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PubMed1990

Direct analysis of bacterial fatty acids by Curie-point pyrolysis tandem mass spectrometry.

Although pyrolysis-mass spectrometry (Py-MS) has been used for bacterial taxonomy, many of the mass spectral peaks used for discrimination of organisms have not been correlated to known biomolecules. This work presents the discrimination of five bacterial species based on Py-MS patterns containing only peaks that can be correlated to fatty acids and fatty acid derivatives. These correlations were confirmed by pyrolysis-tandem mass spectrometry of authentic standards and the organisms. The pattern recognition procedures used gave better results when only the fatty acid peaks were used in the analysis than when full spectra were used.

Bacillus↗

PubMed1990

Characterization of underivatized lipid biomarkers from microorganisms with pyrolysis short-column gas chromatography/ion trap mass spectrometry.

A microvolume Curie-point pyrolysis short-column (5 m) gas chromatography/mass spectrometry (Py-GC/MS) procedure was developed for the characterization of various lipid moieties in microorganisms. High linear flow rates (approximately 175 cm/s) characterized the GC conditions in order to effect an efficient chromatographic transfer and elution of the underivatized diglycerides and monoglycerides, and small modifications were necessary to the ion trap MS system in order for it to accommodate the relatively high gas load. During a typical analysis run anhydrodiacylglycerides eluted within a 5-6-min time frame. Gram-positive bacilli and Gram-negative species were differentiated from each other by the pyrolysis patterns of their lipid components. In spite of the complexity of the analyte, a straightforward visual analysis was achieved with the aid of simple computerized data display procedures. These procedures included examination of (1) total ion current (TIC) profiles of the lipid region of the reconstructed chromatogram, (2) the integrated mass spectrum of this region, (3) selected reconstructed ion chromatograms (RICs), (4) RIC intensity distributions, and (5) corresponding mass spectra. An appealing aspect of the lipid data reduction procedure is that most of it can be accomplished visually without requiring computerized pattern recognition techniques.

Bacteria↗

PubMed2001

Quantitative analysis of detailed lignin monomer composition by pyrolysis-gas chromatography combined with preliminary acetylation of the samples.

Detailed quantitative analysis of lignin monomer composition comprising p-coumaryl, coniferyl, and sinapyl alcohol and p-coumaraldehyde, coniferaldehyde, and sinapaldehyde in plant has not been studied from every point mainly because of artifact formation during the lignin isolation procedure, partial loss of the lignin components inherent in the chemical degradative methods, and difficulty in the explanation of the complex spectra generally observed for the lignin components. Here we propose a new method to quantify lignin monomer composition in detail by pyrolysis-gas chromatography (Py-GC) using acetylated lignin samples. The lignin acetylation procedure would contribute to prevent secondary formation of cinnamaldehydes from the corresponding alcohol forms during pyrolysis, which are otherwise unavoidable in conventional Py-GC process to some extent. On the basis of the characteristic peaks on the pyrograms of the acetylated sample, lignin monomer compositions in various dehydrogenative polymers (DHP) as lignin model compounds were determined, taking even minor components such as cinnamaldehydes into consideration. The observed compositions by Py-GC were in good agreement with the supplied lignin monomer contents on DHP synthesis. The new Py-GC method combined with sample preacetylation allowed us an accurate quantitative analysis of detailed lignin monomer composition using a microgram order of extractive-free plant samples.

Acetylation↗

PubMed2001

Pyrolysis-GC-MS analysis of the formation and degradation stages of charred residues from lignocellulosic biomass.

