The implementation of the proposal from the European Chemical Agency (ECHA) to restrict the use of nanoplastics (NP) and microplastics (MP) in consumer products will require reliable methods to perform size and mass-based concentration measurements. Analytical challenges arise at the nanometre to micrometre interface, e.g., 800 nm-10 µm, where techniques applicable at the nanometre scale reach their upper limit of applicability and approaches applicable at the micrometre scale must be pushed to their lower limits of detection. Herein, we compared the performances of nine analytical techniques by measuring the particle size distribution and mass-based concentration of polystyrene mixtures containing both nano and microparticles, with the educational aim to underline applicability and limitations of each technique. Light scattering-based measurements do not have the resolution to distinguish multiple populations in polydisperse samples. Nanoparticle tracking analysis (NTA), nano-flowcytometry (nFCM) and asymmetric flow field flow fractionation hyphenated with multiangle light scattering (AF4-MALS) cannot measure particles in the micrometre range. Static light scattering (SLS) is not able to accurately detect particles below 200 nm, and similarly to transmission electron microscopy (TEM) and flow cytometry (FCM), is not suitable for accurate mass-based concentration measurements. Alternatives for high-resolution sizing and concentration measurements in the size range between 60 nm and 5 µm are tunable resistive pulse sensing (TRPS) and centrifugal liquid sedimentation (CLS), that can bridge the gap between the nanometre and micrometre range.

E-liquids generally contain four main components: nicotine, flavours, water and carrier liquids. The carrier liquid dissolves flavours and nicotine and vaporises at a certain temperature on the atomizer of the e-cigarette. Propylene glycol and glycerol, the principal carriers used in e-liquids, undergo decomposition in contact with the atomizer heating-coil forming volatile carbonyls. Some of these, such as formaldehyde, acetaldehyde and acrolein, are of concern due to their adverse impact on human health when inhaled at sufficient concentrations. The aim of this study was to correlate the yield of volatile carbonyls emitted by e-cigarettes with the temperature of the heating coil. For this purpose, a popular commercial e-liquid was machine-vaped on a third generation e-cigarette which allowed the variation of the output wattage (5-25W) and therefore the heat generated on the atomizer heating-coil. The temperature of the heating-coil was determined by infrared thermography and the vapour generated at each temperature underwent subjective sensorial quality evaluation by an experienced vaper. A steep increase in the generated carbonyls was observed when applying a battery-output of at least 15W corresponding to 200-250°C on the heating coil. However, when considering concentrations in each inhaled puff, the short-term indoor air guideline value for formaldehyde was already exceeded at the lowest wattage of 5W, which is the wattage applied in most 2nd generation e-cigarettes. Concentrations of acetaldehyde in each puff were several times below the short-term irritation threshold value for humans. Acrolein was only detected from 20W upwards. The negative sensorial quality evaluation by the volunteering vaper of the vapour generated at 20W demonstrated the unlikelihood that such a wattage would be realistically set by a vaper. This study highlights the importance to develop standardised testing methods for the assessment of carbonyl-emissions and emissions of other potentially harmful compounds from e-cigarettes. The wide variety and variability of products available on the market make the development of such methods and the associated standardised testing conditions particularly demanding.

Electronic cigarettes have achieved growing popularity since their introduction onto the European market. They are promoted by manufacturers as healthier alternatives to tobacco cigarettes, however debate among scientists and public health experts about their possible impact on health and indoor air quality means further research into the product is required to ensure decisions of policymakers, health care providers and consumers are based on sound science. This study investigated and characterised the impact of 'vaping' (using electronic cigarettes) on indoor environments under controlled conditions using a 30m(3) emission chamber. The study determined the composition of e-cigarette mainstream vapour in terms of propylene glycol, glycerol, carbonyls and nicotine emissions using a smoking machine with adapted smoking parameters. Two different base recipes for refill liquids, with three different amounts of nicotine each, were tested using two models of e-cigarettes. Refill liquids were analysed on their content of propylene glycol, glycerol, nicotine and qualitatively on their principal flavourings. Possible health effects of e-cigarette use are not discussed in this work. Electronic cigarettes tested in this study proved to be sources for propylene glycol, glycerol, nicotine, carbonyls and aerosol particulates. The extent of exposure differs significantly for active and passive 'vapers' (users of electronic cigarettes). Extrapolating from the average amounts of propylene glycol and glycerol condensed on the smoking machine filter pad to the resulting lung-concentration, estimated lung concentrations of 160 and 220mgm(-3) for propylene glycol and glycerol were obtained, respectively. Vaping refill liquids with nicotine concentrations of 9mgmL(-1) led to vapour condensate nicotine amounts comparable to those of low-nicotine regular cigarettes (0.15-0.2mg). In chamber studies, peak concentrations of 2200μgm(-3) for propylene glycol, 136μgm(-3) for glycerol and 0.6μgm(-3) for nicotine were reached. Carbonyls were not detected above the detection limits in chamber studies. Particles in the size range of 20nm to 300nm constantly increased during vaping activity and reached final peak concentrations of 7×10(6)particlesL(-1). Moreover, the tested products showed design flaws such as leakages from the cartridge reservoirs. Possible long term effects of e-cigarettes on health are not yet known. E-cigarettes, the impact of vaping on health and the composition of refill liquids require therefore further research into the product characteristics. The consumers would benefit from harmonised quality and safety improvements of e-cigarettes and refill liquids.

