Department of Analytical Chemistry, University of Córdoba, Campus of Rabanales, E-14071 Córdoba, Spain.
J Chromatogr A. 2013 Oct 4;1310:113-20. doi: 10.1016/j.chroma.2013.08.036. Epub 2013 Aug 16.
A simple and efficient method has been developed for the extraction and determination of sixteen common volatile halogenated disinfection by-products (DBPs) using the static headspace (HS) technique coupled with gas chromatography-mass spectrometry (GC-MS). The DBPs determined included trihalomethanes (THMs), halonitromethanes (HNMs) and haloacetonitriles (HANs). The extraction parameters (HS conditions, ionic strength and organic modifier) were studied in order to obtain the highest sensitivity. Under optimum conditions (water containing 250 μL of methyl tert-butyl ether and 6g of anhydrous sodium sulphate was heated 20 min at 80°C), the HS-GC-MS method provides limits of detection between 10 and 200 ng/L and a relative standard deviation of ∼5.6%. Samples collected from genuine tap water treated with different oxidising agents (ClO2/Cl2, Cl2/NH2Cl and O3/Cl2) in several disinfection treatment plants were successfully analysed in order to establish their effect on the occurrence of DBPs. In parallel, the influence of the main parameters of the water (pH, conductivity, nitrite, nitrate, free residual chlorine, permanganate oxidability and bromide) was also studied. The results suggest that the permanganate oxidability (related to organic matter) and the bromide concentration as well as disinfection conditions are directly related to the occurrence of THMs, HNMs and HANs, both in their concentrations and speciation. The method developed was compared to the reference EPA Method 551.1 for the analysis of tap water.
已开发出一种简单高效的方法,用于使用静态顶空(HS)技术结合气相色谱-质谱联用(GC-MS)提取和测定十六种常见挥发性卤代消毒副产物(DBPs)。所测定的 DBPs 包括三卤甲烷(THMs)、卤代硝基甲烷(HNMs)和卤代乙腈(HANs)。研究了萃取参数(HS 条件、离子强度和有机溶剂),以获得最高的灵敏度。在最佳条件下(水中含有 250 μL 叔丁基甲基醚和 6g 无水硫酸钠,在 80°C 下加热 20 分钟),HS-GC-MS 方法提供了 10 至 200ng/L 的检测限和约 5.6%的相对标准偏差。从几个消毒处理厂中用不同氧化剂(ClO2/Cl2、Cl2/NH2Cl 和 O3/Cl2)处理的真实自来水采集的样品进行了成功分析,以确定它们对 DBPs 生成的影响。同时,还研究了水的主要参数(pH 值、电导率、亚硝酸盐、硝酸盐、游离余氯、高锰酸盐氧化率和溴化物)的影响。结果表明,高锰酸盐氧化率(与有机物有关)和溴化物浓度以及消毒条件与 THMs、HNMs 和 HANs 的发生直接相关,无论是在浓度还是形态方面。所开发的方法与 EPA 方法 551.1 进行了比较,用于分析自来水。