ABSTRACT
In this work, devices for two-dimensional separations are considered. The device contains a flow distributor, a first-dimension channel, and 17 second-dimension outlets. In the design, all connections between the first-dimension channel, the flow distributor, and the second-dimension outlets were tapered, with a minimal diameter of 20 µm. The use of photo-masking is explored for the fabrication of monolithic frits in all tapered connections. Monolithic frits with optimized permeability and length were successfully fabricated in all 33 tapered channels through light-induced polymerization, photo-masking, and selective exposure. The efficacy of the monolithic frits was demonstrated by creating a packed bed of 15-µm particles, confined within the first-dimension channel. The outlet of the first-dimension channel was successfully connected to a mass spectrometer. Effective flow confinement was demonstrated with a reversed-phase separation of a mixture of five standard peptides.
Subject(s)
Mass SpectrometryABSTRACT
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 °C and the cold region at 4 or 10 °C, 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 â¼4 × 10-15 m2 and a total porosity of 60%.
ABSTRACT
A miniaturized, flexible, and low-cost capillary ion chromatography system has been developed for anion analysis in water. The ion chromatography has an open platform, modular design, and allows for ease of modification. The assembled platform weighs ca. 0.6 kg and is 25 × 25 cm in size. Isocratic separation of common anions (F- , Cl- , NO2- , Br- , and NO3- ) could be achieved in under 15 min using sodium benzoate eluent at a flow rate of 3 µL/min, a packed capillary column (0.150 × 150 mm) containing Waters IC-Pak 10 µm anion exchange resin, and light-emitting diode based indirect UV detection. Several low UV light-emitting diodes were assessed in terms of sensitivity, including a new 235 nm light-emitting diode, however, the highest sensitivity was demonstrated using a 255 nm light-emitting diode. Linear calibration ranges applicable to typical natural water analysis were obtained. For retention time and peak area repeatability, relative standard deviation values ranged from 0.60-0.95 and 1.95-3.53%, respectively. Several water samples were analysed and accuracy (recovery) was demonstrated through analysis of a prepared mixed anion standard. Relative errors of -0.36, -1.25, -0.80, and -0.76% were obtained for fluoride, chloride, nitrite, and nitrate, respectively.
ABSTRACT
Through optimization of the printing process and orientation, a suitably developed surface area has been realized upon a 3D printed polymer substrate to facilitate chromatographic separations in a planar configuration. Using an Objet Eden 260VS 3D printer, polymer thin layer chromatography platforms were directly fabricated without any additional surface functionalization and successfully applied to the separation of various dye and protein mixtures. The print material was characterized using gas chromatography coupled to mass spectrometry and spectroscopic techniques such as infrared and Raman. Preliminary studies included the separation of colored dyes, whereby the separation performance could be visualized optically. Subsequent separations were achieved using fluorescent dyes and fluorescently tagged proteins. The separation of proteins was affected by differences in the isoelectric point (pI) and the ion exchange properties of the printed substrate. The simple chromatographic separations are the first achieved using an unmodified 3D printed stationary phase.