The measurement of physicochemical properties of polydisperse complex biological samples, for example, extracellular vesicles, is critical to assess their quality, for example, resulting from their production and isolation methods. The community is gradually becoming aware of the need to combine multiple orthogonal techniques to perform a robust characterization of complex biological samples. Three pillars of critical quality attribute characterization of EVs are sizing, concentration measurement and phenotyping. The repeatable measurement of vesicle concentration is one of the key‐challenges that requires further efforts, in order to obtain comparable results by using different techniques and assure reproducibility. In this study, the performance of measuring the concentration of particles in the size range of 50–300 nm with complementary techniques is thoroughly investigated in a step‐by step approach of incremental complexity. The six applied techniques include multi‐angle dynamic light scattering (MADLS), asymmetric flow field flow fractionation coupled with multi‐angle light scattering (AF4‐MALS), centrifugal liquid sedimentation (CLS), nanoparticle tracking analysis (NTA), tunable resistive pulse sensing (TRPS), and high‐sensitivity nano flow cytometry (nFCM). To achieve comparability, monomodal samples and complex polystyrene mixtures were used as particles of metrological interest, in order to check the suitability of each technique in the size and concentration range of interest, and to develop reliable post‐processing data protocols for the analysis. Subsequent complexity was introduced by testing liposomes as validation of the developed approaches with a known sample of physicochemical properties closer to EVs. Finally, the vesicles in EV containing plasma samples were analysed with all the tested techniques. The results presented here aim to shed some light into the requirements for the complex characterization of biological samples, as this is a critical need for quality assurance by the EV and regulatory community. Such efforts go with the view to contribute to both, set‐up reproducible and reliable characterization protocols, and comply with the Minimal Information for Studies of Extracellular Vesicles (MISEV) requirements.

A comprehensive physicochemical characterization of heterogeneous nanoplastic (NPL) samples remains an analytical challenge requiring a combination of orthogonal measurement techniques to improve the accuracy and robustness of the results. Here, batch methods, including dynamic light scattering (DLS), nanoparticle tracking analysis (NTA), tunable resistive pulse sensing (TRPS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM), as well as separation/fractionation methods such as centrifugal liquid sedimentation (CLS) and field-flow fractionation (FFF)–multi-angle light scattering (MALS) combined with pyrolysis gas chromatography mass spectrometry (pyGC–MS) or Raman microspectroscopy (RM) were evaluated for NPL size, shape, and chemical composition measurements and for quantification. A set of representative/test particles of different chemical natures, including (i) polydisperse polyethylene (PE), (ii) (doped) polystyrene (PS) NPLs, (iii) titanium dioxide, and (iv) iron oxide nanoparticles (spherical and elongated), was used to assess the applicability and limitations of the selected methodologies. Particle sizes and number-based concentrations obtained by orthogonal batch methods (DLS, NTA, TRPS) were comparable for monodisperse spherical samples, while higher deviations were observed for polydisperse, agglomerated samples and for non-spherical particles, especially for light scattering methods. CLS and TRPS offer further insight with increased size resolution, while detailed morphological information can be derived by electron microscopy (EM)–based approaches. Combined techniques such as FFF coupled to MALS and RM can provide complementary information on physical and chemical properties by online measurements, while pyGC–MS analysis of FFF fractions can be used for the identification of polymer particles (vs. inorganic particles) and for their offline (semi)quantification. However, NPL analysis in complex samples will continue to present a serious challenge for the evaluated techniques without significant improvements in sample preparation. Graphical abstract

Titanium dioxide is a white colourant authorised as food additive E171 in the EU and is applied in a range of food products. Currently the EU specifications for E171 do not refer to the characterisation of particle size distribution; however, this may be requested in the near future. Only a few studies have been published to date reporting data on the size distribution of food grade titanium dioxide. The aim of this study was to characterise the size distribution of titanium dioxide particles contained in eight confectionery products and the pristine titanium dioxide samples used in each of the products. This allowed the direct comparison of the particle size distribution in both the pristine and the extracted materials. By using various analytical techniques, such as transmission electron microscopy, single particle inductively coupled plasma mass spectrometry (sp-ICPMS) and centrifuge liquid sedimentation (CLS) for the characterisation and quantification of the titanium dioxide particle sizes, the impact of the instrumentation on the results was systematically studied. The volume-specific surface area (VSSA) and crystalline structure were also determined for all additives.