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危险废物鉴定中痕量多氯联苯的前处理优化分析 |
Study on Optimization of Sample Preparation for Trace PCBs in Hazardous Waste Identification |
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DOI: |
中文关键词: 多氯联苯 样品前处理 快速溶剂萃取 气相色谱-质谱法 危险废物 |
英文关键词: Polychlorinated biphenyls Sample pretreatment ASE GC MS Hazardous waste |
基金项目:四川省科技创新基地(平台)和人才计划基金资助项目(2019JDKY0016) |
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中文摘要: |
通过开展多种前处理技术对18种多氯联苯(PCBs)痕量分析的应用试验,对前处理影响因素和仪器条件进行优化,得出最佳参数,并将其应用于实际危废样品中痕量PCBs的测定。结果表明,以正己烷为萃取溶剂,萃取温度100 ℃,循环2次做加速溶剂萃取,用Si柱作为净化柱,洗脱溶剂体积为8 mL的净化条件下,18种PCBs在500 μg/L~500 μg/L范围内线性良好,方法检出限为004 μg/kg~031 μg/kg,加标样6次测定结果的RSD为45%~104%。实际危废样品测定结果为未检出~426 μg/kg,加标回收率为720%~105%。 |
英文摘要: |
A variety of extraction techniques for trace analysis of 18 kinds of PCBs were studied, the pretreatment factors and instrument conditions were optimized, and the optimum parameters were applied to the determination of trace PCBs in hazardous waste. The results indicated that under the conditions of n hexane as the extractant, 100 ℃ as the extraction temperature, twice of accelerated solvent extractions, Si column as the purification column,8 mL of eluant,18 kinds of PCBs had good linearity in the range of 5.00 μg/L to 500 μg/L. The detection limits were 0.04 μg/kg~0.31 μg/kg, the relative standard deviations of spiked sample were 4.5%~10.4%(n=6). The measurement result of actual hazardous waste samples ranged from not detected to 4.26 μg/kg, the recoveries ranged from 72.0% to 105%. |
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