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29Si sensitivity test

PRELIMINARY SET-UP
Standard 29Si sensitivity test sample: 85% Hexamethyldisiloxane in benzene-d6.
  • Record a 1H-coupled 29Si spectrum.
  • PARAMETER SET
    The calibration of the 29Si sensitivity test is performed using the standard 1H-coupled 29Si parameter set (the pulse program is set to pulprog zg).  

    MODIFY SPECIFIC PARAMETERS
    It is very important to use a long recycle delay, usually d1=5*T1(29Si) (for instance d1=1000 s). Use a single scan (ns=1).

    Set p1 to the 90º 29Si observe pulse at high power level pl1. This pulse is calibrated reaching the maximum signal for 90º and null point in 180º.

    o1 is set on-resonance of the target resonance.

    ACQUISITION
    PROCESSING
    . Reference the line to 15.28ppm and plot the spectrum between 50 and -15 ppm. The Hexamethyldisiloxane has around ten pekas with a J-coupling of 6.66 Hz. The signal to noise ratio is calculated by typing sino real over a range of 10ppm. The quarz glas tubes give a background signal around -100ppm with a linewidth of approx. 4.8kHz.
    PLOT
    OBSERVATIONS