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PubMed2005

Structure and properties relationships for aromatic polyimides and their derived carbon membranes: experimental and simulation approaches.

The main objective of this study is to investigate the factors of the chemical structure and physical properties of rigid polyimides in determining the performance of derived carbon membranes through both the experimental and simulation methods. Four polyimides made of different dianhydrides were pyrolyzed at 550 and 800 degrees C under vacuum conditions. The resultant carbon membranes exhibit excellent gas separation performances beyond the traditional upper limit line for polymer membranes. The thermal stability and the fractional free volume (FFV) of polyimides were examined by a thermogravimetric analyzer and a density meter. The chain properties of polyimide, such as flatness, chain linearity, and mobility, were simulated using the Cerius(2) software. All above characterizations of polyimides were related to the microstructure and gas transport properties of the resultant carbon membranes. It was observed that the high FFV values and low thermal stability of polyimide produce carbon membranes with bigger pore and higher gas permeability at low pyrolysis temperatures. Therefore, polyimides with big thermally labile side groups should be preferred to prepare carbon membranes at low pyrolysis temperatures for high permeability applications. On the other side, since the flatness and in-plane orientation of precursors may lead carbon membranes to ordered structure, thus obtaining high gas selectivity, linear polyimides with more coplanar aromatic rings should be first choice to prepare carbon membranes at high pyrolysis temperatures for high selectivity applications. The location of the indan group also affects chain flatness and in-plane orientation. As a result, carbon membranes derived from the BTDA-DAI precursor have superior separation performance to those derived from Matrimid.

Journal Article↗

PubMed2000

Biosystematic studies on novel streptomycetes from soil.

Members of three putatively novel Streptomyces species, designated Streptomyces groups A, B and C, were repeatedly isolated from environmental samples taken from four hay meadow plots at Cockle Park Experimental Farm, Northumberland (UK). Representative isolates were found to have properties consistent with their classification in the genus Streptomyces and were recovered in three taxa using different phenotypic criteria, namely morphological and pigmentation properties, rapid enzyme tests, and whole-organism fatty acid, protein electrophoretic and pyrolysis mass-spectrometric data. The isolates were rapidly characterised as three taxonomic groups using pyrolysis mass spectrometry. The three taxa were also distinguished from one another and from validly described species of Streptomyces using rapid enzyme tests based on the fluorophores 7-amino-methylcoumarin and 4-methylumbelliferone, and computer-assisted identification procedures. The results indicate that selective isolation and rapid characterisation of streptomycetes using pyrolysis mass spectrometry provide a practical way of determining the phenotypic species diversity of streptomycetes in natural habitats. The experimental data also indicate that representative sampling of cultivable streptomycetes from soil can best be achieved using a multi-step extraction procedure coupled with the use of selective isolation procedures.

Bacterial Proteins↗

PubMed2000

Genomic and phenomic differentiation of Rhodococcus equi and related strains.

16S rDNA sequence and pyrolysis mass spectrometric analyses were carried out on representatives of Rhodococcus equi and marker strains of genera that encompass mycolic acid containing actinomycetes. The R. equi strains formed a monophyletic clade within the evolutionary radiation occupied by members of the genera Nocardia and Rhodococcus. The 16S rDNA sequence data also showed R. equi to be an heterogeneous taxon. This heterogeneity was underscored by the pyrolysis mass spectrometric data. These observations are in line with those of previous studies where similar profiles of relatedness were found between pyrolysis mass spectral data and the results of DNA:DNA pairing and numerical phenetic studies.

Actinomycetales↗

PubMed1990

Determination of phosphorus in biological material using electrothermal atomisation atomic absorption spectrometry with a molybdenum tube atomiser.

Phosphorus has been determined by electrothermal atomisation atomic absorption spectrometry with a molybdenum tube atomiser. The effects of interferents on the phosphorus signal have been investigated. Chemical interferences were eliminated by high-temperature pyrolysis. The detection limit for the molybdenum tube system was 2.3 ng (corresponding to 2.3 micrograms ml-1 when 1 microliter was injected into the atomiser) and the characteristic mass was 1.9 ng of phosphorus. A calibration graph method combined with high-temperature pyrolysis has been evaluated through the determination of phosphorus in biological materials. The sensitivity, accuracy and precision of the method were superior to or nearly equal to those of graphite furnace atomic absorption spectrometry. The advantages of the high-temperature pyrolysis method are its simplicity and low cost.

Animals↗

PubMed1969

The unextractable organic fraction of the pueblito de allende meteorite: evidence for its indigenous nature.

