Use of chain transfer agent attached to silica particles in preparation of polystyrene‐based stationary phases

Abstract

A new stationary phase has been prepared by attaching a new chain transfer agent on silica particles followed by reversible addition-fragmentation chain transfer polymerization. Porous silica particles were reacted with 3-chloropropyltrimethoxysilane followed by sodium diethyl dithiocarbarmate. The silica particles were then allowed to undergo radical polymerization with styrene. The phase had improved ligand morphology to show better separation performance than that of the conventional C18 phase.

A New Stationary Phase Prepared from Ground Silica Monolith Particles by Reversible Addition-Fragmentation Chain Transfer Polymerization

“…The reason of superiority of a polystyrene bound phase over a C18 bound phase was already discussed in the previous studies [23][24] and attributed to the core/shell like structure of the polystyrene bound phase. The particle of our phase is regarded to have a structure where the deep core is closed, the shallow pores are partially filled, and the outer surface is smoothly covered with bound polystyrene oligomers with relatively high molecular weights.…”

“…[22][23][24] Thus, a frit (commercial screen frit) was placed in the 1/16 inch outlet of a 1/16 -1/32 reducing union, a piece of 30 cm glass lined stainless steel tubing was fitted to the outlet, and the tubing was connected to the packer. The 100 mg particles were suspended in 5 mL methanol, sonicated for 5 min, stood calm for 20 s, and the supernatant was decanted out to remove very fine particles.…”

“…[22][23][24] The initiator silica particles prepared by reacting silica particles with 3-chloropropyltrimethoxysilane followed by sodium diethyldithiocarbarmate resulted in stationary phases with improved morphology and better separation performance [23][24] compared to the initiator silica particles prepared by reacting with 4-(chloromethyl)phenylisocyanate. 22 In the above studies, commercial silica particles were used.…”

Ground Organic Monolith Particles Having a Large Volume of Macropores as Chromatographic Separation Media

“…On the other hand, studies on ground monolith particles have been rare. In our laboratory, C18 modified 12,13 and polystyrene modified [14][15][16][17][18][19] ground silica monolith particles have been employed as new stationary phases of improved separation efficiency. The very first report on study of organic monolith particles as inexpensive chromatographic separation media was also recently published by our group.…”

Ground Organic Monolith Particles as Chromatographic Separation Media

“…On the other hand, studies on ground monolith particles have been rare. C18 modified 19,20 and polystyrene modified [21][22][23][24] ground silica monolith particles have been employed as new stationary phases of improved separation efficiency. Nevertheless, there has been no report on organic ground monolith particles as chromatographic or SPE media so far.…”