Thermodynamic and Kinetic Analysis of Hydrolysis Reactions

Benchtop nuclear magnetic resonance (NMR) spectrometers are adaptable instruments for reaction monitoring, quality control, and structure elucidation and verification.

a picture of an NMR spectrometer full of samples

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They are less costly to procure, have insignificant operating expenses, and require only marginal laboratory setup compared to their larger, floor-standing counterparts.

Despite being inherently less efficient than high-field instruments in some aspects, they are more than sufficient for numerous applications and enable NMR techniques that a wide range of users can adopt.

One less apparent benefit of floor-standing instruments is the prospect of performing experiments at various temperatures. A variable temperature unit is standard on Bruker spectrometers. The room temperature iProbes can manage temperatures between –150 °C and 150 °C by default.

Benchtop equipment differs because their permanent magnets are relatively sensitive to temperature change (100 ppm/K).

The magnet’s thermoregulation is a key challenge when developing such a tool and having a sample cavity that fluctuates in temperature adds to the task.

Bruker offers the Fourier 80 with the Adjustable Temperature (AT) feature, which enables the user to obtain NMR spectra at different sample temperatures while keeping the magnet temperature fixed at 25 °C.

The Fourier 80 equipped with AT enables easy adjustment of the sample cavity’s temperature between 25 °C and 60 °C. After altering the temperature, the magnet will require time to adjust to the new conditions, subject to the temperature difference.

This ranges from 4 to 6 hours when changing between the two possible extremes but can be as little as 1 hour if a temperature series is obtained and the increments are low (e.g., 5 K between steps).

The sample’s temperature stability and reproducibility are on the order of 100 mK. The only added infrastructure required is a supply of pressurized nitrogen or air.

The system has a gas flow box that regulates the incoming gas flow. All Fourier 80 supplied with AT are fully compatible with the automatic sample changer.

The extra inlet on the side of the spectrometer also grants the use of a flow cell, further adding to the expertise of the Fourier 80 with added AT.

Various applications are possible, from polymer science over reaction monitoring to enzyme kinetics.

This article demonstrates the potential of this tool by establishing some kinetic and thermodynamic properties of ester hydrolysis reactions.

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This information has been sourced, reviewed and adapted from materials provided by Bruker BioSpin - NMR, EPR and Imaging.

For more information on this source, please visit Bruker BioSpin - NMR, EPR and Imaging.

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