液液萃取-气相色谱-质谱法测定石化废水中二(2-乙基己基)己二酸酯

Determination of di(2-ethylhexyl)adipate in petrochemical wastewater by liquid-liquid extraction-gas chromatography-mass spectrometry

建立了液液萃取—气相色谱-质谱法测定石化废水中二(2-乙基己基)己二酸酯(DEHA)的新方法。优化的液液萃取条件为:萃取剂乙酸乙酯,水样调成酸性(pH<2),每次加入萃取剂0.1 mL/mL、盐析剂NaCl 0.15 g/mL,萃取6次,每次萃取时间2 min,氮吹浓缩水浴温度35℃。实验结果表明:在质量浓度0.1~100 mg/L的范围内,校准曲线的线性关系良好;检出限为0.15μg/L,定量限为0.5μg/L,加标回收率为93%~101%,相对标准偏差(n=7)小于2.9%。本法适用于石化废水中DEHA的测定。

A new method of liquid-liquid extraction-gas chromatography-mass spectrometry for determination of di(2-ethylhexyl)adipate(DEHA)in petrochemical wastewater was developed.The optimized conditions of liquid-liquid extraction are as follows:the extraction solvent isethyl acetate,thewater sample is adjusted to acidic(pH<2),the extractant amount is 0.1 mL/mL,the salting-out agent NaCl amount is 0.15 g/mL,the extraction number is 6 times,each extraction time is 2 min,and the water bath temperature for concentration with nitrogen is 35℃.The experimental results indicate that:The calibration curve has a good linear relationship within the mass concentration range of 0.1-100 mg/L;The detection limit is 0.15μg/L,the quantification limit is 0.5μg/L,and the standard recovery rate is 93%-101%,with the relative standard deviate(RSD)less than 2.9%(n=7).This method can be used for determination of DEHA in petrochemical wastewater.