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Practical Calibration Correction Method for the Maintenance of an On-Line Near-Infrared Monitoring System for Molten Polymers

Volume 60, Number 5 (May 2006) Page 529-538

Watari, Masahiro; Ozaki, Yukihiro

The present study has investigated a practical calibration correction method for an on-line monitoring system for molten polymers using a near-infrared (NIR) spectrometer. A partial least squares (PLS) calibration model for the ethylene (C2) content in melt polypropylene (PP) was developed for the investigation of changes in the performance of the on-line system before and after maintenance necessitated by the relocation. The predicted values for the C2 content from the spectra measured after maintenance by using the calibration model developed from the spectra collected before maintenance showed that there were some differences between the spectra obtained by the NIR spectrometer system before and after maintenance. The loadings from factor analysis suggested that the main cause for the differences in the system performance before and after maintenance was wavenumber shifts in the NIR spectra of PP in the melt state. Six popular standardization or calibration transfer methods (direct standardization (DS), piecewise direct standardization (PDS), additive correction (AD), multiplicative correction (MP), slope and bias (SB), and difference spectrum with interpolation (DSI)) were evaluated for the calibration correction of the on-line NIR monitoring system. However, the results of the evaluation showed that these standardization methods need more than two samples to obtain the high accuracy for the nonlinearity contained in the spectra set. From the standpoint of practical calibration in a real plant, the acceptable number of samples for the calibration is one or two. Moreover, recalibration using transferred spectra is not preferable because of the traceability for a calibration model. As a practical solution for a calibration correction in a real plant, a method considering wavenumber shift and path-length correction has been proposed in this study. The predicted results for the C2 content in the melt-state PP from the spectra measured after maintenance by using the proposed method have shown that the proposed method is useful for calibration correction in a real plant in spite of using only one sample.