Table 8.
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 phenyl 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 | PS 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 | 282000 | 0.088 | −2.2 | 0.087 | −3.3 | 0.089 | −1.1 | 0.089 | −1.1 | 0.090 | 0.0 | 0.090 |
| 126000 | 0.243 | −1.2 | 0.242 | −1.6 | 0.244 | −0.8 | 0.244 | −0.8 | 0.245 | −0.4 | 0.246 | ||
| 51200 | 0.498 | −0.8 | 0.499 | −0.6 | 0.500 | −0.4 | 0.502 | 0.0 | 0.502 | 0.0 | 0.502 | ||
| 19500 | 0.718 | −0.6 | 0.718 | −0.6 | 0.719 | −0.4 | 0.722 | 0.0 | 0.721 | −0.1 | 0.722 | ||
| 7350 | 0.861 | −0.3 | 0.862 | −0.2 | 0.862 | −0.2 | 0.865 | 0.1 | 0.864 | 0.0 | 0.864 | ||
| 2780 | 0.934 | −0.3 | 0.935 | −0.2 | 0.936 | −0.1 | 0.938 | 0.1 | 0.937 | 0.0 | 0.937 | ||
| 580 | 0.984 | −0.2 | 0.985 | −0.1 | 0.985 | −0.1 | 0.987 | 0.1 | 0.986 | 0.0 | 0.986 | ||
| 70/30 (v/v) THF/ACN | 282000 | 0.072 | −2.7 | 0.073 | −1.4 | 0.073 | −1.4 | 0.073 | −1.4 | 0.073 | −1.4 | 0.074 | |
| 126000 | 0.206 | −1.0 | 0.206 | −1.0 | 0.206 | −1.0 | 0.207 | −0.5 | 0.207 | −0.5 | 0.208 | ||
| 51200 | 0.449 | −0.9 | 0.450 | −0.7 | 0.449 | −0.9 | 0.451 | −0.4 | 0.452 | −0.2 | 0.453 | ||
| 19500 | 0.675 | −0.7 | 0.676 | −0.6 | 0.676 | −0.6 | 0.679 | −0.1 | 0.678 | −0.3 | 0.680 | ||
| 7350 | 0.832 | −0.5 | 0.833 | −0.4 | 0.833 | −0.4 | 0.835 | −0.1 | 0.836 | 0.0 | 0.836 | ||
| 2780 | 0.917 | −0.3 | 0.918 | −0.2 | 0.918 | −0.2 | 0.920 | 0.0 | 0.920 | 0.0 | 0.920 | ||
| 580 | 0.979 | −0.3 | 0.980 | −0.2 | 0.980 | −0.2 | 0.983 | 0.1 | 0.982 | 0.0 | 0.982 | ||
| 70/30 (v/v) THF/EtOH | 282000 | 0.070 | −2.8 | 0.071 | −1.4 | 0.070 | −2.8 | 0.071 | −1.4 | 0.071 | −1.4 | 0.072 | |
| 126000 | 0.201 | −0.5 | 0.201 | −0.5 | 0.201 | −0.5 | 0.201 | −0.5 | 0.201 | −0.5 | 0.202 | ||
| 51200 | 0.440 | −0.2 | 0.440 | −0.2 | 0.440 | −0.2 | 0.440 | −0.2 | 0.441 | 0.0 | 0.441 | ||
| 19500 | 0.666 | −0.1 | 0.666 | −0.1 | 0.667 | 0.0 | 0.667 | 0.0 | 0.668 | 0.1 | 0.667 | ||
| 7350 | 0.825 | −0.1 | 0.825 | −0.1 | 0.826 | 0.0 | 0.827 | 0.1 | 0.827 | 0.1 | 0.826 | ||
| 2780 | 0.913 | 0.0 | 0.913 | 0.0 | 0.913 | 0.0 | 0.914 | 0.1 | 0.915 | 0.2 | 0.913 | ||
| 580 | 0.978 | −0.1 | 0.978 | −0.1 | 0.979 | 0.0 | 0.980 | 0.1 | 0.981 | 0.2 | 0.979 | ||
| 70/30 (v/v) THF/DMF | 282000 | 0.052 | −5.5 | 0.052 | −5.5 | 0.053 | −3.6 | 0.052 | −5.5 | 0.054 | −1.8 | 0.055 | |
| 126000 | 0.156 | −1.3 | 0.156 | −1.3 | 0.158 | 0.0 | 0.155 | −1.9 | 0.157 | −0.6 | 0.158 | ||
| 51200 | 0.370 | −0.8 | 0.370 | −0.8 | 0.374 | −0.3 | 0.369 | −1.1 | 0.372 | −0.3 | 0.373 | ||
