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PubMed2005

Assessing the quantitative reliability of solid-state 13C NMR spectra of kerogens across a gradient of thermal maturity.

Five type II kerogens, shown by elemental analysis and Rock-Eval pyrolysis to represent a gradient of thermal maturity, were further characterized using a range of solid-state 13C NMR spectroscopic techniques. 13C cross polarization (CP) NMR spectra of the kerogens confirmed the well-established pattern of increasing aromaticity with increasing thermal maturity. Spin counting showed that CP observability was around 50% for the immature kerogens, and only 14-25% for the mature kerogens. Spin counting also showed that the direct polarization (DP) observabilities were >80% for all but one of the kerogens. Despite the large differences in observability between the two techniques, aromaticities derived from corresponding CP and DP spectra differed by only 1-15%. The RESTORE technique showed that the low CP observability of the immature kerogens was due mostly to rapid T(1rho)H relaxation, whereas both rapid T(1rho)H relaxation and slow polarization transfer contributed to the low CP observability of the mature kerogens.

Carbon Isotopes↗

PubMed2004

Aquasonolysis of thiophene and its derivatives.

The rate constants and products of the aquasonolysis of thiophene, tetrahydrothiophene, 2-methylthiophene, 2,5-dimethylthiophene, and 2-ethylthiophene have been investigated. The sonolysis of the selected compounds in aqueous solution follows pseudo-first-order kinetics. The aquasonolytical rate constants correlate very well with the water solubility and Henry's Law constants of thiophenes. Surprisingly, vapour pressures and heats of formation of thiophenes have little effect on their aquasonolytical rates. The pseudo-first-order rate constant for the decay of thiophene decreases as its initial concentration increases. These results indicate that the transfer process of organic solutes between cavitation bubbles and the bulk liquid can strongly affect the aquasonolysis. Furthermore, carbon disulfide, diacetylene, and dimers can be detected as common products during ultrasonic irradiations. Hence, the predominant pathway of the aquasonolysis of thiophenes is the pyrolysis during the collapse of cavities.

Sonication↗

PubMed2004

Activation of waste MDF sawdust charcoal and its reactive dye adsorption characteristics.

This paper reports an experimental investigation of converting waste medium density fibreboard (MDF) sawdust into chars and activated carbon using chemical activation and thermal carbonisation processes. The MDF sawdust generated during the production of architectural mouldings was characterised and found to have unique properties in terms of fine particle size and high particle density. It also has a high content of urea formaldehyde resin used as a binder in the manufacturing of MDF board. Direct thermal carbonisation and chemical activation of the sawdust by metal impregnation and acid (phosphoric acid) treatment prior to pyrolysis treatment were carried out. The surface morphology of the raw dust, its chars and activated carbon were examined using scanning electron microscopy (SEM). Adsorptive properties and total pore volume of the materials were also analysed using the BET nitrogen adsorption method. Liquid adsorption of a reactive dye (Levafix Brilliant red E-4BA) by the derived sawdust carbon was investigated in batch isothermal adsorption process and the results compared to adsorption on to a commercial activated carbon (Filtrasorb F400). The MDF sawdust carbon exhibited in general a very low adsorption capacity towards the reactive dye, and physical characterisation of the carbon revealed that the conventional chemical activation and thermal carbonisation process were ineffective in developing a microporous structure in the dust particles. The small size of the powdery dust, the high particle density, and the presence of the urea formaldehyde resin all contributed to the difficulty of developing a proper porous structure during the thermal and chemical activation process. Finally, activation of the dust material in a consolidated form (cylindrical pellet) only achieved very limited improvement in the dye adsorption capacity. This original study, reporting some unexpected outcomes, may serve as a stepping-stone for future investigations of recycle and reuse of the waste MDF sawdust which is becoming an increasing environmental and cost liability.

Adsorption↗

PubMed2005

Changes in organic matter composition during composting of two digested sewage sludges.

