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A monitoring method for solvent exchanges has been developed and demonstrated. The solvent mixture is monitored in real time by a process fiber optic probe, coupled to a near infrared spectrometer. A partial least squares (PLS) calibration model was developed based on typical solvent exchange systems used in a pharmaceutical bulk drug production. The acousto-optic tunable filter (AOTF) NIR is well suited to process monitoring, as it has no moving parts. The AOTF-NIR continuously fits the PLS model to the currently collected spectrum. The returned values can be used to follow the solvent exchange process. The solvent exchange was monitored by placing a dip-probe into the exchange distillation. The results indicate that the percent of lower boiling solvent in the reaction mixture can be monitored in real time and, thus, be used to determine when the exchange distillation is complete.
Frank J. Tarczynski,Joanne M. Anderson,Dwight S. Walker, andKim Purdy
"Near-IR monitoring of lab-scale solvent exchanges", Proc. SPIE 3537, Electro-Optic, Integrated Optic, and Electronic Technologies for Online Chemical Process Monitoring, (26 February 1999); https://doi.org/10.1117/12.341028
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Frank J. Tarczynski, Joanne M. Anderson, Dwight S. Walker, Kim Purdy, "Near-IR monitoring of lab-scale solvent exchanges," Proc. SPIE 3537, Electro-Optic, Integrated Optic, and Electronic Technologies for Online Chemical Process Monitoring, (26 February 1999); https://doi.org/10.1117/12.341028