This article deals with the global aging behavior of three polypropylene random copolymer (PP-R) materials with varying primary structure and morphology. Hot air aging experiments at elevated temperatures from 95 to 135 C were carried out using micro-sized specimens with a thickness of 100 μm. Technological and analytical aging indicators were monitored for an exposure time of up to 750 days. Independent of comonomer type (ethylene vs. butylene) and morphology (α vs. β crystal form) a critical molar mass of 300 kg mol −1 was obtained. The consumption of antioxidants was slower for the β-nucleated PP-R grade with finer spherulitic structure. The β-grade outperformed the α-crystal PP-R grades resulting in about 20% higher time-to-embrittlement values.
The combination of CE and MS is now a widely used tool that can provide a combination of high resolution separations with detailed structural information. Recently, we highlighted the benefits of an approach to add further functionality to this well-established hyphenated technique, namely the possibility to perform chemical reactions within the sheath-liquid of the CE-MS interface . Apart from using hydrogen/deuterium exchange for online determination of numbers of exchangeable protons, the addition of DPPH• (2,2-diphenyl-1-picrylhydrazyl) to the sheath-liquid can be used as a fast screening tool for studying antioxidant characteristics of individual components. Such a CE-MS methodology allows rapid and information-rich analysis with minimal reagent and sample consumption to be performed. In the present work, we demonstrate the applicability of this approach for the characterization of phenolic plant extracts from the Labiatae family, namely Rosmarinus officinalis and Melissa officinalis. Using the described approach, a wide range of compounds (15 and 13 phenolic compounds, respectively) could be confidently identified using a combination of high resolution CE-MS separations with implementation of online deuterium exchange and DPPH• reactions. These compounds included polyphenols, phenolic acids, and triterpene acids. In conjunction with online MS/MS experiments, extensive structural information for aglyconic and glycosylated antioxidants present in the extracts could be obtained using simple experimental changes, which can be carried out prior to the purchasing of expensive chemical standards or the time-consuming preparative isolation of individual compounds.
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