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. Author manuscript; available in PMC: 2019 Jul 2.
Published in final edited form as: J Chromatogr A. 2017 Nov 24;1531:83–103. doi: 10.1016/j.chroma.2017.11.027

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