Bruker BioSpin Solid State NMR, User Manual

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12 (327) BRUKER BIOSPIN User Manual Version 002
Test Samples
13
C Adamantane
α -glycine
CP,DEC
CP 50
110
HH setup, shim
sensitivity,decoupling.Prep.: precipitate
with acetone from aq. solution, C,N fully
labelled for fast setup, recoupling, REDOR
(10% in natrl. abundance)
79
Br KBr MAS 57 d1< 50msec, angle setting
finely powdered, reduced volume
59
Co Co(CN)
6
MAS shift thermometer
55
Mn KMnO
4
MAS >500 kHz pattern
93
Nb
207
Pb PbNO
3
Pb(p-tolyl)
4
MAS
CP -150
shift thermometer, 0,753 ppm/degr.
d1>10s
5ms, 15s
29
Si Q
8
M
8
DSS,TMSS
CPMAS
CPMAS -50
0
d1>5s, reference sample 12.6/-108 ppm
reference sample 0 ppm
77
Se H
3
SeO
3
(NH
4
)
2
SeO
4
CPMAS
CPMAS 1800
-200
HH setup, 8ms contact, d1>10s
3ms, d1>4s
113
Cd Cd(NO
3
)
2
*4H
2
O CPMAS 350 15ms contact, d1>8s
195
Pt K
2
Pt(OH)
6
CPMAS -12000 1ms contact, d1>4s
199
Hg Hg(acetate)
2
Hexakis (dimethyl
sulphoxide)
Hg(II) trifluorome-
thansulfonate
CPMAS 2500
-2313
5ms contact, d1>10s
30-35ms contact, d1>10s *
2
H d-PMMA
d-PE
d-DMSO
2
WL
WL
WL
0
0
0
wideline setup d1 5s
wideline setup d1 0.5s/10s amorphous/
crystalline
exchange expt. at 315K
6
Li LiCl, Li (org.) make sure it is not
6
Li depleted, d1>60s
17
O D
2
O 0 pulse determination, 100scans,0.5s
15
N α -glycine CP 50 sensitivity, 4ms contact,4s
labelled for fast setup
35
Cl KCl WL,MAS 0 pulse determ., 100 scans
33
S K
2
S MAS 0 100 scans in a >=500 MHz instr.
14
N NH
4
Cl MAS,WL 0 100 scans, narrow line.
25
Mg
47/49
Ti Anatas MAS
39
K KCl MAS,WL 0 100 scans
Table 2.1. Setup Samples for Different NMR Sensitive Nuclei