TY - JOUR A1 - Fischer, Tobias A1 - Dietrich, Paul A1 - Streeck, C. A1 - Ray, S. A1 - Nutsch, A. A1 - Shard, A. A1 - Beckhoff, B. A1 - Unger, Wolfgang A1 - Rurack, Knut T1 - Quantification of variable functional-group densities of mixed-silane monolayers on surfaces via a dual-mode fluorescence and XPS label N2 - The preparation of aminated monolayers with a controlled density of functional groups on silica surfaces through a simple vapor deposition process employing different ratios of two suitable monoalkoxysilanes, (3-aminopropyl)diisopropylethoxysilane (APDIPES) and (3-cyanopropyl)dimethylmethoxysilane (CPDMMS), and advances in the reliable quantification of such tailored surfaces are presented here. The one-step codeposition process was carried out with binary silane mixtures, rendering possible the control over a wide range of densities in a single step. In particular, APDIPES constitutes the functional silane and CPDMMS the inert component. The procedure requires only small amounts of silanes, several ratios can be produced in a single batch, the deposition can be carried out within a few hours and a dry atmosphere can easily be employed, limiting self-condensation of the silanes. Characterization of the ratio of silanes actually bound to the surface can then be performed in a facile manner through contact angle measurements using the Cassie equation. The reliable estimation of the number of surface functional groups was approached with a dual-mode BODIPY-type fluorescence label, which allows quantification by fluorescence and XPS on one and the same sample. We found that fluorescence and XPS signals correlate over at least 1 order of magnitude, allowing for a direct linking of quantitative fluorescence analysis to XPS quantification. Employment of synchrotron-based methods (XPS; reference-free total reflection X-ray fluorescence, TXRF) made the traceable quantification of surface functional groups possible, providing an absolute reference for quantitative fluorescence measurements through a traceable measurement chain. KW - Oberflächenanalytik KW - Fluoreszenz KW - XPS KW - TXRF KW - Funktionelle Gruppen PY - 2015 U6 - https://doi.org/10.1021/ac503850f SN - 0003-2700 SN - 1520-6882 VL - 87 IS - 5 SP - 2685 EP - 2692 PB - American Chemical Society CY - Washington, DC AN - OPUS4-34470 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -