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PubMed2003

Highly sensitive determination of a polymeric hindered amine light stabilizer in polypropylene by reactive thermal desorption-gas chromatography using nitrogen-specific detection.

Highly sensitive and specific determination of trace amounts of a polymeric hindered amine light stabilizer (HALS) in polypropylene (PP) materials could be established by improving reactive thermal desorption-gas chromatography (RTD-GC) in the presence of an organic alkali, tetramethylammonium hydroxide. By using nitrogen-phosphorus detection, highly selective detection of the HALS-related components was attained. In addition, the use of a polar poly(ethylene glycol) separation column alleviated the adsorption of minor specific pyrolysis products. This modified RTD-GC method allowed the determination of the polymeric HALS (Mr 1900) in PP even for trace concentrations between 100 and 500 ppm, through observing selectively the characteristic products containing a tetramethylpiperidine moiety, which had been impossible to detect under the previous RTD-GC conditions using a non-polar separation column and conventional flame ionization detection.

Amines↗

PubMed1994

Comparison of derivatization procedures for the determination of diuretics in urine by gas chromatography-mass spectrometry.

Three different GC-MS screening procedures, which use different ways of derivatization (methylation), are compared. In the first one, derivatization with iodomethane in acetone and a previous solid-liquid extraction is used; the second one is based on an extractive alkylation method using iodomethane in toluene (liquid-liquid extraction); and the last one is flash methylation by pyrolysis of tetraalkylammonium salts in the injector of the gas chromatograph using trimethylanilinium as the derivatization agent. The speed of the extraction, reproducibility and accuracy have been compared for 20 diuretics including the ones most often used in sports, such as bumetanide, ethacrynic acid, acetazolamide, dichlorphenamide, furosemide, hydroflumethiazide, hydrochlorothiazide and chlorthalidone; they have also been applied to the two uricosuric agents probenecid and benzbromarone.

Diuretics↗

PubMed2003

Structural characteristics of modified activated carbons and adsorption of explosives.

Several series of activated carbons prepared by catalytic and noncatalytic gasification and subsequent deposition of pyrocarbon by pyrolysis of methylene chloride or n-amyl alcohol were studied by FTIR, chromatography, and adsorption methods using nitrogen and probe organics (explosives). The relationships between the textural characteristics of carbon samples and the recovery rates (eta) of explosives on solid-phase extraction (SPE) using different solvents for their elution after adsorption were analyzed using experimental and quantum chemical calculation results. The eta values for nitrate esters, cyclic nitroamines, and nitroaromatics only partially correlate with different adsorbent parameters (characterizing microporosity, mesoporosity, pore size distributions, etc.), polarity of eluting solvents, or characteristics of probe molecules, since there are many factors strongly affecting the recovery rates. Some of the synthesized carbons provide higher eta values than those for such commercial adsorbents as Hypercarb and Envicarb.

Journal Article↗

PubMed1980

A quantitative study of acetylcholine in Hirschsprung's disease.

This is the first report on acetylcholine (Ach) quanititaion of the aganglionic colon by a chemical assay. Ach content in the colon of Hirschsprung's disease was measured by pyrolysis gas chromatography, which was found to be a simple, accurate, and reliable method. Microwave irradiation on the surgical resected specimens was performed before extraction procedure to abolish acetylcholinesterase (Ach-E) and cholineacetyltransferase (CAT) activity in the tissue. Ach content in the ganglionic colon was 8.51 +/- 3.15 nmole/g (n 5 in contrast to 23.79 +/- 14.17 nmole/g (n = 19) in the aganglionic segment of Hirschsprung's disease. The meaning of elevated Ach level in the aganglionic segment was discussed from the pathophysiologic standpoint.

Acetylcholine↗

PubMed2002

Well-done red meat, metabolic phenotypes and colorectal cancer in Hawaii.

