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PubMed1982

Mutagenicity of pyrolysates from guanidine, ureide, secondary amines and polyamines found by the Salmonella/mammalian-microsome test.

Nitrogenous compounds such as guanidine, ureide, secondary amines and polyamines were pyrolysed at 300, 400, 500 and 600 degrees C for 3 min, and the mutagenic activities of the pyrolysates were assayed on Salmonella typhimurium TA98 and TA100 with or without metabolic activation by S9 mix. Among 21 pyrolysates tested, 14, from methylguanidine, agmatine, dihydrouracil, dimethylamine, diethylamine, trimethylamine, triethylamine, pyrrolidine, morpholine, sarcosine, piperazine, piperidine, spermine and spermidine, showed mutagenic activity. In the presence of S9 mix, the mutagenic activity began to appear from the pyrolysate at 400 degrees C, and the pyrolysate at 600 degrees C showed the highest mutagenic activity except that from methylguanidine. The mutagenic activity formed by pyrolysis was more active on TA98 than TA100. In the absence of S9 mix, only 3 pyrolysates - from dimethylamine, diethylamine and pyrrolidine - showed slight mutagenic activity toward TA100. The highest mutagenic activity was observed with the pyrolysate from spermine, followed by those from piperidine, spermidine, piperazine and triethylamine. Some nitrogenous compounds showed slight mutagenic activity after pyrolysis at 300 degrees C for 20 min, although none of the compounds tested showed any mutagenic activity after pyrolysis at 300 degrees C for 3 min.

Amines↗

PubMed2006

Catalytic destruction of brominated aromatic compounds studied in a catalyst microbed coupled to gas chromatography/mass spectrometry.

The capability of solid porous catalysts has been studied for the destruction or modification of halogenated aromatic compounds contaminating the pyrolysis oil of recycled plastics from electronic waste. A fast and simple experimental procedure is carried out using a micropyrolyser coupled to GC-MS in such a way that catalyst microbed was placed in the sample tube of the pyrolyser. The pyrolysis products of polycarbonate blended with a frequently applied flame retardant tetrabromobisphenol A (TBBPA) and epoxy resin containing TBBPA monomer units have been analysed, and the brominated components were compared with the thermal decomposition products of TBBPA and its diallyl ether. When TBBPA vapour passes through molecular sieve 4A a slight debromination and a partial cleavage of bisphenol A into phenols occur. Over molecular sieves of larger pore size (13X and NaY zeolite) an important decrease of TBBPA amount is observed indicating effective trapping ability of these catalysts of basic character for brominated aromatic compounds. A total chemical modification of the vapour was achieved by Al-MCM-41 catalyst that split TBBPA into bromophenols. Analogous results were obtained by carrying out similar experiments on diallyl ether of TBBPA. Moreover, it was revealed that brominated bisphenol A compounds are modified essentially the same way, either evaporated or evolved from a polycarbonate blend or produced by pyrolysis from an epoxy resin.

Catalysis↗

PubMed2026

Circular upcycling of waste toner into eco-safe superparamagnetic nano-Fe3O4@C core-shell pigment for sustainable magnetic leather coatings.

The widespread use of laser printing and photocopying technologies has led to the accumulation of waste toner powder (WTP), a chemically stable and potentially carcinogenic pollutant. Herein, a scalable pyrolysis approach is demonstrated for converting WTP into a functional magnetic pigment for magnetic leather finishing. Pyrolysis at 600 °C for 2 h, guided by thermogravimetric analysis, enabled controlled phase transformation monitored by hyphenated TGA-FTIR. The resulting material (WTP-600) was comprehensively characterised using VSM, FTIR, XPS, pXRD, FESEM, HRTEM, EDX, 57Fe Mössbauer analysis, ICP-OES and TOC analysis. These analyses confirm near-complete removal of the polymeric fraction during pyrolysis, leading to an ≈ 97% reduction in volume of pristine WTP and the formation of a carbonaceous shell coated on a superparamagnetic nanocrystalline Fe3O4 core (Fe3O4@C). The carbonaceous surface of WTP-600 is enriched with hydroxyl functionalities; it is eco-friendly, and its magnetic strength is ≈ 2.3-fold higher than that of pristine WTP. Both WTP and WTP-600 were formulated with a commercial leather-finishing dispersion and applied as surface finishing on leather. As anticipated, the magnetic strength of WTP-600-coated leather was approximately 2.3 times higher than that of WTP-RT-coated leather. Evaluation of coating performance parameters and organoleptic assessment demonstrated that WTP-600-coated leather exhibited superior surface finishing and tactile properties compared to WTP-RT-coated leather. Magnetic leather of various colours was successfully synthesised by incorporating different pigments into WTP-600, resulting in only a marginal reduction in magnetic properties. The magnetic pigment-coated leather was found to be microbiologically stable, environmentally safe, and cytocompatible with human epidermal HaCaT keratinocyte cell lines. The prepared magnetic leathers demonstrate significant potential for advanced applications, including adhesive-free wall tiling, educational tool fabrication, and energy harvesting from human motion.

