色谱

色谱 ›› 2014, Vol. 32 ›› Issue (9): 936-941.DOI: 10.3724/SP.J.1123.2014.05026

• 特别策划：新型污染物色谱分析专栏 • 上一篇    下一篇

离子色谱-电感耦合等离子体质谱联用测定大气颗粒物PM2.5和PM10中的六价铬

刀谞1, 吕怡兵1, 滕恩江1, 张霖琳1, 王超1, 李丽和2   

  1. 1. 中国环境监测总站, 北京 100012;
    2. 广西壮族自治区环境监测站, 广西 南宁 530000
  • 收稿日期:2014-05-22 修回日期:2014-07-01 出版日期:2014-09-08 发布日期:2014-08-30
  • 通讯作者: 吕怡兵
  • 作者简介:吕怡兵，lvyb@cnemc.cn.
  • 基金资助:

    环保公益性行业科研专项课题（201309050）.

Determination of hexavalent chromium in atmospheric particles PM2.5 and PM10 by ion chromatography with inductively coupled plasma mass spectrometry

DAO Xu1, LÜ Yibing1, TENG Enjiang1, ZHANG Linlin1, WANG Chao1, LI Lihe2   

  1. 1. China National Environmental Monitoring Centre, Beijing 100012, China;
    2. Environmental Monitoring Center of Guangxi Zhuang Autonomous Region, Nanning 530000, China
  • Received:2014-05-22 Revised:2014-07-01 Online:2014-09-08 Published:2014-08-30

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摘要：

建立了大气颗粒物PM2.5、PM10中六价铬（Cr（Ⅵ））的离子色谱-电感耦合等离子体质谱（IC-ICP-MS）检测方法。采用碳酸氢钠（NaHCO3）溶液超声提取大气颗粒物样品中的Cr（Ⅵ），并使用含有0.22 g/L 乙二胺四乙酸二钠盐（Na2EDTA）的75 mmol/L硝酸铵溶液（pH 7.0）淋洗液通过离子色谱柱（AG7，50 mm×4 mm）分离出样品中的Cr（Ⅵ），电感耦合等离子体质谱测定。标准溶液中Cr（Ⅵ）的质量浓度在0.05~5 μg/L范围内呈良好的线性关系，相关系数达0.9999，标准溶液测定的精密度为1.0%~4.0%，标准样品测定的相对误差为3.3%；纤维素滤膜适用于Cr（Ⅵ）的采样，将纤维素滤膜碱化后，Cr（Ⅵ）的回收率从75%增加到102%；样品在20 mmol/L碳酸氢钠溶液中超声30 min后上机测试，提取完全且回收率稳定；当采样体积为20 m3，方法的检出限为0.0004 ng/m3；采集并测定了PM2.5及PM10实际样品，样品的加标回收率为91.6%~102%，精密度为1.7%~7.6%。该方法高效、稳定、灵敏，适用于大气颗粒物中六价铬的测定。

关键词: PM10, PM2.5, 大气颗粒物, 离子色谱-电感耦合等离子体质谱, 六价铬

Abstract:

An analytical method using ion chromatography with inductively coupled plasma mass spectrometry (IC-ICP-MS) for the determination of hexavalent chromium (Cr(Ⅵ)) in atmospheric particles PM2.5 and PM10 was established. The Cr(Ⅵ) in the atmospheric particles was extracted ultrasonically with sodium bicarbonate solution. An anion exchange column (AG7, 50 mm×4 mm) with 75 mmol/L ammonium nitrate solution (containing 0.22 g/L Na2EDTA, pH 7.0) as mobile phase was used for the separation. ICP-MS was used as a detector for the determination of hexavalent chromium. The calibration curve was linear in the range of 0.05-5 μg/L and the correlation coefficient was 0.9999 for Cr(Ⅵ). The cellulose filter was fit for sampling. With the alkaline cellulose filter, the recovery of Cr(Ⅵ) increased from 75% to 102%. The recovery was complete and stable when the samples were sonicated in 20 mmol/L sodium bicarbonate solution for 30 min. The limit of quantification (LOQ) of Cr(Ⅵ) was 0.0004 ng/m3 when the sampling volume was 20 m3. The average recoveries of Cr(Ⅵ) in the spiked PM2.5 and PM10 samples ranged from 91.6% to 102% with the relative standard deviations not more than 7.6%. The method is efficient and reliable. It can meet the requirement for the determination of Cr(Ⅵ) in atmospheric particles.

Key words: atmospheric particles, hexavalent chromium, ion chromatography with inductively coupled plasma mass spectrometry (IC-ICP-MS), PM10, PM2.5

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