Near Infrared Reflection Spectroscopy: A Versatile Tool for Rapid Characterization of Olefin Copolymers and High‐Throughput Experiments

Abstract

Near infrared (NIR) spectroscopy was developed as a rapid analytical method for the determination of the composition of olefin copolymers obtained in high‐throughput screening. NIR spectra of ethene/propene and ethene/1‐hexene copolymers, also characterized by means of 13C NMR spectroscopy, were recorded and used to design multivariate calibration models. Different methods for the preprocessing of the spectra, including the linearization by non‐linear transformations, were compared. Optimal methods and error estimates were established using crossvalidation. This technique is of particular interest for the rapid on‐line analysis of high‐throughput experiments in the field of polymer and catalyst design employing methods from combinatorial chemistry. Predicted versus true value of the propene incorporation and standard deviation for ethene/propene copolymers.magnified imagePredicted versus true value of the propene incorporation and standard deviation for ethene/propene copolymers.

Combinatorial Methods, Automated Synthesis and High‐Throughput Screening in Polymer Research: The Evolution Continues

“…Near infrared (NIR) spectroscopy was also utilized for the composition determination of olefin copolymers (ethene/hex-1-ene and ethane/propene) in a high sample throughput mode. [81] It was stated that NIR spectroscopy can significantly improve the performance of rapid on-line polymer analysis if it is applied in conjunction with mid infrared (MIR) spectroscopy.…”

High‐Output Polymer Screening: Exploiting Combinatorial Chemistry and Data Mining Tools in Catalyst and Polymer Development

“…Also mid-and near infrared spectroscopy were improved by means of multivariate calibration to meet the demands of HOPS and HTS. [31] 4 Online Monitoring ATR-FT-IR probes can also be used as a very effective tool for online monitoring the solution copolymerization of olefins. The semi-and fully automated reactors for HOPS were equipped with ATR-FT-IR online monitoring …”

Comparison of near-infrared and Raman spectroscopy for the determination of the density of polyethylene pellets

“…Near-infrared (NIR) spectroscopy has been extensively studied for quantitative analysis of various properties of diverse polymers since it is simple, fast and non-destructive [1][2][3][4][5][6][7]. When polymer samples are solid (such as pellets or flakes), diffuse reflectance is practically the only choice for obtaining NIR spectra while large samples are rotating or reciprocating to ensure spectral reproducibility.…”