Magnetic leather finishes↗

PubMed2004

Preliminary report of endolaryngeal and endotracheal laser surgery of juvenile-onset recurrent respiratory papillomatosis by Nd:YAG laser and a new fiber guidance instrument.

OBJECTIVES: Recurrent respiratory papillomatosis (RRP) caused by human papilloma virus (type 6 and 11) is the most common benign neoplasm of the larynx in children. Despite being a benign disease, treatment is very difficult and is characterized by frequent recurrence, spread throughout the respiratory tract, and malignant degeneration. Besides surgical resection and the established CO(2) laser treatment, laser surgery by fiber-guided Nd:YAG laser light promises to be a bloodless and effective treatment procedure. To improve this new method, a novel fiber guidance instrument has been developed to aid in endolaryngal laser surgery of RRP. Study design and setting The method described uses a specially designed instrument for fiber guidance that is equipped with a bendable distal tip to move the fiber end precisely. Moreover, the instrument includes an additional channel for the suction of smoke and pyrolysis products. Up to now, 5 patients (aged 4 to 8 years) with RRP were treated by Nd:YAG laser light (lambda = 1064 nm; power, 10 W; irradiance, 3.5 kW/cm(2), continuous wave) with a prototype version of the new instrument and were followed up for 12 months each. RESULTS: Because of the adequate length and the bendable distal tip with a range of -5 degrees up to 45 degrees to the optical axis of the fiber and less than 10% light loss at maximal deflection, RRP can be treated by Nd:YAG laser light easily and precisely. The continuous suctioning ensured an optimum view of the operating field and a minimal load of potential infectious laser plume and toxic pyrolysis products for the patient as well as for the physician. The laser treatment of RRP with the new fiber guidance instrument was only minimally traumatic. During 1-year follow-up visits, all Nd:YAG laser light-treated patients, showed a regression of the disease. CONCLUSIONS: The new fiber guidance instrument enables a precise and easy treatment of the RRP with fiber-guided laser systems (eg, Nd:YAG-, diode-, and KTP-lasers) and an effective removal of infectious laser plume as well as toxic pyrolysis products. A follow-up period of 1 year revealed that Nd:YAG laser surgery seems to prevent a rapid recurrence of juvenile respiratory papillomatosis in the treated patients.

Child↗

PubMed2005

Part I. Identifying anthropogenic markers in surface waters influenced by treated effluents: a tool in potable water reuse.

In potable water reuse, treated wastewater becomes part of the drinking water supply. An important question associated with this practice is whether or not the organic quality of the treated wastewater is chemically different from that of non-human impacted water. This question was addressed in a case study of indirect potable water reuse where the organic matrix of the South Platte River was analyzed upstream and downstream of the discharge of treated wastewater effluent using conventional water quality parameters combined with pyrolysis-GC/MS. Effluent-derived organic material (EfOM) was found to be more aliphatic and had higher organic nitrogen and halogen content compared to organic material derived from "natural" (non-anthropogenic) sources (NOM). Seasonal changes that resulted from the change in the contributions of aquatic and terrestrial sources were not observed in EfOM; but they were strongly observed in NOM under the control of natural processes. Using principal component and factor analyses, the pyrolysis fragments of phenol, alkyl-phenols, and acetic acid were identified as the seasonal indicators for the NOM set of samples. In contrast, benzaldehyde, benzonitrile, chlorobutanoic acid, furancarboxaldehyde, and methylfurancarboxaldehyde were identified as the indicators for wastewater inputs for the EfOM set of samples. Overall, the results from conventional water quality parameters and pyrolysis-GC/MS revealed that: (1) EfOM bears a chemical signature distinct from NOM and (2) under the conditions of this study, EfOM discharged to the South Platte River persisted and controlled organic quality at downstream points.

