Dataset for Mixed-Phase Titania foams via 3D-Printing for Pharmaceutical Degradation

Data collection method:

XRD — Sampling between 2θ of 20–90 with Cu K alpha X-rays. HPLC — Degradation experiments used 1 mL samples taken every 15 or 30 minutes. Analysis was performed on a Thermo Scientific Ultimate 3000 liquid chromatograph with a UV detector. CBZ analysis used a Thermo Scientific Acclaim 120 C18 column (3.0 × 75.0 mm, particle size 3.0 µm) and a Thermo Scientific Acclaim 120 C18 guard column (R) 120 C18 (3.0 × 10.0 mm, particle size 5.0 µm). The mobile phase was made up using 5.0 mM phosphoric acid and acetonitrile 70:30 (v:v) with a flow rate of 0.8 mL min⁻¹, injection volume of 20 µL and detection wavelength of 285 nm. NMR analysis of the titania photoresist was conducted as the orange product (Ti(IV) acrylate) and acrylic acid precursor were dissolved in deuterated chloroform (CDCl3) for analysis on a 400 MHz Bruker Avance III NMR spectrometer Thermogravimetric analysis was conducted using a Setsys Evolution TGA 16/18 by Setaram, with the acquisition program Calisto. 20 mg of sample was loaded in an open alumina crucible. Prior to the analysis, samples were degassed at 90 °C for 1h and 350 °C for 8h at 10 °C min-1 to remove water from the surface. Analysis was performed under air or argon atmosphere (20 mL min-1) and heated up to 800 °C for 1h at a rate of 10 °C min-1. The rheometry of all resins used in this study was conducted on a Brookfield HADV-III Ultra-Viscometer with a CP52 cone spindle. Raman spectra used in this work were collected using a Renishaw InVia Confocal Raman microscope, excitation laser wavelength 532 nm, 100% laser power at 74 mW on the sample with 2.6 s exposure time, and a diffraction grating of size 1800 I/ mm with slit opening of 65 mm. Detector used was a 1040 × 256 pixel CCD camera.

Technical details and requirements:

NMR data requires use of MaestReNova 15 (Mnova 15.0.0) Download available using https://mestrelab.com/download/mnova/