Heterocyclic amines (HAAs) and polycyclic hydrocarbons are suspected colorectal cancer (CRC) carcinogens that are found in well-done meat. They require metabolic activation by phase I enzymes, such as the smoking-inducible CYP1A isoenzymes. N-acetyltransferase 2 (NAT2) also play a role in the further activation of HAAs. We conducted a population-based case-control study in Hawaii to test the associations of preference for well-done red meat and HAA intake with colon and rectal cancers, as well as the modifying effects of NAT2 and CYP1A2. We interviewed 727 Japanese, Caucasian or Native Hawaiian cases and 727 controls matched on sex, age, and ethnicity. HAA intake was estimated based on consumption of meat and fish for each of several cooking methods and doneness levels. A subgroup of 349 cases and 467 controls was phenotyped for CYP1A2 by a caffeine test. We found that preference for well-done red meat was associated with a 8.8-fold increased risk of CRC (95% CI: 1.7-44.9) among ever-smokers with the NAT2 and CYP1A2 rapid phenotypes, compared to ever-smokers with low NAT2 and CYP1A2 activities and who preferred their red meat rare or medium. A dose-dependent association was also found between the HAA intake estimates and male rectal cancer, with a two- to three-fold increase in risk from the low (T(1)) to high (T(3)) tertile of intake for each HAA. This association was strongest for MeIQx. HAA intake was not associated with male colon cancer or colon or rectal cancer in women. These data provide support to the hypothesis that exposure to pyrolysis products through consumption of well-done meat increases the risk of CRC, particularly in individuals who smoke and are genetically susceptible (as determined by a rapid phenotype for both NAT2 and CYP1A2). An attempt to examine the risk associated with specific HAAs suggested that the main HAAs increase risk of rectal cancer in men and that they do not appreciably affect risk of rectal cancer in women or of colon cancer in either sex.

Adolescent↗

PubMed1997

Health risks of heterocyclic amines.

Common cooking procedures such as broiling, frying, barbecuing (flame-grilling), heat processing and pyrolysis of protein-rich foods induce the formation of potent mutagenic and carcinogenic heterocyclic amines. These same compounds produce tumors at multiple organ sites in both mice and rats. One example of these induced tumors has also been seen in nonhuman primates. Risk assessment for the human population consuming these compounds requires the integration of knowledge of dosimetry, metabolism, carcinogenic potency, and epidemiology. When this integration is done in even a preliminary way as is done here, the range of risk for an individual from these compounds is enormous. Exposure contributes a range of 200-fold or more and metabolism and DNA repair differences among individuals could easily be an additional 10-fold between individuals. This indicates that differences in human cancer risk for heterocyclic amines could range more than a thousandfold between individuals based on exposure and genetic susceptibility.

Amines↗

PubMed1997

Chemoprotection against the formation of colon DNA adducts from the food-borne carcinogen 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) in the rat.

The mutagenic heterocyclic aromatic amine, 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP), is a pyrolysis product in cooked foods that has been shown to be a rat colon carcinogen and has been implicated in the etiology of human colon cancer. In order to identify chemoprotection strategies that could be carried out in humans, a pilot study was conducted in which PhIP-DNA-adduct levels were quantified in the colons of male F344 rats that had been subjected to 16 different putative chemoprotection regimens, followed by a gavage of PhIP (50 mg/kg) and sacrifice 24 h later. The 16 treatments (Oltipraz, benzylisothiocyanate, diallyl sulfide, garlic powder, ethoxyquin, butylated hydroxyanisole, glutathione, indole-3-carbinol, alpha-angelicalactone, kahweol/cafestol palmitates, quercetin, green tea, black tea, tannic acid, amylase-resistant starch, and physical exercise) comprised sulfur-containing compounds, antioxidants, flavonoids, diterpenes, polyphenols, high dietary fiber, etc. The strongest inhibition of PhIP-DNA adduct formation in the colon was observed upon pretreatment with black tea, benzylisothiocyanate, and a mixture (1:1) of kahweol:cafestol palmitates, which resulted in 67, 66, and 54% decreases in colon PhIP-DNA adduct levels, as compared with controls. Preliminary studies on their mechanism of action indicated that only kahweol:cafestol caused a substantial induction of glutathione S-transferase isozymes (GSTs) that are thought to be important in the detoxification of PhIP. Notably, this induction occurred in the liver rather than in the colon.

