Combination of extraction induced by microemulsion-breaking and pre-concentration using magnetic nanoparticles for multi-element determination of Cd, Cr, Cu and Pb in gasoline samples using energy dispersive X-ray fluorescence spectrometry

Meira, Lucília A.; Almeida, Jorge S.; Dias, Fábio de S.; Teixeira, Leonardo Sena Gomes

doi:10.1016/j.microc.2019.03.068

Cited by 24 publications

(7 citation statements)

References 26 publications

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“…The differences obtained in the EF values may be related to the different affinities and retention process of each element with the AFB-impregnated CoFe 2 O 4 nanoparticles. These EF agree with those obtained previously when MSPME was also used for multielement determination, and the EF were found to be 10, 13, and 25 for Cd, Cu, and Pb, respectively …”

Section: Resultssupporting

confidence: 91%

“…Previous work has shown that pH values below 4 do not show significant extractions when cobalt nanoparticles were used for metal extraction; and, for pH values above 10, a decay of extractions was observed, probably due to the formation of precipitates. 18,38 In addition, in the case of CoFe 2 O 4 impregnated with AFB, solubilization of the complexant in an alkaline medium may occur. This fact was observed when solutions with pH values above 8.0 were used.…”

Section: Resultsmentioning

confidence: 99%

“…These EF agree with those obtained previously when MSPME was also used for multielement determination, and the EF were found to be 10, 13, and 25 for Cd, Cu, and Pb, respectively. 38 The method was applied to the determination of Cd, Cr, Pb, V, and Mo in six biodiesel samples. The results were obtained as the average of three replicates for each sample and are shown in Table 3.…”

Section: Figures Of Merit and Applicationmentioning

confidence: 99%

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Biodiesel Trace Element Analysis by Energy Dispersive X-ray Fluorescence Spectrometry Using Magnetic Solid-Phase Microextraction

et al. 2020

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One parameter to examine biodiesel quality has to do with the existence of metals, given that their presence can negatively affect fuel stability, by virtue of the alteration to their physicochemical properties. Given the significance of monitoring the concentration of metals in biodiesel, this work is aimed at developing a different mode for multielement determination through the use of energy dispersive X-ray fluorescence (EDXRF) spectrometry. For this purpose, an extraction procedure using sample preparation by emulsification associated with magnetic solid-phase microextraction was proposed for separation of Cd, Pb, Cr, V, and Mo from biodiesel samples for posterior analysis using EDXRF spectrometry. The emulsion was prepared by mixing the sample with n-propyl alcohol and 0.01 mol L −1 nitric acid alongside subsequent contact with the solid phase (CoFe 2 O 4 nanoparticles impregnated with alizarin fluorine blue). Constrained mixing design was used to optimize the emulsion composition, and the recommended conditions were 36% (v v −1 ) n-propyl alcohol, 42% (v v −1 ) biodiesel, and 22% (v v −1 ) nitric acid solution for a total volume of 10 mL, using 100 mg of nanoparticles. The proposed extraction allowed enrichment factors of 9.3, 23, 27, 9.7, and 10 for Cd, Cr, V, Pb, and Mo, respectively. The limits of detection were found to be 13, 32, 17, 14, and 25 μg kg −1 for Cd, Pb, Cr, V, and Mo, respectively. Recovery tests were performed by adding 200 μg kg −1 of all analytes in question to six varying biodiesel samples with outcomes that registered between 85 and 114%. The recommended procedure was applied in the analysis of biodiesel, and the highest concentrations observed were 166 μg kg −1 for Cd, 106 μg kg −1 for Cr, 137 μg kg −1 for Pb, 82 μg kg −1 for V, and 92 μg kg −1 for Mo.

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Section: Resultssupporting

confidence: 91%

Section: Resultsmentioning

confidence: 99%

Section: Figures Of Merit and Applicationmentioning

confidence: 99%

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Biodiesel Trace Element Analysis by Energy Dispersive X-ray Fluorescence Spectrometry Using Magnetic Solid-Phase Microextraction

et al. 2020

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“…The comparison of analytical characteristics of UASPME/ICP-OES method for preconcentration of As(III), Cd(II), Cr(III), Co(II), Ni(II), and Pb(II) ions with previously researched preconcentration procedures specifically (solid-phase based extraction) reported in the literature are summarised in Table 7. It was observed that the proposed method had superior LOD, EF, RSD, and linear range compared to those reported elsewhere 42,43 . In the addition, parameters such as liner calibration range, LOD, EF, and RSD for UASPME/ICP-OES technique were www.nature.com/scientificreports/ Regeneration studies.…”

Section: Analytical Figures Of Merit and Methods Validation Analyticamentioning

confidence: 53%

Magnetic Fe3O4@Mg/Al-layered double hydroxide adsorbent for preconcentration of trace metals in water matrices

