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PubMed1997

[Structural identification of carboxylic esters by pyrolysis gas chromatography].

A pyrolysis gas chromatographic method has been investigated for structural identification of carboxylic esters. The method can be applied to identify not only pure components, but also those separated by thin layer chromatography and scraped from the TLC plate without removing the adsorbent. The samples were pyrolyzed in tube furnace pyrolyzer at 500 degrees C (conventional pyrolysis) or were pyrolyzed at 550 degrees C after mixing with soda-lime powder (pyrolysis with soda-lime). Some esters such as iso-octyl palmitate, glycerol monostearate and diethyl phthalate were pyrolyzed. The pyrolysis products were identified by comparing with the known. The parent alcohols of monohydric and polyhydric alcohol esters can be determined respectively according to alcohols, alkenes produced on pyrolysis and dehydrated products of polyhydric alcohol at high temperature. The parent acids of monocarboxylic esters can be determined according to carboxylic acid produced on conventional pyrolysis or corresponding alkane formed from decarboxylation of parent acids on pyrolysis with soda-lime. For esters formed from dicarboxylic acids that can be dehydrated to produce five-, six-membered cyclic ketones or can be dehydrated and decarboxylated simultaneously to produce five-, six-membered cyclic acid anhydrides, parent acids can be determined according to corresponding cyclic ketones or cyclic acid anhydrides. This method is useful for identification of common carboxylic esters. When the compound or the component of the mixture was confirmed to contain ester-group by infra-red spectroscopy, PGC or TLC-PGC can be employed to make further identification.

Carboxylic Acids↗
PubMed1990

Abuse of smoking methamphetamine mixed with tobacco: II. The formation mechanism of pyrolysis products.

The pyrolysis products of smoking methamphetamine mixed with tobacco were determined by gas chromatography (GC) and GC/mass spectrometry (GC/MS) methods. The mainstream smoke contained methamphetamine (14.5% of the initial methamphetamine), phenylacetone (3.1%). N-cyanomethylmethamphetamine (1.9%), trans-beta-methylstyrene (1.7%), N-formylmethamphetamine (1.5%), and other products (each less than 1%). The amount of each pyrolysis product in the sidestream smoke was less than that in the mainstream smoke by a factor of over 5, except for methamphetamine (10.5%) and N-formylmethamphetamine (1.4%). The formation mechanism of these products was investigated, by use of a pyrolyzer, from the standpoint of the material, pyrolysis temperature, and pyrolysis atmosphere. Although several products (for example, dimethylamphetamine and trans-beta-methylstyrene) were formed by thermal self-decomposition of methamphetamine alone, most of the products, except N-cyanomethylmethamphetamine, were formed chiefly by the thermal reaction of methamphetamine with cigarette components. The formation of N-cyanomethylmethamphetamine required air and a high pyrolysis temperature. Air and a high pyrolysis temperature generally accelerated the formation of the pyrolysis products.

Chromatography, Gas↗
PubMed1995

Effects of cocaine, cocaine metabolites and cocaine pyrolysis products on the hindbrain cardiac and respiratory centers of the rabbit.

Hemodynamic and respiratory effects of vertebral artery or i.v. administration of cocaine, cocaine metabolites and cocaine pyrolysis products were measured in anesthetized rabbits. Vertebral artery administration of 1 mg of cocaine produced decreases in blood pressure and heart rate and respiratory arrest. Cocaethylene (1 mg), a cocaine metabolite produced following co-administration of cocaine and ethanol, had comparable effects except that the respiratory arrest following cocaethylene had a longer duration of action than did cocaine. A decrease in blood pressure was also observed following 1 mg of norcocaine; however, unlike cocaine, norcocaine did not affect respiration. Acute tolerance was not observed to any of the effects of 1 mg of cocaine, cocaethylene or norcocaine following vertebral artery administration. None of these compounds had significant effects following i.v. administration of the same dose. The cocaine metabolites benzoylecgonine and ecgonine methyl ester were without effect by either route in doses up to 3 mg. In contrast to cocaine, the cocaine pyrolysis products anhydroecgonine methyl ester (3 mg) and noranhydroecgonine methyl ester (3 mg) produced similar effects via both routes of administration. Both compounds produced decreases in blood pressure and heart rate and an increase in respiratory rate. Anhydroecgonine ethyl ester (3 mg), a metabolite hypothetically formed from the cocaine pyrolysis product in individuals co-administering ethanol, had effects similar to the other pyrolysis products, although its effects were not as prominent via the i.v. route of administration. Acute tolerance was observed upon administration of the cocaine pyrolysis products. These results indicate that the cocaine pyrolysis products do not share a common mechanism of action with either cocaine or the cocaine metabolites.

