In traditional spin echo double resonance (SEDOR), the echo amplitude
M is decreased when the observed spins S are flipped by pi together wi
th the pi refocusing pulse on the observed spins I; the dependence on
tau is then determined. In the new version of SEDOR, the echo amplitud
e is measured as a function of the S spin flip angle theta at a consta
nt pulse spacing tau. The analysis is simple and powerful for long tau
, where the strong collision limit applies. There, the variation of M
with theta can be fit, yielding the number n of spins S to which each
spin I is coupled. Data from amorphous silicon with H-1 and D-2 show t
he described effect. A MAS version of the new method is used on multip
ly labeled alanine and urea, with results in good agreement with the p
redictions for n = 2, as expected. By Fourier transforming M with resp
ect to the flip angle theta, a stick spectrum results; the largest num
bered non-vanishing stick yields the number n of spins S coupled to ea
ch spin I. Simulations are presented for an n = 2 system. The present
technique is compared to the multiple-quantum spin-counting method, (C
) 1998 Academic Press.