Changes in the chemical and chemical-structural composition of the organic matter of two different sewage sludges (aerobic and anaerobic) mixed with sawdust (1:1 and 1:3, v/v) during composting were determined by monitoring chemical and microbiological parameters as well as by pyrolysis-gas chromatography. Composting was carried out in periodically turned outdoor piles, which were sampled for analysis 1, 30, 60 and 90 days after the beginning of the composting process. Both volatile organic matter and the water soluble C fraction decreased during composting, indicating that the more labile C fractions are mineralized during the process. Microbial activity as measured by microbial respiration (CO(2) evolved from compost samples during incubation) also decreased with composting, reflecting the more stable character of the resulting compost. No major differences were observed between the four composts studied as regards their chemical-structural characteristics. The acetonitrile, acetic acid and phenol pyrolytic fragment tended to increase with composting. Although the final composts were more aromatic in nature than the starting materials, a low degree of humification was observed in all four composts studied, as determined by their high proportion of polysaccharides and alkyl compounds. For this reason, the relationship between pyrolytic fragments, such as benzene/toluene or benzene+toluene/pyrrol+phenols, which are used as indices of humification for soil organic matter, are not of use for such poorly evolved sludge composts; instead, ratios that involve carbohydrate derivatives and aromatic compounds, such as furfural+acetic/benzene+toluene or acetic/toluene, are more sensitive indices for reflecting the transformations of these materials during composting. Both the chemical and microbiological parameters and pyrolytic analysis provided valuable information concerning the nature of the compost's organic matter and its changes during the composting process.

Aerobiosis↗

PubMed2006

Pilot installation for the thermo-chemical characterisation of solid wastes.

The increasing production and the large variety of wastes require operators of thermal treatment units to continuously adapt the installations or the functioning parameters to the different physical and chemical properties of the wastes. Usually, the treated waste is encountered in the form of heterogeneous mixtures. The classical tests such as thermogravimetry and calorimetric bomb operate component by component, separately. In addition to this, they can analyse only small quantities of waste at a time (a few grams). These common tests are necessary but insufficient in the global waste analysis in the view further thermal treatment. This paper presents an experimental installation, which was designed and built at the CNRS Science Division, Department of Industrial Methods, Compiègne University of Technology, France. It allows the determination of waste thermal and chemical properties by means of thermal treatment. Also, it is capable of continuously analysing significant quantities of waste (up to 50kg/h) as compared to the classical tests and it can work under various conditions: The installation reproduces the process conditions from incinerators or pyrolysis reactors. It also provides complete information on the kinetics of the waste thermal degradation and on the pollutant emissions. Using different mixtures of components present in the municipal solid waste and also in the reconstituted MSW samples, we defined a series of criteria for characterising waste behaviour during the stages of the main treatment process such as: feeding, devolatilisation/oxidation, advancement, solid residue evacuation, and pollutants emission.

Oxidation-Reduction↗

PubMed2006

Characterization of char derived from various types of solid wastes from the standpoint of fuel recovery and pretreatment before landfilling.

Carbonization is a kind of pyrolysis process to produce char from organic materials under an inert atmosphere. In this work, chars derived from various solid wastes were characterized from the standpoint of fuel recovery and pretreatment of waste before landfilling. Sixteen kinds of municipal and industrial solid wastes such as residential combustible wastes, non-combustible wastes, bulky wastes, construction and demolition wastes, auto shredder residue, and sludges were carbonized at 500 degrees C for 1h under nitrogen atmosphere. In order to evaluate the quality of char as fuel, proximate analysis and heating value were examined. The composition of raw waste had a significant influence on the quality of produced char. The higher the ratio of woody biomass in waste, the higher heating value of char produced. Moreover, an equation to estimate heating value of char was developed by using the weight fraction of fixed carbon and volatile matter in char. De-ashing and chlorine removal were performed to improve the quality of char. The pulverization and sieving method seems to be effective for separation of incombustibles such as metal rather than ash. Most char met a 0.5 wt% chlorine criterion for utilization as fuel in a shaft blast furnace after it was subjected to repeated water-washing. Carbonization could remove a considerable amount of organic matter from raw waste. In addition, the leaching of heavy metals such as chrome, cadmium, and lead appears to be significantly suppressed by carbonization regardless of the type of raw waste. From these results, carbonization could be considered as a pretreatment method for waste before landfilling, as well as for fuel recovery.

Carbon↗

PubMed2004

Removal of water pollutants with activated carbons prepared from H3PO4 activation of lignin from kraft black liquors.

