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PubMed2003

Investigation of winter atmospheric aerosol particles in downtown Katowice using XPS and SEM.

X-ray photoelectron spectroscopy (XPS) was used to determine the surface chemical composition of atmospheric particles (PM-10 and PM-2.5), collected in downtown Katowice, Upper Silesia, Poland, in the winter season (November and December 2000). Carbon- and oxygen-containing species dominated the particulate surface with traces of N, S, Si, Cl, Na, Zn, Al, Cu, Fe, Ca, K, Mg, Pb, and P present. Additionally, the size, morphology, and chemical composition of about 300 of the individual atmospheric particles were analyzed by high-resolution scanning electron microscopy and electron probe microanalysis. A number of aluminosilicates and metallic elements such as Fe, K, Mg, Zn, as well as rare earth elements, were detected by SEM. The results obtained show that the analyzed aerosol is of natural and anthropogenic origin. Particles containing sulfur compounds as well as oxygen and sodium in downtown Katowice come mainly from the east and southeast sectors.

Journal Article↗
PubMed2002

Unsuitability of Cr(II) reduction for the measurement of sulfides in oxic water samples.

After developing a highly sensitive method for detecting acid-volatile sulfides (AVS) in oxic freshwaters, we hoped to apply that method to measuring a different class of dissolved reduced sulfur compounds, chromium-labile sulfides (CLS). A popular method for measuring this pool of sulfides in sediments relies on reduction dissolution of metal sulfides by Cr(II) and has been employed by researchers for over 15 years. Here, we demonstrate that this method is inappropriate for measuring CLS in oxic freshwaters in which sulfate concentrations are large relative to the dissolved metal sulfides. We observe the reduction of sulfate by Cr(II), and this presents a significant interference.

Chromium↗
PubMed1988

Mechanism-based inhibition of lactoperoxidase by thiocarbamide goitrogens. Identification of turnover and inactivation pathways.

Direct evidence is presented in support of mechanism-based (suicide) inactivation of lactoperoxidase by thiocarbamide thyroid inhibitors. The turnover of 1-methylbenzimidazolidine-2-thione was demonstrated by identifying the inhibitor-derived products 1-methylbenzimidazole and bisulfite ion that are formed concurrent to enzyme inactivation. The turnover of a hydroperoxide cosubstrate, 5-phenyl-4-pentenyl hydroperoxide, was quantitated from formation of the corresponding alcohol during enzyme inactivation. A specific inactivation pathway is suggested by the covalent binding of 1 mol of 14C- and 35S-labeled benzimidazolidine-2-thione and 1-methylbenzimidazolidine-2-thione per mole of inactivated lactoperoxidase. These results are explained by partitioning of inhibitor-derived S-oxygenated intermediates between turnover and inactivation pathways. The properties of the inactivation process are unique among thiono-sulfur compounds and suggest that benzimidazolinesulfenic acids are the reactive intermediates.

Antithyroid Agents↗
PubMedDate not supplied

Biodesulfurization of flue gases and other sulfate/sulfite waste streams using immobilized mixed sulfate-reducing bacteria.

Sulfur dioxide (SO2) is one of the major pollutants in the atmosphere that cause acid rain. Microbial processes for reducing SO2 to hydrogen sulfide (H2S) have previously been demonstrated by utilizing mixed cultures of sulfate-reducing bacteria (SRB) with municipal sewage digest as the carbon and energy source. To maximize the productivity of the bioreactor for SO2 reduction in this study, various immobilized cell bioreactors were investigated: a stirred tank with SRB flocs and columnar reactors with cells immobilized in either potassium-carrageenan gel matrix or polymeric porous BIO-SEP beads. The maximum volumetric productivity for SO2 reduction in the continuous stirred-tank reactor (CSTR) with SRB flocs was 2.1 mmol of SO2/(h.L). The potassium-carrageenan gell matrix used for cell immobilization was not durable at feed sulfite concentrations greater than 2000 mg/L (1.7 mmol/(h.L)). A columnar reactor with mixed SRB cells that had been allowed to grow into highly stable BIO-SEP polymeric beads exhibited the highest sulfite conversion rates, in the range 16.5 mmol/(h.L) (with 100% conversion) to 20 mmol/(h.L) (with 95% conversion). The average specific activity for sulfite reduction in the column, in terms of dry weight of SRB biomass, was 9.5 mmol of sulfite/(h.g). In addition to flue gas desulfurization, potential applications of this microbial process include the treatment of sulfate/sulfite-laden wastewater from the pulp and paper, petroleum, mining, and chemical industries.

