Achten C, Kolb A, Püttmann W
J.W. Goethe-Universität Frankfurt am Main, Institut für Mineralogie--Umweltanalytik, Frankfurt am Main, Germany.
Fresenius J Anal Chem. 2001 Oct;371(4):519-25. doi: 10.1007/s002160100984.
A simple and rapid method for the determination of methyl tert-butyl ether (MTBE) in water by headspace-solid-phase microextraction (headspace-SPME) at sub-microg/L concentrations is described. On using a cooled SPME fiber coated with a 75-microm layer of poly(dimethylsiloxane)/carboxene and heating the sample to 35 degrees C, about 4 times more MTBE is extracted compared to SPME extraction with the fiber placed in the water sample. Stable analytical conditions with a detection limit of 10 ng/L are achieved. By use of a sample volume of 4 mL in a 10 mL vial, a sodium chloride content of 10% (w/w), and an extraction time of 30 min, the total time of an analytical cycle was optimized to 39 min. Precise linearity of R2>0.9991 and R2>0.9916 in the calibration range of 20-5000 ng/L and 20-100 ng/L, both in addition to blanks, respectively, and relative standard deviations of 10% (100 ng/L, long-term) and 11% (20 ng/L, short-term) are presented. The recovery is well within the accepted limits of 83-118% at a concentration of 100 ng/L and even close thereto at trace levels of 20 ng/L (96-125%). The data presented for a concentration of 100 ng/L are examined by statistical methods and show results for the T test at the 95% confidence level. Due to the large concentration range covered, the method is well suited for the monitoring of MTBE in the aquatic environment.
本文描述了一种简单快速的方法,用于在亚微克/升浓度下通过顶空固相微萃取(顶空-SPME)测定水中的甲基叔丁基醚(MTBE)。使用涂有75微米厚聚二甲基硅氧烷/羧烯层的冷却SPME纤维,并将样品加热至35摄氏度,与将纤维置于水样中的SPME萃取相比,MTBE的萃取量大约多4倍。实现了稳定的分析条件,检测限为10纳克/升。通过在10毫升小瓶中使用4毫升样品体积、10%(w/w)的氯化钠含量和30分钟的萃取时间,将一个分析周期的总时间优化至39分钟。在校准范围20 - 5000纳克/升和20 - 100纳克/升(均包括空白)内,分别呈现出R2>0.9991和R2>0.9916的精确线性,以及10%(100纳克/升,长期)和11%(20纳克/升,短期)的相对标准偏差。在100纳克/升浓度下回收率良好,在83 - 118%的可接受范围内,在20纳克/升的痕量水平下甚至更接近该范围(96 - 125%)。针对100纳克/升浓度呈现的数据通过统计方法进行了检验,并显示了95%置信水平下的T检验结果。由于覆盖的浓度范围较大,该方法非常适合监测水生环境中的MTBE。