DOI: 10.17863/cam.111767
title: Research data supporting "WATER SORPTION STUDIES WITH MESOPOROUS MULTIVARIATE MONOLITHS BASED ON UiO-66 "

description: A multivariate conformed metal-organic framework, monoUiO-66-NH2-30%-B, was created using a mixture of benzenedicarboxylate and (30 wt%) amino-benzenedicarboxylate linkers. Subsequent thermolysis induced the degradation of aminated linker, resulting in mesopore formation. The two materials were tested for water sorption properties. The following supporting data are presented: An Exeter Analytical CE-440 Elemental Analyzer was used for C, H, N analysis. A Thermo Fisher Scientific iCAP 7400 Duo ICP spectrometer was used for Zr analysis. MOF was digested in trace metal grade nitric acid and diluted with trace metal grade water. An aliquot was further diluted with water. Standard curves were prepared in the concentration range of 0.01 ppm-10 ppm using commercial standard diluted with 2% nitric acid solution. Powder X-ray diffraction patterns were obtained on a PANalytical Empyrean diffractometer fitted with an X’celerator detector and a Cu-Kα1 (λ = 1.5406 Å) source, with step size 0.002° and scanning speed 0.022° s−1 at 40 kV and 40 mA. Scanning electron microscopy used a TESCAN MIRA3 FEG-SEM at 5.0 keV. Image processing used the Oxford Instruments AzTec Suite. Samples were sputter-coated with a 5 nm layer of chromium before analysis and energy-dispersive X-ray spectroscopy was performed on Oxford Instruments X-maxN 80 EDS system. For transmission electron microscopy (TEM) analysis, monolith was crushed to a fine powder and dispersed in hexane. An aliquot was transferred to a continuous carbon-coated Cu grid, and the solvent evaporated before the sample was mounted in the instrument. Analysis was performed using a Talos F200X G2 FEG Scanning TEM with a 200 keV accelerating voltage. Images were acquired with a Ceta 4k x 4k CMOS camera. Energy dispersive X-ray (analysis used scanning TEM (STEM) mode. Images were acquired with a high-angle annular dark field (HAADF) detector and EDX spectra/maps were collected using a Super-X detector system with 4 windowless silicon drift detectors. A Bruker Avance III 500 MHz DCH Cryoprobe Spectrometer was used. Spectra were obtained using deuterated solvent stored over molecular sieves (3 Å). Chemical shifts were internally referenced to the deuterated solvent. Results were processed using Bruker TOPSPIN 3.0 software. In each case, ~13mg of sample was digested using D2SO4 with sonication at 70 °C achieving dissolution prior to dilution with DMSO-d6. Attenuated total reflectance Fourier transform infrared spectra were recorded on a Perkin-Elmer FTIR spectrometer (Model BX II). For N2 sorption, an Anton Parr Autosorb iQ-XR at 77 K was used. An oven-dried, Type A long cell, 9 mm outer diameter, LG bulb, tarred before loading was used in each case. Degassing was at 110 ℃ for 12 h. Isotherms were collected over 24-30 hours. AsiQwin version 5.21 software was used to evaluate the sorption isotherms. Thermogravimetric analysis used a TA Discovery Instrument TA-Q50. Heating rate 10 °C min−1 from 25−500 °C under dry nitrogen. A KLA iMicro nanoindenter equipped with a 50 mN force actuator and a Berkovich diamond tip was used for nanoindentation. Continuous Stiffness Measurements (CSM) were performed. Indents were performed at a maximum depth of 1000 nm and 2000 nm. A constant indentation strain rate of 0.1 s-1 was used. The maximum load was held for 1 second before unloading. The load was then held at 10% maximum load for 3 minutes upon unloading. Prior to nanoindentation studies, the monoliths were cold-mounted in an epoxy resin (Struers Epofix) and flattened by polishing. An Adventure dynamic vapour sorption analyser was combined with in-situ preheating/drying of samples and two sample balances to allow simultaneous analysis of two samples for water sorption. The system included a sample preheater (160 °C, heating rate programmable up to 10 °C min-1). The instrument could cool/heat the sample from 10 °C to at least 70 °C and covered a broad range of relative humidity (0-98 % from 10-70 °C). Digital mass flow controllers delivered wet and dry flow 0-200 sccm). The instrument ran at ambient pressure conditions. The system had a water reservoir with a 0.25 L capacity and HPLC Gradient Grade water was used. Water vapour sorption analysis was measured at 27 °C.