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Synthesis, characterization, and application of chemically interconnected carbon nanotube monolithic sorbents by photopolymerization in polypropylene caps

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Abstract

A facile and convenient approach for the preparation of interconnected multiwalled carbon nanotube (MWCNT) monolithic sorbents in recycled plastic caps has been developed. The method, which was based on the photopolymerization of the individual MWCNTs via the formation of a W/O medium internal phase emulsion (40/60 w/w%), provides control over the size of pores, rigidity, and the mechanical stability of the final solid. Pluronic L121 was used as a surfactant containing the water phase inside it and, consequently, the organic and non-polar phase, in which the MWCNTs and the cross-linker were trapped, remained on the outside of the droplets. Optical microscopy and scanning electron microscopy (SEM) were employed to characterize the morphology of both the emulsions and the final solids, respectively. In addition, nitrogen intrusion porosimetry was performed in order to study how the specific surface area of the final monolithic solid changed (from 19.6 to 372.2 m2 g−1) with the variables involved in the polymerization step. To exemplify the great sorbent potential of the synthesized material, a colorimetric assay based on the retention of methylene blue within the interconnected MWCNT monolithic structure was carried out. Finally, following the positive results, the carbon nanotube-monolithic stirred caps were applied for the determination of chlorophenols in a biological matrix such as human urine, obtaining excellent recovery values (91–98%) and good precision (5.4–9.1%) under optimized extraction conditions.

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References

  1. Intrchom W, Mitra S. Analytical sample preparation, preconcentration and chromatographic separation on carbon nanotubes. Curr Opin Chem Eng. 2017;16:102–14.

    Article  Google Scholar 

  2. Harris PJ. Carbon nanotubes and related structures: new materials for the twenty-first century. AAPT. 2004.

  3. Herrera-Herrera AV, González-Curbelo MÁ, Hernández-Borges J, Rodríguez-Delgado MÁ. Carbon nanotubes applications in separation science: a review. Anal Chim Acta. 2012;734:1–30.

    Article  CAS  PubMed  Google Scholar 

  4. Speltini A, Merli D, Profumo A. Analytical application of carbon nanotubes, fullerenes and nanodiamonds in nanomaterials-based chromatographic stationary phases: a review. Anal Chim Acta. 2013;783:1–16.

    Article  CAS  PubMed  Google Scholar 

  5. Liu L, Ma W, Zhang Z. Macroscopic carbon nanotube assemblies: preparation, properties, and potential applications. Small. 2011;7:1504–20.

    Article  CAS  PubMed  Google Scholar 

  6. Du R, Zhao Q, Zhang N, Zhang J. Macroscopic carbon nanotube-based 3D monoliths. Small. 2015;11:3263–89.

    Article  CAS  PubMed  Google Scholar 

  7. De Marco M, Markoulidis F, Menzel R, Bawaked SM, Mokhtar M, Al-Thabaiti SA, et al. Cross-linked single-walled carbon nanotube aerogel electrodes via reductive coupling chemistry. J Mater Chem A. 2016;4:5385–9.

    Article  Google Scholar 

  8. Schütt F, Signetti S, Krüger H, Röder S, Smazna D, Kaps S, et al. Hierarchical self-entangled carbon nanotube tube networks. Nat Commun. 2017;8:1215.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  9. Zou J, Liu J, Karakoti AS, Kumar A, Joung D, Li Q, et al. Ultralight multiwalled carbon nanotube aerogel. ACS Nano. 2010;4:7293–302.

    Article  PubMed  Google Scholar 

  10. Lalwani G, Kwaczala AT, Kanakia S, Patel SC, Judex S, Sitharaman B. Fabrication and characterization of three-dimensional macroscopic all-carbon scaffolds. Carbon. 2013;53:90–100.

    Article  CAS  PubMed  Google Scholar 

  11. Fresco-Cala B, Cárdenas S. Potential of nanoparticle-based hybrid monoliths as sorbents in microextraction techniques. Anal Chim Acta. 2018.

  12. Iacono M, Connolly D, Heise A. Fabrication of a GMA-co-EDMA monolith in a 2.0 mm id polypropylene housing. Materials. 2016;9:263.

