Table 2.
Signal ratio to DyEDTA-doped | |||||||
---|---|---|---|---|---|---|---|
Sample | MAS | sample1 |
Recycle delay (s) |
||||
Sample | temperature (K) | frequency (kHz) | 13C NMR | 1H NMR | T1n (s) | 13C NMR | 1H NMR |
1 | 24 | 6.7 | 0.14 ± 0.05 (CP) | 0.15 ± 0.05 | 3.6 ± 0.5 (1H) | 5 | 8 |
2 | 28 | 6.7 | 0.21 ± 0.08 (CP) | 0.21 ± 0.07 | 5.4 ± 0.5 (1H) | 6.5 | 8 |
3 | 23 | 6.8 | 1 | 1 | 23 ± 2 (1H) | 32 | 128 |
1 | 19 | 0 | 0.75 ± 0.30 (CP) | 0.80 ± 0.30 | 13.8 ± 1.5 (1H) | 36 | 8 |
3 | 18 | 0 | 1 | 1 | 37 ± 4 (1H) | 64 | 128 |
1 | 101 | 6.7 | 0.58 ± 0.20 (CP) | … | 3.0 ± 0.2 (1H) | 5 | … |
2 | 87 | 6.8 | 0.55 ± 0.20 (CP) | … | 4.8 ± 0.4 (1H) | 6.5 | … |
3 | 107 | 6.8 | 1 | … | 23 ± 5 (1H) | 32 | … |
6 | 89 | 0 | 0.86 ± 0.30 (CP) | 0.75 ± 0.30 | 7.4 ± 1.0 (1H) | 9.3 | 128 |
3 | 81 | 0 | 1 | 1 | 20 ± 5 (1H) | 32 | 256 |
4 | 24 | 6.6 | 0.53 ± 0.10 (DE) | 0.38 ± 0.10 | 280 ± 50 (13C) | 1600 (DE) | 256 |
0.35 ± 0.10 (CP) | 128 (CP) | ||||||
5 | 29 | 6.7 | 1 | 1 | 900 ± 100 (13C) | 2400 (DE) | 128 |
128 (CP) |
Signal ratios are corrected for differences in numbers of scans, the ratios of recycle delays to T1n values, and temperatures. 13C NMR signals are either cross-polarized (CP) or directly excited (DE).