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By Irven A. Jacobson

The thermal reactions of l-methylindole were studied in the temperature range of 525° to 627° C in a flow reactor. The major products consisted of 2-methylindole, 3-methylindole, indole, quinoline, hydrogen, and methane. 2-Methylindole is formed from 1-methylindole by an irreversible isomerization reaction. The 2-methylindole isomerizes in a reversible manner to 3-methyl-indole, the equilibrium favoring the 3-methyl isomer. Indole is formed directly from 1-methylindole. Quinoline is formed from l-methylindole, 2-methylindole, and 3-methylindole.

Jan 1, 1971

By Ruth A. Holmes

A Bureau of Mines method for recovering nickel, cobalt, and copper from low-grade domestic laterites is described, which includes the unit operations of solvent extraction and electrowinning. Previous Bureau work indicated that addition of Na2S04 (sodium sulfate) to the nickel electrolyte improved current efficiency in nickel electrowinning. The present study determines the compatibility of Na2S04 with nickel strip-ping in the solvent extraction operation of the Bureau method. The effect of adding 100 g/l Na2S04 on nickel stripping, phase disengagement, and pH was determined in comparative laboratory-scale tests. In continuous-circuit testing, Na2S04 reduced stripping efficiency to the extent that five, instead of four, strip stages were required for complete stripping of nickel from the loaded solvent. In tests made in a phase-disengagement cell that had a variable settler area, the addition of Na2S04 did not significantly affect phase separation characteristics. The pH of the nickel electrolyte in the temperature range of 20° to 65° C was also unaffected by the addition of Na2S04. An economic evaluation showed that the energy saved by adding Na2S04 to the electrolyte would more than offset the cost of adding another stripping stage.

Jan 1, 1983

By John P. Gooch

Data for the ternary phase diagram for the system 1,1,2,2-tetrabromoethane/water/2-propanol at 25° C have been measured. Experimental methods used are described, and the complete ternary phase diagram is presented. A simple example is given to review the use of the ternary diagram.

Jan 1, 1972

By R. K. Koch

The vapor pressures of liquid molybdenum and liquid zirconium were determined by the Langmuir free-evaporation method. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. The vapor-pressure data led to the following equations: [log p (atm) = 5.429 - 28,380 T for liquid molybdenum in the range 2,890° to 2,990° K, and log p (atm) = 6.521 - 30,940 T for liquid zirconium in the range 2,229° to 2,795° K.] Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 157.6 ± 1.8 kcal/mole and 148.4 ± 2.4 kcal/mole for molybdenum and zirconium, respectively, where the uncertainties are two standard devia¬tions. Second-law standard heats of sublimation determined from sigma plots and tabulated enthalpies were 143.5 ± 2.7 kcal/mole and 149.2 ± 3.8 kcal/mole for molybdenum and zirconium, respectively. The better agreement in heats of sublimation for zirconium is attributed to the 566° K temperature range studied which permitted a more accurate definition of the vapor pressure curve than could be obtained from the 100° K span for molybdenum. This supposition was verified by making a sigma-prime plot which utilized solid vapor pressure data for molybdenum to extend the evaluation range by 800° K. This gave a standard heat of sublimation of 155.2 ± 1.6 kcal/mole which is in good agree¬ment with the third-law value. The plot also gave a standard entropy of sublimation (298.15° K) of 35.73 ± 0.48 eu.

Jan 1, 1968

By W. L. Staker

The Bureau of Mines investigated methods for selectively eluting mercury, silver, and gold from strong-base anion-exchange resins, including Rohm and Haas resins lRA-430 and 900 and Dow Chemical resins 2lK, SMA-I, and SBR. Resins were typically loaded to 145 oz/st of each metal. Loaded resins were eluted with H2S04, NaCl-H Cl, NaOCl, and NaCl04 solutions. The resins tested had similar elution characteristics for mercury and precious metals. The best selective elution scheme was achieved by eluting in a column with 2N H2S04 to recover 99 to 100 pct Hg, with 200 giL NaCl in IN HCI to rec;ver 99 to 100 pct Ag, and with 2M NaCl04 to recover 79 to 89 pct Au.

