新型固相微萃取技术（SPME）及其在室内环境检测中的应用研究

【作者】 何轶伦；

【导师】 任凤莲；

【作者基本信息】 中南大学 ， 分析化学， 2005， 硕士

【摘要】 随着人们居住水平的不断提高和装饰装修热的不断升温,室内环境污染日益严重,室内环境检测势在必行。采样和浓缩预处理是检测的关键。传统的室内空气污染物采样和浓缩预处理方法操作繁琐、耗时长、大量使用有机溶剂,危害人体,对环境也造成第二次污染。现有的新技术——固相微萃取技术,克服了传统技术的不足,但商品化的固相微萃取装置的萃取头价格昂贵,不能现用。本文根据固相微萃取技术的萃取方式、机理和定量依据,对多种材料进行综合考察后,选择日本产的SAKURA的2H 0.3mm的自动铅笔芯做萃取头,经过一系列处理后,自制了一套固相微萃取装置,并探讨了其性能和处理过程中的影响因素。 本论文用自制的SPME与GC-MS(毛细管柱)联用,对一预处理实验室室内空气中的挥发性有机化合物进行了定性检测,优化了实验条件,同传统的直接进样法和固相萃取法(SPE)进行了对照实验,研究结果表明,直接进样法的离子峰强度明显低于固相萃取和SPME法。 本论文利用SPME技术与GC联用,在上述实验的基础上,对室内空气中的苯、甲苯进行了定量分析,确定了最佳的实验条件。对建立的方法进行了系统评价:在所测的范围内标准曲线具有良好的线性关系,相关系数R=0.9998,最低检出限0.01mg/L,三个含量点的相对标准偏差在允许的范围7%以内。同传统的直接进样法和SPE法进行了系统的比较,研究结果表明:SPME和SPE法的检出限在同一级别上,优于直接进样方法。 论文进一步对室内空气中的甲醛进行了定量分析,同传统的分光光度法和衍生-SPE法进行了系统的比较,用分光光度法,最低检出限为0.05mg/L;衍生-SPE法,最低检出限0.04mg/L;SPME法,最低检出限0.01mg/L。 可见,SPME集采样、萃取、浓缩和进样于一体,操作简单、快速、准确,无需溶剂,萃取效率高,经济适用,具有很好的应用前景。因此,本论文对萃取头的选材和SPME技术在室内环境中的现场检测应用具有一定的指导意义。更多还原

【Abstract】 Detection of in-door air pollutants needs to be made urgently because of improvement of people living conditions and increase of ornament level. Sampling and pretreatment of indoor-air pollutants is the first key. However, Traditional methods are tedious, and have a large consumption of organic solvents that can do harm to people’s health and cause the second environmental pollution. Solid-phase micro-extraction (SPME) is a new technique for sampling and pretreatment. But present commercial SPME device usually are too expensive to be afforded. According to the principles of SPME and after investigation of the properties of different materials, A SPME device was assembled with the usage of SAKURA 2H automatic pencil core (0.03mm, Japan) as the extraction probe and application to detection of indoor air pollutants was investigated.Firstly, the quantitative analysis of indoor Volatile Organic Compounds (VOCs) was done using the improved SPME device combined with GC-MS equipped with a capillary column. After optimization of the experimental conditions, The abundance of ionic apex detected in injecting sampling directly method is markedly less than that in solid phase extraction (SPE) or that in SPME measurement.Secondly, trace benzene and toluene of indoor polluted air were quantitatively analyzed using SPME - GC. The SPME method was evaluated systematically and compared with traditional methods including direct injecting sampling and SPE . The results showed that there are good analytical characteristics with standard curve correlation coefficient of 0.9993, three relative standard deviations are less than 7%, recovery more than 90%. Also, another quantitative analysis of indoor pollutant formaldehyde was done using the same technique as mentioned above. The minimum detection limits determined by the improved SPME, derived SPE, and traditional spectro-photometry are 0.01mg/L, 0.04mg/L, 0.05mg/L, respectively.As a concluding remark, the improved SPME can perform sampling, extracting, concentrating, feeding. Therefore it is a simple, effectiveadsorption and de-sorption technique which eliminates the need for solvents and complicated apparatus, despite of its low price. The application of the improved SPME on-line detection of indoor pollutants will bear economic implications.更多还原