Analytical Sciences

Abstract − Analytical Sciences, 19(10), 1407 (2003).

Separation and Determination of Methyl tert-Butyl Ether and Its Degradation Products by a Laboratory-constructed Micro-cryogenic Chromatographic Oven
Jiemin LIU,*,** Guibin JIANG,*  Qunfang ZHOU,* Jingfu LIU,* and Meijuan WEN**
*Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing, 100085, China
**Department of Chemistry, Beijing University of Science and Technology, Beijing 100083, China
A laboratory-made micro-cryogenic chromatographic oven was mainly improved in size, which was controlled at 6 x 6 x 2.5 cm. A thermoelectric system was used to cool the capillary column instead of the traditional liquid cryogen. A cold block connected to the cryogenic module was directly solidified at room temperature with thermally conductive adhesive so that the uniformity of transferring heat was greatly improved, and the size of the system was reduced. Moreover, this system was inexpensive and convenient for both operation and control. The newly developed device coupled with headspace solid-phase microextraction (SPME) was successfully applied to the determination of methyl tert-butyl ether (MTBE) and its degradation products. During the analysis procedure, a 65 µm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was used to extract MTBE and its degradation products. The extraction was controlled at 50°C for 30 min and the NaCl content in the sample was maintained at 35%. The limits of detection (LODs) ranged from 0.006 µg mL-1 (for MTBE) to 0.206 µg mL-1 (for methyl acetate) and the relative standard deviations (RSD%) were below 4%. The spiked recoveries for the developed method were evaluated using various water samples as a matrix.