En route to traceable reference standards for surface group quantifications by XPS, NMR and fluorescence spectroscopy.

The fluorine content of polymer particles labelled with 2,2,2-trifluoroethylamine was reliably quantified with overlapping sensitivity ranges by XPS and solid-state NMR. This provides a first step towards reference materials for the metrological traceability of surface group quantifications. The extension of this concept to fluorescence spectroscopy is illustrated.

"EASY: A simple tool for simultaneously removing background, deadtime and acoustic ringing in quantitative NMR spectroscopy. Part II: Improved ringing suppression, application to quadrupolar nuclei, cross polarisation and 2D NMR".

A simple experiment for Elimination of Artifacts in NMR SpectroscopY (EASY) was introduced in Part I, and it was shown that NMR probe background signals, spectral distortions due to deadtime effects, and acoustic ringing can be eliminated simultaneously from solid-state NMR spectra. In this Part II, it is shown that acoustic ringing suppression can be improved up to one order of magnitude compared to the original EASY pulse sequence by inserting a delay τ between the two data acquisition scans of the EASY pulse sequence. The achievable ringing suppression depends on the length of this delay and is limited by the spin-lattice relaxation time T1. Furthermore, EASY is considered in conjunction with NMR of quadrupolar nuclei. For strong second-order broadening, EASY can be used to acquire either pure central transition MAS patterns or pure satellite transition NMR spectra. Two further modifications to EASY are introduced. One concerns improved ringing artifact suppression in experiments in which the central transition NMR signal is amplified by Rotor Assisted Population Transfer (RAPT). The second EASY modification enables the acquisition of quantitative NMR spectra if signals with different quadrupole coupling constants are present. In addition, acoustic ringing and (11)B stator signals are removed. Finally, it is demonstrated that the basic idea of EASY for removing ringing artifacts can be realized for heteronuclear one-dimensional and hetero- and homo-nuclear multi-dimensional NMR experiments using extended phase cycling. (15)N{(1)H} CPMAS and (15)N 2D Exchange NMR spectroscopy are considered as examples.

EASY: a simple tool for simultaneously removing background, deadtime and acoustic ringing in quantitative NMR spectroscopy--part I: basic principle and applications.

Elimination of Artifacts in NMR SpectroscopY (EASY) is a simple but very effective tool to remove simultaneously any real NMR probe background signal, any spectral distortions due to deadtime ringdown effects and -specifically- severe acoustic ringing artifacts in NMR spectra of low-gamma nuclei. EASY enables and maintains quantitative NMR (qNMR) as only a single pulse (preferably 90°) is used for data acquisition. After the acquisition of the first scan (it contains the wanted NMR signal and the background/deadtime/ringing artifacts) the same experiment is repeated immediately afterwards before the T1 waiting delay. This second scan contains only the background/deadtime/ringing parts. Hence, the simple difference of both yields clean NMR line shapes free of artefacts. In this Part I various examples for complete (1)H, (11)B, (13)C, (19)F probe background removal due to construction parts of the NMR probes are presented. Furthermore, (25)Mg EASY of Mg(OH)2 is presented and this example shows how extremely strong acoustic ringing can be suppressed (more than a factor of 200) such that phase and baseline correction for spectra acquired with a single pulse is no longer a problem. EASY is also a step towards deadtime-free data acquisition as these effects are also canceled completely. EASY can be combined with any other NMR experiment, including 2D NMR, if baseline distortions are a big problem.

Metal fluoride-based transparent nanocomposites with low refractive indices.

The utilisation of magnesium and aluminium fluoride nanoparticles in the preparation of transparent composites leading to materials with superior properties was investigated. Nanoscopic magnesium and aluminium fluoride has been prepared by the fluorolytic sol-gel route from the alkoxides and was surface modified by the reaction with trifluoroacetic acid or perfluorobutyric acid. IR spectroscopic experiments of the xerogels and crystal structure analysis of a trinuclear [Mg3(µ3F)(µ-TFA)6(OCH3)2(py)](3-) cluster unit indicate that the carboxylate group is bound to the particle surface in a monodentate or bidentate bridging fashion. These particles were successfully incorporated into acrylate polymers with up to 40 wt% content to give fully transparent material. Ellipsometry and m-line measurements of thin films show the reduction of the refractive index of composite films with increasing metal fluoride filler content.