Table 5.
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 C18 column with a variety of 70/30 THF/solvent j mobile phases. Instrumentation: Agilent 1100 with a variable wavelength detector set to 230 nm. Other conditions: injection volume = 1.0 µL; flow rate = 0.30 mL min−1; column temperature varied from 10 °C to 60 °C.
| 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 | |||
| C18 | 70/30 (v/v) THF/MeOH | 46890 | 0.354 | 6.0 | 0.349 | 4.5 | 0.345 | 3.3 | 0.342 | 2.4 | 0.337 | 0.9 | 0.334 |
| 20310 | 0.544 | 2.3 | 0.541 | 1.7 | 0.539 | 1.3 | 0.537 | 0.9 | 0.533 | 0.2 | 0.532 | ||
| 7360 | 0.698 | 0.0 | 0.698 | 0.0 | 0.698 | 0.0 | 0.698 | 0.0 | 0.697 | −0.1 | 0.698 | ||
| 3070 | 0.783 | −1.0 | 0.785 | −0.8 | 0.787 | −0.5 | 0.788 | −0.4 | 0.789 | −0.3 | 0.791 | ||
| 70/30 (v/v) TH F/ACN | 46890 | 0.329 | 2.2 | 0.328 | 1.9 | 0.326 | 1.2 | 0.325 | 0.9 | 0.323 | 0.3 | 0.322 | |
| 20310 | 0.526 | 0.4 | 0.526 | 0.4 | 0.525 | 0.2 | 0.525 | 0.2 | 0.524 | 0.0 | 0.524 | ||
| 7360 | 0.688 | −1.1 | 0.690 | −0.9 | 0.691 | −0.7 | 0.693 | −0.4 | 0.694 | −0.3 | 0.696 | ||
| 3070 | 0.779 | −1.6 | 0.782 | −1.3 | 0.785 | −0.9 | 0.787 | −0.6 | 0.790 | −0.3 | 0.792 | ||
| 70/30 (v/v) THF/EtOH | 46890 | 0.362 | 6.2 | 0.356 | 4.4 | 0.352 | 3.2 | 0.348 | 2.1 | 0.343 | 0.6 | 0.341 | |
| 20310 | 0.549 | 2.2 | 0.545 | 1.5 | 0.543 | 1.1 | 0.541 | 0.7 | 0.538 | 0.2 | 0.537 | ||
| 7360 | 0.701 | −0.1 | 0.700 | −0.3 | 0.701 | −0.1 | 0.701 | −0.1 | 0.701 | −0.1 | 0.702 | ||
| 3070 | 0.786 | −1.1 | 0.787 | −1.0 | 0.789 | −0.8 | 0.791 | 0.5 | 0.793 | −0.3 | 0.795 | ||
| 70/30 (v/v) THF/IPA | 46890 | 0.354 | 6.0 | 0.349 | 4.5 | 0.348 | 4.2 | 0.341 | 2.1 | 0.338 | 1.2 | 0.334 | |
| 20310 | 0.541 | 2.1 | 0.537 | 1.3 | 0.535 | 0.9 | 0.533 | 0.6 | 0.533 | 0.6 | 0.530 | ||
| 7360 | 0.692 | −0.4 | 0.692 | −0.4 | 0.690 | −0.7 | 0.693 | −0.3 | 0.695 | 0.0 | 0.695 | ||
| 3070 | 0.777 | −1.4 | 0.779 | −1.1 | 0.777 | −1.4 | 0.784 | −0.5 | 0.787 | −0.1 | 0788 | ||
| 100% THF | 46890 | 0.342 | 3.3 | 0.340 | 2.7 | 0.339 | 2.4 | 0.337 | 1.8 | 0.333 | 0.6 | 0.331 | |
| 20310 | 0.538 | 1.1 | 0.537 | 0.9 | 0.536 | 0.8 | 0.535 | 0.6 | 0.532 | 0.0 | 0.532 | ||
| 7360 | 0.704 | −0.1 | 0.705 | 0.0 | 0.705 | 0.0 | 0.706 | 0.1 | 0.705 | 0.0 | 0.705 | ||
| 3070 | 0.797 | −0.7 | 0.799 | −0.5 | 0.800 | −0.4 | 0.802 | −0.1 | 0.802 | −0.1 | 0.803 | ||