title: 3D-Printing inside the Glovebox: A Versatile Tool for Inert-Gas Chemistry Combined with Spectroscopy.
abstract: 3D-Printing with the well-established 'Fused Deposition Modeling' technology was used to print totally gas-tight reaction vessels, combined with printed cuvettes, inside the inert-gas atmosphere of a glovebox. During pauses of the print, the reaction flasks out of acrylonitrile butadiene styrene were filled with various reactants. After the basic test reactions to proof the oxygen tightness and investigations of the influence of printing within an inert-gas atmosphere, scope and limitations of the method are presented by syntheses of new compounds with highly reactive reagents, such as trimethylaluminium, and reaction monitoringviaUV/VIS, IR, and NMR spectroscopy. The applicable temperature range, the choice of solvents, the reaction times, and the analytical methods have been investigated in detail. A set of reaction flasks is presented, which allow routine inert-gas syntheses and combined spectroscopy without modifications of the glovebox, the 3D-printer, or the spectrometers. Overall, this demonstrates the potential of 3D-printed reaction cuvettes to become a complementary standard method in inert-gas chemistry.
authors.affiliation: Institute of Organic Chemistry Clausthal University of Technology Leibnizstr. 6 DE-38678 Clausthal-Zellerfeld.
authors.forename: Felix
authors.initials: F
authors.lastname: Lederle
authors.affiliation: Institute of Organic Chemistry Clausthal University of Technology Leibnizstr. 6 DE-38678 Clausthal-Zellerfeld.
authors.forename: Christian
authors.initials: C
authors.lastname: Kaldun
authors.affiliation: Institute of Organic Chemistry Clausthal University of Technology Leibnizstr. 6 DE-38678 Clausthal-Zellerfeld.
authors.forename: Jan C
authors.initials: JC
authors.lastname: Namyslo
authors.affiliation: Institute of Organic Chemistry Clausthal University of Technology Leibnizstr. 6 DE-38678 Clausthal-Zellerfeld.
authors.forename: Eike G
authors.initials: EG
authors.lastname: Hübner
keywords: 3D‐Printing; Inert‐gas synthesis; NMR Spectroscopy; Online analytics; Trimethylaluminium