Monitoring biodegradation of poly(butylene sebacate) by Gel Permeation Chromatography, 1H-NMR and 31P-NMR techniques
Michela Siotto, Luca Zoia, Maurizio Tosin, Francesco Degli Innocenti, Marco Orlandi, Valeria Mezzanotte
Biotechnical Faculty of Ljubljana University, Večna pot 111, 1000 Ljubljana, Slovenia.
The increasing use of new generation plastics has been accompanied by the development of standard methods for studying their biodegradability. Generally, test methods are based on the measurement of CO2production, i.e. the mineralization degree of the tested materials. However, in order to describe the biodegradation process, the determination of the residual amount of tested material which remains in the environment and its chemical characterization can be very important. In this study, the biodegradation in soil of a model polyester (poly(butylene sebacate)) was monitored. Gel Permeation Chromatography and Nuclear Magnetic Resonance (31P-NMR and 1H-NMR) were used in order to obtain information about the polyester structure and the possible by-products that can be found in soil during and at the end of the incubation. The polyester mineralization (i.e. the CO2 production) was tested according to ASTM 5988 standard method for 245 days. When the polyester mineralization was about 21% and 37% (after 78 and 140 days of incubation) and at the end of the process (63% of mineralization, 100% if compared to the cellulose used as reference material), the soil was extracted with chloroform (solvent of the tested substance) and the extracts were analyzed using GPC and NMR acquisitions. The analytical acquisitions showed high molecular weight polyester in soil during the incubation (78 and 140 days): the polyester concentration decreased but its structure remained almost the same with a slow decreasing in molecular weight. At the end of the test (245 days) no film of the polyester could be extracted from the soil: NMR acquisitions and GPC analyses of the extracts suggested a strong degraded structure of the residual polyester. Even if at the end of the process only 63% of carbon had been lost by mineralization, the whole of the added polyester seems to have disappeared after about eight months of incubation, suggesting substantial biomass formation.
Keywords:Polyester biodegradation, Gel Permeation Chromatography, NMR acquisition, 1H-NMR, 31P-NMR.