Nuclear quadrupole double resonance spectrometer with magnetic property measurement system direct current superconducting quantum interference device detector and automatic tuning

A new nuclear quadrupole double resonance spectrometer based on a commercial superconducting quantum interference device (SQUID) setup (a Magnetic Property Measurement System (MPMS) from Quantum Design) is described. The experiment involves the indirect detection of pure quadrupole resonances (PQR) of a dilute spin system via the direct SQUID detected NMR of an abundant spin system. The experiment is conducted at low (3–20 K) temperatures and the magnetic field is cycled between a high (5.5 T) polarizing field, to an intermediate (0.1 T) detection field, to zero field where the sample is irradiated with a modulated search RF and back to the detection field. Loss of the NMR signal indicates the detection of a PQR. The RF circuit used for both the NMR and zero field irradiation is digitally controlled. Use of the External Device Control allows for the complete automation of the system. Test measurements on diphenyl ether are in good agreement with previously reported results. Pure ¹⁷O quadrupole resonances were detected for spin systems with concentrations as low as 120 μM.