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154 Chapter 7
internal standards and normalizing the signals to the DMSO-d6 signal. The samples were
digested in 0.5 ml DMSO-d6 and 0.1 ml DCl (38 wt %)/D2O(99 %) in a NMR tube. Spectra
for Ru-(DE)MOFs were collected with 512 scans and for the other samples with 128 scans.
7.1.4 Thermogravimetric analyses (TGA)
The thermogravimetric analyses (TGA) data were collected and analyzed by W. Zhang
using a TG/DSC NETZSCH STA 409 PC instrument at a heating rate of 5 K min -1 in a
temperature range from 30–600 °C at atmospheric pressure under flowing N2 (N2
,99.999%; gas flow, 20 ml min -1 ). The sample weight is in a range of 7-12 mg. Activated
sample was filled in a crucible with a vial in an Ar-filled glove-box and immediately used
for the measurement.
7.1.5 Scanning Electron Microscopy (SEM) and Energy-dispersive X-ray
spectroscopy (EDX)
SEM images and EDX mapping were recorded from an FEI ESEM Dual Beam TM Quanta 3D
FEG microscope by Dr. K. Khaletskaya and S. Cwik. In order to increase the conductivity
of MOF samples, they were coated with gold by Dr. R. Neuser prior to being loaded in the
instrument. Sample preparation for the SEM measurement and analysis were done by W.
Zhang.
7.1.6 Transmission electron microscope (TEM) and EDX
Bright filed transmission electron microscope (BFTEM) images and EDX spectra for the
composition determination of Ru-DEMOFs were recorded on a Tecnai G 2 F20 equipped
with a Schottky field emission gun operated at an acceleration voltage of 200 kV by Dr. C.
Wiktor at the department of Mechanical Engineering, Ruhr-University Bochum. Data
analysis was done by W. Zhang.
7.1.7 Elemental Analysis / Atomic absorption spectroscopic (AAS)
EA / AAS analysis data for Ru-(DE)MOFs were obtained from the Mikroanalytisches
Laboratorium Kolbe in Mülheim an der Ruhr (http://www.mikro-lab.de/index.html).
Samples were filled into finger schlenks in an Ar-filled glove-box by W. Zhang and