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By H. V. Makar

Laboratory tests were performed to obtain a quantitative description of the effectiveness of sodium sulfate (Na2SO4) for removing copper from molten iron and to determine the effectiveness of Na2SO4 on actual auto scrap. The tests were conducted on induction melted heats of iron averaging 0.58 and 1.50 percent initial copper and on cupola-melted auto scrap containing 0.45 percent initial copper. The Na2SO4 was added in powder form in amounts ranging from 2.9 to 43.8 percent of the weight of iron being treated. The data showed that copper removal for the various Na2SO4 treatments followed a similar trend, regardless of the iron composition that was tested. The equation Y = 1 - e-3.23x approximately reflects the relationship between copper removal and amount of Na2SO4 added, where Y is the fraction of copper removed and x is the ratio of the weight of Na2SO4 added to the weight of metal treated. Copper removals ranged from 3.3 to 74.5 percent and reductions down to less than 0.10 percent final copper were achieved in the auto scrap. Copper removals were generally accompanied by sulfur removal, and initial sulfur contents ranging from 0.10 to 0.20 percent were reduced to as low as 0.02 percent. High temperatures and long slag reaction times tended to induce copper and sulfur reversion from the slag, but, generally, the Na2SO4 treat¬ments were effective up to approximately 2,820° F with reaction times not exceeding 7 minutes.

Jan 1, 1968

By Shiro Watanabe

To determine the potentialities of nickel as a substitute for cobalt in catalysts for the synthesis of hydrocarbons from carbon monoxide and hydrogen, RESULTS The maximum oil yields obtained in bench-scale equipment were as follows: Using 100N1:20Mn:100 kaolin:200 diatomaceous earth catalyst, a maximum yield of 133.8 cm.3/m.3 of pure CO+2H2 was obtained from one pass of the feed gas, With a nickel:cobalt mixed catalyst (Ni:Co - 3:7) having the composition 100(Ni+Co):8MgO: 5Th02:200 diatomaceous earth, a maximum of 172.2 cm.3/m.3 of pure C0+2H2 was obtained.

Jan 1, 1951

By Mary F. Koehler

Continuing a program of thermochemical investigation of compounds of to ferroalloy elements, this paper contains ins values of the heats of formation of two sodium molybdates (Na2Mo04 and Na2Mo207) and three sodium tungstates (NO2W4, Na2W207, and NA2W207, and Na2W4013). The experimental method was solution calorimetry. The solution medium was sodium hydroxide solution, except that hydrofluoric acid solution was used for sodium tetratungstate. The heat of formation values are given with reference both to the constit¬uent elements and to the constituent oxides. These data are of prime impor¬tance in the thermodynamic consideration of these substances, as their accumulation includes the most difficult and time-consuming steps toward evaluating the free energies of formation and thus the potential reactivities and thermal stabilities. Except for values for sodium monomolybdate and monotungstate, no previous similar data were contained in literature sources.

Jan 1, 1962

By K. O. Bennington

Thermodynamic properties were determined by the Federal Bureau of Mines for lithium metasilicate (Li2Si03) and lithium disilicate (Li2Si205). Their enthalpies of formation were investigated by hydrofluoric acid solution calorimetry. The standard values are ?Hf°298 -393.8 ± 0.8 kcal/mole for Li2Si03, and ?Hf°298 -611.8 ± 1.0 kcal/mole for LiSi205. Enthalpy increments above 298 K were measured by copper-block drop calorimetry from 298 to 1,404 K for Li2Si03, and from 298 to 1,281 K for Li2Si205. Low-temperature heat capacities were determined adiabatically from 6 to 305 K for Li2Si205 only. The derived standard entropy is S°298 = 29.20 ± 0.10 cal/deg-mole. The various experimental data were combined with other data from the literature, and resulting properties of ?Hf°, ?Gf°, and log Kf were tabulated as a function of temperature.

Jan 1, 1976

By J. E. Dooley

Reference mass spectra and analytical correlations for 20 alkylcycloalkyl sulfides and two dicycloalkyl sulfides are presented 'to provide information that will facilitate the identification of sulfur compounds occurring in natural or synthetic mixtures. Reference spectra indicate relative intensities in addition to parent and base peak sensitivities. Analytical correlations establish the ionic species that reflect major fragmentation paths for the com-pounds studied. Specifically, the correlations show that base peaks are formed by several different processes: (1) Cleavage of the bond a to the ring, (2) fragmentation of the alkyl chain, and (3) fragmentation of the ring plus fragment contribution from the alkyl chain. Useful correlations for deter-mining alkyl chain length involve the CnH2+3S+ and CnH2n+1 + ions. CnH2n-2+ and CnH2n-1 S+ ions reveal the number of carbon atoms in the cyclic ring. Other important ionic species are also discussed.