The structural transformations undergone by lignocellulosic biomass (freeze-dried rye grass, Lolium rigidum) subjected to progressive isothermal heating (burning at 350 degrees C under oxidizing conditions for 30, 45, 60, 75, and 90 s) have been monitored by Curie-point pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS). The pyrograms suggest that even charred residues after severe heating (carbon loss ca. 50%) still contain substantial concentrations of some resistant plant structural components. Several trends were observed when monitoring the relative concentrations of the different groups of pyrolysis compounds released during successive charring stages: (i) the tetrapyrrole moiety of chlorophylls is rapidly destroyed as indicated by the decreasing yields of pyrroles and pyrrolines, whereas the phytol backbone is comparatively more resistant, leading to phytadienes after dehydration and reduction; (ii) the increasing yields of imidazoles from progressively heated samples (maximum at 45 s stage) suggest accumulation of newly formed nitrogen-containing compounds that may survive natural fires; (iii) the lignin backbone shows a relative resistance, the yields of aromatic products pointing to progressive demethoxylation; and, (iv) a selective accumulation of recalcitrant alkyl material occurred, which is interpreted as the result of thermal condensation of hydrocarbons and fatty acids into macromolecular materials in the charred residue. In terms of the intensity of the isothermal heating, the yields of the different classes of alkyl compounds follow the order phytadienes < fatty acids < alkanes < wax esters < sterols.

Biomass↗

PubMed2000

Flash vacuum pyrolysis of methoxy-substituted lignin model compounds.

The flash vacuum pyrolysis (FVP) of methoxy-substituted beta-O-4 lignin model compounds has been studied at 500 degrees C to provide mechanistic insight into the primary reaction pathways that occur under conditions of fast pyrolysis. FVP of PhCH(2)CH(2)OPh (PPE), a model of the dominant beta-O-4 linkage in lignin, proceeds by C-O and C-C cleavage, in a 37:1 ratio, to produce styrene plus phenol as the dominant products and minor amounts of toluene, bibenzyl, and benzaldehyde. From the deuterium isotope effect in the FVP of PhCD(2)CH(2)OPh, it was shown that C-O cleavage occurs by homolysis and by 1,2-elimination in a ratio of 1.4:1, respectively. Methoxy substituents enhance the homolysis of the beta-O-4 linkage, relative to PPE, in o-CH(3)O-C(6)H(4)OCH(2)CH(2)Ph (o-CH(3)O-PPE) and (o-CH(3)O)(2)-C(6)H(3)OCH(2)CH(2)Ph ((o-CH(3)O)(2)-PPE) by a factor of 7.4 and 21, respectively. The methoxy-substituted phenoxy radicals undergo a complex series of reactions, which are dominated by 1,5-, 1,6-, and 1,4-intramolecular hydrogen abstraction, rearrangement, and beta-scission reactions. In the FVP of o-CH(3)O-PPE, the dominant product, salicylaldehyde, forms from the methoxyphenoxy radical by a 1,5-hydrogen shift to form 2-hydroxyphenoxymethyl radical, 1,2-phenyl shift, and beta-scission of a hydrogen atom. The 2-hydroxyphenoxymethyl radical can also cleave to form formaldehyde and phenol in which the ratio of 1, 2-phenyl shift to beta-scission is ca. 4:1. In the FVP of o-CH(3)O-PPE and (o-CH(3)O)(2)-PPE, products (ca. 20 mol %) are also formed by C-O homolysis of the methoxy group. The resulting phenoxy radicals undergo 1,5- and 1,6-hydrogen shifts in a ratio of ca. 2:1 to the aliphatic or benzylic carbon, respectively, of the phenethyl chain. In the FVP of (o-CH(3)O)(2)-PPE, o-cresol was the dominant product. It was formed by decomposition of 2-hydroxy-3-hydroxymethylbenzaldehyde and 2-hydroxybenzyl alcohol, which are formed from a complex series of reactions from the 2, 6-dimethoxyphenoxy radical. The key step in this reaction sequence was the rapid 1,5-hydrogen shift from 2-hydroxy-3-methoxybenzyloxy radical to 2-hydroxymethyl-6-methoxyphenoxy radical before beta-scission of a hydrogen atom to give the substituted benzaldehyde. The 2-hydroxybenzyl alcohols rapidly decompose under the reaction conditions to o-benzoquinone methide and pick up hydrogen from the reactor walls to form o-cresol.

Biopolymers↗

PubMed1999

Pyrolysis mass spectrometry analysis of free-living and symbiotic cyanobacteria.