Jan 1, 1987

By Ann G. Kim

Samples of gas were obtained directly from the coalbed during drilling of horizontal and vertical boreholes in six different formations. The samples were analyzed by gas chromatography for C1 to C5 hydrocarbons and for O2, N2, H2, He, and Co2. Methane in the gas varied from 63 to 99 percent; carbon dioxide from 0.1 to 15 percent. The CH4/CO2 ratio varied and showed no apparent correlation with age, rank, or bed. The majority of samples contained ethane, propane, and butane; hydrogen and helium were found in some samples. Oxygen and nitrogen were usually present, possibly as a result of air contamination. A more extensive sampling program would be necessary to establish relationship between the amount and composition of the gas in the coalbed and other factors.

Jan 1, 1973

By Kihong Park

A hygroscopicity tandem differential mobility analyzer (HTDMA) technique is used to determine size-effect of nanoparticles (NaCl, (NH4)2 SO4, KCl, NH4NO3, MgCl2,CaCl2) on their hygro­scopic properties (deliquescence relative humidity (DRH) and hygroscopic growth factor (GF)). The HTDMA system uses a combination of two nano DMAs and two regular DMAs to measure particle size change in a wide dynamic particle size range. Particles are subsequently analyzed with a transmission electron microscopy to investigate the potential effect of particle structure or morphology on the hygroscopic properties. We found that structural properties of NaCl and (NH4)2SO4 particles also play an important role in determination of the DRH and GF and are more pronounced at smaller diameters. Data show that the DRH of NaCl nanoparticles increased from *75% up to *83% RH at 8 nm and that their GF decreased with decreasing size. The extent to which the GF of NaCl nanoparticles decreased with decreasing size was greater than theoretically predicted with the Kelvin correction. The GF of furnace-generated NaCl nano­particles that have pores and aggregate shape was found to be smaller than that of atomizer-generated particles that are close to perfectly cubic. For the case of atomizer-generated (NH4)2SO4 nanoparticles, we observed no signi?cant size-effect on their DRH, and the measured GF agreed well with predicted values using the Kelvin correction. For furnace-generated (NH4)2SO4 nanoparticles, a gradual growth at moder­ate RH without noticeable deliquescence behavior occurred. Their TEM images showed that contrary to atomizer-generated (NH4)2SO4 nanoparticles the fur­nace-generated (NH4)2SO4 nanoparticles are not perfectly spherical and are often aggregates having pores and holes, which may favor holding residual water even in the dried condition. For atomizer-generated KCl, MgCl2, and CaCl2 nanoparticles, we observed no signi?cant size-effects on their DRH and GF for the mobility size as small as 20 nm.

Jan 1, 2008

By A. R. Taylor

Using solution calorimetry, the following heats of reaction were determined: (1) NaCN(c) + 1/Cu20(c) + 129H20(l) ? CuCN(c) + NaOH?128.5H2O ?H = -13.44±0.10 kcal/mole, (2) HCN(2) + NaOH?128.5H20 ? NaCN(c) + 129.5H20(l) ? = -2.52±0.02 kcal/mole. From these reactions, the heats of formation for CuCN(c) and HCN(2) were calculated to be 22.7±0.4 kcal/mole and 24.9±0.4 kcal/mole, respectively. Reaction 2 was made to check the consistency of literature values for heats of formation of HCN and NaCN. Adiabatic calorimetric measurements between 10° and 400° K showed the entropy and heat capacity of CuCN(c) to be 21.51±0.06 eu and 14.58±0.04 cal/mole deg, respectively, at 298° K. A broad anomaly in the heat capacity was found in the temperature range 285°-320° K. The heat of transition associated with this anomaly was less than 1 cal/mole, the sensitivity of the measurements.