Acetic Acid↗

PubMed2000

The presence of a SO molecule in [NiFe] hydrogenase from Desulfovibrio vulgaris Miyazaki as detected by mass spectrometry.

The active site of [NiFe] hydrogenase is a binuclear metal complex composed of Fe and Ni atoms and is called the Ni-Fe site, where the Fe atom is known to be coordinated to three diatomic ligands. Two mass spectrometric techniques, pyrolysis-MS (pyrolysis-mass spectrometry) and TOF-SIMS (time-of-flight secondary ion mass spectrometry), were applied to several proteins, including native and denatured forms of [NiFe] hydrogenase from Desulfovibrio vulgaris Miyazaki F, [Fe4S4]2-ferredoxin from Clostridium pasteurianum, [Fe,S2]-ferredoxin from Spirulna platensis, and porcine pepsin. Pyrolysis-MS revealed that only native hydrogenase liberated SO/SO2 (ions of m/z 48 and 64 at an equilibrium ratio of SO and SO2) at relatively low temperatures before the covalent bonds in the polypeptide moiety started to decompose. TOF-SIMS indicated that native Miyazaki hydrogenase released SO/SO2 (m/z 47.97 and 63.96) as secondary ions when irradiated with a high-energy Ga+ beam. Denatured hydrogenase, clostridial ferredoxin, and pepsin did not release SO as a secondary ion. The FT-IR spectrum of the enzyme suggested the presence of CO and CN. These lines of evidence suggest that the three diatomic ligands coordinated to the Fe atom at the Ni-Fe site in Miyazaki hydrogenase are SO, CO, and CN. The role of the SO ligand in helping to cleave H2 molecules at the active site and stabilizing the Fe atom in the diamagnetic Fe(II) state in the redox cycle of this enzyme is discussed.

Desulfovibrio vulgaris↗

PubMed1977

Mutagenicities of protein pyrolysates.

Smoke condensate obtained by pyrolysis of proteins, such as lysozyme and histone, was shown to be mutagenic to Salmonella typhimurium TA100 and TA98. In vitro metabolic activation by a mammaliam postmitochondrial enzyme preparation (S-9 Mix) was required. Smoke condensates obtained by pyrolysis of DNA, RNA, starch and vegetable oil were slightly mutagenic, whereas those from pyrolysis of L- and D-tryptophan and 5-hydroxy-D,L-tryptophan were very strongly mutagenic with metabolic activation by S-9 Mix. Because of the high correlation between mutagenicity and carcinogenicity, it is theorized that the cooking of proteinaceous foods might be an important cause of human cancers.

5-Hydroxytryptophan↗

PubMed2000

Decomposition of isoquinoline and quinoline by supercritical water.

The ability of supercritical water (SCW) to decompose heterocyclic compounds (quinoline and isoquinoline) has been explored in this study. The results obtained suggest that water acts as a chemical reagent above its critical point (374 degrees C and 22.1 MPa). Significant proportions of isoquinoline and quinoline were removed during the reaction with SCW. The response of these compounds to pyrolysis was also compared with their reaction with SCW. Both compounds were relatively more reactive in the presence of SCW than during pyrolysis. Because of the different positions of N atom in the two compounds, they reacted with SCW differently. Breaking of C-N bonds during SCW reaction was by hydrogenation and hydrocracking, while pyrolysis was due to thermocracking mainly.

Chemical Phenomena↗

PubMed2003

Studies of the thermal degradation of waste rubber.

One kind of Chinese waste tire's sample was pyrolyzed under an inert atmosphere by using thermo-gravimetric apparatus (TGA) and differential thermal analysis (DTA). Different pyrolysis temperature ranges were determined according to the reaction transition temperature obtained by TGA and DTA. Then, at each temperature range, the pyrolysis gaseous products were analyzed by gas chromatography (GC). The influence of the temperature range on the relative yields of the major decomposition products is studied, and a mechanism for the formation of the main components was also investigated. The results indicate that pyrolysis of waste rubber follows the radical mechanism, and the major products are not seriously affected by increasing the temperature from room temperature to 420 degrees C and from 421 to 600 degrees C, but the degradation of blend rubber is different for each of the compositional elastomer.

