Packing density of slurry-packed capillaries at low aspect ratios

被引:35
作者
Ehlert, Steffen [1 ]
Roesler, Thomas [1 ]
Tallarek, Ulrich [1 ]
机构
[1] Univ Marburg, Dept Chem, D-35032 Marburg, Germany
关键词
column-to-particle diameter ratio; nano-HPLC; packed capillaries; porosity; wall effect;
D O I
10.1002/jssc.200800018
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The average interparticle voidage or porosity (epsilon(inter)) in cylindrical capillaries is studied in dependence on the column diameter (d(c)) to particle diameter (d(p)) ratio for 5 < d(c)/d(p) < 50. Using optimized slurry and packing solvents, high pressure and ultrasonication, 5 mu m-sized porous C18-silica particles were slurry-packed into fused-silica capillaries having ids from 30 to 250 pm. Packing densities are assessed by a polystyrene standard which is size-excluded from the intraparticle pore space of the packings. For d(c)/d(p) > 35 densely packed beds are realized (epsilon(inter) = 0.36 - 0.37), while for decreasing aspect ratios an exponential increase in epsilon(inter) is observed reaching epsilon(inter) approximate to 0.47 at d(c)/d(p) = 5. This behaviour is ascribed to a combination of the geometrical wall effect operating in the direct vicinity of the column wall, caused by the inability of the particles to form a dense packing against the hard surface of the column wall, and particle characteristics like the size distribution, shape and surface roughness. Results are compared with the literature data to address also the importance of absolute particle size in studying structure-transport relations in packed beds in dependence on the aspect ratio d(c)/d(p).
引用
收藏
页码:1719 / 1728
页数:10
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