Jan 1, 1970

By F. S. Karn

Measurements were made of the flow of helium, methane, ethane, butane, and toluene through thin disks of coal. All measurements were made on a dense layer in the Pittsburgh seam identified as attritus. Flow increased with pressure differential and temperature. At room temperature and a pressure differential of 1 atmosphere flow rates along the bedding plane of Pittsburgh seam coal were helium 881 X 10-10 cm2 sec-1, methane 1.2 X 10 -10 cm2 sec-1, ethane 0.54 X 10-10 cm 2 sec-1, n-butane 0.35 X 10-10 cm2sec-1, and toluene 3.8 X 10-10 cm2sec-1. Flow rates were 50 percent lower across the bedding plane of the coal than along the bedding plane. Activation energies were 3.9 kcal mole-1 for helium and 13.6 kcal mole-1 for methane, with diffusion measured either along or across the bedding plane.

Jan 1, 1970

By H. C. Ko

Calorimetric determinations of low-temperature heat capacities and standard enthalpy of formation were made by the Federal Bureau of Mines for basic aluminum sulfite, A1203?2.0S02?5.3H20. The standard values of entropy (S°), enthalpy of formation (?Hf°), and calculated Gibbs energy of formation (?Gf°) at 298.15 K are 85.2±0.1 cal/deg-mole, -943.1±1.2 kcal/mole, and -820.7±1.2 kcal/mole, respectively.

Jan 1, 1976

By A. L. Engel

The Stayton Mining District in San Benito County, Calif., near Hollister, includes several square miles with many occurrences of antimony ore. The sample submitted for the test described in this paper came from a vein said to have been traced and sampled for 5,000 feet on the surface, 1,500 feet carrying 2-1/2 to 3 percent antimony and the remainder 1/2 to 2 percent. Thirty thousand tons 'With a content of 3 percent antimony are said to be blocked out. A drift of 200 feet on the vein has shown ore containing 4.2 percent antimony. The present sample assayed 3.8 percent. Previous flotation investigation of this are resulted in a recovery of only 71.6 percent in concentrates containing 56.8 percent Sb. It was desired to develop a method of treatment that would give better results. The antimony in the sample occurred as the mineral stibnite, Sb2S3, antimony sulfide.

Jan 1, 1949

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 D. G. Kuehn

Mass spectrographic studies have been conducted on the positive ions and neutral species of glow discharges containing 1.0 pct S02 and 1.0 pct CO in helium. Measurements were conducted for gas pressures from 3.5 to 10.1 torr using both dc and 60-Hz ac excitation. The ion species that were observed included S+, SO+, SO+, 0+, O2+, C+, CO+, and CO2+ with lesser amounts of SO3+, (CO)2+, SCO+, and (SO?CO)+ or CS+2. Interpretation of the functional dependence of the various ionic and neutral species on pressure and applied power showed that CO reacted with the SO formed in the discharges to produce CO2 and sulfur. Deposition of elemental sulfur was observed in the plasma container.

Jan 1, 1973

By W. H. Oppelt

A small, annular-retort gasifier having a nominal capacity of 40 pounds of lignite per hour was designed and constructed at the Lignite Experiment Station, Grand Forks, N. Dak. The purpose of the investigation was to increase the capacity of an annular-retort gasifier by better temperature distribution in the heating chamber (adjacent to the annulus) and by supplemental internal heating with controlled amounts of air. Correct control of air admission should yield crude ammonia-synthesis gas having a (H2+CO)-N2 ratio of 3. Dakota Star stoker-size lignite was used during the exploratory experimental program. The effects of temperature level and distribution in the heating chamber and of addition of air to the reactor were investigated. Hydrogen - carbon monoxide ratios ranged from 1.9 to 2.5, and (H2+C0)-N2 ratios were as low as 2.9. Hourly gas production ranged from 970 to 2,580 cu. ft., or 62.0 to 164 cu. ft. per sq. ft. of heated surface, or 350 to 940 cu. ft. per cu. ft. of reactor volume. Data from the small gasifier could be readily correlated with those previously obtained in the commercial-scale unit under comparable experimental conditions.

