C_8-SBA-15新型介孔涂层SPME-HPLC联用测定水样中的芘

以辛基键合SBA-15为固相微萃取（SPME）的吸附涂层,考察了吸附和解吸时间、萃取温度、搅拌速率对SPME效率的影响。该方法的线性范围为3.0—320μg/L,检出限为0.5μg/L,依据此方法测定了环境水样中芘,具有灵敏度高和精密度好的特点。     

新型动态针捕集阱技术分析大气中低浓度的VOCs

本研究针对大气中挥发性有机物（VOCs）浓度低,难于分析等特点,以Carboxen 1000作为吸附剂,制作一种新型动态针捕集阱（needle trap）装置,可用于主动富集大气中低浓度VOCs.该装置与气相色谱-质谱（GC-MS）联用,操作简单、无需溶剂、容易定性定量.选择空气中苯系物（BTEX）为目标化合物,对needle trap装置从设计原理到实际应用进行了详细分析,将萃取条件与穿透体积等实验条件进行优化,建立了needle trap吸附提取空气中BTEX的最佳条件.结果表明,方法检出限低至0.05ng·mL-1,加标回收率为86.5%～110.5%,符合外场采样要求.     

固相微萃取/气相色谱质谱法测定水中松节油

固相微萃取是一种操作简便、分析快速、无溶剂参与的样品前处理技术。通过采用固相微萃取富集水中的松节油,气相色谱质谱法分析,整个过程只需要25 min。该方法检出限为0.02 mg/L,样品加标回收率为90.0%～130%,相对标准偏差为3.49%～14.6%,完全能够满足日常环境管理需要。     

Relevance study of bare and coated zero valent iron nanoparticles for lindane degradation from its by-product monitorization

Zero-valent iron nanoparticles (NZVI) as well as polymer–stabilized nanoparticles were synthesized and used for lindane (γ-hexachlorocyclohexane) degradation in aqueous solution. To study the effectiveness of the different coated nanoparticles, simple and rapid analytical methods have been developed to measure and to detect lindane and its by-products. For the monitorization of lindane degradation solid-phase extraction (SPE) was used, while volatile by-products formation measurement was carried out by headspace-solid phase microextraction (HS–SPME) followed by GC/MS. The SPE–GC/MS method provides low detection limits (0.2 μg L⁻¹), high recovery (above 95%) and it is a valuable tool for kinetic studies of the degradation process for each polymer used, while HS–SPME–GC/MS has proved to be an effective tool for the extraction and evaluation of volatile degradation by-products.     

Development,validation and application of a method to analyze phenols in water samples by solid phase micro extraction-gas chromatography-flame ionization detector

In this work the development, validation and application of method using Solid Phase Microexctration (SPME) for the analyses of five pollutants (phenol, 2-nitrophenol, 2,4-dimethylphenol, 2,4-dichlorophenol and 4-chloro, 3-methyl phenol) in supplying water, using gas chromatography (GC) with flame ionization detector (FID) is described. The optimal conditions obtained for SPME were: fiber type: Poliacrylate (PA); extraction time: 40 minutes; extraction temperature: 70°C; amount of salt added to sample (NaCl): 15%; desorption temperature: 8 minutes. The parameters studied in the method validation were: limit of detection (0.3 and 3.5 μ g.L^{? 1}); precision, measured by the variation coefficient (between 2.1 and 8.8%); calibration curve and linearity, by using the external standardization method (between 1 and 50 50 μ g.L^{? 1}). After the methodology development, samples of water collected in Atibaia River (São Paulo - Brazil) were analyzed, using the optimized methodology. Three water samples collected in the rain season showed a peak with retention time close to 4-chloro, 3 methyl phenol further analyzed by Gas Chromatography-Mass Spectrometry for the identity confirmation. In spite of the fact that none target compounds were found in the river water samples analyzed, the presence of two phenols different from those investigated (p-terc butyl phenol; butylated hydroxytoluene) were detected. These results together with the results of the limit of detection (that showed to be lower than the maximum concentration of phenols demanded by different environment control agencies), and the results of the validation, indicate the applicability of this method for the analysis of selected phenols in river water samples.     

新型固相微萃取头测定胶粘剂中苯及其同系物

结合分子印迹技术与溶胶-凝胶技术,自制新型联苯分子印迹溶胶-凝胶聚合物涂层固相微萃取头,结合顶空固相微萃取-气相色谱法(HS-SPME-GC),测定水溶液中的苯及其同系物。结果表明,该方法精密度良好(RSD<5%),线性范围超过2个数量级,最低检出限达到10ng/mL。运用该法对市售胶粘剂中苯及其同系物进行检测,结果令人满意。     

Solid-phase microextraction coupled with atomic emission spectroscopy--rapid screening for volatile chlorinated compounds

Solid-phase microextraction (SPME) coupled with atomic emission spectroscopy was evaluated as a rapid screening tool for volatile halogenated compounds in water samples. After extraction, the SPME fiber was introduced to the injector where the analytes were rapidly and efficiently desorbed. The analytes entered the detector over a short period of time and produced one well-defined analyte signal. Element selective responses were measured to confirm the presence and to roughly estimate the content of volatile compounds. The total time for extraction and detection was approximately 5 min, which makes this method a rapid and promising technique for determination of total amount of volatile halogenated compounds. The proposed technique may prove useful as a screening test in order to pinpoint the samples that need further assessment by capillary gas chromatography.     

固相微萃取技术及其应用现状综述

固相微萃取技术（SPME）在固相萃取（SPE）基础上发展而来。作为一种较新的样品前处理技术,固相微萃取技术具有操作简单、快速、集采样、萃取、浓缩和进样于一体等诸多优点,目前已被广泛应用。阐述了 SPME 的技术原理、操作流程、影响因素、应用领域和新的进展。着重指出 SPME 在环境有机污染物分析中具有广泛的应用前景。     

南极长城湾附近和台湾以南部分海域水样中丁基锡化合物分析

对南极长城站附近水域及中国台湾以南海域采集的水样进行了分析研究。应用顶空固相微萃取（SPME）技术富集丁基锡化合物，由气相色谱分离后，表面发射火焰光度检测器测定，在两个水域均未检出三丁基锡，但存在一定量的三丁基锡降解产物，即二丁基锡和一丁基锡。     

固相微萃取-毛细管气相色谱法快速分析水中酞酸酯

用固相微萃取富集水中酞酸酯，毛细管气相色谱分离分析，整个分析过程只需50min，检出限可达0.01-40.0μg／L，实验表明，固相微萃取是一种快速、简便、集萃取浓缩进样于一体的样品前处理技术，具有分析时间短、灵敏度高、无需有机溶剂的优点，已用于地面水源、海水、饮用水中酞酸酯含量的测定。