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Frontiers of Chemical Science and Engineering

ISSN 2095-0179

ISSN 2095-0187(Online)

CN 11-5981/TQ

Postal Subscription Code 80-969

2018 Impact Factor: 2.809

Front Chem Sci Eng    2012, Vol. 6 Issue (3) : 270-275    https://doi.org/10.1007/s11705-012-1298-x
RESEARCH ARTICLE
Determination of aniline derivatives in water samples after preconcentration with oxidized multiwalled carbon nanotubes as solid-phase extraction disk
Hideyuki KATSUMATA1(), Yuta ODA1, Satoshi KANECO1, Tohru SUZUKI2, Kiyohisa OHTA1
1. Department of Chemistry for Materials, Graduate School of Engineering, Mie University, Tsu 514-8507, Japan; 2. Environmental Preservation Center, Mie University, Tsu 514-8507, Japan
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Abstract

A sensitive and selective preconcentration method using solid-phase extraction (SPE) disk made from oxidized multiwalled carbon nanotubes (OMWCNTs), has been developed for the determination of aniline derivatives, such as 2-nitroaniline (2-NA), 4-nitroaniline (4-NA), and 2,4-dichloroaniline (2,4-DCA) in water samples. Anilines were extracted onto OMWCNT disk and then determined by high performance liquid chromatography (HPLC) with UV detector. Several parameters on the recovery of the analytes were investigated. The experimental results showed that it was possible to obtain quantitative analysis when the solution pH was 8 using 200 mL of validation solution containing 2 μg of anilines and 10 mL of acetonitrile/ethanol (8/2, v/v) as an eluent. Relative standard deviations for five determinations were 7.5% (2-NA), 6.5% (4-NA) and 3.8% (2,4-DCA) under optimum conditions. The linear range of calibration curves were 0.5 ng·mL-1 to 15 ng·mL-1 for each analyte with good correlation coefficients. The detection limits (3S/N) of 2-NA, 4-NA and 2,4-DCA were 30 pg·mL-1, 31 pg·mL-1 and 26 pg·mL-1, respectively. Our method was successfully applied to the determination of aniline compounds in river water sample with high precision and accuracy.

Keywords aniline determination      solid-phase extraction      oxidized multiwalled carbon nanotubes      water sample      HPLC-UV     
Corresponding Author(s): KATSUMATA Hideyuki,Email:hidek@chem.mie-u.ac.jp   
Issue Date: 05 September 2012
 Cite this article:   
Hideyuki KATSUMATA,Yuta ODA,Satoshi KANECO, et al. Determination of aniline derivatives in water samples after preconcentration with oxidized multiwalled carbon nanotubes as solid-phase extraction disk[J]. Front Chem Sci Eng, 2012, 6(3): 270-275.
 URL:  
https://academic.hep.com.cn/fcse/EN/10.1007/s11705-012-1298-x
https://academic.hep.com.cn/fcse/EN/Y2012/V6/I3/270
Fig.1  Effect of OMWCNT amount on the recovery of anilines using the OMWCNT disk for SPE. Concentration of sample solution: 10 ng·mL anilines; sample volume: 200 mL; pH: 8.0; eluent: acetonitrile; eluent volume: 5 mL
Fig.2  Effect of eluent type on the recovery of anilines using the OMWCNT disk for SPE. Concentration of sample solution: 10 ng·mL anilines; sample volume: 200 mL; pH: 8.0; eluent volume: 5 mL
Fig.3  Effect of eluent ratio of acetonitrile to ethanol on the recovery of anilines using the OMWCNT disk for SPE. Concentration of sample solution: 10 ng·mL anilines; sample volume: 200 mL; pH: 8.0; eluent volume: 5 mL
Fig.4  Effect of eluent volume on the recovery of anilines using the OMWCNT disk for SPE. Concentration of sample solution: 10 ng·mL anilines; sample volume: 200 mL; pH: 8.0; eluent: acetonitlile/ethanol (8/2 v/v)
Fig.5  Effect of pH of the sample solution on the recovery of anilines using the OMWCNT disk for SPE. Concentration of sample solution: 10 ng·mL anilines; sample volume: 200 mL; eluent: acetonitrile/ethanol (8/2 v/v); eluent volume: 10 mL
CompoundsLinear range a) /(ng·mL-1)Linearity /R2Detection limit b) /( pg·mL-1)Recovery c) /% (n = 5)RSD / % (n = 5)
2-NA0.5 - 150.9943088±37.5
4-NA0.5 - 150.9983181±76.5
2,4-DCA0.5 - 150.9862695±53.8
Tab.1  Performance of OMWCNTs SPE disk-HPLC method
Fig.6  HPLC chromatograms of three anilines. Spiked concentration: 10 ng·mL anilines; sample volume: 200 mL; pH: 8.0; eluent: acetonitrile/ethanol (8/2, v/v); eluent volume: 10 mL
CompoundsConcentration /(ng·mL-1)Recovery /%
SpikedFound a)
2-NA-n.d.
10.010.8±1.2108
4-NA-n.d.
10.010.7±2.4107
2,4-DCA-n.d.
10.09.8±2.498
Tab.2  Determination of aniline compounds in river water sample (sample solution 200 mL)
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