摘要
研究并建立了气相色谱-负化学电离同位素稀释质谱法(GC-NCI-IDMS)同时测定大气颗粒物中27种硝基多环芳烃(NPAHs)的分析方法。采用选择性加速溶剂提取法(SPLE)对颗粒物样品进行一体化的提取与净化,在萃取池中填充0.5g弗罗里硅土及0.5g硅胶作为吸附剂,用二氯甲烷-正己烷(1∶1,v/v)在120℃下循环4次提取。结果表明,27种NPAHs在30分钟内即可完成分离,检出限(LOD,S/N=3)为0.056~8.3pg/m3。27种NPAHs的加标回收率在90.0%~121.3%,相对标准偏差低于6.0%,在环境样品浓度区间内,峰面积与浓度的线性关系良好。该方法快速准确,灵敏度高,可以满足大气颗粒物中NPAHs的准确测定需求。
A gas chromatography-negative chemical ionization isotope dilution mass spectrometry method( GC-NCIIDMS) was developed for the simultaneous determination of 27 nitropolycyclic aromatic hydrocarbons( NPAHs) in atmospheric particulates. Particulate matter samples were extracted and purified by selective pressurized liquid extraction( SPLE).0. 5 g florisil + 0. 5 g silica gel was filled in the ASE cell as adsorbent,and dichloromethane-n-hexane( 1∶1,v/v) was used as an extraction solvent. The samples were extracted at 120℃ for 4 cycles. The results showed that 27 NPAHs could be separated within 30 minutes,and the detection limit( LOD,S/N = 3) was 0. 056 ~ 8. 3 pg/m^3. The recovery of 27 NPAHs was90. 0% ~ 121. 3%,and the relative standard deviation was less than 6. 0%. The linearity of peak area and concentration was good in the concentration range of environmental samples. The developed method is rapid,accurate,and sensitive,which is suitable for the simultaneous analysis of NPAHs in atmospheric particulates.
作者
汤桦
赵新颖
叶昌俊
陈大舟
吴雪
TANG Hua;ZHAO Xinying;YE Changjun;CHEN Dazhou;Wu Xue(National Institute of Metrology,Beijing 100029,China;Beijing Center for Physical and Chemical Analysis,Beijing 100094,China;Beijing University of Chemical Technology,Beijing 100029,China)
出处
《计量技术》
2020年第5期68-73,共6页
Measurement Technique
基金
国家重点研发计划(2016YFF0201102)。
