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  • 1.
    Riboni, Nicolò
    et al.
    Università degli Studi di Parma, Italy.
    Trzcinski, Jakub W.
    Bianchi, Federica
    Massera, Chiara
    Pinalli, Roberta
    Sidisky, Leonard
    Dalcanale, Enrico
    Careri, Maria
    Conformationally blocked quinoxaline cavitand as solid-phase microextraction coating for the selective detection of BTEX in air2016In: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 905, p. 79-84Article in journal (Refereed)
    Abstract [en]

    A tetraquinoxaline cavitand functionalized with methylenoxy bridges at the upper rim is proposed as selective solid-phase microextraction (SPME) coating for the determination of BTEX at trace levels in air. The SPME fibers were characterized in terms of film thickness, morphology, thermal stability and extraction capabilities. An average coating thickness of 35 (±4) μm, a thermal stability up to 350 °C and a good fiber-to-fiber and batch-to-batch repeatability with RSD lower than 15% were obtained. Excellent enrichment factors ranging from 360–700 × 103 were obtained for the investigated compounds. Finally, method validation proved the capabilities of the developed coating for the selective sampling of BTEX, achieving LOD values in the 0.4–1.2 ng m−3 range.

  • 2. Trzciński, Jakub W.
    et al.
    Pinalli, Roberta
    Riboni, Nicolò
    Università di Parma, Italy.
    Pedrini, Alessandro
    Bianchi, Federica
    Zampolli, Stefano
    Elmi, Ivan
    Massera, Chiara
    Uguzzoli, Franco
    Dalcanale, Enrico
    In Search of the Ultimate Benzene Sensor: The EtQxBox Solution2017In: ACS Sensors, ISSN 2379-3694, Vol. 2, no 4, p. 590-598Article in journal (Refereed)
    Abstract [en]

    In this work we report a comprehensive study leading to the fabrication of a prototype sensor for environmental benzene monitoring. The required high selectivity and ppb-level sensitivity are obtained by coupling a silicon-integrated concentration unit containing the specifically designed EtQxBox cavitand to a miniaturized PID detector. In the resulting stand-alone sensor, the EtQxBox receptor acts at the same time as highly sensitive preconcentrator for BTEX and GC-like separation phase, allowing for the selective desorption of benzene over TEX. The binding energies of the complexes between EtQxBox and BTX are calculated through molecular mechanics calculations. The examination of the corresponding crystal structures confirms the trend determined by computational studies, with the number of C–H···N and CH···π interactions increasing from 6 to 9 along the series from benzene to o-xylene. The analytical performances of EtQxBox are experimentally tested via SPME, using the cavitand as fiber coating for BTEX monitoring in air. The cavitand EFs are noticeably higher than those obtained by using the commercial CAR-DVB-PDMS. The LOD and LOQ are calculated in the ng/m3 range, outperforming the commercial available systems in BTEX adsorption. The desired selective desorption of benzene is achieved by applying a smart temperature program on the EtQxBox mesh, which starts releasing benzene at lower temperatures than TEX, as predicted by the calculated binding energies. The sensor performances are experimentally validated and ppbv level sensitivity toward the carcinogenic target aromatic benzene was demonstrated, as required for environmental benzene exposure monitoring in industrial applications and outdoor environment.

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