Animals↗
PubMed2001

Gas chromatographic study of the volatile products from co-pyrolysis of coal and polyethylene wastes.

The aim of this study was to determine the volatile products distribution of co-processing of coal with two plastic wastes, low-density polyethylene from agriculture greenhouses and high-density polyethylene from domestic uses, in order to explain the observed decrease in coal fluidity caused by polyethylene waste addition. Polymeric materials, although they are not volatile themselves, may be analysed by gas chromatography through the use of pyrolysis experiments. In this way, a series of pyrolysis tests were performed at 400 and 500 degrees C in a Gray-King oven with each of the two plastic wastes, one high-volatile bituminous coal and blends made up of coal and plastic waste (9:1, w/w, ratio). The pyrolysis temperatures, 400 and 500 degrees C, were selected on the basis of the beginning and the end of the coal plastic stage. The organic products evolved from the oven were collected, dissolved in pyridine and analysed by capillary gas chromatography using a flame ionization detector. The analysis of the primary tars indicated that the amount of n-alkanes is always higher than that of n-alkenes and the formation of the alkenes is favoured by increasing the pyrolysis temperature. However, this effect may be influenced by the size of the hydrocarbon. Thus, the fraction C17-C31 showed a higher increase of n-alkenes/n-alkanes ratio than other fractions. On the other hand, the difference between the experimental and estimated values from tars produced from single components was positive for n-alkanes and n-alkenes, indicating that co-pyrolysis of the two materials enhanced the chemical reactivity during pyrolysis and produced a higher conversion than that from individual components.

Alkanes↗
PubMed1998

Laser pyrolysis products: sampling procedures, cytotoxic and genotoxic effects.

The use of lasers in medical applications has grown enormously in the last few years. Recent chemical analysis of the laser pyrolysis products revealed that aerosols generated by pyrolytic decomposition of tissue could be health hazards. Therefore we analysed the genotoxic and mutagenic effects of laser pyrolysis products from different types of porcine tissue. The tissues were irradiated with a surgical CO2 laser and the generated aerosols were sampled as particulate fractions as well as low and highly volatile fractions. Then human leukocytes were incubated with the pyrolysis products and subjected to the comet assay. The results of the comet assay indicated the pyrolysis products being inducers of DNA damage. The ability to induce genotoxic effects turned out to be strongly dependent on the type of tissue that had been irradiated during laser treatment. To check whether the pyrolysis products also have mutagenic properties the Salmonella mutagenicity assay was performed. The particulate aerosol fractions of skin, muscle tissue and liver tissue clearly proved to be mutagenic in TA98 in the presence of S9 mix. There was no mutagenic effect detectable without metabolic activation. In conclusion, our experiments showed that the laser pyrolysis products originating from porcine tissues induced very potent genotoxic as well as mutagenic effects and therefore they could be potential health hazards for humans.

Adipose Tissue↗
PubMed2002

Characterization of char from the pyrolysis of tobacco.

