Bruker BioSpin Solid State NMR User Manual

Double-CP
User Manual Version 002 BRUKER BIOSPIN 265 (327)
2D Data Acquisition 20.3
Sample:
15
N,
13C
-labeled histidine, peptide or protein.
Spinning speed: 10 – 15 kHz, depending on
13
C spectral parameters (rotational
resonance must be avoided)
Experiment time: 30 min. – several hours
Acquisition Parameters:
Table 20.2. Recommended Parameters for the DCP 2D Setup
Parameter Value Comments
Pulse program doubcp Pulse program
nuc1
13
C Nucleus on f1 channel
o1p 100 ppm
13
C offset
nuc2
1
H Nucleus on f2 channel
o2p 2-4 ppm
1
H offset, optimize
nuc3
15
N Nucleus on f3 channel
o3p 65 – 150 ppm
15
N offset depending on sample
pl1 Power level for f1 channel, NC contact pulse
pl3 Power level for
15
N channel HN contact
pl5 Power level for
15
N channel, NC contact pulse
pl12 Power level decoupling f2 channel and excitation
p3 Excitation pulse f2 channel
pcpd2 Decoupler pulse length f2 channel (
1
H) TPPM
p15 1-5 msec First contact, optimize on
15
N cp spectrum
p16 3-10 msec Second contact f1 – f3 channel, optimize on 1D dcp spectrum
d1 5-10 s for histidine Recycle delay, optimize on 1d
spnam0 Ramp for 1
st
CP step; e.g. ramp: 80 – 100%
sp0 Power level for Ramp HN contact pulse 1H
spnam1 tcn5500 Tangential or ramp contact pulse
spnam2 square.100 Shape on
15
N channel
cpdprg2 SPINAL64 SPINAL64 decoupling
ns 2 or 16 Number of scans
F2 direct
13
C (left column)
td 2k Number of complex points

Bruker BioSpin Solid State NMR Specifications

General

Brand	Bruker BioSpin
Model	Solid State NMR
Category	Measuring Instruments
Language	English