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| Determination of 53 Semi-volatile Organic Compounds in Solid Waste by Gas Chromatography－Mass Spectrometry with Microwave Extraction and Solid Phase Extraction Column Purification |
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| DOI： |
| KeyWord:semi-volatile organic compounds solid waste microwave extraction solid phase extraction gas chromatography－mass spectrometry |
| Author | Institution |
| JIANG Jian-jun，LU Guang-lei，LIU Li，XIANG Yong |
Hunan Division of GRG Metrology and Test，Changsha ，China |
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| Abstract: |
| A gas chromatography－mass spectrometry（GC－MS） was established for the determination of 53 semi-volatile organic compounds in solid wastes，based on microwave-assisted extraction combined with solid phase extraction（SPE） column cleanup．Extraction was carried out in a microwave extraction tank using 20 mL acetone－hexane （1∶1，by volume） as the extractant，with an extraction temperature of 100 ℃ and an extraction time of 15 min，then the extract was concentrated by nitrogen blowing．The analyte was purified by magnesium silicate solid phase extraction column and separated on a DB－5MS（30 m × 0.25 μm × 0.25 mm） capillary column，finally detected with electron bombardment ionization source（EI） in selected ion monitoring（SIM） mode and quantified by internal standard method．The results showed that there were good linear relationships for 53 semi-volatile organic compounds in the range of 0.2－5.0 mg/L，with their correlation coefficients（r） not less than 0.998．The limits of detection for typical solid waste ash and biochemical sludge samples were in the range of 0.002－0.015 mg/kg and 0.004－0.027 mg/kg，while the limits of quantitation were in the range of 0.008－0.060 mg/kg and 0.016－0.108 mg/kg，respectively．For two typical solid waste negative sample matrices，the average recoveries at three spiked levels of 0.5，1.0 and 2.0 mg/kg for ash sample ranged from 70.7% to 98.5%，with relative standard deviations（RSDs，n = 6） of 1.7%－14%，while the average recoveries for biochemical sludge sample ranged from 71.8% to 105%，with RSDs（n = 6） of 1.2%－15%．The method was applied to the analysis of solid waste samples from Miluo pesticide plant，in which seven semi-volatile organic compounds，i.e．phorate，fenitrothion，heptachlor，hexachlorobenzene，p，p'-DDE，p，p'-DDT and mirex with different concentrations were detected．This method is rapid，accurate，environmentally friendly and reliable，and low reagent consumption，which could meet the requirements for high throughput detection of 53 semi-volatile organic compounds in solid waste，and significantly improve the detection efficiency for semi-volatile organic compounds. |
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