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Applied Spectroscopy

Applied Spectroscopy

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  • Vol. 68, Iss. 4 — Apr. 1, 2014
  • pp: 445–457

On-Line Application of Near-Infrared Spectroscopy for Monitoring Water Levels in Parts per Million in a Manufacturing-Scale Distillation Process

Gordon Lambertus, Zhenqi Shi, Robert Forbes, Timothy T. Kramer, Steven Doherty, James Hermiller, Norma Scully, Sze Wing Wong, and Mark LaPack

Applied Spectroscopy, Vol. 68, Issue 4, pp. 445-457 (2014)


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Abstract

An on-line analytical method based on transmission near-infrared spectroscopy (NIRS) for the quantitative determination of water concentrations (in parts per million) was developed and applied to the manufacture of a pharmaceutical intermediate. Calibration models for water analysis, built at the development site and applied at the manufacturing site, were successfully demonstrated during six manufacturing runs at a 250-gallon scale. The water measurements will be used as a forward-processing control point following distillation of a toluene product solution prior to use in a Grignard reaction. The most significant impact of using this NIRS-based process analytical technology (PAT) to replace off-line measurements is the significant reduction in the risk of operator exposure through the elimination of sampling of a severely lachrymatory and mutagenic compound. The work described in this report illustrates the development effort from proof-of-concept phase to manufacturing implementation.

Citation
Gordon Lambertus, Zhenqi Shi, Robert Forbes, Timothy T. Kramer, Steven Doherty, James Hermiller, Norma Scully, Sze Wing Wong, and Mark LaPack, "On-Line Application of Near-Infrared Spectroscopy for Monitoring Water Levels in Parts per Million in a Manufacturing-Scale Distillation Process," Appl. Spectrosc. 68, 445-457 (2014)
http://www.opticsinfobase.org/as/abstract.cfm?URI=as-68-4-445

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