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华中科技大学硕士学位论文
华
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硕
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速率为 1000 rpm 的条件下萃取 20 min。在此条件下,四种氯苯的检出限为 0.05-0.1
μg/g(S/N=3);方法的线性范围为 0.2-10 μg/g(r2≥0.9959);实际土壤样品的加标回收率 为 82.47-99.94%,相对标准偏差为 1.79-2.97%。
关键词:样品前处理技术 液相微萃取 全氟辛烷羧酸 全氟辛烷磺酸 超声水萃取 氯苯
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Abstract
In the 1990s, a simple and solvent free method known as liquid-phase microextraction has emerged dramatically as an alternative sample preparation technique. This novel technique overcomes a few disadvantages of conventional sample preparation techniques, only requiring umpty microlitres of organic solvents. It combines extraction, concentration and sample introduction in a single step and it is a sensitive and environmental friendly sample preparation technique. In this article, liquid-phase microextraction technology of computer-controlled combined with LC-MS is used in the analysis of PFOA and PFOS in water samples; ultrasound-assisted water extraction combined with liquid-phase microextraction technology of computer-controlled and GC-MS is used in the analysis of chlorobenzenes in soil samples. The main conclusions
are as follows:
Liquid-phase microextraction technology of computer-controlled was established using the high precision injection pump Versa Pump 6 (V6) syringe and switch valve 50120 Intellect valve of American Kloehn company. The volume of liquid-phase microextraction can be precisely controlled by the system which improves the accuracy and precision of liquid-phase microextrction, laying solid foundation for the subsequent experiments.
A novel green analytical method for determination of PFOA and PFOS in water samples, based on liquid-phase microextraction technology of computer-controlled combined with HPLC-MS was developed. The best results were shown as follows: 1-Octanol as extraction solvent, pH=3 water sample as donor phase, pH=11 ammonium acetate of 1 mmol/L as acceptor phase, effective length 10 cm of polypropylene hollow fiber membrane, extraction temperature 20, stirring speed 1300 rpm, extraction
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