Pretreatment method for purifying extract liquor

Abstract

The invention relates to a pretreatment method for purifying dioxin, polychlorinated biphenyl and polybrominated diphenyl ether in extract liquor. Purifying columns which respectively comprise a compound silicagel column, an alkaline aluminium oxide column and a Florisil column are arranged on an extraction module of a full-automatic solid-phase extractor, wherein fillers in each compound silicagel column comprise the following materials from bottom to top in sequence: silica gel, alkaline silica gel, silica gel, acidic silica gel and anhydrous sodium sulfate, and an eluent is normal hexane; fillers in the alkaline aluminium oxide column comprise the following materials from bottom to top in sequence: alkaline aluminium oxide and anhydrous sodium sulfate, and an eluent is mixed liquor of normal hexane and dichloromethane; fillers in the Florisil column comprise the following materials from bottom to top in sequence: Florisil and anhydrous sodium sulfate, the eluent is divided into two types according to the sequence of the steps, the eluent in the first step is the mixed liquor of normal hexane and dichloromethane, and the eluent in the second step is dichloromethane; and among all purifying columns, the eluents are transferred to an online concentrator for evaporation and concentration, and then are transferred to the next purifying column for purifying and treating.

Description

technical field [0001] The invention relates to a pre-purification pre-treatment method for fully automatic purification of sample extracts, in particular to a pre-purification pre-treatment method for dioxins, polychlorinated biphenyls and polybrominated diphenyl ethers in the extract. Background technique [0002] The rapid development of environmental analysis and testing technology provides an effective means for the detection and analysis of pollutants in environmental samples, especially for trace and ultra-trace persistent organic pollutants (POPs) in the environment, such as dioxins (PCDD / Fs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), etc., the development of chromatography and mass spectrometry technology has greatly improved the analysis capabilities of such pollutants. The analysis of such pollutants generally includes sample extraction, sample purification and concentration, instrument detection and analysis, etc. However, the cur...

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Problems solved by technology

The analysis of such pollutants generally includes sample extraction, sample purification and concentration, instrument detection and analysis, etc. However, the current sample purification methods for PCDD / Fs, PCBs and PBDEs are still dominated by traditional manual filling of chromatographic columns, which requires a lot of labor , the sample purification cycle is long, which is the main link that limits the rapid analysis of such pollutants

At present, the only commercial automatic purification equipment developed for PCDD / Fs and PCBs is the FMS system in the United States. It is expensive, the cost of analyzing samples is high, and the batch processing capacity is limited. There are still many restrictions on improving the ability of experimental analysis. In addition, for There is no commercial automatic purification equipment for the purification of PBDEs

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