Jan 1, 1957

By G. B. Atkinson

The Bureau of Mines, in cooperation with McDermitt Mine, investigated a method for recovering mercury metal from mercury sulfide flotation concentrate by a hydrometallurgical technique. This preliminary report shows the feasibility of leaching mercury with a cupric chloride solution and electrowinning mercury from the solution. Proposed chemical reactions are shown in equations 1 through 3: 2CuC12 + HgS + 2CuCl + HgC12 + S°; (1) electrolysis HgC12 ?Hg + C12; (2) 2CuC1 + C12 ? 2CuC12. (3) A bench-scale leaching-electrowinning apparatus capable of treating 2.36 kg of sulfide concentrate in 11 days was operated continuously. An acid chloride solution containing, in grams per liter, 70 Ca, 60 Cu, 30 Fe, and 80 Hg was used as both leachant and electrolyte; 99.5 pct of the mercury was solubilized from the sulfide concentrate. Electrolysis of the leaching solution recovered mercury metal at an average current efficiency of 32 pct and an average energy consumption of 1.2 kwhr/lb Hg. Results from a preliminary economic evaluation indicated that a plant producing 31,500 flasks of mercury per year would have a capital cost of $3.7 million and an operating cost of $62 per flask of mercury.

Jan 1, 1983

By G. A. Smyres

A GaC12--B2 l-eachtng procedure and meEal-recovery method for treating an arsenical Cu-Co sulfide concentrate was developed by the Bureau of Mines as an alternative to smelting, which is no longer considered an environmentally acceptable method for treating arsenic-containing ores. The procedure involved leaching in a CaC12 solution with CaC03 for 96 h at 26 pct solids (concentrate and CaC03), 1150 C, and a pressure of 50 psig (345 kPa) with oxygen. More than 98 pct of the cobalt and 97 pct of the copper were extracted, and 99.98 pct of the arsenic and 99.9 pct of the iron remained in the leached residue. A filtration rate of 2.9 gal/(ft2.h) [118 L/(m2.h)] and a cake formation rate of 36 Ib/(ft2.h) [172 kg/(m2.h)] were obtained by filtering reacted pulp at 1000 C. More than 99 pct of the copper in the pregnant solution was extracted as CuCl2 by golvent extraction with a new copper extractant. Copper was stripped from the loaded organic with a sulfate-chloride solution, which was used as the anolyte for electrowinning of copper in a membrane cell. Copper plate produced was more than 99.99 pct pure and requi.red 0.81 (kW'h)/lb Cu [1.78 (kW·h)/kg Cu]. Cobalt sulfide was precipitated at pH 3 with Ca(HS)2.

Jan 1, 1986

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 Agnes Y. Lee

As part of the U.S. Bureau of Mines program to improve base metal leach systems, pressure leaching of galena (PbS) concentrates in fluosilicic acid (H2SiF6) solution was investigated. Lead extraction was 93 pct when PbS was pressure leached in H2SiF6 at 95° C with 2OO-psig O2 pressure for 40 min, using ferric nitrate [Fe(N03)3] as a catalyst. The effects of several catalysts, O2 pressure, time, and acid concentration on leaching were determined. The purified leach solution was electrowon to recover high-purity Pb metal. The H2SiF6 used in leaching and electrowinning can be recycled continuously. A flow diagram was proposed based on this investigation. Elemental sulfur (SO) was recovered from the leach residue by solvent extraction. A method was also developed for treating the flnal residue to segregate the important byproduct elements such as Ag, Cu, and Zn and enable their recovery by standard commercial processes.

Jan 1, 1990

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 L. J. Froisland

The U.S. Bureau of Mines conducted laboratory studies on sulfuric acid (H2S04) digestion of alunite [KA13(S04)2(OH)6] as a means for treating domestic deposits of this mineral. Digesting alunite ore in boiling H2S04 at concentrations of 88-wt-pct acid or higher breaks down the alunite and permits a convenient separation of potassium and aluminum. The digestion reaction is a complex sulfation reaction occurring in two stages. In this reaction, the potassium component extracts into the H2S04 for eventual recovery as potassium sulfate k2s04 in a separate unit operation. Aluminum is left as acid-insoluble aluminum sulfate [A12(S04)a], which can be extracted by a 95° C water leach. Additional purification of AI2(S04)a produced in this study is needed to meet cell-grade alumina (Al202) purity specifications. Extraction and separation of potassium and aluminum from the alunite ore were consistently above 90 pct.

