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@article{1389321,
author = {Manakhov, Anton and Čechal, Jan and Michlíček, Miroslav and Shtansky, Dmitry V.},
article_location = {Amsterdam},
article_number = {August},
doi = {http://dx.doi.org/10.1016/j.apsusc.2017.04.127},
keywords = {Amine layers; APTES; Derivatization; Plasma polymers; XPS},
language = {eng},
issn = {0169-4332},
journal = {Applied Surface Science},
title = {Determination of NH2 concentration on 3-aminopropyl tri-ethoxy silane layers and cyclopropylamine plasma polymers by liquid-phase derivatization with 5-iodo 2-furaldehyde},
url = {http://www.sciencedirect.com/science/article/pii/S0169433217311546},
volume = {414},
year = {2017}
}
TY - JOUR
ID - 1389321
AU - Manakhov, Anton - Čechal, Jan - Michlíček, Miroslav - Shtansky, Dmitry V.
PY - 2017
TI - Determination of NH2 concentration on 3-aminopropyl tri-ethoxy silane layers and cyclopropylamine plasma polymers by liquid-phase derivatization with 5-iodo 2-furaldehyde
JF - Applied Surface Science
VL - 414
IS - August
SP - 390-397
EP - 390-397
PB - ELSEVIER SCIENCE BV
SN - 01694332
KW - Amine layers
KW - APTES
KW - Derivatization
KW - Plasma polymers
KW - XPS
UR - http://www.sciencedirect.com/science/article/pii/S0169433217311546
L2 - http://www.sciencedirect.com/science/article/pii/S0169433217311546
N2 - The quantification of concentration of primary amines, e.g. in plasma polymerized layers is a very important task for surface analysis. However, the commonly used procedure, such as gas phase derivatization with benzaldehydes, shows several drawbacks, the most important of which are the side reaction effects. In the present study we propose and validate a liquid phase derivatization using 5-iodo 2-furaldehyde (IFA). It was demonstrated that the content of NH2 groups can be determined from the atomic concentrations measured by X-ray photoelectron spectroscopy (XPS), in particular from the ratio of I 3d and N ls peak intensities. First, we demonstrate the method on a prototypical system such as 3-aminopropyl triethoxy silane (APTES) layer. Here the XPS analysis carried out after reaction of APTES layer with IFA gives the fraction of primary amines (NH2/N) of 38.3 +/- 7.9%. Comparing this value with that obtained by N ls curve fitting of APTES layer giving 40.9 +/- 9.5% of amine groups, it can be concluded that all primary amines were derivatized by reaction with IFA. The second system to demonstrate the method comprises cyclopropylamine (CPA) plasma polymers that were free from conjugated imines. In this case the method gives the NH2 fraction similar to 8.5%. This value is closely matching the NH2/N ratio estimated by 4-trifluoromethyl benzaldehyde (TFBA) derivatization. The reaction of IFA with CPA plasma polymer exhibiting high density of conjugated imines revealed the NH2/N fraction of similar to 10.8%. This value was significantly lower compared to 17.3% estimated by TFBA derivatization. As the overestimated density of primary amines measured by TFBA derivatization is probably related to the side reaction of benzaldehydes with conjugated imines, the proposed IFA derivatization of primary amines can be an alternative procedure for the quantification of surface amine groups.
ER -
MANAKHOV, Anton, Jan ČECHAL, Miroslav MICHLÍČEK and Dmitry V. SHTANSKY. Determination of NH2 concentration on 3-aminopropyl tri-ethoxy silane layers and cyclopropylamine plasma polymers by liquid-phase derivatization with 5-iodo 2-furaldehyde. \textit{Applied Surface Science}. Amsterdam: ELSEVIER SCIENCE BV, 2017, vol.~414, August, p.~390-397. ISSN~0169-4332. Available from: https://dx.doi.org/10.1016/j.apsusc.2017.04.127.
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