Standard ²⁹Si sensitivity test sample: 85% Hexamethyldisiloxane in benzene-d₆.

Insert the sample (ij).

Choose the solvent deuterium signal with the lock command

Tune and match the probehead (wobb or atma if required).

Optimize the shim procedure (read an optimized shim file with the rsh command or performs a gradshim if required).

Record a ¹H-coupled ²⁹Si spectrum.

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).  

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.

Start acquisition by rga and zg (the expected experimental time is displayed with the expt command).

The recorded data is Fourier transformed with ft (or ef) and phase and baseline corrections are performed using apk and abs, respectively. Modify processing parameters if required from the ProcPars section or using the ased command.. 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.

Use the TOPSPIN plot editor (xwinplot)