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      Highly sensitive determination of 2, 4, 6-trinitrotoluene and related byproducts using a diol functionalized column for high performance liquid chromatography

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      Author(s)
      Gumuscu, B.
      Erdogan, Z.
      Güler, Mustafa O.
      Tekinay, T.
      Date
      2014
      Source Title
      PLOS ONE
      Print ISSN
      1932-6203
      Publisher
      Public Library of Science
      Volume
      9
      Issue
      6
      Pages
      1 - 8
      Language
      English
      Type
      Article
      Item Usage Stats
      214
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      165
      downloads
      Abstract
      In this work, a new detection method for complete separation of 2,4,6-trinitrotoluene (TNT); 2,4-dinitrotoluene (2,4-DNT); 2,6-dinitrotoluene (2,6-DNT); 2-aminodinitrotoluene (2-ADNT) and 4-aminodinitrotoluene (4-ADNT) molecules in high-performance liquid-chromatography (HPLC) with UV sensor has been developed using diol column. This approach improves on cost, time, and sensitivity over the existing methods, providing a simple and effective alternative. Total analysis time was less than 13 minutes including column re-equilibration between runs, in which water and acetonitrile were used as gradient elution solvents. Under optimized conditions, the minimum resolution between 2,4-DNT and 2,6-DNT peaks was 2.06. The recovery rates for spiked environmental samples were between 95-98%. The detection limits for diol column ranged from 0.78 to 1.17 μg/L for TNT and its byproducts. While the solvent consumption was 26.4 mL/min for two-phase EPA and 30 mL/min for EPA 8330 methods, it was only 8.8 mL/min for diol column. The resolution was improved up to 49% respect to two-phase EPA and EPA 8330 methods. When compared to C-18 and phenyl-3 columns, solvent usage was reduced up to 64% using diol column and resolution was enhanced approximately two-fold. The sensitivity of diol column was afforded by the hydroxyl groups on polyol layer, joining the formation of charge-transfer complexes with nitroaromatic compounds according to acceptor-donor interactions. Having compliance with current requirements, the proposed method demonstrates sensitive and robust separation. © 2014 Gumuscu et al.
      Keywords
      2 aminodinitrotoluene
      2,4 dinitrotoluene
      2,6 dinitrotoluene
      4 aminodinitrotoluene
      Acetonitrile
      Aromatic nitro compound
      Hydroxyl group
      Trinitrotoluene
      Unclassified drug
      Water
      Chemical analysis
      Controlled study
      Environmental monitoring
      High performance liquid chromatography
      Limit of detection
      Molecular interaction
      Process optimization
      Sensitivity analysis
      Ultraviolet radiation
      Permalink
      http://hdl.handle.net/11693/25969
      Published Version (Please cite this version)
      https://doi.org/10.1371/journal.pone.0099230
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      • Institute of Materials Science and Nanotechnology (UNAM) 2258
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