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Dielectric behaviour of α-cyclodextrin, heptakis (2,3,6-tri-Omethyl)-β-cyclodextrin, randomly methylated β-cyclodextrin and low frequency Raman spectra of α- and β-cyclodextrins

The frequency and temperature dependence of the real (ε′) and imaginary (ε″)parts of the dielectric constant of α-cyclodrextrin (form 1; α-CD. 5.9H2O) and α-cyclodextrin (form III; α-CD.7.6H2O) and of the corresponding dried forms (α-CD.1.1H2O, α-CD.2.9H2O, respectively) has been investigated over the frequency range 0–100 k Hz and temperature range 130–350 K. In addition the dielectric behaviour has been investigated of heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin (β-CD.TRIME. 0.3H2O) and randomly methylated β-cyclodextrin (β-CD.RAME.0.8H2O). The dielectric behaviour is described well by Debyetype relaxation (α-disperson). All α-CD systems exhibit an additional ω-dispersion at low frequencies, which is attributed to proton transport. The fact that the ε′ values of α-CD form III are larger than those of α-CD form I is attributed to the different numbers and different strengths of the intramolecular hydrogen bonds. Form III has a stable conformation which is shown by the constant values of ε′ in the temperature range 125–250 K. By contrast, in form I the ε′ values increased linearly with temperature, indicating that the system passed through succesive conformations. The temperature dependence of ε″ and phase shift ∞ in all the specimens of α-CD (forms I, III) and fully methylated β-CD do not reveal any orderdisorder transition, because the developed hydrogen bonds ae not of the flip-flop type according to their crystal structures. The partially methylated β-CD reveals the characteristics of the order-disorder transition, which was observed before in the systems dried β-CD.2H2O and non-dried β-CD.9.8H2O. There is a direct relation between the hydroxyl groups of β-CD and the order-disorder transition. The order-disorder transition could also be shown in dried β-CD.2.4H2O and non-dried β-CD.9.8H2O samples but not in dried α-CD.1.1H2O and non-dried a-CD.5.9H2O samples, by low frequency Raman spectroscopy (< 180 cm−1). The step-like temperature dependence of the band at 33.7cm−1 reveals a transition at about 223K for both β-CD samples. In the case of α-CD samples the almost linear temperature dependence of the band at 49.1 cm−1 does not reveal any transition.