Environmental Pollution↗

PubMed2001

Pyrolytic characteristics of microalgae as renewable energy source determined by thermogravimetric analysis.

Two kinds of autotrophic microalgae, Spirulina platensis (SP) and Chlorella protothecoides (CP) were pyrolyzed at the heating rates of 15, 40, 60 and 80 degrees C/min up to 800 degrees C in a thermogravimetric analyzer to investigate their pyrolytic characteristics. Three stages (dehydration, devolatilization and solid decomposition) appeared in the pyrolysis process. SP and CP mainly devolatilized at 190-560 degrees C and 150-540 degrees C, respectively. A total volatile yield of about 71% was achieved from each microalga. As the heating rate increased, a lateral shift to higher temperatures was observed in their thermograms, and the instantaneous maximum and average reaction rates in the devolatilization stage were increased while the activation energy was decreased. The value of activation energy for CP pyrolysis was 4.22-5.25 x 10(4), lower than that of SP (7.62-9.70 x 10(4)), and the char in final residue of CP was 14.00-15.14%, less than that of SP by 2-3%. This indicated that CP is preferable for pyrolysis over SP. The experimental results may provide useful data for the design of pyrolytic processing systems using planktonic microalgae as feedstock.

Bioelectric Energy Sources↗

PubMed2002

A technique for the determination of 18O/16O and 17O/16O isotopic ratios in water from small liquid and solid samples.

We have developed a new technique in which a solid reagent, cobalt(III) fluoride, is used to prepare oxygen gas for isotope ratio measurement from water derived either from direct injection or from the pyrolysis of solid samples. The technique uses continuous flow, isotope ratio monitoring, gas chromatography/mass spectrometry (irmGC/MS) to measure the delta18O and delta17O of the oxygen gas. Water from appropriate samples is evolved by a procedure of stepped pyrolysis (0-1000 degrees C, typically in 50 degrees C increments) under a flowing stream of helium carrier gas. The method has considerable advantages over others used for water analysis in that it is quick; requires only small samples, typically 1-50 mg of whole rock samples (corresponding to approximately 0.2 micromol of H2O); and the reagent is easy and safe to handle. Reproducibility in isotope ratio measurement obtained from pyrolysis of samples of a terrestrial solid standard are delta18O +/- 0.54, delta17O +/- 0.33, and delta17O +/- 0.10/1000, 1sigma in all cases. The technique was developed primarily for the analysis of meteorites, and the efficiency of the method is illustrated herein by results from water standards, solid reference materials, and a sample of the Murchison CM2 meteorite.

Meteoroids↗

PubMed2005

Carbon position-specific isotope analysis of alanine and phenylalanine analogues exhibiting nonideal pyrolytic fragmentation.

Recent advances in gas chromatography combustion-isotope ratio mass spectrometry (GCC-IRMS) has made compound-specific isotope analysis routine, but reports on position-specific isotopic analysis are still scarce. On-line GC-pyrolysis (Py) coupled to GCC-IRMS is reported here for isolation and isotopic characterization of alaninol and phenethylamine, analogues of alanine and phenylalanine, respectively. Ideally, pyrolytic fragments will originate from unique sites within the parent molecule, and isotope ratios for each position within the parent can either be measured directly or calculated from fragment isotope ratios without substantially degrading the analytical precision. Alaninol pyrolysis yielded several fragments, of which CO and CH4 were used for isotope ratio calculations. Isotope labeling experiments showed that CO derived entirely from the C(1) position, while all three positions of alaninol contributed to CH4 (29.0 +/- 0.3% from C(1), 3.6 +/- 0.2% from C(2), and 66.9 +/- 1.1% from C(3)). We demonstrate iterative use of mass balance to calculate isotope ratios from all positions despite the nonideal positional fidelity of CH4. Pyrolysis of phenethylamine generated benzene and toluene fragments. Benzene derived entirely from C(ring), and toluene was proportionately formed from C(3) and C(ring). Relative intramolecular isotope ratios (Deltadelta13C) were calculated directly from delta13C of fragments or indirectly by mass balance. Though the C(3) isotope ratio was calculated from the benzene and toluene fragments, propagation of errors showed that the final precision of the determination was degraded due to the small contribution that C(3) makes to toluene. Samples of each amino acid from four different vendors showed natural variability between sources, especially at the C(1) position of alaninol (range of Deltadelta13C approximately 50 per thousand). The average precision was SD(Deltadelta13C) < 0.20 per thousand for directly measured positions of alaninol and phenethylamine. The precision of indirectly measured positions was poorer (SD(Deltadelta13C) = 0.94 per thousand for alaninol, 6.54 per thousand for phenethylamine) due to propagation of errors. These data demonstrate that GC-Py-GCC-IRMS data can be used to extract high-precision isotope ratios from amino acids despite nonideal positional fidelity in fragments and that natural intramolecular variability in delta13C can be used to distinguish different sources of amino acids.

