Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheres

Large-sized mesoporous silica spheres loaded with different amounts of ZnO were prepared for the selective and efficient collection of nitrogen-containing compounds from air by in-tube extraction (ITEX) system. Commercial micrometer-sized chromatographic silica beads were modified using the pseudomo...

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Main Authors: Eka Dian Pusfitasari, Cristina Youngren, Jose Ruiz-Jimenez, Saara Sirkiä, Jan-Henrik Smått, Kari Hartonen, Marja-Liisa Riekkola
Format: Article
Language:English
Published: Elsevier 2023-11-01
Series:Journal of Chromatography Open
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S2772391723000051
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author Eka Dian Pusfitasari
Cristina Youngren
Jose Ruiz-Jimenez
Saara Sirkiä
Jan-Henrik Smått
Kari Hartonen
Marja-Liisa Riekkola
author_facet Eka Dian Pusfitasari
Cristina Youngren
Jose Ruiz-Jimenez
Saara Sirkiä
Jan-Henrik Smått
Kari Hartonen
Marja-Liisa Riekkola
author_sort Eka Dian Pusfitasari
collection DOAJ
description Large-sized mesoporous silica spheres loaded with different amounts of ZnO were prepared for the selective and efficient collection of nitrogen-containing compounds from air by in-tube extraction (ITEX) system. Commercial micrometer-sized chromatographic silica beads were modified using the pseudomorphic transformation approach to produce a material with narrow (2.7 nm) mesopores, while the spherical morphology of the particles was retained. The pores were infiltrated with zinc nitrate salt, which was converted to amorphous ZnO via mild thermal treatments at 300 °C. The ZnO infiltration process did not affect the morphology of the particles, but the available surface area decreased with each infiltration cycle. Sampling selectivity and efficiency were increased with the number of infiltration cycles, but problems related to the mechanical stability of the packed ITEX or backpressure were observed when the number of ZnO infiltration cycles was higher than 2. The large particle size of these materials (∼5.0 µm) decreased the backpressure on the ITEX without affecting the sampling selectivity and efficiency. Among nitrogen-containing compounds studied, sampling repeatability (n = 10) ranged between 2.4 (triethylamine) and 16.8% (isobutylamine). ITEX packing reproducibility (n = 3) ranged from 4.8 (pyridine) to 19.4% (isobutylamine). The performance of ITEX sampling devices packed with the material prepared was evaluated for targeted and untargeted analysis of nitrogen-containing compounds in air. Linear regression was used for their quantification in targeted analysis (r2 > 0.995), and the lowest LOD and LOQ values 6.6 and 21.8 ng l-1 were achieved for pyridine. Dipropylamine had the largest linear range from 23.6 to 3194.7 ng l-1. Partial least squared regression was used for the semi-quantification of the compounds identified using untargeted analysis (slope and bias equal to 1 and 0, respectively using full cross validation and Deming regression). The applicability of the ITEX systems with new sorbent materials for the analysis of nitrogen-containing compounds in indoor air, cigarette smoke and outdoor air was demonstrated. The lowest concentration was 0.7 ng l-1 for 1-nitropentane in outdoor air and the highest 1580.4 ng l-1 for acetonitrile in cigarette smoke.
