PubMed · 206802
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P C Jost, O H Griffith. 1978. The spin-labeling technique.. https://doi.org/10.1016/s0076-6879(78)49019-6
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The response of the cavity to the rotation of a point-like sample in the horizontal (y-z) plane passing through the center of the Bruker double TE(104) and single TE(102) rectangular cavities in concentric circles of radii rho = 0, 1, 2, 3, 4, and 5 mm from the cavity center (radial effect) has been analyzed. The experimentally observed dependencies of the EPR signal intensity, I(pp), showed the following: (i) for rho = 0 mm (a sample position in the cavity center), I(pp) is independent of the angle of rotation; (ii) for rho = 1, 2, and 3 mm, the I(pp) dependence progressively changes from circular to oval; (iii) when the radius is further increased to rho = 4 and 5 mm, the I(pp) dependence changes dramatically, giving a figure eight shape. These experimental observations are in very good agreement with the theoretical calculations, in which the response is modeled using modified Cassinian curves, K(rho, phi). Similar trends were observed for any position of the horizontal (y-z) plane at which the sample is situated along the vertical x axis of the cavity; however, the amplitude of the signal decreases with increase in the absolute value of the x coordinate, ||x ||. The variation in the signal amplitude along the cavity x axis (longitudinal effect) can be calculated theoretically using a modified sine-squared curve, G(x). In general, the response of the cavity to a point-like sample situated at any position, P(rho, phi, x), can be represented as a product of the mentioned Cassinian curve, K(rho, phi), and sine-squared curve, G(x), giving for the signal intensity I(pp)(rho, phi, x) approximately K(rho, phi)G(x). The response to a large cylindrical sample which is concentrically situated on the cavity x axis can then be obtained by integrating the above product, K(rho, phi)G(x), over the sample volume. The nonlinear radial effect may give rise to a serious source of systematic error in quantitative EPR spectroscopy and shows that accurate and precise positioning of the sample in the microwave cavity is essential.
A four-pulse version of the pulse double electron-electron resonance (DEER) experiment is presented, which is designed for the determination of interradical distances on a nanoscopic length-scale. With the new pulse sequence electron-electron couplings can be studied without dead-time artifacts, so that even broad distributions of electron-electron distances can be characterized. A version of the experiment that uses a pulse train in the detection period exhibits improved signal-to-noise ratio. Tests on two nitroxide biradicals with known length indicate that the accessible range of distances extends from about 1.5 to 8 nm. The four-pulse DEER spectra of an ionic spin probe in an ionomer exhibit features due to probe molecules situated both on the same and on different ion clusters. The former feature provides information on the cluster size and is inaccessible with previous methods.
Three-dimensional pulsed ESR imaging was performed on a (FA)(2)PF(6) crystal using a three-dimensional Fourier imaging sequence. The best resolution achieved was of 20 microm(3). Comparison with images obtained using the filtered back-projection method shows the superiority of this method under the given conditions.