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The overall interest in nanotoxicity, triggered by the increasing use of nanomaterials in the material and life sciences, and the synthesis of an ever increasing number of new functional nanoparticles calls not only for standardized test procedures1,2 and for efficient approaches to screen the potential genotoxicity of these materials, but also for standardized and validated methods for surface analysis.
4,5 The analysis and quantification of surface chemistry is hence in the focus of an increasing number of standardization organizations and interlaboratory comparisons with different analytical methods are being done.5 For the monitoring of nanomaterial synthesis and the fast assessment of the number of functional groups such as carboxyl and amino functionalities, which are very commonly used functionalities in the life sciences, simple and validated methods are needed that can be performed with common laboratory instrumentation. 5,6 Here we provide a brief overview of the ongoing research in division Biophotonics employing quantitative NMR (qNMR), conductometry, and colorimetric and fluorometric optical assays for the determination of the total and the accessible number of carboxyl and amino groups on differently sized polymer and silica nano- and microparticles.5-7
Risk assessment of nanomaterials requires not only standardized toxicity studies but also validated methods for nanomaterial surface characterization with known uncertainties. In this context, a first bilateral interlaboratory comparison on Surface group quantification of nanomaterials is presented that assesses different reporter-free and labeling methods for the quantification of the total and accessible number of amine functionalities on commercially available silica nanoparticles that are widely used in the life sciences. The overall goal of this comparison is the identification of optimum methods as well as achievable measurement uncertainties and the comparability of the results across laboratories. We also examined the robustness and ease of implementation of the applied analytical methods and discussed method-inherent limitations. In summary, this comparison presents a first step toward the eventually required standardization of methods for surface group quantification.
Photoluminescence techniques are amongst the most widely used tools in the life sciences, with new and exciting applications in medical diagnostics and molecular imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from instrument-dependent effects, which are also time-dependent due to aging of instrument-components, and difficulties to measure absolute fluorescence intensities. Moreover, scattering samples require special measurement geometries and emerging optical Reporters with emission > 1000 nm strategies for reliable measurements in the second
diagnostic window or short wavelength infrared (SWIR) for the comparison of material performance and the rational design of new fluorophores with improved properties.
Here, we provide a brief overview over different types of fluorescence standards for instrument calibration and performance control. Also, strategies to versatile method-adaptable liquid and solid fluorescence standards for different fluorescence parameters and applications are presented. This includes spectral emission standards for the traceable determination of the wavelengthdependent spectral responsivity (emission correction curve) of fluorescence measuring devices in the UV/vis/NIR, solid multi-emitter systems for daily instrument performance control, and new standards for the relative determination of the fluorescence quantum yield, the key performance parameter of all emitters. The latter standards enable also performance Control of increasingly used integrating sphere setups.
The surface chemistry of nanomaterials controls their interaction with the environment and biological species and their fate and is hence also relevant for their potential toxicity. This has meanwhile led to an increasing interest in validated and preferably standardized methods for the determination and quantification of surface functionalities on nanomaterials and initiated different standardization projects within ISO/TC 229 and IEC/TC 113 as well as interlaboratory comparisons (ILCs) of different analytical methods for the quantification of surface coatings by OECD. Here we present the results of a first ILC on the quantification of the amount of amino functionalities on differently sized inorganic nanoparticles done by division Biophotonics and the National Research Council of Canada (NRC) and the PWI 19257 on the Characterization and Quantification of Surface Functional Groups and Coatings on Nanoobjects approved by ISO/TC 229 (WG2) in fall 2022 that will result in a VAMAS study on this topic organized by division Biophotonics. Key words: nanoparticles, surface analysis, surface functional groups, quantification, optical assay, qNMR, VAMAS, standardization, ICL, quality assurance, reference material.
The characterization of the optical properties of photoluminescent systems, that scatter, like dispersions of nanoparticles with sizes exceeding about 25 nm or solid nanophosphors is of increasing importance for many applications in the life and material sciences. Examples present nanoscale optical reporters and dye-doped microparticles for bioimaging, fluorescence assays or DNA sequencing as well as nanocrystalline emitters like semiconductor quantum dots and rods or lanthanide-based nanophosphors embedded into solid matrices for solid state lighting, display technologies, or barcoding/security applications. The assessment and comparison of material performance as well as the development of rational design strategies for improved systems require spectroscopic tools, which enable the determination of the signal-relevant optical properties like photoluminescence quantum yields and brightness values.
This encouraged us to built up an integrating sphere setup enabling absolute measurements of photoluminescence spectra and quantum yields of transparent and scattering photoluminescent dispersions and solid samples in different measurement geometries, i.e., direct and indirect illumination and the combination of both geometries and perform first measurements with selected emitters. Here, the design of this setup is presented and first recommendations concerning suitable measurement geometries are given.
Lanthanide-doped photon-upconversion nanoparticles (UCNPs) have been in the focus of many research activities in the material and life sciences over the last 15 years because of their potential to convert light between different spectral regions and their unique photophysical properties. In order to fully exploit the application potential of these fascinating nanomaterials, a number of challenges has to be overcome such as the low brightness particularly of small UCNPs and the reliable quantification of the excitation power density (P)-dependent upconversion luminescence (UCL). Here, the need and requirements on the characterization of the optical properties of UCNPs are discussed with special focus on the reliabiliy and comparability of relative and quantitative luminescence measurements and prerequisites for their standardization.