), sodium chloride, Super-K (potassium chloride), regular-grade fire extinguishant powder (sodium bicarbonate), Purple-K (potassium bicarbonate), and Monnex (potassium bicarbonate combined with urea). Experiments were extended to clouds containing 1 and 2 volume-percent of methane. The inhibition of lean, stoichiometric, and rich methane-air flames without coal dust was also examined in a few instances; results agreed with those obtained for coal dust-air flames.

Jan 1, 1971

By Verne E. Hooker

Stress relief measurements were made at three underground test sites associated with the Henderson project, American Metal Climax, located in the rugged, mountainous region between Loveland Pass and Berthoud Pass on the Continental Divide in Colorado. Sufficient data were obtained to determine the three-dimensional stress ellipsoid for each site. The measurements were made at hole depths greater than one diameter of the mined opening; thus, calculated stresses are representative of premining in situ conditions. The vertical components of stress are in good agreement with overburden depth including the influence of mountain topography. Horizontal components of stress substantially increase with depth. These components are believed to be influenced by stresses presumably of tectonic origin. The largest measured principal stress was 5,900 psi at a depth of 3.708 feet. The predominant orientation of maximum principal stress for the determinations at greatest depth is in the NW-SE quadrants.

Jan 1, 1972

By Charles L. Kimbell

Tables 16 through 19 continue the series of providing the world merchant fleet distribution by type of vessel and the ranking of the major fleets by country of registry. Table 20 this year provides a summary of the world's liquid gas carrier fleet. These vessels are included in the totals given for the world's tanker fleet, but gives a breakdown demonstrating the growth of the importance of natural gas in the world's energy commodity consumption. Panama and Suez Canals Tables 21 and 22 provide the latest available information on the transit of mineral commodities through the Panama Canal, by number of vessels, direction, and the commodities transported. Although the number of vessels transiting the Panama Canal dropped slightly (0.5%) between 1989 and 1990, the total amount of cargo moved rose by 3.6% and the amount of mineral commodities moved rose by 7.2%.

Jan 1, 1993

By Tobias W. Goodman, Joseph Cervik

This Bureau of Mines report investigates the horizontal trajectory of boreholes drilled in coalbeds using the rotary drilling technique. Test holes drilled in coalbeds showed that the path of a borehole in the horizontal plane depends on drilling assembly configuration, drill bit rotation, and coalbed geologic features. An assembly that contained an 18-ft (5.53) long drill collar and two centralizers had the best horizontal stability evidenced by trajectories that deviated less than 16 ft (4.9 m) from a target at 1,000 ft (305 m). Removal of one of the centralizers resulted in a loss of control of hole trajectory in the horizontal plane. Generally, holes tended to turn to the right, presumably because of right-hand rotation of the bit. Deviations from the original bearing line were as much as 200 ft (61 m) or more at a depth of 1,000 ft (305 m).

Jan 1, 1988

By L. B. Pankratz

The Bureau of Mines determined low-and high-temperature thermodynamic properties for anhydrous ferric sulfate and anhydrous indium sulfate. Low-temperature heat capacities were measured between 50° and 298° K, and enthalpy increments above 298° K were determined. The high-temperature measurements of Fe2(S04)3 extended to 900° K and those of In2(S04)3 to about 1,000° K. A minor transition was found for Fe2(S04)3 at 800° K, with a heat of transition of 540 cal/mole. Tabulations were made of the low-temperature heat capacities and the high-temperature enthalpy and entropy increments. The 298° K entropies derived from the low-temperature measurements were 67.6±0.S ca1/deg mole for ferric sulfate and 72.2±O.5 cal/deg mole for indium sulfate. High-temperature enthalpy increments were also given in equation form.