Pyrolysis of tobacco was studied in oxidative and nonoxidative (inert) environments at atmospheric pressure and temperatures ranging from 150 to 750 degrees C. The objective was to study the effect of pyrolysis conditions on the characteristics of the solid residue, i.e., char. The char was characterized using cross-polarization (13)C nuclear magnetic resonance (CPMAS NMR), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), the Brunauer-Emmett-Teller (BET) surface area, and the elemental composition. The char yield from pyrolysis (i.e., nonoxidative) decreased sharply with an increase in temperature to ca. 22% (dry, ash-free basis) at high temperatures. In oxidative pyrolysis, i.e., in 5% oxygen, the char was completely oxidized above 600 degrees C. The gaseous product from pyrolysis at high temperatures contained a significant concentration of hydrogen. The surface area of the char was low, with a maximum of 8 m(2)/g at 400 degrees C. SEM analysis indicated that pyrolysis of the tobacco led to a gradual accumulation of inorganic crystals on the exposed surfaces, and some constituents also melted, resulting in the formation of vesicles by evolving gas. NMR analysis showed significant changes in pectin and sugar constituents of the tobacco and breaking of glycosidic bonds of cellulose at 300-500 degrees C before the char became predominantly aromatic at high temperatures. FTIR results showed a continuous decrease in the intensity of the OH stretch with temperature and the aromatic character to be at maximum at 550-650 degrees C. The H/C ratio of the char decreased continuously with temperature, while the O/C ratio became constant above 300 degrees C due to the presence of oxides and carbonates in the char. The results are consistent with the analysis of the evolved gases.

Hot Temperature↗
PubMed1971

Pyrolysis of organomercury compounds: investigation by the method of matrix isolation.

The method of matrix isolation has been used to investigate mechanisms of gas-phase chemical reactions, in particular the pyrolysis of some organomercury compounds. A molecular beam of pyrolysis products was condensed simultaneously with a large excess of rare gas at temperatures from 5 to 15 degrees K to form a matrix that was subsequently studied by infrared spectroscopy. In the case of C(6)H(5)HgCCl(3), we found that pyrolysis in the temperature range 220-400 degrees C produced mainly dichlorocarbene. In addition, some trichloromethyl radical was observed and increased in relative importance at increased temperatures. Another identified product of pyrolysis was C(6)H(5)HgCl. In general, the same reactive intermediates, CCl(2) and CCl(3), were found from pyrolysis of Hg(CCl(3))(2) in the temperature range 250-500 degrees C, along with CCl(3)HgCl and HgCl(2). The identity of CCl(2) and CCl(2) was demonstrated by measurement of the relative intensities and isotopic splittings of stretching vibrations due to the chlorine isotopes. Isotopic patterns found for CCl(2) are: v(3) (745.8, 744.0, 741.8 cm(-1)), v(1) (719.5, 717.0, 714.9 cm(-1)) and for CCl(3) are: v(3) (897.8, 896.4, 895.2, 893.9 cm(-1)). Less dilution with the rare gas or warming of the matrix produced a decrease of CCl(2) and CCl(3) spectral bands and an increase of bands due to C(2)Cl(4), C(2)Cl(6), and other products. These results show the usefulness of matrix isolation in the study of such reactive species as CCl(2) produced by pyrolysis in the gas phase.

Journal Article↗
PubMed1979

Pyrolysis products from amino acids and protein: highest mutagenicity requires cytochrome P1-450.

Pyrolysis products of proteins and amino acids are highly mutagenic, but metabolism of these chemicals by rat liver subcellular fractions is known to be required for production of the mutagenic intermediates. We examined the mutagenesis of seven purified pyrolysis products from tryptophan, lysine, glutamic acid, and soybean globulin with Salmonella typhimurium strain TA98 in the presence of liver fractions from genetically "responsive" C57BL/6N and Ah(b)/Ah(d) or "nonresponsive" DBA/2N and Ah(d)/Ah(d) mice that had been pretreated in vivo with benzo[a]pyrene. For all pyrolysis products tested, mutagenesis is 2-fold to more than 1000-fold greater with C57BL/6N and Ah(b)/Ah(d) than with DBA/2N or Ah(d)/Ah(d) liver fractions. A sucrose density gradient assay for detecting the Ah regulatory gene product, the receptor, was studied with C57BL/6N hepatic cytosol. At levels 100 times in excess of [1,6-(3)H]2,3,7,8-tetrachlorodibenzo-p-dioxin, nonlabeled 2,3,7,8-tetrachlorodibenzo-p-dioxin, 3-methylcholanthrene, and beta-naphthoflavone (inducers of cytochrome P(1)-450) are able to displace the radioligand from its hepatic cytosolic receptor; four pyrolysates from tryptophan, glutamic acid, and soybean globulin did not have this capacity. These data indicate that the pyrolysis products tested, although not effective as inducers of cytochrome P(1)-450, are most mutagenic when metabolized by P(1)-450. Potent P(1)-450 inducers-present in pyrolysates during the combustion process-might be present in quantities insufficient to initiate mutagenesis or carcinogenesis but might have a synergistic action, or act as "comutagens" or "cocarcinogens," with the N-containing heterocyclic pyrolysis products. A quantitative relationship between mutagenic and carcinogenic potency of these pyrolysis products remains, however, to be demonstrated.

