CAJ | 학술논문

苯系物是有机化学品泄漏事故中导致土壤污染的主要污染物之一,但我国目前还没建立土壤中苯系物的标准监测方法.采用顶空气相色谱-质谱联用法(GC-MS)研究了模拟污染土壤中苯系物的测定方法,优化了顶空作为土壤中苯系物预处理方法的参数,分析了顶空GC-MS测定的精密度、回收率、检出限和定量限等质量控制参数.结果表明,基质修正液加入量2mL、顶空平衡温度70℃和顶空平衡时间10min为最佳的顶空方法参数;在11～550 μg·kg-1的质量浓度范围内,苯系物各组分的浓度与选择离子峰面积线性相关系数均大于0.99.采用该方法测定土壤中苯系物的平均加标回收率为89.77%～98.64%,相对标准偏差为0.72%～4.64%(n=5);苯系物的检出限(SIN=3)为0.00～0.21 μg·kg-1,定量限(S/N=10)为0.03～0.71 μg·kg-1.
분계물시유궤화학품설루사고중도치토양오염적주요오염물지일,단아국목전환몰건립토양중분계물적표준감측방법.채용정공기상색보-질보련용법(GC-MS)연구료모의오염토양중분계물적측정방법,우화료정공작위토양중분계물예처리방법적삼수,분석료정공GC-MS측정적정밀도、회수솔、검출한화정량한등질량공제삼수.결과표명,기질수정액가입량2mL、정공평형온도70℃화정공평형시간10min위최가적정공방법삼수;재11～550 μg·kg-1적질량농도범위내,분계물각조분적농도여선택리자봉면적선성상관계수균대우0.99.채용해방법측정토양중분계물적평균가표회수솔위89.77%～98.64%,상대표준편차위0.72%～4.64%(n=5);분계물적검출한(SIN=3)위0.00～0.21 μg·kg-1,정량한(S/N=10)위0.03～0.71 μg·kg-1.
Benzene and its analogues are common organic pollutants in soil as consequence of uncontrolled spills, accidents of organic chemicals. However, standard method for monitoring of benzene and its analogues has not been established in China. Method of determination of benzene and its analogues in soil with headspace GC-MS was studied in this paper. Working parameters for beadspace was optimized. Quality control parameters such as precision, recovery of standard, limit of detection and limit of quantification for the process were determined. Results showed that 2 mL of matrix modifying solution with equilibrium temperature 70 ℃ and time 10 minutes were the best for headspace procedure. The linear scope of the method was 11 ～550 μg·kg-1 soil, and the correlation coefficients were higher than 0.99. The average recovery, accuracy, limit of detection and limit of quantification of this method were in the range of 89.77%～98.64 %,0.72%～4.64%,0.01～0.21 μg·kg-1 and 0.03～0.71 μg·kg-1 respectively for benzene and its analogues in soil. Monitoring with headspace GC-MS for benzene and its analogues in soil will be a potential method with the advantages of less loss of analyte and time, easy operation, high sensitive and efficiency.