Jan 1, 1971

By D. N. Nilsen

The Bureau of Mines is developing a method to recover Ni, Co, and Cu from laterites containing less than 1.2 pct Ni and 0.25 pct Co. The method consists of the following basic unit operations: (1) reduction roasting, (2) leaching, (3) solvent extraction, and (4) electrowinning. The method reflects three Bureau of Mines objectives: (1) recovery of critical minerals that are domestically in short supply from low-grade domestic laterites, (2) lower processing energy requirements, and (3) solution recycling. This report deals with the extraction of cobalt and the preparation of a suitable cobalt electrolyte by solvent extraction from liquor produced by this method. Nickel and copper are coextracted with LIX64N from an ammoniacal ammonium sulfate leach liquor containing about 1.00 g/l Ni, 0.30 g/l Co, 0.03 g/l Cu, and 0.02 g/l Zn. Cobalt (III) in the nickel-copper barren raffinate is reduced to cobalt (II) with cobalt metal. Reduction of cobalt (III) to cobalt (II) greatly aids subsequent extraction. Commercially available XI-51 extracts about 94 pct of the cobalt from the treated raffinate in one stage in a laboratory mixer-settler continuous circuit. Ammonia loaded on the solvent is removed in two washing steps. About 94 pct of the cobalt then is stripped from the XI-51 in one stage with spent cobalt electrolyte containing about 77 g/l Co and 18 g/l sulfuric acid (H2S04), Electrolytes containing less H2S04 also may be used. Preliminary data indicate that coextracted zinc may be removed from pregnant cobalt eletrolyte containing 3 g/l or less H2S04 with di-(2 ethylhexyl) phosphoric acid (D2EHPA).

Jan 1, 1980

By A. A. Berk

In the course of a study of the formation of external deposits on tubes in water-tube boilers it became desirable to determine the sulfur dioxide (SO2) and sulfur trioxide (SO3) in the Due gases. Determinations made by the A.S.M.E. method for SO2 and SO3 in gaseous products of combustion did not give accurate results. It was found that minute quantities of copper, present in the flue gases from the coal in use, caused oxidation of sulfite in the absorption bottle and that the carbon dioxide (CO2) in the flue gases caused high values for SO2. The A.S.M.E. test procedure was revised to prevent oxidation of sulfite in the absorption bottle and to allow for the effect of CO2; subsequent analyses of flue gases produced reliable results. The revised procedure is described.

Jan 1, 1950

By Joseph W. Town

The Bureau of Mines conducted studies related to SO2 air pollution to determine attritioning rates, SO2 sorption rates, and sulfur loads that could be obtained on commercial alkalized alumina sorbent pellets. Fluidized-bed attritioning rates ranged from 0.025 pct/hr for alkalized alumina with a crushing strength of 4 kg to 0.075 pct/hr for 0.5 kg crushing strength mate¬rial. Airlift attritioning rates ranged from 0.50 pct/hr for 3 kg crushing strength alkalized alumina to about 3 pct/hr for 0.5 kg material. Attritioning rates for the commercial alkalized alumina were comparable to those obtained for sorbent pellets prepared in the Bureau of Mines laboratory. Sorption rates were related to S02 concentration in flue gas, temperature, and presence of nitrogen oxides in the gas stream. Sorption rates at 300° C were 0.35 X 10-6 gS/gp/sec (grams sulfur per gram pellet per second) in 0.045 pct so, gas, 5.1 x 10-5 gS/gp/sec in 0.34 pct SO2 gas, and 65 X 10-5 gS/gp/sec in 10 pct SO2 gas. For the 0.34 pct S02 gas, sulfur loads of 0.10 gS/gp (the projected load for regeneration) were obtained in 47 min at 130° C and in 116 min at 300° C. The presence of either NO or NO2 in the 0.34 pet S02 gas increased the SO2 sorption rates 2 to 3 times at 300° C, but had no effect at 130° C.