Jan 1, 1989

By A. U. Christensen

THERMODYNAMIC data for many of the common interoxidic compounds are seriously lacking, and appraisal of possible ceramic or metallurgical applications depends upon dubious estimates. In particular, high-temperature heat-content estimates may be invalid because of unknown phase-transformations. This paper reports experimental heat-content values above 298.15° K. for five interoxidic compounds-the aluminates of lithium and sodium (LiAlO2 and NaAlO2), the ferrites of lithium and sodium (LiFeO2 and NaFeO2), and lithium titanate (Li2TiO3), as obtained by the Bureau of Mines. Sodium aluminate, sodium ferrite, and lithium titanate were found to have previously unknown transformations in the crystalline state. The heats and temperatures of these transformations were evaluated as were also the heats and temperatures of fusion of sodium ferrite and lithium titanate. The heat-content results are assembled in both tabular and algebraic-equation form for use in conducting thermodynamic calculations at temperatures in the range 298°-2,000° K.

Jan 1, 1960

By Nicholas Kyriazi

A performance comparison of 14 rescue breathing apparatus was undertaken as an assessment of past and present worldwide technology. Rescue breathing apparatus are self-contained, closed-circuit breathing apparatus used for entry into areas having atmospheres that are immediately dangerous to life and health. Apparatus tested were the Biomarine BioPak 45, 60, and 240; the Draeger BG 4 and BG-174A; the Litton LITPAC II; the MSA Custom 4500 II Air Mask, Chemox, and McCaa; the Sabre Selected Elevated Flow Apparatus (SEFA); the Scott Rescue-Pak; the Siebe Gorman Aerorlox and Proto Ten; and the SurvivairLP-120. The apparatus were tested on an automated breathing and metabolic simulator at the Pittsburgh Research Laboratory of the National Institute for Occupational Safety and Health (NIOSH). Physiological parameters monitored during the testing were average inhaled CO2 and O2, minimum inhaled CO2, inhaled wet-and dry-bulb temperatures, and peak inhalation and exhalation breathing pressures. The metabolic demand on the apparatus was 1.35 L O2/min for most of the test with two 5-min intervals of 2.5 L O2/min, the first beginning 10 min into the test and the second beginning 10 min before the end of the rated duration of the apparatus. Results presented include apparatus service life and test-averages of monitored physiological parameters. Schematic drawings and photographs of the apparatus are also included. The Draeger BG-174A and BG 4 had the highest durations—295 and 291 min, respectively. The BG 4 hadthe lowest minimum inhaled CO2 levels, attesting to the effectiveness of its CO2-absorbent canister. The SabreSEFA had the lowest average inhaled CO2 levels, due mostly to the apparently low-dead-space mask andnose cup. The MSA Air Mask, the only open-circuit device tested, had the lowest wet- and dry-bulb temperatures, with the liquid-O2-source Siebe Gorman Aerorlox having the next lowest temperatures. The only apparatus with a CO2-absorbent not in a packed-bed design, the BG-174A, had the lowest exhalation pressures. The BG 4 had the highest level of positive pressure, with the Biomarine BioPak 60, Survivair LP-120, SEFA, and Litton LITPAC II nearly as high. The BG 4 had the lowest pressure swing, with the SEFA a close second.

Jan 10, 1999

By Larry A. Haas

The chemistry of current or potential SO2 removal processes can be placed into four categories: (1) reduction, (2) Liquefaction, (3) direct dissolution, and (4) oxidation. Methods that involve reducing SO2 to elemental sulfur appear promising since this product can be easily handled, shipped, and stock- piled. Unfortunately, SO2 cannot always be reduced directly when other oxidizing agents are present. Thermodynamic data indicate that some oxidizing reagents will also consume reductant at the reduction temperature. A two- stage process can be applied to waste gases that contain excessive quantities of oxygen, nitrogen oxides, and water vapor. The best sorbent for the first stage appears to be a nonalkali or nonalkaline earth medium since this medium more readily releases the SO2 for reduction in the second stage.

Jan 1, 1973