Department of Chemistry, School of Advanced Science (SAS), Vellore Institute of Technology (VIT), Vellore, Tamil Nadu, 632014, India.
Homi Bhabha National Institute (HBNI), Indira Gandhi Centre for Atomic Research (IGCAR), Kalpakkam, Tamil Nadu, 603102, India.
Mikrochim Acta. 2020 Jun 24;187(7):403. doi: 10.1007/s00604-020-04363-y.
The possibility of a multifunctional and reversible solid-state colorimetric sensor is described for the identification and quantification of ultra-trace Cd and Hg ions, using a honeycomb-structured mesoporous silica monolith conjoined with an indigenous chromoionophoric probe, i.e., 4-hexyl-6-((5-mercapto-1,3,4-thiadiazol-2-yl)diazenyl)benzene-1,3-diol (HMTAR). The amphiphilic probe is characterized using NMR, FT-IR, HR-MS, and CHNS elemental analysis. The structural and surface properties of the monolithic template have been characterized using p-XRD, XPS, TEM-SAED, SEM-EDAX, FT-IR, TG-DTA, and N isotherm analysis. The unique structural features and distinct analytical properties of the solid-state sensor proffer a strong response in selectively signaling the target analytes. The probe (HMTAR) exhibits a 1:1 stoichiometric binding ratio with the target ions (Cd & Hg), with a visual color change from pale orange to dark red for Cd (525 nm, λ), and to purple for Hg (530 nm, λ), respectively, in the pH range 7.0-8.0. The influence of various analytical criteria such as pH, temperature, response kinetics, critical probe concentration, sensor quantity, matrix tolerance, linear response range, reusability, the limit of detection (LOD), and quantification (LOQ) has been investigated to validate the sensor performance. The proposed method displays a linear signal response in the concentration range 5-100 μg/L, with a LOD value of 2.67 and 2.90 μg/L, for Cd and Hg, respectively. The real-world efficacy of the sensor material has been tested with real and synthetic water samples with a significant recovery value of ≥ 99.2%, to authenticate its data reliability and reproducibility (RSD ≤ 3.53%). Graphical abstract.
本文描述了一种多功能、可逆的固态比色传感器,用于识别和定量超痕量 Cd 和 Hg 离子,该传感器使用与一种本土显色探针(即 4-己基-6-((5-巯基-1,3,4-噻二唑-2-基)偶氮基)间苯二酚)结合的蜂窝状介孔硅质整体柱。该两亲性探针通过 NMR、FT-IR、HR-MS 和 CHNS 元素分析进行了表征。使用 p-XRD、XPS、TEM-SAED、SEM-EDAX、FT-IR、TG-DTA 和 N 等温线分析对整体模板的结构和表面特性进行了表征。固态传感器的独特结构特征和独特的分析特性提供了对目标分析物进行选择性信号检测的强烈响应。探针(HMTAR)与目标离子(Cd 和 Hg)以 1:1 的化学计量比结合,在 pH 值为 7.0-8.0 范围内,对 Cd(525nm,λ)的颜色从淡橙色变为深红色,对 Hg(530nm,λ)的颜色变为紫色。研究了各种分析标准,如 pH 值、温度、响应动力学、临界探针浓度、传感器数量、基质容忍度、线性响应范围、可重复性、检测限(LOD)和定量(LOQ),以验证传感器性能。该方法在 5-100μg/L 的浓度范围内显示出线性信号响应,Cd 和 Hg 的检出限(LOD)值分别为 2.67 和 2.90μg/L。传感器材料的实际效果已经在真实和合成水样中进行了测试,具有显著的回收率值≥99.2%,以验证其数据可靠性和重现性(RSD≤3.53%)。