Annealing of silica to reduce the concentration of isolated silanols and peak tailing in reverse phase liquid chromatography

作者：Newby Josh J; Legg Michael A; Rogers Benjamin; Wirth Mary J^*

来源：Journal of Chromatography A, 2011, 1218(31): 5131-5135.

DOI：10.1016/j.chroma.2011.05.080

• Silica
• Tailing
• Isolated silanols
• FTIR
• Annealing

Non-porous, colloidal silica particles were annealed at three different temperatures, 800,900 and 1050 degrees C. The adsorption of lysozyme, a probe of surface roughness, was consistent with progressively reduced surface roughness as temperature increased. The heat treated silica particles were rehydroxylated and then used to pack UHPLC columns. The cationic protein lysozyme was used to probe silanol activity, which exhibited progressively less tailing as the annealing temperature increased. FTIR spectroscopy confirmed that the abundance of isolated silanols on the surface was reduced by annealing at 900 degrees C or 1050 degrees C. FTIR also revealed that there was markedly increased hydrogen bonding of the isolated silanols to neighbors after rehydroxylation. These results combine to support the hypothesis that (a) isolated silanols on silica cause tailing in RP-LC and (b) nonplanar topography gives rise to isolated silanols.

• 出版日期2011-8-5