The Pueblito de Allende meteorite contains only 0.1-0.5 ppm of solvent-extractable carbon, most or all of which is due to terrestrial contamination. Determinations of the total carbon content gives values from 0.23 to 0.35 per cent. The presumed indigenous insoluble carbon is thus present in a ratio of 2300:1 relative to contaminant carbon. A sample of the meteorite was extracted with a deuterated solvent containing benzene:methanol (4:1 w/w) to remove contaminants and then was subjected to pyrolysis-gas chromatography-mass spectrometry to investigate the nature of the remaining carbon. The pyrolysis products (about 20 ppm) consisted chiefly of aromatic and substituted aromatic hydrocarbons. The pyrolysis results were confirmed by oxidative thermal analysis which showed that the bulk of the carbon present was a macromolecular structure and not graphite. This suggests that an insoluble nongraphitic condensed aromatic polymer is indigenous to the meteorite. The origin and precise chemical structure of this material has not been determined, but it bears a superficial resemblance to coal-like structures.

Journal Article↗

PubMed1999

Protein preservation and DNA retrieval from ancient tissues.

The retrieval of DNA from fossils remains controversial. To substantiate claims of DNA recovery, one needs additional information on the preservation of other molecules within the same sample. Flash pyrolysis with GC and MS was used to assess the quality of protein preservation in 11 archaeological and paleontological remains, some of which have yielded ancient DNA sequences authenticated via a number of criteria and some of which have consistently failed to yield any meaningful DNA. Several samples, including the Neanderthal-type specimen from which DNA sequences were recently reported, yielded abundant pyrolysis products assigned to 2,5-diketopiperazines of proline-containing dipeptides. The relative amounts of these products provide a good index of the amount of peptide hydrolysis and DNA preservation. Of these samples, four stem from arctic or subarctic regions, emphasizing the importance of cooler temperatures for the preservation of macromolecules. Flash pyrolysis with GC and MS offers a rapid and effective method for assessing fossils for the possibility of DNA preservation.

Amino Acids↗

PubMed2004

Preparation of sulfurized powdered activated carbon from waste tires using an innovative compositive impregnation process.

The objective of this study is to develop an innovative compositive impregnation process for preparing sulfurized powdered activated carbon (PAC) from waste tires. An experimental apparatus, including a pyrolysis and activation system and a sulfur (S) impregnation system, was designed and applied to produce sulfurized PAC with a high specific surface area. Experimental tests involved the pyrolysis, activation, and sulfurization of waste tires. Waste-tire-derived PAC (WPAC) was initially produced in the pyrolysis and activation system. Experimental results indicated that the Brunauer-Emmett-Teller (BET) surface area of WPAC increased, and the average pore radius of WPAC decreased, as water feed rate and activation time increased. In this study, a conventional direct impregnation process was used to prepare the sulfurized PAC by impregnating WPAC with sodium sulfide (Na2S) solution. Furthermore, an innovative compositive impregnation process was developed and then compared with the conventional direct impregnation process. Experimental results showed that the compositive impregnation process produced the sulfurized WPAC with high BET surface area and a high S content. A maximum BET surface area of 886 m2/g and the S content of 2.61% by mass were obtained at 900 degrees C and at the S feed ratio of 2160 mg Na2S/g C. However, the direct impregnation process led to a BET surface area of sulfurized WPAC that decreased significantly as the S content increased.

Carbon↗

PubMed2000

An improved configuration of a moving wire transport detector.

An improved design of the transport detector is described that uses a pre-oxidized titanium ribbon as the transport medium. The titanium ribbon has a high loading capacity that permits a large proportion of the total column eluent to be taken into the sensing system. The solute is sensed by pyrolysis and the subsequent detection of pyrolysis products by a miniature argon detector. The pyrolyzer and sensor system is designed to ensure that all the pyrolysis products enter the detector with minimum dilution and band dispersion. As a result, the sensitivity of the detector (or minimum detectable concentration) has been reduced by approximately two orders of magnitude compared with the original design. The sensitivity of the system described to sucrose is 8 x 10(-8) g/mL, which is similar to the sensitivity of the fixed-wavelength UV detector to benzene (approximately 5 x 10(-8) g/mL). It would appear that the new design has potentially a sensitivity at least an order of magnitude lower than that reported here.

Journal Article↗

PubMed2000

Free radical intermediates in sonodynamic therapy.

