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PubMed1997

Applications of pyrolysis mass spectrometry in studies on the mode of action of antimicrobial agents.

Changes in overall cell composition during exposure to antimicrobial agents were investigated by pyrolysis mass spectrometry (Py-MS) in parental (O+K+), K antigen deficient (O+K-), and O and K antigen deficient (O-K-) strains of Klebsiella aerogenes NCTC 5055. Changes followed distinct patterns that correlated with mode of action: penicillin binding protein (PBP) 3 blockade (ceftazidime, piperacillin); PBP 2 blockade (imipenem); membrane disruption (colistin); bacteriostatic (chloramphenicol), and bactericidal (gentamicin) protein synthesis inhibition; and DNA synthesis inhibition (ciprofloxacin). Changes were pronounced after exposure for 1 hour at 10 x MIC. In general, the O-K- strain showed the largest compositional shifts, and the parental O+K+ strain the least shifts, correlating with bactericidal kinetic studies. Py-MS may be useful in studies of the mode of action of antimicrobial agents, particularly in early screening of new compounds, and in rapid detection of the effects of antimicrobial agents on micro-organisms.

Anti-Bacterial Agents↗

PubMed1997

Differentiation between bacterial species and sub-species by pyrolysis mass spectrometry of extracted DNA.

Whole cell samples from cultures of Staphylococcus aureus, S. hominis, S. epidermidis and Streptococcus pyogenes were analysed by pyrolysis mass spectrometry and the results were compared with Py-MS-derived analyses of samples of DNA extracted from the same organisms. Py-MS analysis differentiated the four organisms in both circumstances. These results challenge previous assumptions that Py-MS is restricted to detecting phenotypic differences, although the basis for the differentiation of the DNA extracts has yet to be determined.

DNA, Bacterial↗

PubMed1997

Pyrolysis mass spectrometry studies on Bacillus anthracis, Bacillus cereus and their close relatives.

Pyrolysis mass spectrometry was used to examine strains of B. anthracis, of B. cereus, of B.cereus either proven to cause emetic illness or connected with outbreaks of emetic food poisoning and of B.thuringiensis. Analysis of the data-set for all strains allowed differentiation between B.anthracis, the emetic B.cereus and B.thuringiensis but B.cereus strains could not be clearly discriminated. Removal of data for the B.thuringiensis and the emetic B.cereus strains, followed by re-analysis, allowed clear separation of the B. anthracis and B. cereus groups. Furthermore, PyMS was found to be capable of discriminating between some strains of B.anthracis, and demonstrating sub-groupings of others. This work provides further evidence of the ability of PyMS to distinguish rapidly between very closely related organisms and indicates its potential in epidemiology.

Bacillus anthracis↗

PubMed2001

Evaluation of waste pyrolysis characteristics in a pressurized fluidized bed reactor.

To obtain the distribution of fuel components to gas, tar and char in a pressurized fluidized bed waste pyrolyzer, experiments were conducted with a laboratory scale fluidized bed reactor. Waste samples were fed batchwise from the top of the reactor into the fluidized bed of silica sand and pyrolyzed by nitrogen/nitrogen-O2 gas and the effects of pressure, particle size, heating rate and oxygen addition were investigated. In the case of rubber, the char yield tended to increase a little and the tar yield decrease over the pressure of 304-709 kPa. In comparison with the thermogravimetry data it was clearly demonstrated that the char yield from fluidized bed pyrolysis is much lower. A small amount of oxygen addition decreased both tar and char yields but its further increase did not affect them very much.

Air Pollution↗

PubMed2004

Novel and innovative pyrolysis and gasification technologies for energy efficient and environmentally sound MSW disposal.

Within the context of European Union (EU) energy policy and sustainibility in waste management, recent EU regulations demand energy efficient and environmentally sound disposal methods of Municipal Solid Waste (MSW). Currently, landfill with its many drawbacks is the preferred option in the EU and many other industrialised countries. Within the waste management hierarchy thermal disposal especially incineration is a viable and proven alternative. But, the dominating method, mass-burn grate incineration has drawbacks as well particularly hazardous emissions and harmful process residues. In recent years, pyrolysis and gasification technologies have emerged to address these issues and improve the energy output. To keep the many players in the field comprehensively informed and up-to-date, novel and innovative technology approaches emphasising European developments are reviewed.