Air Pollutants↗
PubMed2001

Source regions for atmospheric aerosol measured at Barrow, Alaska.

Aerosol data consisting of condensation nuclei (CN) counts, black carbon (BC) mass concentration, and aerosol light scattering coefficient at the wavelength of 450 nm (SC) measured at Barrow, AK, from 1986 to 1997 have been analyzed. BC and SC show an annual cycle with the Arctic haze maxima in the winter and spring and the minima in the summer. The CN time series shows two maxima in March and August. Potential source contribution function (PSCF) that combines the aerosol data with air parcel backward trajectories was applied to identify potential source areas and the preferred pathways that give rise to the observed high aerosol concentrations at Barrow. Ten-day isentropic back trajectories arriving twice daily at 500 and 1500 m above sea level were calculated for the period from 1986 to 1997. The PSCF analyses were performed based on the 80th percentile criterion values for the 2- and 24-h averages of the measured aerosol parameters. There was a good correspondence between PSCF maps for the 2- and 24-h averages, indicating that 1-day aerosol sampling in the Arctic adequately represents the aerosol source areas. In winter, the high PSCF values for BC and SC are related to industrial source areas in Eurasia. The trajectory domain in winter and spring is larger than in summer, reflecting weaker transport in summer. No high PSCF areas for BC and SC can be observed in summer. The result is related to the poor transport into the Arctic plus the strong removal of aerosol by precipitation in summer. In contrast to the BC and SC maps, the CN plot for summer shows high PSCF areas in the North Pacific Ocean. High CN values appearto be mostly connected with the long-range transport from Eurasia in winter and spring and with the reduced sulfur compound emission from biogenic activities in the ocean in the summer. PSCF analysis was found to be effective in identifying potential aerosol source areas.

Aerosols↗
PubMed2005

Effect of lubricant on the formation of heavy-duty diesel exhaust nanoparticles.

The effect of lubricants on nanoparticle formation in heavy-duty diesel exhaust with and without a continuously regenerating diesel particulate filter (CRDPF) is studied. A partial flow sampling system with a particle size distribution measurement starting from 3 nm, approximately, is used. Tests are conducted using four different lubricant formulations, a very low sulfur content fuel, and four steady-state driving modes. A well-documented test procedure was followed for each test. Two different kinds of nanoparticle formation were observed, and both were found to be affected bythe lubricant but in differentway. Without CRDPF, nanoparticles were observed at low loads. No correlation between lubricant sulfur and these nanoparticles was found. These nanoparticles are suggested to form mainly from hydrocarbons. With CRDPF, installed nanoparticles were formed only at high load. The formation correlated positively with the lubricant (and fuel) sulfur level, suggesting that sulfuric compounds are the main nucleating species in this situation. Storage effects of CRDPF had an effect on nanoparticle concentration as the emissions of nanoparticles decreased over time.

Lubrication↗
PubMed2005

Adsorption of hydrogen sulfide onto activated carbon fibers: effect of pore structure and surface chemistry.

To understand the nature of H2S adsorption onto carbon surfaces under dry and anoxic conditions, the effects of carbon pore structure and surface chemistry were studied using activated carbon fibers (ACFs) with different pore structures and surface areas. Surface pretreatments, including oxidation and heattreatment, were conducted before adsorption/desorption tests in a fixed-bed reactor. Raw ACFs with higher surface area showed greater adsorption and retention of sulfur, and heat treatment further enhanced adsorption and retention of sulfur. The retained amount of hydrogen sulfide correlated well with the amount of basic functional groups on the carbon surface, while the desorbed amount reflected the effect of pore structure. Temperature-programmed desorption (TPD) and thermal gravimetric analysis (TGA) showed that the retained sulfurous compounds were strongly bonded to the carbon surface. In addition, surface chemistry of the sorbent might determine the predominant form of adsorbate on the surface.

