4IR Solutions
Reaction Monitoring
Reaction Monitoring
  • The AI-60’s permanent magnet design requires no cryogens as the system is powered by one standard wall outlet.
  • Samples can be run neat, in conventional protonated solvents, or, in deuterated NMR solvents. Deuterated solvents are not required.
  • Probes accept standard 5mm or 10mm NMR tubes.
  • Flow cell options are also available.
  • Complete automation of all NMR tasks (Acquisition, Processing, Integration, Results Reporting) enables walk-up applications with minimum user training and/or experience.
  • Spectral processing facilitates use of a variety of chemometric based routines for multiple property measurements.
  • The use of an NMR as a simple flow detector for benchtop reaction monitoring, mixing monitoring, dilution monitoring, or conversion monitoring has been limited by the need to bring the 'reaction' to the typical 'supercon' NMR lab.
  • With the AI-60 system continuous flow NMR can be performed “at the bench.” The system uses a high resolution permanent magnet with a simple flow cell and total system volumes of 2 to 5 ml depending on the length and diameter of the transfer tubing.
  • Further, detection limits of analyses in the 200+ ppm range are possible without the use of typical deuterated NMR solvents. Analysis times of 5 to 20 seconds are achieved at flow rates of 1 to 20+ ml/minute.
Case Study - Continuous Flow Reaction Monitoring
  • AI 60 NMR Analyzer was used to monitor three reaction process, Imine formation, CDI mediated, amide coupling and transesterification.
  • Each reaction was monitored at regular intervals by both 400 and 60MHz NMR and the data was overlaid to compare the profiles obtained at the two different field strengths.
  • NMR data generated from these three reactions demonstrates the application of low field NMR as a PAT tool for reaction monitoring.
Case Study - Reaction Monitoring
  • In the figure to the immediate right the expansion plots corresponding to the CH3 region of the 1H NMR spectrum are shown. Peak assignments corresponding to the constituents of the reaction are given. Excellent resolution of each CH3 resonance from each constituent in the reaction (t-butyl alcohol, acetic anhydride, t- butyl methyl ester, and, acetic acid) are well resolved.
  • Integration of each peak allows quantitative determination of each constituent’s concentration over the course of the entire reaction. As shown in the lower right figure, reaction kinetics can be determined. The Lab AI-60 system’s small footprint, high sensitivity, excellent resolution, and automated processing routines enable new opportunities and applications for reaction monitoring by NMR.
Case Study - Reaction Monitoring
Reaction Monitoring

13 May 2020

Proton NMR Investigation of Amide Samples using 60 MHz NMR analyzer

This article establishes the capability of NMR, specifically using a mid-field 60 MHz NMR analyzer, ...