Conservation of Energy Resources↗

PubMed2003

Slow pyrolysis of wood barks from Pinus brutia Ten. and product compositions.

Biomass in the form of pine bark (Pinus brutia Ten.) was pyrolysed in an externally heated fixed-bed reactor. The effects of temperature and heating rate on the yields and compositions of the products were investigated. Pyrolysis runs were performed using reactor temperatures between 300 and 500 degrees C with heating rates of 7 and 40 degrees Cmin(-1). The product yields were significantly influenced by the process conditions. The bio-oil obtained at 450 degrees C, at which the liquid product yield was maximum, was analysed. It was characterized by Fourier transform infrared spectroscopy. In addition, the solid and liquid products were analysed to determine their elemental composition and calorific value. Chemical fractionation of bio-oil showed that only low quantities of hydrocarbons were present, while oxygenated and polar fractions dominated. The empirical formula of the bio-oil with heating value of 31.03 MJkg(-1) was established as CH(1.43)O(0.332)N(0.0013).

Hot Temperature↗

PubMed2003

Pyrolysis of plant, animal and human waste: physical and chemical characterization of the pyrolytic products.

Pyrolysis (carbonization) has been proposed as one of several optional technologies for disposing and recycling waste products in Japan. Plant wastes (sugarcane bagasse and rice husks), animal waste (cow biosolids) and human waste (treated municipal sludge) were pyrolyzed at temperatures from 250-800 degrees C in closed containers. The carbonized materials were evaluated for specific physical properties (yield, surface area, density) and specific chemical properties (total carbon, total nitrogen, pH, fixed carbon, ash content, volatility) in order to compare differences in properties among the four waste products. The results indicated that (1) surface area, total carbon, ash content and pH increased as the carbonization temperature increased, while carbonization yield decreased with increasing temperature, (2) product density however was not affected by temperature and (3) correlation coefficients were determined among the physical and chemical properties and several significant correlations were observed. The data indicate that source material had considerable influence on the physical and chemical properties of the carbonized products.

Carbon↗

PubMed1991

Rapid inter-strain comparison by pyrolysis mass spectrometry of coagulase-negative staphylococci from persistent CAPD peritonitis.

Pyrolysis mass spectrometry (PyMS) was used as a method of rapid inter-strain comparison of 19 isolates of coagulase-negative staphylococci from episodes of CAPD peritonitis. Thirteen isolates were from multiple, but distinct, episodes of peritonitis in 6 patients and the remaining 6 isolates were from 6 patients with single episodes. The results, expressed in terms of identity/non-identity of strains, were compared with those obtained using an established typing system comprising an extended antibiogram, determination of biotype and plasmid profile analysis. The PyMS results for inter-strain comparison were in agreement with the reference typing scheme results. PyMS can be used in this setting to rapidly obtain evidence that persistent infection is/is not likely to be due to the same organism, although it cannot be used for formal typing. The results by both methods showed that serial, apparently distinct, episodes of peritonitis over periods as long as 120 days may be due to the same strain of coagulase-negative staphylococcus. Clinically based distinctions between recurrence of infection (same strain) and re-infection (different strains) may not always be supported by the microbiological evidence.

Coagulase↗

PubMed1991

Incrimination of an environmental source of a case of Legionnaires' disease by pyrolysis mass spectrometry.

Following a case of Legionnaires' disease Legionella pneumophila of the same serogroup was isolated from the hot water system of the hotel which had been epidemiologically implicated as the source of the infection. Pyrolysis mass spectrometry (PyMS) was used to compare 11 isolates from the hotel water sample with the patient's strain. Epidemiologically unrelated isolates, both clinical and environmental, of the same serogroup and monoclonal antibody type of L. pneumophila were included in the same analysis, together with relevant reference strains. The patient strain was shown to be indistinguishable from seven of the hotel water isolates, but clearly different from other unrelated clinical isolates, the reference strains and some of the other environmental isolates. PyMS is a rapid and cheap method for inter-strain comparison for L. pneumophila.

