气相色谱-质谱联用法测定污水中得克隆阻燃剂

Determination of Dechloranes in waste water by GC-NCI/MS

摘要:

为了考察环境中痕量的得克隆阻燃剂的污染现状,建立气相色谱-负离子化学电离源质谱联用法同时测定污水样品中得克隆阻燃剂Dechlorane 602(Dec602),Dechlorane 603(Dec603),Dechlorane 604(Dec604)和Dechlorane Plus(DP)的分析方法.水样采用液液萃取法同时提取水相和颗粒相中的得克隆类物质,经过硅胶净化,采用150℃离子源温度,150℃四级杆温度,280℃进样温度,1000V的电子倍增补偿电压的气相色谱-质谱分析条件进行定量分析.Dec602,Dec603,Dec604和DP在水样中的检测限在0.01～0.1ng·L-1之间,其标准曲线的线性相关系数均大于0.99.通过对某城市污水处理厂的污水进行检测验证了方法的有效性:加标回收率在74%～122%之间,相对标准偏差均小于13.2%.分析污水结果表明,进水和出水得克隆类物质残留总质量浓度分别为3.2ng·L-1和0.19ng·L-1,其中DP为主要污染物.

Abstract:

A method for the determination of Dechlorane 602 (Dec 602),Dechlorane 603 (Dec 603),Dechlorane 604 (Dec 604) and Dechlorane Plus (DP) in wastewater by gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI/MS) has been developed. The water sample was extracted by classical liquid-liquid extraction method to collect the Dechloranes from both particle phase and water phase, cleaned up using silica gel and then analyzed by GC-NCI/MS under the optimized conditions of 150 ℃source temperature,150 ℃ quadrupole temperature,280 ℃ initial temperature and 1 kV electron multiplier (EM) offset voltage. The quantitation limits of Dec 602,Dec 603,Dec 604 and DP were 0. 01-0. 1 ng·L-1. The correlation coefficients were above 0. 99 for the calibration curves. The validity of this method was demonstrated by determination of Dechloranes in wastewater of a municipal wastewater treatment plant in Harbin,China. The results indicate that the recovery rates of all Dechloranes in wastewater are 74%-122% ,the relative standard deviations (DRS) are less than 13. 2% . The concentrations of Dechloranes in influent and effluent are 3. 2 ng·L-1and 0. 19 ng·L-1,respectively. Dechloranes are dominanted by DP in wastewater.