Speciation of inorganic As and Sb in natural waters by total reflection X-ray fluorescence following selective hydride generation and trapping onto quartz reflectors coated with nanostructured Pd,Journal of Analytical Atomic Spectrometry

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Speciation of inorganic As and Sb in natural waters by total reflection X-ray fluorescence following selective hydride generation and trapping onto quartz reflectors coated with nanostructured Pd
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2017-05-04 00:00:00 , DOI: 10.1039/c7ja00113d
Vanesa Romero _{1,

2,

3,

4,

5} , Laura Vilas _{1,

2,

3,

4,

5} , Isela Lavilla _{1,

2,

3,

4,

5} , Carlos Bendicho _{1,

2,

3,

4,

5}

Affiliation

In this work, a novel analytical approach for the speciation of inorganic As (iAs) and inorganic Sb (iSb) by total reflection X-ray fluorescence based on the selective generation of arsine and stibine followed by trapping onto quartz reflectors containing immobilized palladium nanoparticles (Pd NPs) is developed. Pd NPs were synthesized by chemical reduction under mild conditions (i.e., a water : ethanol mixture was used as the reducing agent) and immobilized onto quartz substrates following the silanization strategy with 3-mercaptopropyltrimethoxysilane. For microextraction and preconcentration of iAs and iSb, volatile hydrides generated in a continuous flow system were flushed onto the immobilized Pd NPs for catalytic decomposition at ambient temperature. A 2⁶⁻²_III factorial fractional design was used for screening the effect of the variables involved in the hydride generation and preconcentration steps. Selective trapping of As(III) and Sb(III) was accomplished following arsine and stibine generation under different reaction conditions, i.e., selective determination of As(III) in citric acid/citrate buffer medium (pH 4.5) and selective determination of Sb(III) in a highly acidic medium (pH < 2). In addition, As(V) and Sb(V) were pre-reduced to As(III) and Sb(III) with a KI–ascorbic acid mixture for simultaneous determination of total iAs and total iSb. The As(V) and Sb(V) contents were estimated by the difference between both measurements. Limits of detection (LODs) of 0.09, 0.10, 0.50 and 0.80 μg L⁻¹ for As(III), As(V), Sb(III) and Sb(V) were obtained, respectively. Overall efficiencies of 75% for iAs and 80% for iSb were obtained. Speciation analysis of iAs and iSb in natural waters at the sub-ppb level is demonstrated.

中文翻译：

选择性氢化物生成后，通过全反射X射线荧光并捕获到涂有纳米结构钯的石英反射器上，自然水中无机砷和锑的形态

在这项工作中，一种基于选择性生成of和锑的全反射X射线荧光技术对无机As（iAs）和无机Sb（iSb）进行形态分析的新颖分析方法，然后将其捕获到包含固定化钯纳米粒子的石英反射器上（开发了Pd NPs。通过在温和条件下化学还原（即，使用水：乙醇混合物作为还原剂）合成Pd NP，并按照3-巯基丙基三甲氧基硅烷的硅烷化策略将其固定在石英基板上。为了进行iAs和iSb的微萃取和预浓缩，将连续流系统中生成的挥发性氢化物冲洗到固定的Pd NPs上，以在环境温度下催化分解。A 2 ⁶⁻²_III析因分式设计用于筛选参与氢化物生成和预浓缩步骤的变量的影响。作为（选择性俘获III）和Sb（III）中的溶液来实现不同的反应条件下，下面的胂和锑化氢生成即，作为（的选择性测定III）在柠檬酸/柠檬酸盐缓冲液中（pH 4.5）中和选择性测定的Sb（III）在高酸性介质中（pH <2）。此外，用KI-抗坏血酸混合物将As（V）和Sb（V）预先还原为As（III）和Sb（III），以便同时测定总iAs和总iSb。As（V和Sb（V）含量是通过两次测量之间的差异估算的。对于As（III），As（V），Sb（III）和Sb（V）的检测限（LOD）分别为0.09、0.10、0.50和0.80μgL ^-1。对于iAs和iSb，总效率分别为75％和80％。演示了在亚ppb级的天然水中iAs和iSb的形态分析。

更新日期：2017-05-04

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