Aged↗

PubMed1995

Sporadic isolates of Escherichia coli O157.H7 investigated by pyrolysis mass spectrometry.

Thirty-six encoded isolates of Escherichia coli. 32 of which were of serotype O157, were examined by pyrolysis mass spectrometry (PyMS). Thirty-one of the serotype O157 isolates possessed the flagellar antigen H7 and produced Verocytotoxin (VT), the other isolate serotyped as H45 and was non-toxigenic. Eighteen of the VT-producing E. coli (VTEC) isolates were from sporadic disease in residents of the Northern Region. Standard principal component (PC) and canonical variate (CV) analysis of the data distinguished only the four non-O157 isolates from the remainder which were indistinguishable by this approach. A similarity matrix based on differences between individual CV means distinguished a further ten isolates. The matrix correctly clustered 2 pairs of isolates from siblings and 4 isolates from an affected family. A further 5 clusters of 3 or more isolates and 6 pairs of isolates were defined. These groupings proved to be homogenous for toxin phenotype but occasionally entrained isolates of dissimilar phage type. However, in general, PyMS-derived clustering of apparently sporadic isolates accorded with geographical locations as determined by postcode. PyMS, which is a quick and high volume capacity phenotypic technique, may be a useful addition to existing methods in the investigation of the epidemiology of sporadic VTEC disease.

Escherichia coli↗

PubMed2001

Sulfur and oxygen isotope analysis of sulfate at micromole levels using a pyrolysis technique in a continuous flow system.

The discovery of a mass-independent isotopic composition (delta17O = (delta17O - 0.512 * delta18O) no equal to 0) in aerosol sulfate and the identification of its origin (aqueous-phase oxidation by 03 and H2O2) have renewed interest in measuring the oxygen isotopic content of sulfate. In this paper, we present a new method to measure both delta17O and delta18O in SO4, with the possibility of sulfur isotope analysis on the same sample. The technique takes advantage of the easy pyrolysis of Ag2SO4 to SO2, O2, and Ag metal in a continuous flow system. Because the technique is not quantitative in oxygen (yield approximately 45% for O2), a calibration is needed. Correction factors of +0.87 and +0.44% were obtained for delta18O and delta17O, respectively. A technique to convert micromole levels of sulfate in any form to silver sulfate is described. To reach this goal, a solid electrolyte (Nafion membrane) is used in an electrolysis apparatus. Reproducibilities for micromole sample sizes are (1sigma) 0.5, 0.3, and 0.1% for delta18O, delta17O, and delta17O, respectively. No memory effects or isotopic exchange during the treatment of the sample is observed. The main advantages of this new method over the existing ones are no fluorinating agent is needed, both oxygen and sulfur isotopes can be measured on the same sample, only very small amounts of sulfate are needed (down to 100 microg (1 micromol)), it is relatively fast and inexpensive, and the possibility exists to couple this technique to an on-line analysis.

Journal Article↗

PubMed2005

Multidimensional detection of nitroorganic explosives by gas chromatography-pyrolysis-ultraviolet detection.

We describe a new methodology for the trace detection of organic explosives containing nitro functionalities. Conventional gas chromatography separates the components of an explosive mixture. Effluent from the gas chromatograph is pyrolyzed by passage over a heated Nichrome wire. Nitric oxide produced on pyrolysis of a nitroorganic compound is then detected by ultraviolet absorption spectroscopy between 180 and 240 nm, using a deuterium lamp as the light source. Nitric oxide exhibits a sharply banded, characteristic spectrum in this region, enabling detection of nitroorganics. The system is tested using the explosive simulants nitrobenzene and 2,4-dinitrotoluene, and with the nitramine explosive tetryl. Detection limits are 25 ng for nitrobenzene and 50 ng for 2,4-dinitrotoluene. Tetryl is detected with a detection limit of 50 ng. The system is both easy to implement and could be built as a compact, low-power device.

Journal Article↗

PubMed2005

Characterization of synthetic polymers by electrospray-assisted pyrolysis ionization-mass spectrometry.