Current understanding of the mechanism of sonodynamic action (i.e. the ultrasound-dependent enhancement of the cytotoxic action of certain drugs--sonosensitizers) with potential applications for cancer therapy is presented. The experimental evidence suggests that sonosensitization is due to the chemical activation of sonosensitizers inside or in the close vicinity of hot collapsing cavitation bubbles to form sensitizer-derived free radicals either by direct pyrolysis or due to reactions with .H and .OH radicals, formed by pyrolysis of water. These free radicals (mostly carbon-centered) react with oxygen to form peroxyl and alkoxyl radicals. Unlike .OH and .H, which are also formed by pyrolysis inside cavitation bubbles, the reactivity of alkoxyl and peroxyl radicals with organic components dissolved in biological media is lower and hence have higher probability of reaching critical cellular sites. Sonodynamic therapy appears to be a promising modality for cancer treatment since ultrasound can penetrate deep within the tissue and can be focused in a small region of tumor to chemically activate relatively non-toxic molecules (e.g. porphyrins) thus minimizing undesirable side effects.

Electron Spin Resonance Spectroscopy↗

PubMed1991

Chemical and molecular weight analyses of prosthodontic soft polymers.

A number of studies have been made investigating the properties of dental prosthodontic soft polymer materials. In such materials, which are used as short-term denture soft liners, the polymer component is complexed with one or more plasticizers. This lowers the glass transition temperature, Tg, of the polymer by allowing greater chain mobility and produces a more flexible material. Little information is available relating to the polymer components of such soft-lining materials. The chemical composition and molecular-weight distribution of a polymer help to determine its ability to form a plasticized soft polymer-gel. In the present work, both pyrolysis depolymerization/gas chromatography (GC) and size exclusion chromatography (SEC) have been used to characterize 11 commercial polymer powders. By use of SEC and polymer standards having a narrow molecular-weight range, it has been possible for accurate molecular-weight distributions to be determined for all 11 powders. The peak molecular weights were found to be between 1.79 x 10(5) and 3.28 x 10(5). These values are above the molecular weight at which chain entanglement occurs. The polydispersity ratios (Mw/Mn) were between 2.09 and 4.48. Methacrylate polymers can be readily decomposed thermally to their constituent monomers, which, once recovered, can be analyzed by gas chromatography. The simple pyrolysis apparatus used in the present study was easily assembled and was capable of producing both qualitative and quantitative results. None of the commercial polymers analyzed gave methacrylate decomposition products with pendant chains greater than ethyl (-CH2-CH3). All of the commercial polymers successfully studied by the pyrolysis test method proved to be poly(ethyl [100-79%]/methyl [0-21%] methacrylate) polymers or co-polymers.

Chromatography, Gas↗

PubMed1989

[Non-crystallinity determination by thermal analysis of freeze-dried cephalothin sodium].

Cephalothin sodium (CET-Na) prepared according to the conventional freeze-drying methods is known to easily develop color during storage. Since amorphous CET-Na has been reported to be markedly unstable, the color development is thought to be due to the presence of traces of CET-Na in an amorphous state observed with scanning electron microscopy. Quantitation by use of the powder X-ray diffractometry of such traces of amorphous CET-Na has proved to be of little use. Thermogravimetry (TG) and differential scanning calorimetry (DSC) have demonstrated that the freeze-dried CET-Na by the conventional methods contains three types of CET-Na: amorphous (unstable phase), quasi-crystalline (metastable phase) and crystalline (stable phase). Pyrolysis initiation temperatures of these three types of CET-Na have been demonstrated to become higher in this order. A new parameter for the evaluation of non-crystallinity of CET-Na has been introduced, in which the ratio is calculated from the data of the total weight loss observed through the pyrolysis of both amorphous and quasi-crystalline CET-Na against the total weight loss of all components during the pyrolysis of sample specimen. The ratio thus calculated is defined as "non-crystallinity". This new parameter has successfully been introduced to establish a good correlation to the degree of increasing color intensity with aging of freeze-dried CET-Na.

Calorimetry, Differential Scanning↗

PubMed1989

Thermally induced formation of polychlorinated dibenzofurans from Aroclor 1254-contaminated mineral oil.

