Rapid determination of anhydride content in trans-polyisoprene-graft-maleic anhydride by double-shot pyrolysis gas chromatography–mass spectrometry

• The content of grafted MA in sTPIgMA was quantified using DS-PyGC/MS.
• sTPIgMA containing non-grafted MA and a gel fraction could be directly analyzed.
• The method was shown to be rapid, simple, accurate, and repeatable.

A rapid method for determination of anhydride content in synthetic trans-polyisoprene-graft-maleic anhydride (sTPIgMA) by double-shot pyrolysis gas chromatography mass spectrometry (DS-PyGC/MS) has been developed. The sample preparation step was minimized and samples were easy to handle. Dissolution of the polymer in toxic solvents could be avoided, and solid specimens containing unreacted MA monomer could be analyzed without purification. Unreacted MA monomer, residual solvent, and other volatile substances were eliminated from sTPIgMA during the thermal desorption step. In the subsequent pyrolysis step, grafted anhydride moieties were thermally decomposed to carbon dioxide and quantified. The content of grafted anhydride, measured by the DS-PyGC/MS method, was compared with the values obtained from conventional titration and FTIR methods. The determination of grafted anhydride content in sTPIgMA by DS-PyGC/MS was shown to be fast, simple, accurate, and repeatable.