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We demonstrate the potential of time-resolved luminescence spectroscopy for the straightforward assessment and in situ monitoring of the stability of upconversion nanocrystals (UCNPs). Therefore, we prepared hexagonal NaYF4:Yb3+,Er3+ UCNPs with various coatings with a focus on phosphonate ligands of different valency, using different ligand exchange procedures, and studied their dissolution behaviour in phosphate-buffered saline (PBS) dispersions at 20 °C and 37 °C with various analytical methods. The amount of the released UCNPs constituting fluoride ions was quantified by potentiometry using a Fluoride ion-sensitive electrode and particle disintegration was confirmed by transmission electron microscopy studies of the differently aged UCNPs. In parallel, the luminescence features of the UCNPs were measured with special emphasis on the lifetime of the sensitizer emission to demonstrate its suitability as Screening parameter for UCNP stability and changes in particle composition. The excellent correlation between the changes in luminescence lifetime and fluoride concentration highlights the potential of our luminescence lifetime method for UCNP stability screening and thereby indirect monitoring of the release of potentially hazardous fluoride ions during uptake and dissolution in biological systems. Additionally, the developed in situ optical method was used to distinguish the dissolution dynamics of differently sized and differently coated UCNPs.
Material defects in fiber reinforced polymers such as delaminations can rapidly degrade the material properties or can lead to the failure of a component. Pulse thermography (PT) has proven to be a valuable tool to identify and quantify such defects in opaque materials. However, quantification of delaminations within semitransparent materials is extremely challenging. We present an approach to quantify delaminations within materials being semitransparent within the wavelength ranges of the optical excitation sources as well as of the infrared (IR) camera. PT experimental data of a glass fiber reinforced polymer with a real delamination within the material were reconstructed by one dimensional (1D) mathematical models. These models describe the heat diffusion within the material and consider semitransparency to the excitation source as well to the IR camera, thermal losses at the samples surfaces and a thermal contact resistance between the two layers describing the delamination. By fitting the models to the PT data, we were able to determine the depth of the delamination very accurately. Additionally, we analyzed synthetic PT data from a 2D simulation with our 1D-models to show how the thermal contact resistance is influenced by lateral heat flow within the material.
Pure U-[13C18]-labelled cis-zearalenone (cis-ZEA) has been prepared and characterised as internal standard (ISTD) for a reliable quantification of cis-ZEA in contaminated food and feed products. The cis-isomer of the naturally trans-configurated Fusarium mycotoxin zearalenone is often neglected. However, isomerisation easily occurs by exposure of ZEA to (UV-)light. Thus, the applicability of the new cis-ZEA ISTD was demonstrated in a long-term isomerisation study comparing naturally trans-ZEA-contaminated edible oil with spiked edible oil. To estimate the benefits of the newly prepared cis-ZEA ISTD, various approaches to quantify cis-ZEA by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) were compared. As a result, a significant bias was revealed if no appropriate cis-ZEA standards are used. Furthermore, the new ISTD was applied to the analysis of 15 edible oils by stable isotope dilution analysis in combination with HPLC-electrospray ionisation-MS/MS. One of the maize germ oils showed the presence of cis-ZEA above LOD (>0.3 µg/kg), whereas two out of 15 maize germ oils were found to be contaminated with trans-ZEA (range 17.0-31.0 µg/kg).
Established maximum levels for the mycotoxin zearalenone (ZEN) in edible oil require monitoring by reliable analytical methods. Therefore, an automated SPE-HPLC online system based on dynamic covalent hydrazine chemistry has been developed. The SPE step comprises a reversible hydrazone formation by ZEN and a hydrazine moiety covalently attached to a solid phase. Seven hydrazine materials with different properties regarding the resin backbone, pore size, particle size, specific surface area, and loading have been evaluated. As a result, a hydrazine-functionalized silica gel was chosen. The final automated online method was validated and applied to the analysis of three maize germ oil samples including a provisionally certified reference material. Important performance criteria for the recovery (70–120 %) and precision (RSDr <25 %) as set by the Commission Regulation EC 401/2006 were fulfilled: The mean recovery was 78 % and RSDr did not exceed 8 %. The results of the SPE-HPLC online method were further compared to results obtained by liquid&–liquid extraction with stable isotope dilution analysis LC-MS/MS and found to be in good agreement. The developed SPE-HPLC online system with fluorescence detection allows a reliable, accurate, and sensitive quantification (limit of quantification, 30 µg/kg) of ZEN in edible oils while significantly reducing the workload. To our knowledge, this is the first report on an automated SPE-HPLC method based on a covalent SPE approach.
