An improved automatic analyzer for organic compounds in water based on headspace solid-phase microextraction (SPME) coupled to gas chromatography

Eckhard Belau, Christoph Grote, Manfred Spiekermann, Karsten Levsen
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引用次数: 8

Abstract

An automated analyzer based on solid-phase microextraction (SPME) coupled to gas chromatography (GC) for monitoring organic compounds in water is presented. The instrumental setup, which was tested previously with direct SPME, is now tested in the headspace mode. Memory effects observed in the earlier design were reduced by using glass instead of plastic tubing. Parameters that potentially influence the extraction yield were studied in the laboratory with the use of spiked water samples. These parameters were temperature, salt content, methanol content, pH value, and excess components. The extraction efficiency as a function of the extraction time (absorption profiles) was determined for 24 standard compounds. The method was validated in the laboratory. Good precision (in general <5%) and linearity were observed. With the use of flame ionization, detection limits of quantitation were in the low-ppb range, sufficient for wastewater monitoring. The instrument was tested continuously for 6 days at the wastewater plant of a chemical company in northern Germany. Better stability and robustness were observed in the headspace SPME compared to the direct SPME. © 2001 John Wiley & Sons, Inc. Field Analyt Chem Technol 5: 37–49, 2001

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基于顶空固相微萃取和气相色谱的水中有机化合物自动分析仪
提出了一种基于固相微萃取(SPME)和气相色谱(GC)联用的水中有机化合物自动分析仪。之前使用直接SPME测试的仪器设置,现在在顶空模式下进行测试。在早期设计中观察到的记忆效应通过使用玻璃而不是塑料管来减少。在实验室中使用加标水样研究了可能影响提取率的参数。这些参数是温度、含盐量、甲醇含量、pH值和过量组分。测定了24种标准化合物的萃取效率随萃取时间(吸收谱)的变化规律。该方法在实验室得到了验证。观察到良好的精度(一般为<5%)和线性。采用火焰电离法,定量检出限在低ppb范围内,足以用于废水监测。该仪器在德国北部一家化工公司的污水处理厂连续测试了6天。与直接SPME相比,顶空SPME具有更好的稳定性和鲁棒性。©2001 John Wiley &儿子,Inc。化学工程学报,2001,31 (5):379 - 379
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