Determination of silver nanoparticles in complex aqueous matrices by total reflection X-ray fluorescence spectrometry combined with cloud point extraction,Journal of Analytical Atomic Spectrometry

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Determination of silver nanoparticles in complex aqueous matrices by total reflection X-ray fluorescence spectrometry combined with cloud point extraction
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2017-11-20 00:00:00 , DOI: 10.1039/c7ja00335h
Laura Torrent _{1,

2,

3,

4} , Mònica Iglesias _{1,

2,

3,

4} , Manuela Hidalgo _{1,

2,

3,

4} , Eva Marguí _{1,

2,

3,

4}

Affiliation

The development of methods for the analysis of silver nanoparticles (AgNPs) is of special relevance to achieve detailed insights into the fate, transport and exposure of these emerging pollutants in the environment. In the present contribution, for the first time, the possibilities and drawbacks of cloud point extraction (CPE) in combination with total reflection X-ray fluorescence spectrometry (TXRF) have been evaluated for the determination of AgNPs content in soil and consumer product water extracts. The experimental conditions for the separation and preconcentration of AgNPs with different coatings (PVP, PEG and citrate) and sizes (40–100 nm) were evaluated, paying attention to possible modifications required by the characteristics of the TXRF technique. Single particle inductively coupled plasma mass spectrometry (SP-ICPMS) analysis of the same aqueous extracts was also carried out in order to confirm the presence and percentage of AgNPs. Good agreement with respect to AgNPs concentrations in the analysed soil extracts was obtained between CPE-TXRF and SP-ICPMS, confirming the absence of matrix effects for this type of sample by CPE. On the contrary, large discrepancies were found between both analytical approaches for the studied consumer product water extracts. SP-ICPMS analysis evidenced the presence of ionic silver with a heterogeneous mixture of different sizes including relatively large Ag particles (>100 nm). This fact was also verified by SEM-EDS analysis. The results from this study highlight the necessity to study in more detail the effectiveness of existing methodologies (including CPE-based methods and SP-ICPMS) for the monitoring of AgNPs in complex aqueous matrices involving mixtures of different NPs sizes and coatings.

中文翻译：

全反射X射线荧光光谱-浊点萃取法测定复杂水性基质中的银纳米颗粒

研发用于分析银纳米颗粒（AgNPs）的方法具有特殊的意义，以获得对这些新兴污染物在环境中的命运，运输和暴露的详细了解。在本文稿中，首次评估了浊点萃取（CPE）结合全反射X射线荧光光谱法（TXRF）的可能性和缺点，用于测定土壤和消费品水萃取物中的AgNPs含量。评价了具有不同涂层（PVP，PEG和柠檬酸盐）和尺寸（40–100 nm）的AgNP的分离和预富集的实验条件，并注意TXRF技术特性可能需要的修改。为了确认AgNPs的存在和百分比，还对相同的水提取物进行了单颗粒电感耦合等离子体质谱（SP-ICPMS）分析。在CPE-TXRF和SP-ICPMS之间获得了关于分析的土壤提取物中AgNPs浓度的良好一致性，证实了CPE对这种类型的样品不存在基质效应。相反，对于所研究的消费品水提取物，两种分析方法之间发现很大的差异。SP-ICPMS分析证明存在离子银以及不同大小的异质混合物，其中包括相对较大的Ag颗粒（> 100 nm）。SEM-EDS分析也证实了这一事实。

更新日期：2017-11-20

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