ANALYSIS OF VOLATILE ORGANICS BY SUPERCRITICAL-FLUID EXTRACTION COUPLED TO GAS-CHROMATOGRAPHY .1. OPTIMIZATION OF CHROMATOGRAPHIC PARAMETERS

被引:17
作者
BURFORD, MD [1 ]
HAWTHORNE, SB [1 ]
MILLER, DJ [1 ]
机构
[1] UNIV N DAKOTA,ENERGY & ENVIRONM RES CTR,GRAND FORKS,ND 58202
关键词
D O I
10.1016/0021-9673(94)00638-5
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A solid-based calibration standard (consisting of several n-alkanes and aromatic hydrocarbons spiked onto Tenax-TA) was successfully used to optimize the chromatographic parameters for coupled supercritical fluid extraction-gas chromatography (SFE-GC). A simple and reliable split SFE-GC system was developed utilizing a commercially septumless injector installed on a split/splitless injection port. The high gaseous flow-rate generated inside the injection port during the SFE step was accommodated for by using the correct split ratio, so that high (1 ml/min liquid CO2) SFE flow-rates could be used. The use of thick-film columns (5 mu m film thickness) and cryogenic trapping temperatures in the GC oven as low as -50 degrees C allowed efficient trapping of species as volatile as n-butane, acetone and methylene chloride. The chromatograms obtained using the optimized SFE-GC technique showed good peak shapes (comparable to those obtained using a conventional split injection) and peak area reproducibilities typically <5% relative standard deviation.
引用
收藏
页码:79 / 94
页数:16
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