Table 10.
Calculated Ksec and% OKsec (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 cyano 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 | |||
| Cyano | 70/30 (v/v) THF/MeOH | 282000 | 0.055 | −6.8 | 0.057 | −3.4 | 0.056 | −5.1 | 0.057 | −3.4 | 0.058 | −1.7 | 0.059 |
| 126000 | 0.161 | −1.8 | 0.164 | 0.0 | 0.161 | −1.8 | 0.163 | −0.6 | 0.163 | −0.6 | 0.164 | ||
| 51200 | 0.356 | −1.1 | 0.360 | 0.0 | 0.356 | −1.1 | 0.358 | −0.6 | 0.359 | −0.3 | 0.360 | ||
| 19500 | 0.571 | −0.7 | 0.577 | 0.3 | 0.570 | −0.9 | 0.572 | −0.5 | 0.573 | −0.3 | 0.575 | ||
| 7350 | 0.742 | −0.4 | 0.749 | 0.5 | 0.740 | −0.7 | 0.743 | −0.3 | 0.743 | −0.3 | 0.745 | ||
| 2780 | 0.847 | −0.4 | 0.854 | 0.5 | 0.845 | −0.6 | 0.847 | −0.4 | 0.848 | −0.2 | 0.850 | ||
| 580 | 0.940 | −0.2 | 0.948 | 0.6 | 0.938 | −0.4 | 0.940 | −0.2 | 0.941 | −0.1 | 0.942 | ||
| 70/30 (v/v) THF/ACN | 282000 | 0.055 | −1.8 | 0.055 | −1.8 | 0.055 | −1.8 | 0.056 | 0.0 | 0.055 | −1.8 | 0.056 | |
| 126000 | 0.155 | 0.0 | 0.156 | 0.6 | 0.156 | 0.6 | 0.156 | 0.6 | 0.155 | 0.0 | 0.155 | ||
| 51200 | 0.350 | 0.6 | 0.350 | 0.6 | 0.350 | 0.6 | 0.350 | 0.6 | 0.349 | 0.3 | 0.348 | ||
| 19500 | 0.568 | 0.2 | 0.569 | 0.4 | 0.568 | 0.2 | 0.568 | 0.2 | 0.568 | 0.2 | 0.567 | ||
| 7350 | 0.744 | 0.0 | 0.745 | 0.1 | 0.743 | −0.1 | 0.744 | 0.0 | 0.744 | 0.0 | 0.744 | ||
| 2780 | 0.852 | 0.0 | 0.853 | 0.1 | 0.851 | −0.1 | 0.852 | 0.0 | 0.853 | 0.1 | 0.852 | ||
| 580 | 0.949 | 0.0 | 0.950 | 0.1 | 0.948 | −0.1 | 0.949 | 0.0 | 0.950 | 0.1 | 0.949 | ||
| 70/30 (v/v) THF/EtOH | 282000 | 0.053 | −7.0 | 0.055 | −3.5 | 0.055 | −3.5 | 0.056 | −1.8 | 0.056 | −1.8 | 0.057 | |
| 126000 | 0.158 | −1.9 | 0.159 | −1.2 | 0.159 | −1.2 | 0.160 | −0.6 | 0.160 | −0.6 | 0.161 | ||
| 51200 | 0.354 | −1.1 | 0.355 | −0.8 | 0.355 | −0.8 | 0.357 | −0.3 | 0.356 | −0.6 | 0.358 | ||
| 19500 | 0.572 | −0.7 | 0.574 | −0.3 | 0.574 | −0.3 | 0.575 | −0.2 | 0.574 | −0.3 | 0.576 | ||
| 7350 | 0.746 | −0.7 | 0.748 | −0.4 | 0.748 | −0.4 | 0.750 | 0.1 | 0.749 | −0.3 | 0.751 | ||
| 2780 | 0.853 | −0.5 | 0.855 | −0.2 | 0.855 | −0.2 | 0.857 | 0.0 | 0.856 | −0.1 | 0.857 | ||
| 580 | 0.947 | −0.5 | 0.949 | −0.3 | 0.949 | −0.3 | 0.952 | 0.0 | 0.950 | −0.2 | 0.952 | ||
| 70/30 (v/v) THF/DMF | 282000 | 0.021 | −48.8 | 0.018 | −56.1 | 0.022 | −46.3 | 0.037 | −9.8 | 0.032 | −22.0 | 0.041 | |
| 126000 | 0.135 | −5.6 | 0.139 | −2.8 | 0.141 | −1.4 | 0.142 | −0.7 | 0.141 | −1.4 | 0.143 | ||
