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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 4.

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 C18 column with a variety of 70/30 THF/solvent j mobile phases. Instrumentation: Agilent 1100 with a variable wavelength detector set to 262 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 PS Mp Temperature
10 °C
 20 °C
 30 °C 40 °C 50 °C 60 °C
Ksec % ΔKsec Ksec % ΔKsec Ksec % ΔKsec Ksec % ΔKsec Ksec % ΔKsec Ksec Reference
C18 70/30 (v/v) THF/MeOH 282000 0.057 −1.7 0.058 0.0 0.058 0.0 0.058 0.0 0.058 0.0 0.058
126000 0.166 0.6 0.167 1.2 0.166 0.6 0.167 1.2 0.166 0.6 0.165
51200 0.368 0.3 0.369 0.5 0.368 0.3 0.368 0.3 0.367 0.0 0.367
19500 0.577 0.0 0.578 0.2 0.577 0.0 0.578 0.2 0.577 0.0 0.577
7350 0.740 −0.1 0.741 0.0 0.741 0.0 0.742 0.1 0.741 0.0 0.741
2780 0.840 −0.2 0.842 0.0 0.841 −0.1 0.842 0.0 0.842 0.0 0.842
580 0.934 0.1 0.935 0.0 0.934 0.1 0.935 0.0 0.934 0.1 0.935
70/30 (v/v) THF/ACN 282000 0.056 1.8 0.056 1.8 0.056 1.8 0.055 0.0 0.055 0.0 0.055
126000 0.165 3.1 0.164 2.5 0.163 1.9 0.162 1.3 0.161 0.6 0.160
51200 0.374 2.5 0.373 2.2 0.371 1.6 0.369 1.1 0.367 0.5 0.365
19500 0.593 1.7 0.592 1.5 0.589 1.0 0.588 0.9 0.585 0.3 0.583
7350 0.760 1.1 0.760 1.1 0.757 0.7 0.756 0.5 0.754 0.3 0.752
2780 0.861 0.7 0.860 0.6 0.857 0.2 0.858 0.4 0.856 0.1 0.855
580 0.953 0.8 0.952 0.7 0.948 0.3 0.948 0.3 0.946 0.1 0.945
70/30 (v/v) THF/eEtOH 282000 0.049 −5.8 0.050 −3.8 0.050 −3.8 0.051 −1.9 0.051 −1.9 0.052
126000 0.148 −1.3 0.149 −0.7 0.149 −0.7 0.150 0.0 0.150 0.0 0.150
51200 0.338 −0.9 0.339 −0.6 0.339 −0.6 0.340 −0.3 0.341 0.0 0.341
19500 0.544 −1.1 0.546 −0.7 0.547 −0.5 0.548 −0.4 0.549 −0.2 0.550
7350 0.711 −1.0 0.713 −0.7 0.714 −0.6 0.715 −0.4 0.717 −0.1 0.718
2780 0.816 −1.0 0.819 −0.6 0.820 −0.5 0.820 −0.5 0.823 −0.1 0.824
580 0.921 −0.6 0.924 −0.3 0.924 −0.3 0.924 −0.3 0.927 0.0 0.927
70/30 (v/v) THF/DMF 282000 0.040 −11.1 0.042 −6.7 0.044 −2.2 0.044 −2.2 0.045 0.0 0.045
126000 0.132 −2.2 0.133 −1.5 0.135 0.0 0.135 0.0 0.135 0.0 0.135
51200 0.319 −0.9 0.321 −0.3 0.322 0.0 0.322 0.0 0.322 0.0 0.322
19500 0.536 −0.6 0.538 −0.2 0.539 0.0 0.539 0.0 0.538 −0.2 0.539
7350 0.713 −0.6 0.716 −0.1 0.716 −0.1 0.717 0.0 0.716 −0.1 0.717
2780 0.824 −0.5 0.827 −0.1 0.826 −0.2 0.828 0.0 0.827 −0.1 0.828
580 0.921 −0.8 0.925 −0.3 0.924 −0.4 0.927 −0.1 0.926 −0.2 0.928
70/30 (v/v) THF/IPA 282000 0.053 −5.4 0.054 −3.6 0.054 −3.6 0.055 −1.8 0.055 −1.8 0.056
126000 0.158 0.0 0.158 0.0 0.158 0.0 0.158 0.0 0.159 0.6 0.158
51200 0.351 −0.3 0.352 0.0 0.352 0.0 0.353 0.3 0.353 0.3 0.352
19500 0.556 −0.5 0.557 −0.4 0.558 −0.2 0.559 0.0 0.560 0.2 0.559
7350 0.718 −0.8 0.721 −0.4 0.722 −0.3 0.724 0.0 0.724 0.0 0.724
2780 0.822 −0.7 0.825 −0.4 0.827 −0.1 0.828 0.0 0.828 0.0 0.828
580 0.927 −0.2 0.929 0.0 0.929 0.0 0.930 0.1 0.931 0.2 0.929
70/30 (v/v) THF/chloroform 282000 0.040 −4.8 0.041 −2.4 0.041 −2.4 0.042 0.0 0.042 0.0 0.042
126000 0.129 −1.5 0.130 −0.8 0.130 −0.8 0.131 0.0 0.131 0.0 0.131
51200 0.310 −1.0 0.311 −0.6 0.312 −0.3 0.312 −0.3 0.313 0.0 0.313
19500 0.520 −1.1 0.522 −0.8 0.523 −0.6 0.524 −0.4 0.525 −0.2 0.526
7350 0.694 −1.0 0.696 −0.7 0.698 −0.4 0.699 −0.3 0.701 0.0 0.701
2780 0.806 −0.9 0.808 −0.6 0.810 −0.4 0.811 −0.2 0.813 0.0 0.813
580 0.918 −0.6 0.920 −0.4 0.922 −0.2 0.922 −0.2 0.924 0.0 0.924
100% THF 282000 0.038 −7.3 0.039 −4.9 0.041 0.0 0.042 2.4 0.041 0.0 0.041
126000 0.121 −4.0 0.123 −2.4 0.124 −1.6 0.125 −0.8 0.125 −0.8 0.126
51200 0.297 −2.0 0.299 −1.3 0.299 −1.3 0.302 −0.3 0.302 −0.3 0.303
19500 0.509 −1.4 0.511 −1.0 0.511 −1.0 0.514 −0.4 0.515 −0.2 0.516
7350 0.687 −1.2 0.690 −0.7 0.690 −0.7 0.693 −0.3 0.694 −0.1 0.695
2780 0.802 −0.9 0.805 −0.5 0.805 −0.5 0.808 −0.1 0.808 −0.1 0.809
580 0.915 −0.5 0.917 −0.3 0.917 −0.3 0.920 0.0 0.920 0.0 0.920