Pulse Sequence
User Manual Version 002 BRUKER BIOSPIN 157 (327)
Pulse Sequence 12.1
Figure 12.1. REDOR Pulse Sequence
Setup 12.2
The example of setup given here is based on a biological sample, but of course
the procedure will not change if you are going to analyze different samples with
different combinations of coupled spins.
Sample: fully labelled
15
N/
13
C
a
Glycine (diluted in natural abundance glycine to
10%). Dilution will reduce long range dipolar interactions strongly and lead to a
well defined direct interaction between
15
N and
13
C
a
, so that a single frequency
dipolar modulation is obtained. A triple resonance probe with the X channel tuned
to
13
C and the Y channel tuned to
15
N is required. Set
13
C observe with cross po-
larization from protons. It is recommended that separate preamps are used for C
and N so observation can be changed between C and N without rewiring. There
should be an X-low pass filter or
13
C bandpass filter on
13
C, a
15
N low pass or
bandpass on
15
N.
MAS rate: 5-10 kHz. The MAS spinning speed should be stable within 1 to 2 Hz in
order to get a well refocused echo.
Overall Experimental time, including setup procedure: 3-5 hours.
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