Applications of mass spectrometry to polymers

Schulten, H.‐R.; Lattimer, Robert P.

doi:10.1002/mas.1280030204

Cited by 203 publications

(77 citation statements)

References 156 publications

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“…The thermal decomposition behaviour of high temperature aromatic polyimides has been widely investigated [12][13][14][15][16][17][18][19][20][21][22][23] , but studies on PEI are not yet available, and we report here an investigation on the thermal decomposition mechanisms of this polyetherimide by using direct pyrolysis mass spectrometry (DPMS) [24][25][26][27] . One of the key problems in studying the thermal degradation processes of high temperature polymeric materials is the detection of sizeable pyrolysis products that can give clues on the mechanism of decomposition of the polymer chains.…”

Section: Cmentioning

confidence: 99%

Thermal degradation mechanisms of polyetherimide investigated by direct pyrolysis mass spectrometry

Carroccio¹,

Puglisi²,

Montaudo³

1999

Macromol. Chem. Phys.

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SUMMARY:The thermal degradation mechanisms of poly [2,29-bis(3,4-dicarboxyphenoxy)phenylpropane-2-phenylenediimide] (PEI) have been investigated by thermogravimetry (TG) and by direct pyrolysis mass spectrometry (DPMS). TG data show that PEI has a main decomposition step centred at about 510 8 C followed by a less marked step in the 600 -650 8 C temperature range and leaving about 60% of charred residue at 800 8 C. The total ion curve (TIC) of a purified PEI sample, obtained by DPMS, closely reproduces the two maxima appearing in the derivative TG (DTG) curve, whereas the TIC curve of a crude PEI sample shows two less pronounced maxima in the temperature range of 250 -450 8 C due to low molar mass compounds, which volatilize undecomposed in the high vacuum of the MS. The structure of the pyrolysis compounds obtained in the first thermal degradation step of a purified PEI sample suggest that they are mainly formed by the scission of: i) the isopropylidene bridge of bisphenol A; ii) the oxygen-phthalimide bond; iii) the phenyl-phthalimide bond, which are apparently the weakest bonds of PEI. Extensive hydrogen transfer reactions and subsequent condensation reactions may account for the high amount of char residue. The pyrolysis compounds obtained in the second degradation step (620 8 C) are mainly constituted of CO 2 , benzene, aniline, benzonintrile, phenylenediamine, and dibenzonitrile, which may be generated by further thermal degradation reactions of pyrolysis compounds containing N1H phthalimide as end groups. Another degradation processes which may account for CO 2 formation is the hydrolysis of the imide moiety to form poly(amic acid) units which produce an aromatic amide structure by decarboxylation. The pyrolysis of an aromatic polyamide (NOMEX) was then studied for comparison. The structure of the pyrolysis products detected by the DPMS analysis of both polymers allowed a detailed schematization of the thermal degradation pathways involved in the degradation of PEI and on the reactions leading to the formation of the charred residue.

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Section: Cmentioning

confidence: 99%

Thermal degradation mechanisms of polyetherimide investigated by direct pyrolysis mass spectrometry

Carroccio¹,

Puglisi²,

Montaudo³

1999

Macromol. Chem. Phys.

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“…Thus, changes in these single ions can not be used accurately to estimate the percentage of cells of S. aureus mixed with E. coli. In other, less favourable cases, there may be interactions between constituents of the pyrolysate, which would change the mass spectra in a non-linear fashion (54,94,101). The next stage was to look at the relationship between the pyrolysis mass spectra of the binary bacterial mixtures using principal components analysis (PCA).…”

Section: Resultsmentioning

confidence: 99%

Quantitative Analysis of Multivariate Data Using Artificial Neural Networks: A Tutorial Review and Applications to the Deconvolution of Pyrolysis Mass Spectra

Goodacre

Neal

Kell

1996

Zentralblatt für Bakteriologie

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“…Plage et al 1991), of standard synthetic-and biopolymers (e.g. Schulten & Lattimer 1984;Schulten 1989), on high resolution Py-FIMS (e.g. Hempfling et al 1988) and on Py-GC/MS with library searches (e.g.…”

Section: Methodsmentioning

confidence: 99%

Influence of the mineral matrix on the formation and molecular composition of soil organic matter in a long-term, agricultural experiment

Schulten

Leinweber

1993

Biogeochemistry

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Abstract. The formation of soil organic matter from grass residues was studied in a 34-yearold pot experiment with grass cultivation on loamy marl using pyrolysis-field ionization mass spectrometry (Py-FIMS). For whole soils, the Py-FI mass spectra indicated clear changes in the molecular-chemical composition during SOM formation from grass residues. In particular, the enrichment of heterocyclic N-containing compounds with time was remarkable.For organomineral size fractions, even larger differences in the composition of SOM were found. The changes between the 13th and 34th experimental year are partly explained by a net transfer of phenols, lignin monomers und lignin dimers from medium silt to fine silt. Moreover, it is demonstrated that temperature-resolved Py-FIMS enables the determination of the thermal energy required for the evolution of individual compound classes which is a measure of the strength of humic-and organomineral bonds. At lower temperatures (<400 C), the enrichment of thermally less stable and/or loosely bound organic matter with cultivation time in clay and fine silt is due to carbohydrates, N-containing compounds, phenols and lignin monomers. Shifts of evolution maxima toward a higher pyrolysis temperature (> 400 °C) in clay, fine silt and medium silt are explained by a higher thermal stability of humic and/or organomineral bonds of lignin dimers, alkylaromatics and lipids, that developed during the last two decades of the experiment.

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Applications of mass spectrometry to polymers

Cited by 203 publications

References 156 publications

Thermal degradation mechanisms of polyetherimide investigated by direct pyrolysis mass spectrometry

Thermal degradation mechanisms of polyetherimide investigated by direct pyrolysis mass spectrometry

Quantitative Analysis of Multivariate Data Using Artificial Neural Networks: A Tutorial Review and Applications to the Deconvolution of Pyrolysis Mass Spectra

Influence of the mineral matrix on the formation and molecular composition of soil organic matter in a long-term, agricultural experiment

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