Experimental Section - New Synthetic Routes to Polyoxometalate Containing Ionic Liquids - page 98

quantitative evaluation of the spectral parameters (least-squares fitting to Lorentzian
peaks). The minimum experimental line widths were 0.20 mms -1 . The temperature of
the samples was controlled by an MBBC-HE0106 MÖSSBAUER He/N 2 cryostat within an
accuracy of ±0.3 K. Isomer shifts were determined relative to D -iron at 298 K.
TGA : SETARAM SETSYS Evolution TGA in upstream mode with heating rate of 5 K/min in
the temperature area of 30-600 °C, 50 Nml/min, He carrier gas stream and quartz glass
vessel (0.5 ml).
MS: UHR-TOF Bruker Daltonik (Bremen, Germany) maXis, an ESI-ToF MS capable of
resolution of at least 40,000 FWHM. Detection was in negative ion-mode and the source
voltage was 4.5 kV. The flow rates were 180 μl/hour. The drying gas (N 2 ), to aid solvent
removal, was held at 180 °C, respectively −20 °C for cryo measurements.
DSC : NETZSCH DSC 204F1, known amount of sample placed in Al pan with pierced lid,
gaseous N 2 cooling at 100% with flow rate of 20.0 ml/min and 15 K/min. Calibration
performed using an indium standard. Temperature range: -100 °C - 60 °C.