提出了应用气相色谱法与顶空固相微萃取样品预处理技术相结合的方法测定饮用水中2,4,6-三氯酚(TCP)和五氯酚(PCP)。选用20 mL顶空瓶,其中预置0.1 mol·L-1盐酸溶液0.5 mL及氯化钠4.0 g,加入水样10.0 mL,立即封盖。插入85 μm聚丙烯酸酯萃取头,在500 r·min-1转速振荡条件下于60 ℃萃取40 min,随之进入色谱仪解吸并测定。测定中采用HP-5毛细管柱和程序升温(40 ℃~280 ℃)条件,并用载气流量为3 mL·min-1。测得2,4,6-TCP及PCP的线性范围依次为55 μg·L-1和12 μg·L-1以内,其检出限(3S/N)依次为0.15 μg·L-1和0.13 μg·L-1,加入3个浓度水平的标准溶液对方法的回收率及精密度作了试验,测得回收率在90.0%~112.8%之间,相对标准偏差(n=6)在3.0%~4.9%之间。

Gas chromatography with sample pretreatment by automatic head-space solid phase micro-extraction was applied to the determination of 2,4,6-trichlorophenol (TCP) and pentachlorophenol (PCP) in drinking water. The water sample (10.0 mL) was added to a 20 mL-head-space flask in which 0.5 mL of 0.1 mol·L-1 HCl and 4.0 g of NaCl were added previously. After capping the flask tightly, the polyacrylate extractor (85 μm) was inserted into it and shaked at the rate of 500 r·min-1 at 60 ℃ for 40 min to extract the chlorophenols, which were then desorbed and determined by GC. HP-5 capillary column was used for separation with programmed temperature elevation from 40 ℃ to 280 ℃. Flow-rate of carrier gas taken was 3 mL·min-1. Linear relationships between values of peak area and mass concentration of TCP and PCP were obtained in the ranges within 55 μg·L-1 and 12 μg·L-1 respectively, with detection limits (3S/N) of 0.15 μg·L-1 (for TCP) and 0.13 μg·L-1 (for PCP). Tests for recovery and precision were made by addition of standards at 3 concentration levels, giving results of recovery in the range from 90.0% to 112.8%, and RSD′s (n=6) from 3.0% to 4.9%.