[Preparation and evaluation of open tubular capillary electrochromatographic columns by sol-gel method].
Open-tubular capillary electrochromatographic columns were prepared by sol-gel method. The influence of pH of gel solution on the column performance was investigated with a series of gel solution prepared by hydrochloric acid at different pH value. The results show that the pH of gel solution influences the capacity factors (k') of solutes in a complex way. The general trend is that the values of k' increase as the pH value increases except that at pH of 2.0. The gel solution of pH 2.8 was selected to prepare the column, at which the greatest capacity factors can be obtained within an acceptable reaction rate. The influence of reaction time of gel solution in column was also investigated. Out of expectation, the k' value didn't increase with increase in reaction time. The reason may be that the pore of silica gel is so small that the sample molecule can't migrate into it. The surface area is only offered by outer surface of silica gel, so the phase ratio of column prepared by this method is still not large enough. It was found that the joule heat effect can be neglected since the capillaries used were very small in inner diameter. The electroosmotic flow plays an important role in the separation as it determines the separation time. In order to accelerate the separation, high pH condition is necessary. Therefore, the stability of column under high pH is very important. The column shows a good stability under pH 9 of the mobile phase. The relative standard deviations (RSD) of capacity factor of four solutes were less than 3.7% for 100 times of operations. The separation efficiency was evaluated and the average theoretical plate numbers under optimal conditions for thiourea, phenetole, naphthalene, biphenyl, and 2,6-dimethyl naphthalene were 4.66 x 10(5), 5.24 x 10(5), 5.02 x 10(5), 4.77 x 10(5), and 3.58 x 10(5)/m, respectively. The column shows good repeatability. The RSD values for k' are less than 1% and the RSD values for efficiency are less than 8% (n = 5). In addition, fast separation was obtained with shorter column and higher voltage used, where four aromatic compounds were baseline separated in 101 s.
Ye
M
M
National Chromatographic R. & A. Center, Laboratory of Chromatography, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, 116011.
Zou
H
H
Liu
Z
Z
Ni
J
J
Zhuang
Q
Q
Zhang
Y
Y