Activated carbons with a high BET surface area and a well-developed porosity have been prepared from pyrolysis of H3PO4-impregnated lignin precipitated from kraft black liquors. Impregnation ratios within the range of 1-3 and activation temperatures of 623-873 K have been used, giving rise to carbons with different porous and surface chemical structure. Increasing the activation temperature and the impregnation ratio leads to a widening of the porous structure with a higher relative contribution of mesoporosity. The potential application of these carbons for the removal of water pollutants has been investigated by measuring their adsorption capacities for phenol, 2,4,5-trichlorophenol and Cr (VI) as representative of toxic contaminants found in industrial wastewaters. The results obtained compare well and even favorably with those reported in the literature for other activated carbons. An impregnation ratio and an activation temperature around 2 g H3PO4/g lignin and 700 K, respectively, are recommended as the best combination of operating conditions to prepare activated carbons for aqueous phase applications although at lower values of these two variables carbons with good adsorption capacities are also obtained.

Adsorption↗

PubMed2006

Improvement of thermal reactivation of activated carbon for the removal of 2-methylisoborneol.

Rapid small-scale column tests (RSSCTs) were employed to evaluate the impact of the dissolved oxygen (DO) concentration in the water used to create steam on the reactivation of spent granular activated carbon (GAC) using three novel thermal reactivation procedures: steam-curing, steam-curing with ramped temperature, and steam pyrolysis reactivation. Evaluation of the physical properties of the reactivated carbon showed a change in mass and volume loss with a change in DO. Performance testing of the carbons for removal of the taste- and odor-causing compound 2-methylisoborneol (MIB) showed that MIB uptake generally increased as the DO concentration decreased. Decrease in MIB removal with an increase in surface acidity, a phenomenon found in the literature, may be responsible for the changes in adsorption performance, as the higher DO concentrations yielded carbons with higher total surface acidity. In addition, the steam-curing process, which was implemented at 375 degrees C (i.e. about 400 degrees C lower than typical reactivation temperatures) with a low DO concentration (i.e. 3-4mg/L) had comparable performance to the virgin carbon counterpart, which could manifest cost-savings due to the low temperature associated with this protocol compared to conventional reactivation. Furthermore, since the mass loss associated with this steam-curing protocol was low, less virgin carbon make-up would be required also improving the economic viability of this reactivation protocol.

Adsorption↗

PubMed1988

Reduction of enzyme activity of tyrosine hydroxylase and aromatic L-aminoacid decarboxylase in clonal pheochromocytoma PC12h cells by carcinogenic heterocyclic amines.

Out of carcinogenic heterocyclic amines, which are produced by pyrolysis of tryptophan in food, 3-amino-1,4-dimethyl-5H-pyrido[4,3-b]indole (Trp-P-1) and 3-amino-1-methyl-5H-pyrido[4,3-b]indole (Trp-P-2) were found to reduce the activity of enzymes related to catecholamine metabolism in clonal rat pheochromocytoma PC12h cells. By 6 days' culture in the presence of 10 nM to 10 microM Typ-P-1 and -2, these heterocyclic amines were accumulated in the cells, and activity of tyrosine hydroxylase (TH) and aromatic L-aminoacid decarboxylase (AADC) were reduced markedly. Reduction of these enzyme activity was observed with Trp-P-1 and -2 at the concentrations lower than 1 microM, while cell protein and enzyme activity of a non-specific enzyme, beta-galactosidase were reduced only with 10 microM Trp-P-1. These results show that these heterocyclic amines are neurotoxins specific for dopaminergic neurons.

Animals↗

PubMed1988

Oxidation of the 2-hydroxyamino derivative of 2-amino-6-methyl-dipyrido[1,2-a: 3',2'-d] imidazole (Glu-P-1) to its 2-nitroso form, an ultimate form reacting with hemoglobin thiol groups.

