Table 11.
Calculated Ksec and% ΔKsec (from the reference Ksec at 60 °C) from elution volumes obtained for PMMA standards (Mp 46,890; 20,310; 7360; 3070) on cyano 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 | |||
| Cyano | 70/30 THF/MeOH | 46890 | 0.414 | 6.4 | 0.412 | 5.9 | 0.402 | 3.3 | 0.396 | 1.8 | 0.392 | 0.8 | 0.389 |
| 20310 | 0.627 | 3.0 | 0.627 | 3.0 | 0.617 | 1.3 | 0.613 | 0.7 | 0.610 | 0.2 | 0.609 | ||
| 7360 | 0.799 | 1.4 | 0.802 | 1.8 | 0.791 | 0.4 | 0.789 | 0.1 | 0.788 | 0.0 | 0.788 | ||
| 3070 | 0.876 | 0.1 | 0.883 | 0.9 | 0.874 | −0.1 | 0.873 | −0.2 | 0.874 | −0.1 | 0.875 | ||
| 70/30 THF/ACN | 46890 | 0.378 | 3.6 | 0.376 | 3.0 | 0.374 | 2.5 | 0.370 | 1.4 | 0.367 | 0.5 | 0.365 | |
| 20310 | 0.597 | 1.9 | 0.595 | 1.5 | 0.594 | 1.4 | 0.590 | 0.7 | 0.588 | 0.3 | 0.586 | ||
| 7360 | 0.775 | 0.4 | 0.776 | 0.5 | 0.776 | 0.5 | 0.772 | 0.0 | 0.772 | 0.0 | 0.772 | ||
| 3070 | 0.867 | −0.1 | 0.868 | 0.0 | 0.870 | 0.2 | 0.867 | −0.1 | 0.867 | −0.1 | 0.868 | ||
| 70/30 THF/EtOH | 46890 | 0.437 | 8.7 | 0.428 | 6.5 | 0.421 | 4.7 | 0.414 | 3.0 | 0.407 | 1.2 | 0.402 | |
| 20310 | 0.647 | 4.2 | 0.641 | 3.2 | 0.635 | 2.3 | 0.630 | 1.4 | 0.625 | 0.6 | 0.621 | ||
| 7360 | 0.814 | 2.0 | 0.809 | 1.4 | 0.805 | 0.9 | 0.803 | 0.6 | 0.800 | 0.3 | 0.798 | ||
| 3070 | 0.889 | 0.3 | 0.888 | 0.2 | 0.887 | 0.1 | 0.887 | 0.1 | 0.886 | 0.0 | 0.886 | ||
| 70/30 THF/IPA | 46890 | 0.460 | 11.1 | 0.447 | 8.0 | 0.438 | 5.8 | 0.428 | 3.4 | 0.420 | 1.4 | 0.414 | |
| 20310 | 0.669 | 5.7 | 0.659 | 4.1 | 0.651 | 2.8 | 0.644 | 1.7 | 0.637 | 0.6 | 0.633 | ||
| 7360 | 0.844 | 4.5 | 0.826 | 2.2 | 0.820 | 1.5 | 0.814 | 0.7 | 0.810 | 0.2 | 0.808 | ||
| 3070 | 0.902 | 1.1 | 0.899 | 0.8 | 0.896 | 0.4 | 0.894 | 0.2 | 0.892 | 0.0 | 0.892 | ||
| 100% THF | 46890 | 0.396 | 3.4 | 0.395 | 3.1 | 0.394 | 2.9 | 0.389 | 1.6 | 0.386 | 0.8 | 0.383 | |
| 20310 | 0.614 | 1.8 | 0.613 | 1.7 | 0.613 | 1.7 | 0.607 | 0.7 | 0.606 | 0.5 | 0.603 | ||
| 7360 | 0.791 | 0.5 | 0.791 | 0.5 | 0.793 | 0.8 | 0.788 | 0.1 | 0.788 | 0.1 | 0.787 | ||
| 3070 | 0.882 | 0.2 | 0.882 | 0.2 | 0.884 | 0.5 | 0.880 | 0.0 | 0.881 | 0.1 | 0.880 | ||