A simple dispersive-micro-solid phase extraction based on a colloidal silica sorbent for the spectrophotometric determination of Fe(ii) in the presence of tetrabutylammonium bromide†,New Journal of Chemistry

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A simple dispersive-micro-solid phase extraction based on a colloidal silica sorbent for the spectrophotometric determination of Fe(ii) in the presence of tetrabutylammonium bromide†
New Journal of Chemistry ( IF 2.7 ) Pub Date : 2018-01-15 00:00:00 , DOI: 10.1039/c7nj04172a
S. Metarwiwinit _{1,

2} , S. Mukdasai _{1,

2} , C. Poonsawat _{1,

2} , S. Srijaranai _{1,

2}

Affiliation

This study demonstrates a simplified dispersive micro-solid phase extraction (d-μ-SPE) using silica sol as the sorbent for the preconcentration of ferrous ions. Ferrous ions were prederivatized via complexation with 1,10-phenanthroline (Phen) before being adsorbed by the silica sol. The adsorption of the [Fe²⁺-Phen] complex simultaneously occurred with aggregation of the silica sol with the assistance of the phase transfer catalyst (PTC) tetrabutylammonium bromide. The enriched [Fe²⁺-Phen] complex on the silica sol was directly detected using a spectrophotometer at 510 nm. Several experimental parameters including the amount of silica sol, pH, PTC, extraction and centrifugation times were investigated. Under the optimal conditions, the enrichment factor was 7.3 and the linear range was from 0.07 mg L⁻¹ to 1.43 mg L⁻¹. The limit of detection and the limit of quantitation were 16 μg L⁻¹ and 54 μg L⁻¹, respectively. Furthermore, the precision, expressed as the relative standard deviation, was lower than 4% from ten replicates. The extraction recoveries of Fe²⁺ in cereal and vegetable samples were 71.0–107.5%. In addition, a camera in combination with Image J program was used as an alternative tool for the detection of the adsorbed [Fe²⁺-Phen] complex.

中文翻译：

在四丁基溴化铵存在下，基于胶体二氧化硅吸附剂的简单分散微固相萃取光度法测定Fe（ii）†

这项研究表明，使用硅溶胶作为吸附剂对亚铁离子进行预浓缩，可以简化分散微固相萃取（d-μ-SPE）。亚铁离子通过与1,10-菲咯啉（Phen）络合进行去衍生，然后被硅溶胶吸收。[Fe ²⁺ -Phen]配合物的吸附是在相转移催化剂（PTC）四丁基溴化铵的帮助下硅溶胶的聚集而发生的。富集的[Fe ²⁺使用分光光度计在510 nm处直接检测硅溶胶上的-Phen]配合物。研究了几个实验参数，包括硅溶胶的量，pH，PTC，萃取和离心时间。在最佳条件下，富集因子为7.3，线性范围为0.07 mg L ^-1至1.43 mg L ^-1。检测极限和定量极限分别为16μgL ^-1和54μgL ^-1。此外，精确度（表示为相对标准偏差）在十次重复实验中均低于4％。Fe ²⁺的萃取回收率谷物和蔬菜样品中的总含量为71.0–107.5％。此外，结合Image J程序的照相机被用作检测吸附的[Fe ²⁺ -Phen]配合物的替代工具。

更新日期：2018-01-15

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