The binding to hemoglobin of synthetic 2-hydroxyamino-6-methyldipyrido[1,2-a: 3',2'-d] imidazole from the carcinogenic product of L-glutamic acid pyrolysis 2-amino-6-methyldipyrido[1,2-a: 3',2'-d] imidazole were investigated in vitro. The hydroxylamine required oxidation to its nitroso derivative to bind to rat hemoglobin through thiol groups. Oxidation of the hydroxylamine to the nitroso form was found to be enhanced by oxyhemoglobin and superoxide dismutase at pH 7.4 under aerobic conditions. Since these conditions might also enhance this oxidation in vivo, the conversion of the DNA-reactive arylhydroxylamines to the DNA-non-reactive nitroso compounds and their subsequent binding to highly abundant thiol groups of proteins could be considered as a process for detoxification of toxic arylhydroxylamines.

Animals↗

PubMedDate not supplied

Early cellular effects of Trp-P-1 on adult rat hepatocytes in primary culture.

Trp-P-1, a DL-tryptophan pyrolysis product, was previously known for its mutagenic and hepato-carcinogenic properties and for inducing nucleolar damage in adult rat hepatocytes in primary culture. In this paper, the effect of Trp-P-1 was investigated on DNA, RNA and protein synthesis in hepatocytes treated with 1, 5 and 10 micrograms/ml for 1, 2 and 4 h in order to determine the cascade of events which could occur in cells exposed to this agent. The inhibition of the 3 biosynthetic pathways was linearly dependent on the concentration of Trp-P-1 in the culture medium for each duration of treatment. For a given concentration, the degree of inhibition depended on the duration of incubation and varied according to the type of synthesis. DNA synthesis appeared as the most rapidly and strongly impaired: 16% of control values in hepatocytes treated with 10 micrograms/ml Trp-P-1 for 1 hour against 50.7% for RNA and 66.7% for protein synthesis. These data indicated that DNA should be the primary target of Trp-P-1 action in good agreement with the genotoxic activity of this agent. The complete recovery of RNA synthetic capability within 2 h after the removal of Trp-P-1 from the medium could however indicate that transcription was not definitely altered. By contrast the lack of protein synthesis recovery in a Trp-P-1 free medium for 24 h might signify the extended impairment of a step of translational process at the cytoplasmic level.

Animals↗

PubMed2000

Determination of basic nitrogen-containing polynuclear aromatic hydrocarbons formed during thermal degradation of polymers by high-performance liquid chromatography-fluorescence detection.

A method for the simultaneous determination of 22 nitrogen-containing polynuclear aromatic hydrocarbons (PAHs) (15 azaarenes and seven amino-PAHs) in the gaseous products of the thermal degradation of polymers is described. After desorption and clean-up using cation-exchange chromatography (PRS cartridge) the samples were analyzed by HPLC-FD. The validation was carried out with real nylon 6 combustion samples. The recoveries of the compounds are in the range of 89-99% for the extraction and 91-100% for the clean up procedure. The detection limits ranged from 7 to 160 pg. The high recovery values, due to the quick and efficient clean-up procedure, resulted in low relative standard deviations (with the exception of acridine and 2-aminoanthracene <5%). The applicability of the method is also investigated for the determination of the N-PAHs in a pyrolysis sample.

Chromatography, High Pressure Liquid↗

PubMed1976

Selective detection of N-nitrosamines by gas chromatography using a modified microelectrolytic conductivity detector in the pyrolytic mode.

The pyrolysis of nitrosamines in a modified Hall microelectrolytic conductivity system provides the basis for a highly selective and sensitive determination method. Under the conditions specified, the response of this detector system to nitrosamines is at least 10(7) times greater than that for n-hexane. The influence of several operational parameters on the response of the detector to nitrosamines was studied. For open-chain nitrosamines, the detection limit is 50 pg and the response is linear up to at least 200 ng.

Chromatography, Gas↗

PubMed1986

Ion chromatographic method for the analysis of sulfate in complex carbohydrates.

A procedure is described for the quantitation of sulfate in complex carbohydrates. Samples are taken to dryness in the presence of a small amount of sodium hydroxide and the sulfate is liberated by pyrolysis. Sulfate is then quantitated by single-column ion chromatography eliminating the interference by ions such as phosphate, chloride, sodium and calcium which frequently occurs with colorimetric methods. The reproducibility of the method is approximately 10%. This approach cannot be directly applied to glycoproteins because a portion of the sulfur in sulfur-containing amino acids appears to be converted to sulfate. However, this method can be used to measure sulfate in oligosaccharides of glycoproteins if the protein components are removed prior to analysis.

