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Chapter 5 133
spectra of all prepared Cu/Pd-BTC solids (Figure 5.9). Moreover, 1 H-NMR spectra of the
digested Cu/Pd-BTC_1-3 samples show presence of only BTC-linker (Figure 5.10). Thus,
absence of the resonances at about 1.9 ppm stemming from the acetate protons fully
supports IR results ruling out any residuals of the employed starting Pd-reactant. Hence,
the presence of Pd 2+ -sites should originate from the in-framework nodes rather than Pd 2+ -
precursor loading.
Figure 5.10. 1 H-NMR spectra of the digested activated Cu/Pd-BTC_1-3 samples. The vertical dash
line stands for the position where the peak of CH 3 -protons from the acetic acid commonly appears.
TGA suggests that thermal stability of the obtained Cu/Pd-BTC_1-3 solids is fully
preserved (in comparison with the parent Cu-BTC) [35] with the decomposition
temperatures close to 300 °C (Figure 5.11). The N2 (77 K) sorption isotherms recorded
for obtained samples reveal type I isotherm (Figure 5.12), confirming their permanent
microporosity. Brunauer-Emmett-Teller (BET) surface area of Cu/Pd-BTC_1 and _2
increase a little in comparison with parent Cu-BTC (prepared under similar conditions)
(Table 5.4), indicating that the presence of Pd 2+ incorporation as metal nodes in the