Evaluation of direct analysis in real time mass spectrometry for onsite monitoring of batch slurry reactions

Authors: David S. Cho, Stephen C. Gibson, Deepak Bhandari, Mary Ellen McNally, Ron M. Hoffman, Kelsey D. Cook, Liguo Song
Rapid Communications in Mass Spectrometry 2011, Dec, 15, 25(23), 3575–3580
10.1002/rcm.5269

 

Batch slurry reactions are widely used in the industrial manufacturing of chemicals, pharmaceuticals, petrochemicals and polymers. However, onsite monitoring of batch slurry reactions is still not feasible in production plants due to the challenge in analyzing heterogeneous samples without complicated sample preparation procedures. In this study, direct analysis in real time mass spectrometry (DART®-MS) has been evaluated for the onsite monitoring of a model batch slurry reaction. The results suggested that automation of the sampling process of DART®-MS is important to achieve quantitative results. With a sampling technique of manual sample deposition on melting point capillaries followed by automatic sample introduction across the helium beam, relative standard deviation (RSD) of the protonated molecule signals from the reaction product of the model batch slurry reaction ranged from 6 to 30%. This RSD range is improved greatly over a sampling technique of manual sample deposition followed by manual sample introduction where the RSDs are up to 110%. Furthermore, with the semi-automated sampling approach, semi-quantitative analysis of slurry samples has been achieved. Better quantification is expected with a fully automated sampling approach. Copyright © 2011 John Wiley & Sons, Ltd.