Carbon Isotopes↗

PubMed1998

Reduction of fatty acid methyl esters to fatty alcohols to improve volatility for isotopic analysis without extraneous carbon.

Carbon in derivatization groups cannot be distinguished from analyte carbon by chromatography-based high-precision compound-specific or position-specific isotope analysis. We report the reduction of fatty acid methyl esters to fatty alcohols to facilitate high-quality chromatographic separation, without addition of extraneous carbon, with subsequent high-precision position-specific isotope analysis. Methyl palmitate is quantitatively reduced to 1-hexadecanol by LiAlH4 in a one-step reaction. Gas-phase pyrolysis of 1-hexadecanol results in a series of monounsaturated alcohols and alpha-olefins analogous to fragmentation found for methyl palmitate, as well as an additional peak corresponding to the pyrolytic dehydration product, 1-hexadecene. Carbon isotope analysis of the fragments yielded precision of SD (delta 13C) < 0.4/1000. Results of position-specific analysis of very low enrichment [1-13C]-1-hexadecanol (delta 13C = -4.00/1000) showed no evidence of scrambling of the C1 position, and isotope ratios in accord with expectations. The pyrolysis product 1-hexadecene was isotopically enriched relative to 1-hexadecanol, which may cause minor depletion of other pyrolysis products that can be taken into account by routine calibration. The procedure is general and can be extended to compound-specific and position-specific analysis of moderate molecular weight, low-volatility analytes containing acid groups that would otherwise be blocked with methyl, ethyl, acetyl, or trimethyl silyl groups containing extraneous carbon.

Aluminum Compounds↗

PubMed2002

Carbon nanotubes from organometallic precursors.

Multiwalled as well as single-walled carbon nanotubes are conveniently prepared by the pyrolysis of organometallic precursors such as metallocenes and phthalocyanines in a reducing atmosphere. More importantly, pyrolysis of organometallics alone or in mixture with hydrocarbons yields aligned nanotube bundles with useful field emission and hydrogen storage properties. By pyrolysis of organometallics in the presence of thiophene, Y-junction nanotubes are obtained in large quantities. The Y-junction tubes have a good potential in nanoelectronics. Carbon nanotubes prepared from organometallics are useful to prepare nanowires and nanotubes of other materials such as BN, GaN, SiC, and Si(3)N(4).

Biosensing Techniques↗

PubMed2006

A two step chemo-biotechnological conversion of polystyrene to a biodegradable thermoplastic.

A novel approach to the recycling of polystyrene is reported here; polystyrene is converted to a biodegradable plastic, namely polyhydroxyalkanoate (PHA). This unique combinatorial approach involves the pyrolysis of polystyrene to styrene oil, followed by the bacterial conversion of the styrene oil to PHA by Pseudomonas putida CA-3 (NCIMB 41162). The pyrolysis (520 degrees C) of polystyrene in a fluidized bed reactor (Quartz sand (0.3-0.5 mm)) resulted in the generation of an oil composed of styrene (82.8% w/w) and low levels of other aromatic compounds. This styrene oil, when supplied as the sole source of carbon and energy allowed for the growth of P. putida CA-3 and PHA accumulation in shake flask experiments. Styrene oil (1 g) was converted to 62.5 mg of PHA and 250 mg of bacterial biomass in shake flasks. A 1.6-fold improvement in the yield of PHA from styrene oil was achieved by growing P. putida CA-3 in a 7.5 liter stirred tank reactor. The medium chain length PHA accumulated was comprised of monomers 6, 8, and 10 carbons in length in a molar ratio of 0.046:0.436:1.126, respectively. A single pyrolysis run and four fermentation runs resulted in the conversion of 64 g of polystyrene to 6.4 g of PHA.

