A comparative study of two nanosubstrates for the on-line solid phase extraction of antimony by FI-HG-AAS (original) (raw)
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Journal of Chromatography A, 1997
A method is described for the selective determination of Sb(IlI) in the presence of Sb(V) by capillary column gas chromatography-quartz furnace atomic absorption spectrometry. Sb(III) is complexed with pyrrolidinedithiocarbamate in a medium buffered with acetic acid-acetate at pH 4.5 and extracted into hexane; once extracted, Sb(III) is derivatized into a volatile gas chromatographable species, triphenylstibine, by Grignard reaction with phenylmagnesium bromide. A cool injection programmed-temperature vaporization injector (CTI) was used. Parameters affecting the extraction and derivatization reactions, as well as the atomization temperature in the quartz furnace and the maximum volume of organic phase that can be injected in the CTI, were optimized. The method was applied to the determination of Sb(IIl) in spiked tap water.
Solid-Phase Extraction of Antimony Using Chemically Modified SiO2-PAN Nanoparticles
Journal of AOAC INTERNATIONAL, 2010
A new analytical method using 1-(2-pyridylazo)-2-naphthol (PAN)-modified SiO2 nanoparticles as solid-phase extractant has been developed for the preconcentration of trace amounts of Sb(III) in different water samples. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions, and effects of interfering ions for the recovery of the analyte were investigated. The adsorption capacity of nanometer SiO2-PAN was found to be 186.25 mol/g at optimum pH and the LOD (3) was 0.60 g/L. The extractant showed rapid kinetic sorption. The adsorption equilibrium of Sb(III) on nanometer SiO2-PAN was achieved in 10 min. Adsorbed Sb(III) was easily eluted with 4 mL 2 M hydrochloric acid. The maximum preconcentration factor was 62.20. The method was applied for the determination of trace amounts of Sb(III) in various water samples (tap, mineral water, and industrial effluents).
Talanta, 2016
The determination of Sb(III) on an ex-situ bismuth screen-printed carbon electrode (ex-situ BiSPCE) by means of adsorptive stripping voltammetry (AdSV) using quercetin-5'-sulfonic acid as chelating agent was optimized. The effect of different experimental parameters such pH, ligand concentration (CQSA), accumulation potential (Eacc) and accumulation time (tacc) were studied to obtain a wide linear range, the highest sensitivity and the lowest detection limit. Ex-situ BiSPCE was analytically compared with a sputtered bismuth screen-printed electrode (BispSPE) under optimal conditions. The obtained analytical parameters suggest that ex-situ BiSPCE behaves much better than BispSPE and the first was selected for this study. Optimal parameters were pH=4.6; CQSA=10.0 to 20.0×10(-6)molL(-1); Eacc=-0.5V and tacc=60s. Peak area is proportional to Sb(III) concentration up to 100.0μgL(-1) (tacc 60s) and 45.0μgL(-1) (tacc 120s) range, with detection limits of 1.2μgL(-)(1) (tacc 60s) and 0.8...
Environmental Monitoring and Assessment, 2023
Antimony (Sb) has been classified as a high-priority contaminant in the environment. Sb contamination resulting from the use of antimony containing compounds in industry necessitates the development of efficient methods to remove it from water and wastewater. Adsorption is a highly efficient and reliable method for pollutants removal owing to its availability, recyclability, and low cost. Recently, carbonaceous materials and their applications for the removal of Sb from the aqueous matrices have received special attention worldwide. Herein, this review systematically summarizes the occurrence and exposure of Sb in the environment and on human health, respectively. Different carbon-based adsorbents have been classified for the adsorptive removal of Sb and their adsorption characteristics have been delineated. Recent development in the adsorption performance of the adsorbent materials for improving the Sb removal from the aqueous medium has been outlined. Further, to develop an understanding of the effect of different parameters like pH, competitive ions, and dissolved ions for Sb adsorption and subsequent removal have been discussed. A retrospective analysis of literature was conducted to present the adsorption behavior and underlying mechanisms involved in the removal of Sb using various adsorbents. Moreover, this study has identified emerging research gaps and emphasized the need for developing modified/engineered carbonaceous adsorbents to enhance Sb adsorption from various aqueous matrices.
