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。     

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.     

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.     

室内空气中挥发性有机物采样方法进展

介绍了近年来室内空气中挥发性有机物的各种采样方法及适用范围，其中重点介绍了美国环保署最新版的TO－17方法和J.Pawliszyn发明的固相微萃取法（SPME），并对一系列的采样方法进行了比较，阐述了这些方法在国内外的应用及研究进展，同时讨论了这些方法的局限性。     

固相微萃取-毛细管气相色谱法快速同步分析水中硝基苯类及氯苯类化合物

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。文章用固相微萃取富集水中9种硝基苯类及5种氯苯类化合物,毛细管气相色谱ECD检测器分离分析,整个分析过程只需25min,检出限可达0.0002~0.02μg/L,已用于地表水、海水与工厂废水中硝基苯类及氯苯类化合物含量的测定。     

固相微萃取法提取水中增塑剂

本文利用固相微萃取(SPME)前处理技术与气相色谱质谱技术相结合,测定水中已二酸二(2-乙基)已酯(DEHA),对萃取温度、萃取时间和解析时间等影响因素进行了优化,得出固相微萃取最佳条件。     

介孔涂层SPME- HPLC联用测定水样中的多环芳烃

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,该方法的线性范围分别为0.4-300μg/L、4.0-450μg/L,检出限为0.3μg/L、0.10μg/L,以此方法测定了环境水样中萘、蒽的含量.该方法具有灵敏度高和精密度好的特点.     

利用HS-SPME-GC技术分析环境水样中超痕量的六氯苯,DDT及其代谢产物

利用顶空固相微萃取(HS-SPME)和气相色谱检测技术,通过对三种不同的SPME萃取头(PDMS,PMPVS,PA)实验条件的优化,并参照液液萃取的方法,对水相中六氯苯,DDT及其代谢产物的萃取效果进行了比较．结果表明,SPME方法比液液萃取方法在检测限和回收率上有很大的提高,其中PDMS对检测六氯苯,DDT及其代谢产物的效果较其它两种萃取头好．     

固相微萃取法的应用及其进展

固相微萃取（ＳＰＭＥ） 是在固相萃取（ＳＰＥ） 的基础上结合顶空分析（Ｈｅａｄｓｐａｃｅ） 建立起来的一种新的样品预处理方法,它于１９９０ 年Ｊ．Ｐａｗｌｉｓｚｙｎ 首先提出,因其携带方便、操作简便、测定快速、高效的特点,且是一种无溶剂的样品预处理方法,故在短短几年时间,广泛应用于各个研究领域,如环境（ 包括水样、土壤、空气） 以及食品、药物、毒理学等的分析研究。本文根据所查阅到的文献,对目前国际上固相微萃取法的应用发展及其研究情况作一概述,并就该方法今后的可能发展方向进行初步的探讨（６０ ,１４６ ,１５３） ！