Jan 1, 1969

By David Hoadley, Kenneth R. Maser, Ashok B. Boghani, James E. Billar, D. Randolph Berry, Mackenzie Burnett, Robert H. Trent

4. Guidelines for Implementing the Emergency Escapeway Standards for Metal and Nonmetal Mines The technical discussion of each escapeway component precedes the specific guidelines for the component. Generally, the technical discussion provides the background and reasoning behind the guidelines. Section 5 is a discussion of general escapeway requirements, including the escape route, fire retardants, warning systems, ventilation systems, escapeway signs and signals, auxiliary transportation and fuel storage. The discussion is followed by a list of guidelines pertaining to the escapeways. Section 6 is a summary of the computer simulation of an escapeway system for Mine "C". A complete documentation of the simulation is included in Appendix A and B. Section 7 covers emergency hoisting requirements and concludes with the guideline, for emergency hoists, their inspection and use. Section 8 is a discussion of refuge chambers and life support and is concluded with guidelines for the application o f this equipment.

Jan 1, 1976

By Joan C. Biordi

[Composition profiles for atomic, radical, and stable species, as well as temperature and area expansion ratio profiles, have been determined for a nearly stoichiometric CH4-02-Ar flame and one to which 0.3 percent CF5Br inhibitor had been added. Net reaction rate profiles were calculated for all the observed species. For the normal flame, these and the mole fraction profiles gave rate coefficient information about the elementary reactions in the methane flame, for example, CH. + 0 4- H2CO 0 H, k4 = 1.05 X 1014CM3 mole-1sec-1 for 1,550§T 0,725' K; CO + OH 4 C02 + H, k6= 4.7 X 1011 for 1,350{T X1,750° K. Comparison between the inhibited and normal flame showed that A] and [CH3] were significantly reduced at the lower temperatures in the inhibited flame even though in the hot gas region the [E] [OH!, and [0] were essentially the same in both flames. The CF3Br disappears very early in the flame, relative to the fuel, and the reaction primarily responsible for its disappearance is H v CF3Br 4 HBr + CF3, where k7 is found to be 2.2 X 1014 exp(-9460/RT) for 700-1,550° K. Reaction of the inhibitor with methyl radicals provides for the relatively small amounts of CH3Br observed, but CH3 + Br2 - CHs Br + Br must also occur. The HBr formed reacts rapidly with H atoms to form H2 and Br, but the reaction is soon "balanced" in the flame as may be demonstrated by calculation of the equilibrium constant at various temperatures. The fluoro-carbon fragment produced in reaction (7) also reacts rapidly, in part with methyl radicals to give the observed elimination product CH2CF2 Later in the flame, above -1,400' K, F2CO is formed from the reaction CH2CF2 + 0 P F2CO + CH2 and k., -1.5 X 1013 at 1,600° K. The rather slow decay of carbonyl fluoride is attributed to reaction with H atoms according to the sequence F2CO I H - HF + FCO and FCO + H HF + CO.]

Jan 1, 1975

Studies on coal mine drainage sludge densification have led to the following conclusions: 1. Coal mine waters containing iron principally in the ferrous (Fea+) state can be treated by a modification of the commonly practiced lime neutralization process to yield a ferromagnetic sludge. The sludge, presumably composed in large part of a hydrated ferrosoferric oxide (Fe304.xH20), is much denser and faster settling than the ordinary "yellowboy" sludge obtained by lime neutralization and aeration at ambient temperatures. 2. The magnetic sludge preparation technique involves (quantitative) precipitation of iron (largely as Fe(OH)2) by the addition of hydrated lime to a pH of 8.5, separation of the resulting sludge from the aqueous phase, and heating of the sludge concentrate to at least 80 C (176 F), preferably higher, followed by mild aeration. 3. Magnesium, present as Mg2 in most coal mine drainage waters, inhibits the formation of the magnetic sludge. This inhibition can be adequately minimized by keeping the pH below 9.6 during lime addition (thus avoiding the coprecipitation of Mg(OH)2) and by separating the sludge from the bulk of the aqueous phase before the heating step, as indicated in (2) above. 4. Aluminum, commonly present in coal mine drainage waters, also inhibits the formation of the magnetic sludge. This inhibition is of practical significance when the molar ratio of aluminum/total iron is greater than 0.18. Below this value, sludges are still appreciably magnetic, but are bulkier and slower settling than those obtained when aluminum is absent. Unlike magnesium inhibition, aluminum inhibition cannot be minimized by the scheme indicated above, since aluminum precipitates as Al(OH)3 near pH 4 and remains dispersed within the sludge. 5. The limitation on aluminum content is probably the most serious restriction affecting the feasibility of the magnetic sludge process as presently conceived. Nevertheless, a limited review of available water quality data has indicated that, in terms of relative acid and iron loadings, a significant number of major coal mine discharges in the eastern Ohio River basin may be amenable to treatment by a magnetic sludge process. 6. Data from tests on the use of magnetic seeding materials indicate that seeding did not enhance the formation of a magnetic sludge under the experimental conditions employed.

