Simultaneous Pyrolysis Derivatisation

Challinor [29] has developed a method involving simultaneous pyrolysis-alkylation-GC and applied it to the characterisation of a range of polyesters, phenolic resins and polymer additives. The technique gives additional information about the composition of carboxylic acids, alcohols and substituted phenolic compounds in the pyrolysis products of these polymer types. The procedure involves methylation or butylation, using tetramethyl- or tetrabutyl-ammonium hydroxide, in the pyrolysis zone of the pyrolyser with analysis by flame ionisation GC or GC-MS. The advantages are greater structural information, minimal sample manipulation and increased sensitivity. 

Similarly, Venema and Boom-Van Geest [30] have described an in situ hydrolysis/methylation pyrolysis-GC method for the characterisation of polymers. Carboxyl, aromatic amino and hydroxy functional gronps in polymers were methylated in this procednre. 

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Simultaneous pyrolysis-derivatisation the presence of a suitable reagent followed by immediate analysis by suitable techniques (see Section 5.2). 

Challinor [611,620] has reported the use of pyrolysis derivatisation techniques, simultaneous pyrolysis methylation (SPM), cq. THM. In Py-THM-GC the sample (about 5 /xg) is typically placed in the hollow of a flattened Curie-point pyrolysis wire with approximately 0.5 /u-L tetramethyl ammonium hydroxide (TMAH) (25 wt.% aqueous solution) or tetramethylsulfonium hydroxide (TMSH). The prepared wire is then immediately located in the py-rolyser without allowing aqueous TMAH to evaporate and pyrolysis is carried out at the predetermined temperature. Special injectors for chemolysis (e.g. PTV injector) allow THM also for furnace PyGC experiments. Moldoveanu [499] has listed other common derivatisations utilised in GC analysis. 

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