Quantitative measurement of the polydispersity in the extent of functionalization of glass‐forming calix[4]resorcinarenes |
| |
| Authors: | W. E. Wallace K. M. Flynn C. M. Guttman D. L. VanderHart V. M. Prabhu A. De Silva N. M. Felix C. K. Ober |
| |
| Affiliation: | 1. Polymers Division, National Institute of Standards and Technology, Gaithersburg, MD 20899‐8541, USA;2. The contributions of W. E. Wallace, K. M. Flynn, C. M. Guttman, D. L. VanderHart, and V. M. Prabhu to this article were prepared as part of their official duties as United States Federal Government employees.;3. Department of Chemistry and Chemical Biology, Cornell University, Ithaca, NY 14853, USA;4. School of Chemical and Biomolecular Engineering, Cornell University, Ithaca, NY 14853, USA;5. Department of Materials Science and Engineering, Cornell University, Ithaca, NY 14853, USA |
| |
| Abstract: | The polydispersity in the degree of functionalization for two calix[4]resorcinarenes was determined by measuring quantitatively their molecular mass distribution with matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry. A mathematical method for polydisperse materials is described that creates a calibration curve to correct the ion signal intensities in the mass spectrum to give a more reliable molecular mass distribution. Correction is required due to various sample preparation and instrumental effects that may produce a systematic mass bias in the number of oligomers measured. This method employs gravimetric mixtures of analytes with different degrees of functionalization. One calix[4]resorcinarene was found to give accurate molecular mass distributions with little correction, while another, having a very similar molecular structure, was found to exhibit strong over‐counting of the oligomers having a high degree of functionalization. Copyright © 2009 John Wiley & Sons, Ltd. |
| |
| Keywords: | |
|
|