    Article  CAS  PubMed Central  Google Scholar 

  13. Huang X, Chen L, Lin F, Yuan D. Novel extraction approach for liquid samples: stir cake sorptive extraction using monolith. J Sep Sci. 2011;34:2145–51.

    CAS  PubMed  Google Scholar 

  14. Huang X, Wang Y, Yuan D, Li X, Nong S. New monolithic stir-cake-sorptive extraction for the determination of polar phenols by HPLC. Anal Bioanal Chem. 2013;405:2185–93.

    Article  CAS  PubMed  Google Scholar 

  15. Lin F, Nong S, Huang X, Yuan D. Sensitive determination of organic acid preservatives in juices and soft drinks treated by monolith-based stir cake sorptive extraction and liquid chromatography analysis. Anal Bioanal Chem. 2013;405:2077–81.

    Article  CAS  PubMed  Google Scholar 

  16. Lucena R, Simonet B, Cárdenas S, Valcárcel M. Potential of nanoparticles in sample preparation. J Chromatogr A. 2011;1218:620–37.

    Article  CAS  PubMed  Google Scholar 

  17. Jiménez-Soto JM, Lucena R, Cárdenas S, Valcárcel M. Solid phase (micro) extraction tools based on carbon nanotubes and related nanostructures. 2010.

  18. Cárdenas S, Lucena R. Recent advances in extraction and stirring integrated techniques. Separations. 2017;4:6.

    Article  CAS  Google Scholar 

  19. Lucena R. Extraction and stirring integrated techniques: examples and recent advances. Anal Bioanal Chem. 2012;403:2213–23.

    Article  CAS  PubMed  Google Scholar 

  20. Ahlborg UG, Thunberg TM, Spencer HC. Chlorinated phenols: occurrence, toxicity, metabolism, and environmental impact. CRC Crit Rev Toxicol. 1980;7:1–35.

    Article  CAS  Google Scholar 

  21. Honda M, Kannan K. Biomonitoring of chlorophenols in human urine from several Asian countries, Greece and the United States. Environ Pollut. 2018;232:487–93.

    Article  CAS  PubMed  Google Scholar 

  22. Fresco-Cala B, Cárdenas S, Herrero-Martínez JM. Preparation of porous methacrylate monoliths with oxidized single-walled carbon nanohorns for the extraction of nonsteroidal anti-inflammatory drugs from urine samples. Microchim Acta. 2017;6:1863–71.

    Article  CAS  Google Scholar 

  23. Fresco-Cala B, Mompó-Roselló O, Simó-Alfonso EF, Cárdenas S, Herrero-Martínez JM. Carbon nanotube-modified monolithic polymethacrylate pipette tips for (micro)solid-phase extraction of antidepressants from urine samples. Microchim Acta. 2018;185:127.

    Article  CAS  Google Scholar 

  24. Garcia-Valverde MT, Lucena R, Cardenas S, Valcarcel M. In-syringe dispersive micro-solid phase extraction using carbon fibres for the determination of chlorophenols in human urine by gas chromatography/mass spectrometry. J Chromatogr A. 2016;1464:42–9.

    Article  CAS  PubMed  Google Scholar 

  25. Fresco-Cala B, Cárdenas S. Preparation of macroscopic carbon nanohorn-based monoliths in polypropylene tips by medium internal phase emulsion for the determination of parabens in urine samples. Talanta. 2019;198:295–301.

    Article  CAS  PubMed  Google Scholar 

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Acknowledgments

The authors would like to thank the Central Service for Research Support (SCAI) of the University of Córdoba for the service provided to obtain the micrographs.

Funding

Financial support from the Spanish Ministry of Science and Innovation (CTQ2017-83175R) is gratefully recognized.

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Correspondence to Soledad Cárdenas.

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Informed consent was obtained from all individual participants involved in the study. The study has been approved by the appropriate ethics committee (Comité de Ética de la Investigación de Córdoba) and has been performed in accordance with the ethical standards.

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Oliva-Lamarca, Y., Fresco-Cala, B. & Cárdenas, S. Synthesis, characterization, and application of chemically interconnected carbon nanotube monolithic sorbents by photopolymerization in polypropylene caps. Anal Bioanal Chem 411, 3291–3299 (2019). https://doi.org/10.1007/s00216-019-01795-1

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  • DOI: https://doi.org/10.1007/s00216-019-01795-1

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