Rapid characterization of synthetic polymers based on the differences in the appearance of the polar pyrolysate ions was achieved by electrospray-assisted pyrolysis ionization-mass spectrometry. The pyrolytical products produced by a commercial Curie point pyroprobe were conducted to the tip of a capillary, where charged methanol droplets were generated continuously by electrospray. Polar components in the pyrolysates may react directly with the protonated methanol ions or fuse with the charged methanol droplets; electrospray ionization proceeds from the fused droplets to generate protonated analyte ions. The mass spectra obtained through this approach were used to rapidly distinguish the polymer standards that differ in the nature of building units, degrees of polymerization, and copolymerization coefficients.

Journal Article↗

PubMed1999

Differentiation of microorganisms based on pyrolysis-ion trap mass spectrometry using chemical ionization.

The ability to differentiate microorganisms using pyrolysision trap mass spectrometry was demonstrated for five Gram-negative disease-causing organisms: Brucella melitensis, Brucella suis, Vibrio cholera, Yersinia pestis, and Francisella tularensis. Bacterial profiles were generated for gamma-irradiated bacterial samples using pyrolytic methylation and compared for electron ionization and chemical ionization using several liquid reagents with increasing proton affinities. Electron ionization combined with pyrolysis caused extensive fragmentation, resulting in a high abundance of lower mass ions and diminishing the diagnostic value of the technique for compound identification and bacterial profiling. Chemical ionization reduced the amount of fragmentation due to ionization while enhancing the molecular ion region of the fatty acids. As the proton affinity of the reagent increased, the protonated molecular ions of the fatty acids became the predominant ions observed in the mass spectrum. As a result, chemical ionization was shown to be more effective than electron ionization in bacterial profiling. Whereas the bacteria could be distinguished at the Genera level using electron ionization, further differentiation to the subspecies level was possible using chemical ionization. The greatest separation among the five test organisms, in terms of Euclidean distances, was obtained using ethanol as the chemical ionization reagent and using pooled masses representing specific fatty acid biomarkers rather than total ion profiles.

Fatty Acids↗

PubMed2003

Mechanisms of dioxin formation from the high-temperature pyrolysis of 2-bromophenol.

Brominated hydrocarbons are the most commonly used flame retardants. Materials containing brominated hydrocarbons are frequently disposed in municipal and hazardous waste incinerators as well as being subjected to thermal reaction in accidental fires. This results in the potential for formation of brominated dioxins and other hazardous combustion byproducts. In contrast to chlorinated hydrocarbons, the reactions of brominated hydrocarbons have been studied only minimally. As a model brominated hydrocarbon that may form brominated dioxins, we studied the homogeneous, gas-phase pyrolytic thermal degradation of 2-bromophenol in a 1-cm i.d., fused-silica flow reactor at a concentration of 90 ppm, with a reaction time of 2.0 s, and over a temperature range of 300 to 1000 degrees C. Observed products included dibenzo-p-dioxin (DD), 1-monobromodibenzo-p-dioxin (1-MBDD), 4-monobromodibenzofuran (4-MBDF), dibenzofuran (DF), naphthalene, bromonaphthalene, 2,4- and 2,6-dibromophenol, phenol, bromobenzene, and benzene. These results are compared and contrasted with previous results reported for 2-chlorophenol. At temperatures lower than 700 degrees C, formation of 2-bromophenoxyl radical, which decomposes through CO elimination to form a bromocyclopentadienyl radical, forms naphthalene and 2-bromonaphthalene through radical recombination/rearrangement reactions. However, unlike the results for 2-chlorophenol, where naphthalene is the major product, DD becomes the major product for the pyrolysis of 2-bromophenol. The formation of DD and 1-MBDD are attributed to radical-radical reactions involving 2-bromophenoxyl radical with the carbon- (bromine) centered radical and the carbon- (hydrogen) centered radical mesomers of 2-bromophenoxyl radical, respectively. The potential product, 4,6-dibromodibenzofuran (4,6-DBDF) for which the analogous product, 4,6-dichlorodibenzofuran (4,6 DCDF), was observed in the oxidation of 2-chlorophenol, was not detected. This is attributed to the pyrolytic conditions of our experiments (e.g., shorter reaction times and higher temperatures) that favor reaction intermediates that form DD and 1-MBDD.