Adsorption↗
PubMed2005

Pyrite oxidation by hexavalent chromium: investigation of the chemical processes by monitoring of aqueous metal species.

Pyrite, an iron sulfide, occurs in many soils and sediments, making it an important natural reductant of toxic metal pollutants. This study investigated the processes leading to aqueous Cr(VI) reduction by pyrite in a closed thermostated (25 +/- 0.1 degrees C) system and under an argon atmosphere. Synthetic pyrite suspensions were reacted with a range of Cr(VI) solutions from 0 to 7 x 10(-4) M and at pH 2-8. Metal species concentrations were continuously monitored during a period lasting approximately 20 h. Preliminary experiments carried out in acidic media without Cr(VI) have shown that some pyrite dissolution occurred. Then, metal species concentration changes with time during pyrite oxidation by Cr(VI) solutions exhibited two distinct trends depending on the complete or incomplete Cr(VI) removal. As long as chromate existed in solution, the Cr-(Ill) to Fe(lIl) ratio was found to be an effective parameter to investigate the pyrite reaction stoichiometry with Cr(VI). Experimental values close to 2 suggest that sulfur compounds with oxidation states between 0 and 2 should be formed during pyrite oxidation by Cr(VI). If Cr(VI) was completely reduced from solution, then the pyrite oxidation by Fe(lll) ions took place to generate ferrous ions.

Argon↗
PubMed2006

Stainless steels can be cathodically protected using energy stored at the marine sediment/seawater interface.

Laboratory-scale experiments were performed in which the corrosion protection of stainless steels in seawater was afforded by cathodic protection. The method was implemented for the first time using the potential difference at the marine sediment/seawater interface as the only source of electric power. Graphite electrodes buried in marine sediment, developing a potential of -0.45 V versus a saturated calomel electrode (SCE), were used as anodes to cathodically polarize UNS S30403 stainless steel coupons that were exposed to seawater. The cathodic protection system was operated with low polarization of stainless steel, typically to -0.2 V (vs SCE) and was found to properly prevent material failure even in the presence of a well-developed biofilm. With voltammetry, the protection current was found to be related to the oxidation of reduced sulfur compounds in the sediments. Results demonstrate that this inexpensive and environmentally friendly method can, so far, extend the service life of stainless steels in seawater.

Biofilms↗
PubMed2005

Methyl transfer from CH(3)Co(III)Pc to thiophenoxides revisited: remote substituent effect on the rates.

A two-step mechanism of the reaction of CH(3)Co(III)Pc (Pc = dianion of phthalocyanine) with thiophenoxides in DMA has been confirmed, and the visible spectrum of the inactive transient, CH(3)Co(III)Pc(SAr)(-), has been determined. Rapid rates for ligation of CH(3)Co(III)Pc, yielding CH(3)Co(III)Pc(S-C(6)H(4)-X)(-), are virtually independent of X; this step proceeds probably by an I(d) mechanism. Kinetic data for the follow-up methyl-transfer step yield second-order rate constants and stability constants for CH(3)Co(III)Pc(S-C(6)H(4)-X)(-) consistent with those estimated from concentration dependence of the amplitude of the ligand-exchange step. Cyclic voltammetry provides first reduction potential for CH(3)Co(III)Pc(DMA) of -1.42 V vs Fc(+)/Fc, which makes an OSET mechanism unlikely. Homolytic decay of CH(3)Co(III)Pc(SAr)(-) has also been ruled out. All of the kinetic data, including Hammett's rho = -2.3 +/- 0.1, N-donor inhibition, and alkyl group effect, Me > Et, indicate that the reaction is a normal S(N)2 methyl transfer, only very fast. Methyl transfer to aliphatic thiolates is also rapid and follows the same S(N)2 mechanism. Exceptional methyl-transfer reactivity of the phthalocyanine model sharply contrasting with the inertness of methylcobaloxime is explained.

