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7 Experimental Section
In this Chapter various experimental and analytical procedures are given. In the first part,
general analytical procedures and methods broadly used for characterization of the
prepared MOF materials in this work are provided. In the second part, synthetic
procedures as well as supplementary analytical details are described for each Chapter.
7.1 General methods
7.1.1 X-ray Diffraction (XRD)
Powder XRD (PXRD) for all the bulk as-synthesized samples and most of the activated
samples were performed by Dr. M. Tu, S. Wannapaiboon, and W. Zhang on an X’ Pert PRO
PANalytical equipment (Bragg–Brentano geometry with automatic divergence slits,
position sensitive detector, continuous mode, room temperature, Cu-Kα radiation(λ =
1.54178 Å), Ni-filter, in the range of 2θ = 5–50, step size 0.01). Activated sample were
prepared on a silicon wafer in an Ar-filled glovebox right before the measurement starts.
For the measurement of activated samples (Ru-DEMOFs series 1 and 3), the data were
collected by W. Zhang with the assistance of Dr. C. Sternemann, A. Schneemann, and S.
Wannapaiboon at beam line BL9 of the synchrotron radiation facility DELTA at a
wavelength of 0.4592 Å using a two-dimensional MAR345 image plate detector. The
sample was filled into standard capillaries (0.5-mm diameter) in an Ar-filled glovebox and
measured. The data were integrated using the program package Fit2D [297] and
transformed to the CuKα radiation used for all other PXRD measurements on reported
materials for the convenient comparison. PXRD of some other activated samples were
collected by Dr. K. Khaletskaya, C. Rösler, and I. Schwedler in a D8-Advance Bruker AXS
diffractometer with CuKα radiation at 25 °C (Göbel mirror; θ–2θscan; 2θ= 5–50°; step size
= 0.0142 (2θ); position sensitive detector; α-Al2O3 as external standard. The sample was
filled into 0.7 mm diameter standard capillaries in an Ar-filled glovebox and measured in
Debye-Scherrer geometry. All the data were interpreted/analyzed by W. Zhang.