Table 9.
Calculated Ksec and% OKsec (from the reference Ksec at 60 °C) from elution volumes obtained for PMMA standards (Mp 46,890; 20,310; 7360; 3070) on phenyl column with a variety of 70/30 THF/solvent j mobile phases. Instrumentation and other conditions are as in Table 5.
| Column ID | Mobile Phase | PMMA Mp | Temperature |
||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| 10 °C |
20 °C |
30 °C |
40 °C |
50 °C |
60 °C | ||||||||
| Ksec | % ∆Ksec | Ksec | % ∆Ksec | Ksec | % ∆Ksec | Ksec | % ∆Ksec | Ksec | % ∆Ksec | Ksec Reference | |||
| Phenyl | 70/30 (v/v) THF/MeOH | 46890 | 0.466 | 7.1 | 0.457 | 5.1 | 0.451 | 3.7 | 0.442 | 1.6 | 0.440 | 1.1 | 0.435 |
| 20310 | 0.676 | 3.4 | 0.670 | 2.4 | 0.665 | 1.7 | 0.659 | 0.8 | 0.657 | 0.5 | 0.654 | ||
| 7360 | 0.824 | 1.1 | 0.821 | 0.7 | 0.819 | 0.5 | 0.816 | 0.1 | 0.816 | 0.1 | 0.815 | ||
| 3070 | 0.898 | 0.3 | 0.897 | 0.2 | 0.896 | 0.1 | 0.894 | −0.1 | 0.407 | 0.1 | 0.895 | ||
| 70/30 (v/v) THF/ACN | 46890 | 0.417 | 3.0 | 0.414 | 2.2 | 0.413 | 2.0 | 0.409 | 1.0 | 0.407 | 0.5 | 0.405 | |
| 20310 | 0.634 | 1.3 | 0.631 | 0.8 | 0.632 | 1.0 | 0.629 | 0.5 | 0.627 | 0.2 | 0.626 | ||
| 7360 | 0.795 | 0.0 | 0.794 | −0.1 | 0.797 | 0.3 | 0.795 | 0.0 | 0.795 | 0.0 | 0.795 | ||
| 3070 | 0.879 | −0.5 | 0.879 | −0.5 | 0.883 | 0.0 | 0.882 | −0.1 | 0.882 | −0.1 | 0.883 | ||
| 70/30 (v/v) THF/EtOH | 46890 | 0.486 | 9.5 | 0.476 | 7.2 | 0.466 | 5.0 | 0.458 | 3.2 | 0.450 | 1.4 | 0.444 | |
| 20310 | 0.687 | 4.6 | 0.680 | 3.5 | 0.673 | 2.4 | 0.668 | 1.7 | 0.662 | 0.8 | 0.657 | ||
| 7360 | 0.830 | 1.7 | 0.827 | 1.3 | 0.823 | 0.9 | 0.822 | 0.7 | 0.819 | 0.4 | 0.816 | ||
| 3070 | 0.902 | 0.6 | 0.901 | 0.4 | 0.900 | 0.3 | 0.900 | 0.3 | 0.899 | 0.2 | 0.897 | ||
| 70/30 (v/v) THF/IPA | 46890 | 0.479 | 8.9 | 0.470 | 6.8 | 0.460 | 4.5 | 0.453 | 3.0 | 0.446 | 1.4 | 0.440 | |
| 20310 | 0.684 | 4.1 | 0.677 | 3.0 | 0.671 | 2.1 | 0.665 | 1.2 | 0.660 | 0.5 | 0.657 | ||
| 7360 | 0.831 | 1.6 | 0.828 | 1.2 | 0.824 | 0.7 | 0.822 | 0.5 | 0.819 | 0.1 | 0.818 | ||
| 3070 | 0.903 | 0.3 | 0.902 | 0.2 | 0.901 | 0.1 | 0.901 | 0.1 | 0.900 | 0.0 | 0.900 | ||
| 100% THF | 46890 | 0.419 | 4.0 | 0.415 | 3.0 | 0.412 | 2.2 | 0.408 | 1.2 | 0.406 | 0.7 | 0.403 | |
| 20310 | 0.628 | 1.9 | 0.624 | 1.3 | 0.622 | 1.0 | 0.619 | 0.5 | 0.618 | 0.3 | 0.616 | ||
| 7360 | 0.790 | 0.8 | 0.787 | 0.4 | 0.787 | 0.4 | 0.785 | 0.1 | 0.785 | 0.1 | 0.784 | ||
| 3070 | 0.876 | 0.3 | 0.873 | 0.0 | 0.874 | 0.1 | 0.873 | 0.0 | 0.874 | 0.1 | 0.873 | ||