Cobalt↗
PubMed2007

Quantitative geometric descriptions of the belt iron atoms of the iron-molybdenum cofactor of nitrogenase and synthetic iron(II) model complexes.

Six of the seven iron atoms in the iron-molybdenum cofactor of nitrogenase display an unusual geometry, which is distorted from the tetrahedral geometry that is most common in iron-sulfur clusters. This distortion pulls the iron along one C3 axis of the tetrahedron toward a trigonal pyramid. The trigonal pyramidal coordination geometry is rare in four-coordinate transition metal complexes. In order to document this geometry in a systematic fashion in iron(II) chemistry, we have synthesized a range of four-coordinate iron(II) complexes that vary from tetrahedral to trigonal pyramidal. Continuous shape measures are used for a quantitative comparison of the stereochemistry of the Fe atoms in the iron-molybdenum cofactor with those of the presently and previously reported model complexes, as well as with those in polynuclear iron-sulfur compounds. This understanding of the iron coordination geometry is expected to assist in the design of synthetic analogues for intermediates in the nitrogenase catalytic cycle.

Iron↗
PubMed2006

The true nature of the Di-iron(III) gamma-Keggin structure in water: catalytic aerobic oxidation and chemistry of an unsymmetrical trimer.

The complex [gamma(1,2)-SiW(10){Fe(OH(2))}(2)O(38)](6)(-) (1) has been reported to catalyze the much sought reductant-free selective O(2)-based epoxidation of alkenes (Nishiyama, Y.; Nakagawa, Y.; Mizuno, N. Angew. Chem. Int. Ed. 2001, 40, 3639-3641) in chlorocarbon-acetonitrile solution. The challenge of reproducing catalysis by 1 led us to examine this chemistry in detail. In H(2)O, a desirable solvent for catalysis, 1, does not exist in the proposed organic-medium form in which the two iron atoms are in the binding pocket defined by the equatorial oxygens and, importantly, by two oxygens bound to the central Si heteroatom. Instead, 1 in H(2)O initially forms an unusual trimer [{Fe(2)(OH)(3)(H(2)O)(2)}(3)(gamma-SiW(10)O(36))(3)](15)(-) (2). The X-ray structure of 2 shows that the Fe-O(Si) bonds are cleaved and new bonds (mu-hydroxo bridges) form between these Fe centers and those of the neighboring [gamma(1,2)-SiW(10)Fe(2)] units. Structural, physical, and computational evidence indicate that if the bonds between the d-electron center, M (Fe in the case of 1 and 2), and the terminal ligands on M are stronger than the M-O(x)() bonds, then the out-of-pocket form is more stable and is the one observed. Significantly, 2 in H(2)O forms an intermediate that catalyzes the effective aerobic oxidation of sulfur compounds (mercaptoethanol is oxidized to the corresponding disulfide by O(2) at ambient pressure and temperature). All experimental findings are consistent with dissociation of a gamma-SiW(10) Keggin unit from the trimer, 2, to form the catalytically active species.

Journal Article↗
PubMed2002

Formation of methanethiol and dimethyl disulfide in crushed tissues of broccoli florets and their inhibition by freeze-thawing.

The formation of methanethiol and dimethyl disulfide in crushed, homogenized, and frozen-thawed tissues of broccoli florets was investigated. These volatile sulfur compounds were produced in crushed florets, but their formation was inhibited in frozen-thawed tissues. Only dimethyl disulfide was formed in homogenized tissues. High pH treatment triggered the release of dimethyl disulfide in frozen-thawed tissues and also enhanced the action of cysteine sulfoxide lyase in all disrupted tissues. Methyl methanethiosulfinate and methyl methanethiosulfonate were not detected in crushed florets; thus, the favored mechanism for the formation of methanethiol and dimethyl disulfide is the chemical disproportionation of methanesulfenic acid. In contrast, the formation of dimethyl disulfide in frozen-thawed and homogenized tissues occurs from the chemical disproportionation of methyl methanethiosulfinate that was detected in these tissues. The inhibition of dimethyl disulfide production during freeze-thawing must be caused by a sudden drop in the pH of the tissue, adherence of dimethyl disulfide on the tissue surfaces, and weakening of the cysteine sulfoxide lyase activity under acidic conditions.

