Determination of polycyclic aromatic hydrocarbons in coal pitch by high performance liquid chromatography after Soxhlet extraction and column chromatographic separation
MA Song-jiang1,2,LUO Dao-cheng*1,2
1. School of Chemistry and Chemical Engineering,Hunan University of Science and Technology,Xiangtan 411201,China; 2. Hunan Province Key Laboratory of Coal Resources Clean-utilization and Mine Environment Protection,Xiangtan 411201,China
Abstract：The Soxhlet extraction of coal pitch was conducted using methylbenzene as solvent. The leaching liquor was filtrated by organic membrane followed by dissolution with dichloromethane. The sample solution was separated with silica gel column, which was then eluted with petroleum ether-methylbenzene mixture (1∶1, V/V) at flow rate of 5.0 mL/min. The leacheate was dried by rotary evaporation and then dissolved with acetonitrile to 10 mL. The sample solution was separated on a ZORBAX Eclipse PAH column by gradient elution using acetonitrile-water with different volume ratios as mobile phases. The separation and detection method of 16 polycyclic aromatic hydrocarbons (PAHs) in coal pitch by high performance liquid chromatography (HPLC) was established. The results showed that the linear range of 16 PAHs was 0.50-20 mg/L. The correlation coefficients (r) were not less than 0.999. The limits of detection were between 0.04 μg/L and 0.33 μg/L. The experimental method was applied to the determination of 16 PAHs in actual coal pitch samples from Hunan Valin Xiangtan Iron & Steel Co.,Ltd. The relative standard deviations (RSD, n=6) of results were between 0.20% and 3.5%, and the recoveries were between 97% and 109%. The proposed method was also applied to the determination of 16 PAHs in two coal pitch samples from Hunan Valin Xiangtan Iron & Steel Co.,Ltd. and Lianyuan Iron & Steel Co.,Ltd. The found results were basically consistent with the recommended values provided by two companies. The results showed that the content of 16 carcinogenic PAHs in 1 kg of coal pitch from Hunan Valin Xiangtan Iron & Steel Co.,Ltd. and Lianyuan Iron & Steel Co.,Ltd. was 107.9 g (10.79%) and 104.1 g (10.41%), respectively. The content of benzopyrene [a] was 11.86 g/kg and 13.82 g/kg (i.e., 1.186% and 1.382%), respectively.
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