Nitrile Butadiene Rubber (NBR), known for its superior resistance to hydrocarbon oil, low gas permeability, and excellent thermal stability, finds extensive use in seals, O-rings, conveyor belts etc. Importantly, these performance attributes are chiefly governed by acrylonitrile content in NBR. Analytical characterization of raw NBR is relatively straightforward using conventional techniques such as elemental analysis (CHNS) and liquid state 13C NMR. In contrast, the analysis of vulcanized NBR presents considerable challenges due to its crosslinked structure, which renders it insoluble in most organic and inorganic solvents, thereby restricting direct molecular-level analysis. While solid-state 13C NMR is an established technique for structural characterization in rubber vulcanizates, its high-cost curbs routine industrial analysis. In this study, Pyrolysis-Gas Chromatography-Mass Spectrometry (Py-GC-MS) technique has been explored as a robust, precise, cost-effective alternative.
Quantitative determination of acrylonitrile (ACN) content in vulcanized NBR, covering a compositional range of 15% to 52% is carried out using Py-GC-MS. For sequence distribution of ACN units, liquid-state 13C NMR, is utilized exclusively for soluble, uncured NBR. The absolute ACN content values thus obtained serve as reference standards for validating the Py-GC-MS method, enabling robust quantification across both raw and cured material forms.