Amino Acids↗
PubMed2006

Slow-pyrolysis and -oxidation of different biomass fuel samples.

Pyrolysis and oxidation characteristics of some biomass samples such as almond shell, walnut shell, hazelnut shell, tobacco waste, and rapeseed were investigated using Thermogravimetric Analysis (TGA) technique under slow heating conditions (20 K/min) from ambient to 1173 K. Pyrolysis experiments were carried out under dynamic nitrogen atmosphere of 40 mL/min. Dry air was used at the same rate in the oxidation experiments. The rates of mass losses from the biomass samples regarding temperature were obtained from the Differential Thermogravimetric Analysis (DTG) curves, and these rates were interpreted according to the pyrolysis and oxidation characteristics of the biomass samples. Since the heating rate was relatively very slow, individual peaks on the DTG curves resulting from the pyrolysis or oxidation of the major constituents that forming the complex structure of the biomass samples could be survived and distinguished from the thermograms. The maximum rates of mass losses (dm/dt)max from the oxidation experiments were determined to be higher than those from the pyrolysis experiments. On the other hand, the (dm/dt)max values were determined at about 550 K for pyrolysis, whereas they were below 500 K in case of oxidation irrespective of the type of the biomass samples.

Biomass↗
PubMedDate not supplied

Inhalation efficiency of free-base cocaine by pyrolysis of 'crack' and cocaine hydrochloride.

The inhalation efficiency and pyrolysis products of cocaine by the pyrolysis of crack and cocaine hydrochloride at various temperatures are described. The inhalation efficiency of cocaine by the pyrolysis of crack was 73 +/- 9% and 62 +/- 11% at 170 degrees C and 220 degrees C, respectively. When crack was heated at over 225 degrees C, the higher temperature resulted in a lower inhalation efficiency of cocaine. In that case, more methylecgonidine was produced. Furthermore, in the pyrolysis of crack, the lower concentration of cocaine in crack resulted in a lower inhalation efficiency of cocaine. The major pyrolysis product of cocaine HCl was a mixture of alpha, beta, gamma, and delta-carbomethoxycyclo-heptatrienes, and the major pyrolysis product of crack was methylecgonidine. This study proposes a new method of discrimination between cocaine HCl and crack by GC or GC/MS with a curie point pyrolyzer.

Administration, Inhalation↗
PubMed2000

[Identification of synthetic adhesives by simultaneous pyrolysis methylation gas chromatography].

At present, pyrolysis gas chromatography (Py-GC) is an effective analytical method for trace synthetic adhesives. Synthetic adhesives are usually composed of polar components. Thus, the polar pyrolysis products are normally difficult to measure by Py-GC due to their partial or complete adsorption in the pyrolysis zone, injection system or capillary column and the accuracy of results is seriously affected. Simultaneous pyrolysis methylation gas chromatography (Py-Me-GC) is a fast analytical method which was developed in recent years for polar compounds. The five synthetic adhesives have been identified by using Py-Me-GC in our study. Analytical conditions were: filament pyrolysis apparatus, flame ionization detector (FID), gas chromatograph, FFAP capillary column (30 m x 0.25 mm i.d.) and a quaternary ammonium salt as methylating agent. Major peaks of the products of pyrolysis were analysed qualitatively by GC/MS and comparisons were also made between the results by Py-Me-GC and those by Py-GC. The information gained from the components of substances by Py-Me-GC is more than that by Py-GC. The method is suitable for identifying synthetic adhesives of trace evidence in forensic science.

