Prediction of Ethylene Content in Melt-State Random and Block Polypropylene by Near-Infrared Spectroscopy and Chemometrics: Comparison of a New Calibration Transfer Method with a Slope/Bias Correction Method

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Abstract:

This paper reports the prediction of the ethylene content (C2 content) in random polypropylene (RPP) and block polypropylene (BPP) in the melt state by near-infrared (NIR) spectroscopy and chemometrics. NIR spectra of RPP and BPP in the melt states were measured by a Fourier transform near-infrared (FT-NIR) on-line monitoring system. The NIR spectra of RPP and BPP were compared. Partial least-squares (PLS) regression calibration models predicting the ethylene (C2) content that were developed by using each RPP or BPP spectra set separately yielded good results (SECV (standard error of cross validation): RPP, 0.16%; BPP, 0.31%; correlation coefficient: RPP, 0.998; BPP, 0.996). We also built a common PLS calibration model by using both the RPP and the BPP spectra set. The results showed that the common calibration model has larger SECV values than the models based on the RPP or the BPP spectra sets individually and is not practical for the prediction of the C2 content. We further investigated whether a calibration model developed by using the BPP spectra set can predict the C2 contents in the RPP sample set. If this is possible, it can save a significant amount of work and cost. The results showed that the use of the BPP model for the RPP sample set is difficult, and vice versa, because there are some differences in the molar absorption coefficients between the RPP and BPP spectra. To solve this problem, a transfer method from one sample spectra (BPP) set to the other spectra (RPP) set was studied. A difference spectrum between an RPP spectrum and a BPP spectrum was used to transfer from the BPP calibration set to the RPP calibration set. The prediction result (SEP (standard error of prediction), 0.23%, correlation coefficient, 0.994) of RPP samples by the transferred calibration set and model showed that it is possible to transfer from the BPP calibration set to the RPP calibration set. We also studied the transfer from the RPP calibration set (the range of C2 content: 0–4.3%) to the BPP calibration set. The prediction result of C2 content (the range of C2 contents: 0–7.7%) in BPP by use of the calibration model based on the transferred BPP spectra from the RPP spectra showed that the transfer method is only effective for the interpolation of the C2 content range by the nonlinear change in the peak intensities with the C2 content.

Keywords: CALIBRATION TRANSFER; CHEMOMETRICS; ETHYLENE; NEAR-INFRARED SPECTROSCOPY; ON-LINE MONITORING; PARTIAL LEAST-SQUARES REGRESSION; POLYPROPYLENE

Document Type: Research Article

DOI: http://dx.doi.org/10.1366/0003702042336082

Affiliations: Environmental and Analytical Products Business Division, Yokogawa Electric Corporation, Musashino 180-8750, Japan

Publication date: October 1, 2004

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