• 한국물환경학회지
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• 제22권5호
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• pp.879-886
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• 2006

The analytical methods of polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans (PCDD/Fs) for water sample with extremely low concentration was developed to extract large volume and to improve fast chromatography for clean up. Semi-automated solid phase extraction (SPE) system and column coupling chromatography using elution pump was optimized and applied to each processes of treatment plant. Results of disk type SPE indicated that this system was applicable below 40 L of aqueous sample with a flow rate of 0.08 ~ 0.2 L/min. Average recoveries of SPE using labeled sampling spike of $^{37}Cl$-2,3,7,8-TCDD was 97%. Column coupling method resulted in reduced clean up time, solvent volume, increased average recoveries with constant elution rate. The combined methods were applied to the monitoring of drinking water treatment plant. Limits of detection (LOD) of each process were calculated. For example, LOD of raw and treated water ranged 0.094~0.968 pg/L and 0.028~0.364 pg/L, respectively. Combined methods of extraction and cleanup techniques provided fast analysis of PCDD/Fs with high accuracy and low LODs for water samples.

• Mass Spectrometry Letters
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• 제2권1호
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• pp.12-15
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• 2011

The Korean government has regulated emission of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in waste water of manufacturing facilities producing chlorinated compounds since 2009. As this regulation is expected to be reinforced in 2013 to 50 pg I-TEQ/L, a large sample volume is required for the analysis of trace amounts of PCDD/Fs in waste water. Liquid-liquid extraction (LLE) is used to extract PCDD/Fs from aqueous samples; however, its low efficiency makes it inadequate for analyzing large sample volumes. Herein, we present a disk-type solid-phase extraction (SPE) method for the analysis of dioxin at a part per quadrillion level in waste water. This SPE system contains airtight glass covers with a decompression pump, which enables continuous semi-automated extraction. Small (0.5 L) and large (7 L) samples were extracted using LLE and SPE methods, respectively. The method detection limits (MDLs) were 0.001.0.25 and 0.015.4.1 pg I-TEQ/L for the SPE and LLE methods, respectively. The concentrations of detected congeners with both methods were similar. However, the concentrations of several congeners that were not detected with the LLE method were quantified using the SPE method.