Jan 1, 1971

By W. R. McDonald

The Bureau of Mines, U.S. Department of the Interior, conducted small-scale field tests on acidic copper tailings as part of its effort to develop, improve, and demonstrate technology for stabilizing mining and mineral-processing wastes. Two successful demonstration revegetation plots were established on an abandoned copper-tailings pond located on public land adjacent to Holden Village, Wash. The tailings were neutralized with treatments of either dolomitic lime or limerock and fertilized with processed sewage sludge and/or commercial fertilizer. Excellent plant growths covering 70 and 24 percent of the surface were achieved on 1/8-and 1-1/2-acre test plots planted in 1973 and 1974, respectively. Regar brame, Tegmar intermediate wheatgrass, and tall wheatgrass provided the best plant growth and surface coverage. The target pH of tailings neutralization was 6.8; however, good plant growth occurred in areas where the soil pH ranged from 2.9 to 5.8.

Jan 1, 1978

By C. J. Thompson

In the course of the work currently conducted by the Bureau of Mines in cooperation with the American Petroleum Institute Research Project 48 on identifying sulfur compounds in petroleum, a micromethod was developed (12)5 for catalytically removing the sulfur atom from sulfur compounds. The product is the residual portion of the molecule; the structure otherwise was unaltered except for hydrogenation of any unsaturated bonds that were present in the original compound. Positive identification of sulfur compounds isolated from crude oils is a difficult problem. Direct comparison of properties of the unknown with those of reference compounds is often impossible because of the limited number of reference sulfur compounds available. However, a relatively large number of pure hydrocarbons is available, and the conversion of the sulfur compound to a hydrocarbon enhances the possibility of identification. The technique also can be used to prepare microquantities of scarce hydrocarbons by hydrogenating compounds that are readily available.

Jan 1, 1962

By H. B. Salisbury

The Bureau of Mines conducted research to determine if low-grade California chromite ores could be beneficiated to produce products suitable for commercial use. This research is part of a Bureau goal to provide technology capable of using low-grade domestic ores to meet emergency demands of the Nation for metals and minerals and in particular those minerals, such as chromite, which are considered critical. Two ores from California were ground and treated using gravity concentration and magnetic separation techniques. An are from Auburn in central California, assaying 2.5 pct Cr203, was treated by tabling and magnetic separation to yield a nonmagnetic product containing 44.7 pct Cr203 at a recovery of 36.4 pct. Core drilling samples from the Seiad Creek area of northern California, assaying about 6 pct Cr203, were upgraded by tabling to yield a concentrate containing nearly 50 pct Cr203 with a recovery of 50 pct. Both products are suitable for metallurgical and/or chemical use.

Jan 1, 1981

By Charles L. Kimbell

Available statistics on 1989 worldwide consumption of selected nonfuel minerals shown in table 5 show increases for 11 of 14 listed nonfuel mineral commodities with 1 unchanged from the 1988 level, a departure from the pattern of the past 2 years, in which each of the listed commodities registered gains. The 1989 results, however, were better than those for 1986 when only seven listed nonfuel mineral commodities recorded gains with one un- changed from 1985. Consumption of the two ferrous metal raw materials listed advanced as functions of increased output of pig iron and crude steel. The increase in iron ore consumption exceeded the increase in iron ore output, suggesting a slight drawdown of world iron ore inventories. The estimated in- crease in iron and steel scrap consumption was slightly greater than the minuscule increase in world steel production, but it is believed that there was little change in the ratio of iron ore to scrap in steel plant feed on a global basis.

