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直接热解吸气相色谱飞行时间质谱法在环境颗粒物和个人采样器中小体积样品中非极性有机物测定中的应用。

Application of direct thermal desorption gas chromatography time-of-flight mass spectrometry for determination of nonpolar organics in low-volume samples from ambient particulate matter and personal samplers.

机构信息

Cooperation Group Comprehensive Molecular Analytics, Helmholtz Zentrum München, Neuherberg, Germany.

出版信息

Anal Bioanal Chem. 2011 Dec;401(10):3083-94. doi: 10.1007/s00216-011-5429-x. Epub 2011 Nov 16.

Abstract

Direct thermal desorption and in-situ derivatization thermal desorption methods in conjunction with gas chromatography time-of-flight mass spectrometry have been characterized and evaluated for analysis of trace components from filters loaded with ambient particulate matter (PM). The limits of quantification were in the range of 7-24 pg for n-alkanes, 20 pg for hopanes, and 4-22 pg for polycyclic aromatic hydrocarbons (PAH). The limit of quantification was defined as the minimum amount of substance that conforms to the minimum distinguishable signal plus 9 times the standard deviation of this background signal from PM-loaded filters. The method has been successfully applied to low-volume samples from ambient PM collected with stationary and personal samplers. Stationary samples were collected in winter 2008 and 2010 in Augsburg, Germany. Sample aliquots of 0.2-0.3 m³ from stationary sampling were analyzed. High diurnal variation in concentration and source contribution was found especially during periods with low wind speed and low mixing layer height. High contributions of solid fuel combustion (wood and coal) were found in evening and nighttime samples, leading to peak PAH concentrations at midnight more than 10 times higher than at noon. Finally, the method was applied to samples collected by means of a personal sampler, i.e. a micro aethalometer, in Xi'an, China. Quantitative data on n-alkanes, hopanes, and PAH were obtained from sample volumes of 17 and 24 l. The impact of different sources such as vehicular and biogenic emissions could be distinguished.

摘要

直接热解吸和原位衍生热解吸方法与气相色谱飞行时间质谱相结合,已被用于分析负载环境颗粒物(PM)的过滤器中痕量成分。对于正构烷烃,定量下限在 7-24 pg 范围内;对于藿烷,定量下限在 20 pg 范围内;对于多环芳烃(PAH),定量下限在 4-22 pg 范围内。定量下限定义为符合最小可分辨信号的最小物质量,加上 PM 负载过滤器中该背景信号的 9 倍标准偏差。该方法已成功应用于使用固定和个人采样器采集的环境 PM 的低体积样品。固定采样于 2008 年和 2010 年冬季在德国奥格斯堡进行。对固定采样的 0.2-0.3 m³样品进行分析。发现浓度和源贡献的日变化很大,特别是在风速低和混合层高度低的时期。在傍晚和夜间的样品中发现了固体燃料燃烧(木材和煤)的高贡献,导致午夜的 PAH 浓度比中午高 10 倍以上。最后,该方法应用于在中国西安通过个人采样器(即微气溶胶质谱仪)采集的样品。从 17 和 24 l 的样品体积中获得了正构烷烃、藿烷和 PAH 的定量数据。可以区分不同来源(如车辆和生物源排放)的影响。

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