Numerous laboratory simulations and real-world events have demonstrated the thermal conversion of neat or high concentration of PCBs into the much more toxic PCDFs. Since millions of mineral oil transformers currently in service contain PCB concentrations in the 50 to 5000 ppm range, the thermal behavior of dilute PCB solutions is of practical and regulatory significance. In this work, neat Aroclor 1254 and 5000 ppm Aroclor 1254 in mineral oil were subjected to pyrolysis and combustion under a range of experimental conditions to define parameters resulting in maximal PCDF yields. The dependence of PCDF yield on Aroclor 1254 concentrations was then investigated in the 5000 to 50 ppm range. Combustion experiments demonstrated that PCDF yields expressed as micrograms PCDF/gram PCB were independent of concentration range, confirming that the process is kinetically first order in PCB. Much lower yields of PCDF were observed in the open tube pyrolysis experiments, as compared to combustion experiments and to earlier and concurrent sealed tube experiments. Slightly improved yields were observed in the pyrolysis experiments at lower concentrations, suggesting the existence of a PCB or PCDF destruction process of higher than first order kinetics. In all cases, yields expressed as micrograms PCDF/gram mixture were sharply and monotonically lower as concentrations decreased between neat or 5000 ppm Aroclor 1254 and 50 ppm Aroclor 1254.

Aroclors↗

PubMed2004

The interference effect of a mixture of magnesium, aluminium, sulfate and chloride on the atomization and vaporization of manganese in graphite furnace atomic absorption spectrometry.

In this study, the interference effects of Al3+, Mg2+, Cl- and SO4(2-) ions on the determination of manganese by graphite furnace atomic absorption spectrometry (GFAAS) were investigated. At first, the interferences caused by Al2(SO4)3, AlCl3, MgCl2 and MgSO4, which are the most possible major compounds for the combinations of the ions mixed, were individually considered. Then, the effects caused by mixtures containing various amounts of MgSO4 and AlCl3 were studied. If the pyrolysis temperature is below 800 degrees C, AlCl3 changes the vaporization mechanism of manganese. These interferences disappear at higher pyrolysis temperatures. At the same time, aluminum salts may cause the formation of refractory compounds between aluminum and manganese (like spinel MnAl2O4) that shift the absorption signals of manganese to higher temperatures. Magnesium sulfate, by itself, does not cause any depression of manganese signals. In fact, it acts as a modifier, preventing volatilization losses of manganese during the pyrolysis step. A conclusion was reached that detailed investigation of the interferences in a complex media is a very difficult experimental and theoretical task. To solve practical problems, one may better follow the general notions developed in GFAAS toward complex matrices.

Journal Article↗

PubMedDate not supplied

Degradation of biomacromolecules during high-rate composting of wheat straw-amended feces.

Pig (Sus scrofa) feces, separately collected and amended with wheat straw, was composted in a tunnel reactor connected with a cooler. The composting process was monitored for 4 wk and the degradation of organic matter was studied by two chemical extraction methods, 13C cross polarization magic angle spinning (CPMAS) nuclear magnetic resonance (NMR) and pyrolysis gas chromatography-mass spectrometry (GC-MS). Wet-chemical extraction methods were not adequate to study the degradation of specific organic compounds as the extraction reagents did not give selective separation of hemicellulose, cellulose, proteins, and lignins. A new method was proposed to calculate the contribution of four biomacromolecules (aliphatics, proteins, polysaccharides, and lignin) from the 13C CPMAS NMR spectrum. Pyrolysis GC-MS allowed identification of the composition of the biomacromolecules. The biomacromolecules showed different rates of degradation during composting. High initial degradation rates of aliphatics, hemicellulose, and proteins were observed, where aliphatics were completely degraded and hemicellulose and proteins were partly recalcitrant during the four weeks of composting. The degradation rate of cellulose was much lower and degradation was not completed within the four weeks of composting. Lignin was not degraded during the thermophilic stage of composting but started to degrade slowly during the mesophilic stage. A combination of 13C CPMAS NMR and pyrolysis GC-MS gave good qualitative and semiquantitative assessments of the degradation of biomacromolecules during composting.

Animals↗

PubMed1979

Mutagenic factors in cooked foods.

The charred surface of fish and beef showed strong mutagenic activity in Salmonella typhimurium test strains when activated by S-9 mix of rat liver. The pyrolysis products of proteins and amino acids were also highly mutagenic. Among the pyrolysis products of amino acids, those of tryptophan, serine, and glutamic acid were most active. The new gamma-carboline derivatives, 3-amino-1,4-dimethyl-5H-pyrido[4,3-b]indole and 3-amino-1-methyl-5H-pyrido[4,3-b]indole, were purified from the pyrolysis products of tryptophan. These new compounds were stronger mutagens than aflatoxin B1 towards S. typhimurium TA98, a frameshift type mutant, and they also transformed cryopreserved Syrian hamster embryo cells in vitro. Tryptophan pyrolysate also contained the beta-carboline derivatives, norharman and harman, which are not mutagenic alone, but act as comutagens. A mixture of norharman or harman and nonmutagenic aniline or o-toluidine was strongly mutagenic. The mutagenicities of charred products of other foods, such as seaweed and garlic, are reviewed in this article. Flavonoids, such as kaempferol and quercetin, and glycosides of these flavonoles were mutagenic. The mutagenicity of cooked vegetables depends partly on these flavonoid derivatives. The already-known existence of benzol[a]pyrene and nitroso compounds in cooked food is also reviewed.

