Table 2: Performed experiments with PLAC using setup 2 and PH-INEPT+.
First, the hydrogenation conditions, i.e. hydrogenation duration and temperature, were optimized (PLAC.E1 and PLAC.E2). The free evolution intervals tIN,1 and tIN,2 of the sequence were varied in another experiment PLAC.E3 with a fixed hydrogenation duration thydr = 5 s. The influence of the buffer solutions B.2 and B.3 was examined in an additional set of experiments (PLAC.E4).
Buffer | Timings / Parameters | |
---|---|---|
PLAC.E1 | B.2 |
tpH2 = 2 s, Variation of tbypass tIN,1 = 60.0 ms, tIN,2 = 50.0 ms 60° C |
PLAC.E2 | B.2 |
tpH2 = 2 s, Variation of tbypass tIN,1 = 60.0 ms, tIN,2 = 70.0 ms 90° C |
PLAC.E3 | B.2 |
tpH2 = 2 s, tbypass = 3 s Variation of tIN,1 and tIN,2 90° C |
PLAC.E4 | B.2/3, or no buffer |
tpH2 = 2 s, tbypass = 3 s tIN,1 = 87.8 ms, tIN,2 = 70.7 ms 90° C |