Dioxins↗

PubMed2004

Complete study of the pyrolysis and gasification of scrap tires in a pilot plant reactor.

The pyrolysis and gasification of tires was studied in a pilot plant reactor provided with a system for condensation of semivolatile matter. The study comprises experiments at 450, 750, and 1000 degrees C both in nitrogen and 10% oxygen atmospheres. Analysis of all the products obtained (gases, liquids, char, and soot) are presented. In the gas phase only methane and benzene yields increase with temperature until 1000 degrees C. In the liquids the main components are styrene, limonene, and isoprene. The solid fraction (including soot) increases with temperature. Zinc content of the char decreases with increasing temperature.

Benzene↗

PubMed2005

Surface-mediated formation of polybrominated dibenzo-p-dioxins and dibenzofurans from the high-temperature pyrolysis of 2-bromophenol on a CuO/silica surface.

We studied the surface-mediated pyrolytic thermal degradation of 2-bromophenol, a model brominated hydrocarbon that may form brominated dioxins in combustion and thermal processes, on silica-supported copper oxide in a 1 mm i.d., fused silica flow reactor at a constant concentration of 88 ppm over a temperature range of 250-550 degrees C. Observed products included dibenzo-p-dioxin (DD), 1-monobromodibenzo-p-dioxin (1-MBDD), dibromo-dibenzo-p-dioxin (DBDD),tribromodibenzo-p-dioxin (TrBDD), 4-monobromodibenzofuran (4-MBDF), dibenzofuran (DF), 2,4,6-tribromophenol, 2,4- and 2,6-dibromophenol, and polybrominated benzenes. These results are compared and contrasted with previous work on surface-catalyzed pyrolysis of 2-chlorophenol. Polybrominated dibenzofurans (PBDFs) are formed by the Langmuir-Hinshelwood mechanism, and the formation of polybrominated dibenzo-p-dioxins (PBDDs) is through an Eley-Rideal mechanism. Yields of PBDDs are at least 16x greater for 2-bromophenol than for analogous PCDDs from 2-chlorophenol. Higher yields of polybrominated phenols and polybrominated benzenes are also observed. This can be attributed to the relative ease of bromination over chlorination and the higher concentration of bromine atoms in the 2-bromophenol system versus chlorine atoms for the 2-chlorophenol system.

Benzofurans↗

PubMed2002

Polyferrocenylsilane microspheres: synthesis, mechanism of formation, size and charge tunability, electrostatic self-assembly, and pyrolysis to spherical magnetic ceramic particles.

Pt(0)-catalyzed ring-opening precipitation copolymerization of [1]silaferrocenophanes fcSiMe(2) (3) and the spirocyclic cross-linker fcSi(CH(2))(3) (4) (fc = Fe(eta(5)-C(5)H(4))(2)) was used to prepare polyferrocenylsilane microspheres (PFSMSs) under mild conditions. By varying the reaction conditions, a wide variety of other morphologies was obtained. The effects of temperature, monomer ratio, solvent composition, catalyst concentration, and time on the observed morphology were investigated and interpreted in terms of a mechanism for microsphere formation. The most well-defined particles were formed using equimolar amounts of 3 and 4, in a 50:50 mixture of xylenes and decane at 60 degrees C with gentle agitation. Chemical oxidation of the polymeric microspheres led to positively charged particles (OPFSMSs) which underwent electrostatically driven self-assembly with negatively charged silica microspheres to form core-corona composite particles. Redox titration with controlled amounts of the one-electron oxidant [N(C(6)H(4)Br-p)(3)][PF(6)] in acetonitrile led to the oxidation of the outer 0.15 microm (ca. 32%) of the PFSMSs. The resulting OPFSMSs were reduced back to their neutral form by reaction with hydrazine in methanol. Pyrolysis of the PFSMSs led to spherical magnetic ceramic replicas with tunable magnetic properties that organize into ordered 2-D arrays at the air-water interface under the influence of a magnetic field.

Journal Article↗