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decomposition (ESI Table S3). The inability of this MFI material to catalyse H2O2 atalysts 2015d,ec5omposition at a similar Fe loading to that found in TS-1 as impurities clearly 231 indicates that Ti is required for decomposition to proceed, in good agreement with previous studies [18]. Accordingly, we re-focused our attention on spectroscopic study of the Ti active sites with mor Accordingly, we re-focused our attention on spectroscopic study of the Ti active nsitive spectroscopic techniques. UV-resonance enhanced Raman (UVR) spectroscopy is a particularl sites with more sensitive spectroscopic techniques. UV-resonance enhanced Raman omising tec(hUnViqRu)es,pegcitvroesncoiptsy aisbailiptayrttiocudlairleycptlryompirsoinbge ttehchenTiqiuae,cgtivensitseasbpileitcyiatotidoinreoctflyeach catalys prove sensitivity, minimise fluorescence, and selectively probe the different active sites prese probe the Ti active site speciation of each catalyst, improve sensitivity, minimise fluorescence, and selectively probe the different active sites present through the rough the resonance Raman effect [19–21]. The tremendous insight offered by UVR is illustrate resonance Raman effect [19–21]. The tremendous insight offered by UVR is illustrated Figure 7. Irradiating TS-1 with a progressively higher energy excitation wavelength allows the LMC in Figure 7. Irradiating TS-1 with a progressively higher energy excitation wavelength IV IV IV nds of the TaillowssptehceieLsMtCoTbbeanpdrosboefdth,eaTnid lsepaedcisestototbhepirdoebnetdi,fiacnadtiloeandosftoTthiei-dsepnetcifiifciactivoinbrations mor IV of Ti -specific vibrations more sensitively and selectively. Furthermore, vibrations nsitively and selectively. Furthermore, vibrations that are totally undetectable by conventional Rama that are totally undetectable by conventional Raman spectroscopy with IR (Figure 7a) ectroscopy with IR (Figure 7a) and visible (Figure 7b) sources are also observed due to resonanc and visible (Figure 7b) sources are also observed due to resonance enhancement hancement effects, although it should be added that species that do not undergo resonanc effects, although it should be added that species that do not undergo resonance hancement wenihllancoetmeexnptewriielnl nceotiemxpreoriveendcediemtepcrtoavbeidlidtye.tectability. Figure 7. Impact of Raman excitation laser wavelength on Raman spectrum of Figure 7. Impact of Raman excitation laser wavelength on Raman spectrum of TS-1. TS-1. (a) TS-1 @785 nm excitation; (b) TS-1 @514 nm excitation; (c) TS-1 @325 nm (a) TS-1 @785 nm excitation; (b) TS-1 @514 nm excitation; (c) TS-1 @325 nm excitation; excitation; (d) silicalite-1 @325 nm excitation. (d) silicalite-1 @325 nm excitation. The 325 nm UV-Raman spectrum of TS-1 is presented in Figure 7c. In addition to −1 the two vibrations related to the zeolite framework at 380 and 800 cm (also present The 325 nm UV-Raman spectrum of TS-1 is presented in Figure 7c. In addition to the two vibratio lated to the zeolite framework at 380 and 800 cm−1 (also present in Ti-free silicalite-1, Figure 7d), fo brations associated with the TiIV active sites are visible at 523, 640, 960 and 1125 cm− he first band (532 cm−1) has previously been assigned to the symmetric stretching vibration amework Ti–O–Si species [22,23]. Both the 960 and 1125 cm−1 bands have also been attributed to th iIV active sites of TS-1. These arise from the combination of three asymmetric stretching modes of 108 e rt mn h nT a e p n n n eu i 1 o etrahedral [Ti(OSi) ] unit (960 cm−1), and a totally symmetric stretching mode, i.e., breathing mode, oPDF Image | Zeolite Catalysis
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