Amino Acids↗

PubMed1995

Incineration as a method for resource recovery from inedible biomass in a Controlled Ecological Life Support System.

Resource recovery from waste streams in a space habitat is essential to minimize the resupply burden and achieve self-sufficiency. In a Controlled Ecological Life Support System (CELSS) human wastes and inedible biomass will represent significant sources of secondary raw materials necessary for support of crop plant production (carbon, water, and inorganic plant nutrients). Incineration, pyrolysis, and water extraction have been investigated as candidate processes for recovery of these important resources from inedible biomass in a CELSS. During incineration CO2 is produced by oxidation of the organic components and this product can be directly utilized by plants. Water is concomitantly produced, requiring only a phase change for recovery. Recovery of inorganics is more difficult, requiring solubilization of the incinerator ash. The process of incineration followed by water solubilization of ash resulted in loss of 35% of the inorganics originally present in the biomass. Losses were attributed to volatilization (8%) and non-water-soluble ash (27%). All of the ash remaining following incineration could be solubilized with acid, with losses resulting from volatilization only. The recovery for individual elements varied. Elemental retention in the ash ranged from 100% of that present in the biomass for Ca, P, Mg, Na, and Si to 10% for Zn. The greatest water solubility was observed for potassium with recovery of approximately 77% of that present in the straw. Potassium represented 80% of the inorganic constituents in the wheat straw, and because of slightly greater solubility made up 86% of the water-soluble ash. Following incineration of inedible biomass from wheat, 65% of the inorganics originally present in the straw were recovered by water solubilization and 92% recovered by acid solubilization. Recovery of resources is more complex for pyrolysis and water extraction. Recovery of carbon, a resource of greater mass than the inorganic component of biomass, is more difficult following pyrolysis and water extraction of biomass. In both cases, additional processors would be required to provide products equivalent to those resulting from incineration alone. The carbon, water, and inorganic resources of inedible biomass are effectively separated and output in usable forms through incineration.

Biomass↗

PubMed1991

Prolonged asthma after smoke inhalation: a report of three cases and a review of previous reports.

The development of prolonged obstructive airways disease after smoke inhalation is of concern to fire victims and fire fighters. Three cases of asthma that developed following the inhalation of pyrolysis products are presented along with a review of previous reports of airway injury from smoke inhalation. Polyvinyl chloride pyrolysis products seem to pose a high risk, but other toxic inhalants are also implicated. There is substantial evidence that prolonged airway hyper-responsiveness and asthma may follow numerous inflammatory insults including smoke inhalation. Studies to identify specific individual risk factors and asthmagenic pyrolysis products are needed. Early, postexposure anti-inflammatory treatment may modify the outcome.

Adult↗

PubMed1987

Immunochemically detected nuclear envelope-associated cytochrome P-450 component(s) in rat hepatocyte culture lines.

The presence and location of cytochrome P-450 in Donryu rat hepatocyte culture lines, Ac2F cells and 3 other cell lines were assessed by indirect immunofluorescence examination using anti-cytochrome P-450 monoclonal antibodies. Ac2F cells and other hepatocyte cell lines were selectively stained at their nuclear envelope, but not the cytoplasm, with a monoclonal antibody selective to a high-spin form of cytochrome P-448 (P-448H), although this monoclonal antibody stained primary cultured normal rat hepatocytes at both cellular components and did not stain hepatoma cells of 2 transplantation lines. The results of unscheduled DNA synthesis assay with Ac2F cells using several carcinogenic aromatic amines (4-aminoazobenzene derivatives and amino acid pyrolysis products) suggested that this nuclear envelope-associated cytochrome P-450 activates a restricted portion of these aromatic amines, i.e., a tryptophan pyrolysis component and a glutamic acid pyrolysis component. These results indicate that rat hepatocyte culture lines lack (or contain a reduced amount of) the cytoplasmic cytochrome P-450 but maintain a characteristic type of cytochrome P-450, probably a kind of cytochrome P-448H in their nuclear envelope, and this may be involved in oxidative metabolism of a restricted portion of aromatic amines.

Animals↗