title: Electron spin resonance studies of trityl OX063 at a concentration optimal for DNP.
abstract: We have performed temperature-dependent electron spin resonance (ESR) measurements of the stable free radical trityl OX063, an efficient polarizing agent for dissolution dynamic nuclear polarization (DNP), at the optimum DNP concentration (15 mM). We have found that (i) when compared to the W-band electron spin-lattice relaxation rate T1e(-1) of other free radicals used in DNP at the same concentration, trityl OX063 has slower T1e(-1) than BDPA and 4-oxo-TEMPO. At T > 20 K, the T1e(-1)vs. T data of trityl OX063 appears to follow a power law dependence close to the Raman process prediction whereas at T < 10 K, electronic relaxation slows and approaches the direct process behaviour. (ii) Gd(3+) doping, a factor known to enhance DNP, of trityl OX063 samples measured at W-band resulted in monotonic increases of T1e(-1) especially at temperatures below 20-40 K while the ESR lineshapes remained essentially unchanged. (iii) The high frequency ESR spectrum can be fitted with an axial g-tensor with a slight g-anisotropy: g(x) = g(y) = 2.00319(3) and g(z) = 2.00258(3). Although the ESR linewidth D monotonically increases with field, the temperature-dependent T1e(-1) is almost unchanged as the ESR frequency is increased from 9.5 GHz to 95 GHz, but becomes faster at 240 GHz and 336 GHz. The ESR properties of trityl OX063 reported here may provide insights into the efficiency of DNP of low-γ nuclei performed at various magnetic fields, from 0.35 T to 12 T.
authors.affiliation: Advanced Imaging Research Center, University of Texas Southwestern Medical Center, Dallas, Texas 75390, USA.
authors.forename: Lloyd
authors.initials: L
authors.lastname: Lumata
authors.forename: Zoltan
authors.initials: Z
authors.lastname: Kovacs
authors.forename: A Dean
authors.initials: AD
authors.lastname: Sherry
authors.forename: Craig
authors.initials: C
authors.lastname: Malloy
authors.forename: Stephen
authors.initials: S
authors.lastname: Hill
authors.forename: Johan
authors.initials: J
authors.lastname: van Tol
authors.forename: Lu
authors.initials: L
authors.lastname: Yu
authors.forename: Likai
authors.initials: L
authors.lastname: Song
authors.forename: Matthew E
authors.initials: ME
authors.lastname: Merritt
mesh_terms: D004578:Electron Spin Resonance Spectroscopy; D004583:Electrons; D005609:Free Radicals / Q000737:chemistry*; D005682:Gadolinium / Q000737:chemistry; D013438:Sulfhydryl Compounds / Q000737:chemistry*; D013696:Temperature
chemical_list: D005609:Free Radicals; D013438:Sulfhydryl Compounds; C585292:tris(8-carboxyl-2,2,6,6-benzo(1,2-d-4,5-d)-bis(1,3)dithiole-4-yl)methyl sodium salt; D005682:Gadolinium