Amino Acids, Sulfur↗

PubMed1984

Analysis of phospholipids in cow's milk by high-temperature injection gas chromatography and high-performance liquid chromatography.

An investigation of the high-temperature injection (350 degrees C) gas chromatographic behaviour of standards of various classes of phospholipids has elucidated certain characteristic fragments ("tracers") in the pyrogram of each class. Under these conditions of pyrolysis of the phospholipids, a natural mixture of such substances (extracted and purified from cows' milk) has provided evidence for the same "tracers" as for the standards. Analogous results were obtained with a more representative specimen of cows' milk of various breeds grown in areas of different altitudes. The content of fatty acids in phospholipids, tested on each class (separated by means of radial compression high-performance liquid chromatography from polar lipids of milk) appeared to be relatively similar for all the phospholipid classes, and over half the content consisted of unsaturated fatty acids. The major component was delta 9-octadecenoid (oleic) acid.

Animals↗

PubMed1987

Analysis of fatty acid methyl esters with high accuracy and reliability. VI. Rapid analysis by split injection capillary gas-liquid chromatography.

Of the several facets of technique that must be addressed to allow the generation of highly accurate results by gas chromatographic analysis of fatty acid methyl esters, that of split injection to capillary columns has long been a major problem. A practical solution of this problem is now proposed. Three factors were found to be of major importance in achieving highly accurate results viz. avoidance of needle discrimination when injecting, very rapid vaporisation of the sample and complete homogenisation of the sample with the carrier gas stream. High speed of injection was found to be a highly effective means of avoiding needle discrimination. Rapid vaporisation of the sample was achieved by the use of relatively dilute solutions of analyte in the solvent, the smallest sample size commensurate with obtaining a chromatogram that could be accurately quantitated and, particularly, by the use of injector temperatures considerably higher than those generally adopted. Good mixing of the vaporized sample with the carrier gas was achieved with a number of injector insert designs, but, with improvement of design, it was found possible to achieve linear splitting over a wide range of operating conditions. The most controversial recommendation is to use very high injection temperatures, but it has been shown that the commonly held view that this may cause pyrolysis of fatty acid methyl esters is not true, even when the esters are highly unsaturated.

Chromatography, Gas↗

PubMed1975

Rapid estimation of trace amounts of ethylenimine by high-pressure liquid chromatography.

A rapid procedure utilizing high-pressure liquid chromatography is described for determining trace quantities of ehtylenimine down to 0.01 ppm. The basis for the method is the quantitative reaction of ethyleneimine with the 1,2-naphthoquinone-4-sulphonate ion (Folin's reagent) to give 4-(1-aziridinyl)-1,2-naphthoquinone. Compared with the spectrophotometric procedure, this method provides a high degree of specificity and sensitivity. The method has been employed to determine ethylenimine in the pyrolysis products of polyethylenimine.

Aziridines↗

PubMed2003

Separation methods in the chemistry of humic substances.

Separation methods are widely used to isolate humic substances (HSs), to fractionate them before further investigation, and to obtain information about their structure and properties. Among the chromatographic methods, techniques based on a size-exclusion effect appear to be most useful, as they allow us to relate elution data to the molecular mass distribution of HSs. The limitations of this approach are discussed in this review. Gas chromatography with mass spectrometric detection is typically used to identify the products of pyrolysis or thermochemolysis of HSs; this technique is considered most important in the structural investigation of HSs. Electrophoretic methods (especially capillary zone electrophoresis) provide detailed characterization of HSs, but it is very difficult to relate the electrophoretic data to any specific subfraction, structure or properties of HSs. The electrophoretic patterns are often called "fingerprints" and can potentially be used for the identification and classification of HSs. This is limited, however, by the great diversity of the procedures employed and by the low degree of harmonization--no data on reproducibility and between-laboratory comparability are available. The same holds true, to a certain degree, for most methods utilized for the characterization of HSs. Separation methods play an important role in the examination of the interactions of HSs with heavy metals and other chemical pollutants. They allow us to determine binding constants and other data necessary to predict the mobility of chemical pollutants in the environment.

Chromatography, Gel↗