Brassica↗
PubMed2003

Effects of garlic powders with varying alliin contents on hepatic drug metabolizing enzymes in rats.

The anticarcinogenic effect of garlic has been demonstrated in both epidemiologic and experimental studies. In this study, possible mechanisms involved in the anticarcinogenic effect of garlic consumption were assessed by determining its capacity to alter drug metabolizing enzymes, in relation with its alliin content. Rats were fed a diet for 2 weeks containing 5% garlic powders produced from bulbs grown on soils with different levels of sulfate fertilization and therefore containing differing amounts of alliin. Activities of several hepatic enzymes, which are important in carcinogen metabolism such cytochromes P450 (CYP) and phase II enzymes, were determined. Garlic consumption slightly increased ethoxyresorufin O-deethylase and CYP 1A2 levels. In contrast, garlic consumption decreased CYP 2E1 activity and the level of the corresponding isoform. UDP glucuronosyl transferase and glutathion S-transferase activities were increased by garlic powders. The alliin content of the garlic powders was positively correlated with UGT activity although not with other activities. Effects produced by garlic consumption were qualitatively similar to that of diallyl disulfide, a sulfur compound that has been extensively studied. These data could partially explain the chemoprotective effect of garlic.

Animals↗
PubMed2004

Alpha-mercaptoketone formation during the maillard reaction of cysteine and [1-(13)C]ribose.

The volatiles formed from [1-(13)C]-ribose and cysteine during 4 h at 95 degrees C in aqueous phosphate buffer (pH 5) were analyzed by headspace SPME in combination with GC-MS. The extent and position of the labeling were determined using MS data. The identified volatiles comprised sulfur compounds such as 2-[(13)C]methyl-3-furanthiol, 2-[(13)CH(2)]furfurylthiol, [1-(13)C]-3-mercaptopentan-2-one, [1-(13)C]-3-mercaptobutan-2-one, [4-(13)C]-3-mercaptobutan-2-one, and 3-mercaptobutan-2-one. The results confirm furan-2-carbaldehyde as an intermediate of 2-furfurylthiol, as well as 1,4-dideoxypento-2,3-diulose as an intermediate of 2-methyl-3-furanthiol and 3-mercaptopentan-2-one. Loss of the C-1 and C-5 carbon moieties during the formation of 3-mercaptobutan-2-one suggests two different mechanisms leading to the key intermediate butane-2,3-dione.

Buffers↗
PubMed1999

Chemiluminescent methods in alcoholic beverage analysis.

Chemiluminescent (CL) techniques employed in alcoholic beverage analysis are summarized. Specific applications to wine, beer, brandy, and tequila are described, and the determination of sulfur compounds, phosphate, L-malate, glycerol, fatty acids, phenolic compounds, and urate is included. Possibilities and limitations of the various CL detection systems are evaluated.

Alcoholic Beverages↗
PubMed2000

CS(2) blinds in Brassica crops: false positive results in the dithiocarbamate residue analysis by the acid digestion method.

Various members of the Brassicaceae family (cauliflower, savoy cabbage, red cabbage, turnip-rooted cabbage) grown without any application of pesticides were analyzed according to the acid digestion method commonly used for the determination of dithiocarbamate fungicide residues. Depending on postharvest treatments, high non-anthropogenic CS(2) values up to 4 mg/kg were found in some cases, especially in frozen raw cabbage samples, exceeding maximum residue limits. To explore phytogenic CS(2) occurrences, two model substances (phenylisothiocyanate and methyl tryptaminedithiocarbamate) representing natural mustard oils and brassinines, respectively, were analyzed for their acid hydrolysis decomposition products. In both cases, COS was found generally, but CS(2) was readily formed during acid digestion, too, when sulfides were present. The results obtained clearly demonstrate that CS(2) values determined by using the acid digestion method of crops rich in secondary metabolism sulfur compounds have to be interpreted carefully.

Brassicaceae↗