TY - JOUR A1 - Burger, René A1 - Lindner, Simon A1 - Rumpf, Jessica A1 - Do, Xuan Tung A1 - Diehl, Bernd W.K. A1 - Rehahn, Matthias A1 - Monakhova, Yulia A1 - Schulze, Margit T1 - Benchtop versus high field NMR: Comparable performance found for the molecular weight determination of lignin JF - Journal of Pharmaceutical and Biomedical Analysis N2 - Lignin is a promising renewable biopolymer being investigated worldwide as an environmentally benign substitute of fossil-based aromatic compounds, e.g. for the use as an excipient with antioxidant and antimicrobial properties in drug delivery or even as active compound. For its successful implementation into process streams, a quick, easy, and reliable method is needed for its molecular weight determination. Here we present a method using 1H spectra of benchtop as well as conventional NMR systems in combination with multivariate data analysis, to determine lignin’s molecular weight (Mw and Mn) and polydispersity index (PDI). A set of 36 organosolv lignin samples (from Miscanthus x giganteus, Paulownia tomentosa and Silphium perfoliatum) was used for the calibration and cross validation, and 17 samples were used as external validation set. Validation errors between 5.6% and 12.9% were achieved for all parameters on all NMR devices (43, 60, 500 and 600 MHz). Surprisingly, no significant difference in the performance of the benchtop and high-field devices was found. This facilitates the application of this method for determining lignin’s molecular weight in an industrial environment because of the low maintenance expenditure, small footprint, ruggedness, and low cost of permanent magnet benchtop NMR systems. KW - NMR KW - PLS-regression KW - Molecular weight determination KW - Chemometrics KW - Biomass Y1 - 2022 SN - 0731-7085 U6 - http://dx.doi.org/10.1016/j.jpba.2022.114649 VL - 212 IS - Article number: 114649 PB - Elsevier CY - New York, NY ER - TY - JOUR A1 - Lindner, Simon A1 - Burger, René A1 - Rutledge, Douglas N. A1 - Do, Xuan Tung A1 - Rumpf, Jessica A1 - Diehl, Bernd W. K. A1 - Schulze, Margit A1 - Monakhova, Yulia T1 - Is the calibration transfer of multivariate calibration models between high- and low-field NMR instruments possible? A case study of lignin molecular weight JF - Analytical chemistry N2 - Although several successful applications of benchtop nuclear magnetic resonance (NMR) spectroscopy in quantitative mixture analysis exist, the possibility of calibration transfer remains mostly unexplored, especially between high- and low-field NMR. This study investigates for the first time the calibration transfer of partial least squares regressions [weight average molecular weight (Mw) of lignin] between high-field (600 MHz) NMR and benchtop NMR devices (43 and 60 MHz). For the transfer, piecewise direct standardization, calibration transfer based on canonical correlation analysis, and transfer via the extreme learning machine auto-encoder method are employed. Despite the immense resolution difference between high-field and low-field NMR instruments, the results demonstrate that the calibration transfer from high- to low-field is feasible in the case of a physical property, namely, the molecular weight, achieving validation errors close to the original calibration (down to only 1.2 times higher root mean square errors). These results introduce new perspectives for applications of benchtop NMR, in which existing calibrations from expensive high-field instruments can be transferred to cheaper benchtop instruments to economize. Y1 - 2022 SN - 1520-6882 U6 - http://dx.doi.org/10.1021/acs.analchem.1c05125 VL - 94 IS - 9 SP - 3997 EP - 4004 PB - ACS Publications CY - Washington, DC ER -