Experimental Section - New Synthetic Routes to Polyoxometalate Containing Ionic Liquids - page 97

5.Experimental Section
5.1 Materials
All reagents and chemicals were supplied by SIGMA ALDRICH CHEMICAL COMPANY
LTD., FISHER CHEMICALS, ABCR CHEMICALS and ACROS ORGANICS. The materials were
used without further purification. Unless described otherwise the reactions were
conducted under ambient atmosphere.
5.2 Instrumentation
The following analytical instruments were used for analysis and characterization of the
products:
FT-IR spectroscopy : Shimadzu FT-IR-8400S spectrometer. The ionic liquid samples were
applied as thin film on the surface of a KBr crystal IR-cell and measured in transmission
mode. Intensities are denoted as vs = very strong, s = strong, m = medium, w = weak
EA: Euro Vector Euro EA 3000 elemental analyzer.
UV-Vis-spectroscopy : Shimadzu UV-2401PC spectrophotometer in transmission mode.
Quartz cuvettes with 1.0 cm optical path length were used.
1 H/ 13 C-NMR: Spectra were recorded with Jeol EX- 270 DELTA und Jeol Lambda- 400
spectrometers. Signals of educts, possible sideproducts and solvents are not mentioned.
Chemical shifts are listed according to the G scale in ppm and refer to the not
deuterated part of the solvents used [ Ɂ h (CDCl 3 ) = 7.27ppm]. Coupling constants are
listed in Hertz Hz. For the evaluation of signal multiplicities the following abbreviations
are used: s = singlet, d = doublet, t = triplet, m = multiple, dd = doublet of doublets
EPR spectroscopy: JEOL JES-FA200 ESR spectrometer with an X-band microwave unit.
Mössbauer : 57 Fe Mössbauer spectra were recorded on a with ElMössbauer
spectrometer (MRG-500) at 77 K in constant acceleration mode. 57 Co/Rh was used as
the radiation source. WinNormos for Igor Pro software has been used for the