Chemistry Dept., University of Girona, Campus Montilivi s/n, 17071 Girona, Spain.
J Chromatogr A. 2011 Nov 11;1218(45):8131-9. doi: 10.1016/j.chroma.2011.09.042. Epub 2011 Sep 21.
Combining headspace (HS) sampling with a needle-trap device (NTD) to determine priority volatile organic compounds (VOCs) in water samples results in improved sensitivity and efficiency when compared to conventional static HS sampling. A 22 gauge stainless steel, 51-mm needle packed with Tenax TA and Carboxen 1000 particles is used as the NTD. Three different HS-NTD sampling methodologies are evaluated and all give limits of detection for the target VOCs in the ng L⁻¹ range. Active (purge-and-trap) HS-NTD sampling is found to give the best sensitivity but requires exhaustive control of the sampling conditions. The use of the NTD to collect the headspace gas sample results in a combined adsorption/desorption mechanism. The testing of different temperatures for the HS thermostating reveals a greater desorption effect when the sample is allowed to diffuse, whether passively or actively, through the sorbent particles. The limits of detection obtained in the simplest sampling methodology, static HS-NTD (5 mL aqueous sample in 20 mL HS vials, thermostating at 50 °C for 30 min with agitation), are sufficiently low as to permit its application to the analysis of 18 priority VOCs in natural and waste waters. In all cases compounds were detected below regulated levels.
将顶空(HS)采样与针捕集装置(NTD)相结合,用于水样中优先挥发性有机化合物(VOCs)的测定,与传统的静态 HS 采样相比,灵敏度和效率均得到提高。NTD 采用 22 号不锈钢、51mm 长的针头,内部填充 Tenax TA 和 Carboxen 1000 颗粒。评估了三种不同的 HS-NTD 采样方法,所有方法对目标 VOCs 的检测限均在 ng L⁻¹ 范围内。活性(吹扫捕集)HS-NTD 采样灵敏度最高,但需要对采样条件进行全面控制。NTD 用于采集顶空气体样品,会产生吸附/解吸的综合作用。HS 恒温器测试不同温度时,当允许水样通过吸附剂颗粒被动或主动扩散时,解吸效果更大。在最简单的采样方法中,静态 HS-NTD(5 mL 水样在 20 mL HS 小瓶中,50°C 恒温 30 min 并搅拌)得到的检测限足够低,可用于分析天然水和废水中的 18 种优先 VOCs。在所有情况下,均检测到低于规定水平的化合物。