Table 6.
Calculated Ksec and% ΔKsec (from the reference Ksec at 60 °C) from elution volumes obtained for PS standards (Mp 282,000; 126,000; 51,200; 19,500; 7350; 2780; 580) on C4 column with a variety of 70/30 THF/solvent j mobile phases. Instrumentation and other conditions are as in Table 4.
| 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 | |||
| C4 | 70/30 (v/v) THF/MeOH | 282000 | 0.068 | −1.4 | 0.068 | −1.4 | 0.069 | 0.0 | 0.068 | −1.4 | 0.069 | 0.0 | 0.069 |
| 126000 | 0.191 | 0.0 | 0.191 | 0.0 | 0.191 | 0.0 | 0.191 | 0.0 | 0.191 | 0.0 | 0.191 | ||
| 51200 | 0.419 | 0.2 | 0.418 | 0.0 | 0.418 | 0.0 | 0.418 | 0.0 | 0.418 | 0.0 | 0.418 | ||
| 19500 | 0.644 | 0.2 | 0.644 | 0.2 | 0.643 | 0.0 | 0.644 | 0.2 | 0.644 | 0.2 | 0.643 | ||
| 7350 | 0.812 | 0.2 | 0.811 | 0.1 | 0.811 | 0.1 | 0.812 | 0.2 | 0.811 | 0.1 | 0.810 | ||
| 2780 | 0.910 | 0.2 | 0.909 | 0.1 | 0.908 | 0.0 | 0.909 | 0.1 | 0.908 | 0.0 | 0.908 | ||
| 580 | 0.990 | 0.2 | 0.989 | 0.1 | 0.988 | 0.0 | 0.989 | 0.1 | 0.988 | 0.0 | 0.988 | ||
| 70/30 (v/v) THF/ACN | 282000 | 0.067 | 0.0 | 0.067 | 0.0 | 0.067 | 0.0 | 0.067 | 0.0 | 0.067 | 0.0 | 0.067 | |
| 126000 | 0.191 | 2.1 | 0.190 | 1.6 | 0.189 | 1.1 | 0.189 | 1.1 | 0.188 | 0.5 | 0.187 | ||
| 51200 | 0.427 | 1.7 | 0.426 | 1.4 | 0.423 | 0.7 | 0.423 | 0.7 | 0.421 | 0.2 | 0.420 | ||
| 19500 | 0.659 | 1.1 | 0.658 | 0.9 | 0.655 | 0.5 | 0.656 | 0.6 | 0.654 | 0.3 | 0.652 | ||
| 7350 | 0.825 | 0.5 | 0.825 | 0.5 | 0.824 | 0.4 | 0.824 | 0.4 | 0.823 | 0.2 | 0.821 | ||
| 2780 | 0.919 | 0.2 | 0.919 | 0.2 | 0.918 | 0.1 | 0.919 | 0.2 | 0.919 | 0.2 | 0.917 | ||
| 580 | 0.990 | −0.1 | 0.991 | 0.0 | 0.990 | −0.1 | 0.992 | 0.1 | 0.992 | 0.1 | 0.991 | ||
| 70/30 (v/v) THF/EtOH | 282000 | 0.054 | −6.9 | 0.055 | −5.2 | 0.057 | −1.7 | 0.057 | −1.7 | 0.057 | −1.7 | 0.058 | |
| 126000 | 0.161 | −1.8 | 0.162 | −1.2 | 0.163 | −0.6 | 0.163 | −0.6 | 0.163 | −0.6 | 0.164 | ||
| 51200 | 0.369 | −1.3 | 0.370 | −1.1 | 0.372 | −0.5 | 0.372 | −0.5 | 0.373 | −0.3 | 0.374 | ||
| 19500 | 0.590 | −1.2 | 0.591 | −1.0 | 0.594 | −0.5 | 0.594 | −0.5 | 0.596 | −0.2 | 0.597 | ||
| 7350 | 0.763 | −1.0 | 0.765 | −0.8 | 0.767 | −0.5 | 0.768 | −0.4 | 0.770 | −0.1 | 0.771 | ||
| 2780 | 0.869 | −0.9 | 0.871 | −0.7 | 0.873 | −0.5 | 0.874 | −0.3 | 0.876 | −0.1 | 0.877 | ||
| 580 | 0.966 | −0.6 | 0.968 | −0.4 | 0.969 | −0.3 | 0.970 | −0.2 | 0.972 | 0.0 | 0.972 | ||
| 70/30 (v/v) THF/EtOH | 282000 | 0.049 | −5.8 | 0.050 | −3.8 | 0.051 | −1.9 | 0.051 | −1.9 | 0.052 | 0.0 | 0.052 | |
| 126000 | 0.148 | 0.0 | 0.147 | −0.7 | 0.149 | 0.7 | 0.148 | 0.0 | 0.148 | 0.0 | 0.148 | ||
| 51200 | 0.353 | 0.0 | 0.352 | −0.3 | 0.354 | 0.3 | 0.352 | −0.3 | 0.353 | 0.0 | 0.353 | ||
| 19500 | 0.583 | 0.2 | 0.583 | 0.2 | 0.584 | 0.3 | 0.582 | 0.0 | 0.582 | 0.0 | 0.582 | ||
| 7350 | 0.765 | 0.4 | 0.764 | 0.3 | 0.764 | 0.3 | 0.763 | 0.1 | 0.763 | 0.1 | 0.762 | ||
| 2780 | 0.873 | 0.3 | 0.872 | 0.2 | 0.872 | 0.2 | 0.871 | 0.1 | 0.871 | 0.1 | 0.870 | ||
| 580 | 0.962 | 0.2 | 0.961 | 0.1 | 0.960 | 0.0 | 0.961 | 0.1 | 0.960 | 0.0 | 0.960 | ||
| 70/30 (v/v) THF/IPA | 282000 | 0.057 | −5.0 | 0.058 | −3.3 | 0.059 | −1.7 | 0.059 | −1.7 | 0.060 | 0.0 | 0.060 | |
| 126000 | 0.167 | −1.2 | 0.168 | −0.6 | 0.167 | −1.2 | 0.168 | −0.6 | 0.169 | 0.0 | 0.169 | ||
| 51200 | 0.378 | −1.0 | 0.380 | −0.5 | 0.380 | −0.5 | 0.381 | −0.3 | 0.382 | 0.0 | 0.382 | ||
| 19500 | 0.600 | −1.0 | 0.602 | −0.7 | 0.602 | −0.7 | 0.603 | −0.5 | 0.604 | −0.3 | 0.606 | ||
| 7350 | 0.771 | −0.8 | 0.773 | −0.5 | 0.773 | −0.5 | 0.775 | −0.3 | 0.776 | −0.1 | 0.777 | ||
| 2780 | 0.875 | −0.7 | 0.876 | −0.6 | 0.877 | −0.5 | 0.878 | −0.3 | 0.880 | −0.1 | 0.881 | ||
| 580 | 0.967 | −0.5 | 0.968 | −0.4 | 0.968 | −0.4 | 0.969 | −0.3 | 0.970 | −0.2 | 0.972 | ||
| 70/30 (v/v) THF/chloroform | 282000 | 0.048 | −4.0 | 0.048 | −4.0 | 0.049 | −2.0 | 0.049 | −2.0 | 0.050 | 0.0 | 0.050 | |
| 126000 | 0.144 | −0.7 | 0.144 | −0.7 | 0.144 | −0.7 | 0.145 | 0.0 | 0.145 | 0.0 | 0.145 | ||
| 51200 | 0.343 | −0.6 | 0.344 | −0.3 | 0.344 | −0.3 | 0.344 | −0.3 | 0.344 | −0.3 | 0.345 | ||
| 19500 | 0.567 | −0.5 | 0.569 | −0.2 | 0.569 | −0.2 | 0.569 | −0.2 | 0.570 | 0.0 | 0.570 | ||
| 7350 | 0.747 | −0.4 | 0.749 | −0.1 | 0.749 | −0.1 | 0.749 | −0.1 | 0.750 | 0.0 | 0.750 | ||
| 2780 | 0.858 | −0.3 | 0.860 | −0.1 | 0.860 | −0.1 | 0.860 | −0.1 | 0.861 | 0.0 | 0.861 | ||
| 580 | 0.960 | −0.2 | 0.962 | 0.0 | 0.962 | 0.0 | 0.962 | 0.0 | 0.962 | 0.0 | 0.962 | ||
| 100% THF | 282000 | 0.043 | −8.5 | 0.044 | −6.4 | 0.044 | −6.4 | 0.046 | −2.1 | 0.046 | −2.1 | 0.047 | |
| 126000 | 0.134 | −3.6 | 0.135 | −2.9 | 0.134 | −3.6 | 0.137 | −1.4 | 0.138 | −0.7 | 0.139 | ||
| 51200 | 0.329 | −2.1 | 0.331 | −1.5 | 0.328 | −2.4 | 0.333 | −0.9 | 0.333 | −0.9 | 0.336 | ||
| 19500 | 0.556 | −1.4 | 0.559 | −0.9 | 0.554 | −1.8 | 0.561 | −0.5 | 0.561 | −0.5 | 0.564 | ||
| 7350 | 0.742 | −0.9 | 0.744 | −0.7 | 0.737 | −1.6 | 0.745 | −0.5 | 0.746 | −0.4 | 0.749 | ||
| 2780 | 0.856 | −0.8 | 0.859 | −0.5 | 0.850 | −1.5 | 0.859 | −0.5 | 0.860 | −0.3 | 0.863 | ||
| 580 | 0.961 | −0.5 | 0.963 | −0.3 | 0.953 | −1.3 | 0.963 | −0.3 | 0.963 | −0.3 | 0.966 | ||