光谱学与光谱分析 |
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Flame Atomic Absorption Spectrometric Determination of H2O2 Using (Au)core(Ag)shell Nanoparticles |
JIANG Zhi-liang1, 2, TANG Ya-fang2, LIANG Ai-hui2, GONG Qi3 |
1. School of Environment and Resource, Guangxi Normal University, Guilin 541004, China 2. The Guangxi Key Laboratory of Environmental Engineering, Protection and Assessment, Guilin University of Technology, Guilin 541004, China 3. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China |
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Abstract The 10 nm gold nanoparticles were prepared by Frens procedure. Using tri-sodium citrate as reducer of AgNO3, and 10 nm gold nanoparticles as seed, the (Au)core(Ag)shell nanoparticles the size of about 30 nm were prepared at 90 ℃ for 10 min. Then it was separated by centrifuge at 10000 r·min-1 for 15 min to obtain pure (Au)core(Ag)shell nanoparticles. In pH 3.8 sodium acetate-acetic acid buffer solution, hydroxyl free radical from Fenton reaction between Fe(Ⅱ)-H2O2 oxidized (Au)core(Ag)shell nanoparticles to form silver ions. The silver ions in the centrifugal solutions can be measured by flame atomic absorption spectrometry at 328.1 nm. The silver ions in the centrifugal solutions increased with the H2O2 concentration increasing, and the absorption value at 328.1 nm was enhanced linearly. The influence factors such as pH value, buffer solution volume, concentration of (Au)core(Ag)shell and Fe(Ⅱ), reaction temperature and time, and centrifuging velocity and time were considered, respectively. Under the conditions of 0.20 mL pH 3.8 sodium acetate-acetic acid buffer solution, 50 μL of 2.0 mmol·L-1 FeSO4, 60 μL of 2.94×10-4 mol·L-1 (Au)core(Ag)shell nanoparticle solution, reaction time of 20 min at 60 ℃, and centrifugalization at 14 000 rpm for 10 min, the increased value ΔA is proportional to the H2O2 concentration (c) from 2.64 to 42.24 μmol·L-1, with a detection limit of 0.81 μmol·L-1. The regress equation was ΔA=0.014c-0.013 1, with a coefficient of 0.998 4. The effect of foreign substances such as 100-times glucose, Cu2+, Mg2+, Ca2+,50-times urea, bovine serum albumin, Mn2+, Pb2+, and 30-times Cr3+ on the determination of 13.2 μmol·L-1 H2O2 was examined respectively, with a relative error of ±10%. Results showed that there was no interference. This assay showed high sensitivity and good selectivity for quantitative determination of H2O2 in waste water samples, with satisfactory results. The analytical results were in agreement with that of the reference results.
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Received: 2008-03-06
Accepted: 2008-06-08
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Corresponding Authors:
JIANG Zhi-liang
E-mail: zljiang@mailbox.gxnu.edu.cn
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