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钯-柠檬酸-氟化铵作为基体改进剂用于克服在通过D2-ETAAS直接测定环境样品王水提取物中锡时出现的干扰。

Palladium-citric acid-ammonium fluoride as a matrix modifier for overcoming of interferences occurring during the direct determination of Sn in aqua regia extracts from environmental samples by D2-ETAAS.

作者信息

Husáková Lenka, Srámková Jitka, Cernohorský Tomás, Urbanová-Dolezalová Iva

机构信息

Department of Analytical Chemistry, Faculty of Chemical Technology, University of Pardubice, Pardubice, CZ, Czech Republic.

出版信息

Talanta. 2009 Feb 15;77(4):1504-9. doi: 10.1016/j.talanta.2008.09.039. Epub 2008 Oct 1.

DOI:10.1016/j.talanta.2008.09.039
PMID:19084671
Abstract

When tin is to be determined in such a complex matrix like aqua regia extracts of environmental samples by electrothermal atomic absorption spectrometry (ETAAS), spectral interferences occur when deuterium-lamp (D(2)) background correction is used, even using high pyrolysis temperature of 1400 degrees C achieved with palladium with citric acid chemical modifier. We have found that the further addition of NH(4)F to palladium with citric acid chemical modifier is essential for overcoming the above-mentioned problems for which aluminium oxide is most probably responsible. It is supposed, that NH(4)F enables volatilization of the alumina matrix formed by hydrolysis from the chloride salt and interfering in a gas phase via the formation of AlF(3) which could be, in contrast to aluminium oxide, removed from the graphite furnace during the pyrolysis stage. Using the proposed chemical modifier, the direct and accurate determination of Sn in aqua regia extracts from rocks, soils and sediments is possible even when using matrix free standard solutions. This presumption was confirmed by the analysis of certified reference samples and by the comparison with inductively coupled plasma time of flight mass spectrometry (ICP-TOFMS) method. Characteristic mass and LOD value for the original sample (10-microL aliquots of sample) was 17 pg and 0.055 microg g(-1), respectively.

摘要

当采用电热原子吸收光谱法(ETAAS)测定环境样品王水提取物这类复杂基体中的锡时,即便使用钯与柠檬酸化学改进剂实现1400℃的高灰化温度,在采用氘灯(D(2))背景校正时仍会出现光谱干扰。我们发现,向钯与柠檬酸化学改进剂中进一步添加NH(4)F对于克服上述问题至关重要,这些问题很可能是由氧化铝导致的。据推测,NH(4)F能使由氯化物盐类水解形成并在气相中通过形成AlF(3)产生干扰的氧化铝基体挥发,与氧化铝不同,AlF(3)可在灰化阶段从石墨炉中除去。使用所提出的化学改进剂,即使使用无基体标准溶液,也能够直接准确地测定岩石、土壤和沉积物王水提取物中的锡。通过对有证标准样品的分析以及与电感耦合等离子体飞行时间质谱法(ICP-TOFMS)的比较,证实了这一推测。原始样品(10微升样品等分试样)的特征质量和检测限分别为17皮克和0.055微克/克。

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