The potential of pyrolysis mass spectrometry to distinguish closely related cyanobacterial strains was assessed by using the technique to compare symbiotic cyanobacteria isolated from the hornwort Phaeoceros laevis and free-living cyanobacterial strains at the same field site. The same strains had previously been compared using polymerase chain reaction-based DNA fingerprinting techniques (West & Adams 1997, Appl. Environ. Microbiol. 63: 4479-4484). Many of the strains were grouped identically by the two techniques, although there were some differences, possibly resulting from the ability of these cyanobacteria to develop a range of specialised cell types having different chemical compositions to the vegetative cells. Although growth conditions were chosen to suppress cellular differentiation, this may not always have been completely successful. With careful control of growth conditions pyrolysis mass spectrometry has considerable potential as an additional tool for the phenetic comparison of cyanobacterial strains. It has the advantage that analysis is directly derived from whole cells, and hence is simpler and cheaper than DNA-based methods, although it does require the growth of axenic strains. The technique may be particularly useful in the study of some of the more cryptic unicellular and non-heterocystous filamentous cyanobacterial groups, in which the lack of cellular differentiation should minimise any variability in the chemical composition of cells.

Bacterial Typing Techniques↗

PubMed1985

Low-Mr hydrocarbons generated during hydrous and dry pyrolysis of kerogen.

The validity of applying laboratory pyrolysis experiments to simulating the maturation of organic matter in sedimentary basins has been vigorously debated. We report here results from the generation of hydrocarbons of low relative molecular mass (Mr) in both hydrous and dry pyrolysis. A principal difference is that under dry conditions in the presence of montmorillonite, catalysis occurs with respect to generation of low-Mr hydrocarbons but no such effect is evident for hydrous conditions, probably because of a reduction in the clay's acidity. In addition, olefins which were previously reported as not being present in the products of hydrous pyrolyses were found to be produced in the C2-C6 range in comparable amounts under both hydrous and dry pyrolyses at 300 degrees C and may form in the course of kerogen catagenesis in nature but disappear with geologic time due to their instability. These studies have relevance to understanding the interactions between kerogen and minerals in sedimentary rocks and to processes in the formation of natural gas.

Alkenes↗

PubMed2001

Characterization of Aphanomyces invadans isolates using pyrolysis mass spectrometry (PyMS).

Twenty-one isolates of Aphanomyces invadans, the fungal pathogen associated with the Asian fish disease epizootic ulcerative syndrome (EUS), were compared with other Oomycete fungi in terms of their pyrolysis mass spectrometry (PvMS) profiles. Canonical variate analysis (CVA) of the pyrolysis mass spectra distinguished the Aphanomyces species from a wide scatter of Achlya and Saprolegnia isolates. Further CVA and hierarchal cluster analysis (HCA) separated the Aphanomyces species into two main groups. The first group clustered A. invadans isolates from EUS outbreaks in Thailand, Bangladesh, Indonesia, Philippines, Australia and Japan together. However, HCA also included the crayfish plague fungus Aphanomyces astaci within this group. Non-pathogenic Aphanomyces strains isolated from ulcerative mycosis (UM)-affected fish were shown to be distinct from A. invadans, and instead clustered with saprophytic Aphanomyces strains to form the second group. Recently, an invasive Aphanomyces pathogen has been isolated from UNI-affected fish, but that was not tested here. This is the first report using PyMS in the study of Oomycete systematics. The technique was not sensitive enough to show any intraspecific differences, but it was considered a useful technique for the discrimination of species where taxonomic relationships are uncertain.

Animals↗

PubMed2000

Laser pyrolysis fabrication of ferromagnetic gamma'-Fe4N and FeC nanoparticles.

Using the laser pyrolysis method, single phase gamma'-Fe4N nanoparticles were prepared by a two step method involving preparation of nanoscale iron oxide and a subsequent gas-solid nitridation reaction. Single phase Fe3C and Fe7C3 could be prepared by laser pyrolysis from Fe(CO)5 and 3C2H4 directly. Characterization techniques such as XRD, TEM and vibrating sample magnetometer were used to measure phase structure, particle size and magnetic properties of these nanoscale nitride and carbide particles.

Carbon Compounds, Inorganic↗

PubMedDate not supplied

Hydraulic fluids and jet engine oil: pyrolysis and aircraft air quality.

