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intensity upon NH HF treatment. Since the 960 and 1125 cm−1 bands have been assigned to stretching 42 modes of a purely tetrahedral [Ti(OSi)4] unit [11], it can be proposed that a general decrease in tetrahedral, framework [Ti(OSi)4] atoms occurs upon post-synthetic modification, i.e., extraction of framework Ti occurs. This is in line with the decrease in the intensity of the 210 nm band in the UV-Vis spectra −1 −1 at 695 cm is associated with the 270 nm UV-Vis band, and is hence directly (ESI Figure S2). Based on the relative intensities of the 960 and 1125 cm bands before and after proportional to the decrease in [Ti(OSi) ] atoms. It appears, therefore, that treatment 4 treatment, we estimate the concentration of the original [Ti(OSi)4] atoms have decreased by approximately of TS-1 with NH4HF2 leads to a general extraction of framework [Ti(OSi)4] atoms, 25%–50% following NH4HF2 treatment, in further agreement to the decreased intensity of the Si–O–Ti and the concurrent generation of new Ti sites, which exhibit LMCT bands at ±270 nm, band in the FTIR spectra (ESI Figure S3−).1 and a Raman stretch at 695 cm . Figure 8. UV-Raman (325 nm) spectra of (blue/bottom) TS-1 and (red/top) TS-1B. Figure 8. UV-Raman (325 nm) spectra of (blue/bottom) TS-1 and (red/top) TS-1B. The right The right inset shows the relative intensities of the 960 and 1125 cm−1 bands, whilst inset shows the relative intensities of the 960 and 1125 cm−1 bands, whilst the left inset shows the left inset shows the intensity of the 695 cm−1 band when TS-1B is excited with a 266 nm laser. the intensity of the 695 cm−1 band when TS-1B is excited with a 266 nm laser. −1 ConcurrentlyT,oagnaeiwnfRuratmhearninstsriegthcthinato6t9h5ecamctiveissiotebseprrveesden.tTihnebgoethneTrSat-i1oannodfTaSn-1eBw,wReamanbandis also performed in situ UV-Raman spectroscopy (Figure 9), where both TS-1 and in good agreement to the original UV-Vis data, which demonstrated that a new LMCT band was formed TS-1B were treated with H O . In good agreement to previous in situ Raman studies 22 (270 nm) following NH4HF2 treatment. Given that this Raman stretch is in the framework, i.e., of TS-1, complete elimination of the 960 and 1125 cm−1 bands are observed upon fingerprint, region of the Raman spectrum, it is likely associated with the TiIV active sites. However, to treatment of TS-1 with H2O2 [24,25]. Given that these bands are associated with verify if this new species was indeed responsible of the absorption band at 270 nm (ESI Figure S2), and various stretching and breathing modes of the [Ti(OSi)4] tetrahedron, the total loss is thereforeofrtehleastedstrteotctheesceaxntrbaectaiottnribouftetdheto[tThie(OchSain)4g]euinigtes,omanetrayd(dfirtoiomnateltrRahamedarnaletoxperiment at 266 nm excitation wavelength was performed (Figure 8, left inset). As can be seen, irradiating TS-1B octahedral) that occurs upon the formation of the relevant Ti-(hydro)peroxo species. We note that the original spectrum can be restored by a heat treatment at 90 ◦C, and with a 266 nm laser significantly increases the intensity of this stretch by several orders of magnitude. may even partially be restored by extended scanning under the Raman beam. The 266 nm excitation laser overlaps perfectly with the 270 nm absorbance band, thus allowing true 110PDF Image | Zeolite Catalysis
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