Nyaba

Munonde

Mpupa

et al. 2021

Sci Rep

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A magnetic Fe3O4@MgAl-layered double hydroxide (MLDH) nanocomposite was successfully synthesized and applied as an effective adsorbent for preconcentration of trace As(III), Cd(II), Cr(III), Co(II), Ni(II), and Pb(II) ions from complex matrices. The quantification of the analytes was achieved using the inductively coupled plasma optical emission spectrometry (ICP-OES) technique. The nanocomposite was then characterized using BET, FTIR, SEM, and EDS. Due to its high adsorption surface area, compared to traditional metal oxide-based adsorbents, MLDH nanocomposite exhibited high extraction efficiency. Several experimental parameters controlling the preconcentration of the trace metals were optimized using response surface methodology based on central composite design. Under optimum conditions, the linearity ranged from 0.1 to 500 µg L−1 and the correlation of coefficients (R2) were higher than 0.999. The limits of detection (LODs) and quantification (LOQs) were 0.11–0.22 µg L−1 and 0.35–0.73 µg L−1, respectively. The intra-day (n = 10) and inter-day precisions (n = 5 working days) expressed in the form of percent relative standard deviations (%RSDs) were below 5%. The proposed method was successfully applied for the analysis of the As(III), Cd(II), Cr(III), Co(II), Ni(II), and Pb(II) ions in different environmental water samples.

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“…Compared with the above-mentioned conventional methods, X-ray fluorescence spectroscopy (XRF) is an important spectroscopy technology for the rapid detection of heavy metals. Because of the advantages of non-destructiveness for the sample, simultaneous determination of multiple elements, less spectral line interference, fast measurement speed and good reproducibility [10], XRF spectrometry has been an effective method for rapid, real-time and online analysis of heavy metal elements. However, when XRF spectrometry is directly applied to detect heavy metals in water samples, there are two main problems: The first one is when aqueous solution is irradiated by high energy X-rays, some chemical reactions will happen between elements in the irradiated part due to local heating, at the same time some phenomena such as bubbling and precipitation will appear, which makes the X-ray fluorescence intensity very easy to change and seriously affects the reproducibility and stability of the analytical signal.…”

Section: Introductionmentioning

confidence: 99%

Preconcentration with Chlorella vulgaris combined with energy dispersive X-ray fluorescence spectrometry for rapid determination of Cd in water

et al. 2020

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Freshwater green algae Chlorella vulgaris was selected as an adsorbent, and a simple, rapid, economical and environmentally friendly method for the detection of heavy metal Cd in water samples based on preconcentration with C. vulgaris combined with energy dispersive X-ray fluorescence (EDXRF) spectrometry was proposed. Chlorella vulgaris could directly and rapidly adsorb Cd 2+ without any pretreatment, and the maximum adsorption efficiency could be obtained when the contact time was 1 min with an optimal pH of 10. The obtained Cd-enriched thin samples after preconcentration with C. vulgaris by suction filtration of reaction solution had very good uniformity, which could be directly measured by EDXRF spectrometry, and the net integral fluorescence intensity of Cd K α characteristic peak had a very good linear relationship with the initial concentration of Cd in the range of 0.703–74.957 µg ml −1 with a correlation coefficient of 0.9979. When the Cd thin samples with a Cd-enriched region of 15.1 mm in diameter were formed by the developed preconcentration method with suction filtration of 10 ml reaction solution, the detection limit of this method was 0.0654 µg ml −1 , which was lower than the maximum allowable discharge concentration of Cd in various industrial wastewaters. The proposed method was simple to operate, and could effectively remove the influence of matrix effect of water samples and effectively improve the sensitivity and stability of EDXRF spectrometry directly detecting heavy metals in water samples, which was successfully applied to detect Cd in real water samples with satisfactory results, and the recoveries ranged from 94.80% to 116.94%. Moreover, this method can be applied to the rapid detection and early warning of excessive Cd in discharged industrial wastewaters. This work will provide a methodological basis for the development of rapid and online monitoring technology and instrument of heavy metal pollutants in water.

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Combination of extraction induced by microemulsion-breaking and pre-concentration using magnetic nanoparticles for multi-element determination of Cd, Cr, Cu and Pb in gasoline samples using energy dispersive X-ray fluorescence spectrometry

Cited by 24 publications

References 26 publications

Biodiesel Trace Element Analysis by Energy Dispersive X-ray Fluorescence Spectrometry Using Magnetic Solid-Phase Microextraction

Biodiesel Trace Element Analysis by Energy Dispersive X-ray Fluorescence Spectrometry Using Magnetic Solid-Phase Microextraction

Magnetic Fe3O4@Mg/Al-layered double hydroxide adsorbent for preconcentration of trace metals in water matrices

Preconcentration with Chlorella vulgaris combined with energy dispersive X-ray fluorescence spectrometry for rapid determination of Cd in water

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