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Researchers at the HIMS research group Analytical Chemistry and the Centre for Analytical Sciences Amsterdam (CASA) have successfully developed 3D-printed channels for chromatographical separation of small molecules. They conclude that the applied fused-deposition modelling (FDM) print technology can be used to produce columns in-house, for a fraction of the cost, with the ability to specify bespoke (on-demand) column dimensions. Their method, reported in a paper in the Journal of Chromatography A, can serve as a template for designing 3D-printed devices with monolithic stationary phases for a wide variety of applications.

picture of 3D printed column housings
From left to right: CAD model of the printed housing with a 2 mm ID × 45 mm length channel (a); travel path of the extruder showing the outer casing in red, wall layers in green, and infill in yellow (b); printed housing of glass-reinforced polypropylene (c); and printed housing of standard polypropylene (d). Image: HIMS

Abstract

In the last decade, 3D-printing has emerged as a promising enabling technology in the field of analytical chemistry. Fused-deposition modelling (FDM) is a popular, low-cost and widely accessible technique. In this study, RPLC separations are achieved by in-situ fabrication of porous polymer monoliths, directly within the 3D-printed channels. Thermal polymerization was employed for the fabrication of monolithic columns in optically non-transparent column housings, 3D-printed using two different polypropylene materials. Both acrylate-based and polystyrene-based monoliths were created. Two approaches were used for monolith fabrication, viz. (i) in standard polypropylene (PP) a two-step process was developed, with a radical initiated wall-modification step 2,2′-azobis(2-methylpropionitrile) (AIBN) as the initiator, followed by a polymerization step to generate the monolith; (ii) for glass-reinforced PP (GPP) a silanization step or wall modification preceded the polymerization reaction. The success of wall attachment and the morphology of the monoliths were studied using scanning electron microscopy (SEM), and the permeability of the columns was studied in flow experiments. In both types of housings, polystyrene-divinylbenzene (PS-DVB) monoliths were successfully fabricated with good wall attachment. Within the glass-reinforced polypropylene (GPP) printed housing, SEM pictures showed a radially homogenous monolithic structure. The feasibility of performing liquid-chromatographic separations in 3D-printed channels was demonstrated.

Project

The work described in the paper is part of the larger STAMP project (Separation Technology for a Million Peaks) funded under the Horizon 2020 Excellent-Science program of the European Research Council. The main aim of this project is to realise spatial three-dimensional liquid chromatography separations to achieve peak capacities in the order of a million. These separations are envisaged in an efficient three-dimensional separation device that might be produced using 3D-printing technology, as was explored in the current paper. 

Paper

Noor Abdulhussain, Suhas Nawada, Sinéad Currivan, Marta Passamonti, Peter Schoenmakers: Fabrication of polymer monoliths within the confines of non-transparent 3D-printed polymer housings. J. Chromatogr. A, Vol. 1623, 19 July 2020, 461159 DOI: 10.1016/j.chroma.2020.461159