Microwave-immobilized polybutadiene stationary phase for reversed-phase high-performance liquid chromatography

Characterization of a new stationary phase based on microwave immobilized polybutadiene on titanium oxide-modified silica

“…The amount of PBD immobilized reaches 24.3% Table 3 Chromatographic parameters, final percentages of PBD and layer thickness (τ) of stationary phases microwave immobilized at power level 586 W, for different continuous immobilization times with an immobilization time of 10 min. In this condition, the thickness of the PBD layer on titanized silica was 1.06 nm and, as reported by Lopes et al [23,24], the best phases with PBD immobilized by microwave and gamma radiation onto bare silica presented this same layer thickness. In the present case, however, efficiency values decreased with the increase in PBD layer thickness, reaching the lowest value, 10,800 N m −1 .…”

“…The use of microwave radiation as an immobilization technique was first introduced by our group. It is a low cost technique and provides good reversed-phase packing materials, as reported in an earlier work [24].…”

“…Household microwave ovens do not have the mode stirrer, which distributes the microwaves in diverse directions inside the oven, therefore the intensity of the radiation is variable and some points are warmer than others [43]. To avoid this variation, during the irradiations, the flask was always placed near the edge of the rotating plate, where there was a greater incidence of the microwaves [24].…”

“…Recently, some papers have investigated polymeric coatings on silica with poly(alkylmethysiloxanes) and polybutadiene (PBD). Some of these phases were immobilized by different processes, including thermal treatments [18][19][20], gamma radiation [21][22][23], microwave radiation [24] or induced by radical initiators (peroxide). Others were simply self-immobilized, which means the absence of conventional immobilization procedures [25][26][27].…”

Immobilized polymeric stationary phases using metalized silica supports

“…The stationary phase immobilized at 520 W presented the best performance, with column efficiencies of 86 500 plates/m and good symmetries for apolar compounds ( Table 2). The quantities of PBD immobilized on the titanized silica support were also equivalent, in terms of carbon percent, to the quantities of PBD immobilized on bare silica particles [40].…”