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spelling doaj.art-5469255c1a824369bc29ca64c67be7dd2023-06-18T05:04:01ZengElsevierJournal of Chromatography Open2772-39172023-11-013100081Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheresEka Dian Pusfitasari0Cristina Youngren1Jose Ruiz-Jimenez2Saara Sirkiä3Jan-Henrik Smått4Kari Hartonen5Marja-Liisa Riekkola6Department of Chemistry, P.O. Box 55, FI-00014 University of Helsinki, Finland; Institute for Atmospheric and Earth System Research, Chemistry, Faculty of science, P.O. Box 55, FI-00014 University of Helsinki, FinlandDepartment of Chemistry, P.O. Box 55, FI-00014 University of Helsinki, FinlandDepartment of Chemistry, P.O. Box 55, FI-00014 University of Helsinki, Finland; Institute for Atmospheric and Earth System Research, Chemistry, Faculty of science, P.O. Box 55, FI-00014 University of Helsinki, FinlandLaboratory of Molecular Science and Engineering, Åbo Akademi University, Henriksgatan 2, FI-20500 Turku, FinlandLaboratory of Molecular Science and Engineering, Åbo Akademi University, Henriksgatan 2, FI-20500 Turku, FinlandDepartment of Chemistry, P.O. Box 55, FI-00014 University of Helsinki, Finland; Institute for Atmospheric and Earth System Research, Chemistry, Faculty of science, P.O. Box 55, FI-00014 University of Helsinki, Finland; Corresponding authors.Department of Chemistry, P.O. Box 55, FI-00014 University of Helsinki, Finland; Institute for Atmospheric and Earth System Research, Chemistry, Faculty of science, P.O. Box 55, FI-00014 University of Helsinki, Finland; Corresponding authors.Large-sized mesoporous silica spheres loaded with different amounts of ZnO were prepared for the selective and efficient collection of nitrogen-containing compounds from air by in-tube extraction (ITEX) system. Commercial micrometer-sized chromatographic silica beads were modified using the pseudomorphic transformation approach to produce a material with narrow (2.7 nm) mesopores, while the spherical morphology of the particles was retained. The pores were infiltrated with zinc nitrate salt, which was converted to amorphous ZnO via mild thermal treatments at 300 °C. The ZnO infiltration process did not affect the morphology of the particles, but the available surface area decreased with each infiltration cycle. Sampling selectivity and efficiency were increased with the number of infiltration cycles, but problems related to the mechanical stability of the packed ITEX or backpressure were observed when the number of ZnO infiltration cycles was higher than 2. The large particle size of these materials (∼5.0 µm) decreased the backpressure on the ITEX without affecting the sampling selectivity and efficiency. Among nitrogen-containing compounds studied, sampling repeatability (n = 10) ranged between 2.4 (triethylamine) and 16.8% (isobutylamine). ITEX packing reproducibility (n = 3) ranged from 4.8 (pyridine) to 19.4% (isobutylamine). The performance of ITEX sampling devices packed with the material prepared was evaluated for targeted and untargeted analysis of nitrogen-containing compounds in air. Linear regression was used for their quantification in targeted analysis (r2 > 0.995), and the lowest LOD and LOQ values 6.6 and 21.8 ng l-1 were achieved for pyridine. Dipropylamine had the largest linear range from 23.6 to 3194.7 ng l-1. Partial least squared regression was used for the semi-quantification of the compounds identified using untargeted analysis (slope and bias equal to 1 and 0, respectively using full cross validation and Deming regression). The applicability of the ITEX systems with new sorbent materials for the analysis of nitrogen-containing compounds in indoor air, cigarette smoke and outdoor air was demonstrated. The lowest concentration was 0.7 ng l-1 for 1-nitropentane in outdoor air and the highest 1580.4 ng l-1 for acetonitrile in cigarette smoke.http://www.sciencedirect.com/science/article/pii/S2772391723000051Nitrogen containing compoundsZinc oxidePseudomorphic transformationIn tube extractionAir samples
spellingShingle Eka Dian Pusfitasari
Cristina Youngren
Jose Ruiz-Jimenez
Saara Sirkiä
Jan-Henrik Smått
Kari Hartonen
Marja-Liisa Riekkola
Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheres
Journal of Chromatography Open
Nitrogen containing compounds
Zinc oxide
Pseudomorphic transformation
In tube extraction
Air samples
title Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheres
title_full Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheres
title_fullStr Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheres
title_full_unstemmed Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheres
title_short Selective and efficient sampling of nitrogen-containing compounds from air by in-tube extraction devices packed with zinc oxide-modified mesoporous silica microspheres
title_sort selective and efficient sampling of nitrogen containing compounds from air by in tube extraction devices packed with zinc oxide modified mesoporous silica microspheres
topic Nitrogen containing compounds
Zinc oxide
Pseudomorphic transformation
In tube extraction
Air samples
url http://www.sciencedirect.com/science/article/pii/S2772391723000051
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