Animals↗

PubMed2001

High molecular weight lipids from the trilaminar outer wall (TLS)-containing microalgae Chlorella emersonii, Scenedesmus conmmunis and Tetraedron minimum.

High molecular weight lipids were isolated from Chlorella emersonii, Scenedesmus communis and Tetraedron minimum, thin trilaminar outer wall (TLS)-containing freshwater microalgae producing an insoluble non-hydrolysable biopolymer (i.e. algaenan). Molecular weight determination by gel permeation chromatography indicated that their molecular weights range from ca. 400 to 2000 Da. Flash pyrolysis with in situ methylation using tetramethylammonium hydroxide (TMAH) and alkaline hydrolysis showed that the high molecular weight lipids isolated from C. emersonii and S. communis are mainly composed of saturated n-C26 and n-C28 fatty acids and alcohols and of saturated n-C30 and n-C32 alpha,omega-diols and omega-hydroxy acids. In contrast the high molecular weight lipids isolated from T. minimum are predominantly composed of long-chain fatty acids and omega-hydroxy acids. Aromatic moieties were also identified in small amounts in the thermochemolysate and in the hydrolysate. Chemical structural models containing long-chain mono- and polyesters were proposed for the high molecular weight lipids isolated from the three microalgae in agreement with analytical and spectroscopic data. Structural similarity between the outer cell wall of these microalgae and the cuticular membrane of higher plants is suggested.

Cell Wall↗

PubMedDate not supplied

Stable isotope laser spectrometer for exploration of Mars.

On Earth, measurements of the ratios of stable carbon isotopes have provided much information about geological and biological processes. For example, fractionation of carbon occurs in biotic processes and the retention of a distinctive 2-4% contrast in 13C/12C between organic carbon and carbonates in rocks as old as 3.8 billion years constitutes some of the firmest evidence for the antiquity of life on the Earth. We have developed a prototype tunable diode Laser spectrometer which demonstrates the feasibility of making accurate in situ isotopic ratio measurements on Mars. This miniaturized instrument, with an optical path length of 10 cm, should be capable of making accurate 13C/12C and 15N/14N measurements. Gas samples for measurement are to be produced by pyrolysis using soil samples as small as 50 mg. Measurements of 13C/12C, 18O/16O and 15N/14N have been made to a precision of better than 0.1% and various other isotopes are feasible. This laser technique, which relies on the extremely narrow emission linewidth of tunable diode lasers (<0.001 cm(-1)) has favorable features in comparison to mass spectrometry, the standard method of accurate isotopic ratio measurement. The miniature instrument could be ready to deploy on the 2003 or other Mars lander missions.

Carbon Dioxide↗

PubMed2002

Evaluation of 1-octanol degradation by photocatalysis and ultrasound using SPME.

Solid-phase micro-extraction has been used for identifying, quantifying and following the evolution of intermediate products of octanol degradation by two advanced oxidation treatments (AOTs), photocatalytic and ultrasound processes, inducing mainly the same active species. Headspace extraction enabled direct extraction of the organic compounds in a heterogeneous process like photocatalysis. The presence of a solid does not affect the extraction percentage of alkanes, alkenes and aldehydes while alcohols and carboxylic acids are not completely extracted if the extraction time is too short. To extract C3-C8 alkanes, alkenes and aldehydes a Carboxen/PDMS fiber and an extraction time of 25 min are used. The presence of alcohol and carboxylic acids requires the use of the presence of salt under acidic conditions, a longer extraction time and a polyacrylate fiber (PA), having a polar fiber. The in situ derivatization--pyrenyldiazomethane on a PA fiber--increases the carboxylic acid extraction containing smaller hydrocarboned chain while diazomethane derivatization is not as efficient due to its volatility. Whatever be the treatment, photocatalysis or ultrasound processes, aldehydes are the main intermediate products, which is not surprising since the same oxidation species (HO2(o), O2(o-), OH(o)) are formed. Alkanes and alkenes are also detected in both processes; however, alkane formation is more important in photocatalysis while alkenes are formed in higher amounts by ultrasound. Moreover, the presence of carboxylic acids in more important amounts by ultrasound than by photocatalysis is attributed to the presence of holes (h+) in photocatalysis which induces photo-Kolbe degradation. The sonochemical formation of small-chained dienes and alkynes is probably due to pyrolysis of hydrophobic compounds in cavitation bubbles.