Jan 1, 1992

By Thomas G. Carnahan

The Bureau of Mines conducted research to simulate in situ leaching of a chalcopyrite ore. The purpose was to obtain a direct comparison between moderate-temperature and elevated-temperature in situ leaching of copper trom minus la-inch ore and to analyze the sulfuric acid and oxygen requirements of the leaching system. Experiments employing oxygen were conducted at 35° and 90° C on 362-and 367-1b ore charges, respectively, under flooded conditions and at 400 psig. At 90° C, 47 pct of the copper was extracted in 913 days of leaching; at 35° C, 27 pct of the copper was extracted in 915 days. Diffusion into and out of the ore fragments con-trolled the rate of leaching. Oxygen consumption was 1.46 lb/lb of copper extracted at 35° C and 3.15 lb/lb of copper extracted at 90° C. Sulfuric acid requirements of the ore were 5.49 and 7.48 lb/lb of copper extracted at 35° and 90° C, respectively.

Jan 1, 1982

By D. L. Pool

To increase metal recoveries and to minimize pollution by improved extraction technology, the Bureau of Mines investigated a hydrometallurgical technique to recover copper, lead, nickel, and cobalt from lead smelter mattes. The metals were converted from insoluble sulfides to soluble chlorides using a HCI-CI2-02 leaching system. Parameters studied in a 50-gallon, glass-lined reactor were the ratio of hydrochloric acid to chlorine, chlorine consumption per pound of matte, oxygen reaction pressure, and temperature. The matte material used contained, in percent, 19.7 Cu, 52 Pb, 2.9 Ni, 1.5 Fe, 0.38 Co, 0.19 As, 0.41 Zn, and 0.12 Cd. Extraction of Cu, Pb, Ni, Co, and Cd ranged from 92 to 98 pct, with concomitant extractions of Fe and As of <0.1 pct. The Cu and Pb were recovered as electrowon metals, while the Ni, Co, and Cd were recovered as mixed hydroxides.

Jan 1, 1981

By D. J. MacDonald

The Bureau of Mines has carried out investigations on a method for producing zirconyl sulfate solution from zircon sand, comprising (1) reacting zircon sand with molten NaOH, (2) leaching the resultant fusion frit with water to remove sodium silicate and to convert sodium zircon-ate to hydrous zirconium oxide, and (3) leaching the hydrous zirconium oxide from unreacted sand with hot, dilute H2S04 to produce crude zirconyl sulfate solution. The following conditions were found to be suitable: reacting 0.6 kg of NaOH per kilogram of zircon sand for 10 min at 600° C; leaching the frit with 3 to 4 liters of water per kilogram of solids; leaching the residue with 5.1 liters of water and 1.25 liters of 98-pct H2S04 per kilogram of original solids for 10 min at 90° C; and filtering or decanting to recover unreacted zircon sand. A preliminary cost estimate is included.

Jan 1, 1982

To develop a cost-effective tool for improving the performance of rock drilling systems used in detecting and delineating underground mine voids and for coal exploration. Approach To investigate admixtures of polyethylene oxide (PEO) at zero surface charge concentrations as drilling fluid additives to enhance penetration rates and extend bit life in rock drilling systems. Background Bureau researchers have investigated the use of chemical additives to enhance drilling performance and found that the most efficient drilling occurred when the drilling fluid was able to maintain a zero surface charge (ZSC) on the surface of the rock being drilled. Laboratory drilling studies have been performed on rock types such as quart¬zite, granite, taconite, and marble. The lab tests were conducted using 5/8-inch diameter diamond-impregnated coring bits with cationic compounds as the surface charge neutralizing additives. These studies demonstrated enhanced drilling performance, however, only at the singular additive concentration that produced the ZSC condition.

Jan 1, 1991