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10.3390/molecules30173545
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This is an early access version, the complete PDF, HTML, and XML versions will be available soon.
Article

Rapid On-Field Monitoring for Odor-Active Homologous Aliphatic Aldehydes and Ketones from Hot-Mix Asphalt Emission via Dynamic-SPME Air Sampling with Online Gas Chromatographic Analysis

by
Stefano Dugheri
1,*,
Giovanni Cappelli
2,
Ilaria Rapi
2,
Riccardo Gori
3,
Lorenzo Venturini
2,
Niccolò Fanfani
2,
Chiara Vita
4,
Fabio Cioni
5,
Ettore Guerriero
6,
Domenico Cipriano
7,
Gian Luca Bartolucci
8,
Luca Di Giampaolo
9,
Mieczyslaw Sajewicz
10,†,
Veronica Traversini
2,11,
Nicola Mucci
2,11 and
Antonio Baldassarre
2,11
1
Department of Life Science, Health, and Health Professions, Link Campus University, 00165 Rome, Italy
2
Department of Experimental and Clinical Medicine, University of Florence, 50134 Florence, Italy
3
Department of Civil and Environmental Engineering, University of Florence, 50139 Florence, Italy
4
QuMAP-PIN Foundation—Prato Campus of the University of Florence, 59100 Prato, Italy
5
Regional Agency for Environmental Protection of Tuscany, 50144 Florence, Italy
6
National Research Council of Italy—Institute on Atmospheric Pollution (CNR-IIA), 00010 Montelibretti, Italy
7
RSE SpA—Energy System Research, 20134 Milan, Italy
8
Department of Neuroscience, Psychology, Drug Area and Child Health (NEUROFARBA), University of Florence, 50139 Florence, Italy
9
Department of Innovative Technologies in Medicine and Dentistry, University of “G. D’Annunzio” Chieti, 66013 Chieti, Italy
10
Institute of Chemistry, University of Silesia, 40006 Katowice, Poland
11
Division of Occupational Medicine, Careggi University Hospital, 50139 Florence, Italy
 
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*
Author to whom correspondence should be addressed.
†
These authors contributed equally to this work.
Molecules 2025, 30(17), 3545; https://doi.org/10.3390/molecules30173545
Submission received: 14 July 2025 / Revised: 25 August 2025 / Accepted: 29 August 2025 / Published: 29 August 2025
(This article belongs to the Special Issue Applications of Solid-Phase Microextraction and Related Techniques, the Second Edition)
Versions Notes

Abstract

Odorous emissions from hot-mix asphalt (HMA) plants are a growing environmental concern, particularly due to airborne aldehydes and ketones, which have low odor thresholds and a strong sensory impact. This study presents a field-ready analytical method for monitoring odor-active volatile compounds. The system uses dynamic solid-phase microextraction (SPME and SPME Arrow) with on-fiber derivatization via O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) and is coupled to gas chromatography–mass spectrometry (GC–MS) for direct detection. A flow-cell sampling unit enables the real-time capture of aliphatic aldehydes and ketones under transient emission conditions. Calibration using permeation tubes demonstrated sensitivity (limits of detection (LODs) below 0.13 μg/m3), recovery above 85% and consistent reproducibility. Compound identity was confirmed using retention indices and fragmentation patterns. Uncertainty assessment followed ISO GUM (Guide to the Expression of Uncertainty in Measurement) standards, thereby validating the method’s environmental applicability. Field deployment 200 m from an HMA facility identified measurable concentrations that aligned with CALPUFF model predictions. The method’s dual-isomer resolution and 10 min runtime make it ideal for responding to time-sensitive odor complaints. Overall, this approach supports regulatory efforts by enabling high-throughput on-site chemical monitoring and improving source attribution in cases of odor nuisance.
Keywords: Hot-Mix Asphalt; odor; SPME; PFBHA Hot-Mix Asphalt; odor; SPME; PFBHA

Share and Cite

MDPI and ACS Style

Dugheri, S.; Cappelli, G.; Rapi, I.; Gori, R.; Venturini, L.; Fanfani, N.; Vita, C.; Cioni, F.; Guerriero, E.; Cipriano, D.; et al. Rapid On-Field Monitoring for Odor-Active Homologous Aliphatic Aldehydes and Ketones from Hot-Mix Asphalt Emission via Dynamic-SPME Air Sampling with Online Gas Chromatographic Analysis. Molecules 2025, 30, 3545. https://doi.org/10.3390/molecules30173545

AMA Style

Dugheri S, Cappelli G, Rapi I, Gori R, Venturini L, Fanfani N, Vita C, Cioni F, Guerriero E, Cipriano D, et al. Rapid On-Field Monitoring for Odor-Active Homologous Aliphatic Aldehydes and Ketones from Hot-Mix Asphalt Emission via Dynamic-SPME Air Sampling with Online Gas Chromatographic Analysis. Molecules. 2025; 30(17):3545. https://doi.org/10.3390/molecules30173545

Chicago/Turabian Style

Dugheri, Stefano, Giovanni Cappelli, Ilaria Rapi, Riccardo Gori, Lorenzo Venturini, Niccolò Fanfani, Chiara Vita, Fabio Cioni, Ettore Guerriero, Domenico Cipriano, and et al. 2025. "Rapid On-Field Monitoring for Odor-Active Homologous Aliphatic Aldehydes and Ketones from Hot-Mix Asphalt Emission via Dynamic-SPME Air Sampling with Online Gas Chromatographic Analysis" Molecules 30, no. 17: 3545. https://doi.org/10.3390/molecules30173545

APA Style

Dugheri, S., Cappelli, G., Rapi, I., Gori, R., Venturini, L., Fanfani, N., Vita, C., Cioni, F., Guerriero, E., Cipriano, D., Bartolucci, G. L., Di Giampaolo, L., Sajewicz, M., Traversini, V., Mucci, N., & Baldassarre, A. (2025). Rapid On-Field Monitoring for Odor-Active Homologous Aliphatic Aldehydes and Ketones from Hot-Mix Asphalt Emission via Dynamic-SPME Air Sampling with Online Gas Chromatographic Analysis. Molecules, 30(17), 3545. https://doi.org/10.3390/molecules30173545

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