1-Octanol↗

PubMed2003

Heterogeneity of natural organic matter from the Chena River, Alaska.

Water samples were collected in July 2001 from the Chena River in central Alaska. The natural organic matter (NOM) was size fractionated into particulate (POM,>0.45 microm), colloidal (COM,1kDa-0.45 microm) and dissolved (DOM,<1k Da) organic matter fractions, using filtration and ultrafiltration. The size-fractionated organic matter was then analyzed for organic carbon (OC) and nitrogen (N), isotopic (delta13C and delta15N) and molecular composition, using continuous flow isotope ratio mass spectrometry and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). Results of phase partitioning showed that, on average, about 6% of OC and 16% of N occurred in the form of POM while 66% of OC and 57% of N occurred in the form of COM, and 28% of the OC and 27% of the N were in the DOM form. Organic matter in the river water was found to be highly heterogeneous in terms of chemical composition and isotopic signatures. The C/N ratio was as low as 16+/-1 in the POM (n=2) to as high as 48+/-1 in the COM (n=3) and 38+/-4 in the DOM (n=3), suggesting a diagenetically younger POM. Values of delta13C increased with decreasing size, varying from -29.59+/-0.45% in the POM to -27.47+/-0.06% in the COM to -16.93+/-0.08% in the DOM. In contrast, values of delta15N decreased with decreasing size, from 2.64% in POM to 1.64% in COM to 1.33% in DOM. These results, together with radiocarbon measurements, suggest a preferential decomposition of lighter C isotope (12C) and heavier N isotopic (15N) from POM to COM to DOM. Results of py-GC/MS showed that the percentage of polysaccharides decreased with decreasing size, further supporting a degradation pathway of NOM from POM to COM and DOM in Chena River waters. More studies are needed to examine the seasonal and spatial variations of size-fractionated organic matter.

Alaska↗

PubMed2003

Molecular characterization of dissolved organic matter in freshwater wetlands of the Florida Everglades.

In this study, the molecular composition of dissolved organic matter (DOM), collected from wetlands of the Southern Everglades, was examined using a variety of analytical techniques in order to characterize its sources and transformation in the environment. The methods applied for the characterization of DOM included fluorescence spectroscopy, solid state 13C CPMAS NMR spectroscopy, and pyrolysis-GC/MS. The relative abundance of protein-like components and carbohydrates increased from the canal site to more remote freshwater marsh sites suggesting that significant amounts of non-humic DOM are autochthonously produced within the freshwater marshes, and are not exclusively introduced through canal inputs. Such in situ DOM production is important when considering how DOM from canals is processed and transported to downstream estuaries of Florida Bay.

Ecosystem↗

PubMedDate not supplied

A flexible and stable numerical method for simulating the thermal decomposition of wood particles.