Adhesives↗
PubMed2004

Pyrolysis of EVA and its application in recycling of photovoltaic modules.

The basic pyrolysis behaviour of ethylene vinyl acetate (EVA) copolymer, which is often used as a lamination agent in solar modules, was investigated in thermogravimetry, differential thermal analysis(DTA) and thermovolumetry. The TG analysis showed that the EVA pyrolysis can be accelerated under the partial oxidizing atmosphere but the end pyrolysis temperature must be higher than in nitrogen, to eliminate the coke formed. Meanwhile, a strong exothermal peak occurs at about 450 degrees C under the air condition and gets weaker obviously at the oxygen content lower than 10 vol. %. The mass balance of EVA pyrolysis was given through the thermovolumetry with the output of 10 wt. % permanent gas, 89.9 wt. % condensate and 0.1% residual coke. Besides, the composition of the permanent gas and condensate at different pyrolysis stages were analysed and interpreted on the known pyrolysis mechanism.

Conservation of Energy Resources↗
PubMed2000

Pyrolysis-gas chromatography/mass spectrometry of a coal extract and its fractions separated by planar chromatography: correlation of structural features with molecular mass

The structural characterisation of a coal liquefaction extract and its three fractions separated by planar chromatography has been described. Size exclusion chromatography showed the molecular mass distributions to become progressively larger with decreasing mobility on the plate. UV-fluorescence spectroscopy of the fractions indicated parallel increases in the sizes of polynuclear aromatic ring systems. Analysis by probe-mass spectrometry of the 'whole' coal extract showed the expected array of small polynuclear aromatic groups extending to m/z 450. The probe mass spectra of the lightest fraction ('mobile in pyridine and acetonitrile') showed similar features, except for effects due to vacuum drying to remove solvent. In sharp contrast, the two heaviest fractions ('mobile in pyridine and immobile in acetonitrile' and 'immobile in pyridine') showed no significant ions other than those from residual NMP solvent (m/z 98 and 99). Pyrolysis-gas chromatography/mass spectrometry of these two heaviest fractions showed only traces of aromatic compounds or fragments. The aromatic pyrolysis products of these fractions were too large and involatile to pass through the GC column. The major components observed in the pyrolysis-gas chromatography/mass spectrometry of the two heavy fractions were alkanes and alkenes, ranging between C10-C25. Since none of the samples contained free alkanes, alkenes or cycloalkanes before pyrolysis, they were generated during the pyrolysis step. The shifts of UV-fluorescence spectral intensity to shorter wavelengths with decreasing size indicated by size exclusion chromatography (SEC) provide direct evidence of differences in structure with changing molecular mass. This evidence strongly suggests that species identified as being of large molecular mass in this extract sample are not composed of molecular aggregates. It remains difficult to establish whether and when it would be legitimate to invoke molecular aggregates to explain the large molecular masses (MMs) identified here and in other work. Copyright 2000 John Wiley & Sons, Ltd.

Journal Article↗
PubMed1995

Resolution of batch variations in pyrolysis mass spectrometry of bacteria by the use of artificial neural network analysis.

A simple, but stringent, three group model of bacterial interstrain identity (two cultures of the same strain of Escherichia coli) and difference (a culture of a serologically distinct strain) was used in multiple serial weekly subcultures for five weeks to demonstrate the effect of both growth-related (phenotypic) and machine-related variation on pyrolysis mass spectra. An aliquot of serum from a single sample was included in each pyrolysis batch to distinguish machine drift from culture drift. Conventional principal component (PC) canonical variate (CV) analysis was successful within each pyrolysis batch but the variations between batches precluded the use of data from more than one batch in successful PCCV analysis. In contrast, artificial neural networks (ANNs) trained with data from one batch could be successfully used to identify groups in data from non-contemporaneous pyrolysis batches. Although the ANN method will require validation in more complex settings than this simple model, it is a promising approach to the problem of batch constraint in pyrolysis mass spectrometry.

Bacterial Typing Techniques↗
PubMed2006

Production of bio-fuels by high temperature pyrolysis of sewage sludge using conventional and microwave heating.