Jan 1, 1969

By C. F. Swab

A relatively innocuous halocarbon was investigated as a substitute for the highly toxic carbon tetrachloride in the approval testing of chemical cartridges. The vapor effluent of 1,1,2-trichloro-1,2,2-trifluoroethane from chemical cartridges is continuously monitored by a nondispersive infrared analyzer. Breakthrough times for the cartridges, using the halocarbon, can be equated to those of carbon tetrachloride, if multiplied by the factor, 1.49.

Jan 1, 1970

By Ann G. Kim

Gas samples containing 02, N2, H2, He, CO2, CO, CH4, and trace amounts of C 2 to C6 hydrocarbons are analyzed by a gas chromatographic method that utilizes both thermal conductivity and flame ionization detectors. A porous polymer support and molecular sieve columns are used with argon as the carrier gas. A column selector valve makes it possible to perform a complete analysis either on one 1-ml sample in 40 minutes or on two samples in 20 minutes, one sample for each detector. Samples are introduced either by on-column injection or through a gas sampling valve. By varying operational parameters, the speed, sensitivity, and accuracy of analysis may be modified to suit a particular situation.

Jan 1, 1974

By John W. Buch

"INTRODUCTION The Ruhr coal basin is estimated to cover an area of more than 1,000 square miles. Here, the total thickness of the coal bearing formation (Carboniferous) is 10,500 feet, and drilling-hole have revealed 92 coal beds with a total thickness of 262 feet. 6/ Beds pitch from 0 to 90 degrees and about 70 percent of the wartime production came from beds that pitched less than 30 decrees. 5/For example at the Minisiter Stein mine, there are 24 minable coal beds ranging from 80 centimeters. (2 ft., 7 1/2 in.) to 250 centimeters (8 2 1/2 in.). The vertical thickness of the measures is 1,000 meters (3,200 ft.), and at this mine the deposits are covered with 150 meters (500 ft.) of surface wash. The cross section (fig, 1) at Fritz mine; Hoesch, A.G., Essen, Ruhr, is characteristic, The mines have been developed and worked to vertical depths of 2,000 to 2,500 feet by vertical shafts; main-level intervals are 500 to 700 feet apart. Haulage roads are straight, driven in rock, and centered as nearly as practical between property boundaries. Levels are sectionalized by driving crosscuts at right angles to the main haulage road on 800- to 900-foot centers. The roads are the main transportation arteries for the use of trolley or Diesel locomotives. A plan of the sixth main level (fig. 2) at the Bruchstrasse mine; Gelsenkirchener A.G., Bochum, illustrates main-level development and,sectionalizing with crosscuts. The cross section in figure 3 is that of the fourth crosscut west at the same mine."

Oct 1, 1946

By Arthur M. Hartstein

The Bureau of Mines, through contract with Ultrasystems, Inc., obtained data on the oxidative degradative behavior of a number of materials used in coal mines. Tests were performed using a stagnation burner arrangement. Materials examined included those used in typical coal mining operations such as (1) polyvinyl chloride-containing materials. (2) neoprene compositions, (3) rigid foams (urethanes/isocyanates), (4) miscellaneous materials (including jute, fiber glass, and polyethylene), (5) coal, (6) fluids (phosphate esters, organic esters, oil-water emulsions), and (7) composites. The composite comprised a mixture of a phosphate ester fluid with (1) coal, (2) a representative polyvinyl chloride sample, or (3) a neoprene-type composition. A number of decomposition products are identified that could represent a potential health hazard to miners including HC1, CO, SO2 and H2S, if they were generated to exceed toxic levels.

