快速溶剂萃取-离子色谱-质谱法同时测定爆炸尘土中的氯酸盐和高氯酸盐

Simultaneous determination of chlorate and perchlorate in explosion dust by accelerated solvent extraction-ion chromatography-mass spectrometry

爆炸尘土用去离子水作为提取剂,萃取、离心和0.22μm滤膜净化后,采用Ion Pac AS20离子色谱柱分离,40 mmol/L KOH溶液等度淋洗,采用三重四极杆质谱仪负离子模式检测,多离子监测模式扫描,外标法定量。结果表明,氯酸盐和高氯酸盐在质量浓度0.5~100.0μg/L范围内,线性关系良好,相关系数均大于0.999。检出限分别为0.12和0.01μg/L,定量限为0.5μg/L和0.04μg/L,相对标准偏差为3.0%~5.0%和1.6%~5.0%,回收率范围为82.8%~86.5%和89.3%~93.2%。利用该方法测定爆炸尘土,所有样本均检出氯酸盐和高氯酸盐,含量范围分别为0.16~0.26 mg/kg和7.15~20.90 mg/kg。

The explosion dust sample was quickly extracted by water and purified by centrifugal ultrafiltration and 0.22μm membrane.The separation of chlorate and perchlorate in the extract was carried out on Ion Pac AS20 column with isocratic elution using 40 mmol/L KOH solution as mobile phase followed by triple quadrupole mass spectrometer detection in anion mode.Multi ion monitoring mode scanning and external spiked method were adopted.The results showed that there were good linear relationships for chlorate and perchlorate in the range of 0.5-100.0μg/L with the correlation coefficients above 0.999.The limits of detection for chlorate and perchlorate were 0.12μg/L and 0.01μg/L,and the limits of quantification were 0.5μg/L and 0.04μg/L,respectively.The relative standard deviations were in the range of 3.0%-5.0%and 1.6%-5.0%,and the recoveries of chlorate and perchlorate were in the range of 82.8%-86.5%and 89.3%-93.2%,respectively.The method was successfully used to determine chlorate and perchlorate in explosion dust.Chlorate and perchlorate were detected in all samples,with the contents ranging of 0.16-0.26 mg/kg and 7.15-20.90 mg/kg,respectively.