Determination Of Semi-volatile Organic Pollutants In Water By Solid Phase Extraction And Gc-ms

In recent years, the rapid development of industrial and agricultural production have also brought a series of pollution problems, among which a large part of them are semi-volatile organic pollution. The large number of semi-volatile organic compounds, including nitrobenzene, phthalates category, type of polycyclic aromatic hydrocarbons, chlorobenzenes, organic chlorine pesticides, organic pesticide category, nitroso amines, aniline and phenol etc. . These substances have serious hazards to the environment and human health. To accurate determination and effective control of these pollutants, The key is the sample pre-treatment technology. However, the complex components of the environment often have a serious interference to the analysis, which makes sample preparation is not only time consuming but also the main source of error and restricts the development of analytical chemistry and environmental monitoring.At present, the separation and enrichment methods of semi-volatile organic compounds are mainly liquid - liquid extraction, liquid - solid extraction, and solid-phase microextraction. Solid-Phase Microextraction has not been widely used because of the high cost. The liquid - liquid extraction is numberous steps, long time consuming, solvent usage, achieving automation difficultly, poor precision and the large-scale use of toxic has bad effection on the operators and environment. Solid Phase Extraction (SPE) rises and becomes the widely used sample pre-treatment technology in this context. It implements the selective extraction, separation and enrichment in one process, with a short operation time, a small amount of sample and less interference, etc., can be used for a variety of substances, especially semi-volatile material analysis, has good reproduction quality, and adapted to the modern analytical requirements. It is an environmentally and friendly sample pretreatment technology.In this paper, the first part summarized many pre-treatment technologies in our country and abroad.The second part use SPE-GC-MS determinated 11 kinds of Nitrobenzenes in water sample. Experimental parameters influencing the performance of extraction, such as the pH value of water sample, load speed, breakthrough volume, eluting solvent, eluting volume, eluting rate, etc. were optimized. Under the optimized conditions, the actual water samples were tested. The results showed that: This method overcame many shortcomings of traditional extraction methods, such as solvent usage, toxicity, and numerous steps. Solid phase extraction can meet the requirements of trace analysis, is a good accuracy, high precision, low detection limit, convenient and practical testing methods.The third part compared the performance of liquid-liquid extraction, solid phase extraction on phthalate compounds. Experiments show: The solid phase extraction in the extraction of trace PAEs indeed better than liquid-liquid extraction. In the solid-phase extraction, The extraction efficiency of PAEs on Heaion GDX-403 column, Heaion C18 column, Agilent C18 column and Supelco C18 column were compared. Experimental parameters influencing the performance of extraction, such as the pH value of water sample, load speed, breakthrough volume, eluting solvent, eluting volume, eluting rate, etc. were optimized. In addition, the chromatography conditions of PAEs were optimized and blank experiment were discussed for the higher blank value of environment phthalate. Under the optimized conditions, real sample was successfully analyzed using this method.