Development of large volume injection method for capillary GC.

TAJIMA Haruhiko, SHIMAMURA Naomi, AOKI Minako

doi:10.2116/bunsekikagaku.42.10_573

A new large volume injection method (dynamic retention gap method; DRG) for capillary/GC was developed. The retention gap consisted of a fused silica tube (2 m × 0.53 mm i.d.) and the precolumn (0.5 m × 0.53 mm i.d. × 0.5 μm) was connected with the capillary column by a T-shape connector. A large volume of sample solution (30 μl) vapoized in the injection port was rapidly introduced to the retention gap under large flow rate of carrier gas (20 ml/min). The sample was concentrated on the head of the precolumn by solvent focusing and liquid phase focusing. The sample was rapidly reconcentrated on the head of the analytical column because of a smaller phase ratio of the analytical column to that of the precolumn. This double focusing of sample enabled a large volume injection without decrease of the resolution of the analytical column. High linearity between injection volume and peak area of paraffins (C₁₂ to C₃₆) was observed with an injection volume of 1 to 30 μl in the DRG method. The performance of the DRG method was compared with that of a splitless method using a pesticide mixture and dioxin as test substances. The peak areas of the pesticides by the DRG method were 1.5 to 50.6 times larger than those by the splitless method for the same injection volume. The peak areas of dioxin were 6.6 to 11.7 times large by the DRG method with an injection of 10 μl of sample solution than by the splitless method with an injection of 2 μl. No decrease in resolution of dioxin isomer was observed. Received

Development of large volume injection method for capillary GC.

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