| 51200 | 0.325 | −2.7 | 0.329 | −1.5 | 0.331 | −0.9 | 0.332 | −0.6 | 0.331 | −0.9 | 0.334 | ||
| 19500 | 0.553 | −1.4 | 0.556 | −0.9 | 0.559 | −0.4 | 0.559 | −0.4 | 0.558 | −0.5 | 0.561 | ||
| 7350 | 0.741 | −1.1 | 0.743 | −0.8 | 0.746 | 0.4 | 0.746 | 0.4 | 0.746 | 0.4 | 0.749 | ||
| 2780 | 0.857 | −0.9 | 0.859 | −0.7 | 0.862 | −0.3 | 0.863 | −0.2 | 0.862 | −0.3 | 0.865 | ||
| 580 | 0.960 | −0.9 | 0.962 | −0.7 | 0.966 | −0.3 | 0.967 | −0.2 | 0.966 | −0.3 | 0.969 | ||
| 70/30 (v/v) THF/IPA | 282000 | 0.053 | −5.4 | 0.053 | −5.4 | 0.055 | −1.8 | 0.055 | −1.8 | 0.056 | 0.0 | 0.056 | |
| 126000 | 0.160 | 0.0 | 0.159 | −0.6 | 0.160 | 0.0 | 0.159 | −0.6 | 0.160 | 0.0 | 0.160 | ||
| 51200 | 0.358 | 0.3 | 0.357 | 0.0 | 0.358 | 0.3 | 0.357 | 0.0 | 0.357 | 0.0 | 0.357 | ||
| 19500 | 0.578 | 0.2 | 0.578 | 0.2 | 0.577 | 0.0 | 0.577 | 0.0 | 0.577 | 0.0 | 0.577 | ||
| 7350 | 0.753 | 0.1 | 0.753 | 0.1 | 0.752 | 0.0 | 0.752 | 0.0 | 0.752 | 0.0 | 0.752 | ||
| 2780 | 0.860 | 0.2 | 0.860 | 0.2 | 0.858 | 0.0 | 0.859 | 0.1 | 0.859 | 0.1 | 0.858 | ||
| 580 | 0.951 | −0.1 | 0.952 | 0.0 | 0.950 | −0.2 | 0.952 | 0.0 | 0.952 | 0.0 | 0.952 | ||
| 70/30 (v/v) THF/chloroform | 282000 | 0.026 | −33.3 | 0.020 | −48.7 | 0.036 | −7.7 | 0.038 | −2.6 | 0.039 | 0.0 | 0.039 | |
| 126000 | 0.142 | −1.4 | 0.144 | 0.0 | 0.144 | 0.0 | 0.144 | 0.0 | 0.145 | 0.7 | 0.144 | ||
| 51200 | 0.334 | −0.6 | 0.336 | 0.0 | 0.335 | −0.3 | 0.335 | −0.3 | 0.336 | 0.0 | 0.336 | ||
| 19500 | 0.558 | −0.4 | 0.560 | 0.0 | 0.559 | −0.2 | 0.559 | −0.2 | 0.560 | 0.0 | 0.560 | ||
| 7350 | 0.740 | −0.3 | 0.742 | 0.0 | 0.741 | −0.1 | 0.741 | −0.1 | 0.742 | 0.0 | 0.742 | ||
| 2780 | 0.852 | −0.1 | 0.853 | 0.0 | 0.853 | 0.0 | 0.852 | −0.1 | 0.853 | 0.0 | 0.853 | ||
| 580 | 0.947 | −0.1 | 0.949 | 0.1 | 0.949 | 0.1 | 0.948 | 0.0 | 0.948 | 0.0 | 0.948 | ||
| 100% THF | 282000 | 0.042 | −8.7 | 0.044 | −4.3 | 0.046 | 0.0 | 0.044 | −4.3 | 0.045 | −2.2 | 0.046 | |
| 126000 | 0.135 | −2.9 | 0.136 | −2.2 | 0.138 | 0.7 | 0.137 | −1.4 | 0.138 | −0.7 | 0.139 | ||
| 51200 | 0.319 | −1.5 | 0.321 | −0.9 | 0.323 | −0.3 | 0.322 | −0.6 | 0.323 | −0.3 | 0.324 | ||
| 19500 | 0.543 | −0.7 | 0.544 | −0.5 | 0.546 | −0.2 | 0.544 | −0.5 | 0.546 | −0.2 | 0.547 | ||
| 7350 | 0.728 | −0.4 | 0.730 | −0.1 | 0.731 | 0.0 | 0.729 | −0.3 | 0.731 | 0.0 | 0.731 | ||
| 2780 | 0.843 | −0.2 | 0.845 | 0.0 | 0.846 | 0.1 | 0.843 | −0.2 | 0.845 | 0.0 | 0.845 | ||
| 580 | 0.945 | 0.0 | 0.947 | 0.2 | 0.948 | 0.3 | 0.945 | 0.0 | 0.946 | 0.1 | 0.945 | ||