Fresenius Journal of Analytical Chemistry, 1997
A new method for the fast and simultaneous determination of Sb(III) and Sb(V) is presented involving the use of anion exchange high-performance liquid chromatography (HPLC), a complexing reagent in the mobile phase, and element specific detection with flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic parameters such as nature and concentration of the complexing and
Spectrochimica Acta Part B-atomic Spectroscopy, 2011
A novel absorbent was prepared by dimercaptosuccinic acid chemically modifying mesoporous titanium dioxide and was employed as the micro-column packing material for simultaneous separation/preconcentration of inorganic arsenic and antimony species. It was found that both trivalent and pentavalent of inorganic As and Sb species could be adsorbed quantitatively on dimercaptosuccinic acid modified TiO 2 within a pH range of 4-7, and only As(III) and Sb(III) could be quantitatively retained on the micro-column within a pH range of 10-11 while As(V) and Sb(V) were passed through the micro-column without the retention. Based on this fact, a new method of flow injection on-line microcolumn separation/preconcentration coupled to inductively coupled plasma optical emission spectrometry was developed for simultaneous speciation of trace inorganic arsenic and antimony in natural waters. Under the optimized conditions, an enrichment factor of 10 and sampling frequency of 10 h − 1 were obtained with on-line mode. The detection limits of As(III), As(V), Sb(III), and Sb(V) are 0.53, 0.49, 0.77 and 0.71 ng mL − 1 for on-line mode and as low as 0.11, 0.10, 0.15 and 0.13 ng mL − 1 for off-line mode due to its higher enrichment factor (50), respectively. The relative standard deviations of two modes are less than 6.7% (C = 20 ng mL − 1 , n = 7). The concentration ratio of lower oxidation states/higher oxidation states changing from 1:10 to 10:1 has no obvious effect on the recoveries of As(III) and Sb(III). In order to validate the developed method, two certified reference materials of GSBZ5004-88 and GBW(E)080545 water sample were analyzed and the determined values are in good agreement with the certified values. The proposed method was successfully applied to the simultaneous speciation of inorganic arsenic and antimony in natural waters.
Food Chemistry, 2019
In the present paper, a new analytical preconcentration/speciation method for antimony species determination in bottled mineral water samples using the SiO 2 /Al 2 O 3 /SnO 2 adsorbent was developed. The method is based on selective adsorption of Sb(III) ions by SiO 2 /Al 2 O 3 /SnO 2 under a wide pH range (2.5 to 7.5). Total antimony was determined with previous sample treatment using 0.1% (w/v) Lcysteine and the concentration of Sb(V) species was determined by the difference between total and Sb(III). The proposed method provided an analytical curve ranging from 0.50 to 5.00 μg L −1 (r = 0.999), limit of detection (LD) of 0.17 µg L-1 and preconcentration factor (PF) of 136-fold. The method exhibited tolerance to different metal ions and the accuracy was attested from addition and recovery tests (95.2-106.0%) in bottled mineral water samples using 2.0% (w/v) L-cysteine, as well as by analysis of certified material. Only Sb(III) species were determined in mineral water (0.54-1.04 g L-1).
Sensors and Actuators B: Chemical, 2013
A high sensitivity method for voltammetric determination of Sb(III) using quercetin-5-sulfonic acid (QSA) as complexing and adsorbing agent is presented. The Sb-QSA is accumulated on the electrode surface and then reduced at about −0.67 V. Optimal analytical conditions were pH: 5.5, C QSA : 3.0 mol L −1 , E ads : −0.10 V and t ads : 60 s. The detection limit (3) depends on accumulation time, reaching 3.6 ng L −1 and 1.6 ng L −1 with t ads of 60 s and 180 s, respectively. Peak current is proportional to Sb(III) concentration up to 10.0 g L −1 and 1.5 g L −1 with t ads of 60 s and 180 s, respectively. The relative standard deviation were 1.7% and 2.5% for a solution containing 1.0 g L −1 and 5.0 g L −1 of Sb(III), respectively (n = 10). Interference by other metal ions was studied. The proposed method was applied to the determination of antimony in natural and spiked water samples, with satisfactory results. The method was designed in order to compare the sensitivity of the methods that use quercetin and the sulfonic derivative.
Electroanalysis, 2008
A simple procedure was developed to prepare a glassy carbon (GC) electrode modified with single-walled carbon nanotubes (SWCNTs) and polyoxometalate. With immersing SWCNTs modified GC electrode in silicon polyoxomolybdate (α-SiMo12O404−) solution (direct deposition) for a short period of time (2–10 s) oxoanion adsorbed strongly and irreversibly on SWCNTs. Cyclic voltammograms of the α-SiMo12O404− incorporated-SWCNTs indicates three well-defined and reversible redox couples with surface confined characteristic at wide pH range (1–7). The surface coverage (Γ) of α-SiMo12O404− immobilized on SWCNTs was 2.14 (±0.11)×10−9 mol cm−2 indicating high loading ability of SWCNTs for polyoxometalate. The charge transfer rate constant (ks) of three redox couples of adsorbed α-SiMo12O404− were 9.20 (±0.20), 8.02 (±0.20), and 3.70 (±0.10) s−1, respectively, indicate great facilitation of the electron transfer between α-SiMo12O404− and CNTs. In this research the attractive mechanical and electrical characteristics of CNTs and unique properties and reactivity of polyoxometalates were combined. The modified electrode in buffer solution containing Sb(III) shows a new redox system at 0.38 V in pH 1. The voltammetric peak current increased with increasing Sb(III) concentration. The differential pulse voltammetry (DPV) technique was used for detection micromolar concentration of antimony. Furthermore, the interference effects various electroactive compounds on voltammetric response of Sb(III) were negligible. Finally the ability of the modified electrode for antimony detection in real samples was evaluated.