Determination of quadrupole parameters with a composite pulse for spurious signal suppression.

Spurious signals such as the piezoelectric signal from a ferroelectric crystal or the ringing signal from the NMR probe head tuned for low gyromagnetic ratio nuclei are often observed in pulsed NMR. Both signals are cancelled using the Hahn echo sequence with appropriate phase cyclings. The present paper applies a composite-pulse sequence to cancel the ringing signal. The main advantage of this sequence over the Hahn echo sequence is in the simplicity of optimizing the line intensity: the optimization of only one pulse duration for this sequence but of two pulse durations and the interpulse delay for the Hahn echo sequence. We are interested in half-integer quadrupole spins (I = 3/2, 5/2, 7/2, and 9/2), which means that we must consider the first-order quadrupole interaction during the pulses. For simplicity, we deal mainly with spin I = 3/2 nuclei. Since the central-line intensity depends on the ratio of the quadrupole coupling constant (QCC) to the amplitude of the RF pulse, we can determine the QCC from a featureless lineshape by fitting the variation of the experimental central-line intensity for increasing pulse duration with theoretical results. Contrary to the one-pulse sequence where the central-line intensity is proportional to the pulse duration if the latter is short, there is no such condition with the composite-pulse sequence. In other words, this sequence does not allow us to quantify the relative spin populations in powders. The size of the sample must be much smaller than that of the RF coil in order for the RF magnetic field to become homogeneous for the sample. We used (87)Rb (I = 3/2) in an aqueous solution of RbCl and in RbNb2O5F powder, (131)Xe (I = 3/2) of xenon gas physisorbed in Na-Y zeolite, and (23)Na (I = 3/2) in two well-known powders (NaNO3 and NaNO2) to support our theoretical result. Copyright 2001 Academic Press.