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Chapter 4 75
the Cl-amount was subsequently calculated based on the measured EA values and respective Ru :
Cl ratios.
As observed by the 1 H-NMR, TG and IR analyses, the contribution of the counter-ions and guest
molecules are mainly from Cl, OH, acetate, H2O and used linkers. In analogy to the previously
reported parent Ru-MOF [208] and the Ru-DEMOF with pydc DL, [138] in the currently discussed Ru-
DEMOFs acetic acid is also present, which is clearly evidenced by the 1 H-NMR spectra of the
digested samples. To note, the amount of the acetic acid can be considerably reduced by additional
solvent exchange procedure, namely, soaking of the activated samples in a large amount of water
while intense stirring to exchange the residue acetic acid. However, the risk of leaching out of Ru
needs also to be taken into account here. [208] Hence, our current studies dealt with the obtained
powders applying gently water soak as solvent exchange procedure to decrease the residue of the
acetic acid. And the overall concentration of the acetic acid decreased in comparison with our
previously report on the Ru-DEMOF with pydc DL in spite of the slightly decrease of Ru content.
In addition of the multiple possible status of acetic acid, starting reactant (i.e. linkers) can be also
accommodated into the framework as guest molecules or served as counter-ions, since based on
the NMR data the amount of the DL in some cases appeared to be higher than its respective feeding
amount. Besides, minor quantities of the coordinated H2O might be occluded / resided in the pores
as well, as the TG curves of the activated samples show the slight decrease in the range of 100-250
°C.
Figure 4.13. EDX spectra of the Ru-DEMOFs 4a-4c (with 5-Br-ip DL). The detection of Br
clearly indicates the presence of the employed DL.