Human factors (HF) are little understood, and particularly in non-destructive testing (NDT) experimental data is rare, samples are often small, and statistical methods are rarely used to evaluate results. HF have been widely implicated in major occurrences of technical failure, for example at North Anna Power Plant and on United Airlines Flight 232. Understanding HF is vital for reliable detection and prevention of failures. Reliability assessments, though known to be affected by intrinsic capability, application factors, and HF, have thus far only concentrated to a sufficient degree on intrinsic capability. The addition of HF to that assessment has proven difficult due to the lack of a method of quantifying HF. This paper presents the first attempt from a psychological perspective to quantify HF from qualitative data.
HF data was derived from qualitative human-oriented Failure Modes and Effects Analysis (Human-FMEA) workshops for visual inspection of tunnels by laser scanning and for ultrasonic testing of welds. Data was collected on human failure modes, causes, consequences and preventive measures, as well as eliciting a risk priority number (RPN). Using this data, a system of quantitative weightings was created to allocate errors to inductively derived HF categories for further allocation to existing HF categorisation models.
This weighting model proved useful for creating quantitative summaries of HF, informing and validating qualitative FMEA results, and comparing existing HF categorisation models. Further potential lies within a planned interface to quantitative reliability assessment methods such as POD (Probability of Detection). While providing quantifications, the method retains a qualitative and holistic nature, can, thus, bridge the gap between psychological and engineering concerns of HF and reliability, contributing to future interdisciplinary work.
In Part II of this Review series on lanthanide-doped photon-upconversion nanoparticles (UCNPs), we present and critically discuss the Performance and suitability of UCNPs as background-free luminescent Reporters in bioimaging and bioanalytical applications. The preparation of a biocompatible nanoparticle surface is an integral step for all life - science-related applications. UCNPs have found their way into a large number of diagnostic platforms, homogeneous and heterogeneous assay formats, and sensor applications. Many bioanalytical detection schemes involve Förster resonance energy transfert (FRET), which is still debated for UCNPs and Needs to be much improved. The Need for dedicated and standardized instruments as well as recent studies on the Dissolution and potential toxicity of UCNPs are addressed. Finally we outline future Trends and challenges in the field of upconversion.
The Erfurt Hebrew Giant Bible and the Experimental XRF Analysis of Ink and Plummet Composition
(2007)
Indirect UV-absorption spectrometry was shown to be a valuable tool for chemical characterization of functionalized carbon nanotubes (CNTs). It complements data from X-ray photoelectron spectroscopy (XPS) or FTIR analysis since it helps to clarify the type and concentration of functional groups. The principles of indirect application of UV-spectrometry and its mathematical interpretation are discussed. Their facile application, together with their adequate sensitivity and high flexibility, make UV-absorption-based approaches a valuable alternative to fluorescence spectrometry. Here, the approach was applied to the chemical analysis of oxidizing substances on CNTs. For this, pristine CNTs of low but finite oxygen content as well as brominated CNTs were analyzed by reaction in suspension with UV-active thiol reagents and a styrene derivative. It was shown that carefully selected reagents allow differentiation and quantification of bromine and generally oxidizing entities like oxygen. For brominated CNTs, it was shown that physisorbed bromine may dominate the overall bromine content.
The amount of grafted poly(acrylic acid) on poly(methyl methacrylate) micro- and nanoparticles was quantified by conductometry, 13C solid-state NMR, fluorophore labeling, a supramolecular assay based on high-affinity binding of cucurbit[7]uril, and two colorimetric assays based on toluidine blue and nickel complexation by pyrocatechol violet. The methods were thoroughly validated and compared with respect to reproducibility, sensitivity, and ease of use. The results demonstrate that only a small but constant fraction of the surface functional groups is accessible to covalent surface derivatization independently of the total number of surface functional groups, and different contributing factors are discussed that determine the number of probe molecules which can be bound to the polymer surface. The fluorophore labeling approach was modified to exclude artifacts due to fluorescence quenching, but absolute quantum yield measurements still indicate a major uncertainty in routine fluorescence-based surface group quantifications, which is directly relevant for biochemical assays and medical diagnostics. Comparison with results from protein labeling with streptavidin suggests a porous network of poly(acrylic acid) chains on the particle surface, which allows diffusion of small molecules (cutoff between 1.6 and 6.5 nm) into the network.
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.