Structure and Degradation Behaviour of Synthetic Polymers Using Pyrolysis in Combination With Field Ion Mass Spectrometry

Hummel, Dieter O.

doi:10.1016/b978-0-444-41558-5.50016-x

Analytical Pyrolysis 1977

DOI: 10.1016/b978-0-444-41558-5.50016-x

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Structure and Degradation Behaviour of Synthetic Polymers Using Pyrolysis in Combination With Field Ion Mass Spectrometry

Dieter O. Hummel

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1979

1994

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Cited by 6 publications

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“…Pyrolysis in the solid probe of a mass spectrometer has been used to study structures and pyrolytic reactions of synthetic polymers (4,5). The most common technique is to heat the sample until a strong total ion current is observed, and then record the spectrum at a constant rate of polymer decomposition (6).…”

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“…The most common technique is to heat the sample until a strong total ion current is observed, and then record the spectrum at a constant rate of polymer decomposition (6). Mass spectrometric scans have been recorded as polymers were heated at programmed temperature rates and "ion chromatograms" or "mass fragmentograms" were derived from the spectra (5,7,8). The relatively fast heating rates and slow scan rates limited the amount of information from such experiments.…”

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confidence: 99%

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Direct pyrolysis of cellulose and cellulose derivatives in a mass spectrometer with a data system

Franklin¹

1979

Anal. Chem.

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mentioning

confidence: 99%

mentioning

confidence: 99%

Direct pyrolysis of cellulose and cellulose derivatives in a mass spectrometer with a data system

Franklin¹

1979

Anal. Chem.

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Segmented copolyetherurethane‐ureas and semicarbazides for blood circulation systems, III. Mass spectrometric investigations 1, pyro‐field ion mass spectrometry

Düssel

Wenzel

Hummel

1982

Angew. Makromol. Chem.

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The pyro-field ion mass spectra of urea or semicarbazide linked copolyetherurethanes have been measured with a maximum pyrolysis temperature of 873 K. The polyethers with hydroxy endgroups [poly(oxyethylene), poly(oxytetramethylene), poly(oxypropy1ene)l and the diisocyanates [4,4'-diisocyanatodicyclohexylmethane, 4,4'-diisocyanatodiphenylmethane, 2,4-diisocyanatotoluene] used for the synthesis can be identified from the spectra without difficulty. Among the diamines [ethylenediamine, hexamethylenediamine, 4,4'-diaminodiphenylmethane, 1,3-bis(amino-methy1)benzenel and isophthalic acid dihydrazide used for the coupling of the prepolymers bearing isocyanate endgroups, the aromatic diamines can easily be identified. Aliphatic diamines and isophthalic acid dihydrazide as structural units cannot be identified with the same reliability. Possible pyrolysis fragments suitable for the rapid and unambiguous identification of the building units of the polymer chains ("key fragments") are given. ZUSAMMENFASSUNG: Die Pyro-Feldionenmassenspektren von Harnstoff-oder Semicarbazid-verknupften Copolyetherurethanen wurden bei einer maximalen Pyrolysetemperatur von 873 K gemessen. Die zur Synthese verwendeten Polyether [Poly(oxyethylen), Poly(oxytetramethylen), Poly(oxypropy1en)l und die Diisocyanate [4,4 '-Diisocyanatodicyclohexylmethan, 2,4-Diisocyanatotoluol, 4,4'-Diisocyanatodiphenylmethan] liel3en sich anhand der Spektren leicht identifizieren. Ohne Schwierigkeiten gelingt dies auch bei den aromatischen Diaminen [4,4'-Diaminodiphenylmethan, 1,3-bis-(Aminomethyl)benzol], die zur Verknupfung der Prapolymeren mit Isocyanatendgruppen eingesetzt waren. Aliphatische Diamine (Ethylendiamin, Hexamethylendiamin) und Isophthalsauredihydrazid lassen sich nicht mit gleicher Sicherheit nachweisen. Soweit moglich werden charakteristische Pyrolysefragmente angegeben (,,Schliisselfragmente"), die zur raschen und zweifelsfreien Identifizierung der Bausteine der Polymerketten geeignet sind. POP PO€ = Poly(oxyethy1ene) EME POTM = PoIy(oxytetramahy1ene) POP = Poly(oxypropy1ene) HW = 4, 4'diirocyanatdicyclohexylmethane DDM = 4, 4'-diirocyanatdiphenylmethane TDI = 2, 4'diiMcyanatotoluene Ct = Ethylenediamine Cs = Hexamethylenediamine MDA = 4, 4'diamindiphenylmethane BMB = 1, 3-birlaminomethyl)benzene IDH = lrophthalic acid dihydrazide

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Primary thermal degradation processes of poly(ether/ketone) and poly(ether ketone)/poly(ether‐sulfone) copolymers investigated by direct pyrolysis‐mass spectrometry

Montaudo

Puglisi²,

Samperi³

1994

Macro Chemistry & Physics

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The mechanisms of thermal degradation of poly(ether-ketone) (PEK) and four poly(etherketone)/poly(ether-sulfone) copolymers (PEK/PES) have been investigated by direct pyrolysismass spectrometry (DPMS). Several families of pyrolysis compounds with H, OH and CHO endgroups have been identified in the pyrolysis mass spectra of PEK. All these pyrolysis compounds can arise from degradation mechanisms involving cleavages of the bridged groups (diphenyl ether and dibenzophenone units). Our data show that the main degradation products of PEK are aldehydes, most likely formed by an intramolecular thermal cleavage of benzophenone units. Compounds containing dibenzofuran units have also been observed in the DCI mass spectrum of PEK. The thermal decomposition of a low molecular weight PEK sample occurs in two stages with the maxima of decomposition at 390°C and 490"C, respectively. This fact indicates the occurrence of an end-group initiated thermal decomposition in the early degradation stage which is not present in the case of the high molecular weight PEK sample. The pyrolysis of PEK does not produce compounds containing biphenyl units, indicating that extrusion of carbonyls or recominbation processes are not involved. The thermal degradation compounds of the PEK/PES copolymers originate from the thermal cleavage of the bridge groups (diphenyl ether, benzophenone and diphenyl sulfone). The pyrolysis mass spectra of 1 : 1 (alt.), 1 : 1 (random), 3 : 1 and 1 : 3 PEK/PES copolymers appear essentially identical (apart for obvious differences in peak intensities), indicating that the molecular rearrangements (SO, extrusion, transesterification,

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Structure and Degradation Behaviour of Synthetic Polymers Using Pyrolysis in Combination With Field Ion Mass Spectrometry

Cited by 6 publications

References 28 publications

Direct pyrolysis of cellulose and cellulose derivatives in a mass spectrometer with a data system

Direct pyrolysis of cellulose and cellulose derivatives in a mass spectrometer with a data system

Segmented copolyetherurethane‐ureas and semicarbazides for blood circulation systems, III. Mass spectrometric investigations 1, pyro‐field ion mass spectrometry

Primary thermal degradation processes of poly(ether/ketone) and poly(ether ketone)/poly(ether‐sulfone) copolymers investigated by direct pyrolysis‐mass spectrometry

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