A novel ionic liquid electrostatically supported Nano-Cspolyoxomolybdate modified carbon paste electrode (Nano-PMo12/IL-CPE) has been developed by using 1-n-butyl-3-methylimidazolium tetrafluoroborate (Bmim.BF4) as a hydrophobic binder. The supramolecular gel (PMo12/IL) exhibits an ordered structure, various physicochemical properties, and specifically as a result of its substantial reversible self-assembly, it can be used as an intelligent ion-exchange smart platform in the carbon paste bulk of the electrode. As expected, a significant linear correspondence was found between the sensor output signal (emf/mV) and logarithm of Al(III) ion activity with a Nernstian slope of 19.9 (±0.2) mVdecade-1 over a wide concentration range of 1.0×10-9 to 2.2×10-1 molL-1 (R2=0.9999). The sensor considered, exploits an astounding lower limit of detection and short response time of 7.94×10-10 molL-1 and 8.0 sec. respectively within the working pH range of 2.0 to 5.0. A statistical design of experimental (Taguchi method with Qualitek-4 software and L16 orthogonal array robust design) was implemented in this work to optimize the process to achieve the least number of experimental runs as much as possible. Ultimately, practical capability of the sensor was investigated successfully by assessment of Al(III) ion quantity in some aqueous samples namely mineral water, Al-Mg syrup, black tea extract, and ore samples (Basalt and Andesite), in perfect agreement with flame atomic absorption spectroscopy (FAAS).
A simple strategy has been developed based on 1,2-bis[5,2-thiolmethyl-sulphide-1,3,4-oxadiazol-2-yl]ethane (BTMSOE) as a novel ion-carrier for construction of a voltammetric Hg(II)-CPE. AuNPs not only have strong inter-particle binding affinity (Au-Au), but also have strong tendency to form S-Au covalent bonds with -SH functional groups. In view of this fact, by self-assembling of AuNPs, the spatial configuration of the thiol-terminated BTMSOE compound was switched from podant to macrocycletype ligand. The macrocycle-type BTMSOE-AuNP compound was then immobilized by self-assembly on the super-conductive MWCNT substrate via a (3-mercaptopropyl) trimethoxysilane (MPTS) covalent linker. Under the optimized conditions, the oxidative current I p,a (mA) exhibited a linear dependence on Hg(II) ion concentration in the wide dynamic concentration ranges of 3.5 Â 10 À11 to 3.7 Â 10 À7 M and 1.2 Â 10 À6 to 1.0 Â 10 À4 M (R 2 ¼ 0.9947 and 0.9992, respectively). Moreover, the limit of detection of the proposed sensor was 1.7 Â 10 À12 mol L À1 (S/N ¼ 3) at a working optimal pH of 4.2 adjusted by ABS as an appropriate supporting electrolyte. These features, specifically the high sensitivity and exceptional selectivity, were positively compared with those of previously reported methods in the area of electrochemical Hg(II) detection. Eventually, the practical utility of the prepared MWCNTs/AuNPs/ BTMSOE-CPE was assessed for efficient determination of Hg(II) contents in aqueous environmental samples with different matrices such as tap and mineral water, tuna fish, human hair, and tobacco.
A novel ionic liquid carbon paste electrode has been developed using sol-gel/Au nanoparticle (SGAN) involving (NS) 2 compound of N,N 0 -di-(cyclopentadienecarbaldehyde)-1,2-di(o-aminophenylthio) ethane (CCAE) as an appropriate neutral ion-carrier for ultrahigh-sensitive potentiometric determination of Ag(I). Colloidal gold nanoparticles (AuNPs) also well dispersed self-assembly into the 3-(mercaptopropyl)-trimethoxysilane (MPTS)-derived sol-gel network through Au-S covalent bond engendering continuous and super-conductive nanoporous three-dimensional array. The room-temperature ionic liquid, 1-n-butyl-3-methylimidazolium tetrafluoroborate (BMIM.PF 6 ), was applied as a super-conductive pasting agent (binder). The SGAN/CCAE/IL-CPE exhibited a significantly enhanced sensitivity and preferential selectivity toward Ag(I) over a wide concentration range of 2.4 9 10 -9 to 2.2 9 10 -2 mol L -1 (R 2 = 0.9996) with a lower limit of detection of 7.9 9 10 -10 M and a Nernstian slope of 58.5 (±0.3) mV decade -1 . The electrode has a short response time of *5 s and long-time durability of about 2 months without any considerable divergence in potentials. Moreover, the potentiometric examinations could be carried out within the wide pH range of 3.5-9.5. Eventually, the practical utility of the proposed Ag(I)-sensor was evaluated by volumetric titration of AgNO 3 solution by sodium chloride and recovery of silver content in some real samples using flame atomic absorption spectroscopy as a confident reference.
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