Biodegradation, Environmental↗

PubMed1998

Tris(benzylthiolato)bismuth. Efficient Precursor to Phase-Pure Polycrystalline Bi(2)S(3).

Details of the synthesis, physical and spectroscopic characterization, and thermal decomposition of tris(benzylthiolato)bismuth, (BnS)(3)Bi, Bn = CH(2)C(6)H(5), are presented. Results from pyrolysis of (BnS)(3)Bi demonstrate that this compound is a convenient precursor to phase-pure, polycrystalline Bi(2)S(3) with low carbon and hydrogen contamination under mild thermal conditions (ca. 275 degrees C). Flow-tube pyrolysis produces small ( approximately 1 &mgr;m) spherical particles, whereas sealed-tube pyrolysis produces 6-&mgr;m diameter spherical particles composed of radiating acicular crystallites. Bi(2)S(3) was characterized by X-ray powder diffraction and scanning electron microscopy.

Journal Article↗

PubMed1998

Reactions of H(3)Al.NMe(3) with E(SiMe(3))(3) (E = P, As). Structural Characterization of the Trimer [H(2)AlP(SiMe(3))(2)](3) and Base-Stabilized Adduct [H(2)AlAs(SiMe(3))(2)].NMe(3) and Their Thermal Decomposition toward Nanocrystalline AlP and AlAs, Respectively.

Dehydrosilylation reactions in diethyl ether between H(3)Al.NMe(3) and E(SiMe(3))(3) afforded for E = P a high yield of the trimer [H(2)AlP(SiMe(3))(2)](3) (1), while for E = As a monomeric base-stabilized adduct [H(2)AlAs(SiMe(3))(2)].NMe(3) (2) as well as its degradation solid product were obtained. No reaction occurred for E = N. The single-crystal X-ray structure determination for 1 yielded a planar six-membered ring of alternating four-coordinated Al and P centers. The structural solution for 2 revealed the monomeric unit [H(2)AlAs(SiMe(3))(2)] stabilized by coordination of NMe(3) at the Al site. Pyrolysis of 1 at 450 degrees C promoted further dehydrosilylation and yielded a product which by XRD spectroscopy showed the onset of AlP crystallinity while at 950 degrees C afforded nanocrystalline AlP with 5 nm average particle size. Pyrolysis of 2 at 450 degrees C resulted in the formation of nanocrystalline AlAs with 2 nm average particle size. Under applied pyrolysis conditions for 1 and 2, the target elimination-condensation pathway via dehydrosilylation was accompanied by other decomposition side reactions and retention of some contaminant residues.

Journal Article↗

PubMed2000

Influence of pyrolytic and aqueous-phase reactions on the mechanism of formation of Maillard products.

The influence of the reaction phase on the mechanism of formation of Maillard products was studied by comparison of (13)C-label incorporation patterns of the common products formed in model systems consisting of labeled glycine and D-glucoses subjected to both pyrolysis and heating in aqueous solutions. Pyrolysis experiments were performed at 250 degrees C for 20 s, and aqueous model systems were heated in sealed vials for 3 h at 120 degrees C followed by GC/MS analysis. Label incorporation patterns of the following compounds were analyzed: cyclotene, furanmethanol, acetylpyrrole, 5-methyl-pyrrole, trimethylpyrazine, acetic acid, 3-hydroxy-2-butanone, 2,3-butanedione, and 2-methyl-4, 5-dihydro-3(2H)-furanone. Although pyrolysis reaction produced higher number of products, however, the major pathways of formation of variety of important Maillard products followed the same mechanism under both pyrolytic and aqueous systems. Furthermore, contrary to literature speculations, 2-methyl-4, 5-dihydro-3(2H)-furanone was shown to be formed by ring contraction of 2,3-dihydro-3,5-dihydroxy-6-methyl-4(H)-pyran-4-one, through benzilic acid rearrangement, followed by decarboxylation.

Hot Temperature↗