Incidents of smoke in aircraft cabins often result from jet engine oil and/or hydraulic fluid that leaks into ventilation air, which can be subjected to temperatures that exceed 500 degrees C. Exposed flight-crew members have reported symptoms, including dizziness, nausea, disorientation, blurred vision, and tingling in the legs and arms. In this study, the authors investigated pyrolysis products of one jet engine oil and two hydraulic fluids at 525 degrees C. Engine oil was an important source of carbon monoxide. Volatile agents and organophosphate constituents were released from all the agents tested; however, the neurotoxin trimethyl propane phosphate was not found. The authors hypothesized that localized condensation of pyrolysis products in ventilation ducts, followed by mobilization when cabin heat demand was high, accounted for mid-flight incidents. The authors recommended that carbon monoxide data be logged continuously to capture levels during future incidents.

Air Pollutants↗

PubMed1975

Polyvinyl chloride pyrolysis products. A potential cause for respiratory impairment.

A limited investigation of respiratory and other symptom prevalence, plus before and after shift ventilatory capacity was conducted among a group of 17 meat wrappers exposed to pyrolysis products of polyvinyl chloride and a group of 21 control subjects. Exposed meat wrappers showed a higher prevalence of cough, phlegm, hay fever, and asthma than did the control group. The exposed group also demonstrated relative decreases in forced expiratory volume, one second (FEV1.0) and forced expiratory flow 50% (FEF50) after one shift of work; whereas, the controls showed an opposite tendency. These findings suggest that meat wrappers exposed to pyrolysis products of polyvinyl chloride might be adversely affected. The results, while suggestive, are not totally conclusive owing to the fact that there was not ideal matching of the exposed and control groups in regard to age, height, race, sex, and smoking status.

Age Factors↗

PubMed2003

Pyrolysis of composite plastic waste.

Several different composite plastics were pyrolysed in a fixed bed reactor at final temperatures between 350 and 800 degrees C. The composites studied were polyester, phenolic, epoxy, vinylester, polypropylene and PET resins, reinforced with glass and/or carbon fibre. The product yields of oil gas and solid residue were determined together with a detailed composition of the derived gases. There was evidence to suggest that calcium carbonate filler, present in the polyester and phenolic composites, decomposed to form carbon dioxide at 800 degrees C, which was subsequently involved in char gasification reactions. Polyester, phenolic and epoxy composites generated highly aromatic, oxygenated condensable products. There was no noticeable correlation between the composition of these products and the final pyrolysis temperature. The tensile strength of recovered glass fibre was lower than that of virgin fibre and decreased markedly as the final pyrolysis temperature increased from 650 to 800 degrees C.

Conservation of Natural Resources↗

PubMed2000

Production of activated carbons from pyrolysis of waste tires impregnated with potassium hydroxide.

Activated carbons were produced from waste tires using a chemical activation method. The carbon production process consisted of potassium hydroxide (KOH) impregnation followed by pyrolysis in N2 at 600-900 degrees C for 0-2 hr. The activation method can produce carbons with a surface area (SA) and total pore volume as high as 470 m2/g and 0.57 cm3/g, respectively. The influence of different parameters during chemical activation, such as pyrolysis temperature, holding time, and KOH/tire ratio, on the carbon yield and the surface characteristics was explored, and the optimum preparation conditions were recommended. The pore volume of the resulting carbons generally increases with the extent of carbon gasified by KOH and its derivatives, whereas the SA increases with degree of gasification to reach a maximum value, and then decreases upon further gasification.

Air Pollutants, Occupational↗

PubMed1978

Pyrolysis gas chromatography of enzymes.

Pyrolysis gas chromatography (PGC) has been shown to be useful for differentiating enzymes. The enzymes alpha-chymotrypsin, lactate dehydrogenase, catalase, and urease were easily "fingerprinted" on a 1.8 m 0.5% Carbowax 20 M column. Also, in some cases, isoenzymes of lactate dehydrogenase could be distinguished. Based on the pyrolyses of the free aromatic amino acids, four major enzyme pyrolysis peaks were tentatively identified as organic compounds derived from tyrosine and tryptophan. The use of a nitrogen-selective detector in conjunction with the FID and measurement of peak retention times by computer on three different types of columns permitted confirmations of peak identity.

