M. Mazur et al., ANALYSIS OF THE MOVEMENT OF LINE-LIKE SAMPLES OF VARIABLE-LENGTH ALONG THE X-AXIS OF A DOUBLE TE104 AND A SINGLE TE102 RECTANGULAR CAVITY, Journal of magnetic resonance [1997], 129(2), 1997, pp. 188-200
Movement of line-like samples with lengths from 5 to 50 mm along the x
-axis of the double TE104 rectangular cavity has been analyzed. The ob
served dependencies of the EPR signal intensity versus sample position
showed: (i) a sharp maximum for sample lengths from 5 to 20 mm; (ii)
a plateau, over which the EPR signal intensity remained constant withi
n experimental errors of 0.26-1.07%, for lengths from 30 to 40 mm; and
(iii) a ''sloping plateau,'' which could be approximated by the linea
r function (correlation, r = 0.98) for sample length 50 mm, Theoretica
l values of the experimentally observed dependencies of the intensity
versus sample position were calculated using the modified sine-squared
function and the correlation between observed and theoretically predi
cted dependencies is very good. The experimental dependence of the EPR
signal intensity versus the sample length for samples situated at the
same point in the cavity was nonlinear with a maximum for the 40-mm s
ample. The dependence of the EPR signal intensity upon the movement of
a large cylindrical sample (o.d. 4 mm and length 100 mm) along the x-
axis of the cavity was similar to that found for the 50-mm sample, How
ever, an additional oscillating signal superimposed on the sloping pla
teau was observed. The presence of a large sample fixed in the complem
entary cavity of the double TE104 cavity caused an additional deformat
ion of the signal intensity for a 30-mm sample which was moving in the
first cavity. The primary effect was that the plateau was replaced by
a region in which the intensity increased linearly with sample positi
on, r = 0.99. Each of the above phenomena may be a source of significa
nt errors in quantitative EPR spectroscopy, Cylindrical samples to be
compared should be of identical length and internal diameter. Accurate
and precise positioning of each sample in the microwave cavity is ess
ential. (C) 1997 Academic Press.