The pyrolysis of sewage sludge was investigated using microwave and electrical ovens as the sources of heat, and graphite and char as microwave absorbers. The main objective of this work was to maximize the gas yield and to assess its quality as a fuel and as a source of hydrogen or syngas (H2 + CO). Both gases were produced in a higher proportion by microwave pyrolysis than by conventional pyrolysis, with a maximum value of 38% for H2 and 66% for H2 + CO. The oils obtained were also characterized using FTIR and GC-MS. The use of conventional electrical heating in the pyrolysis of sewage sludge produced an oil that could have a significant environmental and toxicological impact. Conversely, microwave pyrolysis still preserved some of the functional groups of the initial sludge such as aliphatic and oxygenated compounds, whereas no heavy PACs were detected.

Bioelectric Energy Sources↗
PubMed2005

Retention indices as identification tool in pyrolysis-capillary gas chromatography.

Pyrolysis-capillary gas chromatography (Py-cGC) represents important method to identify the analytes in the mixture after thermal degradation. This combines high effective analyte separation on-line coupled with thermal degradation process that depends on analyte structure. System of retention indices has been used for identification of the analytes after on-line pyrolysis and chromatographic separation. The pyrolysate composition has been studied during thermal degradation of polymethylmethacrylate (PMMA) at different pyrolysis temperatures and chromatographic column conditions. Homologues series of n-alkanes have been used for calculation of pyrolysate Kováts retention indices (I) and compared with mass spectrometric (MS) data of pyrolysate model mixture. To identify PMMA thermal degradation products the high density polyethylene (HDPE) as additive standard producing triplets of the olefin homologous series during co-pyrolysis has been used. These homologous series enable to calculate programmed temperature retention indices (ITPGC) to identify the analytes present in the pyrolysate. Calculated I values were compared with published I values databases to identify analytes yielded at different pyrolysis temperatures.

Chromatography, Gas↗
PubMed2006

Analysis of Titan tholin pyrolysis products by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry.

The reddish brown haze that surrounds Titan, Saturn's largest moon, is thought to consist of tholin-like organic aerosols. Tholins are complex materials of largely unknown structure. The very high peak capacity and structured chromatograms obtained from comprehensive two-dimensional GC (GC x GC) are attractive attributes for the characterization of tholin pyrolysis products. In this report, GC x GC with time-of-flight MS detection and a flash pyrolysis inlet is used to characterize tholin pyrolysis products. Identified pyrolysis products include low-molecular-weight nitriles, alkyl substituted pyrroles, linear and branched hydrocarbons, alkyl-substituted benzenes and PAH compounds. The pyrolysis of standards found in tholin pyrolysate showed that little alteration occurred and thus these structures are likely present in the tholin material.

Aerosols↗
PubMed2004

Two possible pathways for the release of arsenic during pyrolysis of chromated copper arsenate (CCA)-treated wood.

The behavior of arsenic during pyrolysis at temperatures between 135 and 500 degrees C has been widely studied. We examined the release of arsenic during the pyrolysis of chromated copper arsenate (CCA)-treated wood, and here we propose two models for the volatilization of arsenic: (a) a reacted arsenic compound, chromium arsenate, in CCA-treated wood was initially decomposed to arsenic pentoxide, which then appeared to be released at around 400-500 degrees C as a form of arsenic trioxide; and (b) an unreacted arsenic compound, arsenic pentoxide, in CCA-treated wood was released at much lower temperatures than reacted arsenic compound, as a form of arsenic trioxide. In order to restrain the release of arsenic during pyrolysis, it is possible to pyrolyze CCA-treated wood carefully at temperatures around 300-350 degrees C only if the wood contains little unreacted arsenic compound. Under these conditions, almost all toxic elements remain in the pyrolysis residue, and a weight reduction of the wood of approximately 50% can be obtained. On the other hand, the release of arsenic can be achieved easily using an unreacted arsenic compound under the same pyrolysis conditions. However, in the present study it was difficult to determine the accurate release point of arsenic in both cases due to the level of experimental uncertainty.

Arsenic↗