Freeze-thaw valves as a flow control mechanism in spatially complex 3D-printed fluidic devices

In this paper, we demonstrate a proof-of-principle of a freeze-thaw valve (FTV) created in a 3D-printed fluidic device. Portions of channels are enveloped by cooling and heating jackets, and a heat transfer liquid is recirculated through the two jackets. A frozen plug is created in selected portions of the target-channel and the heating jacket ensures that a selected temperature is maintained in the rest of the channel. An FTV can be 3D-printed in a wide variety of materials as single piece devices with no moving parts without high resolution requirements of the printing process. Such valves can therefore be incorporated in devices for liquid chromatography or multi-step synthesis process. Computational fluid dynamic simulations of a prototype T-junction piece show the two zones to be well defined at coolant and heating jacket flow-rates greater than 1 mL/min, with power consumptions of 1–3 W. The prototype was printed in Titanium 6Al-4V using selective laser melting and the frozen plug was shown to withstand 20 MPa of pressure. Switching times between states 1 (with a frozen section) and 2 (with both sections thawed) were 0.2–3 min in computational and experimental tests. The scalability of the freeze-thaw system was demonstrated using a multi-gate valve containing 33 junctions without a proportionate increase in operational complexity or switching times

Introduction of Octadecyl-Bonded Porous Particles in 3D-Printed Transparent Housings with Multiple Outlets

Microfluidic devices for comprehensive three-dimensional spatial liquid chromatography will ultimately require a body of stationary phase with multiple in- and outlets. In the present work, 3D printing with a transparent polymer resin was used to create a simplified device that can be seen as a unit cell for an eventual three-dimensional separation system. Complete packing of the device with 5-μm C18 particles was achieved, with reasonable permeability. The packing process could be elegantly monitored from the pressure profile, which implies that optical transparency may not be required for future devices. The effluent flow was different for each of the four outlets of the device, but all flows were highly repeatable, suggesting that correction for flow-rate variations is possible. The investigation into flow patterns through the device was supported by computational-fluid-dynamics simulations. A proof-of-principle separation of four standard peptides is described, with mass-spectrometric detection for each of the four channels separately. SUPPLEMENTARY INFORMATION: The online version contains supplementary material available at 10.1007/s10337-022-04156-w

Confinement of Monolithic Stationary Phases in Targeted Regions of 3D-Printed Titanium Devices Using Thermal Polymerization

In this study, we have prepared thermally initiated polymeric monolithic stationary phases within discrete regions of 3D-printed titanium devices. The devices were created with controllable hot and cold regions. The monolithic stationary phases were first locally created in capillaries inserted into the channels of the titanium devices. The homogeneity of the monolith structure and the interface length were studied by scanning a capacitively coupled conductivity contactless detector (C4D) along the length of the capillary. Homogeneous monolithic structures could be obtained within a titanium device equipped with a hot and cold jacket connected to two water baths. The confinement method was optimized in capillaries. The sharpest interfaces (between monolith and empty channel) were obtained with the hot region maintained at 70 ºC and the cold region at 4 or 10ºC, with the latter temperature yielding better repeatability. The optimized conditions were used to create monoliths bound directly to the walls of the titanium channels. The fabricated monoliths were successfully used to separate a mixture of four intact proteins using reversed-phase liquid chromatography. Further chromatographic characterization showed a permeability (Kf) of similar to 4 x 10-15 m2 and a total porosity of 60%