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Development of a Near-Infrared/Mid-Infrared Dual-Region Spectrometer for Online Process Analysis
Volume 66, Number 7 (July 2012) Page 773-781
TAKUMA GENKAWA, MASAHIRO WATARI, TAKASHI NISHII, and YUKIHIRO OZAKI*
A near-infrared (NIR) and mid-infrared (mid-IR) dual-region spectrometer having two immersion probes, a transmission probe for NIR, and an attenuated total reflection (ATR) probe for mid-IR has been developed for highly reliable process monitoring and deep process understanding. This spectrometer facilitates sequential acquisition of both NIR (10 000–4000 cm−1) and mid-IR (5000–1200 cm−1) spectra by switching the light path leading to the probes without the need for probe replacement. The use of a single light source and a single beam splitter enables achievement of a permanent alignment of the optical system and sequential data acquisition. The transmission NIR and ATR mid-IR probes designed and developed in the present study facilitate the acquisition of NIR/mid-IR spectra with optimized absorption intensities in both regions by simply placing the probes into a sample solution. The performance of the developed spectrometer was demonstrated in monitoring the ethanol fermentation process. NIR/mid-IR spectra of the fermentation solution with multiplicative scatter correction (MSC) represent the relative changes in the concentrations of glucose and ethanol in both regions. Principal component analysis (PCA) was performed on the MSC-treated spectra in the regions 6300–5650 cm−1, 4850–4300 cm−1, and 3500–2880 cm−1 to detect the end-point of the fermentation as an example of process monitoring. For all the regions, the score plot of the first principal component (PC) indicates that the fermentation progresses with the fermentation time and stops after 210 minutes and thus the end-point of the fermentation exists at around 210 minutes. The loading plot indicates that all of the first PCs are the relative changes in the concentrations of glucose and ethanol. This result reveals that the same chemical changes are observed in both transmission NIR and ATR mid-IR spectra. Multiple and simultaneous analysis was also performed, and intensity change in light scattering relating the growth of yeasts was monitored by the NIR spectra.
Index Headings: Near-infrared spectroscopy; NIR spectroscopy; Mid-infrared spectroscopy; Attenuated total reflection; ATR; Process analytical technology; Optical probe; Ethanol fermentation; Principal component analysis.