3-Dimensional X-ray microtomography methodology for characterization of monolithic stationary phases and columns for capillary liquid chromatography - A tutorial

Author(s)

da Silva, Carla G. A. ^{[1, 2]} ; Grespan Bottoli, Carla Beatriz ^[1] ; Collins, Carol H. ^[1]

Affiliation

^[1] Univ Estadual Campinas, Inst Chem, BR-13083970 Campinas, SP - Brazil

^[2] Univ Fed Mato Grosso, Dept Chem, BR-78060900 Cuiaba - Brazil

• Document type: Review article
• Source: Analytica Chimica Acta; v. 991, p. 30-45, OCT 23 2017.
• Web of Science Citations: 0

Abstract

In this tutorial we describe a fast, nondestructive, three-dimensional (3-D) view approach to be used in morphology characterization of capillary monoliths and columns by reconstruction from X-ray microtomography (XMT) obtained by acquiring projection images of the sample from a number of different directions. The method comprises imaging acquisition, imaging reconstruction using specific algorithms and imaging analysis by generation of a 3-D image of the sample from radiographic images. The 3-D images show the morphological data for bulk macropore space and skeleton connectivity of the monoliths and were compared with other images from imaging techniques such as scanning electron microscopy (SEM) and field emission scanning electron microscopy (FESEM) and with chromatographic performance. The 3-D XMT methodology is applicable for organic and inorganic capillary chromatographic monolithic materials and it allows the acquisition of many hundreds (in our case 1001 projections) of longitudinal and cross-sectional images in a single session, resolving morphological details with a 3D-view of the monolithic structure, inclusive inside the column in a sectional structure with volume (three dimensions) when compared to the sectional structure area (with only two dimensions) when using SEM and FESEM techniques. (C) 2017 Elsevier B.V. All rights reserved. (AU)

• FAPESP's process: 12/23518-2 - Preparation of monolithic capillary columns based on poly(methyloctylsiloxane) thermally immobilized onto silica and mixed oxides for use in capillary liquid chromatography
• Grantee: Carla Grazieli Azevedo da Silva
• Support Opportunities: Scholarships in Brazil - Post-Doctoral
• FAPESP's process: 13/25933-0 - Preparation of silica and mixed oxides monoliths for use in capillary liquid chromatography
• Grantee: Carla Beatriz Grespan Bottoli
• Support Opportunities: Regular Research Grants
• FAPESP's process: 08/57805-2 - Institute of Bioanalytics
• Grantee: Lauro Tatsuo Kubota
• Support Opportunities: Research Projects - Thematic Grants