Acetylcholinesterase↗

PubMed2000

Forensic discrimination of automotive paint samples using pyrolysis-gas chromatography-mass spectrometry with multivariate statistics

Analytical pyrolysis-gas chromatography (Py-GC) has been a standard method for the forensic analysis of automotive paint for a number of decades. Automotive paints are often identified by visual comparison of pyrograms for peak presence and intensities; however, such analyses can be subjective and time consuming. A preliminary investigation based on Py-GC-mass spectrometric analysis of 100 automobile paint samples of five different colors is presented. Designed experiments are employed to select pyrolysis conditions for adequate discrimination. Pattern recognition techniques including principal component analysis and canonical variates analysis are used to visualize clustering of pyrograms to validate comparisons between different automotive paint pyrograms. These methods have the potential to ease the interpretation task for data sets involving a large number of comparisons.

Journal Article↗

PubMed2001

Thin-layer chromatography-pyrolysis-gas chromatography-mass spectrometry: a multidimensional approach to marine lipid class and molecular species analysis.

A new multidimensional chromatographic method is described in which material separated into lipid-class bands on silica-coated quartz thin-layer chromatography (TLC) rods (Chromarods) is desorbed using a pyrolysis unit interface and introduced directly into a gas chromatograph-mass spectrometer for molecular species analysis. Steryl esters, wax esters, hydrocarbons, ketones, and fatty-acid methyl esters (FAMEs) are thermally desorbed without pretreatment. In order to desorb free sterols, monoacylglycerols (MAGs), aliphatic alcohols, and free fatty acids, the esters are converted to trimethylsilyl derivatives on the rod. Triacylglycerols and phospholipids are converted to FAMEs by thermochemolysis with tetramethylammonium hydroxide. The method's utility is demonstrated with lipids from seawater particulate matter by first confirming the identity of lipid bands with the appropriate standards. The wax ester-steryl ester TLC band contained no more than 8% steryl esters. Wax esters of up to C42 are detected. In six individual acyl lipid classes, C14-C22 fatty acids are detected with C16 acids predominant in all but wax esters. C16-C22 MAGs are identified in the complex acetone-mobile polar lipid band. The method successfully extends the scope of latroscan TLC-flame-ionization detection on Chromarods, which is a widely used technique for lipid-class analysis. Modification of the pyrolysis probe to handle intact TLC rods is a future objective.

Journal Article↗

PubMed1986

Pyrolysis gas chromatography-mass spectrometry of mycobacterial mycolic acid methyl esters and its application to the identification of Mycobacterium leprae.

Pyrolysis gas chromatography-mass spectrometry of methyl mycolates from 32 species of mycobacteria, including Mycobacterium leprae, was carried out. The mycobacteria could be classified into four groups in respect of the fatty acid ester patterns detected within the range C20 to C26. The applicability of this pyrolysis-gas chromatographic method for identifying M. leprae is discussed.

Chromatography, Gas↗

PubMed1989

A pyrolysis mass spectrometry study of fusobacteria.

Strains of fusobacteria (143) were examined by pyrolysis mass spectrometry (Py-MS) with a Horizon Instruments PYMS 200X. Fusobacterium necrogenes, F. necrophorum, F. nucleatum, F. mortiferum, F. varium, F. gonidiaformans, F. naviforme, F. russii and Leptotrichia buccalis were discriminated. Strains of fusobacteria isolated from tropical ulcers, although similar to F. mortiferum in conventional tests, were discriminated from each of these species in Py-MS. Identification of 416 spectra to species level agreed with conventional bacteriological methods in 91.8% of cases, was equivocal in 3.4% and disagreed in 4.8%. Classification based on pyrolysis data resolved groups largely corresponding to the recognised species. However, F. nucleatum strains were divided between two distinct groups. The tropical ulcer strains were resolved as a distinct homogeneous group. Py-MS is a rapid, inexpensive and convenient procedure for characterisation of bacteria, with the capacity for a high throughput of samples, although the initial cost of the apparatus is high.

Fusobacterium↗