Beccaloni E, Musmeci L, Stacul E
Laboratory of Environmental Hygiene, National Institute of Health, Viale Regina Elena 299, 00161 Rome, Italy.
Anal Bioanal Chem. 2002 Dec;374(7-8):1230-6. doi: 10.1007/s00216-002-1620-4. Epub 2002 Nov 9.
In line with recent European environmental guidelines on biomasses, one of the most important parameters to take into account is the As concentration, especially when present in biomasses and complex matrices. The goal of the present study is to give information about possible technical-analytical problems during the determinations of such elements by means of different instrumental spectroscopy techniques, in particular inductively coupled plasma atomic emission (ICP-AES) and atomic absorption (AAS), using two different wavelengths, 188.98 nm and 193.70 nm. In the Laboratory of Hygiene of National Institute of Health in Italy, a specific study has been carried out concerning the determination of As contents in environmental solid matrices, using as reference material BCR 141 R, represented by a calcareous soil. In particular, whereas recovery tests did not show particular drawbacks, difficulties were met in the As detection in reference material. Spectral interference was seen during determination by ICP-AES and matrix interference during determination by AAS, in particular using ETAAS with deuterium background correction and HAAS. Using ETAAS with Zeeman background correction at 193.70 nm, the As line did not show particular matrix interference during the reading of samples.A ring test involving two more laboratories and another certified reference material (IAEA-356 in marine sediment matrix) produced important information about problems of under/over estimation of data. Two different instrumental techniques, ICP-MS and HAAS, confirmed previous data, i.e., overestimation for inductively coupled plasma mass spectrometry and that As values achieved by HAAS were of the same order as the references, but affected by considerable standard deviation. In the light of this study, data achieved on the environmental matrices investigated suggest that the critical step in As determination is the instrumental reading, rather than the mineralization process. Further, each of the methods proposed, apart from ETAAS with Zeeman background correction, presents its own peculiar drawbacks and no particular advantage over other techniques.
根据欧洲最近关于生物质的环境指南,需要考虑的最重要参数之一是砷浓度,尤其是当砷存在于生物质和复杂基质中时。本研究的目的是提供有关通过不同的仪器光谱技术(特别是电感耦合等离子体原子发射光谱法(ICP-AES)和原子吸收光谱法(AAS))测定此类元素时可能出现的技术分析问题的信息,使用两种不同的波长,即188.98纳米和193.70纳米。在意大利国家卫生研究院卫生实验室,针对环境固体基质中砷含量的测定开展了一项具体研究,使用由钙质土壤代表的BCR 141 R作为参考物质。特别是,回收率测试未显示出特别的问题,但在参考物质的砷检测中遇到了困难。在ICP-AES测定过程中出现了光谱干扰,在AAS测定过程中出现了基质干扰,尤其是使用带氘背景校正的电热原子吸收光谱法(ETAAS)和氢化物发生原子吸收光谱法(HAAS)时。在193.70纳米处使用带塞曼背景校正的ETAAS时,在读取样品过程中砷谱线未显示出特别的基质干扰。一项涉及另外两个实验室和另一种有证参考物质(海洋沉积物基质中的IAEA-356)的比对试验得出了有关数据低估/高估问题的重要信息。两种不同的仪器技术,即电感耦合等离子体质谱法(ICP-MS)和HAAS,证实了先前的数据,即电感耦合等离子体质谱法存在高估情况,并且HAAS获得的砷值与参考值处于同一数量级,但受到相当大的标准偏差影响。根据这项研究,在所研究的环境基质上获得的数据表明,砷测定中的关键步骤是仪器读数,而不是矿化过程。此外,除了带塞曼背景校正的ETAAS外,所提出的每种方法都有其自身的特殊缺点,并且相对于其他技术没有特别的优势。