The objective of this paper is to present a flexible and stable simulation method to predict the thermal conversion of wood particles. A combination of several subprocesses such as heating-up, drying, pyrolysis, gasification and combustion of fuel particles of different properties and sizes represents the global process of thermal conversion. This approach allows for simultaneous processes e.g. reactions in time and covers the entire range between transport-limited (shrinking core) and kinetically limited (reacting core) reaction regimes. Thus, the model is applicable to simulate sufficiently accurate the thermal decomposition of each particle in a packed bed, of which the entire conversion is regarded as the sum of all particle processes. Effects such as fragmentation, swelling, homogeneous reactions e.g. ignition outside a particle are excluded as a tradeoff between complexity and calculation time. However, a description of the particle processes by one-dimensional and transient differential conservation equations for mass and energy is feasible to represent the above mentioned subprocesses. The particles are coupled to the gas phase by heat and mass transfer taking into account the Stefan correction due to the gas outflow during conversion. A general formulation of the conservation equations allows the geometry of a fuel particle to be treated as a plate, cylinder or sphere. In order to achieve a high degree of flexibility, the method distinguishes between data, such as kinetics or material properties and the conversion process, for which relevant data are stored in a data base for easy access and extension. The resulting modules of this subdivision are encapsulated into separate software units cast in a hierarchy of well-defined classes in Tools of Object-oriented Software for Continuum-Mechanics Applications (TOSCA) by object-oriented techniques.

Journal Article↗

PubMedDate not supplied

Research and development to improve naval shipboard waste management using a compact closed-loop-controlled waste incinerator.

Research has been conducted into the application of forced acoustics for enhancing the performance of a pyrolyzed waste afterburner configured as a dump combustor. Subscale studies showed that acoustic forcing of an air jet entering a dump chamber could trigger the formation of coherent vortices generated by entrainment of ambient gases. Subsequent studies showed that combustible gases could be introduced into the coherent vortices, and with additional modulation this configuration would lead to an enhanced combustion rate with low emissions of pollutants. The acoustically forced burner concept was scaled up to practical levels and tested as an afterburner on a commercial waste incinerator operating in pyrolysis mode. Results show that the afterburner can promote both compactness, due to the rapid combustion rate, and low pollutant emissions resulting from enhanced mixing prior to combustion.

Journal Article↗

PubMedDate not supplied

Laboratory study on the high-temperature capture of HCl gas by dry-injection of calcium-based sorbents.

This is a laboratory study on the reduction of combustion-generated hydrochloric acid (HCl) emissions by in-furnace dry-injection of calcium-based sorbents. HCl is a hazardous gaseous pollutant emitted in significant quantities by municipal and hazardous waste incinerators, coal-fired power plants, and other industrial furnaces. Experiments were conducted in a laboratory furnace at gas temperatures of 600-1000 degrees C. HCl gas diluted with N2, and sorbent powders fluidized in a stream of air were introduced into the furnace concurrently. Chlorination of the sorbents occurred in the hot zone of the furnace at gas residence times approximately 1 s. The sorbents chosen for these experiments were calcium formate (CF), calcium magnesium acetate (CMA), calcium propionate (CP), calcium oxide (CX), and calcium carbonate (CC). Upon release of organic volatiles, sorbents calcine to CaO at approximately 700 degrees C, and react with the HCl according to the reaction CaO + 2HCl <=> CaCl2 + H2O. At the lowest temperature case examined herein, 600 degrees C, direct reaction of HCl with CaCO3 may also be expected. The effectiveness of the sorbents to capture HCl was interpreted using the "pore tree" mathematical model for heterogeneous diffusion reactions. Results show that the thin-walled, highly porous cenospheres formed from the pyrolysis and calcination of CF, CMA, and CP exhibited high relative calcium utilization at the upper temperatures of this study. Relative utilizations under these conditions reached 80%. The less costly low-porosity sorbents, calcium carbonate and calcium oxide also performed well. Calcium carbonate reached a relative utilization of 54% in the mid-temperature range, while the calcium oxide reached an 80% relative utilization at the lowest temperature examined. The data matched theoretical predictions of sorbent utilization using the mathematical model, with activation energy and pre-exponential factors for the calcination reaction of 17,000 K and 300,000 (g gas/cm2/s/atm gas), respectively. Thus, the kinetics of the calcination reaction were found to be much faster (approximately 500 times) than those of the sulfation reaction examined previously in this laboratory.

Journal Article↗

PubMed2001

Formation and inhibition of chloroaromatic micropollutants formed in incineration processes.

