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11.
固相微萃取分析条件的优化   总被引:9,自引:0,他引:9  
主要介绍了固相微萃取作为一种样品前处理技术,如何对影响其分配系数的各因素,如:萃取头的选择、萃取方式、萃取温度等进行优化选择,从而提高方法灵敏度及回收率。  相似文献   
12.
On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2–4.0 µg L?1) and low detection limits (1.1–2.9 ng L?1). The high extraction efficiency was determined with enrichment factors ranging from 1.2–2.9 for the lowest level, 1.3–4.9 intermediate level and 1.2–3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.  相似文献   
13.
Solid phase microextraction (SPME) is a fast, cheap and solvent free methodology widely used for environmental analysis. A SPME methodology has been optimized for the analysis of VOCs in a range of matrices covering different soils of varying textures, organic matrices from manures and composts from different origins, and biochars. The performance of the technique was compared for the different matrices spiked with a multicomponent VOC mixture, selected to cover different VOC groups of environmental relevance (ketone, terpene, alcohol, aliphatic hydrocarbons and alkylbenzenes). VOC recovery was dependent on the nature itself of the VOC and the matrix characteristics. The SPME analysis of non-polar compounds, such as alkylbenzenes, terpenes and aliphatic hydrocarbons, was markedly affected by the type of matrix as a consequence of the competition for the adsorption sites in the SPME fiber. These non-polar compounds were strongly retained in the biochar surfaces limiting the use of SPME for this type of matrices. However, this adsorption capacity was not evident when biochar had undergone a weathering/aging process through composting. Polar compounds (alcohol and ketone) showed a similar behavior in all matrices, as a consequence of the hydrophilic characteristics, affected by water content in the matrix. SPME showed a good performance for soils and organic matrices especially for non-polar compounds, achieving a limit of detection (LD) and limit of quantification (LQ) of 0.02 and 0.03 ng g−1 for non-polar compounds and poor extraction for more hydrophilic and polar compounds (LD and LQ higher 310 and 490 ng g−1). The characteristics of the matrix, especially pH and organic matter, had a marked impact on SPME, due to the competition of the analytes for active sites in the fiber, but VOC biodegradation should not be discarded in matrices with active microbial biomass.  相似文献   
14.
The chemical composition of the odors typical of fires has recently been deciphered. Basically the constituents are mixtures of acetophenone, benzyl alcohol, hydroxylated derivatives of benzaldehyde, methoxylated and/or alkylated phenols and naphthalene. This finding makes it possible to develop objective, practical analytic measurement methods for the burnt smell as a contribution to improving fire damage assessment and remediation monitoring. With the aid of an artificially produced burnt smell and a panel of testers the odor detection threshold of a test mixture was determined olfactometrically to 2 μg m−3. Using a defined burnt-smell atmosphere in a test chamber, analytical methods with active sampling, the adsorbents XAD 7 and TENAX TA, and GC/MS measurement were then optimized and tested with a view to being able to carry out sensitive quantitative measurement of burnt smells. A further practical method with particular application to the qualitative characterization of this odor is based on the use of a new SPME (solid-phase microextraction) field sampler with DVB/CAR/PDMS (divinylbenzene/Carboxen™/polydimethylsiloxane) fibers.  相似文献   
15.
Pyrzynska K 《Chemosphere》2011,83(11):1407-1413
With increasing public concerns for agrochemicals and their potential movement in the ecosystem, very sensitive, selective and precise methods for the analysis of pesticides are needed. Because these substances are present usually at trace levels, the extraction and preconcentration steps are so far essential for their detection. Discoveries of novel nanomaterials with unique properties have significant impact on their use also in extraction techniques. This overview reports the recent application of carbon nanotubes in the analysis of pesticides. The largest numbers of reported applications of carbon nanotubes concern their role as a sorbent materials in solid-phase extraction and microextraction techniques.  相似文献   
16.
将四乙氧基硅烷(TEOS)和N-(β-氨乙基)-γ-氨丙基三乙氧基硅烷(AEAPTES)作为共聚前体,采用在毛细管内原位聚合的方式制备得到氨基功能化的有机-无机杂化整体柱,将其作为针式固相微萃取(SPME)介质,建立了现场分离富集环境水中As(V)的SPME方法,优化了有机-无机杂化整体柱富集As(V)的实验条件,并研究了整体柱对As(V)的吸附/洗脱性能和富集能力,实现了环境水样中As(V)的高效、快速、高选择性检测。  相似文献   
17.
固相微萃取-气相色谱法测定水源地水中SVOC   总被引:2,自引:0,他引:2  
采用固相微萃取-毛细管柱电子捕获气相色谱法测定水源地水中18种半挥发性有机物,优化了萃取纤维、时间、温度、pH值、转子转速、离子强度等萃取条件。方法线性良好,18种化合物的检出限为0.000 2μg/L~0.1μg/L,实际水样加标回收率为84.3%~109%。  相似文献   
18.
空气中挥发性有机物监测技术的研究进展   总被引:13,自引:0,他引:13  
讨论了空气中挥发性有机化合物(VOCs)的监测分析方法研究进展。重点介绍了空气中VOCs的采集、分析和测定;简要叙述了样品前处理的新方法--固相微萃取法(SPME)与其它前处理方法的研究概况。  相似文献   
19.
本文采用固相微萃取前处理方法与气相色谱—质谱联用技术相结合对扎龙底泥中邻苯二甲酸二丁酯(DBP)和邻苯二甲酸(2-乙基己基)酯(DEHP)进行测定。  相似文献   
20.
固相微萃取-毛细管气相色谱法快速分析水中酚类化合物   总被引:10,自引:4,他引:10  
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.本工作用固相微萃取富集水中酚类化合物,毛细管气相色谱分离分析,整个分析过程只需45min,检出限可达1.0~10.0μg/L,已用于地面水、海水、工厂废水中酚类化合物含量的测定.  相似文献   
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