A Universal Mass Detector for Liquid Chromatography

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Abstract
The design and operation of a mass detector is described for online monitoring of components separated by LLC. The detector system uses a piezoelectric quartz mass sensor capable of displaying 10−10 gram changes in short-time periods. Effluent from a liquid chromatograph is sprayed on the crystal surface, the solvent is evaporated, and the mass of residual solute determined from the change in crystal frequency. Sampling of the liquid stream and solute deposition can occur at rapid intervals. A system was assembled to demonstrate the feasibility of using the crystal microbalance for LLC purposes. Spraying, drying and measuring was accomplished in 10 seconds, and the sensitivity attained was similar to that observed by commonly used LLC detectors. The mass detector was connected to the effluent from a differential refractometer on a gel permeation chromatograph. Butyl rubber and a mixture of polystyrenes were run. Differential distribution curves of polymer mass vs retention volume compared closely to those obtained with the differential refractometer detector. The paper includes chromatograms performance, speed, sensitivity data and construction details.

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