The formation pathways for chlorinated aliphatic and chlorinated aromatic compounds in technical incineration processes are reviewed. It is shown that acetylene is converted to chloroaromatic compounds including PCDD/F in a special flow reactor by catalytic activity of CuCl2 in the temperature regime of a post-combustion zone of technical incinerators. Mechanistic pathways begin with chlorination of acetylene. Dichloroacetylene is further condensed to C-4 and C-6 units. Hexachlorobenzene is the dominant aromatic compound and a likely precursor to chlorinated phenols and PCDD/F. Two specific mechanisms of formation of chlorinated aromatic compounds including PCDD/F have been advanced. Both mechanisms begin with the formation of dichloroacetylene from flame pyrolysis products like acetylene. Condensation of dichloroacetylene is mediated by copper species via metallacyclic intermediates and/or a catalytic cycle involving copper stabilized trichlorovinyl radicals. The final pathways of conversion of chlorinated benzenes to PCDD/F via chlorophenols are under active investigation.

Acetylene↗

PubMed2001

Characterization of organic matter in pristine and contaminated coastal marine sediments using solid-state 13C NMR, pyrolytic and thermochemolytic methods: a case study in the San Diego harbor area.

Chemical composition of coastal marine sedimentary organic matter (SDOM) is a function of natural and anthropogenic inputs to the system. In this study a combination of analytical techniques: 13C nuclear magnetic resonance (NMR), pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and tetramethylammonium hydroxide thermochemolysis-gas chromatography/mass spectrometry (TMAH thermochemolysis-GC/MS) were used to study the contribution of hydrophobic organic contaminants and terrestrial OM to the SDOM. Sediments were collected from two sites in the San Diego Bay: Paleta Creek, which is contaminated, and Coronado Cayes, which is relatively pristine. Concentrations of polycyclic aromatic hydrocarbons (PAHs) at both sites, as determined by ultrasonically assisted lipid extraction are found to be higher in the surface layer, to generally decrease with depth, and to be present at about two orders of magnitude higher concentration at the contaminated site as compared to the pristine site. The sediment samples were partially deashed with HF/HCI treatment before further analysis. 13C-NMR spectra of the Paleta Creek samples show a higher aromatic carbon content and a distinct phenolic carbon peak. This suggests a large input from terrestrial carbon (lignin). Data from both Py-GC/MS and TMAH thermochemolysis-GC/MS support this and indicate the presence of lignin-derived residues, primarily of the guaiacyl type at the contaminated site. In contrast, SDOM at the Coronado Cayes site exhibits less terrestrial input. In general, the SDOM resembles soil OM rather than typical marine SDOM. Chemical analyses of the lipid-extracted, partially deashed sediments, does not reveal the presence of any PAHs.

California↗

PubMed2002

Amorphous and condensed organic matter domains: the effect of persulfate oxidation on the composition of soil/sediment organic matter.

The composition of amorphous and condensed soil/sediment organic matter (SOM) domains was investigated for one soil sample and four sediment samples. These samples were oxidized with persulfate to remove amorphous SOM, before and after which the composition of SOM was studied by thermogravimetric analysis, pyrolysis-GC/MS, and cross polarization magic angle spinning 13C-NMR. Comparison of the SOM composition before and after oxidation showed that condensed SOM was more thermostable and less polar than amorphous SOM. Condensed SOM was relatively low in O-alkyl C and carboxyl C and it was likely to contain only small amounts of labile organic components (carbohydrates, peptides, fatty acids). Apart from these general characteristics, the composition of the condensed and amorphous domains appeared to be highly dependent on the origin and nature of the SOM investigated. Condensed domains in relatively undecomposed SOM were enriched in aliphatic C, whereas condensed domains in relatively weathered SOM were enriched in aromatic C. Altogether, the compositional changes upon persulfate oxidation were similar to the compositional changes upon humification, which supports the idea that weathered SOM is more condensed than the original material.

Carbon Isotopes↗