Jan 1, 1974

By D. E. Shanks

The Bureau of Mines investigated the effects of HCI concentration and solution temperature on the solubility and crystal form of the chlorides of Co, Mn, and Ni when sparged with HCI gas at temperatures of 20°, 40°, and 60° C. Increasing HCI concentration in solution caused the chlo-rides of Co, Mn, and Ni to crystallize (salt out) because of the common ion effect. The salting-out crystallization was most effective for NiCI2, which had a solubility of 0.7 pct at 20° C and maximum HCI concentration. COCl2 salted out to a minimum solubility of 9.4 pct at 20° C and 22 pct HCI concentration and increased in solubility at greater HCI concentrations because of the formation of chloride complexes. MnCl2 was intermediate in behavior. The effect of temperature on solubility was greatest for CoCl2 and least for NiCI2, 15 and 7 pct change, respectively, over the temperature range of 20° to 60° C. The salted-out chlorides of cobalt and nickel formed the hexahydrates and those of manganese formed the tetrahydrate in saturated metal chlo-ride solutions at 20° C and low concentrations of HCI. Increasing the temperature or the HCI concentration caused a 108s in waters of hydra-tion. At 60° C, the salted-out crystals of NiCl2 formed the tetrahydrate in HCI concentrations up to 18 pct and the dihydrate at higher concentrations, while cobalt and manganese chlorides formed the dihydrates, even in water.

Jan 1, 1985

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 D. N. Nilsen

The U.S. Bureau of Mines investigated the use of unsupported liquid emulsion membranes (LEM's) for the extraction of copper from relatively dilute aqueous solutions (=0.3 and 2.5 g/L Cu), The performance characteristics of the three main unit operations of an LEM circuit (emulsion generation, metal extraction, and emulsion breaking) were assessed in laboratory-scale batch tests. In single-stage extraction tests using 2.5-g/L Cu feed solution, emulsion membranes extracted up to 94 pct of the copper from solutions without pH adjustment and 99.7 pct when the pH was maintained at about 2.5. Simulated two-stage crosscurrent and countercurrent circuits extracted all but 3 and 4 ppm of the original copper content, respectively. Extraction data from solutions containing mixtures of metals indicated a strong preference for Cu2+ extraction when oxime-type extractants were used in the LEM; however, some coextraction of Fe 3+ and Zn2+ was experienced. An electrostatic coalescer was used to break the copper-loaded emulsions for separation of the component phases. Up to 96 pct of the contained stripping solution (internal solution) containing the extracted copper was separated from the organic phase of the emulsion membrane. The recovered organic phase was recycled without apparent problems.

Jan 1, 2010

1. In 2003, a total of 258 metal mining operations reported employment to the Mine Safety and Health Administration (MSHA). Metal mines were the smallest mining sector, comprising 1.8% of all mining operations.1 • Gold mines comprised 44.2% (n = 114) of all metal mining operations. Other common types of metal mines were iron ore (n = 29; 11.2%), copper ore (n = 28; 10.9%), and lead and/or zinc ore (n = 21; 8.1%). • Nevada had the largest number of metal mines (n = 48; 18.6%) followed by Alaska (n = 29; 11.2%).

Feb 1, 2005

By Thomas F. Tomb

The penetration characteristics of a horizontal plate elutriator and of a 10-mm nylon cyclone were evaluated. The test aerosols were polydisperse coal-dust particles ranging from less than 0.3 to 15 micrometers in diameter. Particle densities ranged from 1.3 to 1.4 grams per cubic centimeter. Equivalent Stokes diameters were measured using Coulter counter analytical techniques. Experimental results indicate that the penetration characteristics of the horizontal plate elutriator closely approximate the sampling efficiency curve defining the respirable fraction of the dust cloud recommended and adopted by the Johannesburg Pneumoconiosis Conference in 1959. Penetration characteris-tics of the 10-mm cyclone were evaluated at flow rates of 1.4, 1.5, 2.0, 2.5, and 2.8 liters of air per minute. The data indicate that the penetration curve obtained at 2.0 liters per minute most closely approximates the sampling efficiency curve for respirable dust recommended at a meeting sponsored by the U.S. Atomic Energy Commission in 1961.

Jan 1, 1970