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- Fluorescence (3)
- Quantification (3)
- Polymer surface (2)
- SEM (2)
- Surface analysis (2)
- XPS (2)
- Academic Software (1)
- Acridine orange (1)
- Beads (1)
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Organisationseinheit der BAM
We present a novel, simple, and fast colorimetric method to quantify the total number of carboxy groups on polymer microparticle and nanoparticle surfaces. This method exploits that small divalent transition metal cations (M2+ = Ni2+, Co2+, Cd2+) are efficiently bound to these surface functional groups, which allows their extraction by a single centrifugation step. Remaining M2+ in the supernatant is subsequently quantified spectrophotometrically after addition of the metal ion indicator pyrocatechol violet, for which Ni2+ was identified to be the most suitable transition metal cation. We demonstrate that the difference between added and detected M2+ is nicely correlated to the number of surface carboxy groups as determined by conductometry, thereby affording a validated measure for the trueness of this procedure. The variation coefficient of ~5% found in reproducibility studies underlines the potential of this novel method that can find conceivable applications for the characterization of different types of poly(carboxylic acid)-functionalized materials, e.g., for quality control by manufacturers of such materials.
We report a surface analytical study of poly(methyl methacrylate) (PMMA) microparticles (beads) with a grafted shell of poly(acrylic acid) (PAA) with thicknesses up to 4 nm using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS), and near-edge X-ray adsorption fine structure (NEXAFS) spectroscopy. These polymer microparticles were analyzed before and after reaction of the surface carboxyl (CO2H) groups with 2,2,2-trifluoroethylamine (TFEA) to gain a better understanding of methods with use of covalently bound probe molecules for surface group analysis. The results obtained with chemical derivatization XPS using TFEA are discussed in terms of surface quantification of reactive CO2H groups on these PAA-coated microparticles. A labeling yield of about 50% was found for TFEA-derivatized particles with amounts of surface-grafted CO2H groups of 99 µmol/g or more, which is consistent with predicted reaction yields for homogeneously dispersed PAA hydrogels.
We report a two-step process for the immobilization of gold nanocubes (Au-NCs) on a glass surface using a combination of extraction and exchange reaction using poly (sodium 4-styrenesulfonate) (PSS) and trisodium citrate (TSC). Cetyltrimethylammonium chloride (CTAC) stabilized gold nanocubes (CTAC/Au-NCs) synthesized by a microfluidic synthesis procedure were successfully deposited on silane-modified glass substrate after extraction of excess CTAC using chloroform followed by exchange of CTAC to TSC on the surface of Au-NCs. Further, TSC/Au-NCs were found to be highly stable and suitable for microfluidic sensing of different glucose concentrations using localized surface plasmon resonance (LSPR) spectroscopy offering an improved sensitivity (126.37 nm/RIU).