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76 Chapter 4
As quantitative digest of the samples 3a-d is not sufficient, detection and determination
of the DL contents (5-NH2-ip) from 1 H-NMR measurements was not possible.
Nevertheless, the IR spectra of these samples provide a qualitative evidence for the 5-NH2-
ip incorporation. Indeed, the observed bands at 1651 cm -1 and 1264 cm -1 stem from δ(N-
H) and ν(C-N) vibrations of the 5-NH2-ip (Figure 4.11). In case of the 5-Br-ip (samples 4ac),
the gradual increase of intensities of the respective signals in both 1 H-NMR and TEM-
EDX spectra suggests the presence of DL in these Ru-DEMOFs (see Figures 4.13 and 4.14).
Figure 4.14. 1 H-NMR spectra of the Ru-DEMOFs (4a-4c) digested in DCl/DMSO-d 6 mixture.
DL is 5-Br-ip. H 3 O + comes from H 2 O and HCl contained in DCl. Due to the sensitivity of H 2 O
peak to the solution conditions, the proton resonance of H 3 O + varies here, dependent on pH
value of the total solution.
4.2.2 Porosity of Ru-DEMOF samples and the confirmation of the DL incorporation
To support further the framework incorporation of the DL and rule out its extra
framework inclusion within the pores in a high quantity, we have carried out N2 sorption
measurements for the activated samples. The N2 sorption isotherms at 77 K for all samples