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以聚偏氟乙烯为化学改性剂,采用悬浮液进样电热蒸发电感耦合等离子体发射光谱法和电感耦合等离子体质谱法测定大气颗粒物中的难熔元素。

Determination of refractory elements in atmospheric particulates using slurry sampling electrothermal vaporization inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry with polyvinylidene fluoride as chemical modifier.

作者信息

Zhang Yuefei, Jiang Zucheng, Hu Bin

机构信息

Department of Chemistry, Wuhan University, Wuhan 430072, China.

出版信息

Rapid Commun Mass Spectrom. 2006;20(14):2091-8. doi: 10.1002/rcm.2565.

Abstract

Electrothermal vaporization (ETV) inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) with polyvinylidene fluoride (PVDF) as chemical modifier are critically compared for the determination of refractory elements in coal fly ash and airborne particulates. The atmospheric particulates that collected on a PVDF filter were introduced into the graphite furnace in the form of a slurry by dissolving the filter in dimethylformamide, and the dissolved filter PVDF, along with additional added PVDF powder, was used as a chemical modifier for subsequent ETV-ICP-OES and ETV-ICP-MS determination. The vaporization behaviors of analytes (Ti, Zr, V, Mo, Cr, La) in ETV-ICP-OES/MS were studied in detail, and the optimal ETV operating parameters were obtained. Under the optimized operating conditions, the detection limits of target elements were 0.08-2.7 ng m(-3) for ETV-ICP-OES and 0.5-50 pg m(-3) for ETV-ICP-MS, respectively, with analytical precisions of 3.5-7.3% for ETV-ICP-OES and 3.9-9.6% for ETV-ICP-MS, respectively. The tolerable amounts of matrix elements for ETV-ICP-OES are higher than for ETV-ICP-MS. Both ETV-ICP-OES and ETV-ICP-MS were used to directly determine the trace refractory elements in coal fly ash and airborne particulates and the analytical results are comparable.

摘要

对以聚偏二氟乙烯(PVDF)作为化学改性剂的电热蒸发(ETV)电感耦合等离子体发射光谱法(ICP-OES)和电感耦合等离子体质谱法(ICP-MS)进行了严格比较,用于测定粉煤灰和大气颗粒物中的难熔元素。将收集在PVDF滤膜上的大气颗粒物通过将滤膜溶解在二甲基甲酰胺中制成浆液形式引入石墨炉,溶解的滤膜PVDF以及额外添加的PVDF粉末用作后续ETV-ICP-OES和ETV-ICP-MS测定的化学改性剂。详细研究了ETV-ICP-OES/MS中分析物(Ti、Zr、V、Mo、Cr、La)的蒸发行为,并获得了最佳的ETV操作参数。在优化的操作条件下,ETV-ICP-OES对目标元素的检出限为0.08 - 2.7 ng m(-3),ETV-ICP-MS为0.5 - 50 pg m(-3),ETV-ICP-OES的分析精密度为3.5 - 7.3%,ETV-ICP-MS为3.9 - 9.6%。ETV-ICP-OES对基体元素的耐受量高于ETV-ICP-MS。ETV-ICP-OES和ETV-ICP-MS均用于直接测定粉煤灰和大气颗粒物中的痕量难熔元素,分析结果具有可比性。

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