| 19500 | 0.600 | −0.3 | 0.600 | −0.3 | 0.603 | 0.2 | 0.599 | −0.5 | 0.602 | 0.0 | 0.602 | ||
| 7350 | 0.775 | −0.3 | 0.775 | −0.3 | 0.777 | 0.0 | 0.774 | −0.4 | 0.776 | −0.1 | 0.777 | ||
| 2780 | 0.877 | −0.1 | 0.877 | −0.1 | 0.878 | 0.0 | 0.876 | −0.2 | 0.878 | 0.0 | 0.878 | ||
| 580 | 0.962 | 0.0 | 0.962 | 0.0 | 0.962 | 0.0 | 0.961 | −0.1 | 0.962 | 0.0 | 0.962 | ||
| 70/30 (v/v) THF/IPA | 282000 | 0.074 | −1.3 | 0.074 | −1.3 | 0.074 | −1.3 | 0.074 | −1.3 | 0.075 | 0.0 | 0.075 | |
| 126000 | 0.209 | −0.5 | 0.209 | −0.5 | 0.209 | −0.5 | 0.209 | −0.5 | 0.210 | 0.0 | 0.210 | ||
| 51200 | 0.452 | −0.2 | 0.452 | −0.2 | 0.452 | −0.2 | 0.453 | 0.0 | 0.453 | 0.0 | 0.453 | ||
| 19500 | 0.677 | −0.4 | 0.679 | −0.1 | 0.678 | −0.3 | 0.679 | −0.1 | 0.680 | 0.0 | 0.680 | ||
| 7350 | 0.834 | −0.4 | 0.835 | −0.2 | 0.835 | −0.2 | 0.836 | −0.1 | 0.836 | −0.1 | 0.837 | ||
| 2780 | 0.919 | −0.2 | 0.920 | −0.1 | 0.920 | −0.1 | 0.921 | 0.0 | 0.921 | 0.0 | 0.921 | ||
| 580 | 0.981 | −0.2 | 0.982 | −0.1 | 0.983 | 0.0 | 0.984 | 0.1 | 0.984 | 0.1 | 0.983 | ||
| 70/30 (v/v) THF/chloroform | 282000 | 0.053 | −5.4 | 0.053 | −5.4 | 0.054 | −3.6 | 0.055 | −1.8 | 0.056 | 0.0 | 0.056 | |
| 126000 | 0.161 | −1.2 | 0.161 | −1.2 | 0.161 | −1.2 | 0.162 | −0.6 | 0.163 | 0.0 | 0.163 | ||
| 51200 | 0.378 | −0.8 | 0.379 | −0.5 | 0.378 | −0.8 | 0.380 | −0.3 | 0.381 | 0.0 | 0.381 | ||
| 19500 | 0.606 | −0.7 | 0.607 | −0.5 | 0.607 | −0.5 | 0.608 | −0.3 | 0.609 | −0.2 | 0.610 | ||
| 7350 | 0.778 | −0.5 | 0.780 | −0.3 | 0.779 | −0.4 | 0.781 | −0.1 | 0.781 | −0.1 | 0.782 | ||
| 2780 | 0.878 | −0.6 | 0.881 | −0.2 | 0.880 | −0.3 | 0.882 | −0.1 | 0.882 | −0.1 | 0.883 | ||
| 580 | 0.963 | −0.3 | 0.965 | −0.1 | 0.964 | −0.2 | 0.966 | 0.0 | 0.966 | 0.0 | 0.966 | ||
| 100% THF | 282000 | 0.053 | −3.6 | 0.053 | −3.6 | 0.053 | −3.6 | 0.054 | −1.8 | 0.055 | 0.0 | 0.055 | |
| 126000 | 0.152 | −2.6 | 0.152 | −2.6 | 0.153 | −1.9 | 0.154 | −1.3 | 0.155 | −0.6 | 0.156 | ||
| 51200 | 0.359 | −1.6 | 0.360 | −1.4 | 0.361 | −1.1 | 0.362 | −0.8 | 0.364 | −0.3 | 0.365 | ||
| 19500 | 0.583 | −1.0 | 0.584 | −0.8 | 0.585 | −0.7 | 0.586 | −0.5 | 0.588 | −0.2 | 0.589 | ||
| 7350 | 0.761 | −0.5 | 0.761 | −0.5 | 0.761 | −0.5 | 0.762 | −0.4 | 0.764 | −0.1 | 0.765 | ||
| 2780 | 0.865 | −0.3 | 0.865 | −0.3 | 0.866 | −0.2 | 0.866 | −0.2 | 0.867 | −0.1 | 0.868 | ||
| 580 | 0.955 | 0.0 | 0.954 | −0.1 | 0.954